CN108178833A - A kind of preparation method of silicone oil - Google Patents
A kind of preparation method of silicone oil Download PDFInfo
- Publication number
- CN108178833A CN108178833A CN201711380203.8A CN201711380203A CN108178833A CN 108178833 A CN108178833 A CN 108178833A CN 201711380203 A CN201711380203 A CN 201711380203A CN 108178833 A CN108178833 A CN 108178833A
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- Prior art keywords
- silicone oil
- catalyst
- octamethylcy
- clotetrasiloxane
- microreactor
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The present invention relates to a kind of preparation methods of silicone oil, high containing hydrogen silicone oil, octamethylcy-clotetrasiloxane, hexamethyldisiloxane and catalyst are added in microreactor, or heptamethyltrisiloxane, octamethylcy-clotetrasiloxane and catalyst are added in microreactor, or octamethylcy-clotetrasiloxane, tetramethyl disiloxane and catalyst are added in microreactor, it is reacted under 0 ~ 140 DEG C, 0 ~ 20bar 100 ~ 1000 seconds, then adds in neutralizer and adjust pH>6.5, reaction was completed is made the silicone oil.The present invention is by using microreactor, and preparation method is improved, level of residual monomers is not only reduced to less than 5%, and solve the problems, such as that polymer molecular weight distribution is wide, polymer molecular weight profile exponent is reduced to 1.2 and less, the reaction time is greatly shortened simultaneously, effectively avoids the generation of side reaction.The production technology improve product quality, easy to operate, waste is few, low energy consumption environmental protection.
Description
Technical field
The present invention relates to a kind of preparation methods of silicone oil.
Background technology
At present, based on batch method, this method generally adds in monomer heating for the production of domestic grafted-organosilicon copolymer
After heat (80 DEG C~100 DEG C), catalyst (the generally Bronsted acids such as sulfuric acid) is directly added in a kettle, is polymerize by long-time
After (15~20h), production is completed by processes such as neutralization (alkali neutralization, generally with sodium bicarbonate), cooling, desalination, filterings.
The above method has the following disadvantages：
1) monomer and catalyst impurities residual quantity are high, and generally higher than 8%；
2) polymer molecular weight distribution is wide, molecular weight distribution Index>1.2；
3) there are side reactions in polymerization process；
4) reaction time is long, and energy consumption is high；
5) complex procedures, yield are low (90%~92%).
Invention content
The technical problems to be solved by the invention be to provide it is a kind of it is simple for process, low energy consumption, efficient, high income, rear place
Reason is easy, the preparation method of the silicone oil of narrow molecular weight distribution.
For solution more than technical problem, the present invention adopts the following technical scheme that：
A kind of preparation method of silicone oil, by high containing hydrogen silicone oil (III), octamethylcy-clotetrasiloxane (I), two silica of hexamethyl
Alkane (II) and catalyst are added in microreactor or by heptamethyltrisiloxane (VII), octamethylcy-clotetrasiloxane (I) and are urged
Agent is added in microreactor or is added in octamethylcy-clotetrasiloxane (I), tetramethyl disiloxane (V) and catalyst micro-
It in reactor, is reacted under 0~140 DEG C, 0~20bar 100~1000 seconds, then adds in neutralizer and adjust pH>6.5, terminate anti-
The silicone oil should be made.
Preferably, reaction temperature is 100~140 DEG C, and pressure is 2~8bar.
Preferably, neutralizer adjusts pH to neutrality.
Preferably, the structural formula of the high containing hydrogen silicone oil (III) is：
Wherein, m is the integer between 1~40.
It is reacted when using high containing hydrogen silicone oil (III), octamethylcy-clotetrasiloxane (I), hexamethyldisiloxane (II)
When, reaction equation is：
Wherein, m is the integer between 1~40, and n is the integer between 10~100.
When being reacted using octamethylcy-clotetrasiloxane (I), tetramethyl disiloxane (V), reaction equation is：
Wherein, m is the integer between 10~100.
When being reacted using heptamethyltrisiloxane (VII), octamethylcy-clotetrasiloxane (I), reaction equation is：
Wherein, n is the integer between 5~50.
