CN102898654A - Method for preparing silicon oil - Google Patents
Method for preparing silicon oil Download PDFInfo
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- CN102898654A CN102898654A CN2012103619550A CN201210361955A CN102898654A CN 102898654 A CN102898654 A CN 102898654A CN 2012103619550 A CN2012103619550 A CN 2012103619550A CN 201210361955 A CN201210361955 A CN 201210361955A CN 102898654 A CN102898654 A CN 102898654A
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Abstract
The invention provides a method for preparing silicon oil. The method comprises the following steps of: adding 400 to 600 weight parts of octamethylcyclotetrasiloxane and 250 to 450 weight parts of water into a reaction kettle to carry out hydrolysis; adding 4.8 to 6.8 weight parts of fatty alcohol-polyoxyethylene ether, 5.5 to 7.5 weight parts of emulsifying agent, 5.5 to 7.5 weight parts of dispersant and 7 to 9 weight parts of amino silicon oil into the reaction kettle, stirring, heating to the temperature of between 45 and 60 DEG C, and keeping the temperature for 0.5 to 2.5 hours; adding 8 to 10 weight parts of water and 2 to 4 weight parts of potassium hydroxide into the reactants, stirring, heating to the temperature of between 70 and 90 DEG C, and keeping the temperature for 1 to 3 hours; dripping 10 to 30 weight parts of coupling agent into the reactants, heating to the temperature of between 80 and 100 DEG C, keeping the temperature for 9 to 11 hours, and cooling to the temperature of between 40 and 60 DEG C; and adding 1.5 to 3.5 weight parts of glacial acetic acid into the reactants, stirring for 2 to 4 hours, regulating the pH to be 7-9, and discharging at the temperature of between 30 and 50 DEG C. By adopting the method, the performance of the silicon oil can be improved.
Description
Technical field
The present invention relates to chemical technology field, relate in particular to a kind of preparation method of silicone oil.
Background technology
Common amido silicon oil for example with the synthetic amido silicon oil of α-aminoethyl-β-aminopropyl methyl dimethoxysilane, as fabric finishing agent, possesses good flexibility, has obtained using widely.Because amino bridging property is so that the finishing effect persistence of amido silicon oil is good, but its obvious shortcoming is to lack wetting ability, after the natural fabric material arrangement, although flexibility is improved significantly, but wetting ability is almost comprehensively forfeiture also, has changed the naturally comfortable style of fabric.
In view of this, how designing a kind of silicone oil, so that have the good over-all propertieies such as smooth and resilience through the fiber of its processing, is the problem that the insider needs solution badly.
Summary of the invention
In prior art, through bad this defective of fiber feel that silicone oil is processed, the invention provides a kind of preparation method of silicone oil.
According to the present invention, a kind of preparation method of silicone oil is provided, wherein, in weight part, may further comprise the steps:
Adding 400～600 parts octamethylcyclotetrasiloxane and 250～450 parts water is hydrolyzed in reactor;
Add 4.8～6.8 parts fatty alcohol-polyoxyethylene ether, 5.5～7.5 parts emulsifying agent, 5.5～7.5 parts dispersion agent and 7～9 parts amido silicon oil and in described reactor, stir, and be warming up to 45～60 ℃ of maintenances 0.5～2.5 hour;
Add 8～10 parts water and 2～4 parts potassium hydroxide and in above-mentioned reactant, stir, and be warming up to 70～90 ℃ of maintenances 1～3 hour;
Drip 10～30 parts of coupling agents in above-mentioned reactant, be warming up to 80～100 ℃ and keep being cooled to 40～60 ℃ after 9～11 hours; And
Add 1.5～3.5 parts of Glacial acetic acid and in above-mentioned reactant, stirred 2～4 hours, adjust PH to 7～9, temperature discharging in the time of 30～50 ℃.
Preferably, described coupling agent is silane coupling agent.
Preferably, described silane coupling agent is N-(β-aminoethyl)-a kind of in the γ-aminopropyl methyl dimethoxysilane, N-cyclohexyl-y-aminopropyl methyl dimethoxysilane, γ-divinyl triammonium propyl group methyl dimethoxysilane or their arbitrary combination.
Preferably, described coupling agent dripped off in 10～20 minutes.
