US3276926A - Composite polysulfide propellants containing additives for producing extremely fast burning - Google Patents

Composite polysulfide propellants containing additives for producing extremely fast burning Download PDF

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US3276926A
US3276926A US330365A US33036553A US3276926A US 3276926 A US3276926 A US 3276926A US 330365 A US330365 A US 330365A US 33036553 A US33036553 A US 33036553A US 3276926 A US3276926 A US 3276926A
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perchlorate
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    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B43/00—Compositions characterised by explosive or thermic constituents not provided for in groups C06B25/00 - C06B41/00
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
    • C06B45/04—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive
    • C06B45/06—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component
    • C06B45/10—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component the organic component containing a resin

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  • This invention relates to fast burning solid propellants and the method for making them; more particularly it relates to propellants to which a certain type additive has been added to increase their burning rate.
  • propellants make it necessary to modify the propellant to increase the burning rate. Typical applications are those within a great thrust must be produced in a short time, such as apelooka rockets and other missiles which reach their target shortly after release.
  • Another application of fast burning propellants is their use to increase power output in motors o erating at low chamber pressures.
  • the above perchlorate additives may be prepared by two general methods.
  • One method comprises treating the free amine in a suitable solvent with one equivalent of 70% perchlorate acid, followed by removal of Water and solvent by distillation at reduced pressure and recrystallization of the salt so obtained in a suitable solvent.
  • Another method includes treating the hydrochloride or sulfate salt of the desired amine in absolute ethanol with an alcoholic solution of barium perchlorate, followed by removal of the insoluable barium salt by filtration, concentration of the filtrate at reduced pressure and recrystallization of the salt so obtained in a suitable solvent.
  • the additives are incorporated in the fluid propellant at room temperature, and after thorough mixing this mixture is cast into suitable containers and then conditioned at the appropriate temperature to effect curing of the propellant (i.e. set to a solid).
  • the additives may also be incorporated in double base propellants of either solvent or solvent'less type, prior to rolling and extrusion of the gram.
  • the mechanism of the burning rate increase produced by the additive is believed to be due to a cratering effect on the burning propellant surface caused by the violent decomposition of the additive at relatively low temperatures in the solid phase of the propellant. This effect is achieved by using coarse particles of additive in amounts of 5 to 60% of the total propellant weight.
  • this method of increasing burning rates is not limited to any one type of solid propellant and may be induced by any additive having physical and chemical properties making it susceptible to the catering effect.
  • the propellant composition was prepared by thoroughly mixing 30.0 grams of Thiokol LP-3, 65.0 grams of potassium perchlorate (ground and sieved such that passed a l00-mesh but not a 325-mesh screen, and 30% passed a 325-mesh screen), 2.0 grams of p-quinone dioxime, 1.0 gram of diphenyl guanidine, and 5.0 grams of hydroxylamine perchlorate of 100-200 mesh size.
  • the above ingredient were mixed in the order given, at room temperature. After casting the mix in drinking straws by means of a suitable pressure casting device, the strands were conditioned 18 hours at C.
  • Strands prepared in the above manner were found to burn very rapidly at 1000 p.s.i. whereas strands of the same formulation from which the hydroxylamine perchlorate additive was omitted were found to have a burning rate at 1000 p.s.i. of only 1.06 inches per second.
  • Hydrazine perchlorate was prepared by reacting hydrazine hydrochloride with barium perchlorate.
  • the propellant compositions was prepared by thoroughly mixing 30 grams of Paraplex P-lO, 50 grams of -200 mesh hydrazine perchlorate and 40 grams of potassium perchlorate. Strands of this propellant were found to burn at 2.31 inches per second at 1000 p.s.i., whereas the same size strands of a similar formulation at which the hydrazine perchlorate was entirely replaced by an equal weight of potassium perchlorate burned at only 1.27 inches per second at 1000 p.s.i.
  • a propellant composition was prepared by thoroughly mixing 30 grams of Paraplex P-10, 35 grams of 100-200 e) mesh hydrazine perchlorate and 35 grams of ammonium perchlorate. Strands of this propellant were found to burn at 1.45 inches per second, whereas the same size strands of similar formulation in which the hydrazine perchlorate was entirely replaced by an equal weight of ammonium perchlorate burned at only 0.28 inch per second at 1000 p.s.i.
