Halogen Containing Patents (Class 423/300)
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Patent number: 4327063Abstract: Cyclic dichlorophosphazenes containing trace amounts of protic impurities such as water are purified by treatment with boron trihalides under specified temperature and pressure conditions. The catalytic polymerization of the resultant cyclic dichlorophosphazenes, which are substantially free of protic impurities, is greatly improved.Type: GrantFiled: August 25, 1980Date of Patent: April 27, 1982Assignee: The Firestone Tire & Rubber CompanyInventors: John W. Fieldhouse, Daniel F. Graves
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Patent number: 4327064Abstract: Substantially linear polydichlorophosphazene polymers having a degree of polymerization of from 20 to 50,000 are prepared by an improved solution polymerization process which involves the polymerization of substantially pure cyclic dichlorophosphazene oligomers represented by the formula (NPC1.sub.2).sub.n, in which n is from 3 to 7, in cycloaliphatic solvents in the presence of a boron trihalide catalyst or a complex of a boron trihalide with an oxygenated phosphorus compound.The process provides for the production of substantially gel free linear polydichlorophosphazene polymer, improved polymerization rates and easier handling of the polymerizate for subsequent derivatization reactions.Type: GrantFiled: August 4, 1980Date of Patent: April 27, 1982Assignee: The Firestone Tire & Rubber CompanyInventors: John W. Fieldhouse, Steven L. Fenske
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Patent number: 4319894Abstract: A process is provided for separating gaseous phosphorus trichloride from a gas stream. The process comprises contacting the gas stream with a condensing amount of liquid phosphorus trichloride to c ondense a portion of the gaseous phosphorus trichloride to liquid phosphorus trichloride. The liquid phsphorus trichloride is then separated from the gas stream. A process apparatus is also provided. The process is particularly useful in preventing or reducing the discharge of gaseous phosphorus trichloride to the atmosphere due to the accidental discharge of a high volume gas stream from a phosphorus trichloride reaction vessel.Type: GrantFiled: October 16, 1978Date of Patent: March 16, 1982Assignee: Stauffer Chemical CompanyInventors: Alan L. Kempner, Robert H. Kaplan
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Patent number: 4287165Abstract: High purity phosphorus and phosphorus compounds are prepared by first reacting H.sub.3 PO.sub.4 with a lead compound such as PbO to form Pb.sub.3 (PO.sub.4).sub.2. The Pb.sub.3 (PO.sub.4).sub.2 is reduced with H.sub.2 at a temperature sufficient to form gaseous phosphorus which can be recovered as a high purity phosphorus product. Phosphorus compounds can be easily prepared by reacting the phosphorus product with gaseous reactants. For example, the phosphorus product is reacted with gaseous Cl.sub.2 to form PCl.sub.5. PCl.sub.5 is reduced to PCl.sub.3 by contacting it in the gaseous phase with solid elemental phosphorus. POCl.sub.3 can be prepared by contacting PCl.sub.5 in the gaseous phase with solid P.sub.2 O.sub.5. The general process is particularly suitable for the preparation of radiophosphorus compounds.Type: GrantFiled: April 4, 1980Date of Patent: September 1, 1981Assignee: The United States of America as represented by the United States Department of EnergyInventors: Arthur F. Rupp, David V. Woo
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Patent number: 4279723Abstract: An ionized gas plasma is established in an electrical field in contact with a non-vapor volume monomer (liquid and/or solid). The plasma causes polymerization of the monomers which are of the phosphazene or carborane type.Type: GrantFiled: May 31, 1979Date of Patent: July 21, 1981Assignee: The Regents of the University of CaliforniaInventors: Yoshihito Osada, Alexis T. Bell, Mitchel M. Shen
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Patent number: 4276343Abstract: The invention provides active polymeric phosphorus nitrides containing hydroxyl and halogen. The halogen atoms and hydroxyl groups are linked to phosphorus, and the nitrides contain about 35 to 54 weight % of phosphorus, about 35 to 47 weight % of nitrogen, about 1 to 20 weight % of oxygen and about 0.1 to 8 weight % of chlorine.Type: GrantFiled: March 10, 1980Date of Patent: June 30, 1981Assignee: Hoechst AktiengesellschaftInventors: Joseph Cremer, Heink Harnisch
