Halogen Containing Patents (Class 423/300)
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Patent number: 5230875Abstract: The molecular weights of the poly(dichlorophosphazenes), and of the poly(organophosphazenes) produced therefrom, are controlledly regulated by heating such poly(dichlorophosphazenes) in the presence of an effective molecular weight-regulating amount of phosphorus oxychloride.Type: GrantFiled: October 22, 1990Date of Patent: July 27, 1993Assignee: AtochemInventors: Roger de Jaeger, Guy Pagniez, Philippe Potin
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Patent number: 5183649Abstract: Chlorophosphorus compounds are produced in a loop apparatus wherein chlorine is added to a recycling medium comprising chlorophosphorus compound and elemental phosphorus.Type: GrantFiled: April 11, 1991Date of Patent: February 2, 1993Assignee: Albright & Wilson Ltd.Inventors: William S. Holmes, Robert Marshall
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Patent number: 5152971Abstract: High molecular weight, essentially uncrosslinked polychlorophosphazenes are prepared by bulk polycondensing a monomer of the formula P.sub.2 NXCl.sub.2, in which X is an oxygen or sulfur atom, e.g., N-dichlorophosphoryl- or N-dichlorothiophosphoryl-P-trichlorophosphazene, and wherein at least that final stage of polycondensation following cessation of evolution of PXCl.sub.3 is carried out in a stirred reaction zone, such stirred reaction zone including means to prevent the accumulation of polycondensate on the stirrer.Type: GrantFiled: May 21, 1990Date of Patent: October 6, 1992Assignee: AtochemInventors: Joel Bertrand, Philippe Potin
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Patent number: 5147622Abstract: The invention relates to a method for the stabilization of phosphorus trichloride, wherein one or more derivatives of dithiocarbamic acids are added to the phsophorus trichloride. As derivatives, salts, esters or thiuram sulfides of the dithiocarbamic acids, individually or as a mixture, are preferred. The amounts used generally fall within the range of 10.sup.-4 % to 10.sup.-2 %, based on the amount of phosphorus trichloride. Derivatives, which are only slightly soluble in phosphorus trichloride are advantageously used in amounts of more than 10.sup.-2 %. Due to the inventive addition of derivatives of dithiocarbamic acids, the formation of phosphorus oxychloride in the phosphorus trichloride is delayed significantly and reduced to a minimum value.Type: GrantFiled: March 6, 1991Date of Patent: September 15, 1992Assignee: Chemie AG Bitterfeld-WolfenInventor: Rudolf Schumann
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Patent number: 5147621Abstract: The invention relates to a method for stabilizing phosphorus trichloride. In order to delay the formation of phosphorus oxychloride in phosphorus trichloride and to reduce it to a minimum value which no longer adversely affects further processing, one or more amines which have at least two aromatic hydrocarbon groups linked to one nitrogen atom, such as diphenylamine, phenothiazine, phenyl-4-methylphenylamine and triphenylamine, are added to the phosphorus trichloride. The amines can also be added in the form of their salts, including their quaternary ammonium compounds, or their reaction products with phosphorus halides. The amounts of amines, added fall within the range of 10.sup.-6 % to 10.sup.-1 %, based on the amount of phosphorus trichloride.Type: GrantFiled: March 6, 1991Date of Patent: September 15, 1992Assignee: Chemie AG Bitterfeld-WolfenInventor: Rudolf Schumann
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Patent number: 5132389Abstract: The polycondensation disrupting effects of the impurities in an impure N-dichlorophosphoryltrichlorophosphazene, P.sub.2 NOCl.sub.5, or oligomer thereof, are avoided by polycondensing such impure P.sub.2 NOCl.sub.5 into a high molecular weight uncrosslinked poly(dichlorophosphazene) in the presence of an effective impurity-inhibiting, polymerization-controlling amount of phosphorous pentachloride, PCl.sub.5.Type: GrantFiled: October 22, 1990Date of Patent: July 21, 1992Assignee: AtochemInventors: Roger de Jaeger, Ghislaine D'Halluin, Guy Pagniez, Philippe Potin
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Patent number: 5030430Abstract: Phosphates, e.g., the polyphosphates and halophosphates, are prepared in high purity by melt thermocondensing corresponding precursors thereof, e.g., salts of orthophosphoric, pyrophosphoric or metaphosphoric acid, via electromagnetic induction heating, for example in an auto-crucible furnace.Type: GrantFiled: July 13, 1989Date of Patent: July 9, 1991Assignee: Rhone-Poulenc ChimieInventors: Paul Michel, Francoise Seon, Rene Perrier de la Bathie
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Patent number: 5006324Abstract: High molecular weight phosphonitrillic chloride polymers that are soluble in benzene, toluene and tetrahydrofuran, tetrameric phosphonitrilic chloride, or mixtures thereof at elevated temperatures in the presence of a catalytic amount of an aprotic Lewis acid halogen acceptor. For example, soluble high molecular weight phosphonitrillic chloride can be made by heating the aforementioned trimer at 220.degree.-270.degree. C. in the presence of 5-1000 ppm of AlCl.sub.3.Type: GrantFiled: January 10, 1984Date of Patent: April 9, 1991Assignee: Ethyl CorporationInventors: Charles H. Kolich, Bernard R. Meltsner, Henry G. Braxton, Jr.
