US2921031A

US2921031A - Anti-vesicant composition

Info

Publication number: US2921031A
Application number: US445221A
Authority: US
Inventors: Scherr Harry
Original assignee: Individual
Current assignee: Individual
Priority date: 1942-05-30
Filing date: 1942-05-30
Publication date: 1960-01-12
Anticipated expiration: 1977-01-12

Description

2,921,031 ANTI-VESICANT COMPOSITION Harry Scherr, Baltimore, Md., assignor to the United States of America as represented by the Secretary of War as trustee v i No Drawing. Application May 30, 1942 Serial No. 445,221

6 Claims. (Cl. 252-187) (Granted under Title 35, U.S. Code (1952), sec. 266) The invention described herein may be manufactured and used by or for the Government for governmental purposes without the payment to me of royalty thereon.

This invention relates generally to protective clothing adapted to afford personnel protection against known chemical warfare vesicant agents such as mustard gas and lewisite, and the invention relates in particular to compositions to be used in providing such protective clothing.

It has been found that known chemical warfare vesicant agents, such as mustard gas and lewisite, may be rendered non-vesicant and relatively harmless by some type of halogenation, and particularly by chlorination, so as to convert the vesicants into innocuous products. Conceivably,-any compound having an available halogen atom may be considered as having possible use as an anti-vesicant agent for halogenating or 'chlorinating vesicants. However, due to practical considerations, the chloramides have been found to be most suitable, as a class, to be used as chlorinating agents. Of the class of chloramides, bis dichlorphenyl chlorurea and bis 2,4,6- trichlorphenyl chlorurea have been found to be very satisfactory anti-vesicant agents.

Considerable difliculty has been encountered in, the past in developing compositions and techniques whereby fabric and clothing may be treated with the anti-vesicant agents so as to leave sufficient deposits thereof in the fibers of the fabric or clothing to give effective protection against vesicants and which will adherefirmly thereto so as to resist a reasonable amount of wearand laundering. Generally, the anti-vesicant agents and suitable. inert binders have been dissolved in various volatile organic solvents so as to provide a so-called impregnating com-. position. The fabric and clothing have then been soaked solutions to provide increased solubility of the antirelatively low concentrations of anti-vesicant agents in the impregnating compositions, a large amount of solvent evaporation was required for the amount of anti-vesicant agent deposited in the fabric or clothing.

In view of the foregoing difiiculties of the prior art, one of the principal objects of the present invention is the provision of impregnating compositions for treating fabric or clothing to render the same resistant to chemical warfare vesicants, such as mustard gas and lewisite, which compositions contain in uniform distribution, and at ordinary temperatures, amounts of anti-vesicant or neutralizing agents in excess of the amounts normally soluble therein. Such improved and relatively concentrated impregnating compositions permit very satisfactory impregnation of fabric and clothing at ordinary temperatures, and eliminate the most objectionable difficulties of the prior art in regard to the heating of the impregnating compositions and the extended drying periods required to remove the volatile solvents.

A further object of this invention is the provision of impregnating compositions containing dyeing or coloring material whereby fabric and clothing may, in one operation, be simultaneously dyed and rendered resistant to chemical warfare vesicants such as mustard gas and obvious resides in the inclusion in an impregnating composition; of an ingredient which serves to maintain a substantially uniform distribution throughout the composition of an amount of an anti-vesicant agent in excess of that amount thereof which would be normally soluble and remain uniformly distributed. .When the impregnating composition has only one liquid phase, the added ingredient serves as a suspending agent, while in certain instances where an impregnating composition is in the form of an' emulsion having two liquid phases, the added ingredient appears to function as an emulsifying agent.

For a more complete understanding of the nature and scope of this invention, reference may be had to the following detailed description mentioning certain specific compositions and techniques as illustrative.

One type of impregnating compositions embodying the invention has a single liquid phase and comprises, in

general, an anti-vesicant agent having available chlorine for destroying mustard gas, lewisite and like vesicants, and a hinder, the antivesicant agent and binder being dissolved in an organic solvent in which a suspending agent has been dissolved. The anti-vesicant agents may be such compounds as his dichlorphenyl chlorurea or bis 2,4,6-trichlorphenyl chlorurea, both compounds being selected from the general class of chloramides. Several binders may be used which are inert to the anti-vesicant' agents, such as chlorinated napthalene (Halowax) and chlorinated parafiln. Various organic solvents may be used such as monochlorbenzene, beta trichlorethane, and perchlorethylene. These solvents may be classed as chlororganic solvents. As an example of a suspending agent, ethyl cellulose has been found to be very satisfactory for the purposes intended.

