CN107629080A - A kind of method for preparing pentamethyl disiloxane - Google Patents
A kind of method for preparing pentamethyl disiloxane Download PDFInfo
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- CN107629080A CN107629080A CN201710802256.8A CN201710802256A CN107629080A CN 107629080 A CN107629080 A CN 107629080A CN 201710802256 A CN201710802256 A CN 201710802256A CN 107629080 A CN107629080 A CN 107629080A
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- disiloxane
- pentamethyl disiloxane
- emathlite
- hmdo
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Abstract
The present invention relates to a kind of method for preparing pentamethyl disiloxane, with 1,1,3,3 tetramethyl disiloxane and HMDO for raw material, is balanced reaction under Emathlite catalysis, pentamethyl disiloxane then is made by rectifying.Raw material is simple and easy to get needed for the present invention, reacts efficient stable, and process is simple, is discharged without " three wastes ", and industrialized production can be achieved, have larger market prospects and economic value.
Description
Technical field
The invention belongs to organosilicon chemistry to synthesize field, and in particular to a kind of side for preparing high-purity pentamethyl disiloxane
Method.
Background technology
Pentamethyl disiloxane is a kind of important silicone intermediate, and its feature is there is active silicon-hydrogen bond, can
As the monomer of synthesizing organo-silicon high polymer, carburet thing addition generation silico-carbo polymer.Therefore, pentamethyl disiloxane
There is extremely important status in synthesizing organo-silicon product.The disclosed method for preparing pentamethyl disiloxane in the prior art
It is that raw material is prepared by method for hydrolysis mostly with dimethylchlorosilane or derivatives thereof：Disclosure Te Xu publications JP64031791
Using dimethylethoxysilane and trim,ethylchlorosilane as raw material, disclosure Te Xu publications JP3002188 are with dimethyl chloride silicon
Alkane is raw material with hexamethyldisilazane, and disclosure Te Xu publications JP2157285 is reported with trimethyl silanol and dimethyl chloride
Silane is raw material.The common drawback of these three methods is：Expensive raw material price causes cost higher, and product yield is low, there is " three
It is useless " discharge, be not suitable for mass industrialized production.Patent CN101875662B exists with high containing hydrogen silicone oil in solvent and cosolvent
Lower progress grignard reaction, then hydrolyze and prepare pentamethyl disiloxane, this method equipment requirement is high, raw material RMgBr price
Costliness, process are cumbersome, are difficult to realize industrialized production.Patent publication No CN106046039A alkali metal silicon alkoxide and dimethyl
Halide reacts under solvent condition, prepares pentamethyl disiloxane by filtering rectifying, this method reaction condition is difficult to be controlled, be right
Equipment requirement is high, has " three wastes " discharge, is difficult to realize industrialized production.
The content of the invention
In order to overcome existing preparation method exist product cost height, complex process, it is seriously polluted the shortcomings that, the present invention propose
A kind of preparation method that pentamethyl disiloxane is prepared using acidic catalyst.
Technical scheme is as follows：
A kind of method for preparing pentamethyl disiloxane, reaction equation are as follows：
Formula 1
Reactions steps are as follows：
1）1,1,3,3 ,-tetramethyl disiloxane and HMDO react under Emathlite, and described 1,1,3,3 ,-four
Tetramethyldisiloxane and HMDO weight ratio are 1:1-1:2；Reaction temperature is 50 DEG C, reaction time 2h；
2）The Emathlite in mix products is isolated, mix products are then subjected to atmospheric distillation purification, collects 84-86 DEG C
Cut.Produce purity>99% pentamethyl disiloxane.
Wherein three kinds of mixtures 1,1,3,3 of step 1) generation ,-tetramethyl disiloxane, pentamethyl disiloxane and six
The boiling point of tetramethyldisiloxane is more or less the same, therefore common distillation is unable to reach purification effect, and the present invention selects rectifying mode
Purification.Simultaneously rectifying go out 1,1,3,3 ,-tetramethyl disiloxane and HMDO can reclaim reuse.
In a preferable technical scheme, the step 1）In 1,1,3,3 ,-tetramethyl disiloxane, the silicon of hexamethyl two
The weight of oxygen alkane and Emathlite ratio is 10:10:1.
Compared with traditional organic silicon monomer Hydrolyze method, preparation method of the invention has the following advantages that：
1, raw material is simple and easy to get, simple without solvent, process；2, balanced reaction temp is low, the time is short, efficient stable, and energy consumption is small；
3, without " three wastes ", pollution-free, accessory substance is few, high income；4, it is easier to obtain the product of high-purity, more than 98%；5. industry can be realized
Metaplasia is produced, and has larger market prospects and economic value.