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Patent number: 4272382Abstract: A process for separating cyclic phosphazene oligomers from a mixture containing cyclic phosphazene oligomers and linear phosphazenes by bringing the mixture into contact with a mineral adsorbent composed of mainly silicon and/or aluminum and removing the adsorbent. Cyclic phosphazene oligomers of high purity can be readily separated in high yields by the process.Type: GrantFiled: November 27, 1979Date of Patent: June 9, 1981Assignee: Otsuka Chemical Co. Ltd.Inventors: Yuzuru Ogata, Yoshifumi Nakacho
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Patent number: 4265854Abstract: A process inhibiting the coalescence of flowable phosphorus pentachloride in a closed container. To this end, the invention provides for a readily volatizable organic liquid boiling within the range about 20.degree. to 200.degree. C. and being inert with respect to phosphorus pentachloride to be admitted to the container prior to, during or after the introduction of phosphorus pentachloride thereinto, and for the container to be then hermetically sealed, the liquid being used in a proportion of about 1 to 15 weight %, based on the quantity of phosphorus pentachloride.Type: GrantFiled: October 22, 1979Date of Patent: May 5, 1981Assignee: Hoechst AktiengesellschaftInventors: Joachim Wortmann, Gerhard Rieb, Franz-Josef Dany, Joachim Kandler
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Patent number: 4265865Abstract: Phosphorus pentachloride is manufactured from chlorine and phosphorus trichloride in the presence of molten phosphorus pentachloride. The process can be carried out such that the reaction product flows out from the reactor continuously as a melt. Reaction pressures of more than 1 bar and temperatures of from 160.degree. to 250.degree. C. are preferred.Type: GrantFiled: July 11, 1980Date of Patent: May 5, 1981Assignee: Hoechst AktiengesellschaftInventors: Gerhard Munster, Gerhard Riess, Jurgen Russow
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Patent number: 4259305Abstract: A method for the separation of phosphonitrilic chloride trimer from mixtures containing other higher cyclic and linear phosphonitrilic chlorides involves contacting the crude phosphazene mixture with a ketone and preferably in the presence of a solvent and water so that a separable liquid fraction whose phosphazene constituent consists essentially of cyclic phosphonitrilic chloride is formed. The fraction is then separated and the trimer easily isolated by known methods in the art.Type: GrantFiled: December 31, 1979Date of Patent: March 31, 1981Assignee: Ethyl CorporationInventor: Larry W. Anderson
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Patent number: 4257917Abstract: High molecular weight poly(dihalophosphazenes) which exhibit solubility in benzene and in substituted benzenes are prepared in solution or in bulk from dihalophosphazenes such as (Cl.sub.2 PN).sub.3-7 at moderate temperatures by the use of novel polymerization catalysts.Type: GrantFiled: November 7, 1978Date of Patent: March 24, 1981Assignee: The Firestone Tire & Rubber CompanyInventors: Kennard A. Reynard, Arthur H. Gerber
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Patent number: 4256715Abstract: An improved process for preparing tri- and tetraphosphonitrilic chlorides in a shortened period of time in high yields by reacting ammonium chloride with phosphorus pentachloride produced simultaneously with the progress of the reaction from phosphorus trichloride and chlorine, in an organic solvent inert to chlorine in the presence of a catalyst, while adding dropwise phosphorus trichloride and supplying chlorine gas to the reaction system.Type: GrantFiled: November 29, 1978Date of Patent: March 17, 1981Assignee: Otsuka Chemical Co., Ltd.Inventors: Tsukuru Kinoshita, Yuzuru Ogata, Masayoshi Suzue
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Patent number: 4248845Abstract: A process for preparing tri- and tetra-phosphonitrilic chlorides in a shortened period of time in high yields by reacting ammonium chloride with phosphorus pentachloride in an organic solvent inert to chlorine in the presence of at least one catalyst selected from metal oxides of Groups II-A, II-B, III-A, IV-A, IV-B and VIII of the Periodic Table, metal sulfides, metal salts of fatty acids, metal complexes, organometallic compounds and metal peroxides of Groups II-A and II-B of the Periodic Table, metal hydroxides of Groups III-A and VIII of the Periodic Table, and magnesium hydroxide.Type: GrantFiled: November 29, 1978Date of Patent: February 3, 1981Assignee: Otsuka Chemical Co., Ltd.Inventors: Tsukuru Kinoshita, Yuzuru Ogata, Masayoshi Suzue