Irnpregnating compositions may include the foregoing 7 ingredients or components in various percentage ranges. a By way of example, very satisfactory impregnating com- Patented Jan. 12, 19.60

positions may bemade according to the following formula:

Percent by weight Ethyl cellulose -4 0.30.5

Monochlorbenzene 5 00-600 Beta trichlorethane 30.0-34.0 Chlorinated naphthalene 1.5-2.5 Chlorinated paraffin 3.0-4.0- Bis 2,4,6-trichlorphenyl chlorurea 5.0-8.0

An impregnating composition having the above general formula may be prepared according to the following steps:

(3) Finally, and preferably just prior to the use of the impregnating composition, the bis 2,4,6-trichlorphenyl chlorurea is added. 1 V

(4) On shaking or other mild agitation, a stable suspensionof low viscosity results. All steps are carried out at ordinary temperatures; a

The technique of impregnating clothing with the forei going type of impregnating compositions is simple and may be referred to as the suspension process. Clothing, without previous drying, is immersed in the impregnating composition and soaked for a few minutes so as to thoroughly wet the same. The clothing is then removed and wrung out soas to remove the'impregnating composition in excess of that required for adequate im-' pregnation. It will be n oted that the impregnation is carried out at ordinary temperatures without treating,

and is adapted to either large, or small scale field impregnation.

According to one embodiment of the invention, irhpregnating compositions may be prepared which may beused to simultaneously dye and impregnate fabric and clothing in one stage at ordinary temperatures. Several classes of dyestuflis may be used, such as: solvent soluble anthraquinone dyestuifs; water soluble anthraquinone' dye-' stuffs; pigment powders; pigment pastes; and, flushed pigments- The flushed pigments have been found to be very suitable for the purpose intended; Thesepigm'ents are produced by first grinding the pigment in water and then transferring or flushing the pigment particles to a medium such as one consisting of ethyl cellulose and monochlorbenzene. The resulting flushed pigment corn- Chlorinated parafiin position maythen be readily'incorporated in the base solution used in'the suspension process for clothing im- 7 pregnation.

'While the present invention was particularly concerned with imparting a khaki shade to white cotton drill, it will be understood that any desired color may beimparted to clothing or. fabric by the proper selection of the pigments in the flushed pigment mixture. A typical formula for an impregnating composition adapted to provide for the simultaneous dyeing and impregnation of white cotton drill to give a khaki shade to the clothing is as follows:

An impregnated and dyeing composition following the above general formula, may be prepared according to the following steps:

(1) The ethyl cellulose is dissolved in the monochlorv benzene and beta I trichloroethane, giving aclear, colorless solution.

(2) The chlorinated naphthalene and chlorinated paraffin are added to the solution of step 1.

(3) The flushed pigment is thoroughly mixed into the solution from step 2. N

(4) Finally, and preferably just prior to the use of the composition, the his 2,4,6-trichlorphenyl chlorurea is added with shaking or other mild agitation.

The technique of treating fabric or clothing with a combined impregnating and dyeing composition is the same as that described hereinbefore in connection with the compositions used only for impregnation.

According to a further embodiment of the invention, emulsion-type impregnating compositions have been prepared which can be used for impregnating clothing or. fabric with anti-vesicant material. These emulsions require strong mechanical agitation such as obtained by a colloid mill or homogenizer. Several types of emulsifying agents may be used to impart reasonable stability to the emulsions. The following is a list of some of the emulsifying'agents that may be used:

Monochlorbenzene -l -;l.. l; 15"

Perchlorethylene 10 5' Emulsifying agent 3' Bis 2,4,6-trichlorphenyl: chlorurea 7 Water; 60

The emulsion is prepared byfirst making a mixture of the monochlorbenzene, .p'erchlore'thylene, chlorinated paraffin, emulsifying agent, 'and bis2,4,6-trichlorphenyl chlorurea. The proper amount of water'is then added to V the above mixture, and the complete mixture is then passedthru a colloid mill to give a homogeneous,'stablc emulsion. v I

Clothing and fabric may be impregnated .in the emul- 81011831. ordinary temperatures in the usual manner. Since certain changes and modifications may be made 1n the. foregoing compositionsand techniques .of applicatron without departing from the scope of this invention, it is intended that all matter contained in the abovedcscrlption shall be interpreted as illustrative and not in a limited sense.

What is-claimed as newis: V -1. A fabric impregnating composition for rendering fabric and clothing resistantto mustard gas, lewisite, and like: vesicants susceptible of being rendered non-vesicant by chlorination, which'compn'ses, bis 2,4,6-trichlorphenyl chlorurea' for rendering mustard gas, lewisite, and like vesicants relatively harmless, a binder'comprising a mixture of chlorinated paraffin and chlorinated naphthalene, a solvent comprising a mixture of monochlorbenzene' and beta trichl'orethane, and a small amount of ethyl cellulose as a suspending agent for maintaining a relatively stable suspension'of bis 2,4,6-trichlorphenyl chlorurea in the solvent. V V

2. A fabric impregnating composition for rendering fabric and clothing resistant to mustard gas, lewisite', and

like vesicants susceptible of being'rendered non-vesicant' by chlorination, which c0mprises,.from about5'.0% .to

8.0% r by weight of bis"2,4,6-trichlorphenyl2 chlorure'a for rendering mustard gas, lewisite, and like vesicants relacomposition may havethe fol- V about 1.5% to 2.5% by weight of chlorinated naphthalene and from about 3.0% to 4.0% by weight of chlorinated parafiin, a solvent comprising a mixture of from about 50.0% to 60.0% by weight of monochlorbenzene and from about 30.0% to 34.0% by weight of beta-trichlorethane, and about 0.3% by weight or greater of ethyl cellulose as a suspending agent for maintaining a relatively stable suspension of his 2,4,6-trichlorphenyl chlorurea in the solvent.

