CN110372740B - Method for preparing trimethylchlorosilane from dimethylchlorosilane - Google Patents
Method for preparing trimethylchlorosilane from dimethylchlorosilane Download PDFInfo
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- CN110372740B CN110372740B CN201910785263.0A CN201910785263A CN110372740B CN 110372740 B CN110372740 B CN 110372740B CN 201910785263 A CN201910785263 A CN 201910785263A CN 110372740 B CN110372740 B CN 110372740B
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- 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
- C07F7/122—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20 by reactions involving the formation of Si-C linkages
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention provides a method for preparing trimethylchlorosilane from dimethylchlorosilane, which comprises the following steps: (1) adding ammonia water, hexadecyl trimethyl ammonium chloride and absolute ethyl alcohol into deionized water, stirring until the ammonia water, the hexadecyl trimethyl ammonium chloride and the absolute ethyl alcohol are completely dissolved, adding tetraethoxysilane, heating, continuing stirring to obtain a reaction liquid, filtering to obtain a filter cake, drying and roasting to obtain silicon dioxide; (2) mixing silicon dioxide, a zinc sulfate solution and an aluminum nitrate solution, adding a potassium borohydride solution after stirring, continuously stirring to obtain a reaction solution, filtering to obtain a filter cake, washing, and drying to obtain a catalyst; (3) adding dimethylchlorosilane, methyl aluminum chloride, chloromethane and a catalyst into a stirrer with an ultrasonic wave, introducing nitrogen into the stirrer to displace air, continuing introducing nitrogen to protect and heat the stirrer, starting the ultrasonic wave stirring, reacting at a constant temperature to obtain a reaction liquid, filtering the reaction liquid to obtain a filter cake, and drying the filter cake to obtain the trimethylchlorosilane. The method is simple to operate, and the yield and the purity of the trimethylchlorosilane are high.
Description
Technical Field
The invention relates to a method for preparing trimethylchlorosilane, in particular to a method for preparing trimethylchlorosilane from dimethylchlorosilane.
Background
Trimethylchlorosilane is widely used as a protective agent of functional groups such as hydroxyl, amino, carboxyl and the like in chemical synthesis and drug synthesis, and can also be used as a sealing agent of an organic silicon high molecular polymer in the processes of petroleum production and the like to play a role in regulating the molecular weight of the high polymer. At present, the preparation method of the trimethylchlorosilane mainly uses hydrogen chloride gas as a chlorinating agent to convert hexamethyldisiloxane into the trimethylchlorosilane.
Generally, hexamethyl siloxane is put into a reaction tank, a jacket is filled with a refrigerant for cooling, the temperature is maintained below 20 ℃, and excessive hydrogen chloride gas is continuously filled for several hours until the reaction is finished; absorbing and neutralizing tail gas of the reaction tank by using an alkali solution; the reaction liquid is subjected to phase splitting, and the by-product waste high-concentration hydrochloric acid in the reaction liquid is removed; and (3) dehydrating, dehydrochlorinating and rectifying the organic phase to obtain a product of trimethylchlorosilane. The method has the disadvantages of complex operation and complex steps, and has the disadvantages of serious equipment corrosion, generation of a large amount of high-concentration waste hydrochloric acid, waste acid pollution and environmental protection.
