CN112625058B - Method for preparing monovinyl chlorosilane through disproportionation reaction of polyvinyl silane - Google Patents
Method for preparing monovinyl chlorosilane through disproportionation reaction of polyvinyl silane Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/121—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20
- C07F7/125—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20 by reactions involving both Si-C and Si-halogen linkages, the Si-C and Si-halogen linkages can be to the same or to different Si atoms, e.g. redistribution reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/12—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides
- B01J31/14—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides of aluminium or boron
- B01J31/143—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides of aluminium or boron of aluminium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
- B01J31/30—Halides
Abstract
The invention discloses a method for preparing monovinyl chlorosilane through disproportionation of polyvinyl silane, and belongs to the field of disproportionation of organosilane. Reacting polyvinyl silane and polychlorinated silane in the presence of a disproportionation reaction catalyst to obtain a disproportionation reaction product, namely monovinyl chlorosilane, wherein the disproportionation reaction catalyst is a reaction product of Lewis acid and organosiloxane. The invention adopts the reaction product of Lewis acid and organic siloxane as a disproportionation reaction catalyst, so that the conversion rate of the polyvinyl silane is more than 70 percent; meanwhile, side reactions such as olefinic bond polymerization reaction, addition reaction and the like are avoided to the maximum extent, and the selectivity of the monovinyl chlorosilane is more than 80 percent.
Description
Technical Field
The invention relates to the field of organosilane disproportionation reaction, in particular to a method for disproportionation reaction of polyvinyl silane and polychlorinated silane.
Background
The direct method for synthesizing the organochlorosilane usually generates a series of homologues, wherein some compounds have wide application and large demand, such as dimethyldichlorosilane, and some compounds are difficult to digest, such as methyltrichlorosilane and methyldichlorosilane, and the organochlorosilane compounds are converted through disproportionation reaction, so that the purposes of making the best use of things, balancing productivity and obtaining new compounds are achieved.
US2732282 (a) discloses disproportionation of alkyl hydrochlorosilanes in the presence of nitrile catalysts to produce a class of silanes containing more hydrogen and a class of silanes containing more chlorine, at reaction temperatures up to 1500-2000 ℃.
US2786861 (a) discloses disproportionation of alkylchlorosilanes in the presence of aluminum chloride, with hydrogen-containing silanes promoting the reaction at a temperature of 500-2250 ℃.
US2888478 (a) discloses the disproportionation of phenylchlorosilanes with alkylchlorosilanes in the presence of aluminum chloride, zirconium chloride to give phenylalkylchlorosilanes.
US3399222 (a) discloses the disproportionation of hydrogen-containing silanes with chlorosilanes in the presence of quaternary ammonium salts or quaternary phosphonium salts as catalysts.
US4746752 (a) discloses the disproportionation of hydrosilanes with alkyl, aryl, halogen in the presence of quaternary ammonium or phosphonium salt catalysts.
GB1361434 (A) discloses alkylhydrochlorosilanes at temperatures above 500 ℃ and AlCl 3 ,ZrCl 4 ,KAlCl 4 Disproportionation reaction occurs under the catalysis of CuCl and the like.
However, very few reports have been made on the disproportionation of vinyl silanes, in particular of polyvinylsilanes, sheludyakov, V.D. et al (Zhurnal Obshcheni Khimii (1985), 55 (6), 1345-50) reported in FeCl 3 ,AlCl 3 ,ZnCl 2 ,SnCl 4 And SbCl 3 Under isocatalysis, polyvinylsilanes R m Cl n Si(CH＝CH 2 ) 4-(m+n) Reaction with HCl to form R m Cl n Si(CH＝CH 2 ) 3-(m+n) CH 2 CH 2 Cl, further rearrangement to remove vinyl to obtain R m Cl n+1 Si(CH＝CH 2 ) 3-(m+n) However, the rearrangement de-ethenyl reaction needs base catalysis, the catalytic efficiency in the chlorosilane system is very low, and the HCl removal reverse reaction exists.
