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* GB785293 (A)

Description: GB785293 (A)

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PATENT SPECIFICATION Inventors: ROBERT ISAAC JAFFEE, HORACE RUSSELL OGDEN and RALPH ARTHUR HAPPE 785,293 Date of Application and filing Complete Specification: Nov 9, 1953. No 30990/53. Complete Specification Published: Oct 23, 1957. Index at acceptance:-Class 82 ( 1), A 8 (A 1: A 2: A 3: B: E: H: J: K: M: N: Q: R: T: U: V: W Y), A 8 Z( 2: 5: 8: 9:12), A 21. International Classification:-C 22 c. COMPLETE SPECIFICATION Improvements in or relating to Weldable Titanium Base Alloys and Welded Articles thereof We, REM-C Ru TITANIUM, INC, a corporation organised under the laws of the State of Pennsylvania, United States of America, of Midland, Pennsylvania, United States of America, do hereby declare the invention, for which we pray that a parent may be granted to us, and the method by which it is to be performed to be particularly described in and by the following statement:- This invention pertains to welded articles made of titanium-base alloys, which articles are characterized in being ductile in both the welded and non-welded portions The invention also pertains to ductile and weldable titanium-base alloys, which may be employed for producing the welded articles aforesaid, said alloys being characterized in

either remaining ductile throughout on welding, or in being rendered ductile throughout by appropriate heat treatments, the latter as applied to certain of the alloys which tend to become embrittled in the weld zones as a result of welding. The efforts to develop titanium-base alloys for commercial applications have resulted in widespread disappointment as regards the attempts to produce welded articles thereof, due to the observed poor ductility in general of the welds This has seriously limited the potential field of industrial applications of such materials Thus, for example, in the June 2, 1952 issue of Aviation Week at page 41, P G De Huff and W S Hazleton comment as follows on this aspect: "Welding of alloyed -1 nium is a more difficult matter The main problem, aside from the embrittling effects of gas contamination, is the quench-hardening of this sheet lmateriall during cooling from the welding temperature Heat treatments designed to soften the hardened structure do lPrics 3 s 6 d l not result in the same ductile microstructure produced by hot working " Now, we have found quite contrary to the general experience of others above indicated, certain types of titanium-base alloys, which remain ductile throughout after welding, and we have further found other types of such alloys which, although subject to embrittlement in the weld portions as a result of welding, can have their ductilities restored by appropriate post-heat treatment, or which can be prevented from undergoing embrittlement by appropriate preheat treatments as more fully described below. Microstructurally the titanium-base alloys may be classified into several types, to-wit: (a) those which have an all-alpha microstructure; (b) those which have an all-beta phase microstructure; (c) those which have a mixed alpha-beta microstructure; and (d) those containing compound-forming alloying elements, which on solidification after welding have a microstructure interspersed with networks of such compounds. As is well known, relatively pure titanium has, at relatively low temperatures a closepacked hexagonal crystal structure known as the alpha phase, which transforms at a temperature of about 8850 C to a body centred cubic crystal structure known as the beta phase. Certain substitutional alloying constituents, among which may be mentioned tin, aluminium, indium, antimony, bismuth, lead and silver, as well as the interstitials, carbon, oxygen and nitrogen, tend to stabilize the alpha phase, creating at room temperature an allalpha phase, and at elevated temperatures a mixed alpha-beta phase field, and, finally at still more elevated temperatures a beta phase field Other substitutional alloying ingredients when added in progressively increasing quanSO 7 tities, stabilize the beta phase at progressively lower temperatures, until either a mixed alphabeta or stable all-beta

phase is obtained at normal or atmospheric temperatures, or the beta phase undergoes a eutectoid reaction, depending on the character and amount of the beta stabilizers added Speaking in the broadest sense, the beta stabilizers are Mn, Mio, Cr, Fe, Cu, V, Zr, W, Cb, Ta, Co and Ni Silicon and beryllium may also be considered as beta stabilizing elements, but their solubilities are relatively small, so that it is equally proper to consider them 'as compoundforming elements Within this broad category, however, only certain of the elements mentioned are suitable for producing mixed-phase alpha-beta alloys, or stable beta alloys These are the elements which have beta-isomorphous diagrams, or which have beta eutectoid diagrams such that the decomposition of the beta phase into eutectoid is so sluggish that the alloys behave like those in a beta-isomorphous system The beta stabilizing elements of this type are Mn, Mo, Cr, Fe, V, Cb, W and Ta Copper does not fit into this group, because the beta phase stabilized by copper always decomposes into eutectoid products, and the same is generally true with respect to the other elements above listed under the broad category of beta stabilizers Zirconium is beta stabilizing only with respect to its effect in lowering;the alpha-to-beta transformation of titanium, and, hence, is not by itself suitable for a mixed-phase alpha-beta alloy. Now we have found in accordance with one aspect of the invention that the titanium-base alloys having an all-alpha or substantially allalpha microstructure are in general amenable to welding without appreciable loss of ductility, throughout the entire or throughout the major portions of the ranges and that such alloys are ductile in cast or wrought condition. Thus, we have found that the titaniumaluminium alloys are weldable without appreciable loss of ductility throughout the entire range of ductility of these alloys per se We have further found that the same is generally true with respect to the titanium-tin alloys except that the alloy range resulting in ductile welds is, in this case, only about two-thirds of the entire range throughout which such alloys are ductile per se We have further found that within, limits, as specified below, the weld ductilities are not seriously impaired by additions of one or more of the interstitials carbon, oxygen and nitrogen. In accordance with the invention there is provided a welded titanium base article which is ductile in both the welded and non-welded portions, consisting of titanium, and oxygen, nitrogen and carbon in amounts up to 03 %y oxygen, up 'to 0 2 % nitrogen, and up to 03 % carbon, and up to 30 % O in total of at least one of the following alpha promoting elements: 0.25 to 7 5 %, aluminium, 0 25 to 16 % O tin, 0 25 to 10 % each of silver and lead, 0 25 to 5 %.

each of bismuth, antimony and indium, and/or at least one of the following beta-promoting elements: 0 1 to 10 %,-o each of columbium, tantalum and zirconium, 0 1 to 30 % vanadium, 0 1 to 15 %,o tungsten, 0 1 to 2 % each of iron and cobalt, 0 1 to 2 5 % copper, 0 1 to 1.5 %,' nickel, 0 1 to 2 5 %,h O 4 to 5 % or 7 5 %'' manganese, 0 1 to 2 5,% or 5 ito 12 5 % chromium, 0 1 to 2 5 %,O or 5 to 15 % 1 O molybdenum, and 0 1 to 1 ' silicon. In substantiation of the foregoing, the following Table I gives the results of welding tests on titanium-aluminium alloys, based on forged, rolled and annealed specimens, arcwelded 'in a helium atmosphere The results are based on comparative bend tests of welded versus non-welded specimens. TABLE I. Ti Base Composition % Al-Bal Ti 1 2 2.5 3 6.5 7.5 1 2 3 4 6 Minimum Bend Radius T Welded 0 1.3 0 0 1.6 0.9 2.3 1.4 1.4 2.2 2.1 2.5 2.1 4.0 Not Welded 0 1.3 1.6 1.5 1.2 1.3 2.1 1.3 1.1 1.8 2.0 2.4 2.8 , , Iodide Base. Commercial Purity Base. i 4,= s O 785,293 785,293 3 With reference to the above data, the wefds are sufficiently ductile if they have a minimum bend of less than 7 T From the data it will be seen that titanium-aluminium alloys have adequate ductility in both welded and nonwelded portions up to 7 5 "', Al. TABLE II. Composition % Sn-Bal Ti 1 13 16 The ductile range for the titanium-tin base alloys extends up to about 23 ' tin Table II below gives comparative bend test results for welded versus non-welded specimens of such 10 alloys. Mlinimum Bend Radius T Welded 1.5 0.2 1.4 0.9 3,4 5.5 Brittle Not Welded 0.8 0.9 1.4 1.4 1.8 1.4 1.S These tests show that the maximum tin content for ductile welds is 16 %'' Sn. The effect of the interstitials on the weld ductilities of titanium-base alloys is shown by TABLE III Composition % Bal Ti. A 1-0 1 O A 1-0 1 0, Al-0 2 02 A 1-0 1 N A 1-0 1 0, Al-0 25 C A 1-0 1 C A 1-0 2 C A 1-0 25 C 4 Al-0 2 C n-0 3 C 0.12 C 2 Sn-0 13 C Sn-0 10 C the comparative bend tests of Table III below wherein the interstitials are added to the alpha alloys of Tables I and II. Minimum Bend Radius T Welded 2.0 2.5 5.5 1.5 1.8 1.9 5.4 4.9 6.0 1.5 5.0 2.8 2.1 2.3 Not Welded 3.1 3.5 5.0 2.4 5.5 1.4 1.8 1.1 0.8 2.7 Thus, the upper interstitial limits for ductile welds are 0 3 % for oxygen, 0 2 %o for nitrogen and 0 3 %' for carbon. The effect on weld ductilities of additions of other alpha promoters to titanium-base 25 alloys is shown by the following Table IV.