Chinese patent with application number CN201710039151.1 discloses a new process for producing trimethylchlorosilane by hexamethyldisiloxane, which comprises the following steps: 1) adding hexamethyldisiloxane into a reaction kettle, introducing the hexamethyldisiloxane and hydrogen chloride into a first filler absorption tower for a convection reaction, introducing redundant hydrogen chloride into a second filler absorption tower, and introducing the generated reaction material into a first water separator; 2) the reaction materials are layered in the first water separator to obtain a material layer with light components, the material layer enters the second filler absorption tower to react with the hydrogen chloride gas again, the redundant hydrogen chloride enters the tail gas absorption system, and the generated reaction materials enter the second water separator; 3) layering the reaction materials in a second water separator to obtain a material layer with light components, and recovering the material layer with the content of the trimethylchlorosilane being more than or equal to 80%. The patent also has the problems of complex operation and complicated steps.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing trimethylchlorosilane from dimethylchlorosilane, which is simple to operate and has higher yield and purity of the trimethylchlorosilane.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a method for preparing trimethylchlorosilane from dimethylchlorosilane comprises the following steps:
(1) adding ammonia water, hexadecyl trimethyl ammonium chloride and absolute ethyl alcohol into deionized water, stirring at 30 ℃ until the ammonia water, the hexadecyl trimethyl ammonium chloride and the absolute ethyl alcohol are completely dissolved, adding tetraethoxysilane while stirring, heating to 55 ℃, continuing stirring for 2 hours to obtain reaction liquid, filtering the reaction liquid to obtain a filter cake, drying the filter cake at 80 ℃ for 12 hours, and roasting to obtain silicon dioxide;
(2) mixing the silicon dioxide, the zinc sulfate solution and the aluminum nitrate solution obtained in the step (1), stirring for 5 minutes, adding a potassium borohydride solution, continuously stirring until no bubbles exist to obtain a reaction solution, filtering the reaction solution to obtain a filter cake, alternately washing the filter cake for 3 times by using deionized water and absolute ethyl alcohol, and drying at 80 ℃ for 12 hours to obtain a catalyst;
(3) adding dimethylchlorosilane, methyl aluminum chloride, methyl chloride and the catalyst obtained in the step (2) into an ultrasonic stirrer, introducing nitrogen into the ultrasonic stirrer to replace air for 2 hours, heating to 200 ℃ under the protection of the nitrogen, starting the ultrasonic stirrer to perform ultrasonic stirring, reacting at constant temperature for 4 hours to obtain reaction liquid, filtering the reaction liquid to obtain a filter cake, and drying the filter cake at 80 ℃ for 12 hours to obtain the trimethylchlorosilane.
Further, in the step (1), the pH value of ammonia water is 11, and the mass ratio of the ammonia water, the hexadecyl trimethyl ammonium chloride, the absolute ethyl alcohol, the deionized water and the tetraethoxysilane is 16:5:10:250: 19.
Further, in the step (1) of the present invention, the temperature rise process during firing is: the temperature is increased from room temperature to 300 ℃ within 30 minutes, the temperature is kept constant for 30 minutes, then the temperature is increased to 600 ℃ within 30 minutes, and the temperature is kept constant for 4 hours.
Further, in the step (2), the mass concentrations of the zinc sulfate solution, the aluminum nitrate solution and the potassium borohydride solution are 20%, and the mass ratio of the silicon dioxide to the zinc sulfate solution to the aluminum nitrate solution to the potassium borohydride solution is 1:16:8: 18.
Furthermore, in the step (3), the mass ratio of the dimethylchlorosilane to the methyl aluminum chloride to the methyl chloride to the catalyst is 1 (4-6) to (3-7) to (0.4-0.6).
Further, in the step (3) of the present invention, the ultrasonic frequency of the ultrasonic stirrer is 20kHz, and the stirring frequency is 150 rpm.
Compared with the prior art, the invention has the following beneficial effects:
1) the synthetic route of the invention is different from the prior art, the dimethylchlorosilane reacts with the methyl aluminum chloride under the action of the catalyst to obtain the trimethylchlorosilane, the operation steps are simpler, no waste acid pollution is formed, and the invention is environment-friendly.
2) The zinc and the aluminum are catalysts suitable for the synthesis reaction, and the zinc and the aluminum are easy to absorb moisture and can reduce the catalytic activity of the zinc and the aluminum when being directly used, so that the silica microspheres are firstly prepared by a sol-gel method, and then the zinc and the aluminum are loaded on the basis of the silica microspheres, and the silica can effectively avoid the moisture absorption of the zinc and the aluminum, so that the zinc and the aluminum can fully play the catalytic action, and the yield and the purity of the trimethylchlorosilane are improved.
