CN1277833C - Method for synthesizing methyl chlorosilane - Google Patents
Method for synthesizing methyl chlorosilane Download PDFInfo
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- CN1277833C CN1277833C CN 200410084423 CN200410084423A CN1277833C CN 1277833 C CN1277833 C CN 1277833C CN 200410084423 CN200410084423 CN 200410084423 CN 200410084423 A CN200410084423 A CN 200410084423A CN 1277833 C CN1277833 C CN 1277833C
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- high boiling
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- 238000000034 method Methods 0.000 title claims abstract description 37
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- 238000009835 boiling Methods 0.000 claims abstract description 50
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000126 substance Substances 0.000 claims abstract description 37
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 22
- 239000004411 aluminium Substances 0.000 claims abstract description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 21
- 229940050176 methyl chloride Drugs 0.000 claims abstract description 20
- 239000000178 monomer Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 37
- 239000000203 mixture Substances 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 13
- 229910008045 Si-Si Inorganic materials 0.000 claims description 4
- 229910006411 Si—Si Inorganic materials 0.000 claims description 4
- 229910002808 Si–O–Si Inorganic materials 0.000 claims description 3
- 239000012043 crude product Substances 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- -1 methyl chloride disilane compound Chemical class 0.000 claims description 3
- 150000001282 organosilanes Chemical class 0.000 claims description 3
- 238000012546 transfer Methods 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 238000013019 agitation Methods 0.000 abstract 1
- 230000008021 deposition Effects 0.000 abstract 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 230000009257 reactivity Effects 0.000 abstract 1
- 230000009466 transformation Effects 0.000 description 14
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 6
- 238000004821 distillation Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000012263 liquid product Substances 0.000 description 6
- 239000003550 marker Substances 0.000 description 6
- 238000003822 preparative gas chromatography Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- YHQXBTXEYZIYOV-UHFFFAOYSA-N 3-methylbut-1-ene Chemical compound CC(C)C=C YHQXBTXEYZIYOV-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- YQKRNNCUCHBJFP-UHFFFAOYSA-N [SiH3][SiH3].ClC Chemical compound [SiH3][SiH3].ClC YQKRNNCUCHBJFP-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 1
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
The present invention discloses a method for synthesizing methyl chlorosilane. High boiling substances, low boiling substances or the high boiling substances and low boiling substances which are generated in the production process of an organosilicon monomer (CH3)2SiCl2 are used as main raw materials, the main raw materials react with methyl chloride in an agitated bed reaction vessel which is filled with aluminium powder, a methyl chlorosilane monomer is prepared by synthesizing the main raw materials, the methyl chloride and the aluminium powder, and a general formula of the methyl chlorosilane monomer is (CH3)mSiCl4-m(m is a positive integer from 1 to 3); the reaction temperature of the agitated bed is 250 to 400 DEG C., the rotational speed of agitation is 60 to 200 r/min, the reaction pressure of the agitated bed is 0.1 to 1.0MPa, the coefficient of charge of the aluminium powder in the agitated bed is 0.3 to 0.9, and the quality proportion of the methyl chloride to the high boiling substances, the low boiling substances or the high boiling substances and the low boiling substances is 1 to 10:1. The present invention can improve the mass transfer and the heat transfer of the reactant bed by stir, and reduce the influence of the reaction rate and the product content because of the carbon deposition and the devitalization of the aluminium powder in the reaction process; other catalysts need not be added, and high reactivity can be obtained in the reaction process. Tail gas of the methyl chloride which does not react is recycled by freezing and separating. The method provided by the present invention is used for producing the methyl chlorosilane monomer and has lower costs.
Description
Technical field
The present invention relates to organosilane monomer (CH
3)
2SiCl
2The byproduct comprehensive that produces in the production process utilizes research field.Refer more particularly to a kind of with (CH
3)
2SiCl
2The high boiling material that produces in the monomer production process, low-boiling-point substance or high boiling material and low-boiling-point substance are main raw material, with methyl chloride reaction synthesizing methyl-chloro-silane monomer methods in the agitated bed reactor of filling aluminium powder.