Advantage of the present invention is: by hydrophilic silicone oil is mixed with silicone monomers, reaction generates silicone oil, has increased the flexibility of silicone oil, and the fiber of processing through this silicone oil has the good over-all propertieies such as smooth and resilience.
Embodiment
The below is clearly and completely described the technical scheme in the embodiment of the invention, and obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
Embodiment 1
At first, in weight part, the octamethylcyclotetrasiloxane (D4) that adds 400 parts in the reactor, add again entry as solvent, wherein the weight of water is 250 parts, then the fatty alcohol-polyoxyethylene ether that adds 4.8 parts, add simultaneously 5.5 parts emulsifying agent and 5.5 parts dispersion agent, the amido silicon oil that adds again 7 parts in addition stirs in reactor, and be heated to 45 ℃, react the water that adds 8 parts after 2.5 hours, then add potassium hydroxide as catalyzer, wherein, the weight of potassium hydroxide is 2 parts, with the reactant stirring reaction in the reactor, and be heated to 70 ℃ of reactions after 3 hours, in reactor, drip silane coupling agent N-(β-aminoethyl of 10 parts)-γ-aminopropyl methyl dimethoxysilane, and N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane dripped off in 10 minutes, reheat be warming up to 80 ℃ and react 11 hours after, be cooled to 40 ℃, add 1.5 parts of Glacial acetic acid and stirred 2 hours, the pH value of reactant is adjusted to 9, the mass percent of the effective constituent of silicone oil is 45% in the last product.
Embodiment 2
At first, in weight part, the octamethylcyclotetrasiloxane (D4) that adds 600 parts in the reactor, add again entry as solvent, wherein the weight of water is 450 parts, then the fatty alcohol-polyoxyethylene ether that adds 6.8 parts, add simultaneously 7.5 parts emulsifying agent and 7.5 parts dispersion agent, the amido silicon oil that adds again 9 parts in addition stirs in reactor, and be heated to 65 ℃, react the water that adds 10 parts after 0.5 hour, then add potassium hydroxide as catalyzer, wherein, the weight of potassium hydroxide is 4 parts, with the reactant stirring reaction in the reactor, and be heated to 90 ℃ of reactions after 1 hour, drip 30 parts silane coupling agent N-cyclohexyl-y-aminopropyl methyl dimethoxysilane in the reactor, and N-cyclohexyl-y-aminopropyl methyl dimethoxysilane dripped off in 15 minutes, reheat be warming up to 100 ℃ and react 9 hours after, be cooled to 60 ℃, add 3.5 parts of Glacial acetic acid and stirred 4 hours, the pH value of reactant is adjusted to 7, the mass percent of the effective constituent of silicone oil is 55% in the last product.
Embodiment 3
At first, in weight part, the octamethylcyclotetrasiloxane (D4) that adds 500 parts in the reactor, add again entry as solvent, wherein the weight of water is 350 parts, then the fatty alcohol-polyoxyethylene ether that adds 5.8 parts, add simultaneously 6.5 parts emulsifying agent and 6.5 parts dispersion agent, the amido silicon oil that adds again part in addition stirs in reactor, and be heated to 58 ℃, react the water that adds 8.5 parts after 1.5 hours, then add potassium hydroxide as catalyzer, wherein, the weight of potassium hydroxide is 2.8 parts, with the reactant stirring reaction in the reactor, and be heated to 78 ℃ of reactions after 2 hours, drip 20 parts silane coupling agent γ-divinyl triammonium propyl group methyl dimethoxysilane in the reactor, and γ-divinyl triammonium propyl group methyl dimethoxysilane dripped off in 20 minutes, reheat be warming up to 92 ℃ and react 10 hours after, be cooled to 50 ℃, add 2.55 parts of Glacial acetic acid and stirred 3 hours, the pH value of reactant is adjusted to 8, the mass percent of the effective constituent of silicone oil is 50% in the last product.
Advantage of the present invention is: by hydrophilic silicone oil is mixed with silicone monomers, reaction generates silicone oil, has increased the flexibility of silicone oil, and the fiber of processing through this silicone oil has the good over-all propertieies such as smooth and resilience.
