- Catalysis of triethoxysilane disproportionation with oligoethylene glycol ethers
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Oligoethylene glycol ethers catalyze the disproportionation of triethoxysilane to tetraethoxysilane and silane both at room temperature and upon heating. For comparison, the CsF-catalyzed disproportionation of triethoxysilane has been examined and found m
- Parshina, Lidiya N.,Oparina, Lyudmila A.,Khil'ko, Marina Ya.,Trofimov, Boris A.
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Read Online
- Mechanochemical method of producing triethoxysilane
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A mechanochemical method for synthesis of triethoxysilane from silicon-copper contact mass and ethyl alcohol in the developed vibration reactor is presented. It is shown that the process of a direct alkoxysilane synthesis in the vibro-boiling layer is affected by a series of control parameters such as the ratio between the contact mass and the mass of grinding bodies, the grinding body sizes and their ratios in a polydisperse mixture, power density. Optimization of these parameters allowed us to obtain HSi(OEt)3 with a selectivity of 50% at a silicon conversion of 90% without the use of promoters.
- Temnikov,Anisimov,Chistovalov,Zhemchugov,Kholodkov,Zimovets,Vysochinskaya, Yu. S.,Muzafarova
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Read Online
- Method for removing methyldichlorosilane and silicon tetrachloride impurities in trimethyl chlorosilane
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The invention relates to a method for removing methyldichlorosilane and silicon tetrachloride impurities in trimethyl chlorosilane, which comprises a hydrosilylation reaction, a partial esterification reaction and a complete esterification reaction. Firstly, a mixture of trimethylsilyl chloride containing methyldichlorosilane and silicon tetrachloride impurities is added to a reactor for hydrosilylation reaction, and the reaction product enters a separation system. The silicon tetrachloride in the mixture is partially esterified and reacted by adding the low-carbon alcohol as an esterifying agent, and the reaction product enters a separation system. Finally, the partially esterified product is further fully esterified to valuable tetraalkoxy silicon products. The high-efficiency recycling of trimethylchlorosilane is realized, and high-value utilization is also realized.
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Paragraph 0037-0038; 0045-0046; 0050-0052; 0064; 0079; ...
(2021/08/25)
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- Sustainable Catalytic Synthesis of Diethyl Carbonate
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New sustainable approaches should be developed to overcome equilibrium limitation of dialkyl carbonate synthesis from CO2 and alcohols. Using tetraethyl orthosilicate (TEOS) and CO2 with Zr catalysts, we report the first example of sustainable catalytic synthesis of diethyl carbonate (DEC). The disiloxane byproduct can be reverted to TEOS. Under the same conditions, DEC can be synthesized using a wide range of alkoxysilane substrates by investigating the effects of the number of ethoxy substituent in alkoxysilane substrates, alkyl chain, and unsaturated moiety on the fundamental property of this reaction. Mechanistic insights obtained by kinetic studies, labeling experiments, and spectroscopic investigations reveal that DEC is generated via nucleophilic ethoxylation of a CO2-inserted Zr catalyst and catalyst regeneration by TEOS. The unprecedented transformation offers a new approach toward a cleaner route for DEC synthesis using recyclable alkoxysilane.
- Putro, Wahyu S.,Ikeda, Akira,Shigeyasu, Shinji,Hamura, Satoshi,Matsumoto, Seiji,Lee, Vladimir Ya.,Choi, Jun-Chul,Fukaya, Norihisa
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p. 842 - 846
(2020/12/07)
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- Method for preparing organosilane by utilizing organosilicone byproduct
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The invention relates to the technical field of production of organic silicon by-products. The invention aims to solve the problems of high cost, more three wastes and continuous production of byproducts in the traditional organic silicon byproduct treatment process. The method comprises the following steps: adding the organic silicon by-product into a nitrogen-protected glass lining reaction kettle with a tower, adding a catalyst, dropwise adding alcohol to the bottom of the glass lining reaction kettle, carrying out a heating reaction under a stirring condition, neutralizing the obtained material, and rectifying the neutralized material to obtain the organic silane. According to the method, the multi-component organic silicon by-products trichlorosilane and silicon tetrachloride react and are converted into the same product, the high-purity product can be obtained only through simple rectification and purification, the process is simple, the treatment cost is low, and the product hasgood economic value.
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Paragraph 0021-0023; 0025-0026
(2020/07/13)
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- METHOD FOR PRODUCING TETRAALKOXYSILANE
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An object of the present invention is to provide a method capable of producing a tetraalkoxysilane with a high energy efficiency and with a high yield. The present invention provides a method for producing a tetraalkoxysilane, the method including: a first step of reacting an alcohol with a silicon oxide; and a second step of bringing a vaporized component of the reaction mixture obtained in the first step into contact with a molecular sieve.
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Paragraph 0055; 0056-0061; 0062; 0063-0066; 0069-0073
(2020/12/01)
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- Alkoxy metal powder as well as preparation method and application thereof
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The invention relates to a preparation method and an application of alkoxy metal powder, which are applied to preparation of an alkoxy metal carrier of an olefin polymerization catalyst. The alkoxy metal carrier comprises the following components: metal halide, sodium alcoholate or potassium alcoholate, or a solvent. The molar ratio of the components for preparing the alkoxy metal compound is as follows: metal halide: sodium alcoholate or potassium alcoholate = 1:(0.001-30); wherein the metal halide is a metal chloride, a metal bromide, a metal fluoride or a metal iodide; the metal is a main group metal, a sub-group metal or a VIII group metal. The catalyst prepared from the carrier is used for preparing an olefin polymerization catalyst, and has the advantages of high catalyst activity, good hydrogen regulation performance, good copolymerization performance, low polymer powder content, low wax content and good particle morphology; the catalyst is used for ethylene homopolymerization,ethylene and alpha-olefin copolymerization or ethylene and polar alkene monomer copolymerization, propylene homopolymerization, propylene and alpha-olefin copolymerization, or propylene and polar alkene monomer copolymerization.
