CN110684045A - Preparation method of vinyl tri (2, 2, 2-trifluoroethoxy) silane - Google Patents
Preparation method of vinyl tri (2, 2, 2-trifluoroethoxy) silane Download PDFInfo
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- CN110684045A CN110684045A CN201910017596.9A CN201910017596A CN110684045A CN 110684045 A CN110684045 A CN 110684045A CN 201910017596 A CN201910017596 A CN 201910017596A CN 110684045 A CN110684045 A CN 110684045A
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- KJYQHPHBKOSZLO-UHFFFAOYSA-N ethenyl-tris(2,2,2-trifluoroethoxy)silane Chemical compound FC(F)(F)CO[Si](OCC(F)(F)F)(OCC(F)(F)F)C=C KJYQHPHBKOSZLO-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000010992 reflux Methods 0.000 claims abstract description 83
- 239000000463 material Substances 0.000 claims abstract description 72
- RHQDFWAXVIIEBN-UHFFFAOYSA-N Trifluoroethanol Chemical compound OCC(F)(F)F RHQDFWAXVIIEBN-UHFFFAOYSA-N 0.000 claims abstract description 66
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000005050 vinyl trichlorosilane Substances 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 239000012043 crude product Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 22
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 22
- 239000000706 filtrate Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims description 66
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 33
- 239000002826 coolant Substances 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000010926 purge Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 claims description 6
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 claims description 4
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- 239000003570 air Substances 0.000 claims description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 2
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 17
- 230000015572 biosynthetic process Effects 0.000 abstract description 16
- 239000000047 product Substances 0.000 abstract description 12
- 239000002994 raw material Substances 0.000 abstract description 8
- 238000000926 separation method Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000007664 blowing Methods 0.000 description 39
- 238000010521 absorption reaction Methods 0.000 description 26
- 230000005587 bubbling Effects 0.000 description 26
- 238000004817 gas chromatography Methods 0.000 description 13
- 238000007599 discharging Methods 0.000 description 12
- 239000012535 impurity Substances 0.000 description 12
- 239000011259 mixed solution Substances 0.000 description 12
- 239000007787 solid Substances 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 125000003277 amino group Chemical group 0.000 description 11
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
- 125000001309 chloro group Chemical group Cl* 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 3
- ZQJDGUZEIULPFY-UHFFFAOYSA-N ethenyl(2,2,2-trifluoroethoxy)silane Chemical compound FC(CO[SiH2]C=C)(F)F ZQJDGUZEIULPFY-UHFFFAOYSA-N 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- -1 polysiloxane Polymers 0.000 description 3
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 125000004793 2,2,2-trifluoroethoxy group Chemical group FC(CO*)(F)F 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- DMZWVCJEOLBQCZ-UHFFFAOYSA-N chloro(ethenyl)silane Chemical compound Cl[SiH2]C=C DMZWVCJEOLBQCZ-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 1
- 229920005560 fluorosilicone rubber Polymers 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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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 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention relates to the field of organic chemistry, and provides a preparation method of vinyl tri (2, 2, 2-trifluoroethoxy) silane in order to solve the problems of solvent use and low reaction yield in the synthesis process of the vinyl tri (2, 2, 2-trifluoroethoxy) silane. Dropwise adding trifluoroethanol into vinyl trichlorosilane which is maintained to a certain temperature in advance, keeping the reaction, heating to reflux, and maintaining the reflux process; cooling the reaction material to room temperature to obtain a synthesized crude product, neutralizing the system by using an alkaline neutralizing agent, filtering, and collecting filtrate; and transferring the collected filtrate to a rectifying tower, and treating to obtain the vinyl tri (2, 2, 2-trifluoroethoxy) silane. The method has the advantages of simple operation condition, simple steps, no use of extra solvent except raw materials for reaction, high yield of target products, easy separation and purification, and suitability for large-scale production.
Description
Technical Field
The invention relates to the field of organic synthesis, in particular to a preparation method of vinyl tri (2, 2, 2-trifluoroethoxy) silane.
Background
The polymer containing fluorine silicon is a novel advanced polymer synthetic material, which takes a repeated-Si-O-Si chain link as a main chain, the fluoroalkyl is connected with Si atoms and is positioned on the side chain of polysiloxane, and the fluorine-containing polysiloxane combines the excellent advantages of high and low temperature resistance, ultraviolet ray resistance, oxidation degradation resistance and the like of an organic silicon material and the unique advantages of chemical stability, weather resistance, corrosion resistance, oxidation resistance and the like of the fluorine-containing material. The vinyl tri (2, 2, 2-trifluoroethoxy) silane molecule not only contains easily polymerized C ═ C double bonds, but also contains hydrolyzable 2,2, 2-trifluoroethoxy functional groups, is an important raw material for preparing fluororubber, and can also be used as a crosslinking agent of silicone resin, an adhesive auxiliary agent and a crosslinking agent for dealcoholization and curing of single-component fluorosilicone rubber.