Preferably, the high containing hydrogen silicone oil, the octamethylcy-clotetrasiloxane, the hexamethyldisiloxane
The mass ratio that feeds intake is 1~5：10~100:2~10；Further preferably 1~5：10~50:2~5；More preferably 1~4：20~
30:2~4.
Preferably, the mass ratio that feeds intake of the heptamethyltrisiloxane, the octamethylcy-clotetrasiloxane for 5~
30:10~100；Further preferably 5~20:10~50；More preferably 5~10:10~20.
Preferably, the mass ratio that feeds intake of the octamethylcy-clotetrasiloxane, tetramethyl disiloxane is 20~100:1~
10, further preferably 20~50:1~5, more preferably 20~40:1~2.
Preferably, the quality that feeds intake of the catalyst is the high containing hydrogen silicone oil, four silica of prestox ring
The 1%~10% of the gross mass of feeding intake of alkane, the hexamethyldisiloxane and the catalyst；Further preferably 1%
~5%；More preferably 1%~3%.
Preferably, the quality that feeds intake of the catalyst is the heptamethyltrisiloxane, the prestox ring four
The 1%~10% of the gross mass of feeding intake of siloxanes and the catalyst；Further preferably 1%~5%；More preferably 1%
~3%.
Preferably, the quality that feeds intake of the catalyst is the octamethylcy-clotetrasiloxane, the tetramethyl two
The 1%~10% of the gross mass of feeding intake of siloxanes and the catalyst；Further preferably 1%~5%；More preferably 1%
~3%.
Preferably, the catalyst is selected from sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, heteropoly acid, sulfuric acid, hydrochloric acid, phosphoric acid, vinegar
One or more of acid, heteropoly acid handle one kind in the Emathlite formed, sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, heteropoly acid
Or several handle one or more of acidic resins for forming.
Preferably, the neutralizer is one kind or several in sodium bicarbonate, sodium carbonate, potassium carbonate, saleratus
Kind.
Preferably, the microreactor is the G1-G4 microreactors of Corning Incorporated, and microwell array declines channel reactor
Or the material of the bold and generous Chemical Engineering Technology Co., Ltd of AFR-G1-G4 reactors or Shandong that material is stainless steel, glass or SiC is
316L, FFKM, Du Pont Kalrez0040,304, PEEK, PTFE, fluorine silicone rubber, 6061-T6, carbon steel nickel plating, PTFE, ABS, EVA
MRSS120 reactors.
Preferably, the microreactor is included for warm-up block that material is mixed and preheated, and described
The first heat transfer module that warm-up block is connected and is sequentially connected in series, the second heat transfer module, third heat transfer module, the 4th heat transfer mould
Block, the 5th heat transfer module, the 6th heat transfer module, the 7th heat transfer module, the discharging mode being connected with the 7th heat transfer module
Block；Or
The microreactor is included for by the silicon oil of low hydrogen content, the allyl polyether, the catalyst
The reactive moieties for being exchanged heat, preheated, mixed, reacting and being controlled with the buffer.
Preferably, the mass tranfer coefficient of the microreactor is 1~30Ka, and exchange capability of heat is more than 1700KW/m2*k。
Preferably, the catalyst and the high containing hydrogen silicone oil are first mixed to form mixture or will be described
Catalyst is mixed to form mixture with the octamethylcy-clotetrasiloxane, then controls micro- described in the mixture input
The feed flow of reactor is 1~50g/min.
It is further preferred that the feed flow of the mixture is 10~40g/min, more preferably 15~30g/min.
Due to the implementation of above technical scheme, the present invention has the following advantages that compared with prior art：
The present invention is improved by using microreactor, and to preparation method, and level of residual monomers not only is reduced to 5%
Hereinafter, and solve the problems, such as that polymer molecular weight is wide, polymer molecular weight profile exponent is reduced to 1.2 and hereinafter, simultaneously
The reaction time is greatly shortened, effectively avoids the generation of side reaction.The production technology improves product quality, easy to operate, useless
Environmental protection that gurry is few, low energy consumption.