Above demonstration and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification sheets just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (4)
1. the preparation method of a silicone oil is characterized in that, in weight part, may further comprise the steps:
Adding 400～600 parts octamethylcyclotetrasiloxane and 250～450 parts water is hydrolyzed in reactor;
Add 4.8～6.8 parts fatty alcohol-polyoxyethylene ether, 5.5～7.5 parts emulsifying agent, 5.5～7.5 parts dispersion agent and 7～9 parts amido silicon oil and in described reactor, stir, and be warming up to 45～60 ℃ of maintenances 0.5～2.5 hour;
Add 8～10 parts water and 2～4 parts potassium hydroxide and in above-mentioned reactant, stir, and be warming up to 70～90 ℃ of maintenances 1～3 hour;
Drip 10～30 parts of coupling agents in above-mentioned reactant, be warming up to 80～100 ℃ and keep being cooled to 40～60 ℃ after 9～11 hours; And
Add 1.5～3.5 parts of Glacial acetic acid and in above-mentioned reactant, stirred 2～4 hours, adjust PH to 7～9, temperature discharging in the time of 30～50 ℃.
2. the preparation method of silicone oil as claimed in claim 1 is characterized in that, described coupling agent is silane coupling agent.
3. the preparation method of silicone oil as claimed in claim 2, it is characterized in that, described silane coupling agent is N-(β-aminoethyl)-a kind of in the γ-aminopropyl methyl dimethoxysilane, N-cyclohexyl-y-aminopropyl methyl dimethoxysilane, γ-divinyl triammonium propyl group methyl dimethoxysilane or their arbitrary combination.
4. such as the preparation method of each described silicone oil of claims 1 to 3, it is characterized in that, described coupling agent dripped off in 10～20 minutes.
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| CN2012103619550A CN102898654A (en) | 2012-09-25 | 2012-09-25 | Method for preparing silicon oil |
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| CN2012103619550A CN102898654A (en) | 2012-09-25 | 2012-09-25 | Method for preparing silicon oil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104179000A (en) * | 2014-09-12 | 2014-12-03 | 王朗 | Manufacturing method of waterproof braided fabric |
| CN104452278A (en) * | 2014-11-28 | 2015-03-25 | 周正英 | Finishing agent used for fabric with 30% of wool and 70% of acrylic and having fluffing function |
| CN105175734A (en) * | 2015-10-22 | 2015-12-23 | 上海上萃精细化工有限公司 | Preparation method of terpolymer silicone oil |
| CN105793488A (en) * | 2013-12-03 | 2016-07-20 | Kb都筑株式会社 | Modified fiber and method for producing same |
| CN106835716A (en) * | 2017-02-28 | 2017-06-13 | 青岛奥洛思新材料有限公司 | For processing wool or smooth brightening agent containing wool fabric and preparation method thereof |
| CN106892680A (en) * | 2017-02-27 | 2017-06-27 | 广西青龙化学建材有限公司 | GRC component special-purpose protecting agents and preparation method thereof |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6093841A (en) * | 1998-01-02 | 2000-07-25 | Degussa-Huels Aktiengesellschaft | Method for preparing nonreactive aminosilicone oils |
| CN101280520A (en) * | 2008-05-27 | 2008-10-08 | 建德市白沙化工有限公司 | Production process of raising agent |
| CN101434704A (en) * | 2008-12-19 | 2009-05-20 | 段新峰 | Preparation of fluffy soft amino silicon oil emulsion |
| CN101463134A (en) * | 2008-12-09 | 2009-06-24 | 张家港科道化学有限公司 | Modified amino alkyl polysiloxane, method for synthesizing the same and microemulsion composed thereof |
| CN101503515A (en) * | 2009-03-04 | 2009-08-12 | 深圳天鼎精细化工制造有限公司 | Method for synthesizing hydrophile amino silicon oil |
| CN101509196A (en) * | 2009-03-04 | 2009-08-19 | 深圳天鼎精细化工制造有限公司 | Method of preparing epoxy modified amino-silicone oil softening agent |
| CN101550237A (en) * | 2009-05-18 | 2009-10-07 | 安徽德佳有机硅有限公司 | High springback silicone stiffening agent and preparation method thereof |
