- Method for preparing silane coupling agent Si-69 in water phase
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The invention relates to a method for preparing a silane coupling agent Si-69 in a water phase, and relates to a preparation method of a compound. The problems that a traditional method for preparingthe silane coupling agent Si-69 is long in reaction time, low in product purity, expensive in raw material price, not easy to store, high in production cost, severe in raw material and product hydrolysis phenomenon, high in operation requirement, and not easy to control a process flow are solved. The method comprises the following steps of (1) preparing a buffer solution; (2) preparing a sodium sulfide solution; (3) synthesizing a polysulfide inorganic phase solution; (4) preparing a catalyst solution; (5) synthesizing the silane coupling agent Si-69; (6) filtering, separating, decoloring, impurity-removing, drying, and purifying the silane coupling agent Si-69. The method provided by the invention has the advantages of short reaction period, high product purity, easiness in storing raw materials, low price of the raw materials, easiness in getting the raw materials, simple operation flow, easiness in controlling process conditions, high yield, easiness in controlling average Sulphur content, and low production cost. The product prepared through the method provided by the invention is high in purity (99 percent or more), not hydrolyzed or sulfur-separated, and long in preservationtime.
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Paragraph 0024; 0025; 0026; 0030; 0034
(2018/07/30)
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- A four vulcanized double-(γ-propyl triethoxy silane) of the process for solvent process for synthesizing
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The invention relates to a solvent synthesis process for bis-(Y-triethoxypropylsilane) tetrasulfide, and belongs to the technical field of coupling agents. The bis-(Y-triethoxypropylsilane) tetrasulfide can be used for zero-angle tyres and other rubber products. The process comprises the following processing steps: adding sodium sulfide containing 9 crystal waters and powered sulfur of which the molar weight is 3.2 times that of the sodium sulfide into methylbenzene of which the weight is 2 times that of the sodium sulfide containing 9 crystal waters, heating for dehydration, cooling to below 50 DEG C, and adding Y-chloropropyl triethoxy of which the molar weight is 1.90 times that of the sodium sulfide and absolute ethyl alcohol in an amount which is equal to that of the methylbenzene; cooling a reaction product to room temperature after reaction, filtering the reaction product to remove inorganic salt and impurities, and flushing the inorganic salt and the impurities for many times by using a methylbenzene-ethanol mixed solution; transferring filtrate to a distillator, and performing distillation to obtain a bis-(Y-triethoxypropylsilane) tetrasulfide product (Si-69).
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Paragraph 0027-0030
(2017/03/14)
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- PROCESS FOR PREPARING ORGANOSILANES
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The invention relates to a process for preparing organosilanes of the general formula I by reacting (haloorganyl)alkoxysilane of the formula II with hydrous alkali metal hydrogensulphide, sulphur and alkali metal carbonate in alcohol, wherein the molar (haloorganyl)alkoxysilane of the formula II to alkali metal hydrogensulphide ratio is between 1:0.4 and 1:0.75, and the molar alkali metal hydrogensulphide to alkali metal carbonate ratio is between 1:0.5 and 1:1.5.
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Page/Page column 10
(2010/03/02)
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- PROCESS FOR PREPARING ORGANOSILANES
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The invention provides a process for preparing organosilanes of the general formula (I) wherein a) (haloorganyl)alkoxysilane of the formula (II) is reacted with a sulphurising reagent selected from the group of alkali metal hydrogensulphide, metal sulphide M2S, metal polysulphide M2Sg and any desired combinations thereof and optionally additionally with sulphur and/or with H2S in an organic solvent, b1) subsequently, the organic solvent is removed from the suspension which forms, and the liquid phase comprising the organosilane of the formula (I), and the solid phase comprising MX and residual organosilane of the formula (I), are separated from the remaining suspension, or b2) subsequently, the liquid phase comprising the organosilane of the formula (I) and the organic solvent, and the solid phase comprising MX and residual organosilane of the formula (I), are separated from the suspension which forms, and the organic solvent is removed from the liquid phase, c) the solid phase comprising MX and residual organosilane of the formula (I) is mixed with water and d) the organic phase which forms, comprising the organosilane of the general formula (I), is removed.