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Patent number: 4242316Abstract: Polymerization process for the solution or bulk polymerization of chlorocyclophosphazenes using sulfamic acid compounds or derivatives of sulfamic acid as catalyst. Poly(aryloxyphosphazene) resulting therefrom can be controlled as to molecular weight, and molecular weight distribution.Type: GrantFiled: June 29, 1979Date of Patent: December 30, 1980Assignee: Standard Oil Company (Indiana)Inventor: David P. Sinclair
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Patent number: 4241034Abstract: A process for improving the purity of phosphonitrilic chloride polymers, namely the trimer and tetramer by (1) contacting a solution of open-chain phosphonitrilic chloride oligomers admixed with cyclic oligomers of phosphonitrilic chloride in a normally liquid hydrocarbon with aqueous lower alkylnitrile, (2) separating the liquid hydrocarbon phase laden with trimer and some tetramer from the aqueous phase thereby produced, and (3) recovering highly purified cyclic trimer and tetramer from the hydrocarbon phase.Type: GrantFiled: May 31, 1979Date of Patent: December 23, 1980Assignee: Ethyl CorporationInventor: Charles H. Kolich
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Patent number: 4226840Abstract: Linear polydihalophosphazene polymers which are substantially free of gel are prepared by thermally polymerizing a cyclic polyhalophosphazene represented by the formula (NPX.sub.2).sub.3, wherein X is fluorine, chlorine or bromine in the presence of a catalyst which comprises the reaction product of a boron trihalide compound with an oxygenated phosphorus compound.In addition to producing substantially gel free polymers, the catalyst composition of the process of the invention permits improved control of molecular weight, lower polymerization temperature, high rates of conversion of (NPCl.sub.2).sub.3 to (NPCl.sub.2).sub.n and provides for more readily processible and derivatizable polymers.Type: GrantFiled: September 19, 1979Date of Patent: October 7, 1980Assignee: The Firestone Tire & Rubber CompanyInventors: John W. Fieldhouse, Daniel F. Graves
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Patent number: 4225567Abstract: Solution polymerization of cyclic dichlorophosphazenes represented by the general formula (NPCl.sub.2).sub.n in which "n" is less than 15 to essentially linear polydichlorophosphazenes in which the degree of polymerization is within the range of 20 to 50,000 is improved by the use of selected solvents and by the presence of elemental sulfur or sulfur donating compounds in the polymerization mixture.Type: GrantFiled: November 5, 1976Date of Patent: September 30, 1980Assignee: The Firestone Tire & Rubber CompanyInventors: Adel F. Halasa, James E. Hall
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Patent number: 4198381Abstract: In the first step of a two step process, PCl.sub.3 and Cl.sub.2 are reacted in a suitable medium. In the second step, PCl.sub.3, Cl.sub.2 and NH.sub.3 are concurrently fed into said medium while keeping the temperature at 100.degree. C. to 140.degree. C. The feeds of the reactants are controlled so that until the first 1/2 of the NH.sub.3 has been reacted the molar ratio of PCl.sub.3 :NH.sub.3 (including the PCl.sub.3 of the first step) is kept above 2. Thereafter, the feeds are adjusted so that with respect to the total amount of ammonia, said molar ratio is between 1.2 and 1.5. Linear phosphonitrilic chloride oligomers having a number average degree of polymerization from 2 to 9 are produced in high yield.Type: GrantFiled: August 21, 1978Date of Patent: April 15, 1980Assignee: Ethyl CorporationInventors: Edwin D. Hornbaker, Hsueh M. Li
