- Unexpected disproportionation of tetramethylethylenediamine-supported perchlorodisilane Cl3SiSiCl3
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The addition compound Cl3SiSiCl3·TMEDA was formed quantitatively by treatment of Cl3SiSiCl3 with tetramethylethylenediamine (TMEDA) in pentane at room temperature. The crystal structure of Cl3SiSiCl3·TMEDA displays one tetrahedrally and one octahedrally bonded Si atom (monoclinic, P2 1/n). 29Si CP/MAS NMR spectroscopy confirms this structure. Density functional theory (DFT) calculations have shown that the structure of the meridional isomer of Cl3SiSiCl3· TMEDA is 6.3 kcal lower in energy than that of facial coordinate species. Dissolving of Cl3SiSiCl3·TMEDA in CH 2Cl2 resulted in an immediate reaction by which oligochlorosilanes SinCl2n (n = 4, 6, 8, 10; precipitate) and the Cl--complexed dianions [SinCl2n+2] 2- (n = 6, 8, 10, 12; CH2Cl2 extract) were formed. The constitutions of these compounds were confirmed by MALDI mass spectrometry. Additionally, single crystals of [Me3NCH 2CH2NMe2]2[Si6Cl 14] and [Me3NCH2CH2NMe 2]2[Si8Cl18] were obtained from the CH2Cl2 extract. We found that Cl3SiSiCl 3·TMEDA reacts with MeCl, forming MeSiCl3 and the products that had been formed in the reaction of Cl3SiSiCl 3·TMEDA with CH2Cl2. X-ray structure analysis indicates that the structures of [Me3NCH2CH 2NMe2]2[Si6Cl14] (monoclinic, P21/n) and [Me3NCH2CH 2NMe2]2[Si8Cl18] (monoclinic, P21/n) contain dianions adopting an "inverse sandwich" structure with inverse polarity and [Me3NCH 2CH2NMe2]+ as countercations. Single crystals of SiCl4·TMEDA (monoclinic, Cc) could be isolated by thermolysis reaction of Cl3SiSiCl3·TMEDA (50 °C) in tetrahydrofuran (THF).
- Tillmann, Jan,Meyer-Wegner, Frank,Nadj, Andor,Becker-Baldus, Johanna,Sinke, Tanja,Bolte, Michael,Holthausen, Max C.,Wagner, Matthias,Lerner, Hans-Wolfram
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Read Online
- METHOD FOR THE DEHYDROGENATION OF DICHLOROSILANE
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Dichlorosilane and trichlorosilane are dehydrogenated at elevated temperature in the presence of an ammonium or phosphonium salt as a catalyst, and a halogenated hydrocarbon or hydrogen halide. The method may be used to synthesize organochlorosilane.
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Paragraph 0091
(2021/06/22)
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- A General and Selective Synthesis of Methylmonochlorosilanes from Di-, Tri-, and Tetrachlorosilanes
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Direct catalytic transformation of chlorosilanes into organosilicon compounds remains challenging due to difficulty in cleaving the strong Si-Cl bond(s). We herein report the palladium-catalyzed cross-coupling reaction of chlorosilanes with organoaluminum reagents. A combination of [Pd(C3H5)Cl]2 and DavePhos ligand catalyzed the selective methylation of various dichlorosilanes 1, trichlorosilanes 5, and tetrachlorosilane 6 to give the corresponding monochlorosilanes.
- Naganawa, Yuki,Nakajima, Yumiko,Sakamoto, Kei
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supporting information
p. 601 - 606
(2021/01/13)
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- Method for preparing methylchlorosilanes
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The present invention relates to a method for producing methylchlorosilane by a direct synthesis method and, more specifically, to a method for preparing dimethyldichlorosilane with an improved output of methylchlorosilane (M2) and trimethylchlorosilane (M3). According to the present invention, the method for preparing methylchlorosilane comprises the step of reacting a contact composition including metal silicon, aluminum, a catalyst and a cocatalyst with methyl chloride, wherein the contact composition includes 0.1 to 0.2 parts by weight based on 100 parts by weight of metal silicon.(AA) MCS+ECM+Unreacted MC(BB) ECM+Unreacted MC(CC) FBR(MCS Reactor)(DD) ECM(By-product)(EE) Unreacted MCCOPYRIGHT KIPO 2021
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Paragraph 0040-0056
(2020/10/29)
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- Synthesis of Functional Monosilanes by Disilane Cleavage with Phosphonium Chlorides
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The Müller–Rochow direct process (DP) for the large-scale production of methylchlorosilanes MenSiCl4?n (n=1–3) generates a disilane residue (MenSi2Cl6?n, n=1–6, DPR) in thousands of tons annually. This report is on methylchlorodisilane cleavage reactions with use of phosphonium chlorides as the cleavage catalysts and reaction partners to preferably obtain bifunctional monosilanes MexSiHyClz (x=2, y=z=1; x,y=1, z=2; x=z=1, y=2). Product formation is controlled by the reaction temperature, the amount of phosphonium chloride employed, the choice of substituents at the phosphorus atom, and optionally by the presence of hydrogen chloride, dissolved in ethers, in the reaction mixture. Replacement of chloro by hydrido substituents at the disilane backbone strongly increases the overall efficiency of disilane cleavage, which allows nearly quantitative silane monomer formation under comparably moderate conditions. This efficient workup of the DPR thus not only increases the economic value of the DP, but also minimizes environmental pollution.
- Santowski, Tobias,Sturm, Alexander G.,Lewis, Kenrick M.,Felder, Thorsten,Holthausen, Max C.,Auner, Norbert
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supporting information
p. 3809 - 3815
(2019/02/13)
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- CLEAVAGE OF METHYLDISILANES, CARBODISILANES AND METHYLOLIGOSILANES WITH ALKALI-AND ALKALINE EARTH METAL SALTS
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The invention relates to a process for the manufacture of methylmonosilanes comprising the step of subjecting one or more methyldisilanes, one or more methyloligosilanes, one or more carbodisilanes, or mixtures thereof to cleavage conditions resulting in the cleavage of silicon- silicon bonds or silicon-carbon bonds in carbodisilanes, and optionally a step of separating the resulting methylmonosilanes.