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Patent number: 4902490Abstract: Essentially pure and colorless N-(dichlorophosphoryl)trichlorophosphazene [P.sub.2 NOCl.sub.5 ] is prepared/purified under relatively moderate conditions, by reacting phosphorous pentachloride with ammonium chloride, treating the resulting medium of reaction, containing P.sub.3 NCl.sub.12, with SO.sub.2, and thin film evaporating the medium of reaction, advantageously in two stages, to eliminate SO.sub.2, POCl.sub.3 and SOCl.sub.2 values therefrom.Type: GrantFiled: March 10, 1988Date of Patent: February 20, 1990Assignee: AtochemInventors: Guy Pagniez, Philippe Potin
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Patent number: 4867957Abstract: The invention is a continuous polymerization process for producing high molecular weight linear poly(dichlorophosphazene) polymers in dilute solution. Substantially pure cyclic oligomers represented by the formula (NPCl.sub.2).sub.n are polymerized in dilute solution in an inert solvent at a temperature in the range from 150 degrees Celsius to 300 degrees Celsius for a period of time sufficient to convert a predetermined percentage of oligomer to polymer. The polymer solution may be added to a fresh solution of oligomer, solvent and catalyst to obtain polymers of greater molecular weight. This step may be repeated as many times as necessary to obtain a particular molecular weight. This invention provides a significant improvement in the attainable molecular weight in dilute solution polymerization, with a very high conversion rate of oligomer. The viscosity of the solution during the continuous reaction process is maintained at a level which may be easily handled.Type: GrantFiled: December 19, 1988Date of Patent: September 19, 1989Assignee: The United States of America as represented by the Secretary of the ArmyInventor: Michael S. Sennett
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Patent number: 4824648Abstract: Linear polychlorophosphazenes are more rapidly produced by polycondensing N-(dichlorophosphoryl)trichlorophosphazene [P.sub.2 NOCl.sub.Type: GrantFiled: March 10, 1988Date of Patent: April 25, 1989Assignee: AtochemInventors: Guy Pagniez, Nadine Passimourt, Philippe Potin
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Patent number: 4812297Abstract: N-(Dichlorophosphoryl)trichlorophosphazene [P.sub.2 NOCl.sub.2 ], essentially devoid of oligomeric impurities, is improvedly and reproducibly prepared by reacting phosphorus pentachloride with ammonium chloride, advantageously stoichiometrically, wherein more than 50% by weight of the ammonium chloride is of a particle size less than 0.16 mm.Type: GrantFiled: March 10, 1988Date of Patent: March 14, 1989Assignee: AtochemInventors: Nadine Passimourt, Philippe Potin
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Patent number: 4810480Abstract: Polychlorophosphazene [Cl.sub.2 (O)P[NPCl.sub.2 ].sub.n Cl] is more rapidly produced by polycondensing N-(dichlorophosphoryl)-trichlorophosphazene [P.sub.2 NOCl.sub.5 ] in the presence of a catalytically effective amount of a tertiary amine.Type: GrantFiled: March 10, 1988Date of Patent: March 7, 1989Assignee: AtochemInventors: Jean-Paul Chambrette, Roger de Jaeger, Philippe Potin
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Patent number: 4806322Abstract: The present invention relates to a method of preparing linear polyphosphazene polymers by direct synthesis under anhydrous conditions from NH.sub.4 Cl and at least one chlorophosporous compound selected from the group consisting of PCl.sub.5, XPCl.sub.4, or X.sub.2 PCl.sub.3 wherein X is one or more substituents selected from the group consisting of C.sub.6 H.sub.5 -, C.sub.6 H.sub.4 Cl-, C.sub.6 H.sub.4 F-, C.sub.6 H.sub.4 Br-, C.sub.6 H.sub.2 Cl.sub.3 -, C.sub.6 F.sub.5 -, C.sub.6 H.sub.4 CF.sub.3 -, C.sub.6 H.sub.4 NO.sub.2 -, Cl.sub.3 C-, F.sub.3 C-, F.sub.5 C.sub.2 -, F.sub.7 C.sub.3 -, or HC.sub.2 F.sub.4 -. Each of these compounds may be prepared in situ in a reactor. The instant process controls the pressure in the reactor through continuous venting of by-product HCl at elevated pressures. The instant invention also utilizes an excess of of reactive solvent such as PCl.sub.3, XPCl.sub.2, or X.sub.2 PCl as X is defined above.Type: GrantFiled: November 16, 1987Date of Patent: February 21, 1989Assignee: The Firestone Tire & Rubber CompanyInventors: William L. Hergenrother, James Oziomek
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Patent number: 4795621Abstract: Phosphonitrile chloride oligomer, particularly, phosphonitrile chloride trimer, is produced in high yield while suppressing the formation of by-product phosphonitrile chloride tetramer, by reacting phosphorus pentachloride with ammonium chloride in an inert organic solvent, in the presence of a catalytic amount of a compound selected from the group consisting of quinoline, isoquinoline and their drivatives represented by the general formulae: ##STR1## wherein R stands for an alkyl group or a halogen atom and n stands for zero or an integer of 1 to 7,and pyridine derivatives represented by the general formula: ##STR2## wherein Q stands for a halogen atom or a hydroxyl group; R' stands for an alkyl group; m stands for an integer of 1 to 5 and p stands for zero of an integer of 1 to 4 with the proviso that the total number of m and p is from 1 to 5,and in the presence of a catalytic amount of a polyvalent metal compound.Type: GrantFiled: August 13, 1986Date of Patent: January 3, 1989Assignee: Shin Nisso Kako Co., Ltd.Inventors: Tetsuhiko Okamoto, Shinichiro Ueyama, Kazuhiko Fujikawa
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Patent number: 4780292Abstract: Colorless, or but very faintly tinted N-(dichlorophosphoryl)trichlorophosphazene [P.sub.2 NOCl.sub.5 ] is prepared by reacting phosphorus pentachloride with ammonium chloride in the presence of POCl.sub.3, and then treating the resulting medium of reaction, containing P.sub.3 NCl.sub.12, with SO.sub.2, and wherein the temperature of the medium of reaction is maintained at a value of at most about 30.degree. C.Type: GrantFiled: November 12, 1987Date of Patent: October 25, 1988Assignee: AtochemInventor: Nadine Passimourt
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Patent number: 4708858Abstract: A catalytic method for polymerizing cyclic dihalophosphazene to linear polydihalophosphazene is provided wherein the catalyst is a solid support of silica or alumina containing supported thereon both a transition metal compound and an organometallic compound.Type: GrantFiled: April 17, 1985Date of Patent: November 24, 1987Assignee: The Dow Chemical CompanyInventor: Charles C. Kirkpatrick
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Patent number: 4693876Abstract: A process for preparing linear polychlorophosphazenes having a terminal --PXCl.sub.2 group, wherein X is O or S, by polycondensation of a monomer of the formula P.sub.2 NXCl.sub.5, by heating to release PXCl.sub.3 and continuing the heating after the evolution of PXCl.sub.3 has stopped. In the process, at least the heat induced polycondensation phase after evolution of PXCl.sub.3 has stopped is carried out in solution in a medium which is a solvent for both the monomer and the polymer and which is inert to the constituents of the polycondensation reaction. The process reduces the amount of cross-linking and produces high molecular weight polymers in a reproducible way.Type: GrantFiled: August 14, 1986Date of Patent: September 15, 1987Assignee: Societe Nationale Elf AquitaineInventors: Roger DeJaeger, Guy Pagniez, Philippe Potin
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Patent number: 4663138Abstract: Polymer-grade cyclic phosphonitrilic halide trimer can be obtained by (i) reacting ammonium halide with phosphorus pentahalide in an inert solvent containing pyridine, substituted pyridines or mixtures thereof or hydrogen halide complexes thereof, (ii) washing the solvent phase with an aqueous alkali metal hydroxide and (iii) crystallizing cyclic trimer and/or distilling the cyclic trimer to obtain polymer-grade trimer.Type: GrantFiled: April 21, 1986Date of Patent: May 5, 1987Assignee: Ethyl CorporationInventors: Joseph B. Tedder, Jr., J. Robert Adams, Jr.
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Patent number: 4656018Abstract: Cyclic phosphonitrilic halide trimer is made in high yield and at a rapid rate by adding NH.sub.3 or ammonium halide to a pyridine-hydrogen halide complex and adding phosphorus pentahalide and a solvent for the trimer (e.g. monochlorobenzene) and heating the mixture to above 90.degree. C. to form trimer which dissolves in the solvent and then separating the trimer-solvent phase from the residue phase of pyridine-hydrogen halide complex and recovering trimer from the solvent phase and recycling the pyridine-hydrogen halide phase to a subsequent procedure conducted in the same manner. The process can also be adapted to produce linear species in high yield also.Type: GrantFiled: November 18, 1985Date of Patent: April 7, 1987Assignee: Ethyl CorporationInventors: Gerald M. Sulzer, Joseph B. Tedder, Jr., J. Robert Adams, Jr., Matthew K. Juneau
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Patent number: 4656017Abstract: Cyclic phosphonitrilic halides are formed rapidly and in high yield in a controllable multi-step process including the step of reacting a nitrogenous base (e.g. pyridine) with a phosphorus tetrahalide (e.g. phosphorus pentachloride) in a suitable inert liquid reaction medium (e.g. monochlorobenzene) to form a complex and in a subsequent step reacting this complex with an ammonium halide (e.g. ammonium chloride) at a temperature above about 90.degree. C. up to the reflux temperature of the reaction medium to form cyclic phosphonitrilic halides, mainly trimer.Type: GrantFiled: July 19, 1985Date of Patent: April 7, 1987Assignee: Ethyl CorporationInventors: Harry R. Allcock, S. James Stinnett, Joseph B. Tedder, Jr., J. Robert Adams, Jr.
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Patent number: 4627967Abstract: Polymerization grade phosphonitrilic chloride trimer is made by reacting NH.sub.4 Cl and PCl.sub.5 in a solvent (e.g. monochlorobenzene) to form a crude trimer solution, filtering the solution to remove unreacted NH.sub.4 Cl, distilling a portion of the solvent to form a hot concentrate, cooling the concentrate to obtain a precipitate, distilling the precipitate at reduced pressure to first remove a forecut and then a heart-cut of polymerization grade phosphonitrilic chloride trimer.Type: GrantFiled: October 5, 1984Date of Patent: December 9, 1986Assignee: Ethyl CorporationInventor: W. Dirk Klobucar
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Patent number: 4623525Abstract: The present invention relates to the stabilization against water of solutions of poly(dichlorophosphazene) through the utilization of water reacting complexes of substituted silicon, tin, germanium or titanium chlorides which are complexed with a tertiary amine base.Type: GrantFiled: January 7, 1985Date of Patent: November 18, 1986Assignee: The Firestone Tire & Rubber CompanyInventors: William L. Hergenrother, John W. Fieldhouse, Adel F. Halasa
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Patent number: 4605539Abstract: Polymer-grade cyclic phosphonitrilic chloride trimer can be obtained from crude cyclic polyphosphonitrilic chlorides by forming a solution of the crude cyclics, water washing the solution, distilling solvent to form a hot concentrate, cooling to form a precipitate and distilling the precipitate to form polymer-grade trimer.Type: GrantFiled: November 16, 1984Date of Patent: August 12, 1986Assignee: Ethyl CorporationInventors: J. Robert Adams, Jr., James R. Mitrano, Matthew K. Juneau
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Patent number: 4603038Abstract: Cyclic phosphonitrilic chloride trimer suitable for polymerization to light colored, high molecular weight, linear polyphosphonitrilic chloride can be made by (1) reacting PCl.sub.5 and NH.sub.4 Cl in an inert solvent (e.g. monochlorobenzene) to form a solution of a low molecular weight linear and cyclophosphonitrilic chlorides, (2) evaporating solvent to form a concentrate, (3) adding water and cooling the mixture to precipitate cyclic trimer, (4) separation of the trimer precipitate and (5) distillation of the separated trimer.Type: GrantFiled: October 5, 1984Date of Patent: July 29, 1986Assignee: Ethyl CorporationInventors: J. Robert Adams, Jr., James R. Mitrano, Matthew K. Juneau
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Patent number: 4576806Abstract: Residual alkali metal salt (e.g. NaCl) is removed from an alkali metal alkoxide and/or aryloxide-polyphosphonitrilic halide reaction product by neutralizing the reaction solution with acid and water extracting the salt using a lower water-soluble alcohol (isopropanol) to effect rapid phase separation.Type: GrantFiled: March 29, 1985Date of Patent: March 18, 1986Assignee: Ethyl CorporationInventor: Matthew K. Juneau
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Patent number: 4567028Abstract: A process for the preparation of phosphonitrile chloride oligomer, particularly, phosphonitrile chloride trimer at a high yield while suppressing the by-production of phosphonitrile chloride tetramer by reacting phosphorus pentachloride and ammonium chloride in an inert organic solvent under the presence of a polyvalent metal compound catalyst, wherein a catalytic amount of a compound selected from the group consisting of pyridine and alkyl-substituted pyridine derivatives capable of forming chloropyridinium salts in reaction with phosphorus pentachloride is present in the reaction system.Type: GrantFiled: February 11, 1985Date of Patent: January 28, 1986Assignee: Shin Nisso Kako Co., Ltd.Inventors: Hiroshi Tanino, Tetsuhiko Okamoto, Shinichiro Ueyama
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Patent number: 4554113Abstract: Linear polychlorophosphazenes having a dichlorothiophosphoryl terminal group and corresponding to the formulaCl.sub.2 (S)P--NPCl.sub.2 ].sub.n Clwherein n is a number equal to or more than 4.The aforesaid linear polychlorophosphazenes are prepared by polycondensing P.sub.2 NSCl.sub.5 by heating under conditions adequate for liberating PSCl.sub.3.These polymers can be applied to all the uses of the classical polychlorophosphazenes.Type: GrantFiled: July 6, 1984Date of Patent: November 19, 1985Assignee: Societe Nationale Elf AquitaineInventors: Taher Abou Chakra, Roger De Jaeger
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Patent number: 4551317Abstract: Halophosphazene polymers such as linear phosphonitrilic chloride polymers are prepared in two stages by (i) heating a nitrogen source (e.g., NH.sub.3 ; NH.sub.4 Cl; etc.) with an excess of a phosphorus source (e.g., PCl.sub.5 ; PCl.sub.3 +Cl.sub.2 ; P+Cl.sub.2 ; etc.) so that hydrogen halide is evolved and halophosphazene is formed, and (ii) heating at least a portion of the halophosphazene with at least a stoichiometric amount (preferably an excess) of a nitrogen source (e.g., NH.sub.3 ; NH.sub.4 Cl; etc.) so that hydrogen halide is evolved and halophosphazene polymer of higher molecular weight is formed. Preferably, a third stage is utilized wherein the resultant halophosphazene polymer is then heated, most preferably in an inert solvent or diluent which enhances the fluidity of the reaction mixture, to increase the molecular weight of the polymer.Type: GrantFiled: April 28, 1983Date of Patent: November 5, 1985Assignee: Ethyl CorporationInventor: Hsueh M. Li
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Patent number: 4544537Abstract: Cyclic dichlorophosphazene trimer which is substantially pure except for catalytic impurities is purified by treating the trimer in the liquid phase with P.sub.2 O.sub.5 for 10-30 minutes at a temperature of 120.degree.-170.degree. C. and atmospheric pressure, then subjecting the reaction mix to a single further purification step by sublimation, melt filtration, or distillation. The purified trimer will not polymerize in the absence of added catalyst at 300.degree. C. or below.Type: GrantFiled: December 17, 1984Date of Patent: October 1, 1985Assignee: The Firestone Tire & Rubber CompanyInventors: Daniel F. Graves, Dennis L. Snyder
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Patent number: 4544536Abstract: The present invention relates to novel polychlorophosphazenes and to the process for their preparation.These polychlorophosphazenes of the general formula:Cl.sub.2 (O)P[NPCl.sub.2 ].sub.n Clare prepared by the polycondensation of P trichloro-N dichlorophosphoryl-monophosphazene with the controlled release of POCl.sub.3 according to the equation: ##STR1## The novel polychlorophosphazenes so obtained are useful as antiflame materials, as coatings, as fertilizers, etc.Type: GrantFiled: March 21, 1983Date of Patent: October 1, 1985Assignee: Institut Mondial du PhosphateInventors: Roger De Jaeger, Moncef Helioui, Emile Puskaric
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Patent number: 4537755Abstract: To prepare halophosphazene oligomer enriched in cyclic trimer, a two-stage process is used. In the first stage halogen halide and ammonia are concurrently introduced into an agitated liquid reaction medium in which halophosphazene oligomer is soluble, these materials being proportioned so as to form a reaction system composed of a dilute slurry of finely divided ammonium halide particles. In the second stage phosphorus trihalide and halogen are concurrently introduced into the slurried reaction system from the first stage heated to a temperature of about 80.degree. to about 180.degree. C. In the process the quantities of the reactants introduced into the reaction medium are proportioned such that the ammonium halide:phosphorus trihalide molar ratio is between about 1:1 and about 3:1, and the phosphorus trihalide:halogen molar ratio is kept above about 0.Type: GrantFiled: December 5, 1983Date of Patent: August 27, 1985Assignee: Ethyl CorporationInventor: Hsueh M. Li
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Patent number: 4524052Abstract: New compositions of matter which are halogenated derivatives of borates are disclosed which are catalytically active in the polymerization of halogenated phosphazene trimers and other oligomers are disclosed.Type: GrantFiled: December 24, 1984Date of Patent: June 18, 1985Assignee: The Firestone Tire & Rubber CompanyInventor: Daniel F. Graves