The polyvinyl silane is a byproduct of the reaction for synthesizing the vinyl silane by a sodium condensation method, a thermal condensation method and a direct method, and the application value of the polyvinyl silane can be effectively improved by converting the polyvinyl silane into the monovinyl chlorosilane through a disproportionation reaction.
Disclosure of Invention
Aiming at the defects of the prior art on the disproportionation reaction of vinyl silane, the invention provides a disproportionation reaction method of polyvinyl silane, which converts the polyvinyl silane into monovinyl chlorosilane with high added value.
A method for preparing monovinyl chlorosilane by virtue of disproportionation reaction of polyvinyl silane comprises the steps of reacting polyvinyl silane with polychlorosilane in the presence of a disproportionation reaction catalyst to obtain a disproportionation reaction product monovinyl chlorosilane;
the polyvinyl silane is shown in a chemical formula I:
R 1 n Cl (4-m-n) Si(CH＝CH 2 ) m (I)
in the formula, R 1 Is C1-C4 alkyl or phenyl; m is 2,3 or 4; n is 0,1 or 2; and m + n is not greater than 4;
the polychlorinated silane is shown as a chemical formula II:
R 2 x Si Cl (4-x) (II)
in the formula, R 2 Is C1-C4 alkyl or phenyl; x is 0,1 or 2;
the monovinyl chlorosilane is shown in a chemical formula III:
R 3 y Cl (3-y) Si-CH＝CH 2 (III)
in the formula, R 3 Is R 1 And/or R 2 (ii) a y is 1 or 2;
the disproportionation reaction catalyst is a reaction product of Lewis acid and organosiloxane.
Preferably, the lewis acid is at least one of aluminum chloride, ferric chloride, ferrous chloride, zinc chloride, cupric chloride, cuprous chloride and titanium chloride; the organic siloxane is at least one of organic siloxane ring body, organic siloxane linear body, polydimethylsiloxane, vinyl polysiloxane and hydrogen-containing polysiloxane.
Preferably, the ratio of the lewis acid to the organosiloxane is 1:0.3 to 60.
Further preferably, the ratio of the lewis acid to the organosiloxane is from 1:0.3 to 2.4; the preparation method of the disproportionation reaction catalyst comprises the following steps: the Lewis acid and the organic siloxane react for 5 to 60min at the room temperature to 180 ℃.
Vinyl silane is different from alkyl silane, phenyl silane or hydrogen-containing silane, and is easy to produce olefinic bond polymerization reaction and addition reaction under the heating condition, and particularly, the vinyl silane is connected with a plurality of vinyl groups on silicon atoms or the vinyl silane is subjected to polymerization reaction and addition reaction under the existence of free radicals, anions, cations, lewis acids and the like in a system. In order to prevent the olefinic bond polymerization reaction and the addition reaction, the catalyst for the disproportionation reaction needs to be passivated, and the temperature for the disproportionation reaction cannot be too high.
Most preferably, the Lewis acid is at least one of aluminum chloride, zinc chloride and copper chloride; the organic siloxane is at least one of dimethyl siloxane ring body, polydimethylsiloxane with viscosity not more than 1000mPa.s and vinyl polysiloxane with viscosity not more than 1000mPa.s.
Aluminum chloride, zinc chloride and copper chloride in Lewis acid have better selectivity on disproportionation reaction of polyvinyl silane and chlorosilane, dimethyl siloxane ring bodies, polydimethylsiloxane and vinyl polysiloxane in organosiloxane do not contain active hydrogen, and partial metal-chlorine bonds are converted into metal-oxygen-silicon bonds after the Lewis acid reacts with the organosiloxane, so that the activity of Lewis acid catalytic disproportionation reaction is milder, and the Lewis acid is immobilized to prevent sublimation loss.
The polydimethylsiloxane and the vinyl polysiloxane with lower viscosity are beneficial to uniform dispersion of the Lewis acid, and can not be wrapped by the polysiloxane with high viscosity to lose catalytic activity. The ratio of the metal-chlorine bond to the silicon-oxygen bond directly determines the reaction degree of the metal-chlorine bond, the equivalent ratio of the metal-chlorine bond to the silicon-oxygen bond is too large, the reaction is insufficient, the catalytic disproportionation reaction is too high in activity, and side reactions such as olefinic bond polymerization are increased; the equivalent ratio of the two is too small, the metal-chlorine bond is not enough to be reserved, and the catalytic disproportionation reaction activity is too low or even lost.
