* 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

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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

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.

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* 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.

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* GB785051 (A)

Description: GB785051 (A) ? 1957-10-23

Purification of terephthalic acid

Description of GB785051 (A)

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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.

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.

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* 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