4376 4380.output

* GB784783 (A)

Description: GB784783 (A) ? 1957-10-16

Improvements in or relating to processes for the production of seleniumrectifiers

Description of GB784783 (A)

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CH324326 (A) NL101501 (C) CH324873 (A) CH324326 (A) NL101501 (C) CH324873 (A) less Translate this text into Tooltip

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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.

PATENT SPECIFICATION Date of Application and filing Complete Specification: February 10, 1954. Application made in Germany on February 10, 1953 Complete Specification Published: October 16, 1957 7849783 No 3964/54. Index at acceptance:-Class 37, K( 1 Al:2). International Classification:-HO 11. COMPLETE SPECIFICATION Improvements in or relating to Processes for the Production of Selenium Rectifiers We, SIEMENS-SCHUCKERTWERKE AKTIENGESELLSCHAFT, a Germany Company, of 1 Berlin-Siemensstadt, Berlin and Erlangen, Germany, 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:1 o The invention relates to a process for the production of selenium rectifiers Processes for the production of such rectifiers are known in which an addition is made to the semi-conductor body (composed of selenium) for increasing the conductivity of the semiconductor body, and hence of the finished rectifier The addition for increasing the conductivity of the semi-conductor body consists of a halogen, or halogens, and will hereinafter be referred to as " the first addition " It is also known to make an addition for promoting the formation of the barrier layer In this Specification the barrier layer is to be understood as that which produces the blocking resistance in the rectifier Thus, an addition which promotes the formation of the barrier layer is an addition which increases the blocking resistance of the finished rectifier, the blocking resistance of the rectifier being the resistance offered to the current resulting from an inverse voltage applied to the rectifier Known additions for promoting the formation of the barrier layer are, for example, thallium, gallium, indium or sulphur The addition for promoting the formation of the barrier layer will hereinafter be referred to as the " second addition " In known processes for the production of selenium rectifiers, the second addition is applied with the counter electrode to the surface of the semi-conductor body, or is applied to the surface as a separate layer, the second addition then entering the semiconductor body by diffusion This has the drawback that it is difficult to regulate the lPrice 3 s 6 d l quantity and distribution of the diffused addition in the semi-conductor body. According to the present invention there is provided a process for the production of a selenium rectifier, wherein the semi 50 conductor body is built up of a plurality of individually successively applied selenium layers, each of which layers is provided with the first addition as herein defined, there being added to one layer in which the bar 55 rier layer is formed in the finished rectifier (or in the case wherein the semi-conductor body is to consist of more than two layers, also to the successive layers adjacent to said one layer, with the exception of one or more 60 of the last layers) such a quantity of the second addition as herein defined, that it brings about a reduction of the enhanced conductivity that would be produced by the presence of the first addition alone, and 65 there being added to the layer(s) not to be provided with such quantity of said second addition a further addition, different from said first addition, for increasing the conductivity of the layer(s) to which it is added, 70 the quantity of the second addition in said case being made progressively greater in the layers approaching the barrier layer, the relative quantities of said first, second and further additions being chosen in such a way 75 that the conductivity of the layers decreases as considered in a

direction toward the barrier layer. Since the semi-conductor body is built up of a plurality of individually successively 80 applied layers with the appropriate additions in individual layers, it is simple to effect the required distribution of the additions in the semi-conductor body and to have a precise regulation of the quantities thereof 85 As already stated, each of the layers contains the first addition, but it will of course be appreciated that different halogens or different mixtures thereof may be used in the various layers The layer in which the 90 784,783 barrier layer is formed in the finished rectifier and having the second addition which promotes the formation of the barrier layer, has this addition present in such quantity that, together with the first addition, it brings about a reduction of the enhanced conductivity that would be produced by the presence of the first addition alone in th 6 selenium The layer in the semi-conductor body which adjoins the layer in which the barrier layer is formed, contains the further addition for increasing, together with the first addition, if a suitable choice of quantities is made, the conductivity of the selenium comprising this layer The substance which constitutes the further addition may be such that it would in itself be suitable for use as a second addition to promote the formation of the barrier layer For example, it may be thallium When used as a further addition the quantity or concentration of such a substance must, however, be so chosen that it combines with the halogen addition to produce an increase in the conductance of those selenium layers in which the further addition is present If the same substance is employed both as the second addition in that layer in which the barrier layer is formed in the finished rectifier, and as the further addition in the remaining layers, the quantity of substance in the first-mentioned layer must be made substantially larger than in the other layers. The first addition and the second addition or the first addition and said further addition may, if desired, consist of an appropriate metal halogen compound. The semi-conductor body may, instead of comprising two layers, comprise a larger number of layers In this case, in the layers which are progressively more remote from the layer in which the barrier layer is formed, such quantities of additions are present as to ensure a progressive increase in the conductivity of such layers Thus, for example, the semi-conductor body may comprise three layers as follows, a first layer in which the barrier layer is formed containing the first addition together with such a quantity of the second addition as to produce a considerable reduction in the increase of conductivity that would be produced by the first addition acting alone in the selenium, a next succeeding layer containing a halogen addition and

the second addition in such a quantity that it reduces the conductivity that would be produced in this layer by the halogen addition acting alone but to a smaller extent than is the case in the first 6 () layer, and a third layer containing a halogen addition and the further addition such that the combined action of these two additions produces a greater conductivity in this layer than would be the case due to the halogen addition acting alone. For a better understanding of the invention and to show how the same may be carried into effect, reference will now be made to the accompanying drawing which shows a semi-conductor body of a rectifier 70 In the drawing 1 designates a carrier plate of a rectifier, 2 a a selenium layer with a halogen addition and an addition for increasing conductivity, for example tellurium, 2 b a layer of selenium with a halogen addi 75 tion and an addition promoting the formation of the barrier layer, for example thallium, and 3 the counter electrode which is applied by a suitable known method The counter electrode may advantageously be 80 free from media, such as thallium, which promote the formation of the barrier layer. In the layer 2 a a simultaneous addition of halogen and metal to the selenium may be made by employing a metallic halide 85 such as iron chloride.

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* GB784784 (A)

Description: GB784784 (A) ? 1957-10-16



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PATENT SPECIFICATION 784,784 Date of Application and filing Complete Specification: February 10, 1954. Application made in Germany oil February 10, 1953 Complete Specification Published: October 16, 1957 Index at acceptance:-Class 37, K(MA 1:2). International Classification:-HOI 1 I. COMPLETE SPECIFICATION Improvements in or relating to Processes for the Production of Selenium Rectifiers We, SIEMFNS-SCHUCKERTWERKE AKTIENGESELLSCHAFT, a German Company of I Berlin-Siemensstadt, Berlin and Erlangen, Germany, 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 a process for the production of selenium rectifiers Processes for the production of such rectifiers are known in which an addition is made to the semi-conductor body (composed of selenium) for increasing the conductivity of the semi-conductor, and hence of the finished rectifier The addition for increasing the conductivity of the semi-conductor consists of a halogen, or halogens, and will hereinafter be referred to as the "first addition " It is also known to make an addition for promoting the formation of the barrier layer In this Specification the "barrier layer" is to be understood as that which produces the blocking resistance in the rectifier Thus, an addition which promotes the formation of the barrier layer is an addition which increases the blocking resistance of the finished rectifier, the blocking resistance of the rectifier being the resistance offered to the current resulting from an inverse voltage applied to the rectifier Known additions for promoting the formation of the barrier layer are thallium, gallium, indium or