Ti Base CP Ti Base I CP 3, I CP , , , , 785,293 TABLE IV. Composition Bal Ti -i Minimum Bend Radius T l Welded Not Welded 2.5 Al-l Ag 2.5 A 1-2 5 Ag 2.5 A 1-5 Ag 2.5 Al-10 Ag A 1-1 Ag A 1-2 5 Ag AI-5 Ag n-1 Ag Sn-2 5 Ag l O Sn-5 Ag l O Sn-10 Ag 2.5 Bi (added) Sn-1 Bi (added) l O Sn-2 5 Bi (added) l O Sn-5 Bi (added) 2.55 b l O Sn-I Sb 1 O Sn-2 55 b n-55 b l O Sn-1 In n-5 In Sn-10 In l O Sn-10 Pb (added) For ductile welds the maximum silver addition is 10 ", for bismuth, antimony and indium, 5 % each, and for lead 10 %. Considering the effect on weld ductility of additions of the various beta promoters above discussed, our experimental investigation has established that the individual elements of this group vary widely in their effects As to certain beta promo-er additions, such as Cb, TAB LE V. Composition X' Bal Ti IO Sn-2 5 Cb n-5 Cb l O Sn-O O Cb l O Sn-2 5 Ta l O Sn-5 Ta l O Sn-1 O Ta n-1 V n-2 5 V l O Sn-5 V l O Sn-l OV n-14 V n-15 V n-1 W n-2 5 W l O Sn-5 W n-IOW n-15 W n-l Zr Sn-2 5 Zr n-5 Zr n-10 Zr Ta, V, W and Zr, we have discovered that ductile welds are obtained over substantially the entire ranges for which such additions produce alloys that are per se ductile in cast or wrought condition This is shown by the test 15 results in the following Table V wherein the specified beta promoter additions are added to a titanium-tin base. Minimum Bend Radius T Welded 1.7 3.5 6.8 0.9 1.8 1.8 2.8 4.8 2.5 2.8 2.0 0.8 1.8 2.6 2.8 1.7 5.3 2.5 2.8 5.0 5.5 N'ot Welded 1.8 2.6 2.6 2.3 1.7 2.8 1.9 1.3 1.8 0 0.3 0.7 2.6 2.7 2.7 5.0 2.8 1.6 1.8 2.5 5.2 1 .: Ti Base CP )3 1.2 1.5 5.5 1.6 2.8 2.3 1.9 2.5 1.5 1.7 4.9 4.3 2.3 6.4 2.4 1.2 1.4 2,6 6.6 1.7 5.8 Brittle 4.6 1.2 1.5 1.6 1.3 1.8 1.5 3.4 1.7 1.5 1.7 2.5 1.1 1.5 2.4 1.5 1.7 2.3 1.5 1.7 1.7 1.9 2.7 2.3 Ti Base CP .1 ,3 , ,3 ,3 ,5 ,1 , As compared to the above, ductile welds are obtained only over relatively narrow ranges for additions of the beta promoters, iron, manganese, cobalt, copper and nickel, as shown by the test results of Table VI below 10 Thus as to this group, the beta promoting additions resulting in ductile welds, are those containing: up to 10 % columbium, up to % tantalum, up to 30 '% vanadium, up to 15 % O tungsten, and up to 10 % zirconium. TABLE VI. Composition % Bal Ti AI-2 51 Fe 2 Fe n-2 Fe n-2 Fe 9 Sn-0 25 Fe 9 Sn-0 5 Fe 9 Sn-1 25 Fe 9 Sn-2 5 Fe 1 O Sn-3 Fe l O Sn-4 Fe n-5 Fe 9 Sn-7 5 Fe Sn-7 5 Fe Mn 1 Sn-5 Mn n-5 Mn 9 Sn-0 25 Mn 9 Sn-0 25 Mn l O Sn-l Mln n-2 Mn 9 Sn-2 5 Mn l O Sn-3 Mn l O Sn-4 Mn n-5 Mn l O Sn-5 Mn n-6 Mn l O Sn-7 Mn l O Sn-8 Mn l O Sn-9 Mn l O Sn-12 Mn A 1-1 Mln AI-2 5 Mn A 1-6 5 Mn A 1-7 5 Mn Al-8 5 Mn Al-10 kin n-l Co Sn-2 5 Co n-5 Co Sn-0 5 Cu 1 O Sn-l Cu Sn-2 5 Cu n-5 Cu l O Sn-l Ni l O Sn-2 5 Ni n-5

Ni Minimum Bend Radius T Welded 4.S 6.2 6.6 5.2 1.5 1.3 5.9 Brittle Brittle Brittle Brittle Brittle Brittle Brittle Brittle Brittle 1.4 1.4 Brittle Brittle Brittle Brittle 2.4 4.4 Brittle Brittle Brittle Brittle Brittle Brittle 2.3 4.9 Brittle 3.7 Brittle Brittle 2.6 Brittle Brittle 4.8 2.2 5.2 Brittle 2.8 Brittle Brittle Not Welded 1.5 1.3 3.6 2.5 2.7 1.6 1.3 2.0 1.5 Brittle Brittle 6.1 1.0 0.8 1.6 1.6 1.6 1.6 1.7 1.2 1.4 1.6 1.7 1.4 1.4 1.2 2.9 3.7 Brittle 4.7 Brittle Brittle 2.7 2.6 Brittle 1.6 2.3 2.6 3.6 1.8 2.6 5.7 For this group of beta promoter additions, ductile welds are obtained for the alloys containing: up to 2 % for each of iron and cobalt, up to 2 5 % for copper, and up to 1 5 % for nickel Manganese is somewhat anomalous in that it has a low range of up to 2 5 %S with an isolated higher range of 4-5 % and 7 5 %. In this respect, manganese is similar to chromium and molybdenum discussed below 20 The effect of additions of the beta promoters chromium and molybdenum on weld ductility is somewhat analogous to that of manganese in Ti Base CP ,3 , ,3 , ,) , , J 3 J} > I> ,3 , , , , CP 3 , ,3 ,3 ,) , ,5 ,3 ,3 ,3 785,293 that each of these three metals provides a lower and an upper range of additions throughout which the alloy remains ductile as welded, these ranges being separated by an inzerS mediate range in which embrittlement occurs. While there may be some embrittling in alloys containing molybdenum or chromium or manganese, even when present in their lower or upper ranges of addition, weld ductility in the alloys may be obtained by preheating or restored by the post-heat treatment described below Table VII below gives tests results for such additions. TAB LE VII. Ti Base Composition % Bal Ti Minimum Bend Radius T Welded Not Welded GP 33 : 3 3 I 1 1 4 Cr n-4 Cr n-4 Cr n-4 Cr 9 Sn-0 25 Cr 9 Sn-0 5 Cr 9 Sn-1 25 Cr l O Sn-2 Cr 9 Sn-2 5 Cr n-5 Cr l O Sn-6 Cr n-8 Cr n-1 O Cr AI-2 5 Cr A 1-4 Cr A 1-6 Cr A 1-7 5 Cr A 1-8 5 Cr A 1-10 Cr A 1-12 Cr Mo 1 Sn-5 Mo n-5 Mo n-5 Mo l S Mn-5 Mo 9 S Sn-0 255 Mo 9 Sn-0 51 Mo 9 Sn-2 5 Mo 9 Sn-7 5 Mo Sn-7 5 Mo n-10 Mo n-10 Mo n-15 Mo A 1-2 5 Mo A 1-61 Mo AI-S Mo A 1-l O Mo AI-1 4 MN 1 o 7 Cr-7 Mo Thus the two ranges for chromium productive of ductile welds in the absence of the mentioned heat treatment, are those containing I 0 1 to 2 5, %' Cr for the lower range and containing 5 to 12 5 ' Cr for the upper range. For molybdenum the lower range is 0 1 to 20 2.5 -, and the upper range from 5 to 15 %' Mi o. Table VIII below gives comparative bend tests for additions of the beta promoter silicon. Brittle Brittle Brittle 1.8 1.5 4.8 Brittle Brittle Brittle 1.5 3.2 4.8 0 2.8 Brittle Brittle Brittle Brittle 6.8 0 5.7 4.7 5.9 2.3 Brittle 1.4 1.4 Brittle 1.7 4.3 0.5 0.4 0 5.7 I 3 rirtlc S.6 4.8 5.0

