CN102225947A - Preparation method of polyether modified siloxane - Google Patents
Preparation method of polyether modified siloxane Download PDFInfo
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- CN102225947A CN102225947A CN2011101104536A CN201110110453A CN102225947A CN 102225947 A CN102225947 A CN 102225947A CN 2011101104536 A CN2011101104536 A CN 2011101104536A CN 201110110453 A CN201110110453 A CN 201110110453A CN 102225947 A CN102225947 A CN 102225947A
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- modified siloxane
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Abstract
The invention discloses a synthesis of organosilicon surfactant (polyether modified siloxane), comprising a solvent-free reaction of terminal allyl polyoxyethylene ether (molecular weight: 456-500) with heptamethyl trisiloxane by using chloroplatinic acid (speier catalyst) as catalyst. The catalyst used in the invention has high reactive activity for catalyzing organosilicon, and active hydrogen has high conversion rate, the use of benzene organic solvent is prevented, so that the preparation process is nontoxic and no pollution. The prepared polyether modified siloxane is clear and transparent, and has good wetability and spreadability.
Description
Technical field
The present invention relates to a kind of method for preparing polyether modified siloxane, specifically is a kind of method that adopts addition reaction of silicon with hydrogen to prepare polyether modified siloxane.
Background technology
It is low, wetting and spreadability is good, emulsifying effect is big, compatibility is good that organic silicon surfactant has surface tension, and have foaming, surely steep and press down the bubble effect, and the distinct advantages that has no side effect now has been widely used in agricultural chemicals, coating, the textile industry.By polyether graft modified, the polyether modified siloxane that makes can be in aqueous systems self-emulsifying, good stability, the surface spreading ability is strong.
Organic silicon surfactant generally is to make by addition reaction of silicon with hydrogen, and its production technique exists certain shortcoming.In industrial production,, generally need to add a large amount of benzene kind solvents in order to prevent the crosslinked of Si-H key.This not only contaminate environment, influence workers ' health, reduced single-autoclave yield rate, and these solvents all are inflammable substance, and are dangerous high.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing polyether modified siloxane, specifically be a kind of reaction of under solvent-free condition, carrying out, the method for preparing polyether modified siloxane of have that aftertreatment is simple, side reaction is few, inductive phase is short, reaction being convenient to control, reaction efficiency is high.
In order to solve above technical problem, a kind of method for preparing polyether modified siloxane is characterized in that: addition reaction of silicon with hydrogen takes place in end allyl polyethenoxy ether and seven methyl trisiloxanes under the existence of speier catalyzer, condition of no solvent; Reaction equation:
N=9-10 wherein.
Further, described catalyzer is a Platinic chloride Virahol complex compound, and its preparation method is: concentration is made into isopropyl alcohol solution of chloroplatinic acid at 1g/100ml-1g/150ml Platinic chloride and anhydrous isopropyl alcohol mixing, is stirred well to dissolving fully under 70-80 ℃ of temperature.
Further, described catalyst consumption is the 0.2-0.3ppm of material gross weight.
Further, in the described reaction, the molecular weight ratio of the material of reactant end allyl polyethenoxy ether and its seven methyl trisiloxanes is 1.1:1-1.3:1.
Further, described addition reaction of silicon with hydrogen temperature is 100-110 ℃, and the reaction times is 3-4 hour.
The invention has the advantages that:
Adopt chloroplatinic acid catalyst solventless method synthesizing organo-silicon tensio-active agent, have the following advantages:
1, catalyst activity height, Platinic chloride form complex compound in the presence of Virahol, remove crystal water again, can effectively improve the mixing of catalyzer, reduce side reaction, shorten inductive phase.Side reaction of the present invention only is:
Side reaction:
2, adopt the solvent-free polymeric method, avoid using a large amount of organic solvents, environmentally safe.
3, adopt the solvent-free polymeric method, post processing mode is simple, has improved production efficiency.
4, in addition, in the presence of this catalyzer, reaction is mild, is easy to operate and control.