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Page/Page column 18
(2010/10/03)
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- Process for the preparation of organosilicon compounds
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A process for the preparation of an organosilicon compound of the formula (I) [in-line-formulae](R1R2R3SiR4)2Sx??(I) [/in-line-formulae]by reacting haloalkoxysilanes of the general formula (II) [in-line-formulae]R1R2R3SiR4X??(II) [/in-line-formulae]with a dry polysulphide of the general formula (III) [in-line-formulae]M2Sz??(III) [/in-line-formulae]and/or dry sulphide of the general formula IV [in-line-formulae]M2S??(IV) [/in-line-formulae]and optionally sulphur in an organic solvent, the organic solvent being removed from the resulting suspension, the mixture containing the organosilicon compound of the general formula (I) and the solid MX being mixed with water containing at least one buffer, and the resulting phases being separated.
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Page/Page column 3-4
(2008/06/13)
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- Preparation of sulfide chain-bearing organosilicon compounds
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By reacting a halogenoalkyl group-bearing organosilicon compound and optionally sulfur with an aqueous solution or water dispersion of an ammonium or alkali metal polysulfide or a hydrate thereof in the presence of a phase transfer catalyst, a sulfide chain-bearing organosilicon compound having the average compositional formula (2): [in-line-formulae](R1O)(3-p)(R2)pSi—R3—S—R3—Si(OR1)(3-p)(R2)p ??(2) [/in-line-formulae] wherein m has an average value of 2≦m≦6 is obtained in high yields and at a low cost with minimized formation of a monosulfide-bearing organosilicon compound.
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Page/Page column 4
(2008/06/13)
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- Preparation of sulfide chain-bearing organosilicon compounds
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By reacting a mixture of a halogenoalkyl group-bearing organosilicon compound and sulfur with an aqueous solution or water dispersion of an ammonium or alkali metal sulfide or a hydrate thereof in the presence of a phase transfer catalyst, a sulfide chain-bearing organosilicon compound having the average compositional formula (2): [in-line-formulae](R1O)(3-p)(R2)pSi—R3—Sm—R3—Si(OR1)(3-p)(R2)p??(2) [/in-line-formulae] wherein m has an average value of 2≦m≦6 is obtained in high yields and at a low cost with minimized formation of a monosulfide-bearing organosilicon compound.
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Page/Page column 4
(2008/06/13)
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- Process for the preparation of yellow bis (3-[triethoxysilyl] propyl) tetrasulfane
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Process for the preparation of yellow bis(3-[triethoxysilyl]propyl)tetrasulfane having an iodine color value of ≦10 mg of iodine/100 ml, in which process a small amount of chloropropyltrichlorosilane is added to neutral chloropropyltriethoxysilane and reaction with sodium polysulfide or with Na2S and sulfur in ethanol is then carried out.
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- Direct preparation of anhydrous sodium oligosulfides from metal sodium and elemental sulfur in aprotic organic media directed toward synthesis of silane coupling agent
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Anhydrous sodium oligosulfide was prepared by the heterogeneous reaction of metal sodium and elemental sulfur in aprotic solvents. The oligosulfide consisted of a mixture of several Na2Sn (n = 2 - 8). Organic oligosulfides (R2Sn, n ≥ 2) including moisture-sensitive one were synthesized by the reaction with organic halides in high yeilds under mild conditions.
- Yamada, Nobuo,Furukawa, Mutsuhisa,Nishi, Masayuki,Takata, Toshikazu
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p. 454 - 455
(2007/10/03)
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- Preparation of sulfur-containing organosilicon compounds
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The present invention relates to a process for the production of organosilicon compounds of the formula in which Z is selected from the group consisting of STR1 where R1 is an alkyl group of 1 to 4 carbon atoms, cyclohexyl or phenyl; R2 is alkoxy of 1 to 8 carbon atoms, or cycloalkoxy of 5 to 8 carbon atoms; Alk is a divalent hydrocarbon of 1 to 18 carbon atoms and n is an integer of 2 to 8; comprising reacting (A) a compound of the formula: when X is Cl, Br or I; with (B) a compound of the formula where Me is ammonium, or an alkali metal; wherein the reaction is conducted in the presence of a phase transfer catalyst and an aqueous phase.
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