sulphur The addition for promoting the formation of the barrier layer will hereinafter be referred to as the "second addition " In known processes for the production of selenium rectifiers, the second addition in the form of thallium is applied with -40 the counter electrode to the surface of the semi-conductor, the thallium entering the semi-conductor by diffusion This has the drawback that it is difficult to regulate the quantity and distribution of the diffused ad-45 dition in the semi-conductor body. lPrice 3 s 6 d J According to the present invention there is provided a process for the production of a selenium rectifier, wherein the semi-conductor body is built up of a plurality of individually successively applied selenium 50 layers, there being added to one layer in which the barrier layer is formed in the finished rectifier a second addition as hereinbefore defined, and there being added to the layer(s) adjoining said one layer a first 55 addition as hereinbefore defined and a further addition, different from said first addition, for increasing the conductivity of said adjoining layer(s) said first addition not being added to said one layer 60 For a better understanding of the invention and to show how the same may be carried into effect reference will now be made to the accompanying drawing which shows diagrammatically a selenium rectifier 65 In the drawing, 1 designates a carrier plate, to which has been applied a layer 2 a of selenium with an addition of iron chlorides, (the iron constituting a further addition and the chlorine constituting the first addition) a 70 layer 2 b of selenium with an addition of thallium, and a counter electrode 3 Alternatively a small quantity of a halogen, for example chlorine, and a further addition consisting of a substance which when used 75 as a second addition would promote the formation of the barrier layer, for example thallium, may be added to the layer 2 a. The counter electrode is preferably free from media such as thallium which promote the 80 formation of the barrier layer. As already stated, thallium, for example, may be employed as the second addition for promoting the formation of a barrier layer. Substances suitable for use as a further ad 85 dition for increasing the conductance of a selenium layer containing the first addition are antimony, bismuth, tin, thallium, indium, gallium, cadmium, copper, lead or iron; or non-metals such as, for example, arsenic 90 No 3965/54 2 784,784 or sulphur; or alloys or combinations of these materials Since these substances are intended to increase the conductance of a halogen-containing layer, the allowable maximum concentration of such further additions is known to depend upon the existing halogen concentration If desired, the first and further additions may be used in the form of metal-halogen or metalloid compounds.

As is apparaent from the foregoing list of suitable substances, there may also be used for the further addition substances which are suitable per se for use as a second addition for promoting the formation of the barrier layer Therefore, the same substance may also be employed both for the secoid addition and for the further addition The difference in the action of the same type of substance in the layer in which the barrier layer is formed on the one hand and in the layers adjoining this layer on the other hand is due to the fact that on the one hand the additive, for example thallium as is known, - 25 always produced a reduction in conductance in the halogen free layer, whilst on the other hand if used in a sufficiently low concentration in the other adjoining halogencontaining layers, the additive produces in combination with the halogen an increase in the conductance of the layer concerned over and above the amount which would be produced in the layer by the halogen addition alone The use of the same substance as the second addition and as the further addition has the advantage that the migration of the second addition from the selenium layer in which the barrier layer is formed into the adjoining layers is reduced In this way the further addition also indirectly assists in promoting the formation of the barrier layer. By means of the invention, a rectifier is obtained which has a relatively low total resistance in the forward direction by reason of its layer structure Also the result is 45 obtained that should the further addition migrate into the layer in which the barrier layer is formed, any disadvantage effects resulting from this migration on the formation of the barrier layer will be reduced by the 50 action of the second addition.


* GB784785 (A)

Description: GB784785 (A) ? 1957-10-16







PATENT SPECIFICATION Date of Application and filing Complete Specification: February 10, 1954. 784,785 No 3966154Application made in Germany on February 10 1953 Complete Specification Published: October 16, 1957 Index at acceptance:-Class 37, K( 1 AL:2). International Classification:-H Oll. COMPLETE SPECIFICATION Improvements in or relating to Processes for the Production of Selenium Rectifiers We, SIEMENS-SCHUCKERTWERKE AKTIENGESELLSCHAFT, a Germanl Company, of 1 Berlin-Siemensstadt, Berlin and Erlangen, Germany, 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:The present invention relates to a process for the production of a selenium rectifier. Processes for the production of such selenium rectifiers are known in which an addition is made to the semi-conductor (composed of selenium) for increasing the conductivity of the semi-conductor and hence of the finished rectifier The addition for increasing the conductivity of the semiconductor consists of a halogen, or halogen or halogen compound(s) and will hereinafter be referred to as " the first addition " It is also known to make an addition for promoting the formation of the barrier layer.