3) The ultrasonic stirrer used in the step (3) can effectively improve the contact degree between the dimethylchlorosilane and the methyl aluminum chloride as well as the catalyst, thereby further improving the yield and the purity of the trimethylchlorosilane, effectively shortening the reaction time and saving the cost.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1
The method for preparing trimethylchlorosilane from dimethylchlorosilane comprises the following steps of:
(1) adding ammonia water with the pH value of 11, hexadecyl trimethyl ammonium chloride and absolute ethyl alcohol into deionized water, stirring at the temperature of 30 ℃ until the ammonia water, the hexadecyl trimethyl ammonium chloride and the absolute ethyl alcohol are completely dissolved, adding tetraethoxysilane while stirring, heating to 55 ℃, continuing stirring for 2 hours to obtain a reaction liquid, filtering the reaction liquid to obtain a filter cake, drying the filter cake at the temperature of 80 ℃ for 12 hours, and roasting to obtain silicon dioxide, wherein the mass ratio of the ammonia water to the hexadecyl trimethyl ammonium chloride to the absolute ethyl alcohol to the deionized water to the tetraethoxysilane is 16:5:10:250:19, and the heating process during roasting is as follows: firstly, heating from room temperature to 300 ℃ within 30 minutes, keeping the temperature for 30 minutes, then heating to 600 ℃ within 30 minutes, and keeping the temperature for 4 hours;
(2) mixing the silicon dioxide obtained in the step (1), a zinc sulfate solution with the mass concentration of 20% and an aluminum nitrate solution with the mass concentration of 20%, stirring for 5 minutes, adding a potassium borohydride solution with the mass concentration of 20%, wherein the mass ratio of the silicon dioxide to the zinc sulfate solution to the potassium borohydride solution is 1:16:8:18, continuously stirring until no bubbles exist to obtain a reaction solution, filtering the reaction solution to obtain a filter cake, alternately washing the filter cake for 3 times by using deionized water and absolute ethyl alcohol, and drying at 80 ℃ for 12 hours to obtain a catalyst;
(3) adding dimethylchlorosilane, methyl aluminum chloride and methyl chloride in a mass ratio of 1:5:5:0.5, and the catalyst obtained in the step (2) into an ultrasonic stirrer with an ultrasonic frequency of 20kHz and a stirring frequency of 150rpm, introducing nitrogen into the ultrasonic stirrer to exchange air for 2 hours, continuing introducing nitrogen to protect, heating to 200 ℃, starting the ultrasonic stirrer to perform ultrasonic stirring, performing constant-temperature reaction for 4 hours to obtain a reaction liquid, filtering the reaction liquid to obtain a filter cake, and drying the filter cake for 12 hours at 80 ℃ to obtain trimethylchlorosilane.
Example 2
The method for preparing trimethylchlorosilane from dimethylchlorosilane comprises the following steps of:
(1) adding ammonia water with the pH value of 11, hexadecyl trimethyl ammonium chloride and absolute ethyl alcohol into deionized water, stirring at the temperature of 30 ℃ until the ammonia water, the hexadecyl trimethyl ammonium chloride and the absolute ethyl alcohol are completely dissolved, adding tetraethoxysilane while stirring, heating to 55 ℃, continuing stirring for 2 hours to obtain a reaction liquid, filtering the reaction liquid to obtain a filter cake, drying the filter cake at the temperature of 80 ℃ for 12 hours, and roasting to obtain silicon dioxide, wherein the mass ratio of the ammonia water to the hexadecyl trimethyl ammonium chloride to the absolute ethyl alcohol to the deionized water to the tetraethoxysilane is 16:5:10:250:19, and the heating process during roasting is as follows: firstly, heating from room temperature to 300 ℃ within 30 minutes, keeping the temperature for 30 minutes, then heating to 600 ℃ within 30 minutes, and keeping the temperature for 4 hours;
(2) mixing the silicon dioxide obtained in the step (1), a zinc sulfate solution with the mass concentration of 20% and an aluminum nitrate solution with the mass concentration of 20%, stirring for 5 minutes, adding a potassium borohydride solution with the mass concentration of 20%, wherein the mass ratio of the silicon dioxide to the zinc sulfate solution to the potassium borohydride solution is 1:16:8:18, continuously stirring until no bubbles exist to obtain a reaction solution, filtering the reaction solution to obtain a filter cake, alternately washing the filter cake for 3 times by using deionized water and absolute ethyl alcohol, and drying at 80 ℃ for 12 hours to obtain a catalyst;
(3) adding dimethylchlorosilane, methyl aluminum chloride and methyl chloride in a mass ratio of 1:4:4:0.4, and the catalyst obtained in the step (2) into an ultrasonic stirrer with an ultrasonic frequency of 20kHz and a stirring frequency of 150rpm, introducing nitrogen into the ultrasonic stirrer to exchange air for 2 hours, continuing introducing nitrogen to protect, heating to 200 ℃, starting the ultrasonic stirrer to perform ultrasonic stirring, performing constant-temperature reaction for 4 hours to obtain a reaction liquid, filtering the reaction liquid to obtain a filter cake, and drying the filter cake for 12 hours at 80 ℃ to obtain trimethylchlorosilane.