  • EXAMPLE IV Semicarbazide perchlorate was prepared by mixing, with stirring, solution A containing 44.6 grams of semicarbazide hydrochloride in 400 'cc. of water and solution B containing 82.8 grams of silver perchlorate in 200 grams of water. The resulting solution was filtered to remove silver chloride and the filtrate concentrated under vacuum to yield a damp crystalline solid. This was dissolved in the minimum amount of hot methanol and recrystallized by adding six volumes of ethylene chloride. Filtration and vacuum drying yielded the desired product. The propellent mixture was prepared by thoroughly mixing 30 grams of Paraplex P-lO, 15 grams of 4080 mesh semicarbazide perchlorate and 55 grams of ammonium perchlorate.
  • the presence of the additives of this invention in a propellant increases the burning rate from two to eight fold that of the propellant alone.
  • Other additives which may be used are the N-alkyl substituted hydroxylamine perchlorates, the N-alkyl substituted hydrazine perch'lorates and N-alkyl substituted semicarbazide perchlorates.
  • any other temperature sensitive high explosive such as lead azide, lead styphnate, heavy metal picrates or cobalt-azideerchlorate complexes may be used to produce the burning rate increase effect.
  • the additives were incorporated in the propellants in amounts of to 60% by weight that of the total weight of the propellant, however, varying amounts of additive may be used depending upon the propellant being used and the burning rate required.
  • the propellant used in illustrating the invention were a Thiokol LP-3 type propellant and a Paraplex P- propellant
  • the additives may be used to increase the burning rate of other propellants, as the increase in burning rate is due to the thermal decomposition characteristics of the additives, namely, the rapid decomposition or explosion of large particles of additive at relatively low temperatures. Mixtures of the various additives of the invention may be used rather than a single additive.
  • the Thiokol LP-3 and Paraplex P-10, referred to in the above examples, are well known elastomers.
  • Thiokol LP-3 is a liquid polysulfide polymer having a low molecular Weight.
  • Unconverted Thiokol LP-S is essentially a difunctional mercaptan made from 98 mole percent of bis(2-chloroethyl) formal and 2 mole percent of trichloropropane, a crosslinking agent.
  • the polymer segments are composed of a number of formal groups linked by sulfur bonds and are terminated by mercaptan groups; side mercaptan groups occur occasionally in the chain of repeating formal units and some chain segments are crosslinked at various points.
  • the average structure of Thiokol LP-3 may be represented as follows:
  • Paraplex P10 is a styrene solution of unsaturated polyester or alkyd resins consisting of 50% by weight of styrene and 50% by weight of polyester. It is a reactive, thermosetting resin which, under the influence of heat and peroxides, will polymerize to an inert, insoluble, infusible product.
  • Paraplex P-lO contains no water and pre-drying operations are not necessary. It is percent reactive and cures by polymerization (or copolymerization) rather than by condensation as in the case of phenolics, and, as a result, no volatile byproducts are split out during the reaction.
  • Paraplex Pl0 is an extremely flexible composition.
  • Paraplex P-10 is reactive. Even at room temperature, it will gel eventually and, given infinite time, could polymerize to its ultimate thermoset form. However, there are several ways of accelerating this reaction. First, direct or infra-red heat, or ultra-violet radiation can be used to accelerate the rate of action. Secondly, peroxide catalysts can be used, just as they are used in conventional vinyl monomer polymerizations- Benzoyl peroxide (in the form of Luperco ATC, a benzoyl peroxide supplied in paste form with an equal weight of tricresyle phosphate) tertiary butyl perbenzoate, and others, used in concentrations of 1 to 2 percent on the weight of the Paraplex, have been found suitable.
  • Benzoyl peroxide in the form of Luperco ATC, a benzoyl peroxide supplied in paste form with an equal weight of tricresyle phosphate
  • tertiary butyl perbenzoate and others, used in concentrations
  • the curing is generally accepted as a true copolymerization, and the final product is a homogeneous composition anda three dimensional polymer.
  • the resin first tends to thin as it reaches curing temperature, then gels to a very weak, soft mass and; on subsequent heating, cures to a firm composition, showing an appreciable volume reduction and a corresponding increase in specific gravity during cure.
  • Odor Styrene Spec. gravity .982.984. Refractive index 1.5115.
