CN107987100A - A kind of synthetic method of environment-friendly type silane crosslinker - Google Patents
A kind of synthetic method of environment-friendly type silane crosslinker Download PDFInfo
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- CN107987100A CN107987100A CN201711423973.6A CN201711423973A CN107987100A CN 107987100 A CN107987100 A CN 107987100A CN 201711423973 A CN201711423973 A CN 201711423973A CN 107987100 A CN107987100 A CN 107987100A
- Authority
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- Prior art keywords
- ethyl lactate
- reaction
- triethylamine
- methyl
- petroleum ether
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- 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.)
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 24
- 239000004971 Cross linker Substances 0.000 title claims abstract description 13
- 238000010189 synthetic method Methods 0.000 title claims abstract description 9
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 claims abstract description 64
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 45
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229940116333 ethyl lactate Drugs 0.000 claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 239000003208 petroleum Substances 0.000 claims abstract description 17
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 16
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005055 methyl trichlorosilane Substances 0.000 claims abstract description 13
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 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
- 239000007789 gas Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims description 16
- 238000013019 agitation Methods 0.000 claims description 10
- 238000004064 recycling Methods 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 6
- 238000005292 vacuum distillation Methods 0.000 claims description 6
- 239000012452 mother liquor Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 4
- 230000007613 environmental effect Effects 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000012065 filter cake Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims 1
- 239000005052 trichlorosilane Substances 0.000 claims 1
- 230000003292 diminished effect Effects 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000009972 noncorrosive effect Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- MISQRWJCJZSTQT-UHFFFAOYSA-N [SiH4].C(C(O)C)(=O)OCC Chemical compound [SiH4].C(C(O)C)(=O)OCC MISQRWJCJZSTQT-UHFFFAOYSA-N 0.000 abstract 2
- 208000012839 conversion disease Diseases 0.000 abstract 1
- 239000000565 sealant Substances 0.000 description 13
- 239000012530 fluid Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- -1 acetic acid small-molecule Chemical class 0.000 description 5
- 239000003431 cross linking reagent Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- LIWAQLJGPBVORC-UHFFFAOYSA-N N-ethyl-N-methylamine Natural products CCNC LIWAQLJGPBVORC-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- FSEUPUDHEBLWJY-HWKANZROSA-N diacetylmonoxime Chemical compound CC(=O)C(\C)=N\O FSEUPUDHEBLWJY-HWKANZROSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 235000014214 soft drink Nutrition 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The present invention relates to a kind of synthetic method of environment-friendly type silane crosslinker, belongs to silane crosslinker synthesis field.For the present invention using methyl trichlorosilane, ethyl lactate and triethylamine as raw material, petroleum ether is solvent, reaction generation three ethyl lactate silane of methyl（MTELS）.It is filtered under diminished pressure after reaction, removes triethylamine hydrochloride, is then distilled to recover solvent petroleum ether, obtains three ethyl lactate silane crosslinker of product methyl.The present invention has the advantages that easy to operate, reaction conversion ratio is high, and yield is high, stay in grade, and product is safe to use environmentally friendly, and the non-corrosive hydrogen chloride gas of whole process, environmentally safe.
Description
Technical field
The present invention relates to a kind of synthetic method of environment-friendly type silane crosslinker, belongs to silane crosslinker synthesis field.
Background technology
Organosilicon sealant mainly has three kinds of de-oxime type, dealcoholized type and de- acetic acid type at present, its sulfidation discharges respectively
Go out oximes, alcohols and acetic acid small-molecule substance.Wherein, oximes small molecule has been considered having potential carcinogenesis, alcohol to human body
Micromolecular particularly methanol, eyesight, respiratory system to human body etc. also have negative effect, the penetrating odor of acetic acid small molecule
Also do not liked for major part construction personnel.Fluid sealant equally also will as one of material indispensable in electronic enterprises
Adapt to the higher and higher technical requirements that industrial chain Downstream Market is proposed.Organosilicon sealant because its excellent high-low temperature resistant,
Ageing-resistant, dielectric properties and low-corrosiveness etc., are applied very generally in electronic enterprises, such as pcb board coating, electronics member device
Part adhering and sealing etc..In use, volatile matter is larger for de-oxime type, and is corrosive to many materials such as copper sheet, for ring
Requirement in terms of guarantor, the organosilicon sealant suitable for electronic enterprises are mainly dealcoholized type.With high-precision electronics industry
Development, common dealcoholized type organosilicon sealant can not meet the market demand, and exploitation novel organosilicon fluid sealant is extremely necessary.