The Chinese patent CN103012462A discloses a method for synthesizing vinyl tris (2, 2, 2-trifluoroethoxy) silane, which uses vinyl trichlorosilane and trifluoroethanol as raw materials, dichloromethane as a solvent, and adopts an alcoholysis method to prepare vinyl tris (2, 2, 2-trifluoroethoxy) silane under the protection of inert gases such as argon or nitrogen, and the synthesis yield is 63-75%. The vinyl tris (2, 2, 2-trifluoroethoxy) silane synthesis method disclosed in the patent not only has low synthesis yield, but also uses a large amount of dichloromethane as a reaction solvent, so that the single-kettle yield is low, the separation difficulty of the product is increased, and the economic benefit is low.
Disclosure of Invention
In order to improve the synthesis yield and the utilization rate of raw materials of the vinyl tri (2, 2, 2-trifluoroethoxy) silane, reduce the separation load and the energy consumption of a product separation stage and improve the economic benefits of a synthesis and separation purification process, the invention provides a preparation method of the vinyl tri (2, 2, 2-trifluoroethoxy) silane, the preparation method of the vinyl tri (2, 2, 2-trifluoroethoxy) silane disclosed by the invention does not need to use inert gas for protection, in addition, other solvents except for the reaction raw materials of vinyl trichlorosilane and trifluoroethanol are not used in the reaction process, the yield of the target product of vinyl tri (2, 2, 2-trifluoroethoxy) silane is high, the product is easy to separate, and the high-purity vinyl tri (2, 2, 2-trifluoroethoxy) silane can be separated and obtained through conventional reduced pressure rectification.
The invention is realized by the following technical scheme: the preparation method of the vinyl tri (2, 2, 2-trifluoroethoxy) silane comprises the following steps:
(1) dropwise adding trifluoroethanol into vinyl trichlorosilane which is maintained to a certain temperature in advance, keeping the reaction, heating to reflux, and maintaining the reflux process;
the method specifically comprises the following steps: adding a certain amount of vinyl trichlorosilane into a three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom-inserted tube bubbling blowing device and an HCl tail gas absorption device, maintaining the materials in the three-neck flask to a certain temperature, and then dropping trifluoroethanol into the three-neck flask through the constant pressure dropping funnel; after the dropwise addition of the trifluoroethanol is finished, maintaining the reaction at the temperature for a period of time, or raising the temperature of the materials in the reactor to a certain temperature lower than the reflux temperature and maintaining the temperature for a period of time, then raising the temperature of the materials in the reactor to the reflux temperature and maintaining the temperature for a period of time at the reflux temperature; or directly raising the temperature of the materials in the reactor from the reaction temperature to the reflux temperature and maintaining the materials at the reflux temperature for a period of time; when the materials in the reactor are in a reflux state, sending dry purge gas into the three-neck flask through the bottom inserting tube bubbling blowing device to take away generated HCl gas, and discharging the HCl gas after the HCl gas is neutralized by the tail gas absorption device;
the mass ratio of the vinyl trichlorosilane to the trifluoroethanol is 1: 2.5-7.5, and preferably, the mass ratio of the vinyl trichlorosilane to the trifluoroethanol is l: 3.0-6.0.
The dropping time of the trifluoroethanol is 0.2-5 h, the dropping speed is 0.3-9 g/min, the dropping and reaction temperature is-30-70 ℃, preferably, the dropping time of the trifluoroethanol is 0.5-3 h, the dropping speed is 0.5-6 g/min, and the reaction temperature is-20-70 ℃.
Preferably, after the trifluoroethanol is dripped, the reaction is maintained at the temperature of-30 to 70 ℃ for 0.5 to 8 hours, and the reaction is maintained for 1 to 15 hours after the trifluoroethanol is heated to the reflux temperature; more preferably, after the trifluoroethanol is dripped, the reaction is maintained at-20-70 ℃ for 1-6 h, and the reaction is maintained for 2-12 h after the trifluoroethanol is heated to the reflux temperature;
or after the trifluoroethanol is dripped between minus 30 ℃ and 70 ℃, directly heating to the reflux temperature, wherein the maintaining time of the materials in the reactor at the reflux temperature is 1-20 h, and more preferably the maintaining time of the materials in the reactor at the reflux temperature is 2-18 h.
