- Preparation method of bis-[3-(triethoxy silicon)-propyl]-disulfide
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The invention discloses a preparation method of bis-[3-(triethoxy silicon)-propyl]-disulfide, relates to the technical field of silane coupling agent synthesis, and in particular relates to a preparation method of bis-[3-(triethoxy silicon)-propyl]-disulfide. The preparation method comprises the following steps: step 1, reacting potassium hydroxide with water to prepare a potassium hydroxide solution; step 2, adding potassium carbonate and powdered sulfur into the potassium hydroxide solution, and reacting to obtain a potassium disulfide solution; step 3, adding a phase transfer catalyst into the potassium disulfide solution, then dropwise adding 3-chloropropyltriethoxysilane, and carrying out a reaction so as to obtain bis-[3-(triethoxy silicon)-propyl]-disulfide; the molar ratio of the potassium hydroxide to the potassium carbonate to the sulfur powder to the 3-chloropropyltriethoxysilane is (1.2-1.5) : (0.3-0.6) :(1.2-1.8) : 1. The method has the positive effects of avoiding the generation of hydrogen sulfide gas, being simple in post-treatment, being green and environment-friendly, and improving economic benefits.
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Paragraph 0022-0059
(2021/06/09)
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- Double [propyl triethoxy silane] method for preparing disulfide
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The invention aims at providing a method for synthesizing bis [propyl triethoxysilane] disulfide under an aqueous phase condition free from a buffer. The method comprises the steps of A. carrying out reaction on a sodium polysulfide aqueous solution and chloropropyl triethoxysilane under an aqueous phase condition in presence of a phase transfer catalyst and a water-insoluble organic solvent to generate a reaction mixture; and B. separating bis [propyl triethoxysilane] disulfide from the reaction mixture, wherein the way of separating the product bis [propyl triethoxysilane] disulfide from the reaction mixture in the step B comprises the steps of a. separating an organic phase: separating an organic phase from the upper layer of the reaction mixture obtained from the step A, wherein the lower layer of the reaction mixture is an aqueous phase; and b. purifying the organic phase: distilling and purifying the organic phase to obtain the product bis [propyl triethoxysilane] disulfide. The method disclosed by the invention can improve yield, reduce generation of three wastes and relieve environmental protection pressure.
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Paragraph 0049-0050
(2016/10/20)
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- Sulfur-modified SBA-15 supported amorphous palladium with superior catalytic performance for aerobic oxidation of alcohols
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A series of sulfur-modified SBA-15 supported amorphous palladium catalysts are prepared, and the effects of preparation parameters on the aerobic oxidation of benzyl alcohol are systematically investigated. The optimal catalyst exhibits remarkably enhanced catalytic activity (conversion 100 % and selectivity 99 %) and could be separated conveniently. The catalysts are characterized by X-ray diffraction patterns, BET, ICP, X-ray photoelectron spectroscopy, CO chemisorption and transmitting electron microscopy, and the results show that disulfur bond framework in the optimal catalyst act as both a stable linker and a good chelator for Pd species. Pd2+ is reduced to Pd0 with the increasement of the carbon chain lengths between sulfur bonds, which is the cause of deactivation. The mechanism is that a base abstracts a proton from the coordinated alcohol to form a Pd alcoholate species that subsequently undergo b-hydride elimination to give benzyl aldehyde, which is confirmed by the catalytic and characteristic results. Springer Science+Business Media New York 2014.
