CN1085220A - Production method of pollution-free organo-silicon coupling agent and products thereof - Google Patents
Production method of pollution-free organo-silicon coupling agent and products thereof Download PDFInfo
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- CN1085220A CN1085220A CN 92111484 CN92111484A CN1085220A CN 1085220 A CN1085220 A CN 1085220A CN 92111484 CN92111484 CN 92111484 CN 92111484 A CN92111484 A CN 92111484A CN 1085220 A CN1085220 A CN 1085220A
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- Prior art keywords
- silane
- vinyl
- beta
- oxyethyl group
- methoxy oxyethyl
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Abstract
Production method and paraffin wax type thereof, hard acid type and the potter's clay type product forms of vinyl three ('beta '-methoxy oxyethyl group) silane.Alcoholysis method technology of the present invention absorbs and purification step with by-product hydrochloric acid, being about to ethylene glycol monomethyl ether joins in the mixture of vinyl trichloro silane and toluene, stir simultaneously with hydrochloric acid and absorb, add post-heating and constant temperature, mixture and vinyl three ('beta '-methoxy oxyethyl group) silane that underpressure distillation obtains toluene and ethylene glycol monomethyl ether are carried out in spent glycol methyl ether sodium neutralization after cooling again.Utilize it to make containing formulation from 20%～80% ratio with the performance that paraffin and stearic acid contain, or soak into make the potter's clay formulation in potter's clay, this method product and formulation thereof can be used as organo-silicon coupling agent.
Description
The present invention relates to a kind of organo-silicon coupling agent production method, the production method of vinyl three ('beta '-methoxy oxyethyl group) silane particularly, and the production method of vinyl three ('beta '-methoxy oxyethyl group) silane, and paraffin wax type hard acid type and three types of products of potter's clay type of vinyl three ('beta '-methoxy oxyethyl group) silane.
Existing vinyl three ('beta '-methoxy oxyethyl group) process for producing silicane is long, seriously polluted, and the hydrochloric acid corrosion resistance of discharging is strong, and purity is low, and yield is also lower, and is more low-grade to the course of processing and result all are in, and product forms is incomplete, uses to be subjected to certain limitation.
The object of the present invention is to provide a kind of alcoholysis method, have vinyl three ('beta '-methoxy oxyethyl group) the production of silane method of hydrochloric acid absorption equipment and purifying technique, and three product forms of the organosilane of producing with this method.
Content of the present invention comprises:
1, production method:
(1) under agitation add ethylene glycol monomethyl ether (2.0～5.0 moles) to containing vinyl trichloro silane (1～3 mole) and containing in the mixture of toluene (0.5～2.5 mole), controlled temperature starts the hydrochloric acid absorption equipment simultaneously at 25～110 ℃;
(2) be heated to 50～110 ℃ of constant temperature and (looked Cl in the liquid phase in 5～8 hours
-% and deciding reaches 1.5% ± 0.5 and is advisable);
(3) be cooled to the spent glycol methyl ether sodium of back below 0～60 ℃ and be neutralized to PH6.5～7.5;
(4) underpressure distillation gets vinyl three ('beta '-methoxy oxyethyl group) silane under 70～140 ℃/160～6mmHg;
Above ratio is a mol ratio.
Its reaction is according to following equation: CH
2; CHSiCl
3+ 3HOCH
2CH
2OCH
3→ CH
CHSi(OCH
2CH
2DCH
3)
3+ HCl ↑
Best with 139 ℃/10mmHg gained purity transformation efficiency in described underpressure distillation.
2, paraffin wax product
Matrix is a paraffin wax, in paraffin wax, be inclusive with and under whipped state, join in the described paraffin wax that has melted and when described paraffin wax cools off rapidly, it is included in vinyl three ('beta '-methoxy oxyethyl group) silane in the described paraffin wax, because the two can contain mutually, its proportioning all can be by weight 25%～75% adds.
3, hard acid type product
Matrix is a stearic acid, in stearic acid, be inclusive with in the stearic acid that under whipped state, joins thawing, and when stearic acid cools off, it is included in vinyl three ('beta '-methoxy oxyethyl group) silane in the stearic acid, because the two can contain mutually, its proportioning all can be by weight 20～80% adds.
4, potter's clay type product
Its matrix composition is a potter's clay, in potter's clay or spray add or soak into and add vinyl three ('beta '-methoxy oxyethyl group) silane that 0.01～15% weight is arranged.