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Paragraph 0075-0076
(2019/12/02)
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- Nucleophile induced ligand rearrangement reactions of alkoxy- and arylsilanes
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The ligand-redistribution reactions of aryl- and alkoxy-hydrosilanes can potentially cause the formation of gaseous hydrosilanes, which are flammable and pyrophoric. The ability of generic nucleophiles to initiate the ligand-redistribution reaction of commonly used hydrosilane reagents was investigated, alongside methods to hinder and halt the formation of hazardous hydrosilanes. Our results show that the ligand-redistribution reaction can be completely inhibited by common electrophiles and first-row transition metal pre-catalysts.
- Docherty, Jamie H.,Dominey, Andrew P.,Thomas, Stephen P.
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p. 3330 - 3335
(2019/05/10)
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- Method for continuous production of tetraalkoxysilane
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The present invention relates to a method for continuously manufacturing tetraalkoxysilanes by direction reaction of silicon metal and alcohol. According to the present invention, a basic catalyst is applied to a process without a solvent. Therefore, a distribution ratio of the catalyst is increased in the process, and generation of impurities caused by decomposition of the solvent can be minimized. Compared to existing direction reaction, reaction efficiency is improved and a purification process is simplified. Accordingly, tetraalkoxysilanes can be cost effectively manufactured compared to the prior art.(19) Reuse(AA) Si (particle)COPYRIGHT KIPO 2020
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Paragraph 0169-0180
(2020/03/25)
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- Dipyrromethene and β-Diketiminate Zinc Hydride Complexes: Resemblances and Differences
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A new dipyrromethene (DPM) ligand with bulky DIPP-substituents is introduced (DIPP = 2,6-diisopropylphenyl). The ligand, abbreviated as DIPPDPM, was deprotonated with ZnEt2 to give (DIPPDPM)ZnEt, which reacted with I2 to form (DIPPDPM)ZnI. Reaction of the latter with K[N(iPr)HBH3] afforded a labile Zn amidoborane complex which, after β-hydride elimination, formed (DIPPDPM)ZnH. Crystal structures of (DIPPDPM)ZnX (X = Et, I, H) revealed their monomeric nature. The Zn-N bond distances are somewhat longer than those in the corresponding monomeric β-diketiminate complexes (DIPPBDI)ZnX (DIPPBDI = CH[C(Me)N-DIPP]2). This is in agreement with calculated NPA charges, which are lower on the N atoms of DPM compared to those on BDI. Reaction of (DIPPDPM)ZnH with CO2 gave (DIPPDPM)Zn(O2CH), which crystallized as a monomer with a symmetrically bound η2-formate ligand. In contrast, the β-diketiminate complex crystallizes as a dimer [(DIPPBDI)Zn(O2CH)]2 with bridging formate ligands. Reaction of (DIPPDPM)Zn(O2CH) with various silanes regenerated the hydride complex (DIPPDPM)ZnH. Catalytic CO2 hydrosilylation with (EtO)3SiH using (DIPPDPM)ZnH as a catalyst gave full reduction to [Si]-OMe species, whereas the catalyst (DIPPBDI)ZnH only partially reduced CO2 to [Si]-OC(O)H. The advantage of the DIPPDPM ligand is the arrangement of the DIPP-substituents, which form a pocket around the Zn-X unit, preventing dimerization and influencing its reactivity. In addition, in contrast to the negatively charged central backbone carbon in the DIPPBDI ligand, that in DIPPDPM is neutral. This makes it less nucleophilic and Br?nsted basic, as expected for a true spectator ligand.
- Ballmann, Gerd,Grams, Samuel,Elsen, Holger,Harder, Sjoerd
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supporting information
p. 2824 - 2833
(2019/08/12)
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- Synthesis of Polycyclic and Cage Siloxanes by Hydrolysis and Intramolecular Condensation of Alkoxysilylated Cyclosiloxanes
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The controlled synthesis of oligosiloxanes with well-defined structures is important for the bottom-up design of siloxane-based nanomaterials. This work reports the synthesis of various polycyclic and cage siloxanes by the hydrolysis and intramolecular condensation of monocyclic tetra- and hexasiloxanes functionalized with various alkoxysilyl groups. An investigation of monoalkoxysilylated cyclosiloxanes revealed that intramolecular condensation occurred preferentially between adjacent alkoxysilyl groups to form new tetrasiloxane rings. The study of dialkoxy- and trialkoxysilylated cyclotetrasiloxanes revealed multistep intramolecular condensation reactions to form cubic octasiloxanes in relatively high yields. Unlike conventional methods starting from organosilane monomers, intramolecular condensation enables the introduction of different organic substituents in controlled arrangements. So-called Janus cubes have been successfully obtained, that is, Ph4R4Si8O12, in which R=Me, OSiMe3, and OSiMe2Vi (Vi=vinyl). These findings will enable the creation of siloxane-based materials with diverse functions.
- Sugiyama, Tomoaki,Shiba, Hiroya,Yoshikawa, Masashi,Wada, Hiroaki,Shimojima, Atsushi,Kuroda, Kazuyuki
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p. 2764 - 2772
(2019/02/01)
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- Manganese-Catalyzed Hydrofunctionalization of Alkenes
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The manganese-catalyzed hydrosilylation and hydroboration of alkenes has been developed using a single manganese(II) precatalyst and reaction protocol. Both reactions proceed with excellent control of regioselectivity and in high yields across a variety of sterically and electronically differentiated substrates (25 examples). Alkoxide activation, using NaOtBu, was key to precatalyst activation and reactivity. Catalysis was achieved across various functional groups and on gram-scale for both the developed methodologies with catalysts loadings as low as 0.5 mol %.