Background technology
Organosilicon material mainly is that a class is a main chain with the Si-O key, introduces the macromolecular compound of organic group as side chain on Si again, its excellent performance, function uniqueness.Be widely used in fields such as military project, space flight, medical treatment, chemical industry.Methyl chlorosilane is an important source material of making organosilicon material, and (CH
3)
2SiCl
2Be wherein have the call a kind of.Generally adopt methyl chloride and silica flour to produce (CH at the fluidized-bed reactor synthesis technique at present both at home and abroad through heterogeneous catalytic reaction
3)
2SiCl
2China's methyl chlorosilane industrial synthesis is through the development of recent two decades, and industrial scale also constantly enlarges, and just progressively moves to maturity.
At " direct method " synthetic (CH
3)
2SiCl
2Process in, produce the high boiling material of 5～10wt% and the low-boiling-point substance of 1～3wt% (Shao Yuegang appoints out of the ordinaryly, and Chen Weixin waits .[A] 2002 year Chinese organosilicon seminar collection of thesis [C] .2002.37-40) approximately.Wherein high boiling material be a kind of dark reddish brown, the mixing liquid that has irritating smell and have strong corrosion, the normal temperature and pressure lower density is at 1.13g/cm
3About, 70～215 ℃ of boiling ranges, it mainly consists of and contains Si-Si, Si-O-Si, Si-CH
2The methyl chloride disilane compound of-Si key is formed, and contains a spot of Cu, Al, Zn and silica flour simultaneously, and its topmost composition is (CH
3)
2ClSiSiCl
2CH
3And CH
3Cl
2SiSiCl
2CH
3(Liu Ling, comprehensive utilization of high boiling silane, " petrochemical technology and application ", 2000 (6): 167～70); Low-boiling-point substance is that monomer crude product mid-boiling point is lower than 40 ℃ part, and its main component is (CH
3)
4Si, (CH
3)
2HSiCl, CH
3HSiCl
2, contain a spot of isopentene, iso-pentane, HSiCl simultaneously
3And CH
3Cl.
Chinese patent 92111250.5 discloses the method that methyl chloride disilane cracking in a kind of high boiling material prepares methyl chlorosilane, reaction comprises the formation of Si-Si bond rupture and Si-H key, Si-Cl key, this method is a catalyzer with precious metals such as platinum, palladiums, and its shortcoming is the catalyzer costliness of this method.
Chinese patent 97113213.5 discloses a kind of with methyl chloride disilane and CH in HCl, the high boiling material
3SiCl
3The method of prepared in reaction methyl chlorosilane, catalyst for reaction are aluminum chloride.Chinese patent 97113219.4 discloses a kind of with H
2, high boiling residue and CH
3SiCl
3The method of prepared in reaction methyl chlorosilane, catalyst for reaction are aluminum chloride.Above method needs HCl or H
2Source of the gas, and catalyzer is difficult to recycling utilization.
Summary of the invention
The method that the purpose of this invention is to provide a kind of synthesizing methyl-chloro-silane.
It uses organosilane monomer (CH
3)
2SiCl
2The mixture of the high boiling material that produces in the production process, low-boiling-point substance or high boiling material and low-boiling-point substance is a main raw material, and synthesizing general formula with methyl chloride reaction in the agitated bed reactor of filling aluminium powder is (CH
3)
mSiCl
4-mThe methyl chlorosilane monomer, wherein m is 1～3 positive integer, the agitated bed temperature of reaction is 250～400 ℃, mixing speed is 60r/min～200r/min, the agitated bed reaction pressure is 0.1～1.0MPa, and the coefficient of aluminium powder is 0.3～0.9 in the agitated bed, and methyl chloride is 1～10: 1 with the mixture quality ratio of high boiling material, low-boiling-point substance or high boiling material and low-boiling-point substance, wherein high boiling material is meant that boiling range is 70～215 ℃ a mixture, and it mainly consists of and contains Si-Si, Si-O-Si, Si-CH
2The methyl chloride disilane compound of-Si key; Low-boiling-point substance is meant that monomer crude product mid-boiling point is lower than 40 ℃ mixture, and its main component is (CH
3)
4Si, (CH
3)
2HSiCl, CH
3HSiCl
2
The present invention obtains good improvement by stirring the bed mass transfer that can make reactant with heat transfer, because of of the influence of aluminium powder coking deactivation, need not add other catalyzer in the reaction process and can obtain high reaction activity and high yet in the minimizing reaction process speed of reaction and product content.Unreacted methyl chloride tail gas can recycle by subzero fractionation.Utilize method provided by the invention can produce (CH at lower cost
3)
mSiCl
4-mThe methyl chlorosilane monomeric products of (m is 1～3 positive integer).
