CN103881095A - Preparation method of vinyl silicone oil - Google Patents
Preparation method of vinyl silicone oil Download PDFInfo
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- CN103881095A CN103881095A CN201410060693.3A CN201410060693A CN103881095A CN 103881095 A CN103881095 A CN 103881095A CN 201410060693 A CN201410060693 A CN 201410060693A CN 103881095 A CN103881095 A CN 103881095A
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Abstract
The invention discloses a preparation method of vinyl silicone oil. The preparation method comprises the following steps: 1) adding 2300kg by weight of octamethyl cyclotetrasiloxane into a reactor which has stirring and temperature raising functions and can be vacuumized, raising the temperature to 65 DEG C, introducing dry N2 and dewatering for 1 hour; 2) adding 10.35kg by weight of dry tetramethyl divinyl disiloxane and 0.0184kg by weight of tetramethylammonium hydroxidet, raising the temperature to 100 DEG C and thermally reacting for 3 hours; 3) raising the temperature to 145 DEG C and breaking a medium for 1 hour; 4 further raising the temperature to 180 DEG C, introducing dry N2, lowering molecules at a vacuum degree being greater than -0.098MPa till no liquid flows out; 5) vacuumizing, lowering the temperature to 60 DEG C and discharging a finished product. The vinyl silicone oil prepared through the preparation method has no hydroxyl groups, is rapid to cure and does not stick a mold.
Description
Technical field
The present invention relates to chemical technology field, particularly relate to a kind of preparation method of vinyl silicone oil.
Background technology
In existing technology, vinyl silicone oil production technique is with methylcarbonate (dimethyl carbonate, DMC) be raw material, using Tetramethylammonium hydroxide as catalyzer, taking tetramethyl divinyl disiloxane (Divinyl Tetramethyl Disiloxane) as closure agent, after polyreaction, remove low molecule, obtain vinyl silicone oil product.
But this Countermeasures is more open, easily bring moisture into, thereby make to be prone in target product hydroxyl, thereby affect the curing speed of vinyl silicone oil, be prone to the problems such as sticking to mould after making liquid glue raw material with it.
Summary of the invention
Based on this, the invention provides the preparation method who brings the vinyl silicone oil of hydroxyl in a kind of vinyl silicone oil that prevents from producing.
A preparation method for vinyl silicone oil, comprises the following steps: the first step, by weight, in the reactor with stirring, heat up, can vacuumizing, add the octamethylcyclotetrasiloxane of 2300KG, and be warming up to 65 degree, logical dried N2, dewaters 1 hour; Second step, by weight, adds the 10.35KG tetramethyl divinyl disiloxane of drying and the Tetramethylammonium hydroxide of 0.184KG, and temperature is risen to 100 degree insulation reaction 3 hours; The 3rd step, is warming up to 145 degree, broken matchmaker one hour; The 4th step, continues to be warmed up to 180 degree, logical dried nitrogen, and de-low molecule in the situation that of vacuum tightness >-0.098MPa, extremely till without effluent liquid; The 5th step, goes vacuum, is cooled to below 60 degree discharging.
Further, the alkali glue that described Tetramethylammonium hydroxide is generated by Tetramethylammonium hydroxide and octamethylcyclotetrasiloxane hybrid reaction replaces.
The prepared vinyl silicone oil of preparation method of vinyl silicone oil of the present invention does not contain hydroxyl, and curing speed is fast, not sticking to mould.
Embodiment
The raw material of vinyl silicone oil of the present invention comprises octamethylcyclotetrasiloxane (Octamethyl cyclotetrasiloxane is called for short D4), Tetramethylammonium hydroxide, nitrogen, tetramethyl divinyl disiloxane.The preparation method of vinyl silicone oil of the present invention is: the first step, by weight, in the reactor with stirring, heat up, can vacuumizing, add the octamethylcyclotetrasiloxane of 2300KG, and be warming up to 65 degree, logical dried N2, dewaters 1 hour; Second step, by weight, adds the 10.35KG tetramethyl divinyl disiloxane of drying and the Tetramethylammonium hydroxide of 0.184KG, and temperature is risen to 100 degree insulation reaction 3 hours; The 3rd step, is warming up to 145 degree, broken matchmaker one hour; The 4th step, continues to be warmed up to 180 degree, logical dried nitrogen, and de-low molecule in the situation that of vacuum tightness >-0.098MPa, extremely till without effluent liquid; The 5th step, goes vacuum, is cooled to below 60 degree discharging.