- Liu, Kun,Chen, Zhaoxiang,Hou, Zhiqiang,Wang, Yuanyuan,Dai, Liyi
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p. 935 - 942
(2014/06/23)
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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 9-10
(2010/03/02)
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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 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 preparing organosilanes
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Preparation of organosilane compound (I) comprises reaction of (halo-organo) alkoxysilane compound (II) with sulfurizing agent (alkali hydrogensulfide, metal sulfide and/or metal polysulfide) and optionally in addition with sulfur or hydrogen sulfide in alcohol. Preparation of organosilane compound (I) of formula (Si (R) 2(R1O)(R2)-) nX m comprises reaction of (halo-organo)alkoxysilane compound (II) of formula (Si (R) 2(R1O)(R2)-Hal) with sulfurizing agent (alkali hydrogensulfide (3 wt.%), metal sulfide (Me 2S) and/or metal polysulfide (Me 2S g) (10 wt.%)) and optionally in addition with sulfur or hydrogen sulfide in alcohol. R : 1-8C-alkyl, 1-8C-alkenyl, 1-8C-aryl, 1-8C-aralkyl or OR1; R 1>1-24C-alkyl or alkenyl, aryl, aralkyl, H, alkylether O-(CR 3> 2)-O-alk, O-(CR 3> 2) y-O-alk or alkylpolyether O-(CR 3> 2O) y-alk or O- (CR 3> 2CR 3> 2-O) y-alk; y : 2-20; R 3>H or alkyl; alk : optionally saturated, linear, aliphatic and/or aromatic 1-30C-hydrocarbon; R 2>alk optionally substituted with halo, H, NH 2 or NHR 1>; either X : S; or X : SH; Hal : Cl, Br, F or I; Me : alkali metal, NH 4 or (alkaline earth metal) 1/2; and g : 1, 5-8 or 0. Provided that when n is 2 and m with an average sulfur chain length of 1.5-4.5, then X is S and when n is 1 and m is 1, then X is SH.
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Page/Page column 31; 32
(2008/06/13)
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- Process for preparing mercaptoorganyl alkoxy silanes
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Preparation of (mercaptoorganyl)alkoxysilanes (I) comprises reacting alkali metal sulfide with a mixture of (haloorganyl)alkoxysilane (II) and (haloorganyl)halosilane (III) in an alcohol with exclusion of air and at elevated pressure.
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Page/Page column 9; 10-11; 11; 11-12;
(2008/06/13)
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- Process for the preparation of (mercaptoorganyl)-alkoxysilanen
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Production of mercaptoorganyl alkoxysilanes comprises reacting an alkali metal hydrogen sulfide with a mixture of haloorganyl alkoxysilane and haloorganyl halosilane in an alcohol under pressure in a sealed vessel in the absence of oxygen.
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Page/Page column 11
(2008/06/13)
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- Process for the manufacture of blocked mercaptosilanes
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A process for the manufacture of a blocked mercaptosilane comprising: reacting at least one polysulfane-containing organosilicon compound of the general formula: (R13SiG)2Sn (a) in which each R1is independently methoxy, ethoxy or alkyl of from 1 to about 6 carbon atoms, provided, that at least one R1group is methoxy or ethoxy, G is an alkylene group of from 1 to about 12 carbon atoms and n is from 2 to about 8, with at least one alkali metal, alkaline earth metal or a basic derivative of an alkali metal or alkaline earth metal to provide the corresponding metal salt of the polysulfane-containing organosilicon compound and; (b) reacting the metal salt of the polysulfane-containing organosilicon compound with an acyl halide or carbonyl dihalide to provide a blocked mercaptosilane.
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Page column 9
(2010/02/08)
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- Method of making mercaptoalkylalkoxysilanes
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In a first embodiment of a process for making mercaptoalkylalkoxysilanes, a pH adjusting agent and a sulfide containing compound are mixed in an aqueous phase to provide a pH of 4-9, a phase transfer catalyst is added to the aqueous phase, a haloalkylalkoxysilane is then added to the aqueous phase to form a reaction mixture containing mercaptoalkylalkoxysilanes and water soluble byproducts, and the desired mercaptoalklyalkoxysilanes are separated from the water soluble byproducts. In an alternate embodiment, the haloalkylalkoxysilane, the phase transfer catalyst, and an anhydrous pH adjusting agent such as sulfur dioxide, carbon dioxide, hydrogen sulfide, phosphoric acid, boric acid, and hydrochloric acid, are mixed, then an aqueous solution of a sulfide containing compound is added to form a reaction mixture containing mercaptoalkylalkoxysilanes and water soluble byproducts, and desired mercaptoalklyalkoxysilanes are separated from water soluble byproducts.
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Page column 8
(2008/06/13)
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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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- Process for the preparation of organosilicon disulfide compounds
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The present invention relates to a process for the preparation of organo silicon disulfide compounds. The process involves reacting a mercaptoalkoxysilane with a sulfenamide compound.
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- Process for the preparation of organosilicon disulfide compounds
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The present invention relates to a process for the preparation of organo silicon disulfide compounds. The process involves reacting a mercaptoalkoxysilane with a dithiobis(benzothiazole) compound.
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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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