The invention has the advantages that:
1, in reaction, promptly starts hydrochloric acid and absorb, stop to pollute, reduce corrosion, reclaim the hydrochloric acid commercial performance and obviously improve.
2, be that alkali neutralizes with the ethylene glycol monomethyl ether, not only reduce by-product and obviously improved yield.
3, not only obtain high purity product during underpressure distillation, also obtained toluene and ethylene glycol monomethyl ether blended cut in early stage.
4, be significantly improved than the traditional technology productive rate, general productive rate can reach 50%, is 70～80% preferably, and by claim 6,7 described schemes, product purity can reach 98%, can reach 93.8% in the pure yield of vinyl three oxosilanes.
5, can form three types complete series product, of many uses.
Embodiment 1(most preferred embodiment):
98% vinyl trichlorosilane 2.5Kg feeds intake, toluene 1.5Kg, start pneumatic blending and jet of water acid absorption pump, in mixture, slowly add ethylene glycol monomethyl ether 3.75Kg simultaneously, use the backflow control reaction temperature around here and be no more than 40 ℃, after finishing, adding heats, when being heated to 60 ± 5 ℃, constant temperature 5～8 hours, after (deciding on liquid phase C1 % value) is cooled to 40 ℃ with it, spent glycol methyl ether sodium is neutralized to PH7 ± 0.5, underpressure distillation under 70～140 ℃/160～6mmHg condition, fraction in early stage (about 1.78Kg) is the mixture of toluene and ethylene glycol monomethyl ether, the later stage fraction is vinyl three ('beta '-methoxy oxyethyl group) silane, and when distillation condition during at 139 ℃/10mmHg, can obtain purity is 98%, the pure yield 93.8%(of product is in vinyl three oxosilanes) vinyl three ('beta '-methoxy oxyethyl group) silane, refractive index n
25 01.4275 density C
25 41.03.
Embodiment 2(most preferred embodiment):
98% vinyl trichlorosilane 2.5Kg feeds intake, toluene 1.5Kg, start pneumatic blending and jet of water acid absorption pump, in mixture, slowly add ethylene glycol monomethyl ether 3.75Kg simultaneously, use the backflow control reaction temperature around here and be no more than 30 ℃, after finishing, adding heats, when being heated to 60 ± 3 ℃, according to Cl in the liquid phase
-% content is determined constant temperature time, be generally 6～7 hours, constant temperature can be closed pneumatic blending and sour absorption pump after finishing, after treating its cooling, spent glycol methyl ether sodium neutralization is controlled at 7 ± 0.3 with reaction solution to PH, under 70～140 ℃/160～6mmHg condition, distill, what at first steam is the mixture of toluene and ethylene glycol monomethyl ether, and the product that distills out under 139 ℃/10mmHg is vinyl three ('beta '-methoxy oxyethyl group) silane of the higher yield of higher degree, its refractive index n
25 01.4275 density C
25 41.03.
Embodiment 3:
According to user's the formulation requirement and the different demands of content, vinyl three ('beta '-methoxy oxyethyl group) silane that embodiment 1 or the described method of the 2 or the 5th part can be obtained, make paraffin wax type or hard acid type product forms, be that its matrix composition is paraffin wax (or stearic acid), in matrix, be inclusive with and under whipped state, join in the matrix that has melted, and when matrix cools off rapidly, it is included in vinyl three ('beta '-methoxy oxyethyl group) silane within the matrix, because matrix contains mutually with it, then its weight proportion all can add by 25～75%, as each 50% or 40% and 60%.
Embodiment 4
Vinyl three ('beta '-methoxy oxyethyl group) silane that embodiment 1 or the described method of the 2 or the 5th part can be obtained, make potter's clay type product forms, be matrix promptly with potter's clay, in potter's clay or spray or soak into to add vinyl three ('beta '-methoxy oxyethyl group) silane that 0.01～15% weight is arranged, the ratio of adding is decided according to customer need.
Claims (10)
1, the production method of a kind of vinyl three (Beta-methyl oxyethyl group) silane, its step comprises:
(1) under agitation slowly add ethylene glycol monomethyl ether (2.0～5.0 moles) to containing vinyl trichloro silane (1～3 mole) and containing in the mixture of toluene (0.5～2.5 mole), controlled temperature starts the hydrochloric acid absorption equipment simultaneously at 25～110 ℃;
(2) be heated to 50～110 ℃ of constant temperature 5～8 hours;
(3) be cooled to 0～60 ℃ after spent glycol methyl ether sodium be neutralized to PH6.5～7.5;
(4) underpressure distillation gets vinyl three ('beta '-methoxy oxyethyl group) silane under 70～140 ℃/160～6mmHg;
Above ratio is a mol ratio.