Description of drawings
Fig. 1 is ribbon-raker stirrer structural representation;
Fig. 2 is screw rod-raker stirrer structural representation;
Fig. 3 is ribbon-screw rod-scraper plate combined impeller structural representation;
Fig. 4 is a process flow diagram of the present invention.
Embodiment
A kind of method of synthesizing methyl-chloro-silane, its process is as follows: methyl chloride gas after high pressure mass flowmeter metering with the charging of gas mode, high boiling material, low-boiling-point substance or high boiling material and low-boiling-point substance adopt the charging of high pressure micro-measurement pump, and methyl chloride is controlled at 1～10: 1 with high boiling material, low-boiling-point substance or high boiling material and low-boiling-point substance quality ratio; Two strands of materials are in entering agitated bed reactor after the gasification mixing under 150 ℃ in preheater, the coefficient of aluminium powder in agitated bed reactor is 0.4～0.8, and need not add other catalyzer in the aluminium powder, agitated bed reactor adopts preferred combined impeller form (Fig. 3), the agitated bed temperature of reaction is 280～350 ℃, mixing speed is 80r/min～180r/min, the agitated bed reaction pressure is 0.3～0.8MPa, reaction product is through the aluminum chloride trap, condenser separates, and unreacted methyl chloride gas recycles after the refrigerated cylinder condensation is collected through entering after the soap film flowmeter metering.Its process flow diagram is seen Fig. 4.
The aluminium powder that adopts in the embodiment of the invention and the percentage composition of impurity thereof are as shown in table 1.
The quality percentage composition of table 1 aluminium powder and impurity thereof
| Form | Al | Sn | Zn | Cu |
| Content/% | 99.3 | 3.4×10 -3 | 1.5×10 -4 | 0.2×10 -4 |
Agitated bed reactor is made by stainless material in the embodiment of the invention, and the agitated bed reactor useful volume is 8L, internal diameter 320mm, and high 1050mm adopts chuck oil bath heating, and its bottom is selected the sparger of Stainless Steel Cloth as the gas mixing raw material for use.
High boiling material is from industrial production (CH in the embodiment of the invention
3)
2SiCl
2Monomer process mid-boiling point is higher than 70 ℃ by product, and its composition and content are as shown in table 2 through gas-chromatography-analytical reagent composition.
The composition of table 2 high boiling material and quality percentage composition
| Component | Mass percent/% |
| Cl 2CH 3SiSi(CH 3) 3 | 6.97 |
| (CH 3) 3SiSi(CH 3) 3 | 2.19 |
| Cl 2CH 3SiSi(CH 3) 2Cl | 21.23 |
| Cl 2CH 3SiSiCH 3Cl 2 | 43.66 |
| Cl 2CH 3SiCH 2SiCH 3Cl 2 | 3.97 |
| Cl(CH 3) 2SiCH 2SiCH 3Cl 2 | 3.78 |
| Cl(CH 3) 2SiCH 2Si(CH 3) 2Cl 2 | 5.31 |
| Cl(CH 3) 2SiOSi(CH 3) 2Cl | 4.31 |
| Cl(CH 3) 2SiOSiCH 3Cl 2 | 3.87 |
| Cl 2CH 3SiOSiCH 3Cl 2 | 4.86 |
Low-boiling-point substance is from industrial production (CH in the embodiment of the invention
3)
2SiCl
2Monomer process mid-boiling point is lower than 40 ℃ by product, and its composition and content show through gas-chromatography-analytical reagent composition such as table 3.