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Page/Page column 55
(2019/04/16)
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- Disilane Cleavage with Selected Alkali and Alkaline Earth Metal Salts
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The industry-scale production of methylchloromonosilanes in the Müller–Rochow Direct Process is accompanied by the formation of a residue, the direct process residue (DPR), comprised of disilanes MenSi2Cl6-n (n=1–6). Great research efforts have been devoted to the recycling of these disilanes into monosilanes to allow reintroduction into the siloxane production chain. In this work, disilane cleavage by using alkali and alkaline earth metal salts is reported. The reaction with metal hydrides, in particular lithium hydride (LiH), leads to efficient reduction of chlorine containing disilanes but also induces disproportionation into mono- and oligosilanes. Alkali and alkaline earth chlorides, formed in the course of the reduction, specifically induce disproportionation of highly chlorinated disilanes, whereas highly methylated disilanes (n>3) remain unreacted. Nearly quantitative DPR conversion into monosilanes was achieved by using concentrated HCl/ether solutions in the presence of lithium chloride.
- Santowski, Tobias,Sturm, Alexander G.,Lewis, Kenrick M.,Felder, Thorsten,Holthausen, Max C.,Auner, Norbert
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supporting information
p. 13202 - 13207
(2019/10/22)
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- Neutral-Eosin-Y-Photocatalyzed Silane Chlorination Using Dichloromethane
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Chlorosilanes are versatile reagents in organic synthesis and material science. A mild pathway is now reported for the quantitative conversion of hydrosilanes to silyl chlorides under visible-light irradiation using neutral eosin Y as a hydrogen-atom-transfer photocatalyst and dichloromethane as a chlorinating agent. Stepwise chlorination of di- and trihydrosilanes was achieved in a highly selective fashion assisted by continuous-flow micro-tubing reactors. The ability to access silyl radicals using photocatalytic Si?H activation promoted by eosin Y offers new perspectives for the synthesis of valuable silicon reagents in a convenient and green manner.
- Fan, Xuanzi,Xiao, Pin,Jiao, Zeqing,Yang, Tingting,Dai, Xiaojuan,Xu, Wengang,Tan, Jin Da,Cui, Ganglong,Su, Hongmei,Fang, Weihai,Wu, Jie
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supporting information
p. 12580 - 12584
(2019/08/16)
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- PROCESS FOR THE PRODUCTION OF ORGANOHYDRIDOCHLOROSILANES FROM HYDRIDOSILANES
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The invention relates to a process for the manufacture of organomonosilanes bearing both hydrogen and chlorine substituents at the silicon atom by subjecting one or more organomonosilanes to the reaction with one or more di- or carbodisilanes in the presence of one or more compounds (C) acting as a redistribution catalyst, wherein at least one of the silanes has only hydrogen and organic residues at the silicon atoms.
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Page/Page column 40; 41; 42
(2019/04/16)
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- Exhaustively Trichlorosilylated C1 and C2 Building Blocks: Beyond the Müller-Rochow Direct Process
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The Cl--induced heterolysis of the Si-Si bond in Si2Cl6 generates an [SiCl3]- ion as reactive intermediate. When carried out in the presence of CCl4 or Cl2C=CCl2 (CH2Cl2 solutions, room temperature or below), the reaction furnishes the monocarbanion [C(SiCl3)3]- ([A]- 92%) or the vicinal dianion [(Cl3Si)2C-C(SiCl3)2]2- ([B]2- 85%) in excellent yields. Starting from [B]2-, the tetrasilylethane (Cl3Si)2(H)C-C(H)(SiCl3)2 (H2B) and the tetrasilylethene (Cl3Si)2C=C(SiCl3)2 (B; 96%) are readily available through protonation (CF3SO3H) or oxidation (CuCl2), respectively. Equimolar mixtures of H2B/[B]2- or B/[B]2- quantitatively produce 2 equiv of the monoanion [HB]- or the blue radical anion [B?]-, respectively. Treatment of B with Cl- ions in the presence of CuCl2 furnishes the disilylethyne Cl3SiC≡CSiCl3 (C; 80%); in the presence of [HMe3N]Cl, the trisilylethene (Cl3Si)2C=C(H)SiCl3 (D; 72%) is obtained. Alkyne C undergoes a [4+2]-cycloaddition reaction with 2,3-dimethyl-1,3-butadiene (CH2Cl2, 50 °C, 3d) and thus provides access to 1,2-bis(trichlorosilyl)-4,5-dimethylbenzene (E1; 80%) after oxidation with DDQ. The corresponding 1,2-bis(trichlorosilyl)-3,4,5,6-tetraphenylbenzene (E2; 83%) was prepared from C and 2,3,4,5-tetraphenyl-2,4-cyclopentadien-1-one under CO extrusion at elevated temperatures (CH2Cl2, 180 °C, 4 d). All closed-shell products were characterized by 1H, 13C{1H}, and 29Si NMR spectroscopy; an EPR spectrum of [nBu4N][B?] was recorded. The molecular structures of [nBu4N][A], [nBu4N]2[B], B, E1, and E2 were further confirmed by single-crystal X-ray diffraction. On the basis of detailed experimental investigations, augmented by quantum-chemical calculations, plausible reaction mechanisms for the formation of [A]-, [B]2-, C, and D are postulated.
- Georg, Isabelle,Teichmann, Julian,Bursch, Markus,Tillmann, Jan,Endeward, Burkhard,Bolte, Michael,Lerner, Hans-Wolfram,Grimme, Stefan,Wagner, Matthias
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supporting information
p. 9696 - 9708
(2018/07/21)
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- Technique and device for synthesizing methyl chlorosilane
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The invention provides a technique and device for synthesizing methyl chlorosilane. The method comprises the following steps: a sand bath temperature control device is started to increase the temperature in a stirred bed reactor to the preset temperature; the weighed silicon powder and catalyst are uniformly mixed and pressed into the stirred bed under the action of nitrogen through a charging device on the upper part of the stirred bed reactor, and a magnetic stirring device is started; methyl chloride in a methyl chloride storage tank is vaporized by a methyl chloride vaporizer and enters the sand bath temperature control device through a fluidized bed inlet flowmeter to control the methyl chloride inlet reaction flow rate; and the reaction product is condensed by the product condenser and collected from the lower part of a product collector, and the uncondensed gas enters a tail gas buffer tank to be collected, is absorbed by an NaOH solution tank and discharged to the outside. The reaction temperature, reaction pressure, methyl chloride quality, silicon powder quality, catalyst quality and other reaction conditions in the methyl chlorosilane production process have favorable evaluation effects, thereby greatly lowering the industrial plant adjustment risks and enhancing the production efficiency.
