CN107033351A - A kind of preparation technology of ultralow viscous dimethicone - Google Patents
A kind of preparation technology of ultralow viscous dimethicone Download PDFInfo
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- CN107033351A CN107033351A CN201611079203.XA CN201611079203A CN107033351A CN 107033351 A CN107033351 A CN 107033351A CN 201611079203 A CN201611079203 A CN 201611079203A CN 107033351 A CN107033351 A CN 107033351A
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- dimethicone
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- preparation technology
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- viscosity dimethicone
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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
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Abstract
The invention discloses a kind of preparation technology of ultralow viscous dimethicone, rectifying mode is used to the low molecule separation in dimethicone, by setting rectifying condition, high boiling component and separation low boiling component can farthest be retained, and then better control over octamethylcy-clotetrasiloxane and decamethylcyclopentaandoxane etc. molecule content in the higher ultralow viscous dimethicone of boiling point, it is set to meet the application requirement of some special high-end applications field such as personal care industries, the lower ultralow viscous linear dimethyl silicone oil of boiling point can also be intercepted from rectifying cut simultaneously, improve a yield of reaction.
Description
Technical field
It is adapted to the present invention relates to a kind of preparation technology of ultralow viscous dimethicone, more particularly to one kind in personal nursing row
The preparation technology of the ultralow viscous dimethicone of industry.
Background technology
Dimethicone is the transparency liquid of colorless and odorless, and its surface tension is low, and with high surface-active, excellent disappears
Steep anti-foaming property and good film forming.Dimethicone has hydrophobicity, water insoluble.Dimethicone has good with other materials
Good isolation, greasy property is more excellent.In the case where not influenceing to breathe freely, there is the moist performance of barrier.Dimethicone is in width
Within the temperature range of viscosity B coefficent it is small.Heat resistance acid-proof.Chemical property is stable, and boiling point is high, and freezing point is low, is used as liquid
The wide temperature range of presence.The electrical property of dimethicone is good, and rate factor is small when especially in various frequency ranges, its surface
Power is small.Anti-shear performance is excellent.The excellent property based on more than, dimethicone is widely used in machinery, electric, weaving, applied
The each department of national economy such as material, medical science.In the production process of dimethicone, industrially generally use by low mole of matter
The low molar mass dimethyl polysiloxane (MDnM) that the dimethicone (D4 or DMC) of amount is blocked with trimethylsiloxy group
Through catalytic equilibration, then in the acquisition after pulling out low molecular compound under maximum vacuum at 150-200 DEG C.This method is general
It is adapted to prepare the dimethicone that viscosity is higher than more than 50cs, for the dimethicone of more low viscosity, using this method not only
One time yield is low, high energy consumption, and product quality can not meet the requirement of some special industries.Particularly personal nursing row
Industry, the residual volume control to ring bodies such as D4, D5 is more and more stricter.
CN201410290685 discloses a kind of continuous preparation process of high-purity low-viscosity dimethicone, including with
Lower step：Methyl cyclosiloxane and end-capping reagent are removed water through liquid nitrogen frozen successively, depth water removal makes the water content of mixture extremely
Below 300ppb, then through adsorption filtration, ultrafiltration membrance filter, preheating, enters catalytic reaction in the fluid bed equipped with catalyst,
Gained reactant sloughs low-boiling-point substance through adsorption filtration, ultrafiltration membrance filter, de- low process, obtains dimethicone.The patent is only suitable for
Prepare and be less than 50-1000mm2/ s dimethicone, is not suitable for preparing less than 50mm2/ below s silicