CN106349276A - Ester exchange method for preparing vinyl tri-(2- methoxy ethyoxyl)-silane - Google Patents
Ester exchange method for preparing vinyl tri-(2- methoxy ethyoxyl)-silane Download PDFInfo
- Publication number
- CN106349276A CN106349276A CN201610655812.9A CN201610655812A CN106349276A CN 106349276 A CN106349276 A CN 106349276A CN 201610655812 A CN201610655812 A CN 201610655812A CN 106349276 A CN106349276 A CN 106349276A
- Authority
- CN
- China
- Prior art keywords
- ester exchange
- silane
- catalyst
- double salt
- reaction
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 22
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 title claims abstract description 19
- 229920002554 vinyl polymer Polymers 0.000 title claims abstract description 19
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 13
- 125000004185 ester group Chemical group 0.000 title claims abstract 6
- 239000003054 catalyst Substances 0.000 claims abstract description 40
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 5
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 8
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 229910000358 iron sulfate Inorganic materials 0.000 claims 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000032050 esterification Effects 0.000 abstract description 3
- 238000005886 esterification reaction Methods 0.000 abstract description 3
- 230000007935 neutral effect Effects 0.000 abstract description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 150000002148 esters Chemical group 0.000 description 18
- 239000000047 product Substances 0.000 description 16
- 239000007789 gas Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 6
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000007086 side reaction Methods 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 125000003545 alkoxy group Chemical group 0.000 description 3
- -1 alkoxy silane Chemical compound 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000004103 aminoalkyl group Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
Classifications
-
- 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 Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
-
- 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 Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention relates to an ester exchange method for preparing vinyl tri-(2- methoxy ethyoxyl)-silane, and belongs to the technical field of organic chemical. The ester exchange method uses ethylene glycol monomethyl ether and vinyl trimethoxy silane as raw materials, uses neutral double salt type catalyst to perform the ester exchange reaction, and generates tri-(2- methoxy ethyoxyl)-silane. Through filtering and recycling, the catalyst can be repeatedly used. Compared with traditional esterification method, the method has the advantages that 1, the ester exchange reaction process cannot cause the deepened color of product, methanol is removed by distilling after reaction, and the product can be obtained by direct filtering. 2. The catalyst can be recycled and repeatedly used for 10 times, and the activity is still kept.
Description
Technical field
The present invention relates to one kind prepares the ester exchange method of vinyl three-(2- methoxyethoxy)-silane, belong to organic chemistry
Technical field.
Background technology
The structural formula of vinyl three-(2- methoxyethoxy)-silane is as follows:
The common preparation method of vinyl alkoxy silane is to carry out esterification with vinyl trichlorosilane and alcohols material, then
Neutralized, filter, rectification and (such as Chinese patent cn1320600a) is obtained.Reaction equation is as follows:
Primary response:
Side reaction:
The feed ethylene base trichlorosilane that the method uses and the hydrogen chloride gas of by-product are big to the corrosivity of equipment, and by-product
The bad process of hydrogen chloride, generally require and absorbed using alkaline nertralizer, or increase equipment investment, inhaled using falling liquid film
Receive the equipment such as tower and make it be changed into the hydrochloric acid of high concentration and externally sell.Coexist with alcohol additionally, due to hydrogen chloride in this reaction system,
So such as the side reaction in schema can be led to, lead to portioned product polymerization although adopting solvent and the air being dried in its patent
Take away hydrogen chloride gas in time, but the generation of side reaction cannot be inherently eliminated.
Vinyl alkoxy silane can also be by acetylene and the addition in the presence of platinum group catalyst of siloxy hydrogen silane
And obtain (such as patent cn102898458a), its reaction equation is as follows:
Primary response:
Side reaction:
The shortcoming of the method is that the safety cost of raw material acetylene is high, and acetylene is a kind of inflammable and explosive gas, not only meets naked light meeting
Burn quick-fried work, and operating pressure is excessive will also result in acetylene self-polymerization, quick-fried work occurs, so acetylene to be used is as production
Raw material not only needs higher equipment investment, and also needs to lengthy and tedious examination and approval procedures.Another shortcoming of this method is using high
Expensive chloroplatinic acid, as catalyst, increases cost further, and in addition the method is also not fee from the mistake of acetylene and silane containing hydrogen
Degree addition, generates ethyl bis-alkoxysilane, leads to the yield of principal product to reduce.
A kind of method for alkoxy silane continuous ester interchange is disclosed, the method is contained with one kind in us60272909
The organo-silicon compound of at least one alkoxyl react in the presence of the acidity of effective dose or alkaline ester exchange catalyst, and lead to
Cross controlling reaction temperature and constantly steam the low-boiling point alcohol that ester exchange goes out, realize being continuously separated of product stream.Its reaction equation
As follows:
The alkoxy silane that in this ester exchange method, the selection of catalyst is often handed over by ester determining, for example, aminoalkyl alcoxyl
Base silane generally carries out ester exchange using for example corresponding sodium alkoxide of base catalyst, and non-functional or alkyl that alkali is sensitive and alkane
The silane acidic catalyst of epoxide, such as p-methyl benzenesulfonic acid carry out ester exchange.
Content of the invention
It is an object of the invention to: provide one kind to prepare the ester exchange side of vinyl three-(2- methoxyethoxy)-silane
Method, the method includes adding the multiple saline catalyst of ester exchange, and this catalyst is eco-friendly, the ester exchange catalysis to system
Ability is strong, and catalyst is little in the dissolubility of reaction system, recyclable, and activity is unaffected.
The technical scheme is that
One kind prepares the ester exchange method of vinyl three-(2- methoxyethoxy)-silane it is characterised in that it includes following step
Rapid:
1), in flask, add vinyltrimethoxy silane, glycol monoethyl ether is as reaction substrate, vinyl trimethoxy
The amount of base silane and the material of glycol monoethyl ether is than for 1:3.
2) in this mixture, add double salt ester exchange catalyst, double salt ester exchange catalyst is anhydrous potassium aluminium sulfate, sulfur
Any one in sour ferripotassium, Ferrous ammonium sulfate, double salt ester exchange catalyst consumption accounts for the 0.1-0.5% of reactant gross mass.
3), reacting by heating system, makes reaction temperature rise to 70-80 DEG C, vinyltrimethoxy silane and ethylene glycol list
There is ester exchange reaction in methyl ether.
4), after reaction 2h, start to warm up and methanol is evaporated off, when temperature in the kettle rises to 100 DEG C, reclaim and obtain theoretical amount
Methanol, most double salt catalyst also evolution reaction system therewith simultaneously.
5), it is cooled to less than 50 DEG C, filters, obtain double salt ester exchange catalyst and give over to next pot of use, and obtain colourless
Transparent vinyl three-(2- methoxyethoxy)-silane, its yield is 98.5-99.5%, and through gas chromatographic detection, its content is
99.2-99.5%, can use directly as product.
By step 5) reclaim gained double salt catalyst collection, replace raw catelyst to be used for reacting, reuse 10 times, catalysis
The activity of agent remains in that.
In experimentation it was found that after adding multiple saline catalyst, the temperature of control reaction that need not be strict, instead
Should during crude product color do not occur intensification, the phenomenon such as blackening is it means that catalyst stability is good, strong compared to traditional
Acid, strong alkali catalyst, the side reaction that it leads to is less.Based on this, we only need to be evaporated off ester exchange and produce after the completion of ester exchange
Raw methanol, directly filters, you can obtain the product of coloration compliance, and the step eliminating product distillation is gathered.In addition, we are in experiment
In also find, when distilation is carried out for the material containing ethylene linkage, traditional catalyst, alkaline such as Lithium hydrate,
Highly acid such as p-methyl benzenesulfonic acid is all easily caused ethylene linkage polymerization, and affects product yield.And double salt class used in the present invention
Catalyst is then not result in the polymerization of ethylene linkage, even under conditions of vapo(u)rizing temperature is higher.