0.3 0.8 0.5 1.0 1.8 1.6 1.2 1.9 2.1 1.7 0.9 0.7 1.5 0.9 1.6 5.6 0.3 2.2 1.2 0 0 1.0 1.2 1.7 1.8 1.6 1.6 1.7 1.7 1.1 0.2 0.8 0.8 0.S 2.5 1.5 0 785,293 785,293 TABLE VIII. Composition ,, Bal Ti Minimum Bend Radius T Welded Not Welded Sn-0 55 i n-l Si n-25 i Thus the maximum silicon addition productive of ductile welds ls 1 %. The alpha alloys in accordance with the invention which are ductile as welded, may contain as little as 0 25 % of the alpha-promoting elements; while those containing the beta promoters may contain as little as 0 1 % of the beta promoter additions Preferred lower limits are, however, in general 0 5 % for the alpha and/or beta promoter additions, while for tlhcs elements which may be added in relatively large amounts without embrittling the weld, as shown by the above test results, a lower limit of about 1 is preferred. That the test results above set forth which are based on comparative bend tests of welded versus non-welded specimens, are also substantiated by tensile tests on welded joints is shown by the data of Table IX below. TABLE IX Composition Ti Base % Bal Ti Tensile Strength 1000 psi Welded % Elongation in 1 " Not Welded to Reduction in Area Tensile Strength 1000 psi % Elong.ation in 1 " % Reduction in Area 14 47 88 23 , 3 A 1-1 Sn 4 A 1-02 C , 95 n-3 A 1 2 Sn-0 13 C ) 4 Sn-0 13 C , 7 Sn-0 13 C , 995 Sn-0 15 C 124 48 88 25 48 94 38 140 33 88 28 90 22 100 27 119 , 10 Sn-0 10 C , 6 Mn-9 Cr-55 n 7 Cr-7 Mo 142 126 23 113 21 135 8 45 133 43 16 57 14 50 Based on our study of the foregoing experimental results, we have tentatively evolved certain criteria for classifying and segregating those alloys which are ductile or can be made ductile on welding, from those which become permanently embrittled as a result of welding. In submitting these criteria, however, as set forth below, it is to be understood that we do not vouch for their correctness, inasmuch as the experimental results speak for themselves, but merely advance them as a possible basis for observed. explaining the experimental results It thus appears to us that the titanium-base alloys which are ductile as welded, include those having the following characteristics: To be ductile as welded the alloys should be (a) ductile before welding They should (b) preferably have narrow freezing ranges, so that segregation during freezing is minimized Or, if the freezing range is not narrow, the composition ranges covered by the segregation 1 i g I Ti Base CP 7.1 5.2 Brittle 1.5 5.0 7.0 CP 3 A 1 1 i i 785,293 should not include intrinsically brittle compositions The alloys should (c) not harden and occome excessively brittle wnen rapidly cooled through the transtornation

range. Some of the alloys will fail to show ductile welds in the " as welded ' condition, because they fail to meet the criterion (c) pertaining to transformation hardening, although they do meet the other criteria above noted We have also found that the alloys within this latter category which become embrittled as a result of welding, can have their ductilities restored by post-welding heat treatment or brittleness may be prevented and ductility retained by the use of preheat prior to the welding operation. The alloys which we judge to be of this type are those containing the beta-promoting elements chromium and molybdenum as above mentioned And the heat treatment employed for restoring ductility to the weld zones of such alloys for preventing brittleness as the result of welding is one which will restore ductility to such of these beta stabilized alloys as have become hard and brittle in the weld portions as a result of beta transformation. One such heat treatment consists in heating to the beta field, followed by a slow cooling through the transformation range Another such heat treatment is to heat to a relatively high temperature in the alpha-beta field, followed by slow cooling to about 11000 F, and subsequent cooling to room temperature It must be remembered that to be ductile as welded, the alloys must be ductile before welding, and the above pre-heat treatment produces the necessary alloy ductility. We have found that the all-alpha alloys are in general characterized in having, (a) a narrow freezing range, and (b) in undergoing no hardening or embrittling as a result of rapid cooling through the transformation range We conclude that in consequence of these properties, that ductile alpha alloys as a class will be ductile in the as-welded condition The test data presented above show, in general, that the maximum alloy content resulting in ductile welds for such alloys, is slightly less than the maximum alloy content for ductility of these alloys pei' se in the cast or wrought condition The probable explanation for this is segregation Although alpha alloys generally do not segregate much, such segregation as does occur may include intrinsically brittle compositions at the high alpha-stabilizer contents. The beta alloys, i e, those containing substantial amounts of the beta-promoting elements, do not have such constant characteristics as the alpha alloys as regards freezing range and transformation hardening The freezing ranges and transformation hardening characteristics vary widely in the beta alloys Thus. alloys of titanium and the beta promoter chromium have a narrow freezing range and undergo high hardening as a result of transformation at rapid cooling rates Molybdenum produces alloys

having a moderately wide freezing range and a moderate degree of transformation hardening Alloys with any of columbium, tantalum, vanadium, tungsten and zirconium, have narrow to moderately wide freezing ranges and low degrees of transformation hardening On the other hand, alloys with any of the beta promoters iron, manganese, cobalt, copper and nickel, have moderately wide to wide freezing ranges and high degrees of transformation hardening Silicon produces ailoys having a id;e freezing range but a low degree of transformation hardening. We conclude on the basis of these considerations, that the ductile-weld, alloy ranges for the various beta promoter additions may be forecast as follows, as appears to be confirmed by the test results above submitted: ( 1) For the beta promoter additions which produce narrowv to moderately wide freezing ranges and low transformation hardening, such as columbium, tantalum, vanadium, tungsten and zirconium, ductile welds are obtained over the entire range of such alloys that are ductile in cast or wrought condition, except possibly at the highest alloy contents, in certain instance ( 2) For the beta promoter additions which result in a narrow to moderately wide freezing ranges and moderate to high degrees of transformation hardening, such as chromium and molybdenum, ductile welds will be obtained over two alloy ranges, viz, (a) a low alloy range wherein rapid transformation hardening does not occur to any appreciable extent, and (b) a high alloy range wherein little or no transformation occurs due to retention of the beta phase at room temperature In the intermediate ranges the welds can be ductilized by a post-twelding heat treatment or the use of preheat in welding as aforesaid, in order to eliminate rapid transformation hardening and cmbrittling ( 3) For the beta promoting additions resulting in moderately wide to wide freezing ranges and a high degree of transformation-hardening, such as iron, manganese, cobalt, copper and nickel, ductile welds can be obtainel only over a low range of alloy addition This range wherein ductile welds result, may be extended somewhat by the aforesaid post-welding heat treatment or by the use of preheat in welding to eliminate rapid transformation hardening The higher alloy contents are, however, intrinsically brittle in the welded condition, and hence cannot be ductilized by such heat treatments ( 4) For the beta promoter additions resulting in a wide freezing range and a low degree of transformation hardening such as siilcon ductile welds will be obtained only over an alloy addition range which is low enough to avoid segregation into basically brittle compositions during freezing. The basic characteristics of compoundforming alloying additions are: (a) low alpha and beta solubility, (b) lack of rapid-transI denum, and 0 1 to 1,% silicon.

