Upload
j1075017
View
107
Download
0
Embed Size (px)
Citation preview
* GB785048 (A)
Description: GB785048 (A) ? 1957-10-23
Improvements in and relating to ambulances
Description of GB785048 (A)
COMPLETE SPECIFICATION.
Improvements in and relating to Ambulances.
We, TAGGART & WILSON LIMITED, a
British Company, and JOHN WILSON, a
British Subject, both of "Knowetop", Motherwell, Lanarkshire,
Scotland, 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 has reference to ambulances of the kind provided with
individual seats for the patients and has for its object to provide
improvements whereby the seating accommodation can be utilised for
lying or stretcher cases.
According to the present invention in an ambulance provided with
individual seats having back rests the back rests are provided with
side limbs mounted to swivel about a transverse member of the seat
frame, said limbs having downward extensions engaging sockets by which
the back rests may be maintained in more or less upright position,
upward movement of the back rests permitting the limbs to clear the
sockets whereon the back rests can be turned to a horizontal position
to close the gaps between adjacent seats, the seats and their back
rests then lying in the same plane in horizontal alignment.
A further feature of the invention consists in providing the seats
with vertically adjustable side guard rails or side arms to prevent
the patients, either sitting or lying, from being dislodged and which
can be lowered to allow sitting patients to take their seats and also
for the purpose of permitting a lying case or a pole and stretcher
case to be placed on the bed formed by the combined seats and back
supports.
A still further feature of the invention consists in providing the end
of the series of seats with a pivotally mounted seat extension which
can be erected to form a continuation of the seat. To hold it in its
extended position the extension may be provided with a hinged
supporting leg incorporating a stiff helical spring which holds the
leg in its supporting position but permits it to bold so that it will
extend along the floor below the seat, the extension then assuming a
vertical position.
An embodiment of the invention will now be described with reference to
the annexed drawings wherein:
Figure 1 is an elevation of three individual seats for ambulances, the
seats being constructed in accordance with the invention;
Figure 2 is an end elevation thereof;
Figure 3 is a plan view thereof;
Figure 4 shows to a larger scale the means by which the back rests are
mounted to swivel; and
Figure 5 is a detail showing means whereby the guard rails can be
maintained in the raised position.
An ambulance according to the embodiment shown in the drawings is
provided on one or both sides thereof with a series of three aligned
seats, 10, 11 and 12, the first and second seat of the series having a
back rest 13 while a fixed upright rear support not shown, constitutes
the back rest for the third seat. Should space permit the latter,
however, may have a back rest.
The first and third seats each have tubular supporting side frames 14
and 15 interconnected by cross members 16. The intermediate seat has
an inner tubular side frame 17 connected by cross members 18 to a side
rail 18a which is welded to a longitudinally extending rod 19
interconnecting the outer side frame 15 of the first and third seats.
The omission of the outer side frame of the intermediate seat is
necessitated by reason of the rear wheel arch of the vehicle.
The frame of each back rest has welded to the sides thereof two side
limbs 20 which make a sliding fit in cylindrical guides 21 integral
with horizontal sleeves 22 mounted to swivel on a cross member 16 or
18 of the seat frame.
At its lower ends each of said limbs, when the back rest is in an
upright position, fits into a supporting socket 23 carried by the seat
frame, an elastic strap 24 connecting the back rest to a cross member
of the seat and holding the lower ends of the limbs 20 therein. The
seat frames to the rear or the seats provided with back rests are
provided with cradles or other stops 25 to receive and support the
back rests when the latter are in the horizontal position as indicated
in chain dotted lines Figures 1 and 3.
The inner side frames of the seats are provided with vertical tubular
supports 26 which receive the limbs of frames 27 of U-formation. Said
frames, when in their raised positions, shown in chain dotted lines
Figures 1 and 2, constitute guard rails. To retain the vertical limbs
in their raised position cross pins 28 engage with aligned transverse
slots 29 and 30 in the limbs and supports, the pins being resiliently
held therein by tension springs 31 encircling the support and anchored
to the two ends of the pin. By pressing the side arms or rails
downwards the pins will be forced out of engagement with the vertical
limbs and when raised they will snap back into position.
The seat 10 is provided with a pivotally mounted seat extension 32
having a collapsible leg 33 incorporating a stiff helical spring 34
the upper end of which is anchored in a socket 35 below the seat. When
the extension is in its lowered position the leg extends above the
floor and when raised as shown in dotted line in Figure 1 the spring
serves to retain the leg in its supporting position.
The series of three seats may be formed as a unit.
The back rests, seats and seat extension have the usual supporting
webbing as indicated by the chain dotted lines 36 in
Figures 2 and 3 and may be upholstered or provided with cushions.
Normally the back rests 13 will be in their upright position for
sitting or reclining patients. The guard rails 27 may be lowered to
permit the patients to take their seats and thereafter raised.
Should, however, a patient require to be kept in a lying position the
two back rests are raised so that the foot of the limbs 20 clear the
sockets 23 and are then tilted so Lhat they will be supported by the
cradles or stors 25 of the seat to the rear, as shown in dotted lines
in Figures 1 and 3, the seats and their back rests then lying in the
same wlane in horizontal alignment.
The front seat extension 32 is raised and supported in its raised
position by the leg 33 so that it, together with the seats and the
folded down back rests, lie in horizontal alignment to form a bed or a
support for a pole and canvas stretcher. The side guard rails 27 may
be lowered to permit of this and subsequently raised.
It will be understood that there may be more than three seats in each
series. Further in an emergency the back rests may be lowered to
constitute additional seats for sitting patients. In such case the
patients sit with their backs to the side wall of the vehicle.
If desired, the back of the front seat 10 may be folded down so that a
patient may be seated on the centre seat with his back supported by
the back thereof and his legs rested on the seat 10 and its folded
down back.
The frames 27 at the rear of the ambulance may constitute grab handles
to assist patients and the attendants entering and leaving the
ambulance.
The usual ambulance equipment, i.e. first aid outfit, cuspidor, and
such like, may be accommodated below the seats.
What we claim is:
1. In an ambulance, the provision of individual seats provided with
back rests characterised in that the back rests are provided with side
limbs mounted to swivel about a transverse member of the seat frame,
said limbs having downward extensions engaging sockets by which the
back rests may be maintained in a more or less upright position,
upward movement of the back rests permitting the limbs to clear the
sockets whereon the back rests can be turned to a horizontal position
to close the gaps between adjacent seats, the seats and their back
rests then lying in the same plane in horizontal alignment.
2. In an ambulance, the provision of seats and back rests as claimed
in the preceding claim wherein the seats are provided with vertically
adjustable side guard rails or side arms to prevent the patients,
either sitting or lying, from being dislodged and which can be lowered
to allow sitting patients to take their seats and also for the purpose
of permitting a lying case or a pole and stretcher case to be placed
on the bed formed by the combined seats and back supports.
3. In an ambulance, the provision of seats and back rests as claimed
in either of the preceding claims wherein the end of the series of
seats is provided with a pivotally mounted seat extension which can be
erected to form a continuation of the seat.
4. In an ambulance. the provision of seats and back rests as claimed
in Claim wherein the pivotally mounted seat exter- sion is provided
with a hinged supporting leg incorporating a stiff helical spring
which
* GB785049 (A)
Description: GB785049 (A) ? 1957-10-23
Improvements in or relating to aryloxyaliphatic compounds
Description of GB785049 (A)
A high quality text as facsimile in your desired language may be available
amongst the following family members:
DE1003498 (B) FR1146648 (A) NL90237 (C) US2818425 (A)
DE1003498 (B) FR1146648 (A) NL90237 (C) US2818425 (A) less
Translate this text into Tooltip
[84][(1)__Select language]
Translate this text into
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
Inventor: BASIL JASON HEYWOOD 7859049 Date of filing Complete
Specification: Jan 3, 1956.
Application Date: Jan 10, 1955.
No 751/55.
I/: Complete Specification Published: Oct 23, 1957.
Index at acceptance:-Classes 2 ( 3), C 1 E 7 K( 3: 8), C 1 Fl(A 3: C
4: D 2); 81 ( 1), E 1 C 4 A( 2: 3:4), E 1 C( 11: 12: 13); and 111, B 3
F( 1: 2).
International Classification:-A 611 C 05 f C 07 c.