The reflux temperature is determined by the relative composition content of the vinyltrichlorosilane, the trifluoroethanol and the product vinyl (2, 2, 2-trifluoroethoxy) silane generated by the reaction in the reaction kettle, and the reflux temperature is changed according to the feeding ratio of the vinyltrichlorosilane and the trifluoroethanol in the raw materials and the rate of the vinyl (2, 2, 2-trifluoroethoxy) silane generated by the reaction, wherein the reflux temperature is not a constant value.
The temperature of the cooling medium in the reflux condenser is-40-35 ℃, preferably-30 ℃, so that HCl generated in the reaction escapes from the reaction kettle at the reflux temperature and is neutralized and removed in the neutralization device, and trifluoroethanol is prevented from escaping in a gas form at the reflux temperature, and the conversion rate of the vinyl trichlorosilane is reduced.
And introducing purge gas in the reflux process. The purge gas is selected from one or more of compressed air, nitrogen and argon, and preferably, the purge gas is compressed air or nitrogen.
(2) Cooling the reaction material to room temperature to obtain a synthesized crude product, neutralizing the system by using an alkaline neutralizing agent, filtering, and collecting filtrate;
the method specifically comprises the following steps: after blowing air and purging the reaction mixture for a period of time under a reflux state, cooling the materials in the kettle to room temperature, and dropwise adding or introducing a certain amount of alkaline neutralizing agent into the reaction kettle liquid to neutralize residual HCl or chlorine-containing monomers in the reaction crude product; neutralizing the materials in the kettle to be neutral or alkalescent, filtering, and collecting filtrate to obtain light yellow transparent liquid;
the alkaline neutralizing agent is one or more selected from liquid ammonia, aniline, ethylenediamine, diethylamine, n-butylamine, di-n-butylamine, 1-dimethylpropylamine, 1, 2-propylenediamine, 1, 4-butylenediamine, triethylamine and tripropylamine. The dosage of the alkaline neutralizing agent (calculated by amino groups which can be combined with chlorine atoms or Cl & lt- & gt in the alkaline neutralizing agent) is 0.001-0.2 times of the dosage of chlorine atom substances in the raw material vinyl trichlorosilane; preferably, the alkaline neutralizing agent is one of liquid ammonia, aniline, diethylamine, ethylenediamine, triethylamine, tripropylamine and 1, 4-butanediamine, and the amount of the alkaline neutralizing agent (calculated by the amino group capable of being combined with chlorine atom or Cl & lt- & gt in the alkaline neutralizing agent) is 0.0025-0.15 times of the amount of the chlorine atom substances in the raw material vinyl trichlorosilane; particularly preferably, the basic neutralizing agent is one of diethylamine and triethylamine, and the amount of the basic neutralizing agent (based on the amino group capable of being bonded to chlorine atom or Cl-in the basic neutralizing agent) is 0.005 to 0.1 times the amount of the chlorine atom in the raw vinyltrichlorosilane.
(3) And transferring the collected filtrate to a rectifying tower, and treating to obtain the vinyl tri (2, 2, 2-trifluoroethoxy) silane.
The treatment process comprises the following steps: in the rectifying tower, firstly, recovering trifluoroethanol by adopting an atmospheric rectification mode, and then, separating by adopting a rectification mode to obtain the vinyl tri (2, 2, 2-trifluoroethoxy) silane. The separation is preferably carried out by a decompression rectification method, which has the advantages that the rectification operation temperature can be reduced, and the cross-linking polymerization or isomerization reaction of the target product caused by the ring opening of the C ═ C double bond after the vinyl (2, 2, 2-trifluoroethoxy) silane containing the C ═ C double bond is heated for a long time at a high temperature can be avoided.
The chemical structural formula of the vinyl tri (2, 2, 2-trifluoroethoxy) silane is shown as (I):
after the trifluoroethanol is dripped into the vinyl trichlorosilane which is maintained to a certain temperature in advance, the vinyl trichlorosilane is maintained for a period of time at a certain temperature lower than the reflux temperature, and then the temperature is continuously increased to reflux and is maintained for a period of time; or directly heating to reflux for a period of time after the trifluoroethanol is added dropwise. After the reaction materials are cooled to room temperature, neutralizing residual HCl or vinyl chlorosilane in the system by using an alkaline neutralizing agent, rectifying collected filtrate under normal pressure to recover trifluoroethanol after filtering, and then rectifying under reduced pressure to obtain vinyl tris (2, 2, 2-trifluoroethoxy) silane.
Compared with the prior art, the invention has the beneficial effects that:
(1) no other solvent is used except the vinyltrichlorosilane and the trifluoroethanol which participate in the reaction;
(2) the synthesis method is simple, the reaction condition is mild, the side reaction is less, the synthesis yield is high, the product is easy to separate and recycle, the equipment investment is less, the equipment utilization rate is high, and the industrial production is easy to realize.
Drawings
FIG. 1 is a FT-IR spectrum of vinyltris (2, 2, 2-trifluoroethoxy) silane.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention, and the starting materials used in the examples are commercially available or can be prepared by conventional methods.
Example 1
(1) 48.6g (0.3mol) of vinyl trichlorosilane is added into a 250mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCl tail gas absorption device, a cooling medium with the temperature of minus 30 ℃ is introduced into the reflux condenser, the temperature of materials in the three-neck flask is raised to 50 ℃, 105g (1.05mol) of trifluoroethanol is dripped into the three-neck flask through the constant pressure dropping funnel at a constant speed, the time is taken for 60min, and the dripping speed is 1.75 g/min. After the dropwise addition of the trifluoroethanol is finished, maintaining the materials in the three-neck flask at 50 ℃ for 60 min; and then heating to enable the materials in the three-mouth flask to be in a reflux state, simultaneously sending dry compressed air into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, discharging the HCl gas after being neutralized by a tail gas absorption device, cooling the materials in the three-mouth flask to room temperature after the materials are maintained in the reflux state and the blowing state for 2 hours, obtaining 121.0g of a synthesized crude product, analyzing by gas chromatography, wherein the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 86.10%, the content of residual trifluoroethanol is 12.20%, the vinyl trichlorosilane is taken as a key component, and the synthesis yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is calculated to be 98.31%.
(2) 0.8g of triethylamine (containing 0.0079mol of amino groups) is added dropwise into the synthesized crude product while stirring, the mixed solution is measured to be alkalescent by using a precise pH test paper after the dropwise addition is finished, solid impurities are removed by adopting a filtration mode, and then the filtrate is collected.
Example 2
(1) 48.6g (0.3mol) of vinyl trichlorosilane is added into a 250mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCI tail gas absorption device, a cooling medium with the temperature of minus 20 ℃ is introduced into the reflux condenser, after the temperature of materials in the three-neck flask is reduced to minus 20 ℃, 90g (0.90mol) of trifluoroethanol is dripped into the three-neck flask at a constant speed through the constant pressure dropping funnel, the time is 180min, and the dripping speed is 0.5 g/min. After the dropwise addition of the trifluoroethanol is finished, maintaining the materials in the three-neck flask at the temperature of minus 20 ℃ for 90 min; and then heating to enable the materials in the three-mouth flask to be in a reflux state, simultaneously sending dry nitrogen into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, discharging the HCl gas after the HCl gas is neutralized by a tail gas absorption device, cooling the materials in the three-mouth flask to room temperature after the materials are maintained in the reflux state and the blowing state for 4 hours, obtaining 105.2g of a synthesized crude product, analyzing by gas chromatography, wherein the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 92.70%, the content of residual trifluoroethanol is 5.10%, and the synthesis yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is 92.02% by taking vinyl trichlorosilane as a key component.
(2) Dropwise adding 0.7g of triethylamine (containing 0.0069mol of amino) into the synthesized crude product under stirring, measuring the mixed solution to be alkalescent by using a precise pH test paper after dropwise adding, removing solid impurities by adopting a filtering mode, and collecting filtrate.
Example 3
(1) 48.6g (0.3mol) of vinyl trichlorosilane is added into a 250mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCl tail gas absorption device, a cooling medium with the temperature of minus 10 ℃ is introduced into the reflux condenser, after the temperature of materials in the three-neck flask is raised to 60 ℃, 97.5g (0.975mol) of trifluoroethanol is dripped into the three-neck flask through the constant pressure dropping funnel at a constant speed, the time is 60min, and the dripping speed is 1.63 g/min. After the dropwise addition of the trifluoroethanol is finished, the temperature of the materials in the three-mouth flask is raised to reflux, meanwhile, dry nitrogen is sent into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, the HCl gas is discharged after being neutralized by a tail gas absorption device, the materials are cooled to room temperature after the reflux state and the blowing state are maintained for 6 hours, a synthetic crude product 112g is obtained, through gas chromatography analysis, the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 89.10%, the content of residual trifluoroethanol is 9.40%, the vinyl trichlorosilane is taken as a key component, and the synthetic yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is calculated to be 94.15%.
(2) 0.9g of triethylamine (containing 0.0089mol of amino groups) is added into the synthesized crude product dropwise under stirring, the mixed solution is measured to be alkalescent by using a precise pH test paper after the dropwise addition is finished, solid impurities are removed by adopting a filtering mode, and then the filtrate is collected.
Example 4
(1) 48.6g (0.3mol) of vinyl trichlorosilane is added into a 250mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCl tail gas absorption device, a cooling medium at 0 ℃ is introduced into the reflux condenser, 180.0g (1.8mol) of trifluoroethanol is dripped into the three-neck flask at a constant speed through the constant pressure dropping funnel after the materials in the three-neck flask are kept at a constant temperature to 25 ℃, the time is 30min, and the dripping speed is 6 g/min. After the dropwise addition of the trifluoroethanol is finished, maintaining the materials in the three-neck flask at 25 ℃ for 120min, heating to enable the materials in the three-neck flask to be in a reflux state, simultaneously sending dry argon into the three-neck flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, neutralizing the HCl gas through a tail gas absorption device and discharging, after the materials are maintained in the reflux state and a blowing state for 5h, cooling the materials in the three-neck flask to room temperature to obtain a synthetic crude product of 104.5g, analyzing the materials through gas chromatography to obtain the vinyl tris (2, 2, 2-trifluoroethoxy) silane of which the content is 90.50 percent and the residual trifluoroethanol content is 6.80 percent, and calculating to obtain the synthetic yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane of 89.23 percent by taking the vinyl trichlorosilane as a key component.
(2) Dropwise adding 12.8g of tripropylamine (containing 0.0893mol of amino groups) into the synthesized crude product under stirring, measuring the mixed solution to be alkalescent by using a precision pH test paper after dropwise adding, removing solid impurities by adopting a filtering mode, and collecting filtrate.
Example 5
(1) 48.6g (0.3mol) of vinyl trichlorosilane is added into a 250mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCl tail gas absorption device, a cooling medium with the temperature of 10 ℃ is introduced into the reflux condenser, materials in the three-neck flask are heated to 66 ℃, 105g (1.05mol) of trifluoroethanol is dripped into the three-neck flask through the constant pressure dropping funnel at a constant speed, the time is 120min, and the dripping speed is 0.88 g/min. After the dropwise addition of the trifluoroethanol is finished, maintaining the materials in the three-neck flask at 66 ℃ for 60 min; and then heating to enable the materials in the three-mouth flask to be in a reflux state, simultaneously sending dry compressed air into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, discharging the HCl gas after the HCl gas is neutralized by a tail gas absorption device, cooling the materials in the three-mouth flask to room temperature after the materials are maintained in the reflux state and the blowing state for 4 hours, obtaining 118.5g of a synthesized crude product, analyzing by gas chromatography, wherein the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 82.30%, the content of residual trifluoroethanol is 12.20%, and the synthesis yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is 92.02% by taking vinyl trichlorosilane as a key component.
(2) 0.8g of triethylamine (containing 0.0079mol of amino groups) is added dropwise into the synthesized crude product while stirring, the mixed solution is measured to be alkalescent by using a precise pH test paper after the dropwise addition is finished, solid impurities are removed by adopting a filtration mode, and then the filtrate is collected.
Example 6
(1) 48.6g (0.3mol) of vinyl trichlorosilane is added into a 250mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCl tail gas absorption device, a cooling medium with the temperature of minus 10 ℃ is introduced into the reflux condenser, after the temperature of materials in the three-neck flask is raised to 44 ℃, 90g (0.9mol) of trifluoroethanol is dripped into the three-neck flask at a constant speed through the constant pressure dropping funnel, the time is 120min, and the dripping speed is 0.75 g/min. After the dropwise addition of the trifluoroethanol is finished, heating the materials in the three-mouth flask to reflux, simultaneously sending dry compressed air into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCI gas, discharging the HCI gas after the HCI gas is neutralized by a tail gas absorption device, cooling the materials in the three-mouth flask to room temperature after the materials maintain a reflux state and a blowing state for 18 hours, obtaining 105.6g of a synthesized crude product, analyzing by gas chromatography, wherein the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 91.60%, the content of residual trifluoroethanol is 4.20%, and the synthesis yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is 91.26% by taking vinyl trichlorosilane as a key component.
(2) 1.6g of ethylenediamine (containing 0.0532mol of amino groups) is added dropwise into the synthesized crude product under stirring, the mixed solution is measured to be alkalescent by a precision pH test paper after the dropwise addition is finished, solid impurities are removed by adopting a filtration mode, and then the filtrate is collected.
Example 7
(1) 48.6g (0.3mol) of vinyl trichlorosilane is added into a 250mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCI tail gas absorption device, a cooling medium with the temperature of 20 ℃ is introduced into the reflux condenser, after the temperature of materials in the three-neck flask is maintained at 27 ℃, 97.5g (0.975mol) of trifluoroethanol is dripped into the three-neck flask through the constant pressure dropping funnel at a constant speed, the time is 120min, and the dripping speed is 0.81 g/min. After the dropwise addition of the trifluoroethanol is finished, heating the materials in the three-mouth flask for reflux, simultaneously sending dry compressed air into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, discharging the HCl gas after the neutralization of a tail gas absorption device, cooling the materials in the three-mouth flask to room temperature after the materials maintain a reflux state and a blowing state for 2 hours, obtaining 115g of a synthesized crude product, analyzing by gas chromatography, wherein the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 85.30%, the content of residual trifluoroethanol is 10.90%, the vinyl trichlorosilane is taken as a key component, and the synthesis yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is 92.56% by calculation.
(2) Dropwise adding 2.7g of diethylamine (containing 0.0369mol of amino group) into the synthesized crude product under stirring, measuring the mixed solution to be alkalescent by using a precise pH test paper after dropwise adding, removing solid impurities by adopting a filtration mode, and collecting filtrate.
Example 8
(1) 48.6g (0.3mol) of vinyl trichlorosilane is added into a 250mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCl tail gas absorption device, a cooling medium with the temperature of 0 ℃ is introduced into the reflux condenser, the temperature of materials in the three-neck flask is reduced to-10 ℃, 97.5g (0.975mol) of trifluoroethanol is dripped into the three-neck flask through the constant pressure dropping funnel at a constant speed, the time is 180min, and the dripping speed is 0.54 g/min. After the dropwise addition of the trifluoroethanol is finished, heating the materials in the three-mouth flask to reflux, simultaneously sending dry compressed air into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, neutralizing the HCl gas by a tail gas absorption device and then discharging the HCl gas, cooling the materials in the three-mouth flask to room temperature after the materials maintain a reflux state and a blowing state for 14 hours, obtaining 111g of a synthesized crude product, analyzing by gas chromatography, wherein the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 86.0%, the content of residual trifluoroethanol is 11.80%, and the synthesis yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is calculated to be 90.06% by taking vinyl trichlorosilane as a key component.
(2) Dropwise adding 3.4g of aniline (containing 0.0365mol of amino group) into the synthesized crude product under stirring, measuring the mixed solution to be alkalescent by using a precise pH test paper after dropwise adding, removing solid impurities by adopting a filtration mode, and collecting filtrate.
Example 9
(1) 48.6g (0.3mol) of vinyl trichlorosilane is added into a 250mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCI tail gas absorption device, a cooling medium at 0 ℃ is introduced into the reflux condenser, after the temperature of materials in the three-neck flask is maintained at 25 ℃, 105g (1.05mol) of trifluoroethanol is dripped into the three-neck flask at a constant speed through the constant pressure dropping funnel, the time is 180min, and the dripping speed is 0.58 g/min. After the dropwise addition of the trifluoroethanol is finished, heating the materials in the three-neck flask to 65 ℃ and maintaining the temperature for 180 min; and then heating to enable the materials in the three-mouth flask to be in a reflux state, simultaneously sending dry compressed air into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, discharging the HCl gas after the HCl gas is neutralized by a tail gas absorption device, cooling the materials in the three-mouth flask to room temperature after the materials are maintained in the reflux state and the blowing state for 4 hours, obtaining 120g of a synthesized crude product, analyzing by gas chromatography, wherein the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 86.3%, the content of residual trifluoroethanol is 11.0%, and the synthesis yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is calculated to be 97.71% by taking the vinyl trichlorosilane as a key component.
(2) 0.6g of triethylamine (containing 0.0059mol of amino group) is added dropwise into the synthesized crude product under stirring, after the dropwise addition, a mixed solution is measured to be alkalescent by using a precise pH test paper, solid impurities are removed by adopting a filtration mode, and then filtrate is collected.
Example 10
(1) 162g (1.0mol) of vinyl trichlorosilane is added into a 1000mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCl tail gas absorption device, a cooling medium with the temperature of minus 10 ℃ is introduced into the reflux condenser, 400g (4.0mol) of trifluoroethanol is dripped into the three-neck flask through the constant pressure dropping funnel at a constant speed after the temperature of materials in the three-neck flask is reduced to 0 ℃, the time is consumed for 120min, and the dripping speed is 3.33 g/min. After the dropwise addition of the trifluoroethanol is finished, heating the materials in the three-neck flask to 50 ℃, and maintaining the temperature for 150 min; and then heating to enable the materials in the three-mouth flask to be in a reflux state, simultaneously sending dry compressed air into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, discharging the HCl gas after being neutralized by a tail gas absorption device, cooling the materials in the three-mouth flask to room temperature after the materials are maintained in the reflux state and the blowing state for 12 hours, obtaining 451.0g of a synthesized crude product, analyzing by gas chromatography, wherein the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 76.7%, the content of residual trifluoroethanol is 22.2%, the vinyl trichlorosilane is taken as a key component, and the synthesis yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is calculated to be 97.9%.
(2) Dropwise adding 2.0g of triethylamine (containing 0.020mol of amino) into the synthesized crude product under stirring, measuring the mixed solution to be alkalescent by using a precise pH test paper after dropwise adding, removing solid impurities by adopting a filtering mode, and collecting filtrate.
Example 11
(1) 162g (1.0mol) of vinyl trichlorosilane is added into a 1000mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCl tail gas absorption device, a cooling medium with the temperature of 0 ℃ is introduced into the reflux condenser, the temperature of materials in the three-neck flask is raised to 45 ℃, 350g (3.5mol) of trifluoroethanol is dripped into the three-neck flask through the constant pressure dropping funnel at a constant speed, the time is taken for 90min, and the dripping speed is 3.89 g/min. After the dropwise addition of the trifluoroethanol is finished, heating the materials in the three-neck flask to 55 ℃, and maintaining the temperature for 240 min; and then heating to enable the materials in the three-mouth flask to be in a reflux state, simultaneously sending dry compressed air into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, discharging the HCl gas after being neutralized by a tail gas absorption device, cooling the materials in the three-mouth flask to room temperature after the materials are maintained in the reflux state and the blowing state for 6 hours, obtaining 402.0g of a synthesized crude product, analyzing by gas chromatography, wherein the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 86.0%, the content of residual trifluoroethanol is 12.6%, the vinyl trichlorosilane is taken as a key component, and the synthesis yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is calculated to be 97.84%.
(2) 1.6g of triethylamine (containing 0.016mol of amino) is dripped into the synthesized crude product under stirring, the mixed solution is measured to be alkalescent by a precision pH test paper after the dripping is finished, solid impurities are removed by adopting a filtration mode, and then the filtrate is collected.
Example 12
(1) 162g (1.0mol) of vinyl trichlorosilane is added into a 1000mL three-neck flask provided with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube inserting bubbling blowing device and an HCl tail gas absorption device, a cooling medium with the temperature of 30 ℃ is introduced into the reflux condenser, after the temperature of materials in the three-neck flask is kept constant to 10 ℃, 300g (3.0mol) of trifluoroethanol is dripped into the three-neck flask through the constant pressure dropping funnel at a constant speed, the time is 120min, and the dripping speed is 2.5 g/min. After the dropwise addition of the trifluoroethanol is finished, heating the materials in the three-neck flask to 60 ℃, and maintaining the temperature for 360 min; and then heating to enable the materials in the three-mouth flask to be in a reflux state, simultaneously sending dry compressed air into the three-mouth flask through a bottom inserting tube bubbling blowing device to take away generated HCl gas, discharging the HCl gas after the HCl gas is neutralized by a tail gas absorption device, cooling the materials in the three-mouth flask to room temperature after the materials are maintained in the reflux state and the blowing state for 6 hours, obtaining 350.3g of a synthesized crude product, analyzing by gas chromatography, wherein the content of vinyl tris (2, 2, 2-trifluoroethoxy) silane is 92.7%, the content of residual trifluoroethanol is 5.7%, the vinyl trichlorosilane is taken as a key component, and the synthesis yield of the vinyl tris (2, 2, 2-trifluoroethoxy) silane is calculated to be 91.9%.
(2) 7.0g of 1, 4-butanediamine (containing 0.1588mol of amino) is added into the synthesized crude product dropwise under stirring, the mixed solution is measured to be alkalescent by using a precise pH test paper after the dropwise addition is finished, solid impurities are removed by adopting a filtration mode, and then the filtrate is collected.