2 A welded titanium base article according to claim 1, containing 0 25 to 7 5 % aluminium and/or 0 25 to 16 %V tin in addition to at least one beta promoting element in the amounts specified. 3 A welded titanium base article accord ng to claims 1 or 2 containing 0 25 to 7 5 no aluminium or 0 25 to 16 % tin and at least one of the following elements: O 25 to 10;,, each of silver and lead, and 0 25 to 5 %') each of bismuth, antimony and indium. 4 A welded titanium base article according to claim 1 containing at least one alpha promoting and at least one beta promoting element in the amounts specified. A welded titanium base article according to claims 1-4, containing O 25 to 7 5 i 1 o aluminium, or 0 25 to 16 %/ tin and at least one of the following beta promoting elements: 0.1 to 10 %o each of columbium, tantalum and zirconium, 0 1 to 30 % vanadium, 0 1 to 15 % tungsten, 0 1 to 2 % each of iron and cobalt, 0.1 to 2 5,%, copper, 0 1 to 1 5,% nickel, 0 1 to 2 5 %O, 4 Jto 5 ,% or 7 5 % manganese, 0 1 to 2.5 %O or 5 to 12 5 % chromium, 0 1 to 2 5 %yo or 5 to 15 % molybdenum and 0 1 to 1 %o silicon. STEVENS, LANGNER, PARRY & ROLLINSON, Chartered Patent Agents, Agents for the Applicants. Reference has been directed in pursuance of Section 9, subsection ( 1) of Patents Act 1949 to Patent Nos 733,882, 725,194, 679,705, 679,434 and 677,413. formation hardening efrects, and (c) a tendency of the compounds to form networks at grain boundaries during freezing Carbon is a good example of an element which is both an alpha stabilizer and a compound former To the extent that the carbon is soluble and acts as an alpha stabilizer, the weld ductility is good To the extent that the carbon content is so high that carbides are formed, with resu Iting formation of carbide networks, the ductility of the welds drops off rapidly Therefore, in so far as concerns these compoundforming alloy additions, such as carbon, boron, sulphur, phosphorus, selenium, tellurium, the alloy ranges wherein ductile welds are obtained are generally quite low. The alloys of 'the invention all have in general good mechanical properties, including high hardness and strength.

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* GB785294 (A)

Description: GB785294 (A) ? 1957-10-23

Improvements relating to apparatus for immersing containers in a liquid

Description of GB785294 (A)

PATENT SPECIFICATION Inventor: -CLAUDE JAGO. Date of filing Complete Spec'fication: March 21 1955. Application Date: Dec 22, 1953 No 35673 /53. Complete Specification Published: Oct 23, 1957. Index at Acceptance -Class 41, A( 2 C 4 X: 5). International Classification:-C 23 b. COMPLETE SPECIFICATION. Improvements relating to Apparatus for Immersing Containers in a Liquid. We, Hoo VER LIMITED, a Company registered under the Laws of Great Britain, of Perivale, Greenford, Middlesex, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:- This invention relates to apparatus for the immersion of an opent mouthed container in a liquid treatment bath, comprising a support and tiltably secured to the support a member to which an open mouthed container may be secured, the member carrying a float, the member and float being arranged so that, when the float is out of the liquid, the member and container will tilt to a downwardly inclined position in which all liquid will pour out of the container, but whilst being immersed in the liquid will be tilted by the buoyancy of the float to an upwardly inclined position in which all gas can escape from the container. The invention is particularly applicable in instances where the treatment bath is of the electrolytic type Thus the invention may be applied to the anodising of containers such as washing machine tubs which are made of aluminium or aluminium alloy. According to the present invention the float is open at the bottom In

a convenient arrangement the container is supported on a rack carried by a conveyor which allows the rack to be lowered into thliquid in the treatment bath. In a preferred arrangement the float is mounted within and rigidly secured in relation to the container, and two containers are lPrice 3 s 6 d l mounted on each rack and each is provided with a float. Containers having re-entrant sides, and in practice those having parallel sides, cannot be immersed in a liquid by a movement solely in one direction without either trapping air within the container when immersed, or lifting liquid when withdrawn. It is also preferable to lower the container into the liquid so that its mouth is at first inclined downwardly so as not to have a tendency to float before the liquid enters it. Thereafter it must be tilted so that its mouth faces upwardly and the liquid can rise to fill it completely without trapping any air. When lifted out of the bath the mouth of the container must face downwardly to allow all the liquid to drain out of it. It has been proposed to operate such apparatus automatically by means of a float connected to the container Such floats have consisted of a closed vessel full of air or other gas, but have suffered from the disadvantage that they are difficult to manufacture and as a result of exposure to electrolytic and other baths may gradually become corroded As a result liquid may leak into the float and cause its buoyancy to be reduced with the result that the apparatus does not function properly. In the apparatus according to the present invention such difficulties are overcome The floats are considerably cheaper to produce and any faults arising in their surface can be easily repaired without the necessity of opening up the float to drain liquid from it as is necessary in previous constructions. Even if there should be a slight leak there is no fear of liquid accumulating in the float as it drains out through the open bottom X Li '_, 785,294 f O 7 %_ 785,294 immediately the container is lifted from the bath. One specific embodiment of the invention will now be described by way of example, v with reference to the accompanying drawings in which:Figure 1 is a perspective view of a rack carrying two washing machine containers and incorporating floats in accordance with the present invention; Figure 2 is a front elevation of the lower end of the rack with the tub removed; Figure 3 is a part perspective view from below and to one side of the rack, with part of the frame cut away to show the open bottom of the float; and Figure 4 is a sectional plan on the lines 4-4 of Figure 2. Thus, as is shown in Figure 1, the container 10 is of generally

rectangular form, having straight sides 11 merging into a curved bottom wall 12 The upper edges of the sides 11 merge into a shoulder 13 and an offset portion 14. As is shown in Figure 1, the containers are mounted in pairs on a vertical rack, generally indicated at 15, one container of each pair being above the other The whole of the rack is protected from the electrolyte of the bath, and from the electrolytic action, by a coating of protective plastic material. The frame of the rack is formed in two separable insulated halves and one half acts as a conductor to the anode and the other to the cathode Thus the frame is constituted by two vertical side rails 16 and 17 having hooks 18 at their upper ends for connection respectively to positive and negative conductors of a conveyor The con4 o veyor lowers the racks successively into the electrolytic bath and carries them along in it for a predetermined period, after which it raises them out of the bath, moves them above the next bath, and lowers them into it for further treatment. The two side rails 16 and 17 of the rack are interconnected at their upper and lower ends by cross pieces 19 and 20 respectively. These are rigidly secured to the positive rail W 16 and detachably connected to the negative rail 17 by clamps 21. Each container 10 is secured to the rack by means of a supporting cage shown clearly in Figure 3 and generally indicated at 22. Each cage comprises a generally rectangular frame 23 of tubular metal having at its lower end an elongated hook 24 and at its upper end a wire clamp 25, the hook and clamp being adapted to engage the underside of the it shoulder 13 of the washing machine container to hold it in Position in the manner indicated in Figure 1. The frame 23 is connected to the supporting rails 16 and 17 by means of a U-shared t 55 bracket generally indicated at 26 and formed in two parts, one of which forms the base 27 of the U and one arm 29 whilst the other part forms the other arm 28 The arms 28 and 29 are connected to the respective supporting rails 16 and 17 through beryllium 70 copper spring strips 30 and 31 which can flex to allow the frame to rock up and down. These strips are also covered with insulating material. The arm 28 of the U-shaped bracket is 73 rigidly connected to one side of the frame 23 without the interposition of insulation, so that the frame is electrically as well as permanently mechanically connected to the positive supporting rail 16 50 Thus it will be appreciated that the frame 23 also acts as a positive conductor, the insulated covering not being applied to the hook 24, and accordingly the container, when mounted in the frame, constitutes the SS anode for the bath. The inturned end of the arm 28 of the bracket has an inward extension

33, and the other side of the frame 23 carries a similar inwardly directed lug 32 The base 27 of 90 the bracket overlies both the extension 33 and lug 32 and is clamped to them by clamps 34 and 35. Thus, when the two supporting rails are to be separated these clamps are released and 95 the arm 28 of the U-shaped bracket and the whole of the frame 23 remain connected to the positive rail 16, whilst the base 27 of the bracket remains connected to the negative rail 17 Whilst it is not shown in Figure 4, l Ot it will be appreciated that each half of the frame 23 is completely covered with insulatina material and accordingly the adjacent surfaces of the parts 27 and 33 will be insulated from one another 10)5 Between the inturned extension 33 of the arm 28 and the lug 32, the base of the Ushaped bracket carries a rearwardly projecting U-shaped stirrup 42, the base of which carries a cathode plate 43 which extends into 110 the container when it is mounted on the rack. As has been mentioned the cage 22 is pivotally mounted on the rack so that, as is shown in Figure 1, the mouth of the con 115 tainer mounted on it faces in a direction inclined downwardly at approximately 20 . This is effected by a counterbalance constituted by the whole of the cage 22 together with a float 44 mounted in the container 120 mouth. The float is mounted between the base 27 of the bracket 26 and the U-shaped stirrup 42 Depending from the stirrup 42 5 S a U-shaped rod 47 to which the float is secured 125by tvo pieces of wire 46 As shown in Figure 3 _ the float is of open-er,-' form t I is arraned so that its onen end or Ces Jownwardcs in a plane at right angles to the mouth of the container. 785,294 The extent to which the cage can pivot either above or below the horizontal is controlled by pairs of L-shaped arms 48 connected to each of the arms 28 and 2-9 Each L-shaped arm has a stop 49 which engages its respective side rail of the rack when the cage is pivoted to a maximum extent in a particular direction. Thus the operation of the apparatus is t: as follows The rack, carrying its pair of containers, is carried along the conveyor to a position above the bath of anodising liquid where the rack is lowered into the bath The first part of the container to be immersed is the lowest part of the rim of its open mouth. As it is progressively lowered it gradually is with liquid Liquid also rises a short way up inside the downwardly facing float, but since there is no outlet for the air it acts as a bell jar and remains mainly filled with air As a result the float and cage no longer counterbalance the container but on the contrary, the float's buoyancy pivots the container about the spring strips 30 and 31 "e so that its mouth faces in a direction inclined upwardly until the upper of the stops 49 engage the rails 16 and 17 of the rack.