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Paragraph 0014; 0015; 0016
(2017/07/01)
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- Production method of chloropropylmethyldichlorosilane
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The invention relates to a production method of chloropropylmethyldichlorosilane and belongs to the field of organic chemistry. The production method comprises the following steps: firstly, enabling chloroplatinic acid to react with isopropanol, acetic acid, phenyl silicone oil and the like; secondly, neutralizing by adopting sodium acetate, enabling part of the isopropanol complexed with platinum to be completely substituted under the alkaline conditions, thereby enabling a ligand of a catalyst to be directly substituted with the acetic acid and the phenyl silicone oil; after substitution, by taking tributylamine as a promoter, avoiding the inactivation of the catalyst in the addition reaction; during synthesis, reacting by adopting mixed feeding, adding at low temperature, and raising the temperature for continuous reaction after most reaction is finished; after the reaction is finished, completely distilling low boiling point products at normal pressure, and then distilling foreshot under vacuum conditions; after the foreshot are distilled, obtaining a chloropropylmethyldichlorosilane product with the content of 99.5 percent or above. The synthesized product disclosed by the invention has the advantages of high yield, low capacity, fewer byproducts, low requirement on equipment, and the like; in addition, the production method is relatively-simple in industrial production.
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Paragraph 0015; 0016
(2017/02/17)
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- Porous (CuO)xZnO hollow spheres as efficient Rochow reaction catalysts
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Nowadays, how to achieve both high dimethyldichlorosilane selectivity and silicon conversion in the Rochow reaction still remains a major challenge in the organosilane industry, in which silicon and chloromethane are converted into methylchlorosilanes on Cu-based catalysts mixed with ZnO promoter. Therefore, this calls for the development of outstanding catalysts with both high activity and selectivity for the Rochow reaction and also for a deep fundamental understanding of the catalytic mechanism. In this work, we designed and synthesized a series of copper oxide-zinc oxide catalysts ((CuO)xZnO (0 ≤ x ≤ 49)) with a distinct porous hollow spherical structure for the reaction. These porous hollow spherical catalysts composed of CuO and ZnO nanoparticles were prepared through co-adsorption of Cu2+ and Zn2+ in the interior and outer surfaces of the hydrothermally synthesized carbonaceous spheres, followed by a new hydrothermal treatment and calcination in air. The catalytic properties of the (CuO)xZnO hollow spheres for dimethyldichlorosilane synthesis via the Rochow reaction was investigated, and a deeper understanding of the catalytic mechanism was obtained. As compared to pure CuO hollow spheres, the prepared (CuO)19ZnO hollow spheres exhibited much higher dimethyldichlorosilane selectivity and silicon conversion, which are clearly related to the synergistic electronic effect between Cu and ZnO and to the distinct catalyst structures which allow intimate contact of the reactant molecules with the active component and the efficient transport of the molecules. This work opens a new way for the fabrication of efficient and integrated Cu-based catalysts for the Rochow reaction.
- Zhang, Zailei,Ji, Yongjun,Li, Jing,Zhu, Yongxia,Zhong, Ziyi,Su, Fabing
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p. 2808 - 2819
(2016/05/19)
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- METHOD OF PRODUCING ORGANOHALOSILANES
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A method for producing an organohalosilanes comprising reacting an organic compound comprising a halogen-substituted or unsubstituted alkane, a halogen-substituted or unsubstituted alkene, or an aromatic compound and at least one hydridohalosilane of formula RnSiHmX4-m-n, wherein each R is independently C-1 -C-1 4 hydrocarbyl or C-1 -C-1 4 hologen-substituted hydrocarbyl, X is fluoro, chloro, bromo, or iodo, n is 0, 1, or 2, m is 1, 2 or 3, and m+n=1, 2 or 3, in the presence of a heterogeneous catalyst comprising an oxide of one or more of the elements Sc, Y, Ti, Zr, Hf, B, Al, Ga, In, C, Si, Ge, Sn, or Pb, at a temperature greater than 100 °C, and at a pressure of at least 690 kPa, to produce a crude reaction product comprising the organohalosilane.
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Paragraph 0067
(2016/09/22)
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- Honeycomb-like CuO/ZnO hybrid nanocatalysts prepared from solid waste generated in the organosilane industry
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We report the preparation of honeycomb-like CuO/ZnO (CZx/y) nanocatalysts with CuO nanospheres (NSs) adhered with ZnO nanoparticles (NPs) for the Rochow reaction. The synthesis was carried out via adsorption of Cu2+/Zn2+ ions on carbon black (CB) which acted as both the agglomeration inhibitor and the hard template, and followed by calcination in air. The low cost Cu2+/Zn2+ ions were recovered from the solid waste generated in the organosilane industry via a simple ammonia leaching treatment. The samples were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, and temperature-programmed reduction. The as-obtained CZx/y nanohybrids had a honeycomb-like structure with large voids and openings among the CuO NSs. When re-used as a Cu-based catalyst for the Rochow reaction, the CZx/y NPs sample with an optimized ratio showed significantly improved dimethyldichlorosilane (M2) selectivity and silicon (Si) conversion as compared with the CuO/ZnO NPs prepared in the absence of CB, discrete CuO or ZnO NPs and the CuO/ZnO NPs with different compositions, mainly due to the unique honeycomb-like structure, smaller crystal size and synergistic electronic effect at the interface between Cu and ZnO in CZx/y NPs.