The reaction of Lewis acid and organosiloxane has no strict requirement on the conditions, but the reaction is incomplete due to too low reaction temperature and too short reaction time, and the protection and passivation effect of the organosiloxane on the catalyst are lost in the subsequent disproportionation reaction; too high a reaction temperature may destroy the catalyst structure, and too long a reaction time is wastefully wasted.
The use method of the disproportionation reaction catalyst comprises the following steps:
1. a disproportionation reaction catalyst is directly put into the batch type disproportionation reaction kettle to catalyze the disproportionation reaction of the polyvinyl silane and the polychlorinated silane, and the dosage of the catalyst is 1-25% of the total mass of the disproportionation reaction raw material polyvinyl silane and the polychlorinated silane; alternatively, the first and second liquid crystal display panels may be,
2. the disproportionation reaction catalyst is loaded on a carrier, the carrier is one of alumina, active carbon, zeolite and molecular sieve, and the loading capacity of the disproportionation reaction catalyst is 5-30% of the mass of the carrier; the supported catalyst is filled in a continuous disproportionation reactor such as a tubular reactor and a fixed bed reactor, and the mixture of disproportionation reaction raw materials polyvinyl silane and polychlorinated silane flows through the reactor under the reaction condition.
Preferably, the disproportionation reaction catalyst put into the batch type disproportionation reaction kettle is repeatedly used for 5 to 90 times; alternatively, the first and second liquid crystal display panels may be,
the supported catalyst filled in the continuous disproportionation reactor has the running period of 1-720 hours.
The disproportionation reaction catalyst and the supported disproportionation reaction catalyst prepared by the invention have good stability and continuous catalytic capability, and after repeated use for many times or continuous operation for a period of time, the catalytic capability is reduced, the conversion rate of the polyvinyl silane is reduced, and the catalyst needs to be replaced or supplemented.
Preferably, in said polyvinylsilanes and said polychlorosilanes, R 1 And R 2 The same; the ratio of said polyvinyl silane to said polychlorosilane, in terms of equivalent ratio of silicon-vinyl bonds to silicon-chlorine bonds, is 1:0.4 to 12.
In polyvinyl silane, polychlorosilane, R 1 And R 2 And meanwhile, the types of disproportionation reaction products are obviously reduced, the generation of some foreseeable impurities is avoided, and convenient conditions are provided for the separation and purification of the target product, namely the monovinyl chlorosilane.
The ratio of the polyvinyl silane to the polychlorosilane is not sufficient to cause disproportionation reaction with the Si-vinyl bond when the ratio of the Si-Cl bond is too low, while too high a ratio of the Si-Cl bond not only causes disproportionation of the Si-vinyl bond but also may cause R 1 And R 2 Disproportionation occurs, and the selectivity of the target product is reduced.
Preferably, the disproportionation reaction is carried out for 15-150 min at the temperature of 100-250 ℃, or the retention time in a continuous reactor is 15-150 min; the excessive reaction temperature and the excessive reaction time are easy to cause olefinic bond polymerization reaction and addition reaction, and reduce the reaction yield and selectivity, while the excessive reaction temperature and the short reaction time are low in reaction conversion rate and difficult in product separation.
The invention has the beneficial effects that:
1. the passivated Lewis acid disproportionation reaction catalyst effectively catalyzes the disproportionation reaction of polyvinyl silane and polychlorinated silane to obtain monovinyl chlorosilane, and the conversion rate of the polyvinyl silane is more than 70 percent;
2. side reactions such as olefinic bond polymerization reaction, addition reaction and the like are avoided to the maximum extent, and the selectivity of the monovinyl chlorosilane is more than 80 percent.