This allows all air to escape from the tub and permit it to be filled completely with -30 liquid It is retained in this position throughout its treatment in the bath so that the gases produced inside the container as a result of electrolytic action are also allowed to escape freely At the end of the bath 3 the container rises from the liquid and as it does so it tilts back to its initial downwardly facing position in which all liquid can drain from it back into the bath. The use of the beryllium-copper springs for the pivots when the rack acts as a conductor, avoids metal to metal bearings which cannot be conveniently protected. The float, although held to the cage by the wires 46 is insulated electrically and accordingly it is not necessary to cover it with protective material, the float being made of a material which is not excessively attacked by the electrolyte. The float may alternatively be rigidly con5) nected to the frame in which case it is also covered with the plastic coating. It will be appreciated that the embodiment described is by way of example only The apparatus can be effectively employed in any instances where containers of the type described have to be lowered into a liquid. In another arrangement one float is employed for a frame adapted to carry a number of containers.


* GB785295 (A)

Description: GB785295 (A) ? 1957-10-23

Improvements in or relating to castor wheels


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DE1058851 (B) FR1155109 (A) DE1058851 (B) FR1155109 (A) less Translate this text into Tooltip


The EPO does not accept any responsibility for the accuracy of data and information originating from other authorities than the EPO; in particular, the EPO does not guarantee that they are complete, up-to-date or fit for specific purposes.

We, EMMANUEL KAYE, a British Subject and Jo HN REGINALD SHARP, a British Sub ject, both of Kingsclere Road, Basingstoke Hampshire, do hereby declare the invention S for which we pray that a patent may be granted to us, and the method by which it i to be performed, to be particularly describe( in and by the following statement:- The present invention comprises improve ments in or relating to castor wheels, and i especially concerned with castor wheels fo goods carrying trucks, including fork trucks In trucks which have a single driving wheel for a motor carrying turntable at one end, it has often been found necessary ti provide outriding castor wheels at one o both sides of the driving wheel, as the truck are not correctly positioned The casto wheels serve to prevent the truck from tip ping over but suffer however from th following disadvantages; they cause difficult' in manueuvring on uneven surfaces, as it i possible, provided that the floor on whicl the vehicle is operating is sufficiently un even, to attain a position where the load i supported at the driving end of the trud wholly by the castor wheels, leaving th power-operated driving wheel suspender clear of the floor, yet again overbalancing o the truck can be caused by the castor wheel themselves, if one of them should encounte a projection of size capable of tipping th truck. To overcome these disadvantages, and t reduce the effect of shock loading, the wheel have been connected to the truck chassis b springs However, springs follow a straigli line load-deflection law and if a light sprin is used which is effective on an unlade truck, it will have little stabilizing effec when the truck is loaded; whilst a heav spring capable of stabilizing the laden truc may act as a solid mounting when the truck is unladen. According to the present invention, a castor wheel and mounting

therefor comprise a housing for attachment to the frame s which the castor wheel is to support, a castor d wheel beneath the housing, a castor assembly comprising a wheel axle, an axle-supporting bracket-member and a castoring pivot s mounting therefor within the housing and a r rubber or like resilient cushion disposed in shear in the annular space between the housg ing and the castoring pivot mounting. ve Preferably, the castor pivot mounting comprises a ball race or like member with an upr standing stem attached thereto which stem s enters the housing The stem may be surr rounded by a sleeve, the rubber or the like being bonded to the outside surface of the e sleeve. y A feature of the invention is to provide s a castor wheel and mounting therefor comh prising a castor wheel, a castor assembly comprising a wheel axle, an axle-supporting s bracket-member and a castoring ball bearing k therefor, a non-rotatable stem rigidly cone nected to one race of the ball bearing and d extending upwardly therefrom, a top-plate f connected to the stem and spaced apart from s the said ball bearing in a plane parallel r thereto, a sleeve around the stem, in come bination with a housing for attachment to the element which is to be supported by the o castor wheel, which housing surrounds the ls said sleeve and is spaced therefrom, the said y stem passing through the housing so that the it top-plate thereon may overlie the housing g and a rubber or like material cushion bonded n between the outer surface of the sleeve and t the inner surface of the housing so as to y floatingly connect the castor assembly with k the housing in a manner permitting limited 785,295 PATENT SPECIFICATION Inventor:-DENNIS FREEMAN Date of filing Complete Specification: Feb 8,1955. Application Date: Feb 8, 1954 No 3685154. Complete Specification Published: Oct 23, 1957. Index at Acceptance -Class 52 ( 1), D( 1: 3). International Classification:-A 47 b. COMPLETE SPECIFICATION. Improvements in or relating to Castor Wheels. 785295 movement of the castor wheel and castor assembly relative to the housing. In a preferred construction the housing is provided with an outwardly-directed lip at its uppermost edge and the rubber or like resilient material overlies the outwardlydirected lip so as to form a cushion between the housing and the said top-plate on the said stem, and the ball bearing is provided f with a mounting plate which is rigidly attached to the top of the ball bearing, to which plate the said stem and sleeve are connected. The use of a rubber or like material spring means is in effect quite

different from a steel spring, because its displacement law need not be linear; indeed by varying the shape of the housing and the part of the castor assembly where they engage the rubber or the like, any desired law of resistance can readily be provided. The following is a description by way of example of one construction in accordance with the invention, reference being made to the accompanying drawing which is a side elevation partly in section of a castor wheel and mounting in accordance with the present invention. A castor wheel 10 for a fork truck is mounted beneath the truck chassis 11 on an axle 37 slung between the axle-supporting brackets 12 of a wheel-carrying member 13. The wheel-carrying member is rotatablymounted in a ball bearing 14 of a castoring bearing 15, which in this construction comprises elements 14, 16, 18, 25, hereinafter referred to. The ball bearing 14 is rigidly connected to a mounting plate 16 by counter-sunk screws 17 A castor mounting pin or stem 18 having a boss 19 is secured centrally to the mounting plate 16 and extends upwardly therefrom and is screw-threaded at its outermost end 20 to permit the attachment of a topplate 21 The top-plate 21 has a downwarily depending peripheral skirt 22 and is held in place on the shaft by nut 23 and washer 24. As sleeve 25 is keyed by a Mills pin 26 to the boss 19 of the shaft 18 and extends upwardly and inwardly about the shaft, concentrically therewith, to a point beneath the washer 24. A housing 34 is located in a hole 27 in the truck chassis 11 and is held in place by screws 30 to the underside thereof The housing, which is open at top and bottom, and has an outwardly extending peripheral lip 28, at its top is concentric with the shaft ie O 18 and the sleeve-like member 25 Bonded to the outer surface 32 of the sleeve member and to the inner surface 33 of the housing 34 is a rubber cushion 31 which has flanges 35, 36 overlapping the open ends of n 5 the housing, the upper flange 35 forming a cushion between the lip 28 of the housing and the upper plate 21 on the shaft 18. In operation, when the castor wheel hits a projection in the floor the castor wheel 10 and castoring bearing 15, with its shaft 18 7 i and sleeve 25, and the top-plate 21 move upwardly relative to the housing 34 and truck chassis 11, the movement being damped by the action of the cushion 31, and returns with the same damped action with an added 7, cushioning effect by the flange 35. The cross-sectional shape of the rubber spring-member dictates the spring characteristic of the cushion and can therefor be designed to meet varying requirements 50 Therefore, by altering the cross-section of the cushion 31 and/or by varying the shape of the surfaces 32, 33 to which it adheres, different spring characteristics can be obtained,

that is to say, certain combinations s of shapes and cross-sections will result in a spring-loaded wheel which is lightly sprung at first but which, for a slight further deflection, will become rapidly stiffly sprung, or vice versa 90 It will be clear that a wheel with this variable rate springing has a great advantage over prior wheels as it is free from many of the drawbacks imposed by the prior constructions 95 A further advantage of this form of construction lies in the ability of the castor to move through 180 ' without sideways displacement of the truck chassis, as the castoring axis is able to take up a conical 100 path in the rubber mounting


* GB785296 (A)

Description: GB785296 (A) ? 1957-10-23

A process for the production of fatty acids


A high quality text as facsimile in your desired language may be available amongst the following family members:

FR1098841 (A) NL82494 (C) FR1098841 (A) NL82494 (C) less Translate this text into Tooltip


The EPO does not accept any responsibility for the accuracy of data and information originating from other authorities than the EPO; in particular, the EPO does not guarantee that they are complete,

up-to-date or fit for specific purposes.

