CN106866723A - A kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker - Google Patents
A kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker Download PDFInfo
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 79
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000000758 substrate Substances 0.000 title claims abstract description 60
- PKDCQJMRWCHQOH-UHFFFAOYSA-N triethoxysilicon Chemical compound CCO[Si](OCC)OCC PKDCQJMRWCHQOH-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000010189 synthetic method Methods 0.000 title claims abstract description 21
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 19
- 239000004971 Cross linker Substances 0.000 title claims abstract description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 63
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- PZJJKWKADRNWSW-UHFFFAOYSA-N trimethoxysilicon Chemical compound CO[Si](OC)OC PZJJKWKADRNWSW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000047 product Substances 0.000 claims abstract description 16
- 239000011265 semifinished product Substances 0.000 claims abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 150000002118 epoxides Chemical class 0.000 claims abstract description 9
- 125000005745 ethoxymethyl group Chemical group [H]C([H])([H])C([H])([H])OC([H])([H])* 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 150000001447 alkali salts Chemical class 0.000 claims description 11
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000003431 cross linking reagent Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 4
- 125000004185 ester group Chemical group 0.000 abstract description 3
- 235000019441 ethanol Nutrition 0.000 description 26
- 230000007062 hydrolysis Effects 0.000 description 8
- 238000006460 hydrolysis reaction Methods 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 4
- 229910010272 inorganic material Inorganic materials 0.000 description 4
- 239000011147 inorganic material Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000013212 metal-organic material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- -1 silicon Oxygen alkane Chemical class 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000012757 flame retardant agent Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C07F7/1876—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker, it is related to crosslinking agent field, the method is comprised the following steps：By the ratio between mass parts, 1000 parts of trimethoxy silicon substrate ethane, 1500 parts of ethanol and 1~5 part of catalyst are added into reactor, insulated and stirred under conditions of being 120 DEG C~140 DEG C in temperature, while gathering methyl alcohol to the content of methyl alcohol is less than 95%；Under conditions of being 120 DEG C~140 DEG C in temperature, to being passed through ethanol in reactor, and while reaction collection methanol/ethanol mixture, until the content of five (ethoxymethyl) epoxide silicon substrate ethane in semi-finished product in kettle is less than 1%, obtain semi-finished product；Semi-finished product rectification under vacuum is obtained into double triethoxy silicon substrate ethane finished products.The present invention carries out ester exchange reaction by by double trimethoxy silicon substrate ethane and ethanol, and for corresponding existing synthetic method, reaction condition is more gentle, and yield is higher, and accessory substance can be easily separated collection and further use.
Description
Technical field
The present invention relates to crosslinking agent field, and in particular to a kind of conjunction of the double triethoxy silicon substrate ethane of alcohol silane crosslinker
Into method.
Background technology
Crosslinking agent (cross-linking agent) crosslinking agent is also curing agent, curing agent or curing agent, and it is in line style point
Bridging action is played between son, multiple linear molecules is mutually bonded the material for being cross-linked into network structure, line style or slight side chain can be made
The macromolecular of type is transformed into tridimensional network, it is possible to increase the intensity of product, heat resistance, wearability, optical property, technique add
The performances such as work performance, cohesive, mechanical strength, dimensional stability, solvent resistance, are mainly used in macromolecular material (rubber, thermosetting
Property resin, thermoplastic stool) in, can be used to foam or not foaming product, polyacrylate, polyalkyl acrylate, asphalt mixtures modified by epoxy resin
Ester, DAP (poly- dially phthalate) resin etc. it is modified；It can in addition contain be used as photocureable coating, photoresist, resistance
The intermediate of combustion agent and flame-retardant agent etc..
Alcohol crosslinking agent is a kind of wide crosslinking agent of application, main at present to be closed using vinyltrimethoxy silane
Into, due to building-up process in, substantial amounts of pair of trimethoxy silicon substrate byproduct ethane can be produced, and alcohol crosslinking agent is when in use,
Substantial amounts of methyl alcohol can be produced, environment is polluted, the use of alcohol crosslinking agent is limited.