- Li, Jing,Liu, Hezhi,Ji, Yongjun,Zhang, Yu,Wang, Guangna,Zhu, Yongxia,Zhong, Ziyi,Hu, Xiao,Su, Fabing
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p. 59737 - 59748
(2016/07/06)
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- METHOD FOR PREPARING A HALOSILANE
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A method for preparing a reaction product includes: steps (1) and (2). Step (1) is contacting, at a temperature from 200°C to 1400 °C, a first ingredient including a silane of formula HaRbSiX(4-a-b), where subscript a is an integer from 0 to 4, subscript b is 0 or 1, a quantity (a + b) 4, each R is independently a monovalent organic group, and each X is independently a halogen atom, with the proviso that when the quantity (a + b) 4, then the ingredient further includes H2; with a spinel catalyst including copper; thereby forming a reactant. Step (2) is contacting the reactant with a second ingredient including an organohalide at a temperature from 100°C to 600 °C; thereby forming the reaction product and a spent reactant. The reaction product is distinct from the silane used in step (1). The method may be used to prepare diorganodihalosilanes from silicon tetrahalides.
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Paragraph 0086
(2015/06/03)
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- Heterojunctions generated in SnO2-CuO nanocatalysts for improved catalytic property in the Rochow reaction
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We report the improved catalytic performance of SnO2-CuO hybrid nanocatalysts synthesized by rationally designing and controlling the local heterojunction structure. The SnO2 nanoparticle (NP) decorated CuO nanorods (NRs) (SnO2-CuO) with a mace-like structure and with various CuO:SnO2 ratios were prepared via depositing pre-synthesized SnO2 NPs on CuO NRs in the presence of polyvinylpyrrolidone molecules. The CuO NRs were obtained by a facile hydrothermal reaction using Cu(NO3)2·3H2O as the precursor. The samples were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, and temperature-programmed reduction analyses. The results indicated that in the SnO2-CuO hybrid nanostructures, the heterojunctions were well generated as the SnO2 NPs were well dispersed on the CuO NRs. Their catalytic performances were then explored via the Rochow reaction, in which solid silicon (Si) reacts with gaseous methyl chloride (MeCl) to produce dimethyldichlorosilane (M2). Compared to separate CuO and SnO2 as well as their physical mixture, the SnO2-CuO hybrids exhibit significantly enhanced M2 selectivity and Si conversion because of the enhanced synergistic interaction between SnO2 and CuO due to the generated heterojunctions. This work demonstrates that the performance of heterogeneous catalysts can be improved by carefully designing and controlling their structures even when their composition remains unchanged.
- Zou, Shanying,Ji, Yongjun,Wang, Guangna,Zhu, Yongxia,Liu, Hezhi,Jia, Lihua,Guo, Xiangfeng,Zhong, Ziyi,Su, Fabing
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p. 63355 - 63362
(2015/08/11)
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- Synergistic effect in bimetallic copper-silver (CuxAg) nanoparticles enhances silicon conversion in Rochow reaction
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The oleylamine thermal reduction process was employed to prepare bimetallic copper-silver (CuxAg (0 ≤ x ≤ 50)) nanoparticles, such as Cu, Cu50Ag, Cu20Ag, Cu10Ag, Cu5Ag, CuAg, CuAg2, and Ag, by using Cu(CH3COO)2 and AgNO3 as the precursors. The samples were characterized by X-ray diffraction, transmission electron microscopy, thermogravimetric analysis, and X-ray photoelectron spectroscopy. The CuxAg hybrid nanostructure showed good particle dispersion, and Cu and Ag metals were well mixed. The catalytic properties of these bimetallic CuxAg nanoparticles as model catalysts for the Rochow reaction were explored. Compared to monometallic Cu and Ag nanoparticles, bimetallic CuxAg nanoparticles resulted in a much higher silicon conversion, which is attributed to the synergistic electronic effect between Cu and Ag metals. For example, the Cu atom was observed to have a lower electron density in the CuxAg bimetallic nanoparticle than that in monometallic Cu nanoparticles, which enhanced the formation of methylchlorosilanes on the silicon surface with chloromethane, demonstrating the significance of the CuxAg bimetallic catalysts in catalytic reactions during organosilane synthesis. The insights gained in this study should be conducive to the design of good Cu-based catalysts for the Rochow reaction.
- Zhang, Zailei,Ji, Yongjun,Li, Jing,Zhong, Ziyi,Su, Fabing
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p. 54364 - 54371
(2015/06/30)
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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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supporting information
p. 5600 - 5616
(2015/03/30)
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- Reaction of chloro(ethyl)silanes with chloro(phenyl)silanes in the presence of aluminum chloride. Synthesis of chloro(ethyl)(phenyl)silanes
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Abstract Substituent exchange at the silicon atom between chloro(phenyl)silanes (PhSiCl3, MePhSiCl2, Ph2SiCl2) and chloro(ethyl)silanes (EtSiCl3, Et2SiCl2, Et3SiCl, Et4Si) in the presence of aluminum chloride has been studied. The examined compounds, except for PhSiCl3 and Et4Si, react fairly readily to give chloro(ethyl)-(phenyl)silanes in up to 48-52% yield. A probable mechanism has been proposed.
- Lakhtin,Eremeeva,Gordeev,Ushakov,Bykovchenko,Kirilin,Chernyshev
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p. 595 - 599
(2015/05/13)
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- Method for preparing silicon—sulfur compounds and their use in bitiminous compositions
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A method of producing sulfur modified organosilane compounds that can be used in asphalt binders which method involves: combining together an organosilane or mixtures of organosilanes, a sulfide, a halogen acceptor and solvent to form a reaction mixture; and allowing the organosilane to react with the sulfide in the presence of a halogen acceptor to produce a sulfur modified organosilane compound. The sulfur modified organosilane compound can be introduced into a polymer modified or unmodified asphalt binder in which the sulfur modified organosilane compound reacts with components in the asphalt mixture to form a modified asphalt. The organosilanes used to produce the sulfur modified organosilanes can be from a source of waste products (such as Direct Product Residue) in which case the waste products can be reused in asphalt binders.