CGiPLETE SPECIFICATION A Process for the Production of Fatty Acids We, RUHRCHEMIE A.G., Oberhausen, Holten, Germany, of German nationality, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to he particularly described in and by the following statement: The invention relates to a process for the production of branched-chain fatty acids. It is known to produce primary alcohols by tb e catalytic addition of carbon monoxide and hydrogen to mixtures of isomeric or homologous olefins in the absence or presence of saturated hydrocarbons, the primary alcohols obtained having one more carbon atom in the molecule than the olefins. For further commercial use, the alcohol mixtures obtained in this manner areseparated by distillation. This may result in fractions of narrow boiling range containing branched-chain primary alcohols and saturated hydrocarbons from which the alcohols cannot be separated by simple distillation. These frantions, which are hereinafter referred tn as intermediate fractions. could not hitherto be utilised in an advantageous manner. The intermediate fractions can neither be used as hydrocarbon products because their content of alcohols is too high, hor as alcohol products because their hydrocarbon content is too high. It has now been found, according to the invention, that such an intermediate distillation fraction can be converted in an advantageous manner into valuable branched-chain fatty acids by subjecting the fraction to treatment with a molten alkali metal hydroxide at superatmospheric pressure and at a temperature in the range 250 -350 C., the quantity of alkali metal hvdroxide employed corresponding to or beingslightly in excess of the amount required by the hydroxyl numher of the fraction, separating the hydrocarbons from the oygen-containing product by distillation, injecting water under superatmospheric pressure into the molten oxygen-containing product with agitation of the melt to yield an aqueous paste-like mass of soap, dissolving the paste-like mass in water and treating the solution with a mineral acid to release the fatty acids. The separation of the hydrocarbons by distillation and the injection of water to produce an aqueous, paste-like mass of soap is preferably carried out in the same ?one or vessel as that in which the intermediate fraction is treated with the alkali metal hydroxide, the aqueous, paste-like mass being withdrawn from the zone or vessel ata temperature not in excess of 200 C. prior to solution with water and

decomposition of the soap with mineral acid. whilst the quantity of alkali metal hydroxide emploved is advantageously greater than the quantity theoretically required according to the hydroxyl number of the intermediate fraction, it is preferably not greater than 110% of the theoretical quantity. The reaction of the molten alkali metal hydroxide with the intermediate fraction is advantageously carried out at a pressure greater than 10 kg./sq. cm. and it may, for example, be carried out at a pressure greater thah 50 kg./sq. cm. Thus the hydrogen which is released during the treatment with the alkali metal hydroxide may be continuoualy removed at a pressure greater than 50 kg./sq. cm. The reaction of the alkali metal hydroxide with the intermediate fraction is, however, preferably effected at a, pressure of about 50 kg./sq. cm. The quantity of water injected into the molten product of reaction between tile alkali metal hvdroxide and the intermediate fraction advantageously constitutes from 10% to 50% by weight of the molten mass, and preferably constitutes about 30% by weight of the molten mass. The aqueous, paste-like mass of soap thus obtained may then be removed from the zone or vessel in which the treatment with the molten alkali metal hydroxide is effected, for example, by means of a gas under pressure or by suction. After dissolution of the aqueous, pastelike mass of soap in water, the aqueous solution may be extracted with a waterinsoluble solbent, for example, a hydrocarbon fraction, to remove unsaponifiable constituents before the treatment with mineral acid. A water-soluble alcohol may. with advantage. be added to the aqueous solution prior to the extraction in order to avoid or reduce loss of soaps in lie extraction. The branched-chain fatty acids which may be obtained in accordance with the invention are suitable for various commercial uses. They may, for example, be converted into low pour point ester ails, testile auxiliary agent, cold-resistant plasticizers, or mineral oil additives. The process of the invention thus makes possible the economical conversion into valuable finished products of intermediate fractions which have hjitherto been treated as waste porducts. The process may, for example. be carried out as follows: The mixture of alkali metal hyroxide and intermediate fraction is placed in a pressure-resistant fusion vessel which is advan-tageausly of copper or lined with copper. The pressure vessel is then closed, purged with an inert gas, such as nitrogen, and heated while constantly stirring under an initial pressure of, for example, 1 to 2 kg./cq. cm. gauge. In accordance with the partial pressure of the hydrocarbons present, the pressure in the vessel rises and is furthe

increased by the evolution of hydrogen which commences at about 250 C. After a pressure of about 50 kg./sq. cm. is reached, sufficient hydrogen is allowed to blow off through a pressure relief valve so as to maintain the pressure at about 50 kg./sq. cm. gauge, for example. The reaction is now allowed to proceed to completion whilst the temperature is increased to about 320 c. The hydrogen is removed by completely releasing the pressure, and the hydrocarbons distil as the pressure is reduced. Thus C1, hydrecarbon will distil out of the vessel under a gauge pressure of about 6 kg./sq. cm. at 320 C. As soon as the distillation of hydrocarbons ceases, the distillation is continued by reducing the pressure further whilst maintaining the temperature at the same level. When the intermediate fraction contains hydrocarbons having more than 10 carbon atoms in the molecule, it is desirable to reduce the pressure on the molten mass to below atmospheric in order to ensure that all of such hydrocarbons are removed. After the complete removal of the hydrocarbons, water is injected under superatmospheric pressure into the pressure vessel while the stirring is continued. In this manner, the anhydrous soap which is very hard after solidification, is converted into a soft, water-containing pasty mass. This paste is particularly suitable for processing because the soap in this state can be forced or pumped out of the reaction vesselat temperatures not in excess of 200 C. Moreover, the dissolution of this soap paste in water which is required for precipitating teh branched fatty acids by means of acids, can be effected in the pasty state without difficulty, while the dissolution of an anhydrous soap, even after thorough comminution, requies a long time. The decomposition of the resulting soap by mineral acids for the purpose of recovering free fatty acidsis effected by known processes. The fatty acids may be completely set free by mineral acids. It is possible, if desired, to release part of the fatty acids by means of carbon dioxide. thereby saving a part of the mineral acid required. The branched fatty acid or acids obtained by the process of the invention can be freed from colouring matter by distillation. To obtain chemically pure fatty acids, the aqueous soap solution may, as hereinbefore described, after the admixture of water-soluble alcohols, be extracted with a water-insoluble solvent, for example, a hydrocarbon fraction, thereby removing small portions of unsaponifiable constituents still present. Moreover, it is possible by partial precipitation with mineral acids to remove small amounts of straight-chain fatty acids which may be present in the nnis- ture of branched-chain fatty acids obtained in

accordance with the invenfion. The process of the invention is particularly advantageous for the processing of raw alcohols obtained from olefins obtained by the Fischer-Tropsch synthesis. It is however, also applicable to alcohol mixtures obtained from olefins derived from the other sources. partienlarly olefins which have been formed from paraffins by chlorinationand subsequent dehydrochlorination. Crude alcohol mixtures from plymerized olefins produced from liquid or gaseous unsaturated petroleum hydrocarbons, may also be processed by the process of the invention. The invention is illustrated in the following examples: EX4MPLE 1. 600 grams of a. saturated hydrocarbonalcohol mixture obtained in the recovery by distillation of a C15 alcohol which had been produced by the catalytic addition of water gas to a C14 olefin-containing hydrocarbon mixture (formed by the catalytic hydrogenation of carbon monoxide) and subsequent hydrogenation of the reaction product were placed in an autoclave of 2900 cc. capacity provided with a copper lining and a copper stirrer. This hydrocarbon-alcohol mixture had the following characteristics: Density at 20 C. - - - 0.801 Refractive index nD20 - - 1.4391 Neutralization number - - 0.4 Saponification number - - 4.6 Hydroxyl number - - - 110 Iodine number - - - - 2 Carbonyl number - - - 3 Pour point - - - - - -4 C. 52.2 grams of sodium hydroxide, corresponding to 110% of the hydroxyl number of the hydrocarbon-alcohol mixture, were added to the autoclave. The autoclave was closed, purged twice with nitrogen and the gas space of the autoclave was left with an atmosphere of nitrogen at a gauge pressure of 2 kg./sq. cm. The stirrer was then started and the autoclave heated. At a temperature of 320 C. a pressure of 50 kg./sq. cm. was reached. This pressure was prevented from rising above 50 kg./sq, cm. by opening the needle valve. In this manner, 11 litres (measured at N.T.P) of hydrogen were removed from the pressure vessel. When there was no further tendency for the pressure to rise at 320 C., all of the hydrogen was withdrawn whilst maintainins; the temperature at the same level. The volume of the hydrogen withdrawn was 55 litres (measured at N.T.P.). At a pressure of as low as 6 kg. Isq. cm..