The synthesized crude products after neutralization and filtration prepared in the examples 1 to 12 are combined and transferred into a rectifying tower with the volume of a tower kettle of 3000mL for separation and purification, wherein the height of the rectifying tower is 1500mm, the inner diameter of the rectifying tower is 40mm, and a stainless steel theta ring filler with the diameter of 3mm is filled. After excessive trifluoroethanol is removed by atmospheric distillation, carrying out reduced pressure distillation under the absolute pressure of 1.525kPa, controlling the reflux ratio at the top of the tower, receiving a positive fraction at the top temperature of 60-61 ℃, and analyzing and confirming the structure of the product by GC-MS, FT-IR, 1H NMR and 13CNMR, wherein the structure is shown as the chemical structural formula of vinyltris (2, 2, 2-trifluoroethoxy) silane, and the content of the vinyltris (2, 2, 2-trifluoroethoxy) silane in the product is determined to be 99.5% by analyzing and confirming the product by gas chromatography GC (HP-5 chromatographic column, the length of the column is 50m, the inner diameter is 0.32mm, the temperature of a column box is 120 ℃, the temperature of a gasification chamber is 200 ℃, and the temperature of a FID detector is 200 ℃).
1H NMR(400MHz，CDCl3)66.36(dd，J＝15.1，3.3Hz，1H)，6.22(dd，J＝20.7，3.3Hz，1H)，5.89(dd，J＝20.7，15.1Hz，1H)，4.15(q，J＝8.4Hz，6H).
13C NMR(101MHz，CDCl3)6141.04(d，J＝2.9Hz)，124.92(s)，123.95(s)，122.16(s)，61.69(s)，61.32(s)，60.96(s)，60.59(s).
The FT-IR spectrum is shown in FIG. 1.
The above analysis results show that the synthesized product of the present invention is vinyltris (2, 2, 2-trifluoroethoxy) silane.
Claims (10)
1. A preparation method of vinyl tri (2, 2, 2-trifluoroethoxy) silane is characterized by comprising the following steps:
(1) dropwise adding trifluoroethanol into vinyl trichlorosilane which is maintained to a certain temperature in advance, keeping the reaction, heating to reflux, and maintaining the reflux process;
(2) cooling the reaction material to room temperature to obtain a synthesized crude product, neutralizing the system by using an alkaline neutralizing agent, filtering, and collecting filtrate;
(3) and transferring the collected filtrate to a rectifying tower, and treating to obtain the vinyl tri (2, 2, 2-trifluoroethoxy) silane.
2. The method of claim 1, wherein the mass ratio of vinyltrichlorosilane to trifluoroethanol is 1: 2.5 ~ 7.5.5.
3. The method for preparing vinyltris (2, 2, 2-trifluoroethoxy) silane according to claim 1, wherein the dropping time of trifluoroethanol is 0.2 ~ 5h, the dropping speed is 0.3 ~ 9g/min, and the temperature for maintaining dropping and reaction is-30 ~ 70 ℃.
4. The method for preparing vinyltris (2, 2, 2-trifluoroethoxy) silane according to claim 1, wherein in step (1), after the trifluoroethanol is added dropwise, the temperature is maintained at-30 ~ 70 ℃, the time is maintained at 0.5 ~ 8h, and the time is maintained at 1 ~ 15h after the temperature is raised to the reflux temperature.
5. The method for preparing vinyl tris (2, 2, 2-trifluoroethoxy) silane according to claim 1, wherein in the step (1), after the trifluoroethanol is added, the temperature is directly raised to the reflux temperature, and the holding time of the materials in the reactor at the reflux temperature is 1 ~ 20 h.
6. The method according to claim 1, wherein the temperature of the cooling medium in the reflux condenser is-40 ~ 35 ℃.
7. The method for preparing vinyltris (2, 2, 2-trifluoroethoxy) silane according to claim 1, wherein a purge gas is introduced during the reflux in step (1).
8. The method for preparing vinyltris (2, 2, 2-trifluoroethoxy) silane according to claim 7, wherein the purge gas is selected from one or more of compressed air, nitrogen and argon.
9. The method for preparing vinyltris (2, 2, 2-trifluoroethoxy) silane according to claim 1, wherein the alkaline neutralizing agent in step (2) is one or more selected from the group consisting of liquid ammonia, aniline, ethylenediamine, diethylamine, n-butylamine, di-n-butylamine, 1-dimethylpropylamine, 1, 2-propylenediamine, 1, 4-butylenediamine, triethylamine, and tripropylamine.
10. The method for preparing vinyl tris (2, 2, 2-trifluoroethoxy) silane according to claim 1, wherein the treatment process in the step (3) is as follows: in the rectifying tower, firstly, recovering trifluoroethanol by adopting an atmospheric rectification mode, and then, separating by adopting a rectification mode to obtain the vinyl tri (2, 2, 2-trifluoroethoxy) silane.
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