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Page/Page column
(2015/08/03)
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- Role of N-donor groups on the stability of hydrazide based hypercoordinate silicon(IV) complexes: Theoretical and experimental perceptions
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A triphenylphosphinimino donor group is illustrated as a ligand in pentacoordinate siliconium halide dichelates, [YSiL2]+X-, where L is the bidentate ligand -OC(R)=NN=PPh3)- (R = t-Bu-Ph or Ph), Y = Me, Ph, CH2Cl, CHCl2, Cl or Br, and X = Cl or Br. All the new complexes were characterized by NMR spectroscopy and elemental analysis. The remote substituent, the t-Bu-phenyl or phenyl group, imparts more pentacoordinate character, i.e. more ionization to the complexes, compared to the PhCH2 group. DFT calculations indicate that the central silicon atom, due to the more positive charge, demands greater electron density. As a result of this, shorter Si-O, Si-N and Si-Cl bonds were observed. Both theoretical and experimental analysis indicate that the phosphinimino ligand is a stronger donor than the previously studied dimethylamino and isopropylidenimino ligands, causing all of the complexes to be pentacoordinate siliconium-halide salts in solution. The hypercoordinate silicon dichelates undergo unique intermolecular chelate exchange reactions: (i) complete ligand transfer from the dichelates to PhSiCl3 by a ligand priority order and (ii) bidentate ligand interchange between the dichelates and a trimethylsilyl-hydrazide precursor. Thermolysis of some selected hypercoordinated silicon(IV) complexes containing a silicon-carbon σ-bond significantly undergo a two step decomposition, while other complexes with silicon-halogen σ-bonds follow three steps. The thermal decomposition strongly depends on the nature of the substituents directly attached to the central silicon atom.
- Suman, Pothini,Janardan, Sannapaneni,Lone, Mohsin Y.,Jha, Prakash,Vijayakrishna, Kari,Sivaramakrishna, Akella
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p. 266 - 274
(2015/09/28)
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- Controllable wet synthesis of multicomponent copper-based catalysts for Rochow reaction
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This work aims to provide a facile, low-cost and scalable method for the preparation of multicomponent Cu-Cu2O-CuO catalysts, which are of high interest to the organosilane industry. A series of submicrometer-sized and Cu-based catalysts containing CuO, Cu2O and Cu, or some combination of them, were synthesized by a simple low-temperature wet chemical method using CuSO4·5H2O as the precursor and N2H4·H2O as a reducing agent. The samples were characterized by X-ray diffraction, thermogravimetric analysis, temperature-programmed reduction, X-ray photoelectron spectroscopy, transmission electron microscopy, and scanning electron microscopy techniques. It was observed that the composition of the samples could be tailored by varying the amount of reducing agent at a given reaction temperature and time. These catalysts were then tested in the Rochow reaction, using silicon powder and methyl chloride (MeCl) as reactants to produce dimethyldichlorosilane (M2), which is the most important organosilane monomer in the industry. Compared with bare CuO and Cu particles, the ternary CuO-Cu2O-Cu catalyst displayed much improved M2 selectivity and Si conversion, which can be attributed to the smaller copper particle size and the synergistic effect among the different components in the CuO-Cu2O-Cu catalyst. This catalyst preparation method is expected to yield efficient and low-cost copper catalysts for the organosilane industry.
- Zhai, Yanzhao,Ji, Yongjun,Wang, Guangna,Zhu, Yongxia,Liu, Hezhi,Zhong, Ziyi,Su, Fabing
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p. 73011 - 73019
(2015/09/15)
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- METHOD OF PREPARING AN ORGANOHALOSILANE BY REACTING HYDROGEN, HALOSILANE AND ORGANOHALIDE IN A TWO STEP PROCESS ON A COPPER CATALYST
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The application relates to a method for preparing organohalosilanes in a two-step process: Steps (i) contacting a copper catalyst with hydrogen gas and halogenated silanes forming a silicon-containing copper catalyst; and Step (ii) contacting said silicon-containing copper catalyst with an organohalide to form the organohalosilane.
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Paragraph 0065-0069
(2014/03/22)
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- PROCESS FOR THE PRODUCTION OF SILANE PRODUCTS FROM CALCIUM SILICIDE
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A process for preparing a reaction product including a silane product includes step (i), (ii), and (iii). Step (i) is contacting an organohalide with a calcium silicide at a temperature from 300 °C to 700 °C to form the reaction product including a spent reactant and the silane product. The silane product has formula RmHnSiX(4-m-n), where each R is independently a monovalent organic group, each X is independently a halogen atom; subscript m is 0 to 4; subscript n is 0 to 2; and a quantity (m + n) is 0 to 4. Step (ii) is contacting, at a temperature from 200 °C to 1400 °C, the spent reactant with a silane of formula HaRbSiX(4-a-b), where subscript a is 0 to 4, subscript b is 0 or 1, a quantity (a + b) ≤ 4. The silane of formula HaRbSiX(4-a-b) is distinct from the silane product of formula RmHnSiX(4-m-n). When the quantity (a + b) 2; thereby forming a reactant. Step (iii) is contacting the reactant formed in step (ii) with an additional organohalide at a temperature from 300 °C to 700 °C to form an additional silane product of formula RmHnSiX(4-m-n). Steps (ii) and (iii) are performed separately and consecutively after step (i).
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Paragraph 0052
(2014/11/11)
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- PROCESS FOR SELECTIVE PRODUCTION OF HALOSILANES FROM SILICON-CONTAINING TERNARY INTERMETALLIC COMPOUNDS
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A process includes contacting an organohalide with a ternary intermetallic compound at a temperature of 300 °C to 700 °C to form a reaction product including a halosilane. The ternary intermetallic compound includes three metals. The first metal is Cu or Mg; the second metal is Au, Ni, or Pd; and the third metal is Si.
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Paragraph 0041
(2014/08/06)
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- METHOD OF PREPARING HALOGENATED SILAHYDROCARBYLENES
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A method comprises separate and consecutive steps (i) and (ii). Step (i) includes contacting a copper catalyst with hydrogen gas and a halogenated silane monomer at a temperature of 500 °C to 1400 °C to form a silicon-containing copper catalyst comprising at least 0.1 % (w/w) of silicon. Step (ii) includes contacting the silicon-containing copper catalyst with an organohalide at a temperature of 100°C to 600 °C to form a reaction product. The organohalide has formula HaCbXc, where X is a halogen atom, subscript a is an integer of 0 or more, subscript b is an integer of 1 or more, and subscript c is an integer of 2 or more. The method produces a reaction product. The reaction product includes a halogenated silahydrocarbylene.