Detailed Description
The method for analyzing the disproportionation reaction raw material and product comprises the following steps:
gas chromatography, FID detector, chromatographic column HP-5, 60m × 0.25mm × 0.5 μm, chromatographic column temperature 35 deg.C, 5 min-5 deg.C/min-80 deg.C-15 deg.C/min-200 deg.C, 5min.
Recovery, conversion and selectivity calculation methods:
recovery (%) = (mass of disproportionation product distilled) × 100/(total mass of charged polyvinylsilane and polychlorosilane)
Conversion (%) = (sum of all disproportionation reaction product chromatographic peak areas) × 100/(sum of all disproportionation reaction product chromatographic peak areas + unreacted polyvinyl silane chromatographic peak area)
Selectivity (%) = (chromatographic peak area of monovinyl chlorosilane) × 100/(sum of chromatographic peak areas of all vinyl-containing disproportionation reaction products)
Catalyst preparation example:
catalyst A, 66.7g of anhydrous aluminum trichloride, 80g of polydimethylsiloxane with the viscosity of 500mPa.s and 14g of dimethyl siloxane mixed ring DMC, heating to 120 ℃ under the protection of nitrogen, and stirring for reaction for 30min.
Catalyst B, 44.4g of anhydrous aluminum trichloride, 33.6g of anhydrous copper chloride and 250g of 900mPa.s vinyl polydimethylsiloxane, heating to 60 ℃ under the protection of nitrogen, and stirring for reacting for 60min.
And (3) adding 44.4g of anhydrous aluminum trichloride, 34g of zinc chloride and 38g of dimethyl siloxane mixed ring DMC (dimethyl siloxane), heating to 60 ℃ under the protection of nitrogen, and stirring for reacting for 60min.
Catalyst D, 81g of ferric chloride and 550g of vinyl polydimethylsiloxane with viscosity of 400mPa.
And catalyst AA, wherein the catalyst A is loaded on alumina particles, the alumina particles are 80 meshes, and the loading amount is 8%.
And the catalyst BB is loaded on activated carbon particles, wherein the activated carbon particles are 150 meshes, and the loading capacity is 25%.
Example 1
Adding 413g of methyltriethylvinylsilane, 662g of methyldiethylchlorosilane, 1000g of methyltrichlorosilane and 200g of catalyst A into a 5L stainless steel autoclave, heating to 250 ℃ under nitrogen atmosphere, and reacting for 120min; the temperature was reduced to 80 ℃ and the reaction product was distilled off under reduced pressure to give 1970g of a disproportionation product with a recovery of 94.94% as determined by gas chromatography and the results are given in the following table:
the conversion of polyvinyl silane was 82.44% and the selectivity to methyl vinyl dichlorosilane was 87.32%.
Example 2
Adding 413g of methyltriethylsilane, 662g of methyldiethylchlorosilane, 1000g of methyltrichlorosilane and 200g of catalyst B into a 5L stainless steel autoclave, heating to 200 ℃ under nitrogen atmosphere, and reacting for 150min; the temperature was lowered to 80 ℃ and the reaction product was distilled off under reduced pressure to give 1982g of a disproportionation product with a recovery of 95.52%, a conversion of polyvinyl silane of 88.62% and a selectivity of methyl vinyl dichlorosilane of 92.14%.
Example 3
In an autoclave in which the disproportionation product was distilled out in example 2, without removing the catalyst, 413g of methyltriethylvinylsilane, 662g of methyldiethylchlorosilane and 1000g of propyltrichlorosilane were charged, and under the same reaction conditions as in example 2, 1945g of the disproportionation product was obtained, the recovery rate was 93.73%, the conversion rate of polyvinylsilane was 86.48% and the selectivity of methylvinyldichlorosilane was 50.98%.
Example 4
In an autoclave in which the disproportionation product was distilled out in example 3, without removing the catalyst, 1120g of dimethyldivinylsilane and 1030g of dimethyldichlorosilane were charged, and under the same reaction conditions as in example 3, 2041g of the disproportionation product was obtained, the recovery rate was 94.93%, the conversion rate of dimethyldivinylsilane was 70.57%, and the selectivity of dimethylvinylchlorosilane was 91.45%. The repeated use of the catalyst has no obvious influence on the recovery rate of the disproportionation product and the conversion rate of the polyvinyl silane.
