- ELECTRONIC SPECTRA AND ELECTRONIC STRUCTURE OF TRIALKOXYSILYLALKANETHIOLS
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The ultraviolet absorption spectra of solutions of trialkoxysilylalkanethiols (RO)3Si(CH2)nSH (R=CH3, C2H5; n=1, 2, 3) and also of CH3Si(OC2H5)3 and C2H5Si(OC2H5)2 in heptane and acetonitrile were obtained in the region of 4.0-5.3x106 m-1.Analysis of the obtained photoelectron spectra of the triorganosilylalkanethiols X3Si(CH2)nSH (X=CH3, OCH3; n=1, 3) showed that the first photo-ionization potentials of the trialkoxysilylalkanethiols are lower than the values for the corresponding methyl derivatives.This is due to the participation of the n electrons of the oxygen atom of the methoxyl groups in destabilization of the highest occupied molecular orbital.An empirical and quantumchemical interpretation of the obtained spectra is given.
- Ermakov, A. I.,Kirichenko, E. A.,Makrushin, N. A.,Vlasova, N. N.,Maroshina, M. Yu.,Voronkov, M. G.
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- Method for preparing mercaptosilane in virtue of thiourea process
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The invention relates to a method for preparing mercaptosilane in virtue of a thiourea process, belonging to the technical field of fine chemical engineering. The method comprises the following steps:dropwise adding an alcoholic solution of thiourea into chloropropyl siloxy silane and dodecyl trimethyl phosphorus bromide, carrying out a condensation reaction and an aging reaction, and conductingstanding for layering to obtain a mercaptosilane product. According to the invention, an isomerization reaction is inhibited by adjusting reaction conditions; the consumption of thiourea is reduced; ethylenediamine is used as a neutralization initiator, so solid by-products can be greatly reduced; and a guanidine salt state can be changed, so a crude product and a salt can be better separated, operation is simplified, and yield is improved.
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- Synthesis method of 3- mercaptopropyltrialkoxysilane (by machine translation)
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The, invention belongs, to the technical, field of coupling agent synthesis, 3 - and belongs to 10%-15% the technical field of coupling agent synthesis, 3 - 3 . (by machine translation)
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Paragraph 0045; 0050-0054; 0059-0063; 0067-0070
(2020/02/14)
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- Method for preparing mercaptosilane coupling agent by using phase transfer catalyst
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The invention discloses a method for preparing a mercaptosilane coupling agent by using a phase transfer catalyst. Sodium hydrosulfide and halogenated alkyl alkoxy silane are used as raw materials, and a hydrocarbon organic solvent is adopted as a protective agent. The method comprises the following steps: carrying out synthetic reaction on the sodium hydrosulfide in a water phase and the halogenated organosilane dissolved in the hydrocarbon organic solvent by utilizing a phase transfer catalyst, separating a reaction product organic layer after the synthetic reaction is finished, performing distillation to remove the hydrocarbon organic solvent, and carrying out reduced pressure filtration and distillation to obtain the mercaptosilane coupling agent. The synthesis reaction is relatively complete, the product quality is relatively high, the yield of the prepared mercaptosilane coupling agent is greater than or equal to 93%, and the purity is greater than or equal to 99%; the process issimple, the synthesis reaction process is easy to control, tail gas can be recycled, and the safety of organic synthesis reaction is enhanced; the reaction requires a low temperature, and low requirements on equipment; the hydrocarbon organic solvent is recyclable; and the manufacturing cost is low.
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Paragraph 0022-0024
(2019/12/02)
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- Preparation method of mercaptopropyl alkoxysilane
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The invention relates to a preparation method of mercaptopropyl alkoxysilane, and belongs to the field of organic fine chemical industry. The preparation method comprises the following steps: dissolving anhydrous sodium sulfide into an alcohol solvent, dropwise adding an acetic acid solution to convert the sodium sulfide solution into an alcohol solution of sodium hydrosulfide, and then reacting with chloropropyl alkoxysilane under the action of a phase transfer catalyst to produce the mercaptopropyl alkoxysilane, sodium chloride and sodium acetate; firstly primarily distilling an obtained crude product at low-temperature negative pressure to distill out the alcohol solvent and completely separate out the sodium chloride and sodium acetate, then performing filtering separation, and then rectifying an obtained filtrate to obtain a mercaptopropyl alkoxysilane product. The obtained mercaptopropyl alkoxysilane product has the content being higher than 99.0% and the yield being higher than95%; compared with other synthesis methods, the preparation method provided by the invention has the advantages of a high product content, a high yield, easy obtainment of raw materials, simple synthesis steps, no guanidinium salt byproducts, no use of a dangerous hydrogen sulfide raw material and the like.