In this Specification the "barrier layer" is to be understood as that which produces the blocking resistance in the rectifier Thus, an addition which promotes the formation of the barrier layer is an addition which increases the blocking resistance of the finished rectifier, the blocking resistance of the rectifier being the resistance offered to the current resulting from an inverse voltage applied to the rectifier Known additions for promoting the formation of the barrier layer are, for example, metals such as antimony, bismuth, tin, thallium, indium, gallium, cadmium, copper and lead, or non-metals such as arsenic, or sulphur or alloys or compounds of these substances The addition for promoting the barrier layer will hereinafter be referred to as "the second addition " In known processes for the production of selenium rectifiers, the second addition in the form of thallium is applied with the old el counter electrode to the surface of the semiconductor, thallium entering the semiconductor by diffusion This has the drawback that it is difficult to regulate the quantity distribution in the semi-conductor 50 According to the present invention there is provided a process for the production of a selenium rectifier, wherein the semiconductor body is built up of a plurality of individually successively applied selenium 55 layers, there being added to the selenium layer in which the barrier layer is formed in the finished rectifier only said second addition as herein defined, whilst there is added to the selenium layer most remote 60 from said barrier layer only said first addition as herein defined. Such a process for the production of a selenium rectifier may be further developed -by employing, in addition to layers which 65 contain only said second addition or said first addition, intermediate layers which contain both said first and second additions In this case, use is made of the fact that when selenium is present together with said first 70 addition, the conductivity of the selenium can be reduced by said second addition if the quantity of the latter exceeds a predetermined amount The composition of the layers introduced between that or those con 75 sisting of selenium and said second addition, on the one hand, and that or those consisting of selenium and said first addition on the other hand, must be chosen such that each intermediate layer, lying closer to the site 80 of the barrier layer and consisting of selenium with said first addition, is given such a quantity of said second addition that the conductivity of each layer lying closer to the site of the barrier layer is less than 85 that of a layer which lies further from the site of the barrier layer. For a better understanding of the invention and to show how the same may be carried into effect, reference will now be 90 ra b 784,785 made to the accompanying drawings in which:Figure 1 shows diagrammatically

a selenium rectifier, and, Figure 2 shows diagrammatically a second selenium rectifier. In Figure 1 of the drawings, 1 is the carrier electrode on which is provided a layer 2 a of selenium with a halogen addition, for example chlorine, a layer 2 b of selenium with an addition promoting the formation of the barrier layer, for example thallium, and the counter electrode 3. In Figure 2, 11 designates the carrier electrode on which is provided a layer 12 a of selenium with a relatively high halogen addition, a layer of selenium 12 b containing a smaller halogen addition than 12 a, a layer 12 c of selenium with a small addition of a material promoting the formation of the barrier layer, a layer 12 d of selenium with a larger addition for promoting the formation of the barrier layer than in 12 c, and the counter electrode 13 The counter electrode may advantageously be free from media such as thallium which promote the formation of the barrier layer.


* GB784786 (A)

Description: GB784786 (A) ? 1957-10-16

Dyestuffs and intermediates of the anthraquinone series



CH321525 (A) DE1053114 (B) US2807630 (A) CH321525 (A) DE1053114 (B) US2807630 (A) less Translate this text into Tooltip