3. A fabric impregnating composition for simultaneously coloring and rendering fabric and clothing resistant to mustard gas, lewisite, and like vesicants susceptible of being rendered non-vesicant by chlorination, which comprises, bis 2,4,6-trichlorphenyl chlorurea for rendering mustard gas, lewisite, and like vesicants relatively harmless, a binder comprising a mixture of chlorinated parafiin and chlorinated naphthalene, flushed pigment for coloring said fabric or clothing, a solvent comprising a mixture of monochlorbenzene and beta-trichlorethane, and a small amount of ethyl cellulose as a suspending agent for maintaining a relatively stable suspension of bis 2,4,6-trichlorphenyl chlorurea in the solvent.

4. A fabric impregnating composition for simultaneously coloring and rendering fabric and clothing resistant to mustard gas, lewisite, and like vesicants susceptible of being rendered non-vesicant by chlorination, which comprises, from about 4.7% to 7.5% by weight of bis 2,4,6-trichlorphenyl chlorurea for rendering mustard gas, lewisite, and like vesicants relatively harmless, a binder comprising a mixture of from about 1.4% to 2.4% by weight of chlorinated naphthalene and from about 2.8% to 3.8% by weight of chlorinated paraffin, about 6% by weight of a flushed pigment for coloring said fabric or clothing, a solvent comprising a mixture of from about 47.0% to 56.4% of monochlorbenzene and from about 28.2% to 32.0% by weight of beta-trichlorethane, and about 0.28% by weight or greater of ethyl cellulose as a suspending agent for maintaining a relatively stable suspension of his 2,4,6-trichlorphenyl chlorurea in the said solvent.

5. A fabric impregnating composition for rendering fabric and clothing resistant to mustard gas, lewisite, and like vesicants susceptible of being rendered non-vesicant by chlorination, and which is in the form of an oil-inwater emulsion having an oil phase comprising bis 2,4,6-

like vesicants susceptible of being rendered non-vesicant by chlorination, and which is in the form of an oil-in- Water emulsion having an oil phase comprising about 7% by weight of the composition of his 2,4,6-tn'chlorphenyl chlorurea for rendering mustard gas, lewisite, and like vesicants relatively harmless, a binder comprising about 5% by weight of the composition of chlorinated parafiin, and a solvent comprising a mixture of about 15% by weight of the composition of monochlorbenzene and about 10% by weight of the composition of perchlorethylene, having a water phase comprising about by weight of the composition, and having an emulsifying agent to stabilize the emulsion comprising about 3% by weight of the composition.

References Cited in the file of this patent UNITED STATES PATENTS 1,085,783 Aylsworth Feb. 3, 1914 1,907,521 Dreyfus May 9, 1933 1,950,957 Wilhelm Mar. 13, 1934 1,958,370 Schmelkes July 8, 1934 2,073,256 Schmelkes Mar. 9, 1937 2,136,173 Steingroever Nov. 8, 1938 2,275,593 Muskat Mar. 10, 1942 2,299,612 Clayton Oct. 20, 1942 FOREIGN PATENTS 588,131 Germany July 3, 1929 590,818 Germany Jan. 11, 1934 486,162 Great Britain May 31, 1938 496,734 Great Britain Dec. 5, 1938 OTHER REFERENCES Hoogeveen: Gas Clothing, Chemisch Weekblad (1936), vol. 33, pages 474, 475, in Dutch, translation in Div. 3.

Claims

1. A FABRIC IMPREGNATING COMPOSITION FOR RENDERING FABRIC AND CLOTHING RESISTANT TO MUSTARD GAS, LEWISITE, AND LIKE VESICANTS SUSCEPTIBLE OF BEING RENDERED NON-VESICANT BY CHLORINATION, WHICH COMPRISES, BIS 2,4,6-TRICHLORPHENYL CHLORUEA FOR RENDERING MUSTARD GAS, LEWISTE, AND LIKE VESICANTS RELATIVELY HARMLESS, A BINDER COMPRISING A MIXTURE OF CHLORINATED PARAFFIN AND CHLORINATED NAPHTALENE, A SOLVENT COMPRISING A MIXTURE OF MONOCHLORBENZENE AND BETA-TRICHLORETHANE, AND A SMALL AMOUNT OF ETHYL CELLOUSE AS A SUSPENDING AGENT FOR MAINTAINING A RELATIVELY STABLE SUSPENSION OF BIS 2,4,6-TRICHLORPHENYL CHLORUREA IN THE SOLVENT.