  • a propellent composition consisting of about 65 parts by weight of potassium perchlorate, about 2 parts by 5 6 Weight of p-quinone dioxime, about 1 part by weight of FOREIGN PATENTS diphenyl guanidine, about 5 parts by Weight of hydroxyl- 523,732 4/1921 France amine perchlorate and about 30 parts by Weight of a polysulfide polymer having the average structure OTHER REFERENCES 5 Audrieth: The Chemistry of Hydrazine, John Wiley &

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

Unite States Patent ()fiice Patented Oct. 4, 1966 3,276,926 COMPOSITE POLYSULFIDE PROPELILANTS CON- TAINING ADDITIVES FOR PRODUCING EX- TREMELY FAST BURNING John H. Robson III, 206A Lauritsen. China Lake, Calif. No Drawing. Filed Jan. 8, 1953, Ser. No. 330,365 1 Claim. (Cl. 14919) The invention described herein may be manufactured and used by or for the Government of the United States of America for governmental purposes without the payment of any royalties thereon or therefor.
This invention relates to fast burning solid propellants and the method for making them; more particularly it relates to propellants to which a certain type additive has been added to increase their burning rate.
Various applications of propellants make it necessary to modify the propellant to increase the burning rate. Typical applications are those within a great thrust must be produced in a short time, such as bazooka rockets and other missiles which reach their target shortly after release. Another application of fast burning propellants is their use to increase power output in motors o erating at low chamber pressures.
Various expedients have been used in the past to increase the burning rate of propellants. One such expedient is the use of hollow core grains to obtain larger burning surfaces. This method has the disadvantage that it necessitates an increase in the ratio of motor size to weight. Various additives have been used in the past but have been unsatisfactory for various reasons.
It is therefore an object of this invention to provide propellants which have fast burning rates.
It is another object of this invention to provide additives for producing propellants with fast burning rates which do not seriously detract from other necessary properties of the propellant.
It is still another object of this invention to provide a method for producing fast burning propellants which is relatively inexpensive and simple in application.
It has been found that the above and other objects can be accomplished and the enumerated difiiculties overcome by the addition to propellants of temperature sensitive high explosives, that is, high explosives subject to detonation or explosion within a temperature range of about 100 C. to about 400 C. The range of the particle size of the additive is critical and is from about 20 to about 300 mesh. Examples of these additives are percholo'rate salts for example, the compounds hydroxylamine percholorate, hydrazine mono-perchlorate and semicarbazide perchlorate. Other examples of additives are lead azide, lead styphnate, heavy metal picrates and cobalt-azide-perchlorate complexes.
The above perchlorate additives may be prepared by two general methods. One method comprises treating the free amine in a suitable solvent with one equivalent of 70% perchlorate acid, followed by removal of Water and solvent by distillation at reduced pressure and recrystallization of the salt so obtained in a suitable solvent. Another method includes treating the hydrochloride or sulfate salt of the desired amine in absolute ethanol with an alcoholic solution of barium perchlorate, followed by removal of the insoluable barium salt by filtration, concentration of the filtrate at reduced pressure and recrystallization of the salt so obtained in a suitable solvent.
The additives are incorporated in the fluid propellant at room temperature, and after thorough mixing this mixture is cast into suitable containers and then conditioned at the appropriate temperature to effect curing of the propellant (i.e. set to a solid). The additives may also be incorporated in double base propellants of either solvent or solvent'less type, prior to rolling and extrusion of the gram.
The mechanism of the burning rate increase produced by the additive is believed to be due to a cratering effect on the burning propellant surface caused by the violent decomposition of the additive at relatively low temperatures in the solid phase of the propellant. This effect is achieved by using coarse particles of additive in amounts of 5 to 60% of the total propellant weight. Thus this method of increasing burning rates is not limited to any one type of solid propellant and may be induced by any additive having physical and chemical properties making it susceptible to the catering effect.
The invention is illustrated by the following examples but is not limited thereby:
EXAMPLE I In the following example the hydroxylamine perchlorate used was made by reacting hydroxylamine hydrochloride with barium perchlorate in absolute ethanol and recovering the product by crystallization.
The propellant composition was prepared by thoroughly mixing 30.0 grams of Thiokol LP-3, 65.0 grams of potassium perchlorate (ground and sieved such that passed a l00-mesh but not a 325-mesh screen, and 30% passed a 325-mesh screen), 2.0 grams of p-quinone dioxime, 1.0 gram of diphenyl guanidine, and 5.0 grams of hydroxylamine perchlorate of 100-200 mesh size. The above ingredient were mixed in the order given, at room temperature. After casting the mix in drinking straws by means of a suitable pressure casting device, the strands were conditioned 18 hours at C.
Strands prepared in the above manner were found to burn very rapidly at 1000 p.s.i. whereas strands of the same formulation from which the hydroxylamine perchlorate additive was omitted were found to have a burning rate at 1000 p.s.i. of only 1.06 inches per second.
