CN104672454B - Waste silicone rubber produces the synthetic method of 201 methyl-silicone oils - Google Patents
Waste silicone rubber produces the synthetic method of 201 methyl-silicone oils Download PDFInfo
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Abstract
The present invention relates to the synthetic method that a kind of waste silicone rubber produces 201 methyl-silicone oils.Dimethyl siloxane mixed methylcyclosiloxane in waste silicone rubber is evacuated in reactor, 80 DEG C 90 DEG C is warming up to, using TMAH as catalyst, and adds HMDO, heats up and makes to keep 95 DEG C -98 DEG C in reactor, polymerize 45 hours；Heating valve is opened afterwards, continues to heat up, keeps vacuum, and when temperature rises to 150 DEG C -160 DEG C, then slowly heating is de- low, is incubated when temperature rises to 200 DEG C -210 DEG C；Then low boilers are observed by visor, when its flow to very little, temperature rises to 240 DEG C, opens high-vacuum pump and takes out again 3 hours, silicone oil flash-point and fugitive constituent are improved.The present invention is not only recycled waste, has been obtained the higher silicone oil of economic value, has not only been achieved good economic benefit, avoided the pollution to environment, while has improved the yield of product.
Description
Technical field
The present invention relates to a kind of synthetic method of 201 silicone oil, more particularly to a kind of diformazan produced using waste silicone rubber
The method that radical siloxane mixed methylcyclosiloxane produces 201 silicone oil.
Background technology
The production technology that China produces 201 silicone oil at present is typically all that organic silicon monomer production is extracted from crustal rock
201 silicone oil, this technics comparing is complicated, and energy consumption is huge.
The now industry such as economic rapid development, electronics, communication, IT in China is even more to advance by leaps and bounds, caused waste and old silicon
With regard to more and more, these useless silica gel can not degrade rubber under natural environment, be formerly only available carry out landfill disposal, cause resource
Waste and aggravate the burden of environment.
The content of the invention
The present invention is directed to drawbacks described above, and it is an object of the present invention to provide one kind is obtained waste and old silicon rubber by rational technological design
The method that glue produces 201 silicone oil.
It is for this technical solution adopted by the present invention：The present invention is by the dimethyl siloxane mixed methylcyclosiloxane in waste silicone rubber
It is evacuated in reactor, is warming up to 80 DEG C -90 DEG C, using TMAH as catalyst, and adds HMDO,
Heat up and make to keep 95 DEG C -98 DEG C in reactor, polymerize 4-5 hours；Heating valve is opened afterwards, continues to heat up, and keeps vacuum,
When temperature rises to 150 DEG C -160 DEG C, then slowly heating is de- low, is incubated when temperature rises to 200 DEG C -210 DEG C；Then lead to
Visor observation low boilers are crossed, when its flow to very little, temperature rises to 240 DEG C, opens high-vacuum pump and takes out again 3 hours, silicon
Oil flash point and fugitive constituent improve.
Polymerization reaction time is 4.5 hours.
Polymeric reaction temperature is 95 DEG C.
Dimethyl siloxane mixed methylcyclosiloxane in waste silicone rubber is evacuated in reactor by the present invention, is warming up to 85 DEG C of left sides
The right side, using TMAH as catalyst, and HMDO is added, 95 DEG C -98 DEG C are kept in reactor, gathered
Close 4-5 hours, it is rear to open heating valve, start to warm up, keep vacuum, when temperature rises to 150 DEG C -160 DEG C, start to warm up
When de- low, slowly heating, unsuitable too fast, the unsuitable flash that visor material goes out is seen, unlatching stirring is such as de- low too fast, then stops heating up,
Keep de- low unsuitable too fast, can so make product oil yield higher, be generally possible to the yield of raising 3~10%, save 8% or so
Manpower, production cost is saved.When temperature rises to 200 DEG C -210 DEG C, insulation, the low boilers flow seen in visor is to very
Hour, now temperature can rise to 240 DEG C, open high-vacuum pump and take out again 3 hours, silicone oil flash-point and fugitive constituent are improved.
The present invention is using the advanced technology such as Pintsch process, to caused waste computer in production and life, mobile phone key, useless
The waste silicone rubbers such as old glass cement carry out Pintsch process, and this reaction obtains the silicon of dimethyl siloxane mixed methylcyclosiloxane ring containing prestox four
Oxygen alkane is generally below 80%, compared with the dimethyl siloxane mixed methylcyclosiloxane that organic silicon monomer factory produces, the silica of basic ring containing pregnancy three
Alkane and other low molecular weight polyorganosiloxanes are more, and hexamethyl cyclotrisiloxane is easily true in de- low molecule when producing 201 silicone oil
Sky is extracted out, and the yield of product reduces, therefore the present invention reduces such a situation by slowing down the method for temperature rise.
The present invention is not only recycled waste, has obtained the higher silicone oil of economic value, is not only achieved good
Economic benefit, avoid the pollution to environment, while improve the yield of product.
Embodiment
Embodiment one：
Dimethyl siloxane mixed methylcyclosiloxane in waste silicone rubber is evacuated in reactor by the present invention, is warming up to 90 DEG C, with
TMAH adds HMDO as catalyst, heats up and makes to keep 95 DEG C in reactor, polymerization 4
Hour；Heating valve is opened afterwards, continues to heat up, keeps vacuum, and de- low, slow heating 2 hours is carried out when temperature rises to 180 DEG C
Take off low to 210 DEG C and be incubated；Then low boilers are observed by visor, when its flow to very little, temperature rises to 240 DEG C, beats
Drive high-vacuum pump to take out again 3 hours, silicone oil flash-point and fugitive constituent are improved.
Embodiment two：
Dimethyl siloxane mixed methylcyclosiloxane in waste silicone rubber is evacuated in reactor by the present invention, is warming up to 85 DEG C, with
TMAH adds HMDO as catalyst, heats up and makes to keep 95 DEG C in reactor, polymerization 5
Hour；Heating valve is opened afterwards, continues to heat up, keeps vacuum, and de- low, slow heating 3 hours is carried out when temperature rises to 160 DEG C
Take off low to 210 DEG C and be incubated；Then low boilers are observed by visor, when its flow to very little, temperature rises to 240 DEG C, beats
Drive high-vacuum pump to take out again 3 hours, silicone oil flash-point and fugitive constituent are improved.
Embodiment three：
Dimethyl siloxane mixed methylcyclosiloxane in waste silicone rubber is evacuated in reactor by the present invention, is warming up to 90 DEG C, with
TMAH adds HMDO as catalyst, heats up and makes to keep 98 DEG C in reactor, polymerization
4.5 hour；Heating valve is opened afterwards, continues to heat up, keeps vacuum, is carried out when temperature rises to 150 DEG C de- low, slowly heats up 4
Hour takes off low and is incubated to 210 DEG C；Then low boilers are observed by visor, when its flow to very little, temperature rises to 240
DEG C, open high-vacuum pump and take out again 3 hours, silicone oil flash-point and fugitive constituent are improved.
Example IV：
Dimethyl siloxane mixed methylcyclosiloxane in waste silicone rubber is evacuated in reactor by the present invention, is warming up to 85 DEG C, with
TMAH adds HMDO as catalyst, heats up and makes to keep 96 DEG C in reactor, polymerization 4
Hour；Heating valve is opened afterwards, continues to heat up, keeps vacuum, and de- low, slow heating 1 hour is carried out when temperature rises to 180 DEG C
Take off low to 210 DEG C and be incubated；Then low boilers are observed by visor, when its flow to very little, temperature rises to 240 DEG C, beats
Drive high-vacuum pump to take out again 3 hours, silicone oil flash-point and fugitive constituent are improved
The result that each embodiment obtains is：
Dimethyl siloxane mixed methylcyclosiloxane of the raw material all for waste silicone rubber production produces 1000CS viscosity or so 201 silicone oil
The present invention polymerisation equation be：
Claims (3)
1. waste silicone rubber produces the synthetic method of 201 silicone oil, it is characterised in that by the dimethyl siloxane in waste silicone rubber
Mixed methylcyclosiloxane is evacuated in reactor, is warming up to 80 DEG C -90 DEG C, using TMAH as catalyst, and adds hexamethyl
Disiloxane, heat up and make to keep 95 DEG C -98 DEG C in reactor, polymerize 4-5 hours；Heating valve is opened afterwards, continues to heat up,
Vacuum is kept, when temperature rises to 150 DEG C -160 DEG C, then slowly 3 hours or 4 hours to 210 DEG C of heating is de- low and is incubated；
Then low boilers are observed by visor, when its flow to very little, temperature rises to 240 DEG C, and it is small that opening high-vacuum pump takes out 3 again
When, silicone oil flash-point and fugitive constituent are improved.
2. waste silicone rubber according to claim 1 produces the synthetic method of 201 silicone oil, it is characterised in that polymerisation
Time is 4.5 hours.
3. waste silicone rubber according to claim 1 produces the synthetic method of 201 silicone oil, it is characterised in that polymerisation
Temperature is 95 DEG C.
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| CN106084229A (en) * | 2016-06-06 | 2016-11-09 | 湖北新海鸿化工有限公司 | The preparation method of 201 methyl-silicone oils |
| CN106046378A (en) * | 2016-06-29 | 2016-10-26 | 扬州宏远化工新材料有限公司 | Production method of low-viscosity silicone oil |
| CN110305322A (en) * | 2019-07-11 | 2019-10-08 | 枣阳市华威硅氟材料有限公司 | The production method of dimethicone |
| CN111087620A (en) * | 2019-12-31 | 2020-05-01 | 枣阳市金鹏化工有限公司 | Method for synthesizing 201 methyl silicone oil from waste silicone rubber |
| CN112293725A (en) * | 2020-10-21 | 2021-02-02 | 扬州宏远新材料股份有限公司 | Preparation process of food-grade additive polydimethylsiloxane emulsion |
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| CN101649047A (en) * | 2008-08-14 | 2010-02-17 | 扬州宏远化工新材料有限公司 | Simethicone |
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| CN102140170B (en) * | 2010-12-28 | 2012-12-05 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation process of high-molecular-weight permethyl silicone oil |
| CN104017366B (en) * | 2014-03-24 | 2016-09-28 | 任炳陵 | Silicon rubber cracking reclaiming technique |
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| CN101649047A (en) * | 2008-08-14 | 2010-02-17 | 扬州宏远化工新材料有限公司 | Simethicone |
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Address after: 225200 Hongyuan Road, Shao Industry Park, Jiangdu District, Jiangsu, Yangzhou Patentee after: Yangzhou Hongyuan new material Limited by Share Ltd Address before: 225200 Hongyuan Road, Shao Industry Park, Jiangdu District, Jiangsu, Yangzhou Patentee before: Yangzhou Hongyuan Chemical Industry New Material Co., Ltd. |
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