COMPLETE SPECIFICATION
Improvements in or relating to Aryloxyaliphatic Compounds We, MAY &
BAKER LIMITED, a British Company, of Dagenlham, Essex, do hereby
declare the invention, for which we pray that a patent may be granted
to us, and the method by which it is tof be performed, to be
particularly described in and by the following statement:-
This invention is for improvements in or relating to aryloxy-aliphatic
compounds and to compositions containing one or more of such compounds
and useful for the modification of plant growth.
The use in agriculture and horticulture of various types of chemicals
for the purpose of modifying plant growth is now a customary practice,
and a considerable number of such substances are employed on a very
large scale for producing various different effects upon plant growth
These effects include modification of growth for the purpose of
enhancing the useful yield of crops later to be gathered from the
plants so modified, and the destruction of unwanted plants, i e, weeds
in areas containing useful crops.
Of recent years, the so-called " auxins" have become particularly
important as selective herbicides, their lethal effect being a
physiological and systemic one rather than that of a plant poison
which simply alters and destroys.
The advent of such highly successful auxins as 2:
4-dichlorophenoxyacetic and 4-chloro-2methylphenoxyacetic acid
derivatives has greatly stimulated research and development throughout
the world but there is still much that is not known concerning the
precise relationship between chemical structure of the auxin and
effect upon plant growth as to variation of effect according to
concentration and structure of the chemical employed (in some cases
the chemical acts at low concentration to modify plant growth in a
useful way and at a higher concentration to kill the plant) such that
prediction as to effect on plant growth of change in chemical
structure of the auxin cannot yet be made with anything like
reasonable certainty This is particularly so in the field of the
aryloxyaliphatic compounds.
l 1 Thus, Synerholm and Zinmmerman (Contributions of the Boyce
Thompson Institute 14, ( 7): 369-382, 1947) who have carried out a
considerable amount of research in the field 50 concluded in the case
of the w-( 2:4-dichlorophenoxy)aliphatic acid series that they are
physiologically active or inactive depending upon whether they contain
respectively an even or odd number of carbon atoms in the 55 aliphatic
acid portion of the molecule They further pointed out that it is
impossible to extend the generalisation to include all growth
regulators of the aryloxyaliphatic acid type, observing inactivity in,
e g, the chloro 60 phenoxybutyric acid series Until recently, it
appears to have been generally accepted that this activity of the
higher members of the series containing an even number of aliphatic
carbon atoms arises through degradation 65 thereof in the plant to the
corresponding member of the active acetic acid series In any event,
the few aryloxyaliphatic compounds that have been used on any
substantial scale as selective herbicides, all belong to the acetic 70
acid series And while those compounds of the acetic acid series are of
considerable value, their range of application and general utility are
limited by reason inter alia of the fact that they have a detrimental
effect upon important 75 useful crops.
Recently, however, Wain R L and Wightman F (( 1954) Proc Roy Soc (B)
142, 525) has shown that specific /-oxidase enzyme systems may be
present in the tissues of 80 different plant species and that there
may be a definite relationship between the enzyme make-up of a
particular plant tissue and the chemical character of, including more
particularly the nature and position of nuclear sub 85 stituents in,
an to-aryloxyalkanecarboxylic acid type hormone herbicide derived from
straight chain aliphatic acids higher in the series than acetic acid
such that, due to the enzyme system specific to the plant species in
question, a 90 specific type of such herbicides is not degraded in
that plant to the active acetic derivative, but is nevertheless so
degraded within the tissues of many common weeds of the type normally
to be found in association with the plant species in question More
specifically, Wain has shown that certain compounds of the butyric and
higher homologues series are effective selectively to eradicate weeds
in useful crops (for example, clover) for which the hitherto-used
aryloxyacetic compounds could not be employed successfully because of
their destructive effect not only upon the weeds but also the useful
crops themselves.
It is the object of this invention to provide new aryloxyaliphatic
compounds and compositions containing them which possess useful plant
growth regulating properties which could not have been predicted from
knowledge of their chemical structure, and which offer substantial
advantage over chemically related compounds previously known or
proposed as plant growth regulants.
The compounds of the present invention are the
y-phenoxy-y-alkylbutyric acids of the formula:
ce -C c H 2-c H 2-Ccom wherein R represents a hydrogen atom and R,
represents a hydrogen or chlorine atom or a methyl group or R and R,
both represent chlorine atoms, and R 2 represents an alkyl group
containing not more than 4 carbon atoms, preferably a methyl group,
together with the salts, esters and amides of these acids.
Individual acids of the present invention are: / ( 4 chlorophenoxy) y
methylbutyric acid, /-( 4-chloro-2-methylphenoxy)-y-methylbutyric
acid, y ( 2: 4 dichlorophenoxy) methylbutyric acid and 7-( 2: 4:
5-trichlorophenoxy)-y-methylbutyric acid Their plant growth regulating
effect varies according to the substituents contained in the benzene
ring.
Thus, the 4-chloro-2-methyl compounds are selective herbicides, while
the 4-chloro, 2: 4dichloro and 2:4: 5-trichloro compounds (especially
the dichloro compounds) are surprisingly effective in the prevention
of fruit drop.
By way of illustration of the advantages of the products of the
invention, the results of some of the comparative tests carried out by
the present applicants are now given.
For brevity, the compounds 2-methyl-4chlorophenoxyacetic acid, 2:4:
5-trichlorophenoxypropionic acid, /̂-(
2-methyl-4-chlorophenoxy)butyric acid, y-(
2-methyl-4-chlorophenoxy)-1-methylbutyric acid, 'f-( 2:
4-dichlorophenoxy)-y-methylbutyric acid, and '( 2: 4:
5-trichlorophenoxy) methylbutyric acid are designated "MCPA," " 2: 4:
5-TP," "MCPB," "MCPMB, " " 2: 4-DMB" and " 2: 4: 5-TMB" respectively.
(a) Pot Experiments showing efficiency of MCPMB as Herbicide.
Seedlings of the following crops and weeds were sprayed to run off
with aqueous solutions containing 0 4 % respectively of the sodium
salts of MCPA, MCPB and MCPMB at a rate of 50 English gallons per acre
After four weeks, observations were recorded as follows:
TABLE I
Species MCPMB MCPB MCPA Weeds Chickweed Severe damage Slight damage
Slight damage Poppy Dead Dead Dead Fat hen Dead Dead Dead Charlock
Dead Dead Dead Crops White clover Slight damage Unaffected Severe
damage Dwarf french bean Unaffected Moderate damage Dead Broad bean
Unaffected Severe damage Dead 785,049 chosen as reference compound
because of its known utility, as compared to compounds of related
chemical structure, in the prevention of fruit drop).
Apple trees of the Variety Cox's Orange Pippin (dwarf) were sprayed
while in the fruitlet stage with aqueous solutions containing 10 and
20 p p m, calculated as the acid, of 2: 4-DMB and 2:4: 5-TMB and
compared with the same concentrations of 2:4:5-TP.
The crop was picked 14 weeks later and graded according to the size of
the fruit (size I, diameter greater than 23 ", size II, 1 ' to 2-1,
size III, less than 1-") The results were as follows:
The foregoing results show that as compared to MCPA the compound of
the invention, viz, MCPMB, has the important advantage of destroying
typical weeds without, however, affecting any of the named useful
crops As compared to MCPB, the compound of the invention presents the
advantage of a far greater effect upon chickweed.
(b) Field Experiments showing the advantages of 2: 4-DMB and 2: 4:
5-TMB as compared to 2:4:5-TP.
(In this experiment the selected acids were employed as their
triethanolamine salts It should here be explained that 2: 4: 5-TP was
TABLE II
Mean Number Apples per Tree at Harvest Compound Total Size I Size II
Size III 2:4:5-TP p p m 171 16 52 103 p p m 116 0 8 108 2:4-DMB p p m
58 38 17 3 p p m 74 51 12 11 2:4:5-TMB p p m 56 32 24 0 p p m 39 8 20
11 Untreated 29 19 10 0 It will be observed that, although the highest
total yield was achieved with 2: 4: 5TP, the preponderating percentage
of yield in that case was of Size III apples, the economic value of
which is normally regarded as insignificant compared to apples of
larger average diameter.
In addition, at 20 p p m 2: 4: 5-TP caused severe leaf damage,
principally in the form of severe distortion, whereas neither of the
other two compounds caused any damage whatever, even at 40 p p m.