Description of the drawings
Structure diagram of the attached drawing 1 for the micro passage reaction of the Corning Incorporated used in the present invention；
Structure diagram of the attached drawing 2 for the bold and generous Chemical Engineering Technology Co., Ltd MRSS120 reactors in Shandong used in the present invention,
Wherein, 1, installation frame；2nd, reactor；3rd, heat exchanging pipe；
Monomer test result figure of the attached drawing 3 for the product of embodiment 1；
Monomer test result figure of the attached drawing 4 for the product of comparative example 1；
Attached drawing 5 composes nuclear-magnetism test chart for the silicon of the product of comparative example 2；
Attached drawing 6 composes nuclear-magnetism test chart for the silicon of the product of embodiment 2.
Specific embodiment
With reference to specific embodiment, the present invention will be further described in detail, but the present invention is not limited to following implementations
Example.The implementation condition used in embodiment can do further adjustment according to specifically used different requirements, the implementation being not specified
Condition is the normal condition in the industry.Involved number is parts by weight in the present invention.
Embodiment 1：
At 30 DEG C, by the 5 parts high containing hydrogen silicone oil (III) added with catalyst sulfuric acid, 25 parts of octamethylcy-clotetrasiloxanes
(I) and 2 parts of hexamethyldisiloxane press the G2 microreactors that (II) is respectively delivered to Corning Incorporated using differential responses delivery pump
Warm-up block in mixed and preheated, then flow sequentially through the first heat transfer module, the second heat transfer module, third heat transfer mould
Block, the 4th heat transfer module, the 5th heat transfer module, the 6th heat transfer module, the 7th heat transfer module are reacted, and then add in bicarbonate
Sodium carries out neutralization reaction and adjusts pH as neutrality, finally flow to material discharging module and collects to obtain into collecting tank after discharging after cooling down
Silicone oil (IV).
Wherein, the feed flow of the high containing hydrogen silicone oil (III) added with catalyst sulfuric acid be 20g/min, the throwing of catalyst
Expect 1% that quality is material gross mass, warm-up block, the first heat transfer module, the second heat transfer module, third heat transfer module, the 4th
The temperature control of heat transfer module, the 5th heat transfer module, the 6th heat transfer module, the 7th heat transfer module is 120 DEG C, pressure 6bar,
By warm-up block, the first heat transfer module, the second heat transfer module, third heat transfer module, the 4th heat transfer module, the 5th heat transfer mould
Block, the 6th heat transfer module, the 7th heat transfer module total time be 108 seconds.
Embodiment 2：
At 20 DEG C, by 40 parts of octamethylcy-clotetrasiloxanes (I) added with catalyst heteropoly acid and 2 parts of two silicon of tetramethyl
Oxygen alkane (V) using differential responses delivery pump be respectively delivered to the MRSS120 reactors of the bold and generous Chemical Engineering Technology Co., Ltd in Shandong into
Row reaction, and using potassium carbonate as neutralizer, remaining is same as Example 1.
Embodiment 3：
At 45 DEG C, by 20 parts of octamethylcy-clotetrasiloxanes (I) added with acidity of catalyst carclazyte and 5 part of seven methyl three
Siloxanes (VII) is respectively delivered to the G2 microreactors of Corning Incorporated using differential responses delivery pump, remaining and 1 phase of embodiment
Together.
Comparative example 1：
4.68 parts high containing hydrogen silicone oil (III), 25 parts of octamethylcy-clotetrasiloxanes (I) and 2 parts of hexamethyldisiloxane are pressed
(II) 100 DEG C are heated to, then adds in 0.32 part of catalyst sulfuric acid, is reacted at 120 DEG C 20 hours, then adds in neutralizer carbon
Sour hydrogen sodium carries out neutralization reaction and adjusts pH as neutrality, and desalination, product is obtained by filtration in cooling.
Comparative example 2：
39.58 parts of octamethylcy-clotetrasiloxanes (I) and 2 parts of tetramethyl disiloxanes (V) are heated to 100 DEG C, Ran Houjia
Enter 0.42 part of catalyst heteropoly acid, reacted at 120 DEG C 20 hours, then add in neutralizer potassium carbonate and carry out neutralization reaction and adjust
PH is saved as neutrality, desalination, product is obtained by filtration in cooling.
Table 1 is the test result of each embodiment and comparative example.Table 2 is the performance parameter of microreactor.
