CN1320600A - Preparation method of vinyl trimethoxy silane - Google Patents
Preparation method of vinyl trimethoxy silane Download PDFInfo
- Publication number
- CN1320600A CN1320600A CN 00112219 CN00112219A CN1320600A CN 1320600 A CN1320600 A CN 1320600A CN 00112219 CN00112219 CN 00112219 CN 00112219 A CN00112219 A CN 00112219A CN 1320600 A CN1320600 A CN 1320600A
- Authority
- CN
- China
- Prior art keywords
- preparation
- vinyltrimethoxy silane
- hydrogenchloride
- drive
- silane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 9
- 238000005886 esterification reaction Methods 0.000 claims abstract description 6
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000005050 vinyl trichlorosilane Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 230000032050 esterification Effects 0.000 claims description 5
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical class [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 3
- 239000004744 fabric Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000000178 monomer Substances 0.000 abstract description 3
- 229920002379 silicone rubber Polymers 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000003365 glass fiber Substances 0.000 abstract description 2
- 230000007935 neutral effect Effects 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 239000004698 Polyethylene Substances 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000012752 auxiliary agent Substances 0.000 abstract 1
- 239000007822 coupling agent Substances 0.000 abstract 1
- 238000004132 cross linking Methods 0.000 abstract 1
- 239000000945 filler Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- -1 polyethylene Polymers 0.000 abstract 1
- 229920000573 polyethylene Polymers 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
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Abstract
A process for preparing vinyltrimethoxy silane includes esterifying vinyltrichlorosilane with methanol, neutralizing, filtering and rectifying. In the esterification reaction, neutral solubility and dry air are adopted to take away generated hydrogen chloride gas in time, so that the main reaction is facilitated, byproducts are reduced, and the yield and the product quality are improved. The product prepared by the invention is a universal organic silicon coupling agent, is mainly used for the crosslinking of polyethylene, the surface treatment of inorganic auxiliary agents, fillers and glass fibers, the bonding of silicon rubber with metal and fabrics and the like, and can be copolymerized with various acrylic monomers, thereby being used for preparing high-performance exterior wall coatings and having wide popularization and application prospects.
Description
The present invention relates to a kind of preparation method's of vinyl silanes, particularly vinyltrimethoxy silane preparation method.
Vinyltrimethoxy silane is mainly used in surface treatments such as multiple inorganic assistant agent, weighting agent and glass fibre, improve its electrical property, wear resisting property and flame retardant resistance, and " bridge " that play between organism and inorganics acts on, making both fine connections, is the good accelerator of silicon rubber and metal, adhering fabric.The preparation method of existing vinyltrimethoxy silane carries out esterification by vinyl trichloro silane and methyl alcohol, finishes after neutralization, filtration, rectifying.Do not drive or drive seldom owing in the reaction hydrogen oxide that generates added, reaction is carried out to contrary direction, thereby by product is more, influences yield and quality product.The finished product that makes can not with multiple Acrylic Acid Monomer copolymerization, therefore can not be used to prepare high performance exterior coating, range of application has very big limitation.
The objective of the invention is to overcome weak point of the prior art, a kind of yield height, good product quality are provided, can be used to prepare the preparation method of the vinyltrimethoxy silane of high performance outer wall paint.
Technical scheme of the present invention is: vinyltrimethoxy silane carries out esterification by vinyl trichloro silane and methyl alcohol, through neutralization, filtration, rectifying totally four operations be prepared from.Improvements are that described esterification is in the presence of sherwood oil, press mole ratio 1: 3.6 by vinyl trichloro silane and methyl alcohol, carry out two-way dropwise reaction under 45 ± 4 ℃ of conditions of normal pressure, and reaction equation is:
Above-mentioned being reflected at dripped after 4～5 hours, drove hydrogenchloride with dried compressed air, dripped to be warming up to 60 ± 2 ℃ after finishing, and continued to drive hydrogenchloride with dried compressed air Cl to the solution
-Content is reduced to 1.5% cooling discharge when following, is neutralized to PH=7 with saturated sodium methylate.
Among the present invention, owing to the hydrogenchloride of taking away with the vaporised gas that adds the neutral solvent sherwood oil in the reactor in advance in the reaction, impel reaction to carry out to positive dirction, reduce the generation of by product, further drive hydrogen chloride gas with the pressurized air bubbling that dehydrates in addition, thereby improve the yield and the quality product of vinyltrimethoxy silane greatly, again through the sodium methylate neutralization, filter and desalt, can get the product of content more than 97% after the rectifying.The vinyltrimethoxy silane that is made by the present invention not only can be used for the good accelerator of inorganic assistant agent, weighting agent, fiberglass surfacing processing and silicon rubber and metal, adhering fabric, and because its content raising, increased activity, can with multiple Acrylic Acid Monomer copolymerization, be used to prepare high performance outer wall paint, applied range.