It is an advantage of the current invention that:
The present invention, with glycol monoethyl ether, vinyltrimethoxy silane as raw material, is carried out using neutral multiple saline catalyst
Ester exchange reaction, generates vinyl three-(2- methoxyethoxy)-silane.Catalyst is recovered by filtration, reusable.Should
Advantage compared with traditional esterifications method for the method is: 1, ester-exchange reaction is not result in that product colour deepens, and has reacted distillation
Remove methanol, direct filtration obtains product.2nd, catalyst is recyclable, reuses 10 times, activity remains in that.
Specific embodiment
Embodiment 1
Vinyltrimethoxy silane is added in equipped with magnetic agitation, thermometer, the 1000ml four-hole boiling flask of spherical condensation tube
148g, glycol monoethyl ether 228g, 1g anhydrous potassium aluminium sulfate.It is warming up to 70-80 DEG C, react 2h.Then heat up and start first is evaporated off
Alcohol, when kettle temperature rises to 100 DEG C, Methanol Recovery finishes, and methanol 94g is obtained.Then lower the temperature, after being cooled under 50 DEG C,
Filter, reclaim and obtain anhydrous potassium aluminium sulfate 0.96g, obtain water white vinyl three-(2- methoxyethoxy)-silane product
278g, yield is 99.5%.It is 99.5% using its content of gas chromatographic detection.
Embodiment 2
Vinyltrimethoxy silane is added in equipped with magnetic agitation, thermometer, the 1000ml four-hole boiling flask of spherical condensation tube
148g, glycol monoethyl ether 228g, 1g anhydrous slufuric acid ferripotassium.It is warming up to 70-80 DEG C, react 4h.Then heat up and start first is evaporated off
Alcohol, when kettle temperature rises to 100 DEG C, Methanol Recovery finishes, and it is 90g that quantity of methyl alcohol is obtained.Then lower the temperature, when being cooled under 50 DEG C
Afterwards, filter, reclaim and obtain double salt ester exchange catalyst 0.96g, obtain vinyl three-(2- methoxyethoxy)-silane product
277g, yield is 99.0%.It is 99.3% using its content of gas chromatographic detection.
Embodiment 3
Vinyltrimethoxy silane is added in equipped with magnetic agitation, thermometer, the 1000ml four-hole boiling flask of spherical condensation tube
148g, glycol monoethyl ether 228g, 1g anhydrous slufuric acid ferrous ammonium.It is warming up to 70-80 DEG C, react 4h.Then heat up and start to be evaporated off
Methanol, when temperature rises to 100 DEG C, Methanol Recovery finishes, and it is 90g that quantity of methyl alcohol is obtained.Then lower the temperature, when be cooled to 50 DEG C it
After lower, filter, reclaim and obtain double salt ester exchange catalyst 0.96g, obtain vinyl three-(2- methoxyethoxy)-silane product
276g, yield is 98.5%.It is 99.3% using its content of gas chromatographic detection.
By example 1-3 it is found that when ester exchange catalyst selects aluminium potassium sulfate, its catalytic effect is more preferable, the response time
Short, and product content is high.So carry out reclaiming from aluminium potassium sulfate reusing experiment.