PATENT SPECIFICATION Date of Application and filing Complete Specificatic No 19084/54. Application made in Switzerland on July I, 1953. Application made in Switzerland on June 14, 1954. Ha / Complete Specification Published: Oct 16, 1957. 784,786 in: June 29, 1954. Index at acceptance:-Class 2 ( 4), Q 1 A 4. International Classification:-C 09 b. COMPLETE SPECIFICATION Dyestuffs and Intermediates, of the Anthraquinone Series We, CIBA LIMITED, a body corporate organized according to the laws of Switzerland, of Basle, Switzerland, 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: According to this invention valuable new addition compounds are made by reacting a compound of the formula ( 1) Aq-S-Halogen or contain an ethylene group bound on at least one side to a further carbon atom, as for example in the case of cycloalkylenes, especially cyclohexenes, styrenes and allyl compounds. As examples of such compounds there may be mentioned cyclohexene, styrene, 2-methyl-1phenylethylene, 1-methyl-l-phenyl-ethylene, allylbromide, isobutylene and butadiene. The reaction is advantageously carried out in an organic solvent such, for example, as glacial acetic acid, chloroform or tetrachlorethane, at a raised temperature. There are obtained addition products of the constitution: ( 2) Aq-S-SCN in which Aq represents a vattable residue bound to the sulphur atom by an aryl-carbon atom, and the halogen atom is advantageously a chlorine or bromine atom, with an unsaturated organic compound The vattable residue Aq may be, for example, an anthraquinone residue which is bound to the sulphur atom in the 1 or 2-position If desired this residue may contain further substituents or it may be free from further substituents as in the case of the residue of the constitution o y ( 3) QY 0 do in which one Y represents a hydrogen atom and the other Y an -S-halogen group or -S-SCN group. The unsaturated compounds, with which the vattable starting material

defined above is additively combined, advantageously contain as the unsaturated group a >C=C< grouping Especially advantageous are unsaturated compounds which contain a grouping, that is to say, compounds which lPrice 3 F,4 AL 4 S 6 d ( 4) in which one Z represents a hydrogen atom and the other Z a group of the constitution: I I 1 / or X X xx t 1 -.s-cf-c-scv I d H H in which the two X's represent hydrogen 55 atoms or together with the -C-C group form an advantageously carbocyclic ring, or in which one X represents a hydrogen atom and the other X an alkyl or aryl residue, for example, an aromatic residue of the benzene 60 series. Thus, with the aid of the unsaturated compounds described above, there can be obtained, for example, addition products of the following constitutions: 65 (a) Compounds of the formula ( 4), in which one Z represents a residue of the constitution: D/4 g q Utr or (,i c Y/ H H 784,786 and especially a residue of the formula 0/% H, I a or t Hx, o -s/ \a/oen s (b) Compounds of the formula ( 4), in which one Z represents a residue of the constitution -S-RI in which R, represents an ethyl-benzene residue, of which one carbon atom of the ethyl group is bound to the sulphur atom and the other carbon atom to a halogen atom. (c) Compounds of the formula ( 4) in which one Z represents a residue of the constitution -S-R 2. in which R, represents a dihalogen-propyl residue. Depending on the nature of the unsaturated compound used, the reaction with the sulphenyl halide may in some cases be accompanied by the splitting off of hydrogen halide to form a vinyl sulphide of the formula ( 5) X X l I Aq-S-C = CH in which Aq and X have the meanings given above This is the case, for example, in the reaction of anthraquinone-l-sulphenyl bromide with 1-methyl-l-phenyl-ethylene Accordingly, there can also be obtained by the present process, for example, compounds of the formula ( 6) To in which one Z represents a hydrogen atom and the other Z a residue of the constitution -S-R. in which R, represents an ethylene-benzene residue bound by an ethylene carbon atom to the sulphur atom. With regard to the constitution of the compounds obtainable by the present process it can be assumed that preferential combination takes place between the sulphur atom of the vattable compound and the carbon atom of S the ethylene group which is richer in hydrogen, when the two carbon atoms of the ethylene group differ from one another in this respect. Further reactions can be carried out with 45 the compounds of the formula ( 4) Thus, for example, the halogen atom of a compound of the formula x I /?-$-C-O-Ha/oaen can be exchanged by a method known to be 50 suitable for a primary, secondary or tertiary amino group, an -0