- Carney, Jonathan R.,Dillon, Barry R.,Campbell, Leonie,Thomas, Stephen P.
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p. 10620 - 10624
(2018/07/31)
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- Mechanochemistry-a new powerful green approach to the direct synthesis of alkoxysilanes
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The present work shows a new one-stage mechanochemical method for the direct synthesis of alkoxysilanes by silicon mechanoactivation followed by a reaction with an alcohol. Alkoxysilanes were obtained with nearly complete silicon and alcohol conversion. This method allows for a considerable simplification of the traditional multistage process by eliminating three stages that include silicon and catalyst preparation, and adapts it to green chemistry requirements. Vibration milling removed the oxide film, and the mechanoactivation of the large silicon fraction (1000-2000 μm) occurs in the reactor working space. Abrasion of the reactor walls and grinding bodies made of brass results in a developed catalytic surface on silicon, as it has been proven by a set of physical analytical methods such as scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), powder X-ray diffraction (PXRD), and X-ray photoelectron spectroscopy (XPS).
- Temnikov, Maxim N.,Anisimov, Anton A.,Zhemchugov, Pavel V.,Kholodkov, Dmitry N.,Goloveshkin, Alexander S.,Naumkin, Alexander V.,Chistovalov, Sergey M.,Katsoulis, Dimitris,Muzafarov, Aziz M.
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supporting information
p. 1962 - 1969
(2018/05/23)
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- Method for preparing ethyl orthosilicate in high yield
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The present invention relates to a method for preparing ethyl orthosilicate in a high yield. The method comprises the steps of: (1) adding 0.5 to 10 parts by mole of an inert solvent to a reactor witha cooling reflux device; (2) simultaneously injecting 1 part by mole of silicon tetrachloride and 4 to 4.5 parts by mole of absolute ethanol into the reactor respectively from two undersurface feeding ports of the reactor, and controlling the feeding rate to complete the feeding simultaneously; (3) heating the reactor to reflux, and continuing the reaction under reflux conditions for 30-120 minutes; (4) neutralizing the reaction solution in the reactor with a sodium ethoxide-ethanol solution with a mass ratio of 1% to 10% until the reaction solution is neutral; and (5) rectifying the neutralized reaction solution, and separating products to obtain the ethyl orthosilicate and the solvent. The method for preparing the ethyl orthosilicate in the high yield has the advantages of high productyield, simple preparation method, mild reaction condition and the like.
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Paragraph 0004; 0025-0060
(2018/07/30)
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- Synthesis of a 12-membered cyclic siloxane possessing alkoxysilyl groups as a nanobuilding block and its use for preparation of gas permeable membranes
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A 12-membered cyclic siloxane possessing alkoxysilyl groups was synthesized as a nanobuilding block for siloxane-based materials by the alkoxysilylation of organometallasiloxane containing a 12-membered ring with Si-Me and Si-O- groups as the side groups. The cyclic structure was retained not only in the hydrolysis and condensation reactions (sol-gel process) of the alkoxysilyl groups but also in the xerogel and membrane preparation processes. The degree of condensation of the xerogel derived from the 12-membered ring siloxane was higher than that derived from alkoxysilane monomers, indicating that the alkoxysilylated cyclic oligosiloxane is useful for controlling siloxane networks. A membrane composed of the cyclic siloxane was prepared by coating the hydrolyzed solution onto a porous alumina tube for evaluating the gas permeation properties. The membrane showed a molecular sieving effect for H2/SF6.
- Yoshikawa, Masashi,Shiba, Hiroya,Kanezashi, Masakoto,Wada, Hiroaki,Shimojima, Atsushi,Tsuru, Toshinori,Kuroda, Kazuyuki
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p. 48683 - 48691
(2017/11/06)
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- Direct synthesis of tetraalkoxysilanes from silica and alcohols
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A new simple and efficient process for synthesizing tetraalkoxysilanes (TROS) directly from silica and alcohols was developed using molecular sieves as dehydrating agents. Using this method, a variety of TROS (R = ethoxy, n-propoxy, or n-butoxy) were obtained over 70% yields within 6 h. We also employed various natural silica sources in this process for practical applications.
- Fukaya, Norihisa,Choi, Seong Jib,Horikoshi, Toshio,Kataoka, Sho,Endo, Akira,Kumai, Hiroshi,Hasegawa, Minoru,Sato, Kazuhiko,Choi, Jun-Chul
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supporting information
p. 2224 - 2226
(2017/03/21)
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- Reaction of silicon with alcohols in autoclave
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A reaction of activated silicon with alcohols in an autoclave at 240—270 °C was studied. It was found that primary alcohols form tetraalkoxysilanes Si(OR)4 with high selectivity (up to 97%), while the secondary PriOH gave a mixture of compounds HSi(OPri)3, Si(OPri)4, HSi(OPri)2OSi(OPri)2H, HSi(OPri)2OSi(OPri)3, and Si(OPri)3OSi(OPri)3 with the predominance of trialkoxysilane (up to 67%). Carrying out the reaction under the indicated conditions has the advantage of experimental simplicity, reagent availability, high conversion of silicon, good isolated yields of products.
- Krylova,Egorov,Nefedov
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p. 260 - 266
(2017/07/11)
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- A method for preparing inorganic alkoxy silane
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The invention relates to a method for preparing inorganic alkoxy silanes. The method comprises the following steps of: adding different anhydrous alcohols or inorganic chlorosilanes serving as raw materials into the inorganic chlorosilanes or the anhydrous alcohols in a one-time charging mode or a batch charging mode or a continuous charging mode at the normal temperature of -80 DEG C; stirring at the temperature which is more than or equal to the charging temperature for 30 to 180 minutes; introducing ammonia until a system is alkaline; and filtering, washing, and distilling or distilling under reduced pressure to obtain various inorganic alkoxy silanes. According to the method, different inorganic chlorosilanes react with different anhydrous alcohols, so that various inorganic alkoxy silanes can be obtained. The method can be used for preparing various inorganic alkoxy silanes, ammonium chloride can be used as a fertilizer, ethanol can be recycled, and the integral production process is safe, environment-friendly and economic.