hvdroearbons distilled over from the autoclave. The hydrocarbons were condensed in a cooler and separated from the gaseous products. After atmospheric @ ressure was reached, a vacuum of about 10 mm. Hg. was applied whereupon the remainder of the hydrocarbons distilled off from the reaction product contained in the autoclave. This resulted in 308 grams of oily constituehts, corresponding to 51.4% of the hydrocarbon-alcohol feedstock. Based on the characteristics of the feedstock, a content of neutral oil of 52% was theoretically to be expected. 150. cc. of water were then injected under nitrogen pressure into the autoclave which had meanwhile cooled to 250@ C., whilst the stirring was continued for about a further 10 minutes. The soap paste formed was removed from the autoclave by suction through a discharge pipe which extended down to the bottom of the autoclave. The paste was dissolved in 1500 cc. of water while stirring and mixed with about 6510 cc. of 20% sulphuric acid thereby adjusting the pH valueto 5 and resulting in the separation of a C15 fatty acid mixture as an upper layer. The fatty acid mixture was washed twice with hot water, after which about 300 grams of a finished product remained which had the following characterictics : - Neutralization number - - 227 Saponification number - - 231 Pour point - - - - - - 7 C. The netural oil distilled off had the following characteristics: Density at 20 C. - - - 0.767 Refractive index nD20 - - 1.4300 Hydroxyl number - - - 2 Neutralization number - - 0 Saponification number - - 0.3 EXAMPLE 2. 600 grams of a saturated hydrocarbonalcohol intermediate fraction which had been obtained in the distillation of a C15 alcohol, were placed in the autoclave used in Example 1. The alcohol had been prodyced by the catalytic addition of water gas to olefins and subsequent hydrogenation of the reaction product, whilst the olefins themselves had been obtained by the dehydrochlorination of chlorinated C14 paraffins. The intermediate fraction had the following characteristics: Density at 20 C. - - - 0.804 Neutralization number - - 0.2 Saponification number - - 1.4 Hydroxyl number - - - 104 Iodine number - - - 2

Carbonyl number - - - 12 Refractive index nD20 - - 1.4402 Pour point - - - - 6 C. This intermediate fraction was mixed with 50 grams NaOll and the mixture was further processed in accordance with Example 1. This resulted in 315 grams C14 hydrocarbons having the following characteristics: Density at 20 C. - - - 0.766 Refractive index nD20- 1.4285 Neutralization number - - 0 Hydroxyl number - - - 1 The treatment of the aqueous soap solution with acid resulted in about 290 grams of a C15 fatty acid mixture having the following characteristics: Neutralization number - - 224 Saponification number - 2:31 Hydroxyl number - - - 0 Iodine number - - - - 0 Carbonyl number - - 0 Density at 20 C. - - - 0.883 Refractive index nD20 - - 1.4465 Pour point - - - - - 45 C. What we claim is: 1. A process for the production of branched-chain fatty acids, which comprises subjecting an intermediate distillation fraction containing branched-chain primary alcohols and one or niare saturated aliphatic hydrocarbons and obtained in the distillation of a mixture of alcohols produced by the catalytic addition of carbon monoxide and hydrogen to olefins. to treatment with a molten alkali metal hydroxide at superatmospheric pres. sure and at a temperature in the range 250 -350 C., the quantity of alkali metal hydroxide employed corresponding to or being slightly in excess of the amount required by the bydroxyl number of the intermediate fraction, separating the hydroxarbons from the oxygen-containing product by distillation, injecting water under superatmospheric pressure into the molten oxygen-containing product with agitation of the melt to yield an aqueous paste-like mass of soap dissolving the paste-like mass in water and treating the solution with a mineral acid to release the fatty acids. 2. A process according to Claim 1, in which the quantity of alkali metal hydroxide used is not in excess of 110% of the quantity theoretically required according to the hydroxyl number of the intermediate fraction. .3. A process according to Claim 1 or

Claim 2, in which the treatment with the alkali metal hydroxide, the separation of the hydrocarbons and the injection of water iscarried out in a single zone or vessel, the aqueous paste-like mass being withdrawn from the zone or vessel at a temperature not exceedin 200' C. prior to solution in water. 4. A process according to any one of the preceding claims, in which the aqueous solution of the paste-like mass is extracted with a water-insoluble solvent prior to treatment with the mineral acid. 5. A process according to Claim 4. in which the water-insoluble solbent is a hydrocarbon fraction. 6. A process according to Claim 4 or Claim 5, in which a water-soluble alcohol is added to the aqueous solution of the iaste-like mass prior to the extraction. 7. 9 process according to any one of the preceding claims, in which the treatment with the alkali metal hydroxide is carried out at a pressure greater than 10 kg./sq. cm. S. A process according to Claim 7, in which the treatment is carried out at a pressure of about 50 kg./sq. cm. 9. A process according to any one of Claims 1 to 7, in which the hydrogen which is released during the treatment with the alkali metal hydroxide is continuously removed at a pressure greater than 50 kg./sq. cm. 10. A process according to any one of the preceding claims, in which, after termination of the evolution of the hydrogen released during the treatment with the alkali metal hydroxide, the pressure is reiased to atmospheric pressure. 11. A process according to any one of the preceding claims, in which. when the intermediate fraction contains hydrocarbons having more than 10 carbon atoms in the molecule, the hydrocarbons are removed from the molten mass under subatmospheric pressure. 12. A process according to any one of the preceding claims, in which the quanlily of -a-ater injected constitutes from 10% to @0% by weight of the molten mass. 13. A process according to Claim 12, in which the quantity of water injected constitutes about 30% by weight of the molten mass. 14. A process according to any one of the preceding claims, in which the aqueous paste-like mass is removed from the zone or vessel in which it is produced. 15. a process according to Claim 14, in which the aqueous paste-like mass is removed by a gas under pressure or by suction. 16. A process according to any one of the preceding elaims, in which the treatment with the alkali metal hydroxide is carried out in a copper vessel or copperlined vessel. 17. A process for the production of a branched-chain fatty acid,

substantially as hereinbefore described. 18. A process for the production of branched-chain fatty acids substantially as hereinbefore described with reference to Example 1 or Example 2. 19 A branched-chain fatty acid whenever produced by the process claimed in any preceding claims.

* GB785297 (A)

Description: GB785297 (A) ? 1957-10-23

Improvements in or relating to continuous treatment apparatus


COMPLETE SPECIFICATION. Improvements in or relating to Continuous Treatment Apparatus. I, JOHN ALLEN ELFIN SEABROOK, C/O William Douglas and Sons Limited, Douglas Wharf, Putney, London, S.W.15, formerly of 4 Milner Street, London, S.W.3, a British Subject, do hereby declare the invention, for which I pray that a patent may be granted to me, and the method by which it is to be performed, to be particularly described in and by the following statement: The present invention relates to continuous treatment apparatus. in continuous treatment apparatus use is conventionally made of conveying apparatus. Where articles have to be cooled, frozen, heated, sprayed or otherwise processed within a closed space, the conveyor, upon which the articles are placed or from which the articles are suspended, is caused to travel through a chamber in which the actual processing takes place, the conveyor passing from the outside, into the chamber and then to the outside again. Such a chamber is often referred to as a tunnel, whatever be its shape or size, and this term used hereinafter, means any such chamber convenient to the process envisaged. In a number of continuous treatment processes it is required to perform some preparatory work on the material being processed before