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Patent number: 4196179Abstract: Preparation of high cyclic phosphonitrilic halide, preferably chloride, oligomer mixtures by reaction of phosphorus trichloride, chlorine and ammonia at temperatures from 65.degree. to 180.degree. C. in which the reactants are simultaneously fed to an agitated inert solvent at a rate such that the phosphorus trichloride concentration is at most stoichiometric relative to the chlorine and ammonia concentration and such that petroleum ether insoluble phosphonitrilic chloride formation is suppressed, and recovering the cyclic phosphonitrilic halide oligomer mixture without extracting petroleum ether insoluble materials since these are not produced.Type: GrantFiled: July 3, 1975Date of Patent: April 1, 1980Assignee: Ethyl CorporationInventors: John W. Hudson, Thomas F. Dominick
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Patent number: 4183905Abstract: Improvement in the oxidation of phosphorus trihalide to the oxyhalide in a reactor having a lower reaction zone and at least one upper reaction zone, whereby the trihalide is introduced at the bottom portion of the upper reaction zone and rises upwardly, reacting with oxygen fed in at the bottom portion of said lower reaction zone, the PX.sub.3 -POX.sub.3 mixture exits through exit means in the top portion of said upper reaction zone and is fed therethrough to the topmost portion of said lower reaction zone where said mixture flows downwardly toward the product exit and reacts with upwardly flowing suitable quality oxygen.Type: GrantFiled: August 16, 1978Date of Patent: January 15, 1980Assignee: Mobil Oil CorporationInventor: B. Meredith Winn, Jr.
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Patent number: 4178353Abstract: Residual PCl.sub.3 in POCl.sub.3 which has been prepared by the oxidation of PCl.sub.3 in the presence of air or oxygen-enriched air is converted to POCl.sub.3 by contacting the POCl.sub.3 /PCl.sub.3 mixture with ozone or an ozone-enriched gas.Type: GrantFiled: August 4, 1975Date of Patent: December 11, 1979Assignee: Monsanto CompanyInventors: Joseph W. Baker, Dario R. Cova, James E. White
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Patent number: 4176022Abstract: Disclosed is a method of electrolyzing an alkali metal chloride brine in an electrolytic cell by feeding an aqueous alkali metal chloride brine containing less than 20 parts per billion dissolved alkaline earth metal ions, e.g., calcium, to the anolyte compartment of an electrolytic cell. Also disclosed is an alkali metal chloride brine containing less than 20 parts per billion of alkaline earth metal ions, e.g., calcium ion. There is also disclosed a method of purifying alkaline earth metal-containing brines, e.g., calcium-containing brines, by maintaining the brine alkaline, adding a phosphate to the alkaline brine whereby to form a calcium compound substantially insoluble in brine and thereafter separating the compound from the brine.Type: GrantFiled: April 27, 1978Date of Patent: November 27, 1979Assignee: PPG Industries, Inc.Inventor: William B. Darlington
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Patent number: 4175113Abstract: A process for the purification of crude chlorophosphazene involves the use of an intermediate purification stage in which the crude chlorophosphazene is subjected to at least two water-washings, following which a final purification step is conducted utilizing a conventional chlorophosphazene purification procedure, such as recrystallization, sublimation, distillation, or melt-filtering and at least a very high purity cyclic chlorophosphazene trimer is then recovered. In a preferred process, the crude chlorophosphazene is subjected to three water-washings prior to the final purification step.Type: GrantFiled: April 20, 1978Date of Patent: November 20, 1979Assignee: The Firestone Tire & Rubber CompanyInventor: John W. Fieldhouse
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Patent number: 4172115Abstract: Sulfur tetrachloride derivatives are prepared by reacting suitable sulfur-containing compounds in hydrogen fluoride with a gas containing molecular chlorine in the presence of one or more acidic halides. Such derivatives can be used to remove water from its solutions in hydrogen fluoride.Type: GrantFiled: July 31, 1978Date of Patent: October 23, 1979Assignee: Exxon Research & Engineering Co.Inventor: Roger Hulme