Example 3
The method for preparing trimethylchlorosilane from dimethylchlorosilane comprises the following steps of:
(1) adding ammonia water with the pH value of 11, hexadecyl trimethyl ammonium chloride and absolute ethyl alcohol into deionized water, stirring at the temperature of 30 ℃ until the ammonia water, the hexadecyl trimethyl ammonium chloride and the absolute ethyl alcohol are completely dissolved, adding tetraethoxysilane while stirring, heating to 55 ℃, continuing stirring for 2 hours to obtain a reaction liquid, filtering the reaction liquid to obtain a filter cake, drying the filter cake at the temperature of 80 ℃ for 12 hours, and roasting to obtain silicon dioxide, wherein the mass ratio of the ammonia water to the hexadecyl trimethyl ammonium chloride to the absolute ethyl alcohol to the deionized water to the tetraethoxysilane is 16:5:10:250:19, and the heating process during roasting is as follows: firstly, heating from room temperature to 300 ℃ within 30 minutes, keeping the temperature for 30 minutes, then heating to 600 ℃ within 30 minutes, and keeping the temperature for 4 hours;
(2) mixing the silicon dioxide obtained in the step (1), a zinc sulfate solution with the mass concentration of 20% and an aluminum nitrate solution with the mass concentration of 20%, stirring for 5 minutes, adding a potassium borohydride solution with the mass concentration of 20%, wherein the mass ratio of the silicon dioxide to the zinc sulfate solution to the potassium borohydride solution is 1:16:8:18, continuously stirring until no bubbles exist to obtain a reaction solution, filtering the reaction solution to obtain a filter cake, alternately washing the filter cake for 3 times by using deionized water and absolute ethyl alcohol, and drying at 80 ℃ for 12 hours to obtain a catalyst;
(3) adding dimethylchlorosilane, methyl aluminum chloride and methyl chloride in a mass ratio of 1:6:7:0.6, and the catalyst obtained in the step (2) into an ultrasonic stirrer with an ultrasonic frequency of 20kHz and a stirring frequency of 150rpm, introducing nitrogen into the ultrasonic stirrer to exchange air for 2 hours, continuing introducing nitrogen to protect, heating to 200 ℃, starting the ultrasonic stirrer to perform ultrasonic stirring, performing constant-temperature reaction for 4 hours to obtain a reaction liquid, filtering the reaction liquid to obtain a filter cake, and drying the filter cake for 12 hours at 80 ℃ to obtain trimethylchlorosilane.
Example 4
(1) Adding ammonia water with the pH value of 11, hexadecyl trimethyl ammonium chloride and absolute ethyl alcohol into deionized water, stirring at the temperature of 30 ℃ until the ammonia water, the hexadecyl trimethyl ammonium chloride and the absolute ethyl alcohol are completely dissolved, adding tetraethoxysilane while stirring, heating to 55 ℃, continuing stirring for 2 hours to obtain a reaction liquid, filtering the reaction liquid to obtain a filter cake, drying the filter cake at the temperature of 80 ℃ for 12 hours, and roasting to obtain silicon dioxide, wherein the mass ratio of the ammonia water to the hexadecyl trimethyl ammonium chloride to the absolute ethyl alcohol to the deionized water to the tetraethoxysilane is 16:5:10:250:19, and the heating process during roasting is as follows: firstly, heating from room temperature to 300 ℃ within 30 minutes, keeping the temperature for 30 minutes, then heating to 600 ℃ within 30 minutes, and keeping the temperature for 4 hours;
(2) mixing the silicon dioxide obtained in the step (1), a zinc sulfate solution with the mass concentration of 20% and an aluminum nitrate solution with the mass concentration of 20%, stirring for 5 minutes, adding a potassium borohydride solution with the mass concentration of 20%, wherein the mass ratio of the silicon dioxide to the zinc sulfate solution to the potassium borohydride solution is 1:16:8:18, continuously stirring until no bubbles exist to obtain a reaction solution, filtering the reaction solution to obtain a filter cake, alternately washing the filter cake for 3 times by using deionized water and absolute ethyl alcohol, and drying at 80 ℃ for 12 hours to obtain a catalyst;
(3) adding dimethylchlorosilane, methyl aluminum chloride and chloromethane with the mass ratio of 1:4.5:3:0.45 and the catalyst obtained in the step (2) into an ultrasonic stirrer with the ultrasonic frequency of 20kHz and the stirring frequency of 150rpm, introducing nitrogen into the ultrasonic stirrer to exchange air for 2 hours, continuing introducing nitrogen to protect, heating to 200 ℃, starting the ultrasonic stirrer to perform ultrasonic stirring, performing constant-temperature reaction for 4 hours to obtain reaction liquid, filtering the reaction liquid to obtain a filter cake, and drying the filter cake for 12 hours at the temperature of 80 ℃ to obtain trimethylchlorosilane.