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Patent number: 4522798Abstract: A mixture of compounds of the formulas:[X--(PX.sub.2 .dbd.N).sub.n --PX.sub.3 ].sup.+ [R].sup.-andX--(PX.sub.2 .dbd.N).sub.n --POX.sub.2wherein X is a halogen atom, R is X or PX.sub.6 or both of them, and n is an integer, usually below about 15, is heated either with no other reactant or with a suitable phosphorus reactant such as PX.sub.5 ; PX.sub.3 +X.sub.2 ; P+X.sub.2 ; or a mixture of two or more such phosphorus reactants so that a halophosphazene having a --PX.sub.3.sup.+ end group is formed as one of the co-products of the reaction. This co-product is a substance having the general formula[X--(PX.sub.2 .dbd.N).sub.n --PX.sub.3 ].sup.+ [R].sup.-wherein X, R and n are as defined above. The other co-product is phosphoryl trihalide, POX.sub.3. In a second stage the resultant reaction product is heated with at least a stoichiometric amount (preferably, an excess) of a nitrogen source (e.g., NH.sub.3 ; NH.sub.4 Cl; etc.Type: GrantFiled: September 8, 1983Date of Patent: June 11, 1985Assignee: Ethyl CorporationInventors: Genevieve S. Lum, Hsueh M. Li, F. Alexander Pettigrew
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Patent number: 4522796Abstract: Linear phosphonitrilic chloride polymers are produced from phosphonitrilic chloride oligomers by means of an improved process wherein a mixture of phosphonitrilic chloride oligomers enriched in linear oligomer is heated with at least a stoichiometric amount (and preferably an excess) of ammonia or ammonium chloride while concurrently removing hydrogen chloride to produce a higher molecular weight polyphosphonitrilic chloride product. Cyclic phosphonitrilic chloride oligomer may be and preferably is present in the initial oligomer. Preferably, cyclic phosphonitrilic chloride oligomer is recovered from the reaction mixture during (but more preferably after) completion of the polymerization reaction. At least a portion of the recovered cyclic oligomer may be used in a subsequent polymerization reaction.Type: GrantFiled: April 22, 1983Date of Patent: June 11, 1985Assignee: Ethyl CorporationInventor: Hsueh M. Li
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Patent number: 4522689Abstract: A process for completely separating tri(phosphonitrile chloride) from tetra(phosphonitrile chloride) and/or phosphonitrile chloride oligomer which includes vacuum distillation of the phosphonitrile chloride mixture together with an inert mixture of hydrocarbons as solvent.Type: GrantFiled: October 9, 1984Date of Patent: June 11, 1985Assignee: Shin Nisso Kako Co., Ltd.Inventors: Hiroshi Tanino, Tetsuhiko Okamoto, Shinichiro Ueyama, Kazuhiko Fujikawa, Takatoshi Tsumiyama
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Patent number: 4522797Abstract: One or a mixture of compounds of the formula:X--(PX.sub.2 .dbd.N).sub.n --POX.sub.2wherein X is a halogen atom and n is an integer, usually below about 15 is heated with a suitable phosphorus reactant such as PX.sub.5 ; PX.sub.3 +X.sub.2 ; P+X.sub.2 ; or oligomer of the formula[X--(PX.sub.2 .dbd.N).sub.n --PX.sub.3 ].sup.+ [R].sup.-wherein X is a halogen atom, R is PX.sub.6 or X, and n is an integer usually below about 15; or a mixture of two or more such phosphorus reactants so that a halophosphazene having a --PX.sub.3.sup.+ end group is formed as one of the co-products of the reaction. This co-product is a substance having the general formula[X--(PX.sub.2 .dbd.N).sub.n --PX.sub.3 ].sup.+ [R].sup.-wherein X, R and n are as defined above. The other co-product is phosphoryl trihalide, POX.sub.3. In a second stage the resultant reaction product is heated with at least a stoichiometric amount (preferably, an excess) of a nitrogen source (e.g., NH.sub.3 ; NH.sub.4 Cl; etc.Type: GrantFiled: September 8, 1983Date of Patent: June 11, 1985Assignee: Ethyl CorporationInventors: F. Alexander Pettigrew, Hsueh M. Li, Genevieve S. Lum
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Patent number: 4522795Abstract: Linear phosphonitrilic chloride polymers are produced from phosphonitrilic chloride oligomers by means of a two-stage process. In the first stage a mixture of phosphonitrilic chloride oligomers enriched in linear oligomer is heated with at least a stoichiometric amount (and preferably an excess) of ammonia or ammonium chloride while concurrently removing hydrogen chloride to produce an intermediate reaction product. In the second stage the molecular weight of the reaction product is increased by heating the product to a higher temperature than the average temperature used in the first stage. Cyclic phosphonitrilic chloride oligomer may be present in the initial oligomer. Preferably, cyclic phosphonitrilic chloride oligomer is recovered from the reaction mixture after the start of the second stage. Most preferably it is recovered after completion of the second stage. At least a portion of the recovered cyclic oligomer may be used in a subsequent first stage reaction.Type: GrantFiled: April 22, 1983Date of Patent: June 11, 1985Assignee: Ethyl CorporationInventor: Hsueh M. Li