O-acyl group, such as an -O 0-acetyl group, an alkoxy or hydroxyl group A hydroxyl group may also be formed by hydrolysis of an -0 O-acyl group All 55 these reactions can be carried out by methods in themselves known. The new compounds of the formula ( 4), and the compounds obtainable therefrom in the manner described in the preceding para 60 graph, are valuable intermediate products which are suitable, for example, for the manufacture of vat dyestuffs Furthermore they can be used directly as dyestuffs, for example, as pigments, and especially as dispersion dye 65 stuffs for dyeing or printing cellulose acetate artificial silk or polyamide fibres, or fibres of polyesters of aromatic dicarboxylic acids. The following Examples illustrate the invention, the parts and percentages being by 70 weight unless otherwise stated and the relationship of parts by weight to parts by volume being the same as that of the kilogram to the litre: EXAMPLE 1 75 parts of anthraquinone 1 sulphenyl bromide (obtainable as described by Fries. Berichte, Vol 45, page 2967 l 1912 l), 12 parts of cyclohexene and 250 parts of glacial acetic acid are boiled together under reflux for 10 80 minutes Upon cooling the hot filtered solution handsome small yellow needles crystallise out The latter are filtered off with suction, washed with alcohol and petroleum ether, and dried in vacuo at 60 C In this manner about 85 8.5 parts of 1-( 21-bromo-cyclohexyl-mercapto)anthraquinone of the formula are obtained The latter product melts at 174-175 C Analysis of a product so ob 90 tained, after recrystallisation from glacial acetic acid, gave the following results: 784,786 C,0 H,70,S Br Calculated: C= 59 85, H= 4 27, S= 7 99 Br= 19 91 % ( 401,3) Found: C= 59 99, H= 4 44, S= 7 88 Br= 20 20 % EXAMPLE 2. 1 part of 1-( 21-bromo-cyclohexylmercapto)anthraquinone is dissolved in 30 parts by volume of hot glacial acetic acid, the whole is mixed with 1 part of silver acetate and boiled for a few minutes After cooling it the mix/ ture is allowed to stand for 3 hours, filtered, the filtrate is mixed with water, the resulting 10 precipitate is filtered off with suction, and washed with water The resulting 1-( 21-acetoxy-cyclohexylmercapto) anthraquinone of the formula crystallises from ethanol in the form of small yellow needles which melt at 168 C A product prepared in this manner and further C,2 H 2,004 S Calculated: C= 69 45 ( 380 4) Found: C = 69 61 EXAMPLE 3. 2 parts of 1-( 2 '-bromo-cyclohexyl)-mercaptoanthraquinone are suspended in 100 parts of absolute methanol, and mixed with a methylate solution prepared from 0 2 part of sodium and 20 parts of absolute methanol.

After boiling the mixture for 2 hours under reflux, it is filtered and the filtrate is mixed with a large quantity of water The yellow powder which precipitates is filtered off with suction, washed with water and dried By recrystallisation froan ethanol there is obtained 1 ( 21-methoxy-yclohexyl)-mercapto-anthraquinone of the formula C,,H 2,O 0,S Calculated: C= 71 56 Found: C = 71 41 EXAMPLE 4. 3.5 parts of 1 ( 2 ' acetoxy cyclohexyl)mercapto-anthraquinone are dissolved hot in 400 parts of ethanol After adding a solution of 3 5 parts of potassium hydroxide, 35 parts of water and 315 parts of ethanol, the whole is boiled for 2 hours under reflux After cooling the mixture, a large quantity of water is added, the whole is filtered with suction, and the filter residue is washed with water and dried The resulting 1-( 2 '-oxycyclohexyl)mercapto-anthraquinone of the formula /M a purified by additional recrystallisation from ethanol, melted at 169-170 C and gave the 20 following analysis: 5, H= 5 30, S= 8 43 % 1, H = 5 33, S = 8 11 %. in the form of small yellow-orange crystals, which melt at 138-139 C A product obtained in this manner had the following analysis: 6, H= 5 72, S= 9 10 % H= 5 42, S= 9 36 %. is an orange powder, which can be recrystallised from alcohol. Ex AMPLE 5. parts of anthraquinone 2 sulphenyl chloride are boiled under reflux for 15 minutes with 10 parts of glacial acetic acid and 6 parts of cyclohexene Upon cooling the mixture, the addition product crystallises out in the form of yellow crystals The latter are filtered off with suction, washed with alcohol, and recrystallised, for example, from glacial acetic acid, in the form of coalesced lemon yellowr needles melting at 131-132 C. S (Calculated)= 8 98 %, S (Found)= 9 14 %. EXAMPLE 6. 3.19 parts of anthraquinone-l-sulphenyl bromide are boiled under reflux for 15 minutes with 75 parts of glacial acetic acid and 3 2 parts of freshly distilled styrene After cooling the mixture, a small amount of precipitated dianthraquinonyl-1: P-disulphide is filtered off, and the solution is allowed to crystallise after being concentrated to half its volume. The yellow crystals so obtained can be recrystallised from benzene The addition product melts at 142 C. Bromine (calculated)= 18 9 %, Bromine (found) = 18 93 %. It crystallises from glacial acetic acid or alcohol in the form of yellow crystals which melt at 60 154 C Analysis: C Calculated 77 50 Found 77 53 H S 4.52 9 00 % 4.55 9 11 %. EXAMPLE 7. parts of anthraquinone 2 sulphenyl chloride are boiled under reflux