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Paragraph 0037
(2014/05/07)
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- Controllably oxidized copper flakes as multicomponent copper-based catalysts for the Rochow reaction
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The metallic Cu flakes prepared by milling metallic Cu powder were controllably oxidized in air at different temperatures to obtain the Cu-based catalysts containing multicomponents of Cu, Cu2O, and CuO. These catalysts are explored in the Rochow reaction using silicon powder and methyl chloride (MeCl) as reactants to produce dimethyldichlorosilane (M2), which is the most important organosilane monomer in the industry. The samples were characterized by X-ray diffraction, temperature-programmed reduction, thermogravimetric analysis, oxidimetry analysis, particle size analysis, transmission electron microscopy, and scanning electron microscopy. Compared to the metallic Cu powder and Cu flakes, the controllably oxidized Cu flakes containing Cu, Cu2O, and CuO species show much higher M2 selectivity and silicon conversion in the Rochow reaction. The enhanced catalytic performance may stem from the larger interfacial contact among the gas MeCl, solid Si particles, and solid Cu-based catalyst flakes, as well as the synergistic effect among the different Cu species. The work would be helpful to the development of novel Cu-based catalysts for organosilane synthesis.
- Liu, Shaomian,Wang, Yingli,Zhu, Yongxia,Wang, Guangna,Zhang, Zailei,Che, Hongwei,Jia, Lihua,Su, Fabing
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p. 7826 - 7833
(2014/02/14)
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- Flower-like ZnO grown on urchin-like CuO microspheres for catalytic synthesis of dimethyldichlorosilane
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We report the rational growth of flower-like ZnO on urchin-like CuO (f-ZnO@u-CuO) microspheres via a facile solvothermal method using copper nitrate and zinc nitrate as precursors in the presence of sodium nitrate and ethanol. A formation mechanism was proposed based on the observation of a series of reaction intermediates. The samples were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, inductively coupled plasma optical emission spectrometer, and temperature-programmed reduction. It was found that the morphology of the samples was highly dependent on the synthesis conditions, particularly the reaction time and the ammonia amount added. As a copper-based catalyst for dimethyldichlorosilane synthesis via the Rochow reaction, f-ZnO@u-CuO microspheres show better catalytic performance than the Cu-based catalysts physically mixed with ZnO promoter, probably because of the well-developed p-n heterojunction structures at the CuO and ZnO interfaces that generate a much strong synergistic effect. The work provides a simple method to synthesize hierarchical CuO/ZnO composites and would be helpful for understanding the catalytic mechanism of the Rochow reaction.
- Zhu, Yongxia,Wang, Yingli,Song, Lianying,Chen, Xin,Liu, Wuyuan,Sun, Jin,She, Xilin,Zhong, Ziyi,Su, Fabing
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p. 9794 - 9802
(2013/09/02)
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- Alternative methods for the synthesis of organosilicon compounds
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A method of forming chloro-substituted silanes from the reaction of an alkoxy-or acetoxy-substituted silane with a chlorinating agent in the optional presence of a catalyst is provided. For instance, chloro-substituted silanes, including but not limited to silicon tetrachloride, are formed by reacting a chlorinating agent, such as thionyl chloride, with an alkoxysilane having the formula (R'O)4-xSiRx, where R and R' are independently selected alkyl groups comprising one or more carbon atoms and x is 0, 1, 2, or 3. The catalyst may be dimethylformamide, (chloromethylene)dimethyliminium chloride, or triethylamine, among others. The chloro-substituted silane formed in the reaction along with several by-products has the formula (R'O)4-x-ySiRxCly; where x is 0, 1, 2, or 3 and y is 1, 2, 3, or 4. One of the by-products of the reaction is an alkyl chloride.
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Paragraph 0035; 0062-0064
(2013/09/26)
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- ALTERNATIVE METHODS FOR THE SYNTHESIS OF ORGANOSILICON COMPOUND
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A method of forming chloro-substituted silanes from the reaction of an alkoxysilane with a chlorinating agent in the optional presence of a catalyst is provided. More specifically, chloro-substituted silanes, including but not limited to silicon tetrachloride, are formed by reacting a chlorinating agent, such as thionyl chloride, with an alkylalkoxysilane having the formula (R'0)4-xSiRx, where R and R' are independently selected alkyl groups comprising one or more carbon atoms and x is 0, 1, 2, or 3. The catalyst may be dimethylformamide, (chloromethylene)dimethyliminium chloride, or triethylamine, among others. The chloro- substituted silane formed in the reaction along with several by-products has the formula (RO)4-x-ySiRxCly; where x is 0, 1, 2, or 3 and y is 1, 2, 3, or 4. One of the by-products of the reaction is an alkyl chloride.
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Paragraph 0062-0064
(2013/09/26)
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- METHOD OF PREPARING A DIORGANODIHALOSILANE
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A method of preparing a diorganodihalosilane, the method comprising the following separate and consecutive steps: (i) treating a preformed metal silicide with a mixture comprising hydrogen gas and a silicon tetrahalide at a temperature from 300 to 1400 °C to form a treated metal silicide, wherein the preformed metal silicide comprises a metal selected from at least one of Ni, Pd, or Pt; and (ii) reacting the treated metal silicide with an organohalide according to the formula RX at a temperature from 250 to 700 °C to form a diorganodihalosilane, wherein R is C1 -C10 hydrocarbyl and X is halo.
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Page/Page column 11
(2012/08/08)
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- METHOD FOR HYDROSILYLATION USING A PLATINUM CATALYST
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The selectivity of hydrosilylation of unsaturated organic compounds by Si—H functional organosilicon compounds is improved by use of a silyl polyphosphate ester in conjunction with a platinum hydrosilylation catalyst.