The alkali metal salts of the compounds of the present invention may
be prepared from the -y-lactones of the formula R 2 CH CH 2 CH 2 GO
I-O _ (where R is as hereinbefore defined), for example, readily
available y-valerolactone, by heating the lactone corresponding to the
yalkylbutyric acid desired under substantially anhydrous conditions
with an alkali metal salt, for example, the sodium salt, of the phenol
corresponding to the compound desired The free acids or derivatives
other than alkali metal salts may be readily obtained by treating the
alkali metal salt thus formed, or the crude reaction product
containing it, by known methods (by "known methods" is meant methods
heretofore used or described in the chemical literature) for the
isolation of a carboxylic acid or derivative in question from a
corresponding alkali metal salt or medium containing such salt Such
processes are illustrated by the Examples which follow As the 785,049
4 785 049 compounds of the present invention can exis as optical
isomers, which isomers, as well as mixtures thereof, and the
corresponding racemates are included within the scope of the present
invention, the process may, if desired include the step of resolution.
For industrial use the compounds of thi, invention may be employed in
any of the physical forms in which plant-growth regulant.
or herbicides of the 2: 4-D type are customarily used; in all cases in
association with an inert diluent In the case of wvatersoluble
compounds, e g, the alkali metal salts, it is convenient to employ an
aqueous solution where application in liquid form is desired
Alternatively, they may be used as solid compositions in conjunction,
thereforewith solid diluents such as talc, clay or other such inert
material In the case of compounds insoluble or but sparingly soluble
in water, it is convenient to employ them in the form of an aqueous
emulsion incorporating a wetting, dispersing or emulsifying agent of
the ionic or non-ionic type, the latter being preferred since they are
not affected by electrolytes The latter type of formulation is
preferably made up as a self-emulsifying concentrate containing the
active substance dissolved in the dispersing agent or in a solvent
compatible with that dispersing agent, the composition being made
ready for use by the simple addition of water.
Specific compositions include aqueous solutions of water-soluble salts
which may contain a wetting agent, wettable powders containing either
acid or amide in association with diluent powder and wetting agent,
oil emulsions containing one or more of the esters and micronised oil
suspensions of either acid.
The present invention is illustrated by the following Examples:
EXAMPLE I.
4-Chloro-2-methylphenol ( 71 25 g) is converted to its dry sodium salt
by azeotropic distillation with chlorobenzene in the presence of
caustic soda ( 5 % excess) y-Valerolactone ( 62 5 g) is added and
chlorobenzene is distilled off until the liquid reaches a temperature
of 180 C, which is then maintained for 2 j hours under reflux Water is
then added and the solution is steam-distilled to remove unchanged
4-chloro-2-methylphenol After cooling, the product is precipitated by
the addition of sulphuric acid and dried at 35 C.
Recrystallisation from petroleum ether gives y ( 4 chloro 2
methylphenoxy) 7methylbutyric acid, m p 75-76 C This acid is resolved
by conversion to a salt with either D or L 2-phenylisopropylamine The
dried salt is repeatedly crystallised from petroleum ether On
conversion back to the free acid, oils are obtained which have the
rotation of li.l 18 of + 39 0 and -39 3 (both in ethyl alcohol),
respectively.
EXAMPLE II.
2:4-Dichlorophenol ( 81 5 g) is converted to its dry sodium salt by
azeotropic distillation with chlorobenzene in the presence of caustic
soda ( 42 c c: 50 ,'),-Valerolactone ( 62 5 g) is added and the
temperature of the melt maintained at 1800 C for 2 hours Working up as
in Example I yielded -,-( 2:4-dichlorophenoxy)-y-methylbutyric acid, m
p 66670 C.
EXAMPLE III.
4-Chloro-2-methylphenol ( 14 25 g) is converted to its dry sodium salt
by azeotropic distillation with n-butanol in the presence of caustic
soda ( 5 %o excess) y-Valerolactone ( 12 5 g) is added and the
temperature of the reaction mixture allowed to rise to 155 C.
while some of the excess n-butanol is allowed to distil out The melt
is held at 1550 + 5 C.
for four hours and then the reaction product is isolated in the same
way as that given in Example I.
EXAMPLE IV.
In place of the 4-chloro-2-methylphenol used in Example III, 2:4:
5-trichlorophenol is employed Using exactly the same reaction
conditions, y ( 2: 4: 5 trichlorophenoxy) 7methylbutyric acid, m p
64-65 C, is obtained.
EXAMPLE V.
In place of the 4-chloro-2-methylphenol used in Example III,
4-chlorophenol is 95 employed Using exactly the same reaction
conditions, 7 ( 4 chlorophenoxy) y methylbutyric acid, m p 62-64 C is
obtained.
EXAMPLE VI.
o-Cresol is reacted with y-valerolactone in 100 a similar way to that
described in Example III to give methyl-y-( 2-methylphenoxy)butyric
acid, m p 78-79 C 194 g of this compound is heated to 1000 C when
sulphuryl chloride ( 10 % molar excess) was run in 105 gradually to
the stirred molten compound.
Hydrogen chloride and sulphur dioxide were evolved vigorously The
reaction was maintained at 100 G C for two to three hours and then
poured into water Sodium bicarbonate 110 was added, the solution
treated with carbon, and, after filtering, the y-(
4-chloro-2-methylphenoxy)-7-methylbutyric acid thrown out by the
addition of acid Isomer-free product could be obtained by
crystallisation of this crude 115 reaction product from aqueous
methanol.
In place of the sulphuryl chloride, chlorine and a catalyst, for
example, iodine, ferric chloride, could be employed.
EXAMPLE VII 120 7 ( 4 chloro 2 methylphenoxy) methylbutyric acid ( 121
25 g), n-butanol ( 100 c c) and concentrated sulphuric acid ( 2 c.c)
were stirred and heated in such a way that the butanol distilling
removed the water 125 from an azeotropic separator After six hours,
when no more water was separating, the reaction product was cooled,
diluted with water and acidic materials removed by an alkali wash
Distillation in vacuum gave pure n-butyl 130 785,049 excess thionyl
chloride was removed first at ordinary pressure and then in vacuum to
give a residue of the corresponding acid chloride.
The acid chloride was run into an excess of an amine, for example
ammonia, and the amide formed was isolated When ammonia was used the
product was filtered off and crystallised from benzene-petroleum ether
to give y-( 2:4dichlorophenoxy) y methylbutyramide, m p.
82-83 C.
For the purpose of the invention the aforesaid new compounds will be
used in a concentration of at least 0 0002 % by weight, the balance
consisting of a vehicle, fillers, etc The optimum concentration will
naturally vary according to the intended purpose but, in general, in
the case of herbicidal compositions concentrations of at least one lb
per acre, and in the case of fruit drop formulations, concentrations
of 20-40 parts per million by weight for normal high volume spraying,
rising to 400 to 800 parts per million if very low volume applications
are employed, will be satisfactory.
The following ate illustrative Examples of plant growth regulating
compositions according to the invention; parts stated are by weight
unless otherwise specified.
y ( 4 chloro 2 methylphenoxy) Tmethylbutyrate as a colourless liquid,
boiling at 157-158 C at 0 3 mm Both the crude ester and the distilled
ester are suitable for the preparation of formulations for use as
selective herbicides In a similar manner, there may be prepared N
butyl y ( 4 chlorophenoxy) ymethylbutyrate boiling at 126-30 C J
0.11-0 14 mm.
EXAMPLE VIII.
7 y( 4 Chloro 2 methylphenoxy) ymethylbutyric acid ( 28 5 g),
fi-n-butoxyethanol ( 24 8 g), concentrated sulphuric acid ( 0.8 cc)
and benzene ( 100 cc) were heated as above and the water again removed
continuously The ester was purified in the same way as that described
in the preceding Example and the product f-n-butoxyethyl y ( 4 chloro
2 methylphenoxy) methylbutyrate, boiled at 189-190 C at 0 3 mm Again,
both the crude and the pure ester are suitable for the preparation of
non-volatile formulations of selective herbicides.
EXAMPLE IX.
V ( 2:4 Dichlorophenoxy) y methylbutyric acid ( 14 25 g) was refluxed
for two hours with an excess of thionyl chloride The EXAMPLE X.
