CN101463126A - Preparation of polyether silane - Google Patents
Preparation of polyether silane Download PDFInfo
- Publication number
- CN101463126A CN101463126A CNA2008101771843A CN200810177184A CN101463126A CN 101463126 A CN101463126 A CN 101463126A CN A2008101771843 A CNA2008101771843 A CN A2008101771843A CN 200810177184 A CN200810177184 A CN 200810177184A CN 101463126 A CN101463126 A CN 101463126A
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- CN
- China
- Prior art keywords
- preparation
- silane
- polyether silane
- polyether
- organosilicon
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Abstract
The invention discloses a preparation method of polyether silane. The method comprises the following steps: taking allyl-terminated ethyleneoxide epoxypropane polymer as a raw material; stirring and heating the material to certain temperature; adding a catalyst and dropwise adding hydrogen-containing silane slowly; controlling the temperature of a reaction system, and continuing to preserve heat for a period of time after finishing adding dropwise; and vacuumizing to extract a low-molecular substance that is the desired polyether silane. The preparation method has the following advantages: the polyether silane can be taken as a hydrophilic monomer and easily introduced into an organosilicon macromolecular chain fragment by a copolymerization reaction so that lipophilicity of organosilicon macromolecules changes and the organosilicon macromolecular chain fragment has hydrophilicity and lipophilicity; the amount of the introduced polyether silane can be controlled to cause self emulsifying characteristic of the organosilicon macromolecules, remove the requirement that the traditional organosilicon macromolecules are required to be emulsified by an emulsifier before use, and cause microemulsion containing the organosilicon macromolecules with the introduced polyether silane on the molecular chain to be more stable.
Description
Technical field
The invention discloses a kind of preparation method of polyether silane.
Background technology
At present, the application of polyether-based silane does not still cause everybody attention, thus in the research of polyether silane and preparation method thereof rarely seen report, its structural formula is as follows:
Its synthesis mechanism can be represented with following equation:
Summary of the invention
The object of the present invention is to provide the preparation method of polyether silane.
For achieving the above object, the present invention realizes by the following technical solutions:
With end allyl group oxyethane epoxypropane polymer is raw material, stirring is warming up to 90～100 ℃, add catalyst A, the temperature of control reaction system is in 120～140 ℃ of scopes, beginning slowly drips silane containing hydrogen, after being added dropwise to complete, continues insulation reaction 4h～6h, vacuumize lower-molecular substance, be required polyether silane; The outward appearance of polyether silane is the oily liquids of little Huang or yellow transparent, and its viscosity (25 ℃) is 10～400mPa.S, nonvolatile substances content 〉=99% (110 ℃/3h);
The structural formula of described end allyl group oxyethane epoxypropane polymer is as follows:
CH
2＝CH—(CH
2CH
2O)
A(CH
2CH
2CH
2O)
BR
Wherein: A, B are positive integer, and A〉B;
A=3～20, preferred A=6～10;
B=0～10, preferred B=0～4;
R is selected from H, CH
3Or C
4H
9
The structure of described silane containing hydrogen is as follows:
Wherein: R ' is selected from CH
3Or C
2H
5
The mol ratio of described end allyl group oxyethane epoxypropane polymer and silane containing hydrogen is 1:1～1:5;
Described catalyst A is selected from Platinic chloride ethanolic soln, isopropyl alcohol solution of chloroplatinic acid or Platinic chloride-vinyl complex compound; Wherein Platinic chloride-vinyl complex structure formula is H
2PtCl
66H
2O; Consumption is 15～30ppm to contain Pt.
Advantage of the present invention is:
This polyether silane can be used as a kind of hydrophilic monomer, be incorporated into the silicone macromolecule segment by copolyreaction at an easy rate, thereby the lipophilicity of silicone macromolecule is changed, make and have hydrophilic and oleophilic characteristics on the silicone macromolecule segment simultaneously, the introducing amount of control polyether silane, can make silicone macromolecule have self emulsifiable characteristics, changing traditional silicone macromolecule all needs the requirement that could use after the emulsifying agent emulsification, makes the microemulsion of the silicone macromolecule of introducing polyether silane on the molecular chain more stable simultaneously.
Embodiment
In order to describe particularly and to explain technical characterstic of the present invention, list following each implementation method, but invention is not limited to following embodiment.
Embodiment 1
(structural formula is C to add 394g (1mol) end allyl group oxyethane epoxypropane polymer in the 1000ml there-necked flask of Dropping feeder is housed
2H
3(C
2H
4O)
8CH
3), stirring is warming up to 90～100 ℃, (wherein in platinum Pt, 28PPm), beginning slowly drips 201g (1.5mol) methyl diethoxy hydrogen silane to add the catalyzer isopropyl alcohol solution of chloroplatinic acid, exothermic heat of reaction, the control rate of addition, the temperature of controlling reaction system is at 130 ℃, after being added dropwise to complete, continue insulation reaction 6h, vacuumize lower-molecular substance.Obtain the oily liquids that outward appearance is a yellow transparent, its viscosity (25 ℃) is 280mPa.S, nonvolatile substances content 〉=99% (110 ℃/3h).