Comparative example 1
Adding 413g of methyltriethylvinylsilane, 662g of methyldiethylchlorosilane and 1000g of methyltrichlorosilane into a 5L stainless steel autoclave, wherein 100g of anhydrous aluminum trichloride is used as a catalyst, heating to 200 ℃ under the protection of nitrogen, and reacting for 90min; the temperature is reduced to 80 ℃, the reaction product is evaporated under reduced pressure, and 1264g of disproportionation product is obtained, the recovery rate is 60.92%, the conversion rate of polyvinyl silane is 59.83%, and the selectivity of methyl vinyl dichlorosilane is 72.66%. The recovery rate of disproportionation product is obviously low, which indicates that after disproportionation reaction, a large amount of raw material is polymerized into macromolecular impurities.
Comparative example 2
Adding 413g of methyltriethylvinylsilane, 662g of methyldiethylchlorosilane and 1000g of methyltrichlorosilane into a 5L stainless steel autoclave, wherein a catalyst is a mixture of 80g of anhydrous aluminum trichloride and 30g of anhydrous copper chloride, heating to 240 ℃ under the protection of nitrogen, and reacting for 45min; the temperature was reduced to 80 ℃ and the reaction product was distilled off under reduced pressure to obtain 712g of disproportionation product with a recovery of 34.31%, a conversion of polyvinyl silane of 73.69% and a selectivity of methyl vinyl dichlorosilane of 81.62%. The recovery rate of disproportionation product is obviously low, which indicates that after disproportionation reaction, a large amount of raw material is polymerized into macromolecular impurities.
Examples 5 to 9
Adding polyvinyl silane, polychlorinated silane and a catalyst into a 5L stainless steel autoclave, and heating to react under a nitrogen atmosphere; the temperature is reduced to 80 ℃, the reaction product is evaporated under reduced pressure to obtain a disproportionation product, the recovery rate is calculated, the conversion rate and the selectivity are calculated after the disproportionation product is measured by gas chromatography, and the results are shown in the following table.
Example 10
400mL of catalyst AA is filled in a carbon steel tubular reactor DN25 x 1200, and three tubular reactors are connected in series to form a disproportionation reaction device; continuously pumping 3.5mL/min of methyl trivinyl silane, 5.0mL/min of methyl divinyl chlorosilane and 6.1mL/min of methyl trichlorosilane, keeping the temperature of a disproportionation reaction device at 200 ℃, and keeping the average retention time of materials at 58min; the disproportionation reaction liquid was continuously collected for 8 hours, and vacuum distillation was performed, so that the recovery rate was 97.72%, the conversion rate of polyvinyl silane was 80.26%, and the selectivity of methyl vinyl dichlorosilane was 63.93%.
Example 11
Filling 400mL of catalyst BB in a carbon steel tubular reactor DN25 x 1200, and connecting three tubular reactors in series to form a disproportionation reaction device; continuously pumping 3.3mL/min diphenyldivinyl silane and 3.6mL/min diphenyldichlorosilane, keeping the temperature of a disproportionation reaction device at 250 ℃, and keeping the average material residence time of 123min; continuously collecting the disproportionation reaction liquid for 12 hours, and distilling under reduced pressure, wherein the recovery rate is 98.25%, the conversion rate of diphenyldivinyl silane is 74.33%, and the selectivity of diphenylvinyl chlorosilane is 88.56%.