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Patent number: 4447408Abstract: Linear phosphonitrile chloride polymers are produced from linear phosphonitrilic chloride oligomers by means of a two-step proess. In the first step a mixture of linear phosphonitrilic chloride oligomer having an average degree of polymerization of at least 3 and preferably at least 4 is heated with an excess of ammonia or ammonium chloride having a relatively small particle size such that the Mean Value is within the range of from about 1 micron to about 110 microns. Cyclic phosphonitrilic chloride oligomer formed during the course of the first step is removed from the reaction mixture. After the removal of the cyclic oligomer the reaction mixture is subjected to the second step which involves heating the mixture in an inert liquid solvent (optionally in the presence of ammonia or ammonium chloride having a relatively small particle size) whereby the molecular weight of the linear phosphonitrilic chloride polymer is increased.Type: GrantFiled: December 7, 1982Date of Patent: May 8, 1984Assignee: Ethyl CorporationInventor: Hsueh M. Li
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Patent number: 4438081Abstract: Oligomeric chlorophosphazenes of the formula(N.dbd.PClR).sub.nin which n is an integer of from 3 to 8 and R is phenyl, C.sub.1 -C.sub.6 -alkyl or chlorine, are treated with sulfur dioxide or sulfur oxide chlorides, and so purified. The chlorophosphazene is for example recrystallized with a sulfur oxide chloride.Type: GrantFiled: October 29, 1982Date of Patent: March 20, 1984Assignee: Hoechst AktiengesellschaftInventor: Hans-Peter Rieck
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Patent number: 4431619Abstract: Process for the production of phosphazo polymers by thermal polymerization of a cyclic compound of the formula (NPCl.sub.2).sub.n in which n is an integer from 3 to 10 in the presence of a catalyst of the general formula R-O-SO.sub.2 -R.sup.1.Type: GrantFiled: October 8, 1982Date of Patent: February 14, 1984Assignee: Akzo NVInventors: Joachim Behnke, Dieter Huff
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Patent number: 4409195Abstract: A process is disclosed for the purification of trichlorosilane and other silicon source materials. Trace impurities of boron and phosphorous are removed from trichlorosilane or dichlorosilane by reacting small amounts of oxygen with the trichlorosilane or dichlorosilane at a temperature between about 60.degree. C. and 300.degree. C. The oxygen reacts with the Si--H bond in HSiCl.sub.3 or H.sub.2 SiCl.sub.2 to form a "SiOH" species which in turn complexes impurities such as BCl.sub.3 or PCl.sub.3 present in the chlorosilane. Purification of the chlorosilane is then easily accomplished during a subsequent distillation step which separates the purified chlorosilane from the less volatile complexed boron or phosphorous compounds.Type: GrantFiled: August 19, 1982Date of Patent: October 11, 1983Assignee: Motorola, Inc.Inventors: Robert D. Darnell, William M. Ingle
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Patent number: 4402926Abstract: A process is disclosed for producing chlorinated trisodium phosphate, comprising:(a) producing a hot sodium phosphate liquor, preferably with an overall Na/P mole ratio from 2.60 to 2.85;(b) adding sodium hypochlorite solution, preferably with an available chlorine content greater than 14%;(c) mixing the components, preferably from 70.degree. C. to 80.degree. C., only long enough to form a true solution;(d) cooling the melt by evaporative cooling under reduced pressure to form crystalline chlorinated trisodium phosphate;(e) air drying the product, if necessary, below about 40.degree. C.Type: GrantFiled: September 28, 1981Date of Patent: September 6, 1983Assignee: Monsanto CompanyInventor: Chung Y. Shen
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Patent number: 4386020Abstract: The present invention provides a process for the production of solid ion ductor materials (electrolytes) based on lithium or sodium compounds which stand in thermodynamic equilibrium with their alkali metal and have a high decomposition voltage, wherein two or more binary lithium or sodium compounds with an anion which is formed from one or more elements of the group consisting of nitrogen, phosphorus, arsenic, oxygen, sulphur, selenium, tellurium, hydrogen, fluorine, chlorine, bromine and iodine and which stand in thermodynamic equilibrium with their alkali metal are reacted together in such amounts and for such a period of time that a radiographically phase-pure product is formed.The present invention also provides ion conductor materials based on lithium or sodium compounds, which have the general formula:A.sub.3u+2v+w X.sub.u Y.sub.v Z.sub.Type: GrantFiled: May 1, 1980Date of Patent: May 31, 1983Assignee: Max Planck Gesellschaft zur Forderung der Wissenschaften E.V.Inventors: Peter Hartwig, Werner Weppner, Winfried Wichelhaus
