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United States Patent 19 11 Patent Number: 5,691,436 Blount 45 Date of Patent: Nov

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United States Patent 19 11 Patent Number: 5,691,436 Blount 45 Date of Patent: Nov US005691436A United States Patent 19 11 Patent Number: 5,691,436 Blount 45 Date of Patent: Nov. 25, 1997 (54) PRODUCTION OF SILICON-PHOSPHORUS 56 References Cited CONTAINING COMPOSITIONS U.S. PATENT DOCUMENTS 76 Inventor: David H. Blount, 6728 Del Cerro Blvd., San Diego, Calif. 92120 4,389,530 6/1983 Arit et al. .............................. 55.6/404 4,523,009 6/1985 Neilson et al. ..................... 556,404X 21 Appl. No.:767,416 5,082,958 1/1992 Wright et al........................ 556,404X 5,563,285 10/1996 Blount .................................... 556/404 22 Filed: Dec. 16, 1996 Related U.S. Application Data Primary Examiner-Paul F. Shaver 63 Continuation-in-part of Ser. No. 680,651, Jul. 16, 1996, Pat. 57 ABSTRACT No. 5,693,840. A mixture of silicon and phosphorus are heated and reacted 51 Int. Cl. ............. C07F 7/08; CO7F 7/10 with halide to produce silicon tetrahalides, silicon 52 U.S. Cl. .......................... 528/26; 528/26.5; 528/27; 528/28; 528/29; 556/402; 556/404: 556/405; phosphorus halide and phosphorus trihalides compositions. 556/9; 556/12; 554/77; 554/75; 548/402; These compositions are reacted with any suitable organic, 548/403; 548/405; 548/406; 549/483; 549/505; inorganic-organic and/or inorganic compound to produce 540/486; 540/487 novel organic silicon-phosphorus containing compositions. 58 Field of Search ............................ 528/26, 25.5, 28, These compositions may be utilized as flame retardants, 528/27, 29; 556/402,404, 405, 9, 12:554/75, coating agents, adhesives and many other uses. 77; 548/402, 403, 405, 406; 549/483,505; 540/486, 487 21 Claims, No Drawings 5,691436 1. 2 PRODUCTION OF SILICON-PHOSPHORUS silicon-phosphorus containing compound thereby pro CONTAINING COMPOSITIONS ducing a resinous composition; then electively with F. basic salt forming compound; then electively with This application is a continuation-in-part of Pat. No. G. Water; then 08/680,651, filed Jul 16, 1996, now Pat. No. 5,693,848. 5 H. polymerize by any means that will complete the This invention concerns novel compositions containing polymerization to produce an organic silicon silicon and phosphorus atoms and their preparation and use. phosphorus containing resinous composition. These novel compounds may contain a plurality of silicon The sequence of the addition of the components A, B, C, atoms or a plurality of phosphorus atoms. These compounds D, E.F and G may be varied depending on the end product may be utilized as flame-retardants, insecticides, hydraulic 10 desired. In the production of silicon tetrahalide and phos fluid, adhesives, coating agents, polymers, plastics, and phorus halide reaction compounds, the halide may be many other uses. reacted separately with the silicon compound, and separately with the phosphorus compound then the silicon halide BACKGROUND reaction compounds are mixed with the phosphorus halide 15 reaction compounds. This mixture is then reacted with an The production of silicone compounds and organic phos organic compound, in an amount wherein halide atoms are phorus containing compounds are well known in the arts. left on the silicon and/or phosphorus atoms, to produce an The utilization of silicon-phosphorus and their halide reac organic silicon-phosphorus halide composition. This com tion products to produce novel silicon-phosphorus halide position is then reacted with more organic anior inorganic compounds and novel organic silicon-phosphorus 20 compounds to produce organic silicon-phosphorus contain compositions, polymers and products is new. The organic ing products. The silicon-phosphorus halide mixture may be silicon-phosphorus compounds and polymers have novel reacted with an amount of organic compound to produce and desirable properties which decrease flammability and organic silicon-phosphorus containing compounds, poly smoke production when these products are burned. These mers and products. compounds, polymers and products have many uses such as 25 In another process the silicon compound may be mixed reactants to produce novel compounds, polymers and with the phosphorus compound, then reacted with a halide plastics, as a flame-retardant in plastics, as a lubricant, as compound to produce a composition of silicon halide, phos hydraulic fluid, as an adhesive, as a coating agent, as a rust phorus halide and silicon-phosphorus halide which are then inhibitor, as building materials, foamed to produce insula reacted with an organic and/or inorganic compound. In tion and sound proofing and many other uses. The phospho 30 another method the halide compound is reacted with an rushalide are highly active compounds and will readily react organic