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Patent number: 4157425Abstract: A process is disclosed for the catalytically-induced preparation of phosphazene polymers. Cyclic halophosphazenes are polymerized in the presence of a catalytically sufficient amount of a compound having the formula M(OR').sub.x where M is an alkali metal or alkaline earth metal, x is equal to the valence of the metal and R' is C.sub.1 to C.sub.10 linear or branched alkyl, C.sub.1 to C.sub.10 substituted linear or branched alkyl, the substituent selected from the group consisting of nitro, C.sub.1 to C.sub.10 alkyl, C.sub.1 to C.sub.10 alkoxy, C.sub.6 to C.sub.10 aryl and C.sub.6 to C.sub.10 aryloxy, or N.sub.3 P.sub.3 Cl.sub.z (OR').sub.6-z wherein R' is as defined above and z equals 0 to 5.Type: GrantFiled: April 10, 1978Date of Patent: June 5, 1979Assignee: Armstrong Cork CompanyInventors: Ronald L. Dieck, Alan B. Magnusson
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Patent number: 4139598Abstract: High molecular weight poly(dihalophosphazenes) which exhibit solubility in benzene and in substituted benzenes are prepared in solution or in bulk from dihalophosphazenes such as (Cl.sub.2 PN).sub.3-7 at moderate temperatures by the use of novel polymerization catalysts.Type: GrantFiled: January 12, 1977Date of Patent: February 13, 1979Assignee: Horizons Research IncorporatedInventors: Kennard A. Reynard, Arthur H. Gerber
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Patent number: 4137330Abstract: A process for producing benzene-soluble substantially linear dichlorophosphazene polymer having the formula (NPCl.sub.2).sub.x, in which x is greater than 20 and may be as high as 50,000 or higher, from a cyclic oligomer having the formula (NPCl.sub.2).sub.n, in which n is from 3 to 9, particularly the trimer (NPCl.sub.2).sub.3 or tetramer (NPCl.sub.2).sub.4, in the presence of a small but significant amount of an inorganic salt, preferably a halide of a metal such as Cr, Ni, Co, Cu, Fe, Mn or Mg which affords control of the molecular weight and avoids the formation of large amounts of gel.Type: GrantFiled: February 9, 1978Date of Patent: January 30, 1979Assignee: The Firestone Tire & Rubber CompanyInventors: Mark S. Prichard, Ashley S. Hilton, Mark L. Stayer, Jr., Thomas A. Antkowiak
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Patent number: 4124567Abstract: A process is disclosed for the catalytically-induced preparation of phosphazene polymers. Cyclic halophosphazenes are polymerized in the presence of a catalytically sufficient amount of a compound having the formula M(OR').sub.x where M is an alkali metal or alkaline earth metal, x is equal to the valence of the metal and R' is C.sub.1 to C.sub.10 linear or branched alkyl, C.sub.1 to C.sub.10 substituted linear or branched alkyl, the substituent selected from the group consisting of nitro, C.sub.1 to C.sub.10 alkyl, C.sub.1 to C.sub.10 alkoxy, C.sub.6 to C.sub.10 aryl and C.sub.6 to C.sub.10 aryloxy, or N.sub.3 P.sub.3 Cl.sub.z (OR').sub.6-z wherein R' is as defined above and z equals 0 to 5.Type: GrantFiled: April 10, 1978Date of Patent: November 7, 1978Assignee: Armstrong Cork CompanyInventors: Ronald L. Dieck, Alan B. Magnusson
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Patent number: 4123503Abstract: Thermal polymerization of (NPCl.sub.2).sub.3,4 is improved by conducting the polymerization in the presence of Lewis Acid type compounds of Al or B.Type: GrantFiled: March 23, 1977Date of Patent: October 31, 1978Assignee: The Firestone Tire & Rubber CompanyInventors: Dennis L. Snyder, Mark L. Stayer, Jr., Jung W. Kang
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Patent number: 4116891Abstract: A process is disclosed for the catalytically-induced preparation of phosphazene polymers. Cyclic halophosphazenes are polymerized in the presence of a catalytically sufficient amount of a Lewis acid catalyst.Type: GrantFiled: December 6, 1976Date of Patent: September 26, 1978Assignee: Armstrong Cork CompanyInventors: Ronald L. Dieck, Thomas B. Garrett, Alan B. Magnusson
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Patent number: 4110421Abstract: A process is disclosed for the catalytically-induced preparation of phosphazene polymers. Cyclic halophosphazenes are polymerized in the presence of a catalytically sufficient amount of a compound having the formula M(OR').sub.x where M is an alkali metal or alkaline earth metal, x is equal to the valence of the metal and R' is C.sub.1 to C.sub.10 linear or branched alkyl, C.sub.1 to C.sub.10 substituted linear or branched alkyl, the substituent selected from the group consisting of nitro, C.sub.1 to C.sub.10 alkyl, C.sub.1 to C.sub.10 alkoxy, C.sub.6 to C.sub.10 aryl and C.sub.6 to C.sub.10 aryloxy, or N.sub.3 P.sub.3 Cl.sub.z (OR').sub.6-z wherein R' is as defined above and z equals 0 to 5.BACKGROUND OF THE INVENTIONThe present invention relates to a process for the preparation of phosphazene polymers. More specifically, the present invention relates to a method for catalytically producing polyphosphazenes.Type: GrantFiled: October 12, 1976Date of Patent: August 29, 1978Assignee: Armstrong Cork CompanyInventors: Ronald L. Dieck, Alan B. Magnusson