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Paragraph 0013-0014; 0016-0018; 0019-0024; 0025-0027
(2018/06/15)
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- Method for synthesizing gamma-thiopropyl triethoxy silane by means of compound solvent and three-component catalyst
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The invention provides a method for synthesizing gamma-thiopropyl triethoxy silane by means of compound solvent and a three-component catalyst. The method comprises the steps that raw materials are prepared, wherein the weight ratio of gamma-chloropropyl triethoxy silane to anhydrous sodium hydrosulphide is 1 to 0.256-0.303, ethyl alcohol, butanone and dimethylformamide are adopted as the compound solvent, sodium iodide, tetramethyl guanidine and a sodium ethoxide ethanol solution are adopted as the three-component catalyst, and the weight percentage of sodium ethoxide in the sodium ethoxide ethanol solution is 18%-21%; gamma-chloropropyl triethoxy silane is dropwise added. According to the method, the purity of the prepared product is 99.51%-99.56%, the product yield is 95.1%-95.4%, the conversion rate of chloropropyl triethoxy silane is 98.2%-98.5%, the content of compounds such as hydrolysate, colloid and polymer polysiloxane is 0.3%-0.5%, and the reaction time is shortened by six hours compared with an existing technology.
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Paragraph 0090; 0091; 0092; 0093; 0094; 0095; 0096-0105
(2016/12/26)
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- Method for preparing mercaptosilane coupling agent by using channel reactor
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The invention provides a method for preparing a mercaptosilane coupling agent by using a channel reactor. In a solvent, a channel reactor is utilized to prepare the mercaptosilane coupling agent. The structural general formula of the mercaptosilane coupling agent is XmSiC3H6S(C=O)nY, wherein each X is independently alkyl group, alkoxy group, hydroxy group, R(OR')LO-, -ORO- or N(RO-)3, and at least one X is alkoxy group, hydroxy group or N(RO-)3; Y is hydrogen or alkyl group; R and R' are respectively independently straight-chain or branched-chain alkyl group; the average value of L is 1-30; m is 1, 2 or 3; and n is 0 or 1. The corrected diameter of the channel reactor channel is one micrometer to several centimeters; and the channel reactor is connected with an after-treatment device. The method solves the problems of long reaction period, poor stability, existence of impurity polymers and the like in the large-size reactor, and especially reduces the odor caused by the large-size reactor production.
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Paragraph 0055; 0056; 0057; 0058
(2016/11/17)
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- Process for the production of mercaptoalkylalkoxysilanes
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Mercaptoalkylalkoxysilane is obtained by reacting at least one sulfide of the general formula MHS wherein M is an alkali metal or ammonium with a haloalkyl silane in an aqueous reaction medium in the presence of an acidic gas to maintain the pH of the reaction medium at or below about 10, and in the additional presence of alkylguanidinium salt phase transfer catalyst to provide mercaptoalkylalkoxysilane, the alkylguanidinium salt phase transfer catalyst being represented by the general formula: wherein each of R1-5 is a primary alkyl radical and R6 is a primary alkyl or bis(primary alkylene) radical, or at least one of the R1–R2, R3–R4 and R5–R6 combinations with the respective connecting nitrogen atom forms a heterocyclic radical; X is an anion; and n is 1 or 2.
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Page/Page column 5
(2008/06/13)
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- Process for preparing mercaptoorganyl (alkoxysilanes)
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The present invention relates to a process for preparing mercaptoorganyl(alkoxysilanes), by hydrogenating bis(alkoxy-silylorganyl) polysulphides with hydrogen in the presence of at least one alcohol and a doped metal catalyst. The doped metal catalyst comprises at least one substance from the group consisting of iron, iron compound, nickel, nickel compound, palladium, palladium compound, osmium, osmium compound, ruthenium, ruthenium compound, rhodium, rhodium compound, iridium and iridium compound plus at least one doping component.
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Page/Page column 7-9
(2008/06/13)
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- Process for producing mercaptoorganyl (alkoxysilane)
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The invention concerns a process for producing mercaptoorganyl(alkoxysilanes), wherein bis(alkoxysilylorganyl)polysulfides are hydrogenated at temperatures of 2S.
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Page/Page column 8-10
(2008/06/13)
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- Process for the preparation of mercaptoorganyl (alkoxysilanes)
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The invention relates to a process for the preparation of mercaptoorganyl(alkoxysilanes), wherein bis(alkoxysilylorganyl)polysulfides are hydrogenated with hydrogen and a transition metal catalyst in a solvent without the addition of alcohols, H2S or water.
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Page/Page column 9-12
(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 7-9
(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 10-11
(2008/06/13)
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- Method of producing silylalkylthiols
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Silylalkylthiols are produced by reacting silylalkylsulfanylsilanes with water. The silylalkylsulfanylsilanes used as starting products can be produced by reacting bil-silylalkylpolysulfanes or bis-silylalkyldisulfanes with alkali metal and chlorosilanes.
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- Process for the preparation of mercaptosilanes
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Mercaptosilanes are prepared from haloorganylsilyl compounds and an alkali metal hydrogen sulfide in the presence of a polar, aprotic medium.
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- Synthesis of mercapto-substituted silicon compounds
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This invention relates to a method of reducing β-cyanoethyltrialkoxysilane to the corresponding mercaptopropyltrialkoxysilane by reaction with sulfur.
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