Sodium y ( 2 methyl 4 chlorophenoxy) methylbutyrate (acid dissolved in
theoretical quantity of caustic soda) Ethylene di-amine tetra-acetic
acid Sodium hydroxide Water 47 parts 0.2 parts 0.5 parts to 100 parts
by volume The foregoing constitutes a stock concentrate one part by
volume of which can be added to 29 parts by volume of water for weed
control application at the rate of 15 gallons per acre.
EXAMPLE XI.
In the concentrate of Example X the said sodium salt was replaced by
50 parts of the corresponding potassium salt.
EXAMPLE XII.
To either of the formulations of Example X or XI, 2 O parts by weight
of sodium lauryl sulphate may be added.
EXAMPLE XIII.
42 parts by weight of y-( 4-chloro-2-methylphenoxy)-y-methylbutyric
acid was warmed with 25 parts by weight of diethanolamine until the
acid had dissolved Water was added to give 100 parts by volume.
One part by volume of this concentrate could be diluted with 14 parts
by volume of water for weed control application at the rate of 15
gallons per acre 85 EXAMPLE XIV.
In a formulation of the type described in Example XIII 20 parts of
diethylamine were substituted for the diethanolamine.
EXAMPLE XV 90
In formulations as described in Examples XIII and XIV, a quantity of
"Texofor" F, a non-ionic wetting agent of the alkyl phenolethylene
oxide type, may be incorporated.
The next following Example illustrates 95 ester formulations made up
as emulsions.
These are usually prepared in the form of self-emulsifying
concentrates in which the ester and the emulsifying agent is dissolved
in a larger bulk of a solvent (usually a mineral 100 oil or an
aromatic solvent such as xylene) or in which the emulsifying agent is
dissolved in the ester with the possible addition of a sma 13 bulk of
a co-solvent.
785,049 785,049 EXAMPLE XVI.
Ethyl y ( 4 chloro 2 methyl phenoxy)7-methylbutyrate Sodium di-nonyl
sulpho-succinate "Texofor" D 40 (a castor-oil polyethylene oxide
condensation product) 48 parts 3 parts 11 parts Shell oil 132 (a light
grade mineral oil) to 100 parts by volume 1 part by volume of this
concentrate can the rate of 15 gallons per acre as a weed killer be
mixed with 59 parts by volume of water preparation to form a stable
emulsion for application at EXAMPLE XVII.
Triethanolamine salts of y-( 2: 4-dichorophenoxy)-y-methylbutyric acid
Water 9 parts (calculated as the acid) to 100 parts This concentrate
is diluted at the rate of 200 c c to 100 gallons of water and applied
for the prevention of fruit drop at the rate of to 400 gallons per
acre according to the density of the orchard It can, if desired,
contain one part of Texofor F.
EXAMPLE XVIII.
2,000 parts of y-( 2: 4-dichlorophenoxy)y-methylbutyramide (calculated
as the acid) is made up to 1,000,000 parts with a mixture consisting
of one part of talc and 3 parts of kaolin It is applied for the
prevention of fruit drop at the rate of 2 to 4 cwts per acre according
to the density of the orchard.
In the foregoing Examples reference is made to the words "Texofor" and
"Shell"; these words as used therein are Registered Trade Marks.
* Sitemap
* Accessibility
* Legal notice
* Terms of use
* Last updated: 08.04.2015
* Worldwide Database
* 5.8.23.4; 93p
* GB785050 (A)
Description: GB785050 (A) ? 1957-10-23
Improvements in or relating to nuclear reactor heated boiler systems
Description of GB785050 (A)
PATENT SPECIFICATION 785,
Inventors:-RICHARD VALENTINE MOORE and WILLIAM ROBERT WOOTTON.
X mi Date of filing Complete Specification: Jan10, 1956.
Application Date: Jan 10, 1955 No 759155.
Complete Specification Published: Oct 23,1957.
Index at Acceptance:-Classes 110 ( 3), B 2 M 6; 122 ( 3 W, Q; and 123
( 2), A( 4 A: 8 G 1).
International Classification:-F Old F 021 F 22 b.
COMPLETE SPECIFICATION.
Improvements in or relating to Nuclear Reactor Heated Boiler Systems.
We, BABCOCK AND WI Lcox L Imi TED, of Babcock House, Farringdon
Street, London, E C 4, a British Company, and RICHARD VALENTINE MOORE,
of the United Kingdom Atomic Energy Authority, London, a British
Subject, 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 nuclear reactor heated boiler
systems of the kind comprising a nuclear reactor and a boiler having
means for circulating a heat transferring fluid through the reactor
and then through the boiler in a closed circuit.
It is a desirable object in such a system to operate the reactor in a
manner so that the temperatures of the fluid on entering and leaving
the reactor are controlled at or substantially at predetermined
figures or range of figures as the heat output of the reactor changes
This object may be achieved by providing a controlled by-pass to the
boiler, but in many systems, for example in the case of a system using
a pressure gas fluid, the massive duct or piping, valve gear and
expansion joints associated with a by-pass are so cumbersome that a
more simple form of control is sought.
According to the present invention a method of operating a nuclear
reactor heated boiler system of the kind described and in the manner
specified comprises controlling the mass flow of the heat transferring
fluid to maintain the temperature at the outlet from the reactor at or
substantially at a predetermined figure or range of figures according
to load and controlling the preslPrice 3 s 6 d l sure in the boiler to
maintain the temperature at the inlet to the reactor at or
substantially at another predetermined figure or range of figures
according to load.
The advantage that primarily arises from the invention relative to the
by-pass operation is that the cumbersome by-pass ducting, valves and
expansion joints are substituted by a simple pressure control valve on
the boiler and a speed controller on the circulators for the heat
transferring fluid.
Further advantages arise from another form of the invention wherein a
multiple pressure boiler system is used (The use of a double pressure
boiler in combination with a nuclear reactor has been referred to
previously in " Nuclear Reactors and Power Production " by Sir
Christopher Hinton:
James Clayton Lecture 1954; The Institution of Mechanical Engineers) A
multiple pressure boiler system may comprise high and low pressure
boiler units in series or parallel relative to the reactor coolant
flow and may also include multiple units in parallel With a multiple
pressure boiler it is possible to arrange that the temperature of the
fluid on entering the reactor is controlled at or substantially at a
predetermined figure, or range of figures as the heat output of the
reactor changes, by manipulating one boiler pressure only or by
manipulating first the lowest pressure and then higher pressures in
ascending order In the case of a double pressure steam generating
boiler coupled to drive a turbo-electric generating plant using a
double pressure cycle for example, it can be arranged that the
pressure of the high pressure part is kept constant at the turbine
whilst the low pressure part is adjusted to give the required .,,,c,,
L___J Lio SO 785,0510 control of temperature at the inlet of the
reactor.
Automatic control can be obtained with apparatus providing automatic
control of ) the mass flow of the heat transferring fluid by varying
the speed of the fluid circulators according to impulses received from
thermostats measuring the outlet fluid temperature of the reactor, and
automatic control of the 10) boiler pressures by varying the opening
and therefore the throttling action of the steam outlet valves
according to impulses received from thermostats measuring the inlet
fluid temperature of the reactor, and 1.5 from pressure-stats
measuring the steam pressure at the high pressure inlet of the turbine
in the case of multiple pressure plant.
The invention therefore also resides in a nuclear reactor heated
boiler system comprising a nuclear reactor, a vapour generator, means
for circulating a heat transferring fluid through the reactor and in
heat exchange relationship with a working fluid in the vapour
generator, means for varying the mass flow of the heat transferring
fluid in order to maintain its temperature on leaving the reactor at
or substantially at one predetermined figure or range of figures
according to load and means for varying the pressure in the working
fluid to maintain the temperature of the heat transferring fluid on
entering the reactor at or substantially at another predetermined
figure or range of 3,5 figures according to load.
An example (constant reactor temperature system) according to the
invention will now be described with reference to the drawings:Figures
1-4 of which accompanied the -o Provisional Specification and Figure 5
accompanies the Complete Specification.
Figure 1 is a flow diagram showing manual control.
Figures 2, 3 and 4 are graphs.
4-5 Figure 5 is a flow diagram showing automatic control.