The composition of table 3 low-boiling-point substance and quality percentage composition
| Component | Mass percent/% |
| C 4H 12Si (tetramethylsilane) | 30.65 |
| C 5H 12(2-methylbutane) | 10.63 |
| C 5H 10(isopentene) | 11.55 |
| C 2H 7ClSi (dimethyl silicane hydroxide) | 16.65 |
| CH 4Cl 2Si (methyl hydrogen dichlorosilane) | 29.03 |
The present invention describes with following embodiment, but can not limit content of the present invention.
Embodiment 1
The coefficient of aluminium powder is 0.5 in the agitated bed reactor, the agitated bed temperature of reaction is 280 ℃, mixing speed is 80r/min, the agitated bed reaction pressure is 0.3MPa, the charging mass ratio of control methyl chloride and high boiling material is 2: 1, collects the interior liquid product of condenser behind the reaction 4h and adopts the vapor-phase chromatography marker method to analyze its composition in conjunction with distillation method; CH wherein
3SiHCl
2Be 0.53%, CH
3SiCl
3Be 16.73%, (CH
3)
2SiCl
2Be 11.91%, (CH
3)
3SiCl is 35.24%, (CH
3)
4Si is 5.09%; The high boiling material transformation efficiency is 69.1% in the entire reaction course, CH
3The Cl transformation efficiency is 78.2%.
Embodiment 2
The coefficient of aluminium powder is 0.8 in the agitated bed reactor, the agitated bed temperature of reaction is 320 ℃, mixing speed is 180r/min, the agitated bed reaction pressure is 0.8MPa, the charging mass ratio of control methyl chloride and high boiling material is 9: 1, collects the interior liquid product of condenser behind the reaction 4h and adopts the vapor-phase chromatography marker method to analyze its composition in conjunction with distillation method; CH wherein
3SiHCl
2Be 1.32%, CH
3SiCl
3Be 18.73%, (CH
3)
2SiCl
2Be 21.91%, (CH
3)
3SiCl is 32.24%, (CH
3)
4Si is 10.09%; The high boiling material transformation efficiency is 83.9% in the entire reaction course, CH
3The Cl transformation efficiency is 49.2%.
Embodiment 3
The coefficient of aluminium powder is 0.5 in the agitated bed reactor, the agitated bed temperature of reaction is 300 ℃, mixing speed is 90r/min, the agitated bed reaction pressure is 0.5MPa, the charging mass ratio of control methyl chloride and low-boiling-point substance is 3: 1, collects the interior liquid product of condenser behind the reaction 4h and adopts the vapor-phase chromatography marker method to analyze its composition in conjunction with distillation method; CH wherein
3SiHCl
2Be 21.23%, CH
3SiCl
3Be 10.73%, (CH
3)
2SiCl
2Be 27.91%, (CH
3)
3SiCl is 20.24%, (CH
3)
4Si is 7.19%; The low-boiling-point substance transformation efficiency is 87.1% in the entire reaction course, CH
3The Cl transformation efficiency is 69.2%.
Embodiment 4
The coefficient of aluminium powder is 0.5 in the agitated bed reactor, the agitated bed temperature of reaction is 300 ℃, mixing speed is 90r/min, the agitated bed reaction pressure is 0.5MPa, the charging mass ratio of control methyl chloride and low-boiling-point substance is 9: 1, collects the interior liquid product of condenser behind the reaction 4h and adopts the vapor-phase chromatography marker method to analyze its composition in conjunction with distillation method; CH wherein
3SiHCl
2Be 18.23%, CH
3SiCl
3Be 10.73%, (CH
3)
2SiCl
2Be 24.91%, (CH
3)
3SiCl is 23.24%, (CH
3)
4Si is 16.19%; The low-boiling-point substance transformation efficiency is 92.8% in the entire reaction course, CH
3The Cl transformation efficiency is 57.3%.