The use of more alcohol crosslinking agent is at present to swap to react with ethanol using double triethoxy silicon substrate ethane
Arrive, reaction equation is as follows：
C2H5OH+HCl→C2H5Cl+H2O
But not only activity is higher for the reaction, and reaction relatively acutely, and can produce substantial amounts of hydrogen chloride gas, due to hydrogen chloride
Gas have acidity higher, directly discharge pollute the environment, recycling it is relatively costly, cause its production be subject to it is larger
Limitation.
And in above-mentioned reaction, water can cause double three chloro silicon substrate ethane, double trimethoxy silicon substrate ethane hydrolysis generation silicon
Oxygen alkane polymer, causes reaction yield to reduce.
The content of the invention
For defect present in prior art, it is an object of the invention to provide a kind of double three second of alcohol silane crosslinker
The synthetic method of epoxide silicon substrate ethane, can avoid polluting environment, improve reaction yield.
To achieve the above objectives, the present invention is adopted the technical scheme that：
A kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker, comprises the following steps：
S1, by the ratio between mass parts, 1000 parts of trimethoxy silicon substrate ethane, 1500 parts of ethanol and 1~5 part of catalyst are added
Reactor, insulated and stirred under conditions of being 120 DEG C~140 DEG C in temperature, while gathering methyl alcohol to the content of methyl alcohol is less than 95%；
S2, be 120 DEG C~140 DEG C in temperature under conditions of, to being passed through ethanol in reactor, and gathered while reaction
The mixture of methanol/ethanol, until the content of five (ethoxymethyl) epoxide silicon substrate ethane in semi-finished product in kettle is less than 1%, obtain half into
Product；
S3, semi-finished product rectification under vacuum is obtained into double triethoxy silicon substrate ethane finished products.
On the basis of above-mentioned technical proposal, the catalyst is strong acid, strong acid salt, highly basic or highly basic salt.
On the basis of above-mentioned technical proposal, the catalyst is highly basic salt.
On the basis of above-mentioned technical proposal, when the catalyst is highly basic salt, the addition of the catalyst is three
The 3 ‰ of methoxyl group silicon substrate ethane.
On the basis of above-mentioned technical proposal, when the catalyst is highly basic salt, the reaction temperature is 130 ± 2 DEG C.
On the basis of above-mentioned technical proposal, in described and double triethoxy silicon substrate ethane finished products, double triethoxy silicon substrates
The content of ethane is more than 98%.
On the basis of above-mentioned technical proposal, the tailings of the rectifying can be recycled as catalyst.
On the basis of above-mentioned technical proposal, the chemical equation of the synthetic method is：
On the basis of above-mentioned technical proposal, the reaction raw materials are the accessory substance of vinyltrimethoxy silane, described
The reaction equation of vinyltrimethoxy silane is：
Compared with prior art, the advantage of the invention is that：
(1) a kind of synthetic method of the double triethoxy silicon substrate ethane of the alcohol silane crosslinker in the present invention, reactant comes
From the double trimethoxy silicon substrate ethane of accessory substance in vinyltrimethoxy silane, can after double trimethoxy silicon substrate ethane hydrolysis
Firm covalent bond, and not facile hydrolysis are formed with the hydroxyl of metal or inorganic materials surface, inorganic materials or metal is typically used as
Face coat, but double trimethoxy silicon substrate ethane can discharge methyl alcohol in hydrolysis, pollute environment, and double trimethoxy silicon
Base ethane price in itself is more cheap, and economic worth is relatively low.
The present invention carries out ester exchange reaction by by double trimethoxy silicon substrate ethane and ethanol, and productive value is higher, application
The more preferable and environment-friendly double triethoxy silicon substrate ethane of prospect, and high purity methanol in course of reaction will not corrosion reaction
Kettle, and can effectively be collected, do not pollute the environment not only, additionally it is possible to used as the high-quality raw material of industry.
(2) a kind of synthetic method of the double triethoxy silicon substrate ethane of the alcohol silane crosslinker in the present invention, reaction temperature
It is 120~140 DEG C, condition is more gentle, and double triethoxy silicon substrate ethane in the double triethoxy silicon substrate ethane finished products for obtaining
Content be more than 98%, purity is higher, while yield is higher；It is anti-that tailings after rectifying can be directly used in circulation as catalyst
Should, no raw material is wasted, course of reaction environmental protection.
Specific embodiment
The present invention is described in further detail with reference to embodiments.
A kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker of embodiment of the present invention offer, including with
Lower step：
S1, by the ratio between mass parts, 1000 parts of trimethoxy silicon substrate ethane, 1500 parts of ethanol and 1~5 part of catalyst are added
Reactor, insulated and stirred under conditions of being 120 DEG C~140 DEG C in temperature, and steam the methanol content at the top of methyl alcohol to reaction tower
Less than 95%.
S2, be 120 DEG C~140 DEG C in temperature under conditions of, be passed through ethanol synthesis from reactor bottom, and in the same of reaction
When collection methanol/ethanol mixture, until five (ethoxymethyl) epoxide silicon substrate ethane in semi-finished product in kettle content be less than 1%, obtain
To semi-finished product.
S3, semi-finished product rectification under vacuum at least 72h is obtained double triethoxy silicon substrate ethane finished products, and double triethoxy silicon substrates
The content of double triethoxy silicon substrate ethane is more than 98% in ethane finished product, and the tailings of rectification under vacuum can work as catalyst circulation to be made
With.
Catalyst in the embodiment of the present invention selects strong acid, strong acid salt, highly basic or highly basic salt, preferably highly basic salt, catalyst
During for highly basic salt, its adding proportion is 3 ‰, and reaction temperature is 130 ± 2 DEG C.
Main chemical equation is：
Wherein, the reactant in the present invention comes from the accessory substance of vinyltrimethoxy silane, vinyl trimethoxy
Silane is the larger silane coupler of usage amount in the market, and its production reaction equation is：
Can be formed firmly with the hydroxyl of metal or inorganic materials surface after the double trimethoxy silicon substrate ethane hydrolysis of accessory substance
Covalent bond, and not facile hydrolysis is typically used as inorganic materials or metallic surface coating, but double trimethoxy silicon substrate ethane exist
Can discharge methyl alcohol during hydrolysis, pollute environment, and double trimethoxy silicon substrate ethane price in itself is more cheap, economic worth compared with
It is low.
The present invention carries out ester exchange reaction by by double trimethoxy silicon substrate ethane and ethanol, and productive value is higher, application
The more preferable and environment-friendly double triethoxy silicon substrate ethane of prospect.
And for the corresponding existing synthetic method of the reaction, reaction condition is more gentle, and yield is higher, and accessory substance is easy
Separate and collect and further use.
Below by 7 specific embodiments, the present invention is described in detail.
Embodiment 1：
To tetra- mouthfuls of 2000ml and with putting into double trimethoxy silicon substrate ethane 540g, anhydrous in 1 meter of flask of packed tower high
Ethanol 810g and highly basic saline catalyst 1.62g, heats while stirring, and with the rising of temperature, tower top has backflow, controls back
Stream temperature, starts to gather methyl alcohol 75g when tower top temperature is 64.5 DEG C, while detecting the purity of methyl alcohol.
When methanol purity is less than 95%, gathers the first and second alcohol mixtures and started to drag using high-order dropping funel
Persistently it is slowly introducing absolute ethyl alcohol, persistently overheating to 130 DEG C reactions, until the (ethoxymethyl) epoxide silicon substrate ethane of sampling analysis five
Content stops heating when being less than 1%, obtains semi-finished product 815g, the first and second alcohol mixture 1200g (GC chromatography methanol contents
9.5%th, ethanol 90.5%), semi-finished product are cooled to carries out rectifying after normal temperature, collect 150~160 DEG C of cuts of (10pa)
The main content 98.2% of 679g, GC chromatography, rectifying tailings 32g is directly used as the catalyst for synthesizing next time, from the reaction that feeds intake
70h is taken to product is gone out.
In this example, product 708g should be obtained in theory, actually get 679g finished products and tailings 32g, common 711g,
The difference of theoretical value and actual value is 3g, and unnecessary part has with product itself hydrolysis in the catalyst and course of reaction of addition
Close.
The theoretical value 192g of methyl alcohol in the present embodiment, actual recovered 185g, the rate of recovery is 98.4%.
Embodiment 2：
In the present embodiment in addition to the 32g tailings that catalyst is used in embodiment 1, other conditions are same as Example 1,
The present embodiment obtains finished product 700g, rectifying tailings 35g.