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Patent number: 4080432Abstract: Dihalophosphazene polymers are solubilized and stabilized whereby their tendency for gelatin or crosslinking is inhibited or overcome, by the addition of oxygen containing organic compounds such as alcohols, ketones, esters, ethers, or polyethers to hydrocarbon solvents for the polymer.Type: GrantFiled: August 22, 1975Date of Patent: March 21, 1978Assignee: The Firestone Tire & Rubber CompanyInventors: Dennis La Verne Snyder, Mark Lutz Stayer, Jr.
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Patent number: 4065546Abstract: Process for the preparation of chlorophosphazene mixtures having a high proportion of cyclic trimer and tetramer by preparing a dispersion of finely divided ammonium chloride in an amount sufficient to initiate the formation of chlorophosphazene, then, after heating the dispersion to reflux, co-feeding ammonia and a solution of phosphorus pentachloride in a suitable solvent at a rate such that no free PCl.sub.5 concentration is allowed to exist in the reaction mass, and then recovering the cyclic chlorophosphazene produced.Type: GrantFiled: December 8, 1975Date of Patent: December 27, 1977Assignee: Ethyl CorporationInventor: James T. F. Kao
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Patent number: 4046857Abstract: Polymeric phosphonitrilic chlorides are produced from ammonia and phosphorus pentachloride in a continuous process in a plurality of reaction zones characterized by simultaneous addition of reactants and continuous withdrawal of product.Type: GrantFiled: May 19, 1975Date of Patent: September 6, 1977Assignee: FMC CorporationInventors: Thomas M. Fekete, John F. Start
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Patent number: 4008299Abstract: A method is provided for preparing a fibre from a solution of a halogen-containing complex phosphate of aluminium. The complex contains at least one chemically-bound molecule of a hydroxy compound R-OH, where R is a hydrogen atom or an organic group. The complex is dissolved in water or an organic solvent. The solution is fibrized and then dried to produce the fibre.Type: GrantFiled: October 21, 1974Date of Patent: February 15, 1977Inventors: James Derek Birchall, John Edward Cassidy
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Patent number: 4005171Abstract: HIgh molecular weight poly(dihalophosphazenes) which exhibit solubility in benzene and in substituted benzenes are prepared in solution or in bulk from dihalophosphazenes such as (Cl.sub.2 PN).sub.3.sub.-7 at moderate temperatures by the use of novel polymerization catalysts.Type: GrantFiled: May 28, 1974Date of Patent: January 25, 1977Assignee: Horizons Incorporated, a division of Horizons Research IncorporatedInventors: Kennard A. Reynard, Arthur H. Gerber
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Patent number: 4005172Abstract: Complex phosphates of aluminum containing a halogen and chemically-bound molecule of a hydroxy compound, namely, water. A typical example is a complex phosphate having the empirical formulate AlPClH.sub.11 O.sub.9. They are most conveniently prepared by the reaction of an aluminum halide with water and orthophosphoric acid, under relatively cool conditions. The compounds are generally soluble in water and polar organic solvents. They decompose at low temperatures to give aluminum orthophosphate, thereby providing a method for producing aluminum phosphate in many forms, for example, fibers, coatings, binders and fine particles, from a solution in water or organic solvents.Type: GrantFiled: October 21, 1974Date of Patent: January 25, 1977Assignee: Imperial Chemical Industries LimitedInventors: James Derek Birchall, John Edward Cassidy