The preparation method of vinyl silicone oil of the present invention obtains product weight, counts by weight 2070KG, and yield is: 90%, and viscosity (25 degree): 10000mpa.s, volatile matter (150 degree * 3 hours) < 1%, and do not contain hydroxyl.
Wherein, in second step, in other embodiments, described Tetramethylammonium hydroxide is replaced by alkali glue, this alkali glue generates (first dehydration, rear temperature reaction) by Tetramethylammonium hydroxide and octamethylcyclotetrasiloxane hybrid reaction, has better dehydration property and processable; In second step, the weight part meter of alkali glue is similarly 0.184KG.
The preparation method of vinyl silicone oil of the present invention, taking octamethylcyclotetrasiloxane as starting material, using Tetramethylammonium hydroxide as catalyzer, taking tetramethyl divinyl disiloxane as closure agent, removes low molecule after polyreaction, obtain vinyl silicone oil product.Wherein, in the present invention, below 4 make in production process, to have avoided occurring moisture: 1: with octamethylcyclotetrasiloxane be starting material, be difficult for bringing into moisture; 2: Tetramethylammonium hydroxide is first made alkali glue in use, and its moisture is thoroughly driven away; 3: the nitrogen using in production process first uses after super-dry; 4: tetramethyl divinyl disiloxane also needs dry rear use.Therefore, the vinyl silicone oil that the present invention prepares does not contain hydroxyl, and curing speed is fast, not sticking to mould.
It should be noted that; for the person of ordinary skill of the art; without departing from the inventive concept of the premise; identical or similar component and formula described in employing the above embodiment of the present invention; or same or analogous method described in employing and the embodiment of the present invention, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (2)
1. a preparation method for vinyl silicone oil, is characterized in that, comprises the following steps: the first step, by weight, in the reactor with stirring, heat up, can vacuumizing, add the octamethylcyclotetrasiloxane of 2300KG, be warming up to 65 degree, logical dried N2, dewaters 1 hour; Second step, by weight, adds the 10.35KG tetramethyl divinyl disiloxane of drying and the Tetramethylammonium hydroxide of 0.184KG, and temperature is risen to 100 degree insulation reaction 3 hours; The 3rd step, is warming up to 145 degree, broken matchmaker one hour; The 4th step, continues to be warmed up to 180 degree, logical dried nitrogen, and de-low molecule in the situation that of vacuum tightness >-0.098MPa, extremely till without effluent liquid; The 5th step, goes vacuum, is cooled to below 60 degree discharging.
2. the preparation method of vinyl silicone oil according to claim 1, is characterized in that: the alkali glue that described Tetramethylammonium hydroxide is generated by Tetramethylammonium hydroxide and octamethylcyclotetrasiloxane hybrid reaction replaces.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410060693.3A CN103881095A (en) | 2014-02-21 | 2014-02-21 | Preparation method of vinyl silicone oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410060693.3A CN103881095A (en) | 2014-02-21 | 2014-02-21 | Preparation method of vinyl silicone oil |
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| CN103881095A true CN103881095A (en) | 2014-06-25 |
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| CN201410060693.3A Pending CN103881095A (en) | 2014-02-21 | 2014-02-21 | Preparation method of vinyl silicone oil |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105218824A (en) * | 2015-11-06 | 2016-01-06 | 东莞市天桉硅胶科技有限公司 | The vinyl silicone oil of low hydroxyl value and its preparation method thereof |
| CN105367798A (en) * | 2015-11-27 | 2016-03-02 | 广州市银讯光电科技有限公司 | Organosilicone basic adhesive for LED chip packaging and preparation method for organosilicone basic adhesive |
| CN105367796A (en) * | 2015-12-10 | 2016-03-02 | 湖北兴瑞化工有限公司 | Technology for promoting storage performance of alkali gel |
| CN105482121A (en) * | 2015-12-29 | 2016-04-13 | 江苏创景科技有限公司 | Synthesis method of polyvinyl silicon oil |
| CN106279697A (en) * | 2016-08-22 | 2017-01-04 | 深圳市新亚新材料有限公司 | A kind of low viscosity vinyl silicone oil and preparation method thereof |
| CN106589379A (en) * | 2016-11-08 | 2017-04-26 | 扬州宏远化工新材料有限公司 | Production method of vinyl silicone oil |
| CN104448315B (en) * | 2014-11-17 | 2017-09-19 | 东莞兆舜有机硅科技股份有限公司 | A kind of transparent alkali glue, preparation method and its usage |
| CN107189069A (en) * | 2017-06-09 | 2017-09-22 | 湖北兴瑞化工有限公司 | A kind of synthetic method of methyl blocking type methyl vinyl silicone rubber |
| CN108484913A (en) * | 2018-03-07 | 2018-09-04 | 江苏科幸新材料股份有限公司 | The preparation method of high-purity ethylene base silicone oil |
| CN109054354A (en) * | 2018-07-25 | 2018-12-21 | 佛山皖阳生物科技有限公司 | A kind of preparation method of artificial tree tree bark materials |
| CN112280304A (en) * | 2020-10-20 | 2021-01-29 | 深圳市诺丰电子科技有限公司 | Efficient heat-conducting silica gel sheet and processing technology |
| CN114736376A (en) * | 2022-04-21 | 2022-07-12 | 广东新硅源新材料科技有限公司 | Preparation method of vinyl silicone oil |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333338A (en) * | 2013-07-11 | 2013-10-02 | 江苏天辰硅材料有限公司 | Vinyl silicone oil and synthetic method thereof |
-
2014
- 2014-02-21 CN CN201410060693.3A patent/CN103881095A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333338A (en) * | 2013-07-11 | 2013-10-02 | 江苏天辰硅材料有限公司 | Vinyl silicone oil and synthetic method thereof |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104448315B (en) * | 2014-11-17 | 2017-09-19 | 东莞兆舜有机硅科技股份有限公司 | A kind of transparent alkali glue, preparation method and its usage |
| CN105218824A (en) * | 2015-11-06 | 2016-01-06 | 东莞市天桉硅胶科技有限公司 | The vinyl silicone oil of low hydroxyl value and its preparation method thereof |
| CN105367798A (en) * | 2015-11-27 | 2016-03-02 | 广州市银讯光电科技有限公司 | Organosilicone basic adhesive for LED chip packaging and preparation method for organosilicone basic adhesive |
| CN105367796A (en) * | 2015-12-10 | 2016-03-02 | 湖北兴瑞化工有限公司 | Technology for promoting storage performance of alkali gel |
| CN105367796B (en) * | 2015-12-10 | 2017-11-21 | 湖北兴瑞化工有限公司 | A kind of technique for lifting alkali glue storge quality |
| CN105482121A (en) * | 2015-12-29 | 2016-04-13 | 江苏创景科技有限公司 | Synthesis method of polyvinyl silicon oil |
| CN106279697A (en) * | 2016-08-22 | 2017-01-04 | 深圳市新亚新材料有限公司 | A kind of low viscosity vinyl silicone oil and preparation method thereof |
| CN106279697B (en) * | 2016-08-22 | 2019-06-25 | 深圳市新亚新材料有限公司 | A kind of low viscosity vinyl silicone oil and preparation method thereof |
| CN106589379A (en) * | 2016-11-08 | 2017-04-26 | 扬州宏远化工新材料有限公司 | Production method of vinyl silicone oil |
| CN107189069A (en) * | 2017-06-09 | 2017-09-22 | 湖北兴瑞化工有限公司 | A kind of synthetic method of methyl blocking type methyl vinyl silicone rubber |
| CN108484913A (en) * | 2018-03-07 | 2018-09-04 | 江苏科幸新材料股份有限公司 | The preparation method of high-purity ethylene base silicone oil |
| CN109054354A (en) * | 2018-07-25 | 2018-12-21 | 佛山皖阳生物科技有限公司 | A kind of preparation method of artificial tree tree bark materials |
| CN112280304A (en) * | 2020-10-20 | 2021-01-29 | 深圳市诺丰电子科技有限公司 | Efficient heat-conducting silica gel sheet and processing technology |
| CN114736376A (en) * | 2022-04-21 | 2022-07-12 | 广东新硅源新材料科技有限公司 | Preparation method of vinyl silicone oil |
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