for 1 hours with 30 parts of chloroform and 4 parts of freshly distilled styrene After allowing the mixture to stand for a long time in a mixture of ice and water, the precipitated crystals are filtered off with suction and recrystallised from benzene The pure substance melts at 159 C. Sulphur (calculated) = 8 46 %, Sulphur (found) = 8 29 % EXAMPLE 8. 2 97 parts of anthraquinone-1-sulphenyl thiocyanate are boiled under reflux for one hour with 50 parts of glacial acetic acid and one part of cyclohexene After cooling the mixture, it is filtered to remove a small amount of precipitated dianthraquinonyl-1: 1-disulphide, and the filtrate is evaporated in vacuo until crystallisation sets in The yellow addition product is dissolved and reprecipitated several times from benzene or a mixture of benzene and petroleumn ether. N (calculated)= 3 69 %/, N (found)= 3 85 % Anthraquinone-l-sulphenyl thiocyanate may be prepared, for example, as follows: 3.19 parts of anthraquinone-1-sulphenyl bromide are stirred for 24 hours at room temperature with 1 part of dried and finely pulverised potassium thiocyanate in 50 parts of dry chlorobenzene The suspension is filtered with suction and the filter residue is thoroughly washed with alcohol and water By recrystallisation from ethyl acetate the sulphenyl thiocyanate is obtained in the form of small pale yellow needles, which melt at 208 C. Analysis: s Calculated 21 58 Found 21 46 IN 4.72 % 4.81 %. EXAMPLE 9. 16 parts of anthraquinone-1-sulphenylbromide and 9 parts of 1-methyl-1-phenylethylene are boiled in 40 parts of glacial acetic acid until hydrogen bromide is no longer formed Upon cooling the hot filtered solution, a 1 (phenyl vinyl mercapto)-anthraquinone crystallises out in golden yellow crystals The reaction product has the probable formula EXAMPLE 10. 16 parts of anthraquinone-l-sulphenyl bromide and 12 parts of freshly distilled allyl bromide are boiled for one hour in 40 parts of glacial acetic acid Upon cooling the hot filtered solution the addition product crystallises out in yellow crystals By crystallisation from alcohol there is obtained a crystalline yellow powder, which melts at 138 C The reaction product so obtained having the probable formula o l gave the following analysis: C Calculated 46 39 Found 46 36 H 2.75 % 2.84 %. EXAMPLE 11. 0.5 part of the 1-( 21-bromo-cyclohexylmercapto)-anthraquinone obtained as described in Example 1 is dissolved at O C in 10 parts of sulphuric acid of 90 per cent strength, the solution is poured on to ice and water and then filtered The filter cake is ground in a roller

mill with 1 part of dried sulphite cellulose waste liquor The resulting suspension is added to a dyebath, which contains 3000 parts of water and 9 parts of soap, and 100 parts of well wetted cellulose acetate artificial silk are entered into the dyebath at 40 C, the temperature is raised to 80 C and dyeing is carried on for one hour at 80-85 C Cellulose acetate artificial silk is dyed yellow. Instead of cellulose acetate artificial silk, nylon may also be dyed in the manner described above The products of the other examples can also be used in the above manner for dyeing cellulose acetate artificial silk or nylon.