Embodiment:
For the effect of this synthetic method is described, now be exemplified below:
Embodiment 1
The end allyl polyethenoxy ether and the 5ml speier catalyzer that in the four-hole boiling flask of the 1000ml that has agitator, thermometer, add 550g earlier, N
2Start stirring under the protection; slow elevated temperature to 90 ℃; activation is 1 hour under this temperature; drip 220g seven methyl trisiloxanes then in system continuously, control reaction temperature dropwised afterreaction 3-4 hour between 100-110 ℃; infrared analysis is carried out in serial sampling; after reaction finishes, go out catalyzer with charcoal absorption earlier, carry out underpressure distillation again and go out by product.Than popular response, the reaction times has shortened nearly 1 hour, and through detecting, the result shows product content more than 95%, and side reaction significantly reduces, and has improved reaction efficiency effectively.
Embodiment 2
The end allyl polyethenoxy ether and the 5ml speier catalyzer that in the four-hole boiling flask of the 1000ml that has agitator, thermometer, add 575g earlier, N
2Start stirring under the protection; slow elevated temperature to 90 ℃; activation is 1 hour under this temperature; drip 220g seven methyl trisiloxanes then in system continuously, control reaction temperature dropwised afterreaction 3-4 hour between 100-110 ℃; infrared analysis is carried out in serial sampling; after reaction finishes, go out catalyzer with charcoal absorption earlier, carry out underpressure distillation again and go out by product.Than popular response, the reaction times has shortened nearly 1 hour, and through detecting, the result shows product content more than 96%, and side reaction significantly reduces, and has improved reaction efficiency effectively.
Embodiment 3
The end allyl polyethenoxy ether and the 5ml speier catalyzer that in the four-hole boiling flask of the 1000ml that has agitator, thermometer, add 620g earlier, N
2Start stirring under the protection; slow elevated temperature to 90 ℃; activation is 1 hour under this temperature; drip 220g seven methyl trisiloxanes then in system continuously, control reaction temperature dropwised afterreaction 3-4 hour between 100-110 ℃; infrared analysis is carried out in serial sampling; after reaction finishes, go out catalyzer with charcoal absorption earlier, carry out underpressure distillation again and go out by product.Than popular response, the reaction times has shortened nearly 1 hour, and through detecting, the result shows product content more than 95%, and side reaction significantly reduces, and has improved reaction efficiency effectively.
Embodiment 4
The seven methyl trisiloxanes and the 5ml speier catalyzer that in the four-hole boiling flask of the 1000ml that has agitator, thermometer, add 222g earlier, N
2Start stirring under the protection; slow elevated temperature to 90 ℃; activation is 1 hour under this temperature; the continuous end allyl polyethenoxy ether of Dropwise 5 60g in system then, control reaction temperature dropwised afterreaction 3-4 hour between 100-110 ℃; infrared analysis is carried out in serial sampling; after reaction finishes, go out catalyzer with charcoal absorption earlier, carry out underpressure distillation again and go out by product.Than popular response, the reaction times has shortened nearly 1 hour, and through detecting, the result shows that product content can reach 95%, and side reaction significantly reduces, and has improved reaction efficiency effectively.
Embodiment 5
The seven methyl trisiloxanes and the 3ml speier catalyzer that in the four-hole boiling flask of the 500ml that has agitator, thermometer, add 111g earlier, N
2Start stirring under the protection; slow elevated temperature to 90 ℃; activation is 1 hour under this temperature; drip the end allyl polyethenoxy ether of 300g then in system continuously, control reaction temperature dropwised afterreaction 3-4 hour between 100-110 ℃; infrared analysis is carried out in serial sampling; after reaction finishes, go out catalyzer with charcoal absorption earlier, carry out underpressure distillation again and go out by product.Than popular response, the reaction times has shortened nearly 1 hour, and through detecting, the result shows product content more than 97%, and side reaction significantly reduces, and has improved reaction efficiency effectively.