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Patent number: 4382914Abstract: This invention provides a process for preparing cyclic phosphonitrilic chloride oligomers characterized by the combination of:(I) The first step of reacting phosphorus pentachloride with ammonium chloride in an inert organic solvent in the presence of a catalyst comprising at least one of (a) chlorides of bivalent metals and (b) organic acid salts of bivalent metals, and distilling off the solvent from the resulting reaction mixture to obtain a reaction product consisting essentially of cyclic phosphonitrilic chloride oligomers, and(II) the second step of contacting a solution of the reaction product in at least one solvent selected from the group consisting of aliphatic hydrocarbons and ethers with water at a temperature of about 40.degree. to about 100.degree. C.Type: GrantFiled: March 16, 1981Date of Patent: May 10, 1983Assignee: Nippon Fine Chemical Company, Ltd.Inventors: Kiyoshi Horie, Yoshiaki Morita, Yukio Mikamori, Masaharu Suzuki, Susumu Yano
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Patent number: 4377558Abstract: The present invention relates to novel polychlorophosphazenes and to the process for their preparation.These polychlorophosphazenes of the general formula:Cl.sub.2 (O) P [NPCl.sub.2 ].sub.n Clare prepared by the polycondensation of P trichloro-N dichlorophosphoryl-monophosphazene with the controlled release of POCl.sub.3 according to the equation: ##STR1## The novel polychlorophosphazenes so obtained are useful as antiflame materials, as coatings, as fertilizers, etc. . . .Type: GrantFiled: September 15, 1980Date of Patent: March 22, 1983Assignee: Institut Mondial du PhosphateInventors: Roger De Jaeger, Moncef Helioui, Emile Puskaric
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Patent number: 4374815Abstract: Linear phosphonitrilic chloride polymers are produced from linear phosphonitrilic chloride oligomers by means of a two-step process. In the first step a mixture of linear phosphonitrilic chloride oligomer having an average degree of polymerization of at least 4 is heated with an excess of ammonia or ammonium chloride. Cyclic phosphonitrilic chloride oligomer formed during the course of the first step is removed from the reaction mixture. After the removal of the cyclic oligomer the reaction mixture is subjected to the second step which involves heating the mixture in an inert liquid solvent (optionally in the presence of ammonia or ammonium chloride) whereby the molecular weight of the linear phosphonitrilic chloride polymer is increased.Type: GrantFiled: October 26, 1981Date of Patent: February 22, 1983Assignee: Ethyl CorporationInventor: Hsueh M. Li
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Patent number: 4374108Abstract: An alkali monofluorophosphate expressed by the formula M.sub.2 PO.sub.3 F, where M represents Na or K, can readily be synthesized under a relatively mild reaction condition by making HF gas contact with powdery or fine granular M.sub.4 P.sub.2 O.sub.7 or M.sub.2 HPO.sub.4 placed in a reaction vessel and maintained at a temperature in the range from about 200.degree. C. to about 450.degree. C., and more preferably in the range of 280.degree.-360.degree. C. It is suitable to make HF gas continuously flow into and pass through the reaction vessel until the total quantity of HF flowed into the vessel amounts to 100 to 150% of the theoretical value for conversion of M.sub.4 P.sub.2 O.sub.7 or M.sub.2 HPO.sub.4 to M.sub.2 PO.sub.3 F.Type: GrantFiled: November 20, 1980Date of Patent: February 15, 1983Assignee: Central Glass Company, LimitedInventors: Yasuji Nakaso, Kyoji Tanaka, Hiromi Kawamoto
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Patent number: 4371509Abstract: The invention relates to a process for oxidizing organic phosphorus compounds of the general formula (I)R.sub.3-n PX.sub.n (I)in which R stands for an organic radical, X stands for halogen and n stands for 0, 1, 2 or 3, to obtain compounds of the general formula (II)R.sub.3-n P(O)X.sub.n (II)in which R, X and n have the meanings given above. To this end, chlorosulfonic acid is used as oxidant and the oxidation is effected in homogeneous liquid phase.Type: GrantFiled: September 8, 1981Date of Patent: February 1, 1983Assignee: Hoechst AktiengesellschaftInventor: Jurgen Grosse
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Patent number: 4335085Abstract: The invention relates to a process for the preparation of highly pure phosphorus pentachloride in the form of a free-flowing crystalline powder by reaction of phosphorus trichloride with chlorine. The reaction is carried out in two stages. In the first stage, phosphorus trichloride is combined with 0.1 to 0.999 times the molar amount of chlorine at a temperature of 0.degree. to 150.degree. C., while stirring, and is thereby reacted to give a crystal sludge comprising phosphorus pentachloride and phosphorus trichloride. In the second stage, this sludge is allowed to react with an excess of chlorine at 0.degree. to 150.degree. C. to give phosphorus pentachloride.Type: GrantFiled: March 2, 1981Date of Patent: June 15, 1982Assignee: Hoechst AktiengesellschaftInventors: Hans-Peter Rieck, Jurgen Russow