Comparative example 1
Compared with the example 1, the steps (1) and (2) are omitted, the catalyst in the step (3) is untreated zinc and aluminum, and the rest steps are the same as the example 1.
Comparative example 2
Compared with the embodiment 1, the steps (1) and (2) are omitted, the catalyst in the step (3) is replaced by activated carbon loaded zinc and aluminum, and the rest steps are the same as the embodiment 1.
Comparative example 3
Compared with the embodiment 1, the ultrasonic stirrer in the step (3) is replaced by a common stirrer, and the rest steps are the same as the embodiment 1.
Comparative example: example 1 of patent application No. CN 201710039151.1.
Yield of trimethylchlorosilane
The yields of examples 1 to 4, comparative examples 1 to 3 and comparative examples were recorded. The test results are shown in table 1:
TABLE 1
As is apparent from Table 1, the yields of examples 1 to 4 of the present invention are higher than those of the comparative examples. The steps of comparative examples 1-2 are different from example 1 in part, wherein the yield of comparative examples 1 and 3 is reduced a lot, which shows that the higher yield can be achieved by using silica-supported zinc aluminum and an ultrasonic stirrer; the yield of comparative example 2 is reduced to a lesser extent than that of comparative example 1, which shows that the effect of using silica to support zinc and aluminum is better than that of using activated carbon.
Purity of trimethylchlorosilane
The purities of examples 1-4, comparative examples 1-3, and comparative examples were recorded, respectively. The test results are shown in table 2:
| purity (%) | |
| Example 1 | 98.5 |
| Practice ofExample 2 | 98.2 |
| Example 3 | 98.3 |
| Example 4 | 98.1 |
| Comparative example 1 | 91.5 |
| Comparative example 2 | 94.6 |
| Comparative example 3 | 91.0 |
| Comparative example | 90.4 |
TABLE 2
As is apparent from Table 2, the inventive examples 1-4 are all higher in purity than the comparative examples. Comparative examples 1-2 differ from example 1 in part of their steps, wherein comparative examples 1 and 3 both had a significant reduction in purity, indicating that higher purity was achieved using silica-loaded zinc, aluminum, and an ultrasonic stirrer; the purity of comparative example 2 is reduced less than that of comparative example 1, which shows that the effect of using silica to support zinc and aluminum is better than that of using activated carbon to support.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (6)
1. A method for preparing trimethylchlorosilane from dimethylchlorosilane is characterized by comprising the following steps: the method comprises the following steps:
(1) adding ammonia water, hexadecyl trimethyl ammonium chloride and absolute ethyl alcohol into deionized water, stirring at 30 ℃ until the ammonia water, the hexadecyl trimethyl ammonium chloride and the absolute ethyl alcohol are completely dissolved, adding tetraethoxysilane while stirring, heating to 55 ℃, continuing stirring for 2 hours to obtain reaction liquid, filtering the reaction liquid to obtain a filter cake, drying the filter cake at 80 ℃ for 12 hours, and roasting to obtain silicon dioxide;
(2) mixing the silicon dioxide, the zinc sulfate solution and the aluminum nitrate solution obtained in the step (1), stirring for 5 minutes, adding a potassium borohydride solution, continuously stirring until no bubbles exist to obtain a reaction solution, filtering the reaction solution to obtain a filter cake, alternately washing the filter cake for 3 times by using deionized water and absolute ethyl alcohol, and drying at 80 ℃ for 12 hours to obtain a catalyst;
(3) adding dimethylchlorosilane, methyl aluminum chloride, methyl chloride and the catalyst obtained in the step (2) into an ultrasonic stirrer, introducing nitrogen into the ultrasonic stirrer to replace air for 2 hours, continuing introducing nitrogen to protect, heating to 200 ℃, starting the ultrasonic stirrer to perform ultrasonic stirring, performing constant-temperature reaction for 4 hours to obtain reaction liquid, filtering the reaction liquid to obtain a filter cake, and drying the filter cake at 80 ℃ for 12 hours to obtain trimethylchlorosilane.