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Patent number: 3995013Abstract: Processes for the preparation of high-purity free-flowing crystalline powder phosphorus pentachloride which processes comprise reacting phosphorus trichloride with a deficit of chlorine, cooling the reaction mixture to form a crystalline mass containing the pentachloride, and recovering and/or purifying the pentachloride.Type: GrantFiled: January 2, 1975Date of Patent: November 30, 1976Assignee: Produits Chimiques Ugine KuhlmannInventor: Michel Demarq
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Patent number: 3992159Abstract: A process is described for purifying liquids by cryogenic sublimation. This process involves solidifying the liquid by reducing the temperature and pressure to below the triple point. Purification is then carried out by direct transformation from the solid to the vapor phase. Because of increased differentials in vapor pressures at the low temperature at which the procedure is carried out, this purification process is highly efficient and is also particularly suitable for liquids that are susceptible to decomposition with ordinary purification procedures requiring elevated temperatures. The procedure is also advantageous in separating azeotropes, structurally similar compounds, as well as treating flammable, hydroscopic, corrosive and fuming compounds.Type: GrantFiled: June 23, 1975Date of Patent: November 16, 1976Assignee: Bell Telephone Laboratories, IncorporatedInventor: James Windfield Mitchell
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Patent number: 3982036Abstract: Novel feed grade calcium phosphate compositions are provided which contain calcium chlorophosphate in varying amounts. This novel composition and other heretofore known varieties of feed grade calcium phosphates are prepared by low temperature drying steps (spray drying or crystallization-evaporation) of solutions or slurries which have been partially defluorinated to the extent that the solution P/F ratio is at least 30-35 but less than 100. The novel compositions described above have adequate levels of phosphorus availability to animals thereby permitting their usage as an animal feed supplement.Type: GrantFiled: October 15, 1973Date of Patent: September 21, 1976Assignee: American Cyanamid CompanyInventor: Ashok Babubhai Amin
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Patent number: 3974261Abstract: A method for the selective purification of phosphonitrilic chloride polymer mixtures to obtain substantially pure cyclic trimeric and tetrameric phosphonitrilic chloride polymers by distillaton under reduced pressure with inert solvent passed through the molten phosphonitrilic chloride mixture, optionally with prior solvent extraction and/or subsequent recrystallization from solvent.Type: GrantFiled: November 6, 1974Date of Patent: August 10, 1976Assignee: Ethyl CorporationInventor: Charles R. Bergeron
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Patent number: 3960592Abstract: There is provided a composition suitable for use as a coating composition which contains a halogen-containing complex phosphate of aluminum, other than a phosphate ester, dissolved in an organic solvent. The complex contains at least one chemically-bound molecule of an alcohol having from one to 10 carbon atoms. The complex is prepared by interacting an aluminum compound, such as aluminum halides, with an alcohol containing one to 10 carbon atoms and with phosphoric acid.Type: GrantFiled: October 21, 1974Date of Patent: June 1, 1976Assignee: Imperial Chemical Industries LimitedInventors: James Derek Birchall, John Edward Cassidy
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Patent number: 3956463Abstract: Improvement in the oxygen oxidation of phosphorus trihalides, particularly phosphorus trichloride, to phosphorus oxyhalide, particularly oxychloride, by introducing phosphorus trihalide and gaseous oxygen into the bottom of an elongated, substantially vertical reaction zone, passing said phosphorus trihalide and oxygen upwardly through said zone while reacting such together; withdrawing a portion of the upwardly flowing reaction mixture from an intermediate point in said zone; introducing oxygen into admixture with said withdrawn admixture and cooling, agitating and reacting such; returning said admixture reaction mass to said elongated reaction zone; and recovering substantially pure phosphorus oxyhalide from the downstream end of said reaction zone.Type: GrantFiled: April 2, 1975Date of Patent: May 11, 1976Assignee: Mobil Oil CorporationInventor: B. Meredith Winn, Jr.