1) content of monomer in product is measured by gas chromatography.
GC conditions
Gas phase surveys spectrum：PE Clanus 600 FID
Chromatographic column：Capillary column Elite-1
Size：30m*0.25mm*0.25um
Chromatography column condition：60 DEG C maintain 3 minutes, then 280 DEG C are risen to 10 DEG C/min of heating rate, at 280 DEG C
It maintains 8 minutes
Carrier gas：Nitrogen, 1.2ml/min
Injector temperature：260℃
Sampling volume：1.0ul
Detector type and temperature：FID, 325 DEG C
Front and rear cleaning solvent：THF
Practical measurement result is shown referring to table 1, Fig. 3, Fig. 4, testing result：Fig. 3 is that the monomer in embodiment 1 in sample is surveyed
Test result, the content of monomer being computed are 3.5%.Fig. 4 is the monomer test result in 1 sample of comparative example, the monomer being computed
Content is 9.45%, hence it is evident that less than usual mode.
2) the side reaction situation in nuclear-magnetism test product is composed by silicon.
Test equipment：BRUKER 400MHz
Test condition：PROBHD 5mm NUCl 29-Si
65536 solvent C DCl of TD surface sweepings number3
Test result is shown in Table 1, Fig. 5, Fig. 6, it is seen that 1 peak (A) is had more in 2 sample of comparative example, is secondary anti-through analyzing this peak
The middle silanol generated is answered, does not have peak detection in the sample of embodiment 2, illustrates without side reaction to occur in example 2.
3) in traditional mode of production, neutralization procedure generates salt, and oversaturated salt can in the product occur as crystalline state.Pass through
Sodium potassium content in Atomic absorption wide spectrum method test sample tests acid ion content by titration mode.Above knot
Fruit all indicates that this instance method sample ions content is significantly lower than the usual mode of production.
Table 1
Table 2
The present invention is described in detail above, its object is to allow the personage for being familiar with this field technology that can understand this
The content of invention is simultaneously implemented, and it is not intended to limit the scope of the present invention, all Spirit Essence institutes according to the present invention
The equivalent change or modification of work should all cover within the scope of the present invention.
Claims (10)
1. a kind of preparation method of silicone oil, it is characterised in that：By high containing hydrogen silicone oil, octamethylcy-clotetrasiloxane, two silicon of hexamethyl
Oxygen alkane and catalyst add in microreactor or add in heptamethyltrisiloxane, octamethylcy-clotetrasiloxane and catalyst
It is added in microreactor in microreactor or by octamethylcy-clotetrasiloxane, tetramethyl disiloxane and catalyst, 0~
140 DEG C, react under 0~20bar 100~1000 seconds, then add in neutralizer and adjust pH>6.5, reaction was completed is made the silicon
Oil.
2. the preparation method of silicone oil according to claim 1, it is characterised in that：The structural formula of the high containing hydrogen silicone oil
For：
Wherein, m is the integer between 1~40.
3. the preparation method of silicone oil according to claim 1 or 2, it is characterised in that：It is the high containing hydrogen silicone oil, described
Octamethylcy-clotetrasiloxane, the hexamethyldisiloxane the mass ratio that feeds intake for 1~5：10~100:2~10；
The heptamethyltrisiloxane, the octamethylcy-clotetrasiloxane the mass ratio that feeds intake be 5~30:10~100；
The octamethylcy-clotetrasiloxane, tetramethyl disiloxane the mass ratio that feeds intake be 20~100:1~10.
4. the preparation method of silicone oil according to claim 1 or 2, it is characterised in that：The quality that feeds intake of the catalyst
For the high containing hydrogen silicone oil, the octamethylcy-clotetrasiloxane, the hexamethyldisiloxane and the catalyst
Gross mass of feeding intake 1%~10%；
The quality that feeds intake of the catalyst is the heptamethyltrisiloxane, the octamethylcy-clotetrasiloxane and described
Catalyst gross mass of feeding intake 1%~10%；
The quality that feeds intake of the catalyst is the octamethylcy-clotetrasiloxane, the tetramethyl disiloxane and described
Catalyst gross mass of feeding intake 1%~10%.