2. The method for preparing trimethylchlorosilane from dimethylchlorosilane according to claim 1, wherein the reaction is carried out by the following steps: in the step (1), the pH value of ammonia water is 11, and the mass ratio of the ammonia water, the hexadecyl trimethyl ammonium chloride, the absolute ethyl alcohol, the deionized water and the tetraethoxysilane is 16:5:10:250: 19.
3. The method for preparing trimethylchlorosilane from dimethylchlorosilane according to claim 1, wherein the reaction is carried out by the following steps: in the step (1), the temperature rise process during roasting is as follows: the temperature is increased from room temperature to 300 ℃ within 30 minutes, the temperature is kept constant for 30 minutes, then the temperature is increased to 600 ℃ within 30 minutes, and the temperature is kept constant for 4 hours.
4. The method for preparing trimethylchlorosilane from dimethylchlorosilane according to claim 1, wherein the reaction is carried out by the following steps: in the step (2), the mass concentrations of the zinc sulfate solution, the aluminum nitrate solution and the potassium borohydride solution are all 20%, and the mass ratio of the silicon dioxide to the zinc sulfate solution to the aluminum nitrate solution to the potassium borohydride solution is 1:16:8: 18.
5. The method for preparing trimethylchlorosilane from dimethylchlorosilane according to claim 1, wherein the reaction is carried out by the following steps: in the step (3), the mass ratio of the dimethylchlorosilane to the methyl aluminum chloride to the methyl chloride to the catalyst is 1 (4-6) to 3-7 to 0.4-0.6.
6. The method for preparing trimethylchlorosilane from dimethylchlorosilane according to claim 1, wherein the reaction is carried out by the following steps: in the step (3), the ultrasonic frequency of the ultrasonic stirrer is 20kHz, and the stirring frequency is 150 rpm.
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| US5440063A (en) * | 1993-11-05 | 1995-08-08 | Shin-Etsu Chemical Company, Limited | Concurrent preparation of dimethylchlorosilane and triorganochlorosilane |
| JPH08245654A (en) * | 1995-03-15 | 1996-09-24 | Shin Etsu Chem Co Ltd | Production of both dimethylchlorosilane and trimethylchlorosilane |
| CN101531674A (en) * | 2009-04-23 | 2009-09-16 | 嘉兴学院 | Preparation method of methyl chlorosilane |
| CN106883258A (en) * | 2017-01-19 | 2017-06-23 | 浙江硕而博化工有限公司 | HMDO produces trim,ethylchlorosilane new technology |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2403370A (en) * | 1945-03-15 | 1946-07-02 | Gen Electric | Alkylation of halogenosilanes |
| US2427605A (en) * | 1945-03-15 | 1947-09-16 | Gen Electric | Preparation of alkylhalogenosilanes |
| US4155927A (en) * | 1977-10-03 | 1979-05-22 | Wacker-Chemie Gmbh | Process for preparing trimethylchlorosilane |
| US4888435A (en) * | 1989-06-22 | 1989-12-19 | Dow Corning Corporation | Integrated process for alkylation and redistribution of halosilanes |
| US5440063A (en) * | 1993-11-05 | 1995-08-08 | Shin-Etsu Chemical Company, Limited | Concurrent preparation of dimethylchlorosilane and triorganochlorosilane |
| JPH08245654A (en) * | 1995-03-15 | 1996-09-24 | Shin Etsu Chem Co Ltd | Production of both dimethylchlorosilane and trimethylchlorosilane |
| CN101531674A (en) * | 2009-04-23 | 2009-09-16 | 嘉兴学院 | Preparation method of methyl chlorosilane |
| CN106883258A (en) * | 2017-01-19 | 2017-06-23 | 浙江硕而博化工有限公司 | HMDO produces trim,ethylchlorosilane new technology |
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