CN105085921B - A method of preparing Methyl Hydrogen Polysiloxane Fluid using organic silicon byproduct - Google Patents
A method of preparing Methyl Hydrogen Polysiloxane Fluid using organic silicon byproduct Download PDFInfo
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- CN105085921B CN105085921B CN201510508540.5A CN201510508540A CN105085921B CN 105085921 B CN105085921 B CN 105085921B CN 201510508540 A CN201510508540 A CN 201510508540A CN 105085921 B CN105085921 B CN 105085921B
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- polysiloxane fluid
- organic silicon
- hydrogen polysiloxane
- methyl
- methyl hydrogen
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Abstract
A kind of method preparing Methyl Hydrogen Polysiloxane Fluid using organic silicon byproduct is to utilize organic silicon byproduct monomethyl dichlorosilane, end-capping reagent tri-methyl-chlorosilane and the washing diluted acid of recycling cohydrolysis reaction under certain condition, the hydrogen chloride gas that hydrolysis generates is removed using compressed air blowback, stratification and depickling repeatedly washed to upper solution after the completion of reaction, product is neutralized again, filtering, takes off low process and obtains Methyl Hydrogen Polysiloxane Fluid finished product.It was verified that Methyl Hydrogen Polysiloxane Fluid viscosity prepared by the present invention is controllable, stable quality is easy to industrialized production, greatly improves the comprehensive utilization value of organic silicon byproduct monomethyl dichlorosilane.
Description
Technical field
The invention belongs to organic silicon byproduct production technical fields, and in particular to a kind of to utilize organic silicon byproduct monomethyl
The method that dichlorosilane prepares Methyl Hydrogen Polysiloxane Fluid.
Background technology
As silicone industry rapidly develops, organosilicon chlorosilane monomer yield is also increasing, it is contemplated that current year Mo, state
Interior organic silicon monomer manufacturing enterprise aggregated capacity about 2500kt/a.Monomethyl dichlorosilane is the pair of organosilicon chlorosilane monomer production
One of product accounts for about monomer capacity 1.5% or so, only 41.1 DEG C of boiling point under normal pressure, explosion limit ranging from 6 ~ 55%, summer temp
It is excessively high to be also easy to produce vaporization phenomenon, cause safety accident；Containing Si-Cl and active Si -- H bond inside the substance, after contacting humid air
A large amount of acid mists are generated, and then cause secondary accident, therefore, analyzes, is necessary in terms of saving production cost and safety and environmental protection
The substance is comprehensively utilized.
Currently, most of organosilicon enterprise prepares Methyl Hydrogen Polysiloxane Fluid using monomethyl dichlorosilane both at home and abroad, main point
For solvent method and solventless method.Wherein solvent method prepares Methyl Hydrogen Polysiloxane Fluid and not only needs a large amount of toxic organic solvents, such as benzene, first
Benzene etc., and the defects of finished product is there are solvent odor, storage time is short, easy acid reflux, cannot be used in high-end product.It is solvent-free
Method can avoid the various deficiencies of solvent method product, can produce higher gears product, meet high-end user demand, be conducive to high-end
The cultivation in market, potential market capacity are huge.102643428 A of Chinese patent CN provide a kind of solventless method production methyl
The method of containing hydrogen silicone oil instills in hydrolytic reaction pot, passes through after mixing monomethyl dichlorosilane and tri-methyl-chlorosilane
Hydrolysis temperature and material dropping speed are controlled to control reaction process, hydrolysate is centrifuged, filters, taking off low three-procedure
Refined Methyl Hydrogen Polysiloxane Fluid is obtained afterwards.Solvent-free consumption in this method production process, reduces product processing operation, carries
High product quality；It is deacidified and is detached to crude product using centrifugal method, life cycle of the product is shortened, still, due to operation ring
Border is harsh,
The centrifugation apparatus of use is expensive, and it still needs further improvement etc. that factors limit making for the technology for separating effect
With.102030905 A of Chinese patent CN describe the method that another solventless method prepares Methyl Hydrogen Polysiloxane Fluid, i.e., by one
Reaction kettle is added in dimethyl dichlorosilane (DMCS), tri-methyl-chlorosilane, and inorganic salt solution water is added dropwise with certain speed under stirring
Solution, stratification obtains crude containing hydrogen silicone oil after the completion of reaction, then it is neutralized, de- it is low after obtain refined methyl hydrogen silicon
Oil.This method process equipment is simple, and investment cost is low, still, since monomethyl dichlorosilane and tri-methyl-chlorosilane hydrolyze
Speed is inconsistent, and mixing is uneven will to directly affect hydrolysis quality, and then influence product quality, in addition, stirring apparatus for reaction kettle
Easily the factors such as damage also limit the use of the technology to sealing surface under strong acidic environment.
Invention content
It is an object of the invention to overcome the above-mentioned prior art, a kind of utilization monomethyl dichlorosilane preparation is provided
The method of Methyl Hydrogen Polysiloxane Fluid.
The method provided by the invention for preparing Methyl Hydrogen Polysiloxane Fluid using monomethyl dichlorosilane includes the following steps：
（A）Enamel reaction still is added in the washing dilute acid soln of recycling, opens reaction kettle cooling device and bottom blowback pressure
Contracting air；
（B）Monomethyl dichlorosilane, end-capping reagent tri-methyl-chlorosilane are added dropwise after static mixer mixing in proportion
Into reaction kettle, temperature of reaction kettle is controlled at -5-45 DEG C, wherein：Monomethyl dichlorosilane and tri-methyl-chlorosilane mass ratio
Example is 1:0.05~0.005；
（C）After the completion of hydrolysis, hydrolysate is sent into after standing head tank standing 30-60min, discharge lower layer 25 ~
31% concentrated hydrochloric acid obtains crude containing hydrogen silicone oil, wherein：Lower layer's concentrated hydrochloric acid whole export trade；
（D）It is repeatedly passed through appropriate technique water washing crude containing hydrogen silicone oil, the dilute hydrochloric acid solution that recycling washing generates is simultaneously
It is completely used for step（A）In washing diluted acid.
（E）The Methyl Hydrogen Polysiloxane Fluid after depickling is washed again after alkaline matter neutralizes, into filter device except impurity.
（F）The Methyl Hydrogen Polysiloxane Fluid come out from filter through it is de- it is low after be obtain Methyl Hydrogen Polysiloxane Fluid finished product, wherein：It is de- low
System vacuum：0.09-0.01MPa, temperature：110~125℃.
The present invention compared with the existing technology the advantage is that：
1, using the advance mixing reaction mass of static mixer and end-capping reagent, it can make that entire hydrolysis is more stable, water
It is more excellent to solve effect；
2, it using cheap compressed air blowback reaction solution, takes the hydrogen chloride gas that a large amount of hydrolysis generate out of, reduces
Hydrogen chloride gas is dissolved in the heat of water release, reduces the consumption of public work cold；A large amount of hydrogen chloride gas are carried over system
The concentration of hydrochloric acid remained in silicone oil is reduced, neutralizer usage amount is reduced；Air blowback causes hydrating solution internal disturbance,
Alternative stirring apparatus for reaction kettle, reduces industrial production cost；
3, hydrochloric acid inside crude containing hydrogen silicone oil solution removal is repeatedly washed using process water, reduces follow-up neutralizer
The solid matters such as the salt that usage amount and reaction generate, and then mitigate filter device load；The diluted acid water that washing is generated is whole
Reuse alleviates the effluent pressure of enterprise, greatly reduces the industrial production cost of product.
Specific implementation mode
Embodiment 1
The washing sour water of recycling is added into enamel reaction still, opens reaction kettle cooling device and blowback compression in bottom is empty
Gas；1000kg monomethyls dichlorosilane, 10kg tri-methyl-chlorosilanes are added dropwise to reaction kettle after static mixer mixing, tieed up
Temperature in the kettle is held at 15 ± 5 DEG C；After the completion of hydrolysis, hydrolysate is delivered to standing head tank, 30min is stood and isolates
Lower layer's sour water obtains crude containing hydrogen silicone oil；After technique water washing crude containing hydrogen silicone oil 3 times, then use sodium bicarbonate
It is 6-7 or so to be neutralized to pH value, is filtered, and low point is removed in silicone oil under 120 ± 5 DEG C of 80 ± 5KPa of vacuum degree, temperature environment
Son can obtain Methyl Hydrogen Polysiloxane Fluid finished product after 3h, wherein：Hydrogen content：1.58%, index of refraction（25℃）：1.4016, viscosity (25
DEG C, mm2/s）：30, proportion：0.9956, volatile matter：2.536%.
Embodiment 2
Other implementation conditions are such as 1, when end-capping reagent tri-methyl-chlorosilane is 20kg, gained Methyl Hydrogen Polysiloxane Fluid
Hydrogen content：1.55%, index of refraction（25℃）：1.4048, viscosity (25 DEG C, mm2/s）：22, proportion：0.9945, it volatilizees
Point：2.584%.