Embodiment 6
The end allyl polyethenoxy ether of the seven methyl trisiloxanes of disposable adding 110g, 280g and 3ml speier catalyzer in the four-hole boiling flask of the 500ml that has agitator, thermometer, N
2Protection is down started stirring, slow elevated temperature, and control reaction temperature react 3-4 hour between 90-110 ℃, and infrared analysis is carried out in serial sampling, and after the reaction end, catalyzer is gone out with charcoal absorption by elder generation, carries out underpressure distillation again and goes out by product.Than popular response, the reaction times has shortened nearly 1 hour, and through detecting, the result shows that product content has reached 96.5%, and side reaction significantly reduces, and has improved reaction efficiency effectively.
Claims (5)
1. a method for preparing polyether modified siloxane is characterized in that: hold allyl polyethenoxy ether and seven methyl trisiloxanes under the existence of speier catalyzer, condition of no solvent addition reaction of silicon with hydrogen to take place;
Reaction equation:
N=9-10 wherein.
2. a kind of method for preparing polyether modified siloxane according to claim 1, it is characterized in that: described catalyzer is a Platinic chloride Virahol complex compound, its preparation method is: concentration is made into isopropyl alcohol solution of chloroplatinic acid at 1g/100ml-1g/150ml Platinic chloride and anhydrous isopropyl alcohol mixing, is stirred well to dissolving fully under 70-80 ℃ of temperature.
3. a kind of method for preparing polyether modified siloxane according to claim 1 is characterized in that: described catalyst consumption is the 0.2-0.3ppm of material gross weight.
4. a kind of method for preparing polyether modified siloxane according to claim 1 is characterized in that: in the described reaction, the molecular weight ratio of the material of reactant end allyl polyethenoxy ether and its seven methyl trisiloxanes is 1.1:1-1.3:1.
5. a kind of method for preparing polyether modified siloxane according to claim 1 is characterized in that: described addition reaction of silicon with hydrogen temperature is 100-110 ℃, and the reaction times is 3-4 hour.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030966A (en) * | 2012-12-24 | 2013-04-10 | 建德市顺发化工助剂有限公司 | Preparation method of high-efficiency penetrant for PU synthetic leather |
| CN103356402A (en) * | 2013-07-26 | 2013-10-23 | 联谊水处理技术（大连）有限公司 | Skin-care product additive modified by polysiloxane and dodecene |
| CN105727940A (en) * | 2014-12-09 | 2016-07-06 | 仲恺农业工程学院 | Organosilicon thickening agent catalytic synthesis method with ultra-microporous platinum catalyst prepared with response surface optimization method |
| CN106866970A (en) * | 2017-03-17 | 2017-06-20 | 华东交通大学 | The non-solvent preparation of octyl group silicone oil under a kind of normal temperature |
| CN106867023A (en) * | 2017-03-13 | 2017-06-20 | 谭国权 | Multifunctional assistant and multi-functional coupling agent |
| CN106928267A (en) * | 2017-03-06 | 2017-07-07 | 汕头大学 | The preparation method of quaternary trisiloxanes Gemini surface active agent |
| CN107226911A (en) * | 2017-07-31 | 2017-10-03 | 王琪宇 | A kind of preparation method for producing fabric softener polyether modified silicon oil |
| CN107254044A (en) * | 2017-06-22 | 2017-10-17 | 江苏赛欧信越消泡剂有限公司 | Preparation method for the polymer emulsion defoamer of fermentation |
| CN110241471A (en) * | 2019-05-29 | 2019-09-17 | 苏州世名科技股份有限公司 | Viscose rayon original liquid coloring polymer overmold dispersible pigment color paste and preparation method thereof |
| CN110583642A (en) * | 2019-09-27 | 2019-12-20 | 浙江工业大学 | Low-foam type organic silicon agricultural additive and synthesis method thereof |
| CN111841438A (en) * | 2020-07-23 | 2020-10-30 | 吉林大学 | Solubilizing material for restoring PCE pollution in underground environment and preparation method thereof |