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Page/Page column 4
(2013/02/27)
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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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- METHOD OF MAKING ORGANOHALOSILANES
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The invention pertains to a process for the preparation of organohalosilanes. The process comprises contacting a first finely-divided silicon comprising from 0.08 to 0.25 % (w/w) of aluminum with an organohalide in a reactor at a temperature of from 250 to 350 °C in the presence of a Direct Process catalyst comprising copper, and a promotor; and introducing a second finely-divided silicon into the reactor comprising from 0.001 to 0.10 % (w/w) of aluminum into the reactor as needed in an amount sufficient to maintain an aluminum concentration of from 0.08 to 0.2 % (w/w), based on a weight of unreacted silicon and aluminum.
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Page/Page column 12-13
(2011/05/05)
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- METHOD OF PREPARING AN ORGANOHALOSILANE
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A method of preparing organohalosilanes comprising combining an organohalide having the formula RX (I), wherein R is a hydrocarbyl group having 1 to 10 carbon atoms and X is fluoro, chloro, bromo, or iodo, with a contact mass comprising at least 2% (w/w) of a palladium suicide of the formula PdxSiy (II), wherein x is an integer from 1 to 5 and y is 1 to 8, or a platinum suicide of formula PtzSi (III), wherein z is 1 or 2, in a reactor at a temperature from 250 to 700 °C to form an organohalosilane.
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Page/Page column 11-12
(2011/08/21)
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- PREPARATION OF ORGANOHALOSILANES
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A process for preparing organohalosilanes comprising combining hydrogen, a halosilane having the formula HaSiX4-a (I), and an organohalide having the formula RX (II), wherein R is C1-C10 alkyl or C4-C10 cycloalkyl, each X is independently halo, and the subscript a is 0, 1, or 2, in the presence of a sufficient amount of a catalyst effective in enabling the replacement of one or more of the halo groups of the halosilane with the R group from the organohalide, at a temperature from 200 to 800 °C, to form an organohalosilane and a hydrogen halide, wherein the volumetric ratio of hydrogen to halosilane is from 1 :3 to 1 :0.001 and the volumetric ratio of hydrogen to organohalide is from 1 : 1 to 1 :0.001, and wherein the catalyst is optionally treated with the hydrogen or the halosilane prior to the combining.
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Page/Page column 14
(2011/12/14)
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- METHOD FOR PRODUCING -HETERO-SUBSTITUTED ALKYLHALOHYDROSILANE AND USE THEREOF
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Method for efficiently producing α-hetero-substituted alkylhalohydrosilane,and use thereof. A method for producing (A) a halohydrosilane compound represented by the general formula (1): H-SiR2c(CR13-bYb)aX3-a-c (1) (wherein, R1 represents a hydrogen atom or a substituted or unsubstituted hydrocarbon group; R2 represents a substituted or unsubstituted hydrocarbon group; X represents a halogen atom; Y represents a hetero substituent; a is 1 or 2; b is any one of 1, 2 and 3; c is 1 or 0), by allowing (B) a halosilane compound represented by the general formula (2) : SiR2c(CR13-bYb)aX4-a-c (2) (wherein, R1, R2, X, Y, a, b and c are as defined above) to react with (C) a hydrosilane compound. A method for producing a reactive silicon group-containing polymer using the halohydrosilane compound (A).
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Page/Page column 24; 25; 26
(2011/04/25)
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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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- Formation of silicon-carbon bonds by photochemical irradiation of (η5-C5H5)Fe(CO)2SiR3 and (η5-C5H5)Fe(CO)2Me to Obtain R3SiMe
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Photochemical irradiation of an equimolar mixture of (η5 -C5H5)Fe(CO)2SiR3, FpSiR 3, and FpMe leads to the efficient formation of the silicon-carbon-coupled product R3SiMe, R3 = Me 3, Me2Ph, MePh2, Ph3, ClMe 2, Cl2Me, Cl3, Me2Ar (Ar = C 6H4-p-X, X = F, OMe, CF3, NMe2). Similar chemistry occurs with related germyl and stannyl complexes at slower rates, Si > Ge Sn. Substitution of an aryl hydrogen to form FpSiMe2C6H4-p-X has little effect on the rate of the reaction, whereas progressive substitution of methyl groups on silicon by Cl slows the process. Also, changing FpMe to FpCH2SiMe3 dramatically slows the reaction as does the use of (η5-C 5Me5)Fe(CO)2 derivatives. A mechanism involving the initial formation of the 16e intermediate (η5-C 5H5)Fe(CO)Me followed by oxidative addition of the Fe-Si bond accounts for the experimental results obtained.
- Fortier, Skye,Zhang, Yongqiang,Sharma, Hemant K.,Pannell, Keith H.
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experimental part
p. 1041 - 1044
(2010/04/25)
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- IMPROVEMENTS IN THE PREPARATION OF ORGANOHALOSILANES AND HALOSILANES
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A semi-continuous process for producing organohalosilanes or halosilanes in a fluidised bed reactor, from silicon-containing contact mass, comprising removing silicon-containing contact mass that has been used in said reactor by: (i) elutriation in an unreacted organohalide or hydrogen halide stream and/or an organohalosilane or halosilane product stream and (ii) direct removal using gravitational or pressure differential methods and returning removed silicon-containing contact mass to the fluidised bed reactor and/or fresh silicon-containing contact mass. When used for producing organohalosilanes (e.g. alkylhalosilanes) the silicon-containing contact mass may contain catalysts and promoters in addition to silicon.
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Page/Page column 19-21
(2009/12/28)
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- Continuous Preparation of Organosilanes
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The invention relates to a process for the continuous preparation of organosilanes in a reactive distillation column, wherein a homogenous hydrosilylation catalyst is introduced into the column.
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Page/Page column 4-5
(2008/06/13)
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- Process For Preparing Si-H-Containing Silanes
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Silanes of the general formula (1) [in-line-formulae]RaSiHbX4-b-a ??(1)[/in-line-formulae] are prepared by disproportionating at least one more highly chlorinated silane in the presence of a homogeneous catalyst in an apparatus with at least one reactive distillation column and at least one additional reactor selected from among prereactors and side reactors, where R is an alkyl, aryl, alkaryl or haloalkyl radical, X is a halogen atom, a is 0 or 1, and b is 2, 3 or 4.