The catalyst 1g of every pot of input in embodiment 1-3, but reclaiming the catalyst obtaining is 0.96g, in order to keep urging
The amount of agent is constant, so when doing the reply of catalyst using experiment, the new catalyst of 0.04g is added in each pot of meeting.Other
Reaction condition is identical with example 1, so repeats to react 10 times, the yield of product and content results are as follows:
Quality/product theory the quality of product yield=vinyl three-(2- methoxyethoxy)-silane
Claims (1)
1. one kind prepare vinyl three-(2- methoxyethoxy)-silane ester exchange method it is characterised in that it include following
Step:
1), in flask, add vinyltrimethoxy silane, glycol monoethyl ether is as reaction substrate, vinyl trimethoxy
The amount of silane and the material of glycol monoethyl ether is than for 1:3；
2) in this mixture, add double salt ester exchange catalyst, double salt ester exchange catalyst is anhydrous potassium aluminium sulfate, iron sulfate
Any one in potassium, Ferrous ammonium sulfate, double salt ester exchange catalyst consumption accounts for the 0.1-0.5% of reactant gross mass；
3), reacting by heating system, makes reaction temperature rise to 70-80 DEG C, vinyltrimethoxy silane and glycol monoethyl ether
There is ester exchange reaction；
4), after reaction 2h, start to warm up and methanol is evaporated off, when temperature in the kettle rises to 100 DEG C, reclaim the first obtaining theoretical amount
Alcohol, most double salt catalyst also evolution reaction system therewith simultaneously；
5), it is cooled to less than 50 DEG C, filters, obtain double salt ester exchange catalyst and give over to next pot of use, and obtain water white transparency
Vinyl three-(2- methoxyethoxy)-silane, its yield be 98.5-99.5%, through gas chromatographic detection, its content is
99.2-99.5%, can use directly as product；
By step 5) reclaim gained double salt catalyst collection, replace raw catelyst to be used for reacting, reuse 10 times, catalyst
Activity remains in that.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610655812.9A CN106349276B (en) | 2016-08-12 | 2016-08-12 | A kind of ester exchange method preparing vinyl three-(2- methoxyethoxy)-silane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610655812.9A CN106349276B (en) | 2016-08-12 | 2016-08-12 | A kind of ester exchange method preparing vinyl three-(2- methoxyethoxy)-silane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106349276A true CN106349276A (en) | 2017-01-25 |
| CN106349276B CN106349276B (en) | 2019-03-15 |
Family
ID=57844790
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610655812.9A Active CN106349276B (en) | 2016-08-12 | 2016-08-12 | A kind of ester exchange method preparing vinyl three-(2- methoxyethoxy)-silane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106349276B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591106A (en) * | 2019-09-11 | 2019-12-20 | 西北工业大学 | Phosphorus-silicon synergistic flame retardant with hyperbranched structure and preparation method thereof |
| CN112708135A (en) * | 2020-12-29 | 2021-04-27 | 江西晨光新材料股份有限公司 | Degradable organic silicon elastomer and synthesis method thereof |
| CN115317941A (en) * | 2022-08-24 | 2022-11-11 | 东南大学 | Method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic distillation |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085220A (en) * | 1992-09-30 | 1994-04-13 | 哈尔滨化工研究所 | Production method of pollution-free organo-silicon coupling agent and products thereof |
| CN1489593A (en) * | 2001-03-02 | 2004-04-14 | ��³�նٹ�˾ | Continuous transesterification process for alkoxyorganosilicon compounds |
| CN105273851A (en) * | 2014-06-17 | 2016-01-27 | 中国石油化工股份有限公司 | Method for preparing fatty acid ester |
| JP2016053021A (en) * | 2014-09-03 | 2016-04-14 | 国立研究開発法人産業技術総合研究所 | Alkoxysilanes, and oligosiloxanes and method for producing the same |
-
2016
- 2016-08-12 CN CN201610655812.9A patent/CN106349276B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085220A (en) * | 1992-09-30 | 1994-04-13 | 哈尔滨化工研究所 | Production method of pollution-free organo-silicon coupling agent and products thereof |
| CN1489593A (en) * | 2001-03-02 | 2004-04-14 | ��³�նٹ�˾ | Continuous transesterification process for alkoxyorganosilicon compounds |
| CN105273851A (en) * | 2014-06-17 | 2016-01-27 | 中国石油化工股份有限公司 | Method for preparing fatty acid ester |
| JP2016053021A (en) * | 2014-09-03 | 2016-04-14 | 国立研究開発法人産業技術総合研究所 | Alkoxysilanes, and oligosiloxanes and method for producing the same |
Non-Patent Citations (3)
| Title |
|---|
| 林开涵等: "乙烯基三(β-甲氧乙氧基)硅烷的合成及其偶联效果", 《福州大学学报》 * |
| 王珊珊: "新型功能硅烷偶联剂的催化合成、表征新型功能硅烷偶联剂的催化合成、表征新型功能硅烷偶联剂的催化合成、表征与研究", 《曲阜师范大学硕士学位论文》 * |
| 马梅红等,: "乙烯基三(β-甲氧基乙氧基)硅烷的合成工艺研究", 《精细与专用化学品》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591106A (en) * | 2019-09-11 | 2019-12-20 | 西北工业大学 | Phosphorus-silicon synergistic flame retardant with hyperbranched structure and preparation method thereof |
| CN110591106B (en) * | 2019-09-11 | 2022-03-15 | 西北工业大学 | Phosphorus-silicon synergistic flame retardant with hyperbranched structure and preparation method thereof |
| CN112708135A (en) * | 2020-12-29 | 2021-04-27 | 江西晨光新材料股份有限公司 | Degradable organic silicon elastomer and synthesis method thereof |
| CN112708135B (en) * | 2020-12-29 | 2022-10-21 | 江西晨光新材料股份有限公司 | Degradable organic silicon elastomer and synthesis method thereof |
| CN115317941A (en) * | 2022-08-24 | 2022-11-11 | 东南大学 | Method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic distillation |
| CN115317941B (en) * | 2022-08-24 | 2024-06-25 | 东南大学 | Method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic rectification |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106349276B (en) | 2019-03-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106349276A (en) | Ester exchange method for preparing vinyl tri-(2- methoxy ethyoxyl)-silane | |
| CN103833780B (en) | A kind of continuous reaction rectification prepares the processing method of trimethyl borate | |
| CN106748763B (en) | The method of two kettles joint phase-transfer Wittig reaction methyl benzoate | |
| CN102471203B (en) | Process for preparation of hexafluoroacetone monohydrate | |
| CN101948374B (en) | Method for synthesizing alpha-bromoketone and coproducing bromohydrocarbon | |
| CN108558943B (en) | Method for dissociating methyl phosphine dichloride and aluminum trichloride complex | |
| CN100503623C (en) | Process for preparing high-purity butoxy ethyl phosphate | |
| CN100427494C (en) | Prepn of fire retardant resorcinol tetraphenyldiphosphate | |
| CN104803873B (en) | A kind of recycling method of Al resource in Friedel-Crafts reaction | |
| CN103641780A (en) | Method for purifying isoquinoline from crude product of coal tar | |
| CN106397481A (en) | Synthesis method of triethyl phosphonoacetate | |
| CN103613609A (en) | Method for preparing dimethyl phenyl ethoxy silane | |
| US6580000B1 (en) | Process for the manufacture of alkoxysilanes and alkoxy orthosilicates | |
| CN105032473B (en) | A kind of method using the sulfuric acid modified catalyst preparation dialkoxy methanes for the treatment of nanoscale HZSM 5 | |
| CN109053454B (en) | Preparation method of nitromethane and application of poly (4-vinylpyridine) | |
| CN208071616U (en) | Cyclic phosphonic acid anhydrides recycle preparation facilities | |
| CN104151342B (en) | A kind of method synthesizing connection boric acid pinacol ester | |
| US1446872A (en) | Process of making organic oxides | |
| CN102134320B (en) | Preparation method of organic silicon methoxy/ethoxy high boiling silicone oil | |
| CN109096042A (en) | A kind of novel production process of Benzene Chloride | |
| CN114181118A (en) | Synthesis process of fatty acyl taurate | |
| CN103012477A (en) | Preparation method of trialkyl phosphine borofluoride | |
| CN108373485A (en) | A kind of production method and device of cyclic phosphonic acid anhydrides | |
| CN103980307B (en) | The preparation method of 2,4,6-trimethylbenzoyl phenyl phosphinicacid ethyl ester | |
| CN101941988A (en) | Process for preparing triethyl phosphate by utilizing sodium diethyl phosphate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: Luochang Town, Shashi District, Jingzhou City, Hubei Province Patentee after: Hubei Jianghan New Material Co.,Ltd. Address before: 434000 No.2 Road, Shashi District Economic and Technological Development Zone, Jingzhou City, Hubei Province Patentee before: JINGZHOU JIANGHAN FINE CHEMICAL Co.,Ltd. |
|
| CP03 | Change of name, title or address |