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Paragraph 0018; 0019
(2017/04/03)
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- Preparation technology of ethyl silicate
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The invention relates to a preparation technology of ethyl silicate. The preparation technology comprises the following steps: (1) adding a metered silicon tetrachloride crude product and an active metal catalyst in a reaction kettle, and adding an ethanol solution in a head tank; (2) gradually dropwise adding ethanol in the reaction kettle under a certain vacuum degree, reacting rapidly after dropwise adding, regulating and controlling reaction speed by controlling the amount of the ethanol added dropwise, slowly heating up the reaction kettle and refluxing after the ethanol is added completely, absorbing HCl generated during reaction with water to prepare by-product hydrochloric acid, refluxing for about 0.5-1 hour, and then heating up and steaming out the unreacted ethanol; and (3) cooling down to room temperature after reaction is finished, decolorizing by using activated carbon, distilling to remove the ethanol, and collecting fraction at the temperature of 160-180 DEG C. According to the preparation technology of ethyl silicate, the silicon tetrachloride crude product is utilized effectively, environmental pollution is avoided, clean production is realized, production cost is reduced, yield is improved, and economic benefit and social benefit are significant.
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Paragraph 0017
(2016/10/09)
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- Bis(acetylacetonato)Ni(II)/NaBHEt3-catalyzed hydrosilylation of 1,3-dienes, alkenes and alkynes
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The utility of commercially available Ni(II) salts, Ni(acac)2 (acac = acetylacetonato) (1a) and its derivatives bis(hexafluoroacetylacetonato)nickel(II) (1b) and bis(2,2,6,6-tetramethyl-3,5-heptanedionato)nickel(II) (1c) as versatile hydrosilylation catalyst precursors is described. Complexes 1a-c catalyze 1,4-selective hydrosilylation of 1,3-dienes in the presence of NaBHEt3 at ambient temperature. The reactions exhibit good regioselectivity to give the branched isomers as major products. The catalytic system also catalyzes hydrosilylation of alkenes including industriary important siloxy-, amino-, and epoxy-substituted ones as well as both terminal and internal alkynes.
- Srinivas, Venu,Nakajima, Yumiko,Ando, Wataru,Sato, Kazuhiko,Shimada, Shigeru
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- SYNTHESIS METHOD OF ALKOXYSILANES
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The direct depolymerization of biogenic and other high surface area silica sources uses both simple and hindered diols to produce alkoxysilanes in one or two steps that can be separated and purified directly from the reaction mixture by distillation, extraction or filtration followed by solution modification and distillation or extraction. The alkoxysilanes can take the form of spirosiloxanes or simple alkoxysilanes or oligomers thereof. Thereafter they can be treated with acid to produce colloidal or precipitated silica or aerosolized and combusted to provide fumed silica without the intervention of SiCl4.
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Paragraph 0086; 0089
(2016/11/09)
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- Avoiding carbothermal reduction: Distillation of alkoxysilanes from biogenic, green, and sustainable sources
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The direct depolymerization of SiO2 to distillable alkoxysilanes has been explored repeatedly without success for 85 years as an alternative to carbothermal reduction (1900 °C) to Simet, followed by treatment with ROH. We report herein the base-catalyzed depolymerization of SiO2 with diols to form distillable spirocyclic alkoxysilanes and Si(OEt)4. Thus, 2-methyl-2,4-pentanediol, 2,2,4-trimethyl-1,3-pentanediol, or ethylene glycol (EGH2) react with silica sources, such as rice hull ash, in the presence of NaOH (10 %) to form H2O and distillable spirocyclic alkoxysilanes [bis(2-methyl-2,4-pentanediolato) silicate, bis(2,2,4-trimethyl-1,3-pentanediolato) silicate or Si(eg)2 polymer with 5-98 % conversion, as governed by surface area/crystallinity. Si(eg)2 or bis(2-methyl-2,4-pentanediolato) silicate reacted with EtOH and catalytic acid to give Si(OEt)4 in 60 % yield, thus providing inexpensive routes to high-purity precipitated or fumed silica and compounds with single Si-C bonds. No detours: The base-catalyzed depolymerization of SiO2 from different sources with diols led directly to distillable alkoxysilanes, including spirocyclic compounds, thus providing inexpensive routes to high-purity silica and compounds with single Si-C bonds (see scheme): The alkoxysilanes could be converted either into Si(OEt)4 by treatment with EtOH and a catalytic amount of acid or into high-purity precipitated (ppt) or fumed silica.
- Laine, Richard M.,Furgal, Joseph C.,Doan, Phi,Pan, David,Popova, Vera,Zhang, Xingwen
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supporting information
p. 1065 - 1069
(2016/01/20)
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- Dehydrogenative silylation of alcohols catalysed by half-sandwich iron N-heterocyclic carbene complexes
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A new series of tetramethylcyclopentadienyl-functionalised N-heterocyclic carbene complexes of iron bearing different wingtips of general type (Cp?-NHCR)Fe(CO)I (R = nBu, iBu, Et, CH2CH2OMe, CH2Ph) were prepared by direct reaction of Fe3(CO)12 and the corresponding imidazolium proligands. These new iron-NHC complexes have been found to be efficient catalysts for the dehydrogenative silylation of alcohols with silanes. Iron metal complexes bearing iso-butyl and n-butyl wingtips displayed slightly better catalytic performances than the related complexes (Cp?-NHCR)Fe(CO)I (R = Et, CH2CH2OMe, CH2Ph), affording quantitative yields of the corresponding silylethers in 8 h at 70 °C in acetonitrile.