Further specify technical process example of the present invention (as figure) below
Claims (3)
1, a kind of preparation method of vinyltrimethoxy silane, carry out esterification by vinyl trichloro silane and methyl alcohol, through neutralization, filtration, rectifying totally four operations finish, it is characterized in that described esterification is in the presence of sherwood oil, pressed mole ratio 1: 3.6 by vinyl trichloro silane and methyl alcohol, carry out two-way dropwise reaction under 45 ± 4 ℃ of conditions of normal pressure, reaction equation is:
2, press the preparation method of the described vinyltrimethoxy silane of claim 1, it is characterized in that being reflected at dropping after 4～5 hours, drive hydrogenchloride with exsiccant pressurized air, dropping is warming up to 60 ± 2 ℃ after finishing, continue to drive hydrogenchloride Cl to the solution with exsiccant pressurized air
-Content is below 1.5%.
3, by the preparation method of the described vinyltrimethoxy silane of claim 2, it is characterized in that treating Cl in the solution
-Content is reduced to 1.5% cooling discharge when following, is neutralized to PH=7 with saturated sodium methylate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00112219 CN1320600A (en) | 2000-04-21 | 2000-04-21 | Preparation method of vinyl trimethoxy silane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00112219 CN1320600A (en) | 2000-04-21 | 2000-04-21 | Preparation method of vinyl trimethoxy silane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1320600A true CN1320600A (en) | 2001-11-07 |
Family
ID=4582096
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00112219 Pending CN1320600A (en) | 2000-04-21 | 2000-04-21 | Preparation method of vinyl trimethoxy silane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1320600A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100334096C (en) * | 2002-10-11 | 2007-08-29 | 陶氏康宁公司 | Method for preparing organofunctional silanes |
| CN100366661C (en) * | 2006-02-17 | 2008-02-06 | 浙江大学 | Synthesis method of silicane coupling agent having long chain polyether chain section |
| CN102924498A (en) * | 2012-10-09 | 2013-02-13 | 湖北兴发化工集团股份有限公司 | Method for preparing unsaturated alkyl alkoxy silanes |
| CN103788120A (en) * | 2013-12-31 | 2014-05-14 | 湖北力美达硅氟科技有限公司 | Solid-state silane coupling agent (vinyl octadecyl silicate) as well as preparation method and application thereof |
| CN105061483A (en) * | 2015-08-19 | 2015-11-18 | 湖北兴瑞化工有限公司 | Method for preparing hexamethyldisiloxane by using organic silicon by-product |
| CN114805427A (en) * | 2022-04-06 | 2022-07-29 | 浙江锦华新材料股份有限公司 | Solvent-free synthesis method of vinyl trimethoxy silane |
| CN115160358A (en) * | 2022-08-04 | 2022-10-11 | 浙江锦华新材料股份有限公司 | Method for producing vinyltriethoxysilane by supergravity method |
-
2000
- 2000-04-21 CN CN 00112219 patent/CN1320600A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100334096C (en) * | 2002-10-11 | 2007-08-29 | 陶氏康宁公司 | Method for preparing organofunctional silanes |
| CN100366661C (en) * | 2006-02-17 | 2008-02-06 | 浙江大学 | Synthesis method of silicane coupling agent having long chain polyether chain section |
| CN102924498A (en) * | 2012-10-09 | 2013-02-13 | 湖北兴发化工集团股份有限公司 | Method for preparing unsaturated alkyl alkoxy silanes |
| CN103788120A (en) * | 2013-12-31 | 2014-05-14 | 湖北力美达硅氟科技有限公司 | Solid-state silane coupling agent (vinyl octadecyl silicate) as well as preparation method and application thereof |
| CN103788120B (en) * | 2013-12-31 | 2015-02-18 | 湖北力美达硅氟科技有限公司 | Solid-state silane coupling agent (vinyl octadecyl silicate) as well as preparation method and application thereof |
| CN105061483A (en) * | 2015-08-19 | 2015-11-18 | 湖北兴瑞化工有限公司 | Method for preparing hexamethyldisiloxane by using organic silicon by-product |
| CN114805427A (en) * | 2022-04-06 | 2022-07-29 | 浙江锦华新材料股份有限公司 | Solvent-free synthesis method of vinyl trimethoxy silane |
| CN114805427B (en) * | 2022-04-06 | 2024-05-14 | 浙江锦华新材料股份有限公司 | Solvent-free synthesis method of vinyl trimethoxy silane |
| CN115160358A (en) * | 2022-08-04 | 2022-10-11 | 浙江锦华新材料股份有限公司 | Method for producing vinyltriethoxysilane by supergravity method |
| CN115160358B (en) * | 2022-08-04 | 2024-04-12 | 浙江锦华新材料股份有限公司 | Method for producing vinyl triethoxysilane by supergravity method |
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| C06 | Publication | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |