5021-93-2Relevant articles and documents
Chlorosilane alcoholysis acid removing agent and regeneration method thereof
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Paragraph 0018, (2017/04/28)
The invention discloses a chlorosilane alcoholysis acid removing agent and a regeneration method thereof. The regeneration method is characterized in that at a temperature of -10-130 DEG C, a substituting agent and an acid removing agent are added into a reactor in advance, chlorosilane is gradually added, the liquid phase obtained through filtration separation is subjected to rectification after the alcoholysis reaction is completed so as to obtain a silane finished product and the excessive substitution agent, the excessive substitution agent is recycled, and the acid removing agent obtained through filtration separation is recycled after being regenerated. According to the present invention, the yield of the silane prepared by using the process is more than or equal to 95%, and the recovery rate of the acid removing agent is more than or equal to 95%.
Continuous and batch organomagnesium synthesis of ethyl-substituted silanes from ethylchloride, tetraethoxysilane, and organotrichlorosilane for production of polyethylsiloxane liquids. 2. Continuous one-step synthesis of ethylethoxy- and ethylchlorosilanes
Klokov, Boris A.
, p. 234 - 240 (2013/09/07)
Development of a continuous one-step manufacturing process for ethylethoxy- and ethylchlorosilanes is described. The methodology of synthesis of ethyl-substituted silanes has been improved. The important factors for the successful synthesis have been determined. Among them are (1) the replacement of some tetraethoxysilane 3 by ethyltrichlorosilane 10, (2) the optimum concentration of 3 and 10, (3) the excess of the granulated magnesium (the supply rate 50-110 g h-1), and, finally, (4) the columnar apparatus with the stirrer, resulting in high yields of di-and triethylsilanes, low duration of synthesis, and high selectivity of Grignard reagent. Continuous one-step synthesis has been assimilated into industry (up to a scale 7-40 kg h-1 of magnesium) for production of oligoethylsiloxanes with low (5-20%) and high content (up to 40%) of the terminal triethylsiloxy groups. The rules for R/D process of the Grignard synthesis are described.
Continuous and batch organomagnesium synthesis of ethyl-substituted silanes from ethylchloride, tetraethoxysilane, and organotrichlorosilane for production of polyethylsiloxane liquids. 1. Batch one-step synthesis of ethylethoxysilanes and ethylchlorosilanes
Klokov, Boris A.
, p. 49 - 54 (2013/09/07)
Development of batch one-step manufacturing process for ethylethoxy- and ethylchlorosilanes is desribed. The methodology of synthesis of ethyl-substituted silanes has been improved. The important factors for the successful synthesis have been determined. Among them are the replacement of the part tetraethoxysilane 3 by ethyltrichlorosilane 10, the optimum concentration of 3 and 10 resulting in high yield of triethylsilanes, low duration of synthesis, and high selectivity of Grignard reagent. Batch one-step synthesis has been assimilated into industry (up to a scale 240 kg of magnesium) for production of oligoethylsiloxanes with the high content (>40%) of a terminal triethylsiloxy group. The rules for R/D process of the Grignard synthesis are described.
Continuous single-stage organomagnesium synthesis of a mixture of ethylethoxysilanes and dimethylethylethoxysilane
Klokov, Boris A.
, p. 122 - 128 (2013/09/07)
Simultaneous synthesis of ethylethoxysilanes and dimethylethylethoxysilane from a mixture of ethyl chloride, tetraethoxysilane, and dimethyldichlorosilane with magnesium (supply rate 75-100 g h-1) was studied. Schemes of intermediate processes are proposed. Reactivity of dimethyldichlorosilane and diethyldichlorosilane relative to each other is evaluated. Various grades of magnesium are tested. To reduce the amount of regenerated solvent (toluene) its mixtures with oligodiethylsiloxanes are used. The mixture of ethyl-substituted silanes can be used in subsequent preparation of oligo-ethylsiloxane liquids modified with the terminal dimethylethylsiloxy groups, which are characterised by improved lubricating properties.
Stepwise organomagnesium synthesis of mixtures of ethyletoxysilanes and ethylchlorosilanes
Klokov
, p. 1863 - 1865 (2007/10/03)
Mixture of ethylethoxy- and ethylchlorosilanes was prepared in a toluene solution by successive reaction of magnesium with a mixture of ethyl chloride and tetraethoxysilane and then with a mixture of ethyl chloride and tetrachlorosilane.
Continuous single-stage organomagnesium synthesis of a mixture of ethylethoxysilanes with methylethylphenylethoxysilane
Klokov
, p. 1587 - 1592 (2007/10/03)
A continuous reaction of ethyl chloride, tetraethoxysilane, and methylphenyldichlorosilane with magnesium in toluene or in a mixture of toluene with oligoethylsiloxanes was performed in a column apparatus with a stirrer under conditions of counterflow of magnesium and the reagent mixture.
Continuous organomagnesium synthesis of a mixture of ethylethoxysilanes and methylethyl(thienyl- or haloorgano)ethoxysilane
Klokov
, p. 479 - 482 (2007/10/03)
Simultaneous synthesis of ethylethoxysilanes and methylethyl(thienyl- or haloorgano)ethoxysilane from a mixture of ethyl chloride, tetraethoxysilane, and methyl(thienyl- or haloorgano)dichlorosilane with magnesium (supply rate 75-100 g h-1) was studied. The mixture of these compounds can be used in subsequent preparation of oligoethylsiloxane liquids modified with the terminal methylethyl(thienyl- or haloorgano)siloxy groups, which are characterized by improved lubricating properties.
Continuous Single-Stage Organomagnesium Synthesis of Ethylethoxysilanes and Ethylchlorosilanes from a Mixture of Tetraethoxysilane and Diethylchlorosilane
Klokov, B. A.
, p. 100 - 104 (2007/10/03)
Basic parameters are presented of novel highly efficient technology for the synthesis of organosilicon monomers for producing practically useful polyethylsiloxane liquids.
Iodine- or Iodine Monobromide-Catalyzed Alkoxy-Alkoxy Exchange Reactions of Alkylalkoxysilanes: Formation of the Catalyst-Alkoxysilane Complexes and the Reaction Mechanism
Ito, Katsuko,Ibaraki, Takeshi
, p. 2853 - 2858 (2007/10/02)
The formation of charge-transfer complexes of iodine and of iodine monobromide with alcohols and alkoxysilanes has been established spectroscopically, and the formation constants of iodine-ethoxytriethylsilane and iodine-diethoxydimethylsilane complexes has been determined as 0.55+/-0.01 and 0.61+/-0.02, respectively.On the basis of these observations and the kinetic information recently reported, the previously proposed mechanism for the iodine or iodine monobromide catalyzed alkoxy-alkoxy exchange reactions of alkoxysilanes is dicussed afresh.It has been confirmed that a mechanism involving a four-centered transition state containing a CT-complex is most favorable.