In Figure 1 a pressure gas cooled nuclear reactor vessel 250 contains
a reactor core structure 260 and control rods 251, and has 54)s four
outlet ducts 252 and four inlet ducts 253 for a gas coolant The ducts
252 connect with respective boilers 254 through valves 255 (only two
boilers being shown) The ducts 253 connect with the respective boilers
w 254 via valves 286 and circulators 287 driven by variable speed
motors 256 One small capacity circuit 266 having a blower 272 is
provided to circulate gas through the core in a closed circuit Drying
and filter units kw 295 are provided across the circulators 287.
About 2 % of the coolant circulation is treated in these units For
emergency purposes D C pony motors 257 are coupled with the
circulators 287 via freewheels 255 k 55 which run disengaged under
ordinary conditions and engaged under emergency conditions.
On the steam generating side there is provided within each boiler 254,
sections 296 and 297 for generating high and low pressure 70 steam
respectively The high pressure steam leaves the section 296 by way of
a non-return valve 259 and a valve 261 whence it passes to a turbine
264 via a speed and pressure control valve 262 The low pressure steam
75 leaves each low pressure section 297 by way of a non-return valve
267 and pressure regulating valve 268 whence it passes via a pressure
control valve 269 to a suitable point in the turbine 264 The valve 269
is an 81) automatic spillover valve operated by upstream pressure and
the spill-over is adjusted over a control line 290 The turbine has a
condenser 273 and cooling tower 274 A dump condenser 275 is provided
and to 85 this are connected the high and low pressure lines via
valves 276 and 277 respectively.
Safety valves 278 are provided Feed water passes from the condensers
273, 275 to the boilers 254 by lines 291 90 On the electrical side an
alternator 279 is coupled with the turbine 164 (A second turbine and
alternator are associated with the two boilers not shown in the
drawing) The output of the alternator 279 goes to a 130 generator
control room 289 by a line 280 whence the electricity is distributed
to an output line 281 and to a line 282 feeding the motors 256.
On the control side there are three main 1 tf control functions each
controlled remotely by manual control from a reactor control room 283
The first of these control functions is that of reactor heat output
which is controlled in the normal way by inanipula 1 o) tion of
control rods 251 This control is indicated in the drawing by line 284
The second of the functions that of speed control of the circulators
287 to keep the temperatures of the gas in ducts 252 constant This 110
control is indicated by the line 285 The third control is that of
setting the pressure control valve 269 over control line 290 so that
the pressures of the associated low pressure boiler sections are
controlled and 115 hence the temperature of the coolant gas emerging
from the boilers 254 and entering the reactor This control is
indicated by the line 290 Temperature measuring lines 265 are taken
from measuring points 293, 294 o The valves 261 and 268 can be trimmed
and the speeds of circulators 287 can also be trimmed to give
identical conditions on all boilers.
The operation of the reactor is described I' 3 with reference to the
graphs of Figures 2, 3 and 4.
In the design chosen the reactor gas coolant is carbon-dioxide at 115
p s i a and it is arranged to leave the reactor at 637 VF 13 o) :}
temperature conditions of the low pressure section of the boiler at
full load and curve O shows the temperature conditions at 10 % full
load The arrow P shows the temperature variation in the low pressure
evapora 70 tor section as the load varies from 109 % to 10 % full load
It is this temperature variation which serves to shape the temperature
curves Q, R of the reactor coolant gas in the boiler If one considers
the case 75 of load falling, then the reactor coolant gas mass flow
decreases, so that the gas temperature throughout the boiler gas flow
path tends to fal L If conditions in the low pressure section of the
boiler were to remain Sq unaltered, then at 10 % of full load the gas
temperature would be below curve R, and the outlet gas temperature in
particular would be appreciably lower than T 2, so that the inlet
temperature to the reactor would 8,5 be correspondingly too low By
increasing the pressure and hence the water and steam temperatures in
the low pressure section of the boiler as the load decreases, the
outlet gas temperature is maintained at suitable 90 values such as the
value T 3 at 10 % of full load, and the inlet gas temperature to the
reactor kept constant at 284 1 F (curve B of Figure 2).
In the high pressure section of the boiler 95 as shown in Figure 4
conditions in the evaporator and superheater do not vary substantially
between 10 % full load and full load As the load falls the temperature
of the superheated steam rises slightly l O;) The evaporator
temperature falls slightly as the boiler drum pressure (curve M of
Figure 3) is reduced to keep constant pressure at the turbine with
reduced steam generation.
Now referring to Figure 5, the automatic 105 control is described (The
same reference numerals are used in both Figures 1 and 5 for the same
components) The reactor vessel 250 and core structure 260 are shown
There are four outlet ducts 11 252 and four inlet ducts 253 for
reactor gas coolant which is circulated (as described with reference
to Figure 1) by circulators 287 driven by variable speed motors 256
Now it is required that the temperature in the 115 outlet ducts 252 is
maintained constant.
This is achieved by a hydraulically operated system comprising a
pressure source 300 feeding four temperature sensitive valves 301 via
a feed line 302 and return line 303 The 120 valves 301 are temperature
sensitive according to the temperature of bimetallic elements 304
associated with each duct 252, the valve at the maximum temperature
exerting overriding control The position taken up by 125 the
over-riding valve 301 governs the pressure in a control line 305 which
is coupled with a relay 306 arranged to move a lever 307, thereby to
adjust the setting of the speed controller of motors 256 to alter the
130 (curve A of Figure 2) and to enter the reactor at 284 F (cur ve B
of Figure 2).
The temperature fall in the boiler 254 is to just under 28-4 F at 10 %
full load and to 275 F at full load (Curve C of Figure 2) The
temperature rise in the circulators 256 restores the temperature to
the predetermined constant value of 23 i F on the reactor inlet side.
The quantity of steam evaporated is indicated by curve D of Figure 2
for the low pressure section and by curve E of Figure 2 for the high
pressure section.
Figure 3 (curve F) shows a relationship I 5 between reactor heat
output and reactor coolant gas mass flow This is a straight line at a
gradient such that the temperature of the reactor coolant gas on the
outlet side of the reactor is constant at the predetermined
temperature for all values of reactor heat output between 10 % full
load and full load The curves G and H respectively show low pressure
and high pressure superheated steam temperatures, whilst curves J and
I show low pressure steam pressures, and curves K, L and M show high
pressure steam pressures over the range 10 % full load to full load
Curves J and K are of particular interest These carves show that 3 ')
whilst the pressure at the high pressure inlet to the turbine (curve
K) remains constant over a load range variation of 90 %, the low
pressure boiler drum pressure (curve J) falls as the load increases
That is, the temperature of low pressure steam generation also falls
as the load increases which stabilises the reactor coolant gas
temperature on the inlet side of the reactor which would, in the
ordinary course, rise with the increased mass 44) flow brought about
when the load increases.
In Figure 4 the mechanism of control is shown in more detail In this
figure the temperatures of the steam and reactor coolant gas through
the boiler are shown for full load and 10 % full load conditions As
marked at the top of this figure the boiler is constructed of nests of
tubes in the following sequence: at the bottom, an economiser serving
high and low pressure sections of the boiler, next, a low pressure
evaporator followed by a low pressure superheater, then a high
pressure economiser followed by a high pressure evaporator and a high
pressure superheater.
The boiler inlet gas temperature to the boiler is represented by T 1,
the boiler outlet gas temperature at full load (curve Q) by T, and the
outlet gas temperature at 10 % full load (curve R) by T 3 As mentioned
above, d O when heat has been added in the circulators, the gas
temperature in to the reactor is constant regardless of load, that is,
Ts and T 2 are both raised to a common temperature after passing
through the circulators.
Curve N shows the water and steam 785,050 785,050 mass flow of coolant
in a sense to stabilise the temperature of coolant flowing in ducts
252.
The complementary requirement is that the temperature in the inlet
ducts 253 is kept constant This is achieved by a hydraulically
operated system comprising the same pressure source 300 but feeding
four temperature sensitive valves 308 via a feed line 309 and return
line 310 The valves 308 are temperature sensitive according to the
temperature of bimetallic elements 311 associated with each duct 253,
and again, the valve at maximum temperature exerts over-riding control
The position taken up by the over-riding valve 308 governs the
pressure in a control line 312 which is coupled with a relay 313
arranged to move a lever 314, thereby to adjust the setting (bias) of
the valve 269 to alter the pressure in the line 299 from the L P
section of the boilers, in a sense to stabilise the temperature of
coolant flowing in ducts 253.