compound, and then reacted with a mixture of with inorganic and organic compounds. The silicon halide silicon and phosphorus compounds to produce organic are not as active but their activity is greatly increased in the silicon-phosphorus containing compositions. In another presence of phosphorus halide and will react with phospho method the organic compound is reacted with halide com rus halide, organic phosphorus compounds and many inor 35 pounds to produce and organic halide, which is then reacted ganic and organic compounds. with a metal compound to produce a metal organic halide The object of this invention is to provide silicon (Grignard reagent). The metal organic halide compound is phosphorus halide compositions which are utilized to pro then reacted with the mixture of silicon tetrahalide and duce inorganic silicon-phosphorus halides, organic silicon phosphorus halide to produce organic silicon-phosphorus phosphorus halides compounds and polymers, organic containing compositions. In another method a metal is silicon-phosphorus compounds, polymers and products. reacted with an organic compound to produce a metal organic compound, which is then reacted with the reaction SUMMARY product of component A, B and C to produce and organic The invention comprises silicon-phosphorus compounds, silicon-phosphorus halide and/or an organic silicon silicon-phosphorus halides, silicon-phosphorus halides reac 45 phosphorus containing composition. In another method the tion compositions and their reaction products with organic silicon halide may be reacted with an organic compound to and/or inorganic compounds. Another aspect of the inven produce an organic trior di-chlorosilane compound, and the tion is a process to produce silicon-phosphorus halide and phosphorus halide may be reacted with an organic com the process to react these compounds with organic and/or pound to produce an organic phosphorus halide compound, inorganic compounds to produce organic silicon-phosphorus 50 then these compounds are mixed, and reacted with an halide and organic silicon-phosphorus containing composi organo-metal compound to produce organic silicon tions which utilize the following components: phosphorus containing compounds, polymers and products. A. silicon compound The organic silicon-phosphorus halide may be reacted with water and or basic salts to produce organic silicon B. phosphorus compound 55 phosphorus containing compounds, polymers and products. C. halide compound. The silicon tetrahalide, phosphorus trihalides and silicon Components A, B and C are reacted to produce silicon phosphorus halide compositions may also be produced by phosphorus halides compounds, silicon tetrahalide and mixing powdered silica, phosphorus or alkaline earth metal phosphorus trihalide, which are reacted with: phosphates and carbon or a metal such as magnesium, then D. organic compound in an amount to wherein there are heating the mixture to a high enough temperature in an halogen atoms and/or radical with active hydrogen or electric furnace to where the carbon combines with the metal left on the compound thereby producing an oxygen thereby producing a mixture of silicon-phosphorus, organic silicon-phosphorus containing compound; then phosphorus and silicon. An excess amount of halogen atoms reacted with or compounds are passed through this hot mixture thereby E. saturated or unsaturated organic compound, Grignard 65 producing a mixture containing silicon tetrahalide, silicon reagent and/or organio-metalic compound that will phosphorus halide and phosphorus halide. Phosphorus is react by condensation or addition with the organic commercially produced from a mixture of calcium 5,691436 3 4 phosphate, silica and carbon by heating the mixture. The COMPONENT C phosphorus is recovered by distillation. Silicon is commer cially produced from a mixture of silica and carbon. This Any suitable halide compound may be utilized in this mixture is heated in an electric furnace and the carbon reacts invention such as chlorine, fluorine, bromide and iodine and with the oxygen on the silica, and silicon and carbon dioxide mixtures thereof. Chlorine is the preferred halide compound. are produced. Carbonyl chloride (phosgene) may also be used. Hydrogen The phosphorus trihalide, silicon-phosphorus halide halide such as hydrogen chloride, hydrogen fluoride, hydro (Si-Phalides) and silicon tetrahalide may be modified by gen iodide and hydrogen bromide may also be utilized. the addition of water in the amount of 1-2 mols to one mol Organic halides may also be used such as alkyl halides. The of phosphorus trihalide to produce a silicon-phosphorus O phosphorus trihalides and phosphorus oxytrihalides may oxyhalides composition. This Si-Phalide mixture may also also be used to react with the heated silicon. be modified by the addition of phosphorus pentaoxide in the amount of about 1
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