Embodiment 3
The present embodiment is in addition to reaction temperature is 100 DEG C, and other conditions are same as Example 1, except reaction in reaction
Time lengthening is to outside 150h, and other results are same as Example 1.
Embodiment 4
In the present embodiment, in addition to reaction temperature is 140 DEG C, other reaction conditions are same as Example 1, the present embodiment
In 70h, five (ethoxymethyl) epoxide silicon substrate ethane contents are 16.6%, because reaction temperature is higher, cause ethanol to volatilize too fast,
Ethanol has little time normal reaction and just volatilizees, and the reaction time is increased on the contrary.
Embodiment 5
In the present embodiment, in addition to the catalyst that uses is for the concentrated sulfuric acid, other reaction conditions and result with the phase of embodiment 1
Together, the reaction time extended, when reacted between for 70h when five (ethoxymethyl) epoxide silicon substrate ethane contents be 35%.
Embodiment 6
In the present embodiment, in addition to the addition of catalyst is for 1 ‰, other reaction conditions are same as Example 1, when anti-
When between seasonable for 70h, five (ethoxymethyl) epoxide silicon substrate ethane contents have 27%, and reaction process is slower compared with embodiment 1.
Embodiment 7
In the present embodiment, in addition to the consumption of catalyst is for 5 ‰, other conditions are same as Example 1, in reaction result
Rectifying tailings is changed into 46g from original 32g, illustrates that high-boiling components content substantially increases.
The present invention is not limited to the above-described embodiments, for those skilled in the art, is not departing from
On the premise of the principle of the invention, some improvements and modifications can also be made, these improvements and modifications are also considered as protection of the invention
Within the scope of.The content not being described in detail in this specification belongs to prior art known to professional and technical personnel in the field.
Claims (9)
1. the synthetic method of the double triethoxy silicon substrate ethane of a kind of alcohol silane crosslinker, it is characterised in that comprise the following steps：
S1, by the ratio between mass parts, 1000 parts of trimethoxy silicon substrate ethane, 1500 parts of ethanol and 1~5 part of catalyst are added into reaction
Kettle, insulated and stirred under conditions of being 120 DEG C~140 DEG C in temperature, while gathering methyl alcohol to the content of methyl alcohol is less than 95%；
S2, be 120 DEG C~140 DEG C in temperature under conditions of, to being passed through ethanol in reactor, and methyl alcohol is gathered while reaction
The mixture of ethanol, until the content of five (ethoxymethyl) epoxide silicon substrate ethane in semi-finished product in kettle is less than 1%, obtains semi-finished product；
S3, semi-finished product rectification under vacuum is obtained into double triethoxy silicon substrate ethane finished products.
2. a kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker as claimed in claim 1, its feature
It is：The catalyst is strong acid, strong acid salt, highly basic or highly basic salt.
3. a kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker as claimed in claim 2, its feature
It is：The catalyst is highly basic salt.
4. a kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker as claimed in claim 2, its feature
It is：When the catalyst is highly basic salt, the addition of the catalyst is the 3 ‰ of trimethoxy silicon substrate ethane.
5. a kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker as claimed in claim 2, its feature
It is：When the catalyst is highly basic salt, the reaction temperature is 130 ± 2 DEG C.
6. a kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker as claimed in claim 1, its feature
It is：In described and double triethoxy silicon substrate ethane finished products, the content of double triethoxy silicon substrate ethane is more than 98%.
7. a kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker as claimed in claim 1, its feature
It is：The tailings of the rectifying can be recycled as catalyst.
8. a kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker as claimed in claim 1, its feature
It is：The chemical equation of the synthetic method is：
9. a kind of synthetic method of the double triethoxy silicon substrate ethane of alcohol silane crosslinker as claimed in claim 1, its feature
It is：The reaction raw materials are the accessory substance of vinyltrimethoxy silane, the reaction equation of the vinyltrimethoxy silane
For：
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| EP4099467A4 (en) * | 2020-01-30 | 2024-01-03 | Panasonic Intellectual Property Management Co., Ltd. | Additive for nonaqueous electrolyte solutions, nonaqueous electrolyte solution containing same, and nonaqueous electrolyte secondary battery |
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Application publication date: 20170620 |