Ethyl lactate has special Rum, fruit and cream fragrance, is a kind of important fine chemical material.Food
Industry is widely used in spices, spices synergist and Wine additive, can be used to allocate food flavor, wine essence and foodstuff flavouring
Fumet, it is also possible to modulate soft drink and inebriant.Simultaneously because ethyl lactate has, nontoxic, dissolubility is good, is not easy to wave
Send out, have the features such as fruity smell, and there is biodegradable, therefore ethyl lactate is great Development volue and application prospect again
" green solvent ".Demulsification acetoacetic ester type fluid sealant is a kind of organosilicon sealant using novel crosslinker, it uses lactic acid
Ethyl ester type crosslinking agent, discharges nontoxic ethyl lactate small molecule in reaction process, harmless, to copper non-corrosiveness, and
Fluid sealant volatile matter is low, superior electrical property, is very suitable for the more demanding high-precision electronics industry of glue.
The content of the invention
It is an object of the present invention to provide a kind of technique is simple, product with stable quality, high income, and to environment without any
Pollution, the synthetic method of the environment-friendly type silane crosslinker of safety and environmental protection.
The technical scheme is that：
A kind of synthetic method of environment-friendly type silane crosslinker, it is characterised in that it includes the following steps：
1）, a certain amount of ethyl lactate, three second are put into the reactor with mechanical agitation, constant pressure funnel and condenser
Amine, solvent petroleum ether（60-90 DEG C of boiling range）.
2）, weigh a certain amount of methyl trichlorosilane and be added in constant pressure funnel, be every point in mechanical agitation speed
Under conditions of 100 ~ 300 turns of clock, controlling reaction temperature starts dropwise reaction, during the dropwise addition of methyl trichlorosilane at 30 ~ 100 DEG C
Between for 3 ~ 6 it is small when, react generation hydrogen chloride gas absorbed by triethylamine after form triethylamine hydrochloride.
3）, after reaction, filtered by water vacuum pump pressure, remove the triethylamine hydrochloride in reaction system, with few
The petroleum ether filter cake of amount.
4）, mother liquor pass through air-distillation and recycle petroleum ether solvent, the then a small amount of excessive ethyl lactate of vacuum distillation recycling
And a small amount of impurity component is removed, the product of colourless transparent liquid is obtained after filtering.
5）, triethylamine hydrochloride neutralized by sodium hydrate aqueous solution, be dry, recycling.Whole process safety, ring
Protect, superior product quality, do not produce a large amount of corrosive hydrogen chloride gas and produce.
Its chemical equation is as follows：
The molar ratio of the methyl trichlorosilane, triethylamine and ethyl lactate is 1：3：3.3.
The solvent petroleum ether quality is three kinds of total matter of reaction raw materials such as methyl trichlorosilane, triethylamine and ethyl lactate
The 50 ~ 100% of amount.
The reaction principle of the present invention：
The present invention is to put into methyl trichlorosilane, triethylamine, ethyl lactate and petroleum ether solvent in reactor by a certain percentage
Reacted, the hydrochloride of reaction generation three ethyl lactate base silane of methyl and triethylamine, wherein petroleum ether solvent was reacting
Effect in journey is to reduce the viscosity of mixture.
After reaction, then system is recycled by air-distillation again first through being filtered under diminished pressure removing triethylamine hydrochloride
Petroleum ether solvent, vacuum distillation obtain product.For triethylamine hydrochloride by neutralizing, after drying process, obtained triethylamine can be with
Absorbent as hydrogen chloride gas again.Whole building-up process, molar yield more than 94.0%, product content reaches 94.0 ~
96.0%, effective content reaches（The sum of main content and effective high-boiling components component content）To 98.0% or so, chloride ion content is less than
5ppm, and material can be recycled fully, non-corrosive hydrogen chloride gas produces, process safety, environmental protection.
The advantages of present invention is compared with existing product is as follows：
（1）The present invention is reacted by methyl trichlorosilane and ethyl lactate first using under the conditions of triethylamine and solvent petroleum ether
Three ethyl lactate base silane crosslinking agent of synthesizing methyl, product are mainly used in organosilicon neutrality fluid sealant, to copper non-corrosiveness,
And fluid sealant volatile matter is low, superior electrical property, is very suitable for the more demanding high-precision electronics industry of glue.