Embodiment
With reference to embodiment, the present invention will be further described, but protection scope of the present invention is not limited to implement
Example.
Embodiment 1
500 milliliters equipped with thermometer, agitator, condenser three-necked flask in, add 134g1,1,3,3, the silicon of-tetramethyl two
Oxygen alkane, 162g HMDOs and the 23.68g concentrated sulfuric acids, 8h is reacted at 10 DEG C, sulfuric acid is separated, obtains the silica of pentamethyl two
Alkane content is 50.7% mix products, and rectifying collects 84-86 DEG C of cut, obtains the target compound of water white transparency, meteorological color
Compose purity assay and be more than 99%, yield 38%.
Embodiment 2
500 milliliters equipped with thermometer, agitator, condenser three-necked flask in, add 180g1,1,3,3, the silicon of-tetramethyl two
Oxygen alkane, 90g HMDOs and 8.1g strong acid ion exchange resins, 4h is reacted at 30 DEG C, has filtered resin, get Wu Jia
Base disiloxane content is 44.8% mix products, and rectifying collects 84-86 DEG C of cut, obtains the target chemical combination of water white transparency
Thing, chromatography of gases purity assay are more than 98%, yield 32%.
Embodiment 3
500 milliliters equipped with thermometer, agitator, condenser three-necked flask in, add 100g1,1,3,3, the silicon of-tetramethyl two
Oxygen alkane, 100g HMDOs and 10.0g Emathlites, 2h is reacted at 50 DEG C, Emathlite is filtered to remove, obtains pentamethyl
Disiloxane content is 51.5% mix products, and rectifying collects 84-86 DEG C of cut, obtains the target compound of water white transparency,
Chromatography of gases purity assay is more than 99%, yield 40%.
Embodiment 4
500 milliliters equipped with thermometer, agitator, condenser three-necked flask in, add 90g1,1,3,3, the silicon of-tetramethyl two
Oxygen alkane, 180g HMDOs and 2.7g solid super-strong acids, 5h is reacted at 40 DEG C, solid super-strong acid is filtered, obtains pentamethyl
Disiloxane content is 46.2% mix products, and rectifying collects 84-86 DEG C of cut, obtains the target compound of water white transparency,
Chromatography of gases purity assay is more than 98%, yield 35%.
It is above the description to the embodiment of the present invention, by the foregoing description of the disclosed embodiments, makes this area special
Industry technical staff can realize or using the present invention.A variety of modifications to these embodiments come to those skilled in the art
Say and will be apparent.Generic principles defined herein can not depart from the situation of the spirit or scope of the present invention
Under, realize in other embodiments.Therefore, the present invention is not intended to be limited to these implementation columns shown in this article, but to accord with
Close the most wide scope consistent with principles disclosed herein and novel point.
Claims (2)
1. a kind of method for preparing pentamethyl disiloxane, reaction equation are as follows：
Formula 1
Reactions steps are as follows：
1）1,1,3,3 ,-tetramethyl disiloxane and HMDO react under Emathlite, and described 1,1,3,3 ,-four
Tetramethyldisiloxane and HMDO weight ratio are 1:1-1:2；Reaction temperature is 50 DEG C, reaction time 2h；
2）The Emathlite in mix products is isolated, mix products are then subjected to atmospheric distillation purification, collects 84-86 DEG C
Cut.
A kind of 2. method for preparing pentamethyl disiloxane according to claim 1, it is characterised in that：The step 1）In
1,1,3,3 ,-tetramethyl disiloxane, the weight ratio of HMDO and Emathlite is 10:10:1.
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| CN201710802256.8A CN107629080A (en) | 2017-09-07 | 2017-09-07 | A kind of method for preparing pentamethyl disiloxane |
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| CN201710802256.8A CN107629080A (en) | 2017-09-07 | 2017-09-07 | A kind of method for preparing pentamethyl disiloxane |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384763A (en) * | 2014-09-04 | 2016-03-09 | 上海楚青新材料科技有限公司 | 1,1,1,3,3,5,5-heptamethyltrisiloxane preparation method |
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2017
- 2017-09-07 CN CN201710802256.8A patent/CN107629080A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384763A (en) * | 2014-09-04 | 2016-03-09 | 上海楚青新材料科技有限公司 | 1,1,1,3,3,5,5-heptamethyltrisiloxane preparation method |
Non-Patent Citations (2)
| Title |
|---|
| KOPYLOV ,V. M. ET AL: "Disproportionation reaction of organodisiloxanes with various silicon-atom substituents"", 《ZHURNAL OBSHCHEI KHIMII》 * |
| 来国桥等著: "《有机硅产品合成工艺及应用》", 31 March 2013, 化学工业出版社 * |
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Application publication date: 20180126 |