it is passed through the tunnel and conveniently such work is done at a work table at which the operators sit or stand. After such preparatory work, the material is collected by any suitable means and taken to the place where the tunnel is situated. Such arrangements involve much handling of the material and the apparatus takes up a great deal of floor space. It is the specific object of the present invention to remedy these inconveniences and according thereto the processing chamber is integral with a work table which forms the top of the chamber, the conveyor having an upper run passing along and above the work table in front of an operator or operators whereby the material may be loaded on to and removed from the conveyor by the operator or operators without moving from his or their working positions at the table, and the lower run of the conveyor passing through the said chamber. Preferably one or more subsidiary delivery conveyors are additionally provided to run On the surface of the work table, and upon which the material may be placed for delivery to the operators so that they may place it on the main treatment conveyor and upon which the operators may place the material after processing for delivery to another place for example for packing. The material placed on the subsidiary conveyor does not pass through the processing chamber or treatment tunnel at all. In order that the present invention may be more clearly understood, reference will now be made to the accompanying drawings which show, largely in schematic form, an arrangement according to one specific embodiment of the invention by way of example, and in which: Fig. 1 shows a side view with certain parts broken away; Fig. 2 shows a plan view partly in section, along the line Il-Il of Fig. 1; Fig. 3 shows a section along the line III--III of Fig. 1; and Fig. 4 shows a perspective view of one of the carrier members. In the drawings which show apparatus particularly for use in the twisting, cooling or freezing, bunching and packaging of sausages, there is provided a working table 1 that is long in relation to its width, for example, three times as long, and this table is divided longitudinaliy into two portions 2 and 3 respectively which portions are divided for convenience by means of a low metal barrier 4. Operators, who are preferably seated, work along either side of the apparatus. It will be appreciated that the drawings do not show the complete length of the working table, which may, in fact, be as long as desired. The drawing is broken away and shows merely the two end portions of the working table and associated parts. The working table 1 forms the top of a cooling tunnel 5 and is preferably built upon a framework which also forms a support for a

conveyor system, some of the frame members being shown, for example, at 6. Since the shape of the apparatus may be varied within the needs of the potential user, it is not thought necesary to illustrate more fully the framework and casings of the apparatus according to this specific embodiment. At the ends of the working table and cooling tunnel are provided housings 7 and 8 which house sprockets 9 and 10 around which pass the chains of a main chain conveyor system. The sprockets 9 are all driven from a motor 11 which drives a driving shaft 12 by means of a chain or belt 13 and on the driving shaft 12 is provided a plurality of drive gears 14 respectively connected one to each of the gears 19 by means of chains 15. Each gear 19 is connected to a sprocket 9 to drive same. Four sprockets 9 are shown, the outer ones being mounted upon axles 16 secured in any suitable manner to the housing 7 or to a framework upon which the housing is built, and the inner ones being carried by a common shaft 17 that is mounted within the housing 7, for example, upon supporting frame members 18. The gears 19 are also mounted on the stub axles 16 and the shaft 17 respectively. The sprockets 10 are mounted in the housing 8 is a similar fashion but are not driven in this embodiment although they may be driven if desired. Passing around the sprockets 9 and 10 are two pairs of chains 20 and 21. The chains thus form an elongated loop passing over the sprockets 9 and 10 and have an upper run 22 and a lower run 23. The upper run 22 is located above the surface of the working table 1, and the lower run 23 passes into the cooling tunnel 5. Between each pair 20, 21 of chains there is located a plurality of carrier members indicated generally by the reference 24, upon which the material for processing, in this example sausages S, may be hung. Each carrier member, one of which is shown in more detail in the perspective view of Figure 4, comprises a supporting bar 26 transversely carried between its pair of chains and upon this bar 26 is swingably mounted a holding member 27 which is located substantially parallel to its pair of chains, and a plurality of elongated hook members 28 is secured to the holding member 27, the material for processing being hung on the said hook members. The holding member 27 also carries a pair of guide rods 29 transversely arranged with respect thereto, one end of each of these guide rods having a roller 30 located to run on a guide rail 31 mounted adjacent the upper run 22 of the outer chain of each pair. The height of the hooks 28 above the surface of the working table 1 is such that a convenient amount of sausages in strings may be loaded on

to the hooks without the operators leaving their seats, and the length of the hook members transversely to the apparatus is such that an economic load can be mounted upon each of them. In the specific example shown, each hook member 98 is designed to carry five strings of sausages, each string comprising eight sausages weighing one pound but it will, of course, be obvious that the hook members may be designed to carry any form of produce and of any desired size or weight. When the machine is running, the chains 20, 21 are moved in the direction of the arrows A taking the carrier members with them and, owing to the fact that the holding members are swingably mounted upon the supporting bars 26, the said member 27 will maintain a substantially horizontal position whatever be the relative positions between the carrier members and the chains. To this end it is desirable that the hook members 28 be equally loaded so that the members 27 can, in fact, balance in a horizontal position but, in case there may be some slight misbalance, a steering rail 32 is provided within the housing 8 against which the rollers 30 impinge on the upward travel of the carrier members, this steering rail acting to straighten any carrier member that has, in fact, become out of balance during its travel through the cooling tunnel. Mounted within the cooling tunnel are refrigerating coils schematically denoted by the reference numeral 33, and these may be incorporated with fans (not shown) for blowing cooling air by means of suitably shaped baffles (also not shown), on to the strings of sausages S during their passage through the cooling tunnel. The housings 7 and 8 have walls 34, 35 respectively facing the table 1, which are suitably apertured at 34a, 35a to allow the produce to pass thereinto during running of the conveyor and these apertures are made as small as possible so that cold air spillage to the outside is minimised. In point of fact, since cold air is heavies than warm air, it will be found that to.e cold air tends to remain within the cooling tunnel. Between the two rows of operators on either side of the working table and on the surface of the table, there are provided two subsidiary delivery conveyors 36 and 37 which run in the opposite direction to the chain conveyors 20, 21, as is indicated by the arrows B. The delivery conveyors may be belts of any desired kind and may be about 6" wide. They pass over common rollers 38, 39 at the ends of the apparatus, these rollers preferably being covered with crepe rubber or similar material to afford a good frictional contact with the conveyor belts. The roller 39 is driven by means of a motor 40, reduction gearing 40a and a chain 41 passing over a sprocket 42 at one end of the roller 39.

The conveyor belts 36 and 37 extend at either end of the apparatus and into the working surface of two end tables 43, 44 respectively, which tables are supported by means of legs or frames 45, 46. The end work table 43 is used as a receiving table for sausage meat extruded into skins and arriving from a suitable extruding machine (not shown). A weighing machine may also be provided at this location so that an operator may cut off and weigh a suitable length of extruded sausages, the object being to provide a length of standard weight. e.g. one pound. After weighing, the lengths of sausage are placed on one of the subsidiary delivery conveyors 36, 37 and are passed through a channel through the housing 7 and up the main working table 1 and during this travel they are taken off by the operators who twist them into sausage shapes and hang them in strings on the carrier members, as is indicated in Figure 1. This twisting and hanging operation takes place in the left-hand end of the length of the working table 1 with reference to Figures 1 and 2. The conveyor then conveys the strung sausages into the cooling tunnel and, after cooling, the sausage strings come out at the further right-hand end and pass again in front of the operators at that end of the table who remove the cooled strings and form them into bunches. These bunches are then placed on the delivery conveyors 36, 37, as indicated on the right-hand end of Figures 1 and 2, where they are taken through a channel formed through the housing 8 to the table 44 where they may be wrapped or packaged in any desired manner. There are, therefore, two operations performed by the operators seated at the work table. A first preliminary twisting and hanging operation and then a removal and bunching operation, and the invention ensures that the operators do not have to leave their places to perform these duties. There is thus a considerable saving n space, time and handling in order to process the products finally. Tile division of the table 1 into two longitudinal parts is particularly useful where it is desired to segregate two varieties of produce. For example, in the processing of sausages, one portion of the table can be devoted to pork and the other to beef sausages. At the base of the cooling tunnel there is provided a drain 47 to collect moisture resulting from the cooling process and this fnoisture may be run off by means of a suitable pipe (not shown). Suitable inspection doors 48 may be provided in the walls of the tunnel and the walls are preferably suitably insulated to prevent loss of cooling effect. It will also be understood that the invention has been described specifically in connection with the processing of sausages purely by

way of example and that the apparatus according to the invention is capable of modification to suit individual needs. For example, the invention may be used in connection with drying tunnels, for instance, for use in drying paint-sprayed articles or, indeed, for many other purposes. It will thus be apparent that various modifications may be made to the specific details hereinbefore set forth without in any way departing from the scope of the invention. What I claim is : - 1. Continuous treatment apparatus comprising a processing chamber through which material for processing is passed by means of a conveyor, in which the processing chamber is integral with a work table which forms the top of the chamber, the conveyor having an upper run passing along and above the work table in front of an operator or operators whereby the material may be loaded on to and removed frown the conveyor by the operator or operators without moving from his or their working positions at the table, and the lower run of the conveyor passing through the said chamber.


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