Embodiment 2
(structural formula is C to add 350g (1mol) end allyl group oxyethane epoxypropane polymer in the 1000ml there-necked flask of Dropping feeder is housed
2H
3(C
2H
4O)
6(C
3H
6O)
1H), stirring is warming up to 90～100 ℃, (wherein in platinum Pt, 26PPm), beginning slowly drips 268g (2mol) methyl diethoxy hydrogen silane to add the catalyzer isopropyl alcohol solution of chloroplatinic acid, exothermic heat of reaction, the control rate of addition, the temperature of controlling reaction system is at 125 ℃, after being added dropwise to complete, continue insulation reaction 5h, vacuumize lower-molecular substance.Obtain the oily liquids that outward appearance is a yellow transparent, its viscosity (25 ℃) is 220mPa.S, nonvolatile substances content 〉=99% (110 ℃/3h).
Claims (7)
1. its structural formula of polyether silane is as follows:
It is characterized in that, the preparation method is: with end allyl group oxyethane epoxypropane polymer is raw material, stirring is warming up to 90～100 ℃, add catalyst A, beginning slowly drips silane containing hydrogen, and the temperature of control reaction system is in 120～140 ℃ of scopes, after being added dropwise to complete, continue insulation reaction 4h～6h, vacuumize lower-molecular substance, be required polyether silane.
2. the preparation method of polyether silane according to claim 1, it is characterized in that: the structural formula of described end allyl group oxyethane epoxypropane polymer is as follows:
CH
2＝CH—(CH
2CH
2O)
A(CH
2CH
2CH
2O)
BR
Wherein: A, B are positive integer, and A〉B;
A＝3～20；
B＝0～10；
R is selected from H, CH
3Or C
4H
9
3. the preparation method of polyether silane according to claim 2 is characterized in that: in the structural formula of described end allyl group oxyethane epoxypropane polymer:
A＝6～10；
B＝0～4。
4. the preparation method of polyether silane according to claim 1, it is characterized in that: the structure of described silane containing hydrogen is as follows:
Wherein: R ' is selected from CH
3Or C
2H
5
5. the preparation method of polyether silane according to claim 1, it is characterized in that: the mol ratio of described end allyl group oxyethane epoxypropane polymer and silane containing hydrogen is 1:1～1:5.
6. the preparation method of polyether silane according to claim 1, it is characterized in that: described catalyst A is selected from Platinic chloride ethanolic soln, isopropyl alcohol solution of chloroplatinic acid or Platinic chloride-vinyl complex compound; Wherein the Platinic chloride structural formula is H
2PtCl
66H
2O.
7. according to the preparation method of claim 1 or 6 described polyether silanes, it is characterized in that: the consumption of described catalyst A is 15～30ppm to contain Pt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101771843A CN101463126A (en) | 2008-12-09 | 2008-12-09 | Preparation of polyether silane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101771843A CN101463126A (en) | 2008-12-09 | 2008-12-09 | Preparation of polyether silane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101463126A true CN101463126A (en) | 2009-06-24 |
Family
ID=40803934
Family Applications (1)
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|---|---|---|---|
| CNA2008101771843A Pending CN101463126A (en) | 2008-12-09 | 2008-12-09 | Preparation of polyether silane |
Country Status (1)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921393A (en) * | 2010-09-19 | 2010-12-22 | 东莞市普赛达密封粘胶有限公司 | Method for synthesizing silyl-terminated polyether |
| CN101921571A (en) * | 2010-08-13 | 2010-12-22 | 东莞市英迈新能源材料有限公司 | High-temperature resistant packaging adhesive for high-power LED lamp and preparation method thereof |
| CN105473150A (en) * | 2013-08-20 | 2016-04-06 | 3M创新有限公司 | Boron-silane polyether complex |
| CN105503029A (en) * | 2015-08-18 | 2016-04-20 | 江苏苏博特新材料股份有限公司 | Concrete air-entraining agent |
| CN110117357A (en) * | 2019-04-12 | 2019-08-13 | 浙江新安化工集团股份有限公司 | A kind of silane modified polyether and preparation method thereof |
| CN115819780A (en) * | 2022-12-21 | 2023-03-21 | 万华化学集团股份有限公司 | Polyether modified silicone oil and preparation method thereof |
-
2008
- 2008-12-09 CN CNA2008101771843A patent/CN101463126A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921571A (en) * | 2010-08-13 | 2010-12-22 | 东莞市英迈新能源材料有限公司 | High-temperature resistant packaging adhesive for high-power LED lamp and preparation method thereof |
| CN101921571B (en) * | 2010-08-13 | 2014-11-05 | 王行柱 | High-temperature resistant packaging adhesive for high-power LED lamp and preparation method thereof |
| CN101921393A (en) * | 2010-09-19 | 2010-12-22 | 东莞市普赛达密封粘胶有限公司 | Method for synthesizing silyl-terminated polyether |
| CN101921393B (en) * | 2010-09-19 | 2012-06-27 | 东莞市普赛达密封粘胶有限公司 | Method for synthesizing silyl-terminated polyether |
| CN105473150A (en) * | 2013-08-20 | 2016-04-06 | 3M创新有限公司 | Boron-silane polyether complex |
| CN105503029A (en) * | 2015-08-18 | 2016-04-20 | 江苏苏博特新材料股份有限公司 | Concrete air-entraining agent |
| CN110117357A (en) * | 2019-04-12 | 2019-08-13 | 浙江新安化工集团股份有限公司 | A kind of silane modified polyether and preparation method thereof |
| CN115819780A (en) * | 2022-12-21 | 2023-03-21 | 万华化学集团股份有限公司 | Polyether modified silicone oil and preparation method thereof |
| CN115819780B (en) * | 2022-12-21 | 2023-09-19 | 万华化学集团股份有限公司 | Polyether modified silicone oil and preparation method thereof |
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Open date: 20090624 |