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Patent number: 3955029Abstract: The new product, a Cl.sub.3 P=N--N=PCl.sub.3 + NH.sub.3 reaction product, has been found to be an excellent flameretardant for material made from cellulose such as cotton, paper and sponge; polyester, wool and blends thereof. Conveniently the material can be treated with an aqueous solution containing a sufficient amount of the product and the material dried to make the material self-extinguishing. Then the treated and dried material is cured at a sufficient temperature to bond the product to the material. Alternatively, and usually preferably, the drying and curing can be accomplished as a single operation.Type: GrantFiled: July 22, 1974Date of Patent: May 4, 1976Assignee: Monsanto Research CorporationInventor: Albert Y. Garner
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Patent number: 3952086Abstract: A process for the purification of crude chlorophosphazene involves adding a Bronsted base to a vessel containing crude chlorophosphazene, removing water formed in the vessel from the reaction of the Bronsted base with the impurities in crude chlorophosphazene and then removing at least a very high purity cyclic chlorophosphazene trimer.Type: GrantFiled: October 7, 1974Date of Patent: April 20, 1976Assignee: The Firestone Tire & Rubber CompanyInventor: John William Fieldhouse
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Patent number: 3948820Abstract: Copolymers and terpolymers comprising randomly repeating units represented by the general formulae ##EQU1## wherein the R' radicals contain OH functionality and R being at least one member of the group of monovalent radicals selected from alkyl, substituted alkyl, aryl, substituted aryl and arylalkyl, and R' is represented by ##EQU2## wherein Q represents either --(CH.sub.2).sub. n or --C.sub.6 H.sub.4 X(CH.sub.2).sub. m, the --X(CH.sub.2).sub. m group being either meta or para and n is an integer from 1 to 6, m is an integer from 1 to 3, X is O or CH.sub.2, and R" is H or a lower alkyl radical with up to four carbon atoms (methyl, ethyl, etc.). The ratio of R to R' is between 99.5 to 0.5 and 65 to 35.Type: GrantFiled: August 7, 1974Date of Patent: April 6, 1976Assignee: Horizons IncorporatedInventors: Kennard A. Reynard, Selwyn H. Rose
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Patent number: 3939188Abstract: A process for preparing oxygenated products comprising aldehydes, which have high normal to branched-chain isomer ratios. The process involves using particularly characterized rhodium-containing complex catalysts under a specific combination of carefully controlled reaction conditions. The product aldehydes as made above may be condensed and hydrogenated to form saturated aldehyde dimers thereof.Type: GrantFiled: March 24, 1972Date of Patent: February 17, 1976Assignee: Exxon Research and Engineering CompanyInventor: Gary B. McVicker
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Patent number: 3937790Abstract: The polymerization of hexachlorocyclotriphosphazene to poly(dichlorophosphazene) at elevated temperatures is a highly unpredictable process. The rate of polymerization varies over a wide range and is dependent on the history of the trimer and on the method of handling prior to polymerization.It appears that small amounts of water may possibly function as catalytic species for the polymerization. The addition of controlled amounts of water to the system results in a marked increase in reaction rate, and the rigorous exclusion of water from the system inhibits the reaction. The results favor the view that complete exclusion of water from the system may result in a system that cannot be polymerized. Thus, water appears to be a key component for polymerization.Type: GrantFiled: October 2, 1974Date of Patent: February 10, 1976Assignee: The Firestone Tire & Rubber CompanyInventors: Harry Rex Allcock, James Earl Gardner, deceased, Karen M. Smeltz