- Cardoso, Jo?o M.S.,Lopes, Rita,Royo, Beatriz
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p. 173 - 177
(2015/02/19)
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- Amorphous silicon: New insights into an old material
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Amorphous silicon is synthesized by treating the tetrahalosilanes SiX4 (X=Cl, F) with molten sodium in high boiling polar and non-polar solvents such as diglyme or nonane to give a brown or a black solid showing different reactivities towards suitable reagents. With regards to their technical relevance, their stability towards oxygen, air, moisture, chlorine-containing reaction partners RCl (R=H, Cl, Me) and alcohols is investigated. In particular, reactions with methanol are a versatile tool to deliver important products. Besides tetramethoxysilane formation, methanolysis of silicon releases hydrogen gas under ambient conditions and is thus suitable for a decentralized hydrogen production; competitive insertion into the MeO-H versus the Me-OH bond either yields H- and/or methyl-substituted methoxy functional silanes. Moreover, compounds, such as MenSi(OMe)4-n (n=0-3) are simply accessible in more than 75% yield from thermolysis of, for example, tetramethoxysilane over molten sodium. Based on our systematic investigations we identified reaction conditions to produce the methoxysilanes MenSi(OMe)4-n in excellent (n=0:100%) to acceptable yields (n=1:51%; n=2:27%); the yield of HSi(OMe)3 is about 85%. Thus, the methoxysilanes formed might possibly open the door for future routes to silicon-based products. Amorphous silicon is easily synthesized from tetrahalosilanes SiX4 (X=Cl, F) and molten sodium in different solvents. Reactivity studies prove the resulting materials as versatile tools for the formation of technical important silanes, such as the silicon chloro-, alkoxy-, and methylalkoxy-substituted derivatives (see figure; bl=black, br=brown).
- Spomer, Natalie,Holl, Sven,Zherlitsyna, Larissa,Maysamy, Fariba,Frost, Andreas,Auner, Norbert
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p. 5600 - 5616
(2015/03/30)
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- Etyle Silicate Manufacture method
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The present invention relates to a manufacturing method of ethyl silicate. The manufacturing method may include the steps of: injecting, into a reactor, a mixture comprising silicon metal powder, potassium ethoxide, and ethyl silicate 40; stirring the mixture at 150-180anddeg;C at atmospheric pressure for 4-8 hours; synthesizing anhydrous ethanol with the mixture; transferring the synthesized ethyl silicate and non-reacted ethanol from the reactor to a condenser; storing the mixture condensed by the condenser in a storage tank and transferring the stored mixture to a distillation column; separating the ethyl silicate from ethanol through the distillation column; and accommodating the separated ethanol in storing means for reuse and accommodating the ethyl silicate in extracting means. The present invention does not have a catalyst process, which reduces the cost; and by using a fluid fluidized bed reactor, the ethyl silicate can be manufactured easily at atmospheric pressure and the time of contacting the metal becomes longer, increasing the yield.(40) Ethyl silicateCOPYRIGHT KIPO 2015
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Paragraph 0055; 0056
(2016/12/22)
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- The study of an alcoholysis reaction of silicon tetrafluoride with alcohols and magnesium to prepare tetraalkoxysilanes and magnesium fluoride
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An efficient alcoholysis reaction of silicon tetrafluoride with alcohols in the presence of magnesium can directly prepare tetraalkoxysilane and magnesium fluoride. The reaction can afford tetraethoxysilane, tetramethoxysilane, and magnesium fluoride in good yields with the aid of a catalytic amount of iodine.
- Zhang, Zongfan,Huang, Zhong,Tian, Qiang,Li, Yuye,Li, Xia,Liang, Xuesong,Du, Lusha
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p. 567 - 573
(2015/05/20)
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- Mononuclear Heteroscorpionate Zwitterionic Zinc Terminal Hydride: Synthesis, Reactivity, and Catalysis for Hydrosilylation of Aldehydes
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Treatment of heteroscorpionate zinc benzyloxy complex LZnOBn (1, L = (MePz)2CP(Ph)2NPh, MePz = 3,5-dimethylpyrazolyl) with phenylsilane (PhSiH3) gave a zinc hydride complex LZnH (2) containing a rare terminal hydride fragment. X-ray diffraction analysis and the DFT calculation confirm the zwitterionic structure of complex 2. The stoichiometric reaction of 2 with CS2 readily afforded a dithioformate complex LZnSCH(S) (3) of the C = S insertion into the Zn-H product. Moreover, complex 2 was an efficient catalyst for the hydrosilylation reaction of a series of silanes and aldehydes under mild conditions, featuring excellent functional group tolerance. The preliminary mechanistic study revealed that both zinc benzyloxy complex 1 and zinc hydride complex 2 were involved in the hydrosilylation process as the reaction intermediates. (Chemical Equation Presented).
- Mou, Zehuai,Xie, Hongyan,Wang, Meiyan,Liu, Na,Yao, Changguang,Li, Lei,Liu, Jingyao,Li, Shihui,Cui, Dongmei
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p. 3944 - 3949
(2015/09/01)
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- METHOD FOR PREPARING TRIALKOXYSILANE
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The present invention relates to a method for preparing SiH(OR3)-type trialkoxysilane (wherein, R is a C1-C3 methyl, ethyl, propyl or isopropyl group), and more specifically, the method comprises the steps of: preventing the oxidation of a silicon surface by pulverizing raw silicon material in a solvent environment without contact with the air so that the initial induction period of the direct synthesis of trialkoxysilane is dramatically reduced; and removing impurities from a reaction environment by continuously selecting a part of the solvent through a membrane filter provided in a reactor body.
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Paragraph 0062
(2014/07/23)
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- METHOD FOR PREPARING TRIALKOXYSILANE
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The present invention relates to a method for preparing SiH(OR3)-type trialkoxysilane (wherein, R is a C1-C3 methyl, ethyl, propyl or isopropyl group), and more specifically, the method comprises the steps of: preventing the oxidation of a silicon surface by pulverizing raw silicon material in a solvent environment without contact with the air so that the initial induction period of the direct synthesis of trialkoxysilane is dramatically reduced; and removing impurities from a reaction environment by continuously selecting a part of the solvent through a membrane filter provided in a reactor body.
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Paragraph 0100
(2015/01/06)
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- COSMETIC TREATMENT METHOD COMPRISING THE APPLICATION OF A COATING BASED ON AN AEROGEL COMPOSITION OF LOW BULK DENSITY
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The present invention relates to a cosmetic treatment method comprising the formation of a coating on keratin fibres characterized in that it comprises: 1) the preparation of an aerogel precursor composition comprising:—at least one organic solvent chosen from acetone, C1-C4 alcohols, C1-C6 alkanes, C1-C4 ethers, which may or may not be perfluorinated, and mixtures thereof and at least one precursor compound that contains:—at least one atom chosen from silicon, titanium, aluminium and zirconium,—at least one hydroxyl or alkoxy function directly attached to the atom chosen from silicon, titanium, aluminium and zirconium by an oxygen atom, and,—optionally an organic group directly attached to the atom chosen from silicon, titanium, aluminium and zirconium by a carbon atom, 2) the removal of the solvent or solvents resulting in the formation of an aerogel composition having a bulk density less than or equal to 0.35 g/cm3, 3) the application to the keratin fibres of the aerogel composition resulting from step 2) or of the aerogel precursor composition resulting from step 1). Advantageously, the molar ratio between the precursor compounds and the solvent is at most 1/20.
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Paragraph 0067
(2014/02/15)
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- Heterogeneous-gold-catalyzed acceptorless cross-dehydrogenative coupling of hydrosilanes and isocyanic acid generated in situ from urea
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Support structure: In the presence of gold nanoparticles supported on alumina (Au/Al2O3), various hydrosilanes can be converted into the corresponding silyl isocyanates using urea as an isocyanate source. The observed catalysis is truly heterogeneous, and the retrieved Au/Al 2O3 catalyst can be reused several times without any loss of its high catalytic performance. Copyright
- Taniguchi, Kento,Itagaki, Shintaro,Yamaguchi, Kazuya,Mizuno, Noritaka
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supporting information
p. 8420 - 8423
(2013/09/02)
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- Copper-catalyzed formic acid synthesis from CO2 with hydrosilanes and H2O
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A copper-catalyzed formic acid synthesis from CO2 with hydrosilanes has been accomplished. The Cu(OAc)2?H 2O-1,2-bis(diphenylphosphino)benzene system is highly effective for the formic acid synthesis under 1 atm of CO2. The TON value approached 8100 in 6 h. The reaction pathway was revealed by in situ NMR analysis and isotopic experiments.
- Motokura, Ken,Kashiwame, Daiki,Miyaji, Akimitsu,Baba, Toshihide
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experimental part
p. 2642 - 2645
(2012/08/13)
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- Mechanistic insights into the hydrosilylation of allyl compounds - Evidence for different coexisting reaction pathways
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The hydrosilylation of allyl compounds is often accompanied by the formation of high amounts of byproducts. The formation processes have not been fully understood so far. In this work, the allyl hydrosilylation mechanism is investigated in detail and experimental and theoretical evidence for multiple, coexisting reaction pathways is provided. Based on earlier reports and the observations during an extensive catalytic study, different pathways, leading to the observed byproducts, were identified and proven by labeling experiments and DFT calculations. Oxidative addition of the silane and the insertion of the allyl compound into the Pt-H bond turned out to be the crucial, selectivity-determining steps within the catalytic cycle. Based on these findings, it should be possible to systematically influence these steps and pave the way to a rational and straightforward design of more selective catalysts.
- Gigler, Peter,Drees, Markus,Riener, Korbinian,Bechlars, Bettina,Herrmann, Wolfgang A.,Kuehn, Fritz E.
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- MCM-41-immobilised bidentate nitrogen platinum complex: A highly efficient and recyclable phosphine-free catalytic system for the hydrosilylation of olefins
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An MCM-41-immobilised bidentate nitrogen platinum complex (MCM-41-2N-Pt) was very conveniently synthesised from commercially available and cheap 3-(2-aminoethylamino)propyltrimethoxysilane by immobilisation on the mesoporous silica nanoparticles, MCM-41, followed by reaction with potassium chloroplatinite. It was found that the MCM-41-2N-Pt complex is a highly efficient catalyst for the hydrosilylation of olefins with triethoxysilane and can be easily recovered and reused several times without significant loss of activity.
- Zhang, Hean,Liu, Jiaqin,Cheng, Shaojuan,Cai, Mingzhong
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experimental part
p. 241 - 243
(2012/09/08)
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- MCM-41-supported bidentate phosphine rhodium complex: An efficient and recyclable heterogeneous catalyst for the hydrosilylation of olefins
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MCM-41-supported bidentate phosphine rhodium complex (MCM-41-2P-RhCl 3) was conveniently synthesized from commercially available and cheapγ-aminopropyltriethoxysilane via immobilization on MCM-41, followed by reacting with diphenylphosphinomethanol and rhodium chloride. It was found that the title complex is a highly efficient catalyst for the hydrosilylation of olefins with triethoxysilane and can be recovered and recycled by a simple filtration of the reaction solution and used for at least 10 consecutive trials without any decreases in activity.
- Hu, Ronghua,Hao, Wenyan,Cai, Mingzhong
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experimental part
p. 1629 - 1634
(2012/01/13)
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- Effect of catalysts on the reaction of allyl esters with hydrosilanes
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The reaction of hydrosilylation of allyl esters XOCH 2CH=CH 2 (X = MeCO, CF 3CO, C 3F 7CO) and PhOCH 2CH=CH 2 with hydrosilanes HSiY 3 (Y = Cl, OEt) in the presence of the Speier catalyst, the Speier catalyst with additives, and of various nickel complexes was studied. The catalytic hydrosilylation reaction in the presence of the Speier catalyst is accompanied by the reduction. Additives to the Speier catalyst (vinyltriethoxysilane and some ethers) allow to suppress considerably the reduction reaction. In the presence of the studied nickel complexes mainly reduction and isomerization reactions occurred. The best nickel catalysts of hydrosilylation were the mixtures of NiCl 2 or Ni(acac) 2 with phosphine oxides. In contrast to allyl esters, the hydrosilylation of simple olefins proceeds easier, the content of the product of hydrosilylation in the reaction mixture reaches 94.3%. Pleiades Publishing, Ltd., 2010.
- Belyakova,Pomerantseva,Efimova,Chernyshev,Storozhenko
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experimental part
p. 728 - 733
(2011/01/05)
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- Steric parameters for substituents bound to atoms of silicon and some other elements of the third period
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The kinetics of a tetraethoxysilane reaction with n-butylmagnesium chloride, stoichiometrically monosolvated with isopropyl ether or with methyl tert-butyl ether, was studied in toluene. The pseudo-first-order rate constants determined at a great excess of Grignard reagent were used for separation of the appropriate equilibrium and rate constants. Equilibrium constants for five alkyl ether ligands at the magnesium center are in an excellent correlation with isosteric ES(Si) parameters. It was concluded that these constants should be applicable to all elements of the third period of the periodic table. Taylor & Francis Group, LLC.
- Ploom, Anu,Tuulmets, Ants,Jaerv, Jaak
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experimental part
p. 2503 - 2510
(2011/02/25)
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- Hydrosilylation of allyl glycidyl ether with triethoxysilane
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Hydrosilylation of allyl glycidyl ether with triethoxysilane in presence of Speier's catalyst leads to triethoxy(3-glycidoxypropyl)silane and triethoxy(2-glycidoxy-1-methylethyl)silane and is accompanied by isomerization of allyl glycidyl ether and cleavage of the oxirane ring and the ether bond. An effect of admixtures in allyl glycidyl ether on the process is revealed. Some other hydrosilylation catalysts and additives to Speier's catalyst are studied.
- Chernyshev,Belyakova,Knyazeva,Khromykh
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- Process for the direct synthesis of trialkoxysilane
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This invention discloses a process to improve reaction stability in the Direct Synthesis of trialkoxysilanes. The process is particularly effective in the Direct Synthesis of triethoxysilane and its higher alkyl cognates providing improved triethoxysilane yields.
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Page/Page column 19
(2008/06/13)
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- Hydrosilylation of cyclohexene and allyl chloride with trichloro-, dichloro(methyl)-, and chlorodimethylsilanes in the presence of Pt(0) complexes
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Hydrosilylation of cyclohexene and allyl chloride in the presence of Pt(0) complexes with tetramethyldivinyldisiloxane (Karstedt catalyst) and hexavinyldisiloxane was studied. It was shown that these catalysts are much more active in the hydrosilylation of cyclohexene with trichloro-, dichloro(methyl)-, and chlorodimethylsilane than the Pt(II)-containing Speier catalyst. In the hydrosilylation of allyl chloride in the presence of Pt(0) complexes, the ratio of the fraction of addition products to the fraction of reduction products increases from 5.7 (Speier catalyst) to 10-16. Quantum-chemical calculations showed that Pt(0) complexes are more active than Pt(II) complexes on the stage of formation of platinum silicon hydride complexes. Pleiades Publishing, Inc., 2006.
- Belyakova,Chernyshev,Storozhenko,Knyazev,Turkel'taub,Parshina,Kisin
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p. 925 - 930
(2008/02/03)
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- Hydrosilylation of ethylene
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Hydrosilylation of ethylene with trialkoxysilanes in the presence of Pt(0) complexes as catalysts affords ethyltrialkoxysilanes in almost quantitative yields. No impurities of vinyltrialkoxysilanes were detected. Experiments and ab initio calculations showed that the Pt(0) catalysts are considerably more active in ethylene hydrosilylation than Pt(II) catalysts. Pleiades Publishing, Inc., 2006.
- Chernyshev,Belyakova,Knyazev,Turkel'taub,Parshina,Serova,Storozhenko
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p. 225 - 228
(2008/02/08)
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- PROCESS FOR PRODUCTION OF TRIALKOXYHALOSILANES, PROCESS FOR PRODUCTION OF ALKOXY(DIALKYLAMINO)SILANES, CATALYSTS FOR (CO)POLYMERIZATION OF ALPHA-OLEFINS, CATALYST COMPONENTS THEREFOR, AND PROCESS ES FOR POLYMERIZATION OF ALPHA-OLEFINS WITH THE CATALYSTS
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A process for the production of trialkoxyhalosilanes which comprises reacting a tetrahalosilane [37] with a tetra- alkoxysilane [38] in the presence of an alcohol whose alkoxy group is the same as those of the tetraalkoxysilane to thereby obtain a trialkoxyhalosilane [39], characterized in that the alcohol is used in an amount of 5 to 50 % by mole based on the total amount of Si of the tetrahalosilane and the tetraalkoxysilane: SiX4 [37] (wherein X is halogeno) Si(OR1)4 [38] (wherein R1 is a hydrocarbon group having 1 to 6 carbon atoms) XSi(OR1)3 [39] (wherein X and R1 are each as defined above).