| CN101805994A (en) * | 2010-03-18 | 2010-08-18 | 佛山市顺德区德美瓦克有机硅有限公司 | Organosilicon emulsion used for hand feel finishing of wool and blended yarn thereof and preparation method and application thereof |
| CN101838395A (en) * | 2010-03-31 | 2010-09-22 | 广州市天河区诺信精细化工研究所 | Double-end amino silicone oil with conditioning functions and preparation method and application of emulsion thereof |
| CN102002162A (en) * | 2010-08-10 | 2011-04-06 | 佛山市顺德区德美瓦克有机硅有限公司 | Cation amino silicone oil micro-emulsion and preparation method thereof |
| JP4723083B2 (en) * | 2000-12-08 | 2011-07-13 | 信越化学工業株式会社 | Method for producing silicone branched polyether-modified silicone compound and cosmetic containing compound obtained by this method |
| CN102336912A (en) * | 2010-07-21 | 2012-02-01 | 宁波晨光纺织助剂有限公司 | Silicone oil emulsion with multiple functional groups and preparation method thereof |
-
2012
- 2012-09-25 CN CN2012103619550A patent/CN102898654A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6093841A (en) * | 1998-01-02 | 2000-07-25 | Degussa-Huels Aktiengesellschaft | Method for preparing nonreactive aminosilicone oils |
| JP4723083B2 (en) * | 2000-12-08 | 2011-07-13 | 信越化学工業株式会社 | Method for producing silicone branched polyether-modified silicone compound and cosmetic containing compound obtained by this method |
| CN101280520A (en) * | 2008-05-27 | 2008-10-08 | 建德市白沙化工有限公司 | Production process of raising agent |
| CN101463134A (en) * | 2008-12-09 | 2009-06-24 | 张家港科道化学有限公司 | Modified amino alkyl polysiloxane, method for synthesizing the same and microemulsion composed thereof |
| CN101434704A (en) * | 2008-12-19 | 2009-05-20 | 段新峰 | Preparation of fluffy soft amino silicon oil emulsion |
| CN101503515A (en) * | 2009-03-04 | 2009-08-12 | 深圳天鼎精细化工制造有限公司 | Method for synthesizing hydrophile amino silicon oil |
| CN101509196A (en) * | 2009-03-04 | 2009-08-19 | 深圳天鼎精细化工制造有限公司 | Method of preparing epoxy modified amino-silicone oil softening agent |
| CN101550237A (en) * | 2009-05-18 | 2009-10-07 | 安徽德佳有机硅有限公司 | High springback silicone stiffening agent and preparation method thereof |
| CN101805994A (en) * | 2010-03-18 | 2010-08-18 | 佛山市顺德区德美瓦克有机硅有限公司 | Organosilicon emulsion used for hand feel finishing of wool and blended yarn thereof and preparation method and application thereof |
| CN101838395A (en) * | 2010-03-31 | 2010-09-22 | 广州市天河区诺信精细化工研究所 | Double-end amino silicone oil with conditioning functions and preparation method and application of emulsion thereof |
| CN102336912A (en) * | 2010-07-21 | 2012-02-01 | 宁波晨光纺织助剂有限公司 | Silicone oil emulsion with multiple functional groups and preparation method thereof |
| CN102002162A (en) * | 2010-08-10 | 2011-04-06 | 佛山市顺德区德美瓦克有机硅有限公司 | Cation amino silicone oil micro-emulsion and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105793488A (en) * | 2013-12-03 | 2016-07-20 | Kb都筑株式会社 | Modified fiber and method for producing same |
| US10590599B2 (en) | 2013-12-03 | 2020-03-17 | Kb Tsuzuki K.K. | Modified fiber and method for producing same |
| CN104179000A (en) * | 2014-09-12 | 2014-12-03 | 王朗 | Manufacturing method of waterproof braided fabric |
| CN104452278A (en) * | 2014-11-28 | 2015-03-25 | 周正英 | Finishing agent used for fabric with 30% of wool and 70% of acrylic and having fluffing function |
| CN105175734A (en) * | 2015-10-22 | 2015-12-23 | 上海上萃精细化工有限公司 | Preparation method of terpolymer silicone oil |
| CN106892680A (en) * | 2017-02-27 | 2017-06-27 | 广西青龙化学建材有限公司 | GRC component special-purpose protecting agents and preparation method thereof |
| CN106835716A (en) * | 2017-02-28 | 2017-06-13 | 青岛奥洛思新材料有限公司 | For processing wool or smooth brightening agent containing wool fabric and preparation method thereof |
| CN106835716B (en) * | 2017-02-28 | 2019-01-01 | 青岛奥洛思新材料有限公司 | For handling wool or the smooth brightening agent containing wool fabric and preparation method thereof |
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