EXAMPLE II Hydrazine perchlorate was prepared by reacting hydrazine hydrochloride with barium perchlorate. The propellant compositions was prepared by thoroughly mixing 30 grams of Paraplex P-lO, 50 grams of -200 mesh hydrazine perchlorate and 40 grams of potassium perchlorate. Strands of this propellant were found to burn at 2.31 inches per second at 1000 p.s.i., whereas the same size strands of a similar formulation at which the hydrazine perchlorate was entirely replaced by an equal weight of potassium perchlorate burned at only 1.27 inches per second at 1000 p.s.i.
EXAMPLE III A propellant composition was prepared by thoroughly mixing 30 grams of Paraplex P-10, 35 grams of 100-200 e) mesh hydrazine perchlorate and 35 grams of ammonium perchlorate. Strands of this propellant were found to burn at 1.45 inches per second, whereas the same size strands of similar formulation in which the hydrazine perchlorate was entirely replaced by an equal weight of ammonium perchlorate burned at only 0.28 inch per second at 1000 p.s.i.
EXAMPLE IV Semicarbazide perchlorate was prepared by mixing, with stirring, solution A containing 44.6 grams of semicarbazide hydrochloride in 400 'cc. of water and solution B containing 82.8 grams of silver perchlorate in 200 grams of water. The resulting solution was filtered to remove silver chloride and the filtrate concentrated under vacuum to yield a damp crystalline solid. This was dissolved in the minimum amount of hot methanol and recrystallized by adding six volumes of ethylene chloride. Filtration and vacuum drying yielded the desired product. The propellent mixture was prepared by thoroughly mixing 30 grams of Paraplex P-lO, 15 grams of 4080 mesh semicarbazide perchlorate and 55 grams of ammonium perchlorate. Strands of this propellant were found to burn at 0.35 inch per second at 1800 p.s.i., whereas the same size strands of a similar formulation in which the semicarbazide perchlorate was entirely replaced by an equal weight of ammonium perchlorate burned at 0.32 inch per second at 1800 p.s.i. The Sigmoid rate-pressure curve showed conclusively that the semi-carbazide perchlorate had a rate-increasing effect similar to that of hydrazine perchlorate.
As the above results shown, the presence of the additives of this invention in a propellant increases the burning rate from two to eight fold that of the propellant alone. Other additives which may be used are the N-alkyl substituted hydroxylamine perchlorates, the N-alkyl substituted hydrazine perch'lorates and N-alkyl substituted semicarbazide perchlorates. In double base type propellants where it is not necessary to maintain a high oxygen balance, any other temperature sensitive high explosive such as lead azide, lead styphnate, heavy metal picrates or cobalt-azideerchlorate complexes may be used to produce the burning rate increase effect.
In the illustrative examples the additives were incorporated in the propellants in amounts of to 60% by weight that of the total weight of the propellant, however, varying amounts of additive may be used depending upon the propellant being used and the burning rate required. Although the propellant used in illustrating the invention were a Thiokol LP-3 type propellant and a Paraplex P- propellant, the additives may be used to increase the burning rate of other propellants, as the increase in burning rate is due to the thermal decomposition characteristics of the additives, namely, the rapid decomposition or explosion of large particles of additive at relatively low temperatures. Mixtures of the various additives of the invention may be used rather than a single additive.
The Thiokol LP-3 and Paraplex P-10, referred to in the above examples, are well known elastomers.
A bulletin published November 21, 1952 by the Thiokol Corporation and entitled Thiokol Liquid Polymer LP-3, disloses that Thiokol LP-3 is a liquid polysulfide polymer having a low molecular Weight.
Unconverted Thiokol LP-S is essentially a difunctional mercaptan made from 98 mole percent of bis(2-chloroethyl) formal and 2 mole percent of trichloropropane, a crosslinking agent. The polymer segments are composed of a number of formal groups linked by sulfur bonds and are terminated by mercaptan groups; side mercaptan groups occur occasionally in the chain of repeating formal units and some chain segments are crosslinked at various points. The average structure of Thiokol LP-3 may be represented as follows:
The following are a number of the more important typical physical properties of the unconverted liquid polymer:
Physical state Mobile liquid. Color Clear, amber. Specific gravity 20/ 20 C 1.27 Viscosity 25 C., centipoises 700-1200. Average molecular weight 1000 Pour point 15 F. Flash point (open cup) 418 F.