5. the preparation method of silicone oil according to claim 1, it is characterised in that：The catalyst is selected from sulfuric acid, salt
The acidity that the processing of one or more of acid, phosphoric acid, acetic acid, heteropoly acid, sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, heteropoly acid forms is white
One or more of acidic resins that the processing of one or more of soil, sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, heteropoly acid forms.
6. the preparation method of silicone oil according to claim 1, it is characterised in that：The neutralizer is selected from bicarbonate
One or more of sodium, sodium carbonate, potassium carbonate, saleratus.
7. the preparation method of silicone oil according to claim 1, it is characterised in that：The microreactor is Corning Incorporated
G1-G4 microreactors, decline channel reactor or material of microwell array are reacted for the AFR-G1-G4 of stainless steel, glass or SiC
The material of the bold and generous Chemical Engineering Technology Co., Ltd of device or Shandong for 316L, FFKM, Du Pont Kalrez0040,304, PEEK, PTFE,
Fluorine silicone rubber, 6061-T6, carbon steel nickel plating, PTFE, ABS, EVA MRSS120 reactors.
8. the preparation method of the silicone oil according to claim 1 or 7, it is characterised in that：The microreactor includes being used for
The warm-up block that material is mixed and preheated, the first heat transfer mould for being connected and being sequentially connected in series with the warm-up block
Block, the second heat transfer module, third heat transfer module, the 4th heat transfer module, the 5th heat transfer module, the 6th heat transfer module, the 7th heat transfer
Module, the material discharging module being connected with the 7th heat transfer module；Or
The microreactor is included for by the silicon oil of low hydrogen content, the allyl polyether, the catalyst and institute
The reactive moieties that the buffer stated is exchanged heat, preheated, mixed, react and controlled.
9. the preparation method of the silicone oil according to claim 1 or 7, it is characterised in that：The mass transfer system of the microreactor
Number is 1~30Ka, and exchange capability of heat is more than 1700KW/m2*k。
10. the preparation method of silicone oil according to claim 1, it is characterised in that：First by the catalyst with it is described
High containing hydrogen silicone oil is mixed to form mixture or is mixed to form with the octamethylcy-clotetrasiloxane catalyst mixed
Material is closed, the feed flow for the microreactor for then controlling the mixture input described is 1~50g/min.
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| CN201711380203.8A CN108178833A (en) | 2017-12-20 | 2017-12-20 | A kind of preparation method of silicone oil |
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| CN201711380203.8A CN108178833A (en) | 2017-12-20 | 2017-12-20 | A kind of preparation method of silicone oil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110938207A (en) * | 2019-12-10 | 2020-03-31 | 烟台开发区金宏化工有限公司 | Preparation method of hydrogen-containing silicone oil |
| CN111548500A (en) * | 2020-05-29 | 2020-08-18 | 广州星粤新材料有限公司 | Method for preparing polyether grafted polysiloxane by using microchannel reactor |
| CN115386080A (en) * | 2021-05-25 | 2022-11-25 | 江西蓝星星火有机硅有限公司 | Method for preparing polyether modified siloxane |
| WO2022270336A1 (en) * | 2021-06-23 | 2022-12-29 | 東レ・ファインケミカル株式会社 | Method for producing silicone polymer |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110938207A (en) * | 2019-12-10 | 2020-03-31 | 烟台开发区金宏化工有限公司 | Preparation method of hydrogen-containing silicone oil |
| CN110938207B (en) * | 2019-12-10 | 2022-02-22 | 烟台开发区金宏化工有限公司 | Preparation method of hydrogen-containing silicone oil |
| CN111548500A (en) * | 2020-05-29 | 2020-08-18 | 广州星粤新材料有限公司 | Method for preparing polyether grafted polysiloxane by using microchannel reactor |
| CN115386080A (en) * | 2021-05-25 | 2022-11-25 | 江西蓝星星火有机硅有限公司 | Method for preparing polyether modified siloxane |
| CN115386080B (en) * | 2021-05-25 | 2023-09-19 | 江西蓝星星火有机硅有限公司 | Method for preparing polyether modified siloxane |
| WO2022270336A1 (en) * | 2021-06-23 | 2022-12-29 | 東レ・ファインケミカル株式会社 | Method for producing silicone polymer |
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