Starting up the plant described in Figure 1 is carried out by
connecting steam lines 298 and 299 to the dump condenser 275 and
setting the circulators 287 to a speed associated with a moderate
reactor power The reactor is brought to a critical state at a low
power (about 1 KW), the reactor power is then progressively increased
whilst the core temperature is strictly limited to avoid too rapid
heating of fuel elements and plant.
The inlet gas temperature to the reactor is observed and the pressure
setting of valves 268 adjusted to be at a low value so that heating-up
of the whole system takes place over a safe period The outlet gas
temperature is also observed and controlled, at this stage, either by
control rod adjustment or by the speed of the circulators 287 As steam
is generated it flows to the dump condenser 275 When full steam
pressures and temperatures have been reached the generator control
room staff can utilise the steam by diverting it from the dump
condenser to the turbine.
For shut down, the reactor heat output is decreased until the plant is
down to 10 % full load with reactor gas inlet and outlet temperatures
still constant The dump condenser 275 is then commissioned, the
reactor shut down and the circulators speeded up (e.g 40 % full flow)
to achieve cooling As the gas temperatures fall, pressure in the high
pressure evaporators falls and valves 268 are unthrottled gradually in
order to give eventually a low pressure section evaporator drum
pressure of 30 p s i g.
The reactor outlet gas temperature is then about 150 TC and the power
is about 1 % full load The gas system is depressurised and two of the
four circulators are run at full speed to maintain temperature
conditions with the depressurised gas.
Control of electrical output independently of reactor output can be
achieved by using the dump condenser 275 in parallel with the turbines
264.
Whilst the invention has been described 7 io in relation to generating
electrical power by steam other uses of the invention are envisaged
For example the steam could be used for propulsion such as in a ship
or for space heating or for chemical processes I.
The invention is not limited in its application to steam generation
Other working fluids such as diphenyl jdiphenyl-oxide eutectics may be
used.
* Sitemap
* Accessibility
* Legal notice
* Terms of use
* Last updated: 08.04.2015
* Worldwide Database
* 5.8.23.4; 93p
* GB785051 (A)
Description: GB785051 (A) ? 1957-10-23
Purification of terephthalic acid
Description of GB785051 (A)
Translate this text into Tooltip
[75][(1)__Select language]
Translate this text into
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.
COMPLET SPECIFICATION
Purification of-Terephthalic Acid
We, IMPERIAL CHEMICAL INDUSTRIES
LIMITED, of Imperial Chemical House, Millbank, London, S. W. 1, a
British Company, 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 purification of
terephthalic acid.
Terephthalic acid as commercially produced often contains coloured and
colour-forming impurities. We have now found that this crude
terephthalic acid can be purified by recrystallisation from a lower
member of the fatty acids group.
According to our present invention we provide a process for purifying
crude terephthalic acid, which comprises heating-the-crude
terephthalic acid with a fatty acid having less than 7 carbon
atoms,-until solution occurs, cooling the resultant solution and
allowing the terephthalic acid to crystallise out.
We have found acetic acid, propionic acid and butyric acid to be very
suitable for use in our process and of these three acids we prefer to
use acetic acid. Although not as efficient in removing the impurities
as the pure acids, we have found aqueous solutions of the lower fatty
acids to be efficient for many purposes.
Terephthalic acid is sparingly soluble in these fatty acids at their
boiling points at atmospheric pressure and under these conditions
coloured and colour-forming impurities can be partly extracted from
terephthalic acid.
In the preferred process of our-invention we operate under pressure at
temperatures above that of the normal boiling point of these acids, or
their aqueous solutions and under these conditions the coloured and
colour-forming impurities are effectively removed.
If preferred, a first purification may be made by using any known
method, such as a simple recrystallisation of the crude terephthalic
acid from water under pressure, before subjecting the terephthalic
acid to a further purification according to the process of our present
invention.
We have found the process to be particu- lary suitable in removing
impurities from crude terephthalic acid which has been obtained by an
air oxidation process.
The particle size of crude terephthalic acid obtained by an air
oxidation process is normally in the rangeof5-50whilst terephthalic
acid purified by crystallisation from water under pressure has a
particle size in the range of 100500je. By the-process of our
invention,-terephthalic acid is obtained having a particle-size of the
erder of 1000 which size has been~found to be very suitable for use in
the manufacture of the highly polymeric polymethylene terephthalates,
these materials..being of great commercial importance in the
manufacture of filaments, fibres and films.
The following examples in which all parts and percentages are by
weight illustrate but do not limit the scope of our invention :-
EXAMPLE 1
5 parts of crude terephthalic acid are refluxed at 118~ C. with 95
parts of glacial acetic acid for one hour after which time the
terephthalic acid is removed by filtration at 100 C. and washed with
glacial acetic acid.
This process is once more repeated.
A 4% solution of the purified terephthalic acid in 17% 1 aqueous
ammonia is found on spectrophotometric examination to-have an optical
density of 1. 60,-when measured at-a wavelength of 380 m.
EXAMPLE 2
12 parts of the same crude terephthalic acid as used in Example 1 are
added to 88 parts of glacial acetic acid. The resulting suspension is
heated at 200 C. for one hour under pressure and then allowed to cool.
The crystallised terephthalic acid is removed by filtration and washed
with gradal acetic add.
A*4%'ablutionofthispurinedterephtbalic 'sadd in 17% : aqueous ammonia
has an optical
density when measured as in Example 1) of
0. 795.-'---""
By comparison, the crude terephthalic acid,
used in Examples 1 and 2 has an optical-den-
sity of 1. 73. Thus under the conditions of
purification in Example 1 the impurities are
only partly extracted as compared with those
of Example 2 where the impurities are effec-
tively removed.
The table below gives the optical densities
of samples of crude terephthalic acid, obtained
by an air-oxidation process and purified
according to the process of our invention from
each of the three preferred acids-acetic, pro
pionic and butyric adds* and from a 50%-
aqueous solution of acetic acid. For pur poses of comparisbn, the
optical densitie. s. are given-of the crude terephthalic acid and- :
that
of the crude acid purifiez by a known method,
i. e. :,fromwateraloneunderpressure.
TABLE -Optical
Terephthalicladd;'-'densjny
Recrystallised from acetic acid - 0.795
Recrystallised from propionic acid 1.10
Recrystallised from butyric acid - 0.95
Recrystallised from 50/50 acetic actd/water-''- :"-''-:r-1\14'
Recrystallised from water - - 1.48
Crude terephthalic acid - - - 1.73 Whatwedaimis:-
1. A process for purifying crude terephthalic
acid, which comprises heating the crude
terephthalic acid with a fatty acid having less
than 7 carbon atoms, until solution occurs, cooling the resultant
solution and allowing the
terephthalic add to crystallise out.
* Sitemap
* Accessibility
* Legal notice
* Terms of use
* Last updated: 08.04.2015
* Worldwide Database
* 5.8.23.4; 93p
* GB785052 (A)
Description: GB785052 (A) ? 1957-10-23
Improvements in or relating to pressure vessels
Description of GB785052 (A)
COMPLETE SPECIFICATION Impro,vemen,ts in, or, relating,to Pressure'
Vessels.
I, GORGE HUGO- VON Fucus, a citizen of the United States of America,
of 1221 Garfield
Avenue, Niagara Falls, New York, United
States of America, 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:
This invention relates to pr & ssure' vessels or bombs and is
particularly concerned with small pressure vessels or bombs which are
to be heated to elevated temperatures for example in a liquid bath.
It is an' object of the invention to provide such a bomb or pressure
vessel which may be utilized in carrying out chemical reactions and
tests of various types at elevated temperatures and pressures.
Another object of the present invention is to provide a bomb which is
resistant to attack by substances contained therein.
Another object of the invention is to provide a bomb which has a high
thermal conductivity.
A further object of the invention is to provide a bomb which is of
siffiple, durable construction, arid which may be readily assembled
and taken apart, and easily and effectively sealed.
According to one aspect of the invention there is provided a bomb for
use at elevated temperatures and pressures comprising~ a hollow,
cylindrical body open at one end, a cap for said open end, a retainer
for said cap detachably secured to said body, and a tubular stem
carried by said cap and providing communication with the interior of
said body, said body and said cap being formed of metal having a
thermal conductivity between room temperature and about 300'C. 'of at
least 0.100, said stem being formed of a metal having a relatively low
thermal conductivity as compared to said body, and the interior
surfaces of said bomb being provided with a metal coating resistant to
chemical attack.