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Page/Page column 13
(2010/11/08)
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- Monosodiumoxyorganoalkoxysilanes: Synthesis and properties
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The reaction of organoalkoxysilanes with sodium hydroxide was studied in detail. Studies indicate that this reaction involves more than one stage and involves rather complex multistep process, which leads to the formation of both monosodiumoxyorganoalkoxysilanes (MSOAS) and several secondary products. Analysis of experimental evidence makes it possible to advance the mechanism behind this phenomenon and to define the optimum conditions for the preparation of pure MSOAS with high yields. Different MSOAS were synthesized and their basic physicochemical properties were studied. MSOAS are shown to constitute multifunctional reagents with chemically independent functional groups, and their reaction with trimethylchlorosilane selectively proceeds via - ONa groups, whereas their interaction with triethylesilanol and higher alcohols proceeds exclusively via - OAlk groups. Exchange interaction between MSOAS and organoalkoxysilanes via - ONa and - OAlk groups was found and studied in detail. Temperature corresponding to the onset of thermal degradation of MSOAS was estimated to be equal to ～ 180-190°C.
- Rebrov,Muzafarov
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p. 514 - 541
(2007/10/03)
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- 1,1-Dimethyl-1-(trialkoxysilylmethyl)hydrazinium and 1,1-dimethyl-1-(silatranylmethyl)hydrazinium Halides
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Formerly unknown 1,1-dimethyl-1-(trialkoxysilylmethyl)- and 1,1-dimethyl-1-(silatranylmethyl)hydrazinium halides were prepared by reaction of 1,1-dimethylhydrazine with (halomethyl)trialkoxysilanes XCH 2Si(OR)3 (X = Cl, I; R=Me, Et) and 1-(halomethyl)silatranes XCH2Si(OCH2CH2) 3N (X = Cl, Br). 1,1-Dimethyl-1-(silatranylmethyl)hydrazinium chloride and iodide were also obtained by transetherification of corresponding 1,1-dimethyl-1-(trimethoxysilylmethyl)hydrazinium halides with tris(2-hydroxyethyl)amine.
- Sorokin,Voronkov
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p. 862 - 866
(2007/10/03)
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- Process for making haloalkylalkoxysilanes
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A haloalkylalkoxysilane is prepared by reacting an olefinic halide with an alkoxysilane in which the alkoxy group(s) contain at least two carbon atoms in the presence of a catalytically effective amount of ruthenium-containing catalyst. The process can be used to prepare, inter alia, chloropropyltriethoxysilane which is a key intermediate in the manufacture of silane coupling agents.
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- Ion exchange purification of dielectric condensate precursor fluids and silicate esters such as tetraethylorthosilicate (TEOS)
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A method of removing inorganic contamination from dielectric condensate precursor fluids and silicate esters, such as tetraethylorthosilicate (TEOS), methyltriethoxyorthosilicate (MTEOS), hydrogen silsesquioxane (HSQ), methyl silsesquioxane (MSQ), polyarylene ether, benzocyclobutene (BCB), or OSG, includes obtaining a commercial grade fluid having up to 10,000 ppb individual metallic contaminants; converting the sodium form of one or more macroporous ion exchange resin beds to a hydrogen form; converting the chloride form of one or more macroporous ion exchange resin beds to a hydroxide form; drying the macroporous ion exchange resin beds to remove substantially all water from the ion exchange resin beds; passing fluids through the ion exchange resin beds one or more times by recirculating all or a portion of the fluid to obtain a purified fluid having less than 1 ppb of individual metallic contaminants, less than 10 ppb of boron contaminants, and less than 1 ppb of chloride contaminants; and collecting the purified fluid product within a container to prevent the subsequent addition of contaminants.
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Page column 5
(2008/06/13)
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- Process for producing an alkoxysilane
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The present invention provides a process for producing an alkoxysilane, safely and constantly in the commercial scale, from an inexpensive and readily available raw material, via a completely new reaction route, and in an energy-saving manner as well as under a low environmental load. The process of the present invention is a process comprising a reaction of an inorganic compound having Si—O bonds with an alcohol in the presence of an alkali metal element and/or an alkaline earth metal element.
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- Molecularly-imprinted material made by template-directed synthesis
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A method of making a molecularly imprinted porous structure makes use of a surfactant analog of the molecule to be imprinted that has the imprint molecule portion serving as the surfactant headgroup. The surfactant analog is allowed to self-assemble in a mixture to create at least one supramolecular structure having exposed imprint groups. The imprinted porous structure is formed by adding reactive monomers to the mixture and allowing the monomers to polymerize, with the supramolecular structure serving as a template. The resulting solid structure has a shape that is complementary to the shape of the supramolecular structure and has cavities that are the mirror image of the imprint group. Similarly, molecularly imprinted particles may be made by using the surfactant to create a water-in-oil microemulsion wherein the imprint groups are exposed to the water phase. When reactive monomers are allowed to polymerize in the water phase to form particles, the surface of the particles have cavities that are the mirror image of the imprint group.
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- Process for producing alkoxysilanes
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The present invention provides a process for producing an alkoxysilane, safely and constantly on a commercial scale, from an inexpensive and readily available raw material, via a completely new reaction route, and in an energy-saving manner as well as under a low environmental load. The process of the present invention is a process comprising the reaction of an inorganic compound having Si-O bonds with an alcohol in the presence of an alkali metal compound and/or an alkaline earth metal compound.
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- Catalyst for use in production of epoxide, method for producing the catalyst, and method for producing epoxide
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To provide an epoxide-production-use catalyst that is suitably used for producing an epoxide by partial oxidation of an unsaturated hydrocarbon, a catalyst in accordance with the present invention is obtained by fixing gold fine particles to a carrier containing an oxide containing at least one of titanium and zirconium, and has an acid quantity of not more than 0.1 mmol/g determined by the NH3-TPD method. Such a catalyst for epoxide producing use can be produced by, for instance, fixing gold fine particles to a carrier having an acid quantity of not more than 0.15 mmol/g. The catalyst for epoxide producing use arranged as above is preferably used as a catalyst in partial oxidation of an unsaturated hydrocarbon to produce a corresponding epoxide.
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