Claims (6)
1. A method for preparing monovinyl chlorosilane by disproportionation reaction of polyvinyl silane comprises reacting polyvinyl silane and polychlorinated silane in the presence of disproportionation catalyst to obtain disproportionation product monovinyl chlorosilane;
the polyvinyl silane is shown in a chemical formula I:
R 1 n Cl (4-m-n) Si(CH＝CH 2 ) m (I)
in the formula, R 1 Is C1-C4 alkyl or phenyl; m is 2,3 or 4; n is 0,1 or 2; and m + n is not greater than 4;
the polychlorinated silane is shown as a chemical formula II:
R 2 x Si Cl (4-x) (II)
in the formula, R 2 Is C1-C4 alkyl or phenyl; x is 0,1 or 2;
the monovinyl chlorosilane is shown in a chemical formula III:
R 3 y Cl (3-y) Si-CH＝CH 2 (III)
in the formula, R 3 Is R 1 And/or R 2 (ii) a y is 1 or 2;
the disproportionation catalyst is a reaction product of Lewis acid and organosiloxane;
the preparation method of the disproportionation reaction catalyst comprises the following steps: the Lewis acid and the organic siloxane react for 5 to 60min at the room temperature to 180 ℃; the ratio of the Lewis acid to the organosiloxane is 1:0.3 to 2.4;
wherein the Lewis acid is at least one of aluminum chloride, ferric chloride, ferrous chloride, zinc chloride, cupric chloride, cuprous chloride and titanium chloride; the organic siloxane is at least one of dimethyl siloxane ring body, polydimethylsiloxane with viscosity not more than 1000mPa.s and vinyl polysiloxane with viscosity not more than 1000mPa.s.
2. A process for the preparation of monovinylchlorosilane by disproportionation of polyvinylsilane as claimed in claim 1, wherein said disproportionation process is:
a disproportionation reaction catalyst is directly put into the batch type disproportionation reaction kettle to catalyze the disproportionation reaction of the polyvinyl silane and the polychlorinated silane, and the dosage of the catalyst is 1-25% of the total mass of the disproportionation reaction raw material polyvinyl silane and the polychlorinated silane; alternatively, the first and second electrodes may be,
the disproportionation reaction catalyst is loaded on a carrier, the carrier is one of alumina, activated carbon, zeolite and molecular sieve, and the load of the disproportionation reaction catalyst is 5-30% of the mass of the carrier; the supported catalyst is filled in a continuous disproportionation reactor, and the mixture of disproportionation reaction raw material polyvinyl silane and polychlorinated silane flows through the reactor under reaction conditions.
3. A process for the preparation of monovinylchlorosilane by disproportionation of polyvinylsilane as claimed in claim 2, wherein said disproportionation process is:
putting the disproportionation reaction catalyst into an intermittent disproportionation reaction kettle, and repeatedly using for 5-90 times; alternatively, the first and second electrodes may be,
the supported catalyst filled in the continuous disproportionation reactor has the running period of 1-720 hours.
4. The process for the disproportionation of polyvinylsilanes to produce monovinylchlorosilanes as claimed in claim 1 wherein R in said polyvinylsilanes and said polychlorosilanes is 1 And R 2 The same is true.
5. The process for the disproportionation of polyvinylsilanes to produce monovinylchlorosilanes as claimed in claim 1 wherein the ratio of said polyvinylsilane to said polychlorosilane, in terms of equivalent ratio of silicon-vinyl bonds to silicon-chlorine bonds, is from 1:0.4 to 12.
6. The method for preparing monovinyl chlorosilane by disproportionation of polyvinyl silane according to claim 1, wherein the disproportionation is carried out in a batch disproportionation reactor at a temperature of 100-250 ℃ for 15-150 min, or in a continuous reactor for 15-150 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1361434A (en) * | 1970-12-21 | 1974-07-24 | Gen Electric | Redistribution of alkylhydrosilanes |
| JPS5265226A (en) * | 1975-11-26 | 1977-05-30 | Shin Etsu Chem Co Ltd | Preparation of halogenosilanes |
| CN105753895A (en) * | 2016-03-09 | 2016-07-13 | 张玲 | Preparation method of dimethyl dichlorosilane |
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- 2020-12-16 CN CN202011485822.5A patent/CN112625058B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1361434A (en) * | 1970-12-21 | 1974-07-24 | Gen Electric | Redistribution of alkylhydrosilanes |
| JPS5265226A (en) * | 1975-11-26 | 1977-05-30 | Shin Etsu Chem Co Ltd | Preparation of halogenosilanes |
| CN105753895A (en) * | 2016-03-09 | 2016-07-13 | 张玲 | Preparation method of dimethyl dichlorosilane |
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