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Page/Page column 4-5
(2009/01/24)
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- Surface Active Organosilicone Compounds
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The present invention relates to new organodisilanes or carbodisilanes, a process for manufacturing the same and their use, in particular, as surface active agents, especially as spreading agents.
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Page/Page column 6-7
(2008/12/09)
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- Process For Preparing Methylchlorosilanes
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The invention relates to a process for the direct synthesis of methylchlorosilanes by reaction of chloromethane with a contact composition comprising silicon and copper catalyst, wherein the concentration of oxygen in the chloromethane used is reduced by mixing a) chloromethane which contains oxygen, and b) chloromethane which contains a gaseous boron compound.
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Page/Page column 3
(2008/06/13)
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- Direct Method for Synthesising Alkylhalogenosilanes
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Process for the preparation of alkylhalosilanes by reaction of an alkyl halide, preferably CH3Cl, with a solid body, referred to as contact body, formed of silicon and of a catalytic system comprising (α) a copper catalyst and (β) a group of promoting additives comprising: an additive β1 chosen from metallic zinc, a zinc-based compound and a mixture of these entities, an additive β2 chosen from tin, a tin-based compound and a mixture of these entities, optionally an additive β3 chosen from cesium, potassium, rubidium, a compound derived from these metals and a mixture of these entities, said direct synthesis process being characterized by the following points, taken in combination: the copper catalyst (α) is in the form of metallic copper. of a copper halide or of a mixture of these entities, the contact body additionally includes a supplementary promoting additive β4 chosen from a derivative of an acid of phosphorus and a mixture of these entities.
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Page/Page column 3; 4
(2008/06/13)
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- Si-C coupling reaction of polychloromethanes with HSiCl3 in the presence of Bu4PCl: Convenient synthetic method for bis(chlorosilyl)methanes
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Coupling reaction of polychloromethanes CH4-nCln (n = 2-4) with HSiCl3 in the presence of tetrabutylphosphonium chloride (Bu4PCl) as a catalyst occurred at temperatures ranging from 30 °C to 150 °C. The reactivity of polychloromethanes increases as the number of chlorine-substituents on the carbon increases. In the reactions of CCl4 with HSiCl3, a variety of coupling products such as bis(chlorosilyl)methanes CH2(SiCl3)(SiXCl2) [X = Cl (1a), H (1b)], (chlorosilyl)trichloromthanes Cl3CSiXCl2 [X = Cl (2a), H (2b)], and (chlorosilyl)dichloromthanes Cl2HCSiXCl2 [X = Cl (3a), H (3b)] were obtained along with reductive dechlorination products such as CHCl3 and CH2Cl2 depending on the reaction temperature. In the reaction of CCl4, 2a is formed at the initial stage of the coupling reaction and converted to give CHCl3 at low temperature of 30 °C, to give 1a, 3a, and CHCl3 at 60 °C, and to afford 1a as major product and CH2Cl2 in competition above 100 °C. Si-H bond containing silylmethanes can be formed by the H-Cl exchange reaction with HSiCl3. Reaction of CHCl3 with HSiCl3 took placed at 80 °C to give three compounds 1a, 3a, and CH2Cl2, and finally 3a was converted to give 1a and CH2Cl2 at longer reaction time. While the condition for the reaction of CH2Cl2 with HSiCl3 required a much higher temperature of 150 °C. Under the optimized conditions for synthesizing bis(chlorosilyl)methanes 1a,b, a mixture of 1a and 1b were obtained as major products in 65% (1a:1b = 64:1) and 47% (42:5) yields from the reaction of CCl4 and CHCl3 at 100 °C for 8 h, respectively, and in 41% (34:7) yield from that of CH2Cl2 at 170 °C for 12 h. In the Si-C coupling reaction of polychloromethanes with HSiCl3, it seems likely that a trichlorosilyl anion generated from the reaction of HSiCl3 with Bu4PCl is an important key intermediate.
- Jung, Dong Euy,Kang, Seung-Hyun,Han, Joon Soo,Lim, Weon Cheol,Park, Young-ae W.,Yoo, Bok Ryul
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p. 3901 - 3906
(2008/03/12)
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- Continuous hydrosilylation process
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Continuous hydrosilylation of compounds (A) bearing C—C multiple bonds by means of silicon compounds (B) having Si—H groups, in which the reaction components (A) and (B) are reacted continuously in an integrated loop-tube reactor, with reaction mixture being conveyed from the tube into the loop and back again so that a section of the tube is part of the loop circuit, provides a highly controllable reaction process with high product yields.
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Page/Page column 4-5
(2008/06/13)
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- Composite copper/tin/alkali metal catalysts for the direct synthesis of alkylhalosilanes
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The alkylhalosilanes are directly synthesized while diminishing the formation of coke by reacting an alkyl halide with silicon in the presence of a catalytically effective amount of (α) a copper metal or a copper-based compound catalyst and (β) a catalyst promoter intermixture therefor which comprises an effective minor amount of an additive β1 selected from the group consisting of tin, a tin-based compound and mixture thereof, optionally, an effective minor amount of an additive β2 selected from the group consisting of zinc metal, a zinc-based compound and mixture thereof, an effective minor amount of an additive β3 selected from the group consisting of cesium, potassium and rubidium, and compound and mixture thereof, and, optionally, an effective minor amount of an additive β4 selected from the group consisting of the element phosphorus, a phosphorus-based compound and mixture thereof.
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Page/Page column 4
(2008/06/13)
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- Composite catalysts for the direct synthesis of alkylhalosilanes
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The alkylhalosilanes are directly synthesized by reacting an alkyl halide with silicon in the presence of a catalytically effective amount of (α) a copper metal or a copper-based compound catalyst and (β) a catalyst promoter intermixture therefor which comprises an effective minor amount of an additive β1 selected from the group consisting of tin, a tin-based compound and mixture thereof, an effective minor amount of an additive β2 selected from the group consisting of cesium, potassium and rubidium, and compound and mixture thereof, and an effective minor amount of an additive β3 selected from the group consisting of the element phosphorus, a phosphorus-based compound and mixture thereof.
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Page/Page column 3-4
(2010/02/15)
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