According to a second aspect of the invention there is provided a bomb
for use at elevated temperatures and pressures comprising a hollow,
cylindrical body open at one end, a cap for said open wend,' a
retainer for said cap, detachably secured to said bddy, and a tubular
stem carried by said cap and providing communication with the interior
of said body, said body and said cap being formed of "'metal having a
thermal conductivity between room temperature and about 300 C. of at
least 0.100, said stem being formed of a metal having a relatively low
thermal cpnductivity as compared to said body, and the interior of
said bomb having a. catalytic metal surface.
The preferred embodiments of the invention will now be described by
way of'-example with reference to the accompanying drawings, in which:
Figure 1 is a vertical sectional view of one embodiment of the present
invention;
Figure 2, is a bottom view of the bomb shown in Figure 1;
Figure 3 is a top plan sectional view of the assembled bomb without
the stem and with a portion of the cover or cap and the retainer
therefor broken away;
Figure 4 is a vertical sectional view of a second embodiment of the
present invention showing the stem in elevation;
Figure 5 is a transverse sectional view on the line 5-5 of Figure 4;
and
Figure 6 is a bottom view of the bomb of
Figure 4.
Referring now to Figures 1 to 3 of the drawings, the bomb comprises a
hollow cylindrical body portion 11, which is preferably formed by
casting or by machining from a forged or cast metal block, although it
may be produced by drawing or extrusion. The block 11 has an integral
bottom 12 and adjacent its upper end is provided with external threads
which gre preferably finned on a thickened portion 16- of the
cylindrical wall, thereby avoiding weakening of the wall.
A cap 18 in the form of a disc is provided
for the body 11. The lower portion of the cap 18 is reduced in
diameter to permit it to extend
into the top of the body 11. The periphery
of the top portion of the cap-therefore provides
an annular flange 21- which is of approximate y
the same external diameter as the external
diameter of the body 11- at its lop. Centrally
of the top face of the cap 18 there is provided
a short, upwardly projecting boss 22. Extend
ing axially through the boss 22 and the cap 18
is a passage 23, the upper portion of which
is internally threaded.
The cap 18 is held-in place on the-body 11
by a tubular retainer 28, the upper end of
which is preferably formed externally as a
hexagonal nut 29. The lower end 31 of the
retainer, of larger diameter, is provided with
internal threads adapted to engage the threads
formed on the thickened portion 16. adjacent
the upper end of the body 11. A bore 33 is
provided in the nut portion 2'9 of the retainer
-2-8 and is of suffiaent diameter to receive and
permit access to the boss 22 of the cap 18.
As will be seen from Figure 1, the interior,
annular shoulder 34 in the lower end of the
retainer 28 engages the flange 21of the cap
18 when the retainer is threaded onto the body.
To permit tight sealing of the bomb, the outer
end of the body 11 is provided with an annular
groove 36, preferably rectangular in cross
section and the lower, surface of the flange 21
on the cap 18 is formed with a registering
annular rib or bead 37. The latter may be of
rectangular cross section or may be convex.
Complete sealing is obtained by inserting a
suitable gasket (not shown) within the groove
36, the gasket being compressed by the bead
37 when the retainer 28 is tightened. Only
the annular shoulder 34 of the retainer engages
the cap 18 when the bomb is closed. The
relatively small surface areas ,in contact makes
it easier to seal the bomb as excessive friction
is avoided and greater force is exerted on the
flange 21.
The threaded portion of the passage 23 is
adapted to receive a tubular stem or connector 38, an axial- nipple 41
on the lower end 40 of the stem being externally threaded for
engagement therein. At its outer end the stem 38 may be enlarged as
shown at 39 and the bore 42 therein provided with internal threads 43.
A threaded radial passage 44 may also be
provided in the enlarged end 39 if desired.
Preferably the lower end 40-of the stem 38 is provided with a
hexagonal or other desired non-circular exterior-for such a distance
from the nipple, 41 as to extend substantially above the retainer 28,
thereby permitting convenient engagement of a wrench on the stem.
In using a bomb of the type described, one or ,more solid or liquid
reacting materials is placed in the body 11, a suitable gasket is
inserted in-the groove 36 atid the cap 18 is put
in place. The threads of the retainer 28 are then engaged with the
external threads on the
body and the retainer is turned down until the
shoulder 34 engages the flange 21 of the cap
and the vessel is sealed by the-gasket. The stem 38 may then be
connected to -the cap, and
a desired gaseous reactant may be admitted
through the bore 42 in the stem and the com
municating bore 23 in the cap: if desired, the
bomb may ,be evacuated prior:tolling with
gas or it may be flushed out by repeatedly
filling it with the desired gas under pressure
and releasing the pressure. A pressure gauge
(not shown) may, if desired be connected to
one of the passages at the outer end 39 of, the
stem 38.
Heating of the bomb may be accomplished
in any desired manner. When, however, as is
usually the case, it is necessary to have accurate temperature
coritrol, heating by immersion in
an oil bath or the like is preferred. In the event agitation of the
contents of the bomb is desired, it may be easily obtained by
inclining the bomb .in the oil bath or the like and rotating it. For
convenience in securing rotation, the bottom
12 of the bomb body 11 is provided with spaced projections 14 which
may be engaged by a suitable driving element (not shown) beneath the
surface of the bath. The degree of agitation may.be increased by
including in the bomb charge one or more inert objects of
substantial size which will tumble about as the bomb is rotated.
Referring now to the second embodiment
shown in Figures 4 to 6, the bomb, generally
designated by the reference character 111, com
prises as before a hollow cylindrical body por
tion 112, the bottom 113 of which is integral
with the cylindrical wall thereof. Adjacent its
upper end the body 112 is provided with
external threads 114 which are preferably
formed on a thickened portion 116 of the
cylindrical. wall in order to avoid weakening thereof.
A cap 117, formed as a disc, is provided for the body 112. The
external diameter of the cap 117 is approximately the same as the
external diameter of the body 112. However, the lower portion 118 of
the cap is of smaller diameter so that said lower portion may extend
downwardly into the mouth of the body portion 112. A short, upwardly
projecting boss 119 is provided centrally of the top face of the cap
117 and a passage 121 extenas axially through the cap and the boss
119. At its upper end the passage 1Z1 is provided with screw threads.
In the lower face of the portion of the cap 117 which extends
outwardly beyond the lower portion 118 thereof, there is provided an,
annular groove 122 in which is seated a gasket 123. When the cap 117
is in place, the gasket 123 rests on an annular rib or bead 124 formed
around the top of the body portion 112. As shown, the bead 124 is
substantially semi-circular in cross section. However, beads of other
configurations may be used if desired.
A tubular retainer, generally dersignated by the numeral 126, is
employed for holding.the cap .117 in place on the body 112 of the bomb
111. The lower portion of the retainer. 126 is cylindrical and is
provided with internal threads adapted to engage the threads 114 at
the top of the body portion 112. The upper portion. 128 of the
retainer 126, which may conveniently be of smaller- diameter, is also
preferably cylindrical and is provided. with a bore- 129 of; somewhat
larger diameter than the boss 119- on the cap 117. A plurality of
equally spaced radially arranged holes or b.ores
131 for convenient engagement of, a spanner wrench (not shown) are
provided in the upper portion -128'. of the retainer 126. The cuplike,
lower portion 127 of the retainer is also provided with a plurality of
radial drain holes
132 ,that extend inwardly from the periphery to the interior thereof;
A threaded nipple 134 provided on the lower
end 136 of a tubular stem or connectbr 133 is threadedly engaged in
the upper portion of the passage 121 through the boss 119 At its
outer or upper end the stem 133 may be of
greater diameter as shown at 137 and the bore
138 therein is preferably enlarged and provided with internal threads
139. There may also be provided, if desired, a radial passage --141 in
the end 1-37. For convenience in assembly, the lower. end 136 of the-
tubular stem 133 is preferably enlarged above the nipple 134 and
formed with a hexagonal or other non-circular cross-section for a
distance above the. nipple sufficient to permit the engagement of a
wrench thereon,
Sealing of the bomb of the present invention is obtained by pressing
the gasket 123 carried by the cap 117 against the annular bead 124.