Embodiment 5
The coefficient of aluminium powder is 0.5 in the agitated bed reactor, the agitated bed temperature of reaction is 300 ℃, mixing speed is 80r/min, the agitated bed reaction pressure is 0.3MPa, the first mass ratio by 3: 1 of the high and low thing that boils mixes as raw material, the charging mass ratio of control methyl chloride and high boiling material is 2: 1, collects the interior liquid product of condenser behind the reaction 4h and adopts the vapor-phase chromatography marker method to analyze its composition in conjunction with distillation method; CH wherein
3SiHCl
2Be 8.13%, CH
3SiCl
3Be 10.73%, (CH
3)
2SiCl
2Be 22.91%, (CH
3)
3SiCl is 27.24%, (CH
3)
4Si is 4.19%; Remaining product is unreacted high boiling material and low-boiling-point substance, and the transformation efficiency of high boiling material is 58.3% in the entire reaction course, and the transformation efficiency of low-boiling-point substance is 67.3%, CH
3The Cl transformation efficiency is 64.2%.
Embodiment 6
The coefficient of aluminium powder is 0.8 in the agitated bed reactor, the agitated bed temperature of reaction is 320 ℃, mixing speed is 180r/min, the agitated bed reaction pressure is 0.8MPa, the first mass ratio by 4: 1 of the high and low thing that boils mixes as raw material, the charging mass ratio of control methyl chloride and high boiling material is 9: 1, collects the interior liquid product of condenser behind the reaction 4h and adopts the vapor-phase chromatography marker method to analyze its composition in conjunction with distillation method; CH wherein
3SiHCl
2Be 4.43%, CH
3SiCl
3Be 12.73%, (CH
3)
2SiCl
2Be 24.41%, (CH
3)
3SiCl is 28.94%, (CH
3)
4Si is 8.31%; Remaining product is unreacted high boiling material and low-boiling-point substance, and the transformation efficiency of high boiling material is 46.3% in the entire reaction course, and the transformation efficiency of low-boiling-point substance is 75.8%, CH
3The Cl transformation efficiency is 45.7%.
Claims (3)
1. the method for a synthesizing methyl-chloro-silane is characterized in that, with organosilane monomer (CH
3)
2SiCl
2The mixture of the high boiling material that produces in the production process, low-boiling-point substance or high boiling material and low-boiling-point substance is a main raw material, and synthesizing general formula with methyl chloride reaction in the agitated bed reactor of filling aluminium powder is (CH
3)
mSiCl
4-mThe methyl chlorosilane monomer, wherein m is 1～3 positive integer, the agitated bed temperature of reaction is 250～400 ℃, mixing speed is 60r/min～200r/min, the agitated bed reaction pressure is 0.1～1.0MPa, and the coefficient of aluminium powder is 0.3～0.9 in the agitated bed, and methyl chloride is 1～10: 1 with the mixture quality ratio of high boiling material, low-boiling-point substance or high boiling material and low-boiling-point substance, wherein high boiling material is meant that boiling range is 70～215 ℃ a mixture, and it mainly consists of and contains Si-Si, Si-O-Si, Si-CH
2The methyl chloride disilane compound of-Si key; Low-boiling-point substance is meant that monomer crude product mid-boiling point is lower than 40 ℃ mixture, and its main component is (CH
3)
4Si, (CH
3)
2HSiCl, CH
3HSiCl
2
2. the method for a kind of synthesizing methyl-chloro-silane according to claim 1 is characterized in that, said agitated bed temperature of reaction is 280～350 ℃; Mixing speed is 80r/min～180r/min; The agitated bed reaction pressure is 0.3～0.8MPa, and the coefficient of aluminium powder is 0.4～0.8 in the agitated bed.
3. the method for a kind of synthesizing methyl-chloro-silane according to claim 1 is characterized in that, the agitator of said agitated bed reaction unit is: helical-ribbon type, screw or ribbon-screw rod group are box-like, and are welded with scraper plate in the agitator bottom.
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|---|---|---|---|
| CN 200410084423 CN1277833C (en) | 2004-11-17 | 2004-11-17 | Method for synthesizing methyl chlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410084423 CN1277833C (en) | 2004-11-17 | 2004-11-17 | Method for synthesizing methyl chlorosilane |
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