2, the production method of vinyl three according to claim 1 ('beta '-methoxy oxyethyl group) silane is characterized in that: the slow adding of described ethylene glycol monomethyl ether is aided with cooling simultaneously to drip to well, and controlled temperature is at 0～60 ℃.
3, the production method of vinyl three according to claim 1 and 2 ('beta '-methoxy oxyethyl group) silane is characterized in that: after described ethylene glycol monomethyl ether adds, be heated to 60 ± 3 ℃, constant temperature 6～7 hours.
4, the production method of vinyl three according to claim 1 and 2 ('beta '-methoxy oxyethyl group) silane is characterized in that: behind described constant temperature, spent glycol methyl ether sodium is neutralized to PH7 ± 0.3 when being cooled to below 40 ℃.
5, the production method of vinyl three according to claim 3 ('beta '-methoxy oxyethyl group) silane is characterized in that: behind described constant temperature, when being cooled to below 40 ℃, spent glycol methyl ether sodium is neutralized to PH7 ± 0.3.
6, according to the production method of claim 1,2, one of 5 described vinyl three ('beta '-methoxy oxyethyl group) silane, it is characterized in that: in the described distillation of under 70～140 ℃/160～6mmHg, carrying out when 139 ℃/10mmHg fraction be vinyl three ('beta '-methoxy oxyethyl group) silane.
7, the production method of vinyl three according to claim 4 ('beta '-methoxy oxyethyl group) silane is characterized in that: what obtain when 139 ℃/10mmHg in the described distillation of carrying out under 70～140 ℃/160～6mmHg is vinyl three ('beta '-methoxy oxyethyl group) silane.
8, a kind of paraffin wax type vinyl three ('beta '-methoxy oxyethyl group) silane goods, its matrix composition is a Paraffin Wax Semi Refined, it is characterized in that: be inclusive with in the described Paraffin Wax Semi Refined and under whipped state, join in the described paraffin wax that has melted and when described paraffin wax cools off rapidly, it is included in vinyl three ('beta '-methoxy oxyethyl group) silane in the described paraffin wax, because the two can contain mutually, its proportioning all can be by weight 25%～75% adds.
9, a kind of hard acid type vinyl three ('beta '-methoxy oxyethyl group) silane goods, its matrix composition is a stearic acid, it is characterized in that: the Paraffin Wax Semi Refined described in claim 8 feature is replaced with stearic acid, the gained technical scheme is this programme, and its proportioning all can be by weight 20～80% adds.
10, a kind of potter's clay type vinyl three ('beta '-methoxy oxyethyl group) silane goods, its matrix composition is a potter's clay, it is characterized in that: in the described potter's clay or spray add or soak into and add vinyl three ('beta '-methoxy oxyethyl group) silane that 0.01～15% weight is arranged.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92111484 CN1085220A (en) | 1992-09-30 | 1992-09-30 | Production method of pollution-free organo-silicon coupling agent and products thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92111484 CN1085220A (en) | 1992-09-30 | 1992-09-30 | Production method of pollution-free organo-silicon coupling agent and products thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1085220A true CN1085220A (en) | 1994-04-13 |
Family
ID=4945366
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92111484 Withdrawn CN1085220A (en) | 1992-09-30 | 1992-09-30 | Production method of pollution-free organo-silicon coupling agent and products thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1085220A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106349276A (en) * | 2016-08-12 | 2017-01-25 | 荆州市江汉精细化工有限公司 | Ester exchange method for preparing vinyl tri-(2- methoxy ethyoxyl)-silane |
-
1992
- 1992-09-30 CN CN 92111484 patent/CN1085220A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106349276A (en) * | 2016-08-12 | 2017-01-25 | 荆州市江汉精细化工有限公司 | Ester exchange method for preparing vinyl tri-(2- methoxy ethyoxyl)-silane |
| CN106349276B (en) * | 2016-08-12 | 2019-03-15 | 荆州市江汉精细化工有限公司 | A kind of ester exchange method preparing vinyl three-(2- methoxyethoxy)-silane |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WW01 | Invention patent application withdrawn after publication |