Embodiment 3
Other implementation conditions are such as 1, and when end-capping reagent tri-methyl-chlorosilane is 5kg, gained Methyl Hydrogen Polysiloxane Fluid is hydrogeneous
Amount：1.61%, index of refraction（25℃）：1.4021, viscosity (25 DEG C, mm2/s）：35, proportion：0.9949, volatile matter：2.576%.
Embodiment 4
Other implementation conditions are such as 1, when using sodium carbonate for neutralizer, gained Methyl Hydrogen Polysiloxane Fluid hydrogen content：
1.56%, index of refraction（25℃）：1.4075, viscosity (25 DEG C, mm2/s）：37, proportion：0.9959, volatile matter：2.539%.
Embodiment 5
Other implementation conditions are such as 1, when using ammonia for neutralizer, gained Methyl Hydrogen Polysiloxane Fluid hydrogen content：1.55%、
Index of refraction（25℃）：1.4087, viscosity (25 DEG C, mm2/s）：40, proportion：0.9963, volatile matter：2.541%.
Claims (1)
1. a kind of method preparing hexamethyldisiloxane using organic silicon byproduct, which is characterized in that include the following steps：
The washing sour water of recycling is added into enamel reaction still, opens reaction kettle cooling device and bottom blowback compressed air；It will
1000kg monomethyls dichlorosilane, 10kg tri-methyl-chlorosilanes are added dropwise to reaction kettle after static mixer mixing, maintain kettle
Interior temperature is at 15 ± 5 DEG C；After the completion of hydrolysis, hydrolysate is delivered to standing head tank, 30min is stood and isolates lower layer
Sour water obtains crude containing hydrogen silicone oil；It is neutralized after technique water washing crude containing hydrogen silicone oil 3 times, then with sodium bicarbonate
It is 6-7 to pH value, filters, and remove low molecule in silicone oil under 120 ± 5 DEG C of 80 ± 5KPa of vacuum degree, temperature environment, is after 3h
Methyl Hydrogen Polysiloxane Fluid finished product can be obtained, wherein：Hydrogen content：1.58%, 25 DEG C of index of refraction：1.4016,25 DEG C of viscosity, mm2/s：30, compare
Weight：0.9956, volatile matter：2.536%.
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| CN107603230B (en) * | 2017-08-25 | 2020-06-26 | 山东东岳有机硅材料股份有限公司 | Silicone rubber prepared by using organosilicon low-boiling hydrolysate and preparation method thereof |
| CN113307974B (en) * | 2021-06-21 | 2022-11-22 | 江西蓝星星火有机硅有限公司 | Method for rapidly recovering hydrogen-containing silicone oil in acid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030905A (en) * | 2010-12-06 | 2011-04-27 | 唐山三友硅业有限责任公司 | Method for preparing solvent-free high hydrogen containing silicone oil |
| CN104193997A (en) * | 2014-08-21 | 2014-12-10 | 湖北兴发化工集团股份有限公司 | Method and device for preparing high-boiling silicon oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102408566A (en) * | 2011-10-10 | 2012-04-11 | 衢州瑞力杰化工有限公司 | Production method of methyl hydrogen-containing silicone oil |
| CN102643428A (en) * | 2012-04-27 | 2012-08-22 | 泸州北方化学工业有限公司 | Method for preparing methyl hydrogen polysiloxane oil |
| CN103923319B (en) * | 2014-04-08 | 2016-03-30 | 吉林华丰有机硅有限公司 | The method of high containing hydrogen silicone oil is produced in the solvent-free hydrolysis of monomethyl dichlorosilane |
| CN104140532A (en) * | 2014-07-30 | 2014-11-12 | 成都博达爱福科技有限公司 | Solvent-free process method for continuously producing methyl hydrogen silicone oil |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030905A (en) * | 2010-12-06 | 2011-04-27 | 唐山三友硅业有限责任公司 | Method for preparing solvent-free high hydrogen containing silicone oil |
| CN104193997A (en) * | 2014-08-21 | 2014-12-10 | 湖北兴发化工集团股份有限公司 | Method and device for preparing high-boiling silicon oil |
Non-Patent Citations (1)
| Title |
|---|
| 三甲基氯硅烷水解合成六甲基二硅氧烷的研究;张丹丹，陈海平，苗刚;《有机硅材料》;20150527;全文 * |
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Address after: 443007 No. 66-2 Ting Ting Road, Ting Ting District, Yichang, Hubei Patentee after: Hubei Xingrui silicon material Co., Ltd. Address before: 443006 No. 29 Changjiang Road, Ting Ting District, Yichang, Hubei Patentee before: HUBEI XINGRUI CHEMICAL CO., LTD. |