| CN112143269A (en) * | 2020-09-07 | 2020-12-29 | 中国石油大学胜利学院 | Water-based inorganic zinc-rich coating and preparation method thereof |
| CN115873388A (en) * | 2022-12-30 | 2023-03-31 | 中广核高新核材科技（苏州）有限公司 | Hydrophobic high-bamboo-powder-filled biodegradable composite material and preparation method thereof |
| CN116898745A (en) * | 2023-09-04 | 2023-10-20 | 广州市胜梅化妆品有限公司 | Water-light stable component and ginseng truffle yeast combined component prepared from same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101637708A (en) * | 2009-09-01 | 2010-02-03 | 陕西科技大学 | Method for preparing solvent-free polyether grafting organosilico/diamide compound emulsion defoamer |
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2011
- 2011-04-29 CN CN2011101104536A patent/CN102225947A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101637708A (en) * | 2009-09-01 | 2010-02-03 | 陕西科技大学 | Method for preparing solvent-free polyether grafting organosilico/diamide compound emulsion defoamer |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030966B (en) * | 2012-12-24 | 2014-10-08 | 建德市顺发化工助剂有限公司 | Preparation method of high-efficiency penetrant for PU synthetic leather |
| CN103030966A (en) * | 2012-12-24 | 2013-04-10 | 建德市顺发化工助剂有限公司 | Preparation method of high-efficiency penetrant for PU synthetic leather |
| CN103356402A (en) * | 2013-07-26 | 2013-10-23 | 联谊水处理技术（大连）有限公司 | Skin-care product additive modified by polysiloxane and dodecene |
| CN105727940B (en) * | 2014-12-09 | 2018-10-23 | 仲恺农业工程学院 | A method of ultramicropore platinum catalyst is prepared using response surface optimization method and catalyzes and synthesizes organosilicon thickener |
| CN105727940A (en) * | 2014-12-09 | 2016-07-06 | 仲恺农业工程学院 | Organosilicon thickening agent catalytic synthesis method with ultra-microporous platinum catalyst prepared with response surface optimization method |
| CN106928267A (en) * | 2017-03-06 | 2017-07-07 | 汕头大学 | The preparation method of quaternary trisiloxanes Gemini surface active agent |
| CN106867023A (en) * | 2017-03-13 | 2017-06-20 | 谭国权 | Multifunctional assistant and multi-functional coupling agent |
| CN106866970B (en) * | 2017-03-17 | 2020-08-11 | 华东交通大学 | Solvent-free preparation method of octyl silicone oil at normal temperature |
| CN106866970A (en) * | 2017-03-17 | 2017-06-20 | 华东交通大学 | The non-solvent preparation of octyl group silicone oil under a kind of normal temperature |
| CN107254044A (en) * | 2017-06-22 | 2017-10-17 | 江苏赛欧信越消泡剂有限公司 | Preparation method for the polymer emulsion defoamer of fermentation |
| CN107226911A (en) * | 2017-07-31 | 2017-10-03 | 王琪宇 | A kind of preparation method for producing fabric softener polyether modified silicon oil |
| CN110241471A (en) * | 2019-05-29 | 2019-09-17 | 苏州世名科技股份有限公司 | Viscose rayon original liquid coloring polymer overmold dispersible pigment color paste and preparation method thereof |
| CN110583642A (en) * | 2019-09-27 | 2019-12-20 | 浙江工业大学 | Low-foam type organic silicon agricultural additive and synthesis method thereof |
| CN111841438A (en) * | 2020-07-23 | 2020-10-30 | 吉林大学 | Solubilizing material for restoring PCE pollution in underground environment and preparation method thereof |
| CN112143269A (en) * | 2020-09-07 | 2020-12-29 | 中国石油大学胜利学院 | Water-based inorganic zinc-rich coating and preparation method thereof |
| CN112143269B (en) * | 2020-09-07 | 2022-07-12 | 中国石油大学胜利学院 | Water-based inorganic zinc-rich coating and preparation method thereof |
| CN115873388A (en) * | 2022-12-30 | 2023-03-31 | 中广核高新核材科技（苏州）有限公司 | Hydrophobic high-bamboo-powder-filled biodegradable composite material and preparation method thereof |
| CN116898745A (en) * | 2023-09-04 | 2023-10-20 | 广州市胜梅化妆品有限公司 | Water-light stable component and ginseng truffle yeast combined component prepared from same |
| CN116898745B (en) * | 2023-09-04 | 2024-02-02 | 广州市胜梅化妆品有限公司 | Ginseng truffle composition |
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Application publication date: 20111026 |