* GB784787 (A)

Description: GB784787 (A) ? 1957-10-16

Improvements in direct current supply systems for use in arc welding


We, LINCOLN ELECTRIC COMPANY LIMITED, a British Company, of Broadwater Road, Welwyn Garden City, Hertfordshire, 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:- The invention relates to direct current supply systems for use in arc welding A difficulty with such systems as norma Ry constructed is that the normal source of current supply is incapable of maintaining a satisfactory voltage under conditions, substantially equivalent to a short-circuit, which arise at the instant of striking the arc or when, during welding, a globule of metal bridges the arc It is an object of

the present invention to provide means by which the output from the normal supply source may be temporarily augmented or boosted when the voltage falls below a predetermined value. According to the invention a direct current supply system for use in arc welding comprises a main source of direct current with connections to be made to the work and a welding electrode or to two electrodes and, in a circuit parallel with the main current source, an auxiliary current source having a voltage less than the voltage in the welding circuit during normal welding and a rectifier which is arranged to prevent back flow in the parallel circuit when the welding voltage is greater than that of the auxiliary source but to permit flow from the auxiliary source to augment the supply from the main source if the welding current voltage (e g during striking of the arc) falls below the voltage of the auxiliary source. lPrice 3 s 6 d l The auxiliary source may provide alternating current which is converted to direct current by the rectifier or it may itself be a source of direct current and be in series with the rectifier. The rectifier is preferably of the selenium type. The invention is particularly suited for use in manual arc welding employing covered electrodes. In the accompanying diagram Figure 1 shows one circuit arrangement which may be used in carrying out the invention As shown in the diagram there is a main D C. generator 10, driven for example by an electric motor or an internal combustion engine or other prime mover and arranged to supply direct current to a welding arc indicated at 11 In parallel with the generator 10 there is an auxiliary D C. generator 12, driven in any suitable manner (e.g by the same means as the generator 10), in series with a selenium rectifier 14. The accompanying diagram, Figure 2, shows another circuit arrangement in which both the main and auxiliary sources are derived from an alternating current supply. The main source comprises a transformer 20, a choke 21 and a selenium rectifier 22. The auxiliary source com Drises a transformer 24 and a -selenium rectifier 25. It is an advantage of the invention that there may be used for the auxiliary source supply means capable of producing a heavy current for only a short period of time. The main source may have an open circuit voltage of 70-80 volts, and under normal welding conditions, a voltage of about 25-50 volts, and the auxiliary source a voltage of about 15-20 volts. In Specification No 718,871 there is 784,787 PATENT SPECIFICATION

Inventor:-WILLIAM PATRICK HAMILTON HATTY. Date of filing Complete Specification: Sept 27, 1955. Application Date: July 22, 1954 No 2146615. Complete Specification Published: Oct 16, 1957. Index at Acceptance:-Class 38 ( 4), A( 1 DS: 2 84). International Classification:-HO 2 i. COMPLETE SPECIFICKAION. Improvements in Direct Current Supply Systems for Use in Arc Welding. ( 8 ( 784,787 claimed an arc welding apparatus, comprising terminals for supplying current for welding: a transformer having a primary winding and a secondary winding: and main rectifier means connected between said secondary and said terminals, said secondary having a number of turns such that it is adapted to supply a voltage equal to the normal welding voltage of said terminals: characterised in that said transformer has another secondary which is connected to said terminals through auxiliary rectifier means, the number of turns of said other secondary being such that it is adapted to deliver at said terminals an auxiliary or "arc drive" voltage which is substantially smaller than said normal welding voltage. We make no claim herein to arc welding apparatus embodying a transformer with a primary winding and two secondary windings arranged as claimed in Specification No 718,871.


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