Fire point (open cup) 465 F.
pH (water extract) 6.0-8.0 Moisture content 0.1% max. Stability Unlimited (over 3 years).
A booklet published August 8, 1947 by Resinous Products and Chemical Company of Philadelphia, Pennsylvania, and entitled Paraplex for Laminating and Casting Applications, discloses that Paraplex P10 is a styrene solution of unsaturated polyester or alkyd resins consisting of 50% by weight of styrene and 50% by weight of polyester. It is a reactive, thermosetting resin which, under the influence of heat and peroxides, will polymerize to an inert, insoluble, infusible product. Paraplex P-lO contains no water and pre-drying operations are not necessary. It is percent reactive and cures by polymerization (or copolymerization) rather than by condensation as in the case of phenolics, and, as a result, no volatile byproducts are split out during the reaction. In its final form, Paraplex Pl0 is an extremely flexible composition.
As stated above, Paraplex P-10 is reactive. Even at room temperature, it will gel eventually and, given infinite time, could polymerize to its ultimate thermoset form. However, there are several ways of accelerating this reaction. First, direct or infra-red heat, or ultra-violet radiation can be used to accelerate the rate of action. Secondly, peroxide catalysts can be used, just as they are used in conventional vinyl monomer polymerizations- Benzoyl peroxide (in the form of Luperco ATC, a benzoyl peroxide supplied in paste form with an equal weight of tricresyle phosphate) tertiary butyl perbenzoate, and others, used in concentrations of 1 to 2 percent on the weight of the Paraplex, have been found suitable. Actually, a combination of heat and peroxide generally is used in practice. The curing is generally accepted as a true copolymerization, and the final product is a homogeneous composition anda three dimensional polymer. In curing, the resin first tends to thin as it reaches curing temperature, then gels to a very weak, soft mass and; on subsequent heating, cures to a firm composition, showing an appreciable volume reduction and a corresponding increase in specific gravity during cure.
The physical properties of unpolymerized Paraplex P-10 are as follows:
Viscosity (cps.) 350550. Color Amber. Appearance Clear. Acid number Less than 2.
Odor Styrene. Spec. gravity .982.984. Refractive index 1.5115.
Obviously many modifications and variations of the present invention are possible in the light of the above teachings. It is therefore to be understood that within the scope of the appended claim the invention may be practiced otherwise than as specifically described.
What is claimed is:
A propellent composition consisting of about 65 parts by weight of potassium perchlorate, about 2 parts by 5 6 Weight of p-quinone dioxime, about 1 part by weight of FOREIGN PATENTS diphenyl guanidine, about 5 parts by Weight of hydroxyl- 523,732 4/1921 France amine perchlorate and about 30 parts by Weight of a polysulfide polymer having the average structure OTHER REFERENCES 5 Audrieth: The Chemistry of Hydrazine, John Wiley &
HS (CZHQOCHZ"OC2H4'S' S)6 Sons, New York City 1951 pages 177, 189.
2 4 2 2 4 McLarren: Automotive and Aviation Industries,
August 15, 194-6, pages 20-23, inclusive, and 76. References Cited by the Examiner UNITED STATES PATENTS 1Q BENJAMIN R. PADGETT, Aclirzg Primary Examiner. 2,406,572 8/1946 VOg1 WILLIAM G. WILES, ROBERT L. CAMPBELL, 2,479,470 8/1949 Carr 52.5 Emmmm' 2,479,828 8/ 1949 Geckler. LEON D. ROSDOL, Assistant Examiner.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR523732A (en) * 1921-08-18 1921-08-24 Christen Johannes Stautsboell Explosives upgrades
US2406572A (en) * 1941-06-13 1946-08-27 Ralph E Svoboda Explosive perchlorates of aliphatic nitrogenous compounds
US2479470A (en) * 1944-03-13 1949-08-16 Union Oil Co Asphaltic jet propulsion fuel
US2479828A (en) * 1947-11-20 1949-08-23 Aerojet Engineering Corp Propellant charge for rocket motors

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR523732A (en) * 1921-08-18 1921-08-24 Christen Johannes Stautsboell Explosives upgrades
US2406572A (en) * 1941-06-13 1946-08-27 Ralph E Svoboda Explosive perchlorates of aliphatic nitrogenous compounds
US2479470A (en) * 1944-03-13 1949-08-16 Union Oil Co Asphaltic jet propulsion fuel
US2479828A (en) * 1947-11-20 1949-08-23 Aerojet Engineering Corp Propellant charge for rocket motors

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