（2）During ketoxime type crosslinking agent use, the diacetylmonoxime chemical substance of release is a kind of potential carcinogenic substance, by
European Union disables in many occasions, limits use scope and potentiality.Ketoxime type crosslinking agent is substituted using ethyl lactate type crosslinking agent,
Nontoxic ethyl lactate small molecule is discharged in reaction process, it is harmless.
（3）Hydrogen chloride absorbs to form triethylamine hydrochloride by triethylamine in the reaction process of the present invention, and precipitation is easy to point
From not producing a large amount of corrosive hydrogen chloride gas, technique is simple, safety and environmental protection.
Three ethyl lactate base silane of methyl provided by the invention, has good cross-linking effect, the demulsification acid second worked it out
Ester type organosilicon sealant has excellent insulation performance, and fluid sealant volatile matter is low, is very suitable for copper metal non-corrosiveness
High high-precision electronics industry is required with glue, existing similar-type products methyl tributanoximo silane can be substituted completely.
Embodiment
Embodiment 1：
Ethyl lactate is put into tetra- mouthfuls of reaction flasks of 3000ml with mechanical agitation, constant pressure funnel and condenser
779.5g and triethylamine 607.1g, adds solvent petroleum ether 1179.9g, methyl trichlorine is added in most backward constant pressure funnel
Silane 299g.Methyl trichlorosilane is added dropwise under 300 turns per minute of mechanical agitation.Temperature control is at 30 DEG C, time for adding control
System is when 6 is small.After dripping, the reaction was continued 30 minutes, reaction generation three ethyl lactate base silane of methyl and triethylamine hydrochloride
Mixture.It is filtered under diminished pressure after reaction, except the triethylamine hydrochloride of dereaction generation, mother liquor air-distillation recycling design oil
The ethyl lactate raw material of ether, the then a small amount of excess of vacuum distillation recycling.Obtain the three ethyl lactate base silane of methyl of water white transparency
Finished product 770g, product yield reach 95.6%, and main content 95.1%, effective content reaches 98.0%, chloride ion content 2ppm.
Embodiment 2：
Ethyl lactate is put into tetra- mouthfuls of reaction flasks of 3000ml with mechanical agitation, constant pressure funnel and condenser
779.5g and triethylamine 607.1g, is adding solvent petroleum ether 1011.4g, methyl trichlorine is added in most backward constant pressure funnel
Silane 299g.Methyl trichlorosilane is added dropwise under 300 turns per minute of mechanical agitation.Temperature control is at 50 DEG C, time for adding control
System is when 5 is small.After dripping, the reaction was continued 30 minutes, reaction generation three ethyl lactate base silane of methyl and triethylamine hydrochloride
Mixture.It is filtered under diminished pressure after reaction, except the triethylamine hydrochloride of dereaction generation, mother liquor air-distillation recycling design oil
The ethyl lactate raw material of ether, the then a small amount of excess of vacuum distillation recycling.Finally obtain the three ethyl lactate base of methyl of water white transparency
Silane finished product 764.8g, product yield reach 94.6%, and main content 94.3%, effective content reaches 97.6%, chloride ion content
3ppm。
Embodiment 3：
Ethyl lactate is put into tetra- mouthfuls of reaction flasks of 3000ml with mechanical agitation, constant pressure funnel and condenser
779.5g and triethylamine 607.1g, is adding solvent petroleum ether 842.8g, methyl trichlorine is added in most backward constant pressure funnel
Silane 299g.Methyl trichlorosilane is added dropwise under 300 turns per minute of mechanical agitation.Temperature control is at 70 DEG C, time for adding control
System is when 4 is small.After dripping, the reaction was continued 30 minutes, reaction generation three ethyl lactate base silane of methyl and triethylamine hydrochloride
Mixture.It is filtered under diminished pressure after reaction, except the triethylamine hydrochloride of dereaction generation, mother liquor air-distillation recycling design oil
The ethyl lactate raw material of ether, the then a small amount of excess of vacuum distillation recycling.Finally obtain the three ethyl lactate base of methyl of water white transparency