The bead and gasket are forced into tight contact by ,the engagement
with the upper surface of the cap 117 of an internal, annular shoulder
143 located at the inner end of the cup-like, lower portion 127 of the
retainer 126.
The bomb of Figures 4 to.'6 is used in-much the same manner as the
bomb shown in Figures
1 to 3. One or more solid or liquid materials is placed in the body
112, a suitable gasket is inserted in the groove 122 of the cap 117
and the cap is put in place on the open end of the body. The internal
threads in the lower portion 127 of the retainer ,126 are - then
engaged with the threads 114 on the outside of the body 112 adjacent
its top and the
retainer is turned down on the body until the shoulder 143 engages the
upper face of the cap 117 to compress the gasket 123 against the
annular bead 124, thus sealing the bomb.
The tubular stem 133 may then be connected to the cap 117 by the
threaded nipple 134 and any desired gaseous or liquid reacting
material may'be admitted through the bore 138 of,the stem and. the
communicating bore or passage
121 in the cap.
During heating by immersion in an oil bath orthe like the bomb while
immersed may be rotated and a plurality of spaced holes or sockets 146
are provided in the bottom of.the bomb. body 112 for convenienc in
rotating it.
These.sckets-may be engaged by a suitably
formed plate .,or shaft end (not shown) immersed in the- heating bath
and connected to rotating means (not shown).
.As mentioned above,-the present invention is particularly designed
for use in a. heating
bath such as hot oil or the like. - -When the bomb is withdrawn from
the bath any heating
fluid remaining around the stem- 133-will drain ;out between the, cap
117 and the top portion
128 of the. retainer 126 through the ports or drain holes. 132 in the
latter. Any heating fluid, remaining in the lower portion 127 of the
retainer will also drain outward when the retainer is-. unscrewed and
removed from the
body .112 because of the upwardly projecting
annular bead 124 around the top of the bogy.
Contamination of the bomb contents.by heating
fluid is thus avoided. The drain features just
described make use ,of the- bomb very convenient since practically all
of the heating fluid will drain from the bomb while it is held
momentarily over the heating tank. Spilling of quantities Of the
heating fluid in undesired places as the bomb is dismantled is conse
quently prevented.
Bombs of the type with which the present invention is concerned are
adapted for a wide variety of, uses involving temperatures and
pressures above normal. For example, they may be used in carrying out
various catalytic reactions such as hydrogenation, for chlorination or
oxidation of organic materials, and for other reactions in which a
closed system is
desired or pressure is necessary.
The - materials- fro which bombs constructed in accordance with the
present invention are formed. are. of great importance.
While attack of the bomb by one or more of the reacting
materisil's'is5'of course, two be avoided; it will be realized that
other factors are also involved. Thus, sinceheating-of-the
body contents, if heat must be supplied, will usually be by
application of heat to the exterior
of the bomb, the bomb body should - have a relatively high heat
conductivity, i.e. at least
0.100 between room temperatures and about 300 C. Further, operation at
superatmospheric pressures necessitates a body having adequate
strength. The latter is preferably
obtained by the use of metals having relatively
high strengths rather than by making the body
walls thicker since the amount of heat stored in the body and the
consequent lag in heating
and cooling will thus .be less.
Ordinary low carbon steels, i.e. mild steels, have adequate. strength
for bombs of the present general type and have a rather good thermal
conductivity. Such steels are, more
over, relatively,- inexpensive and easy to machine.. However, iron.
'is strongly catalytic for many reactions and may interfere with the
carrying out of a particular desired reacticin
Furthermore, steel is not resistant to corrosion by many of the
materials which may be used or formed "ill a bomb. "On the other
'hand, materials which-have a high resistance to corrosion such as
tantaluin, stainless steel,'titanium and the like are either
prohibitively expensive or, like stainless steel, have very' low
thermal conductivities, thus p-teventing rapid heating and cooling.
It has now been found that, by~ providing a thin coating' "of a:
suitable - metal on- the interior surfaces-of a bomb formed from mild
steel, there may be obtained a relatively in- expensive bomb having
the necessary strength, a desirable thermal conductivity, and lack of
reaction with' the bomb contexts. -For many purposes thin platings of
'nickel 'or chromium will be' satisfactory. Obviously, however, where
special conditions require it; coaungs of other metals may be
employed.
Mild -steels have thermal-conductivities from room temperature up to
about 300 C. of at least .100 as contrasted with those of stainless
steels which ma'y be as low as .045 'at 300C.
It will be understood that there are other metals and alloys having
good thermal conductivities which, when used for the constnic- tion of
a bomb in accordance with the present invention, will in many
cases.have adequate strength. Thus; for example, aluminium and many
aluminium alloys have thermal conductivities at 300 C.. at least as
high as .200.
Certain of such alloys are quite strong.' Magnesium alloys, brass,
phosphor bronze arid even;
cast iron are further examples of metals having thermal conductivities
-of at least' -.100 at elevated temperatures which are suitable for
bombs for certain reactions when provided with an interior coating of
metal inert with respect to the desired bomb contents. When using
certain-metals for coating the interior surfaces of a bomb according
to the present invention the coating may be conveniently applied by
electrpde,position, in some cases over metal undercoats. In
appropriate cases the metal coating may be applied molten or in spray
form. Obviously, the metal coating, however applied, should when
finished be nonporous and smooth to facilitate cleaning of the bomb.
The heat conductivity of the bomb is not materially reduced by the
metal coating of its interior surfaces, even when the metal used for
the coating has a very low thermal conductivity, since the coating
employed may frequently be less than .003 in. In some special cases
such as for certain catalytic reactions the metal coating form the
interior surfaces of the bomb may be active rather than inert. Thus;
for example, copper being an excellent catalyst for oxidation of many
hydrocarbons may be employed as a coating for the interior of a bomb
used in carrying out such reactions. Other similar possibilities will
be apparent to those skilled in the art.
Preferably, the cap -18 or 117is formed of the same metal as the body
11 or 111 of the bomb although this is not essential as there is
little heat transferred to the bomb through the cap. Obviously, the
surfaces of the cap which may come into contact with the bomb contents
should be provided with a suitable metal coating which is desirably
the same as that on the interior of the bomb body. "The retainer 28 or
126 does not come into contact with the bomb contents. Hence, nd
protective coating thereon is required. Care should, however, be taken
to avoid the use of a metal having a thermal expansion greatly
exceeding that of the bomb body in order to prevent loosening of the
retainer when the bomb is heated. The stem 38 br'133 is formed of some
metal different from the metal of the body 11 or 111 and having a low
thermal conductivity. For the purpose, stainless steel, the metal sold
under the Registered Trade mark " Inconel," or other similar alloy is
desirable. Such metals have, from about 300"C. down to room
temperature, thermal conductivities of .065 or less. Consequently, the
heat lost to the air by radiation from the stem will be less and less
heat will be conducted to:the gauge and gas connections provided at
the outer end of the stem. - Gaskets for bombs according to the
present invention may be of various materials, but should, of course,
he inert with respect to the bomb contents. In 'some' cases, a soft
metal such as lead may be used. In other instances, gaskets of
neoprene, plyethylene, polymerized polyhalogenated ethylene materials
such as those sold under the registered trade marks " Kel-F " and "
Teflon ", silicone rubber or similar resilient, plastic materials may
be used.
The 'thermal conductivities set forth above and in the appended claims
are expressed as calories per cm2 per second per C. per cm.
What I claim is: -
1. A bomb for use at elevated temperatures and pressures comprising a
hollow, cylindrical body open at one end, a cap for said open end, a
retainer for said cap detachably secured to said body, and a tubular
stem carried by said cap and providing communication with the interior
of said body, said body and said cap being formed of metal having a
thermal conductility between room temperature and about 300 C. of at
least 0.100, said stem being formed of a metal having a relatively low
thermal conductivity as compared to said body, and the interior
surfaces of said bomb being provided with a metal coating resistant to
chemical attack.
2~-A bomb for use at elevated temperatures and pressures comprising a
hollow, cylindrical body 'open at one end, a cap for said open end, a
retainer for said cap detachably secured to said body, and a tubular
stem carried by said cap and providing communication with the interior
of said body, said body and said cap being formed of metal having a
thermal con