Silane finished product 760.5g, product yield reach 94.7%, and main content 94.4%, effective content reaches 98.3%, chloride ion content
2ppm。
Claims (3)
1. a kind of synthetic method of environment-friendly type silane crosslinker, it is characterised in that it includes the following steps：
1）, a certain amount of ethyl lactate, three second are put into the reactor with mechanical agitation, constant pressure funnel and condenser
Amine, solvent petroleum ether（60-90 DEG C of boiling range）；
2）, weigh a certain amount of methyl trichlorosilane and be added in constant pressure funnel, be per minute 100 in mechanical agitation speed
Under conditions of ~ 300 turns, controlling reaction temperature starts dropwise reaction at 30 ~ 100 DEG C, the time for adding of methyl trichlorosilane for 3 ~
6 it is small when, react generation hydrogen chloride gas absorbed by triethylamine after form triethylamine hydrochloride；
3）, after reaction, filtered by water vacuum pump pressure, the triethylamine hydrochloride in reaction system removed, with a small amount of
Petroleum ether filter cake；
4）, mother liquor petroleum ether solvent is recycled by air-distillation, then a small amount of excessive ethyl lactate of vacuum distillation recycling and remove
A small amount of impurity component is removed, the product of colourless transparent liquid is obtained after filtering；
5）, triethylamine hydrochloride neutralized by sodium hydrate aqueous solution, be dry, recycling；
Whole process safety, environmental protection, superior product quality, does not produce a large amount of corrosive hydrogen chloride gas and produces.
A kind of 2. synthetic method of environment-friendly type silane crosslinker according to claim 1, it is characterised in that the methyl
The molar ratio of trichlorosilane, triethylamine and ethyl lactate is 1：3：3.3.
A kind of 3. synthetic method of environment-friendly type silane crosslinker according to claim 1, it is characterised in that the solvent
Petroleum ether quality is methyl trichlorosilane, the 50 ~ 100% of three kinds of reaction raw materials gross masses of triethylamine and ethyl lactate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711423973.6A CN107987100A (en) | 2017-12-25 | 2017-12-25 | A kind of synthetic method of environment-friendly type silane crosslinker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711423973.6A CN107987100A (en) | 2017-12-25 | 2017-12-25 | A kind of synthetic method of environment-friendly type silane crosslinker |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107987100A true CN107987100A (en) | 2018-05-04 |
Family
ID=62042664
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711423973.6A Pending CN107987100A (en) | 2017-12-25 | 2017-12-25 | A kind of synthetic method of environment-friendly type silane crosslinker |
Country Status (1)
| Country | Link |
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| CN (1) | CN107987100A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375096A (en) * | 2020-11-24 | 2021-02-19 | 江西晨光新材料股份有限公司 | Synthesis method of amidosilane |
| CN113583037A (en) * | 2021-08-27 | 2021-11-02 | 湖北新蓝天新材料股份有限公司 | Environment-friendly silane coupling agent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120016072A1 (en) * | 2007-08-31 | 2012-01-19 | NITRO-CHEME ASCHAU GmbH | hardener for silicone rubber materials |
| CN106749381A (en) * | 2016-11-17 | 2017-05-31 | 湖北新蓝天新材料股份有限公司 | A kind of preparation method of three lactic acid alkyl esters silane |
-
2017
- 2017-12-25 CN CN201711423973.6A patent/CN107987100A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120016072A1 (en) * | 2007-08-31 | 2012-01-19 | NITRO-CHEME ASCHAU GmbH | hardener for silicone rubber materials |
| CN106749381A (en) * | 2016-11-17 | 2017-05-31 | 湖北新蓝天新材料股份有限公司 | A kind of preparation method of three lactic acid alkyl esters silane |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375096A (en) * | 2020-11-24 | 2021-02-19 | 江西晨光新材料股份有限公司 | Synthesis method of amidosilane |
| CN112375096B (en) * | 2020-11-24 | 2023-05-02 | 江西晨光新材料股份有限公司 | Synthesis method of amido silane |
| CN113583037A (en) * | 2021-08-27 | 2021-11-02 | 湖北新蓝天新材料股份有限公司 | Environment-friendly silane coupling agent and preparation method thereof |
| CN113583037B (en) * | 2021-08-27 | 2024-05-10 | 湖北新蓝天新材料股份有限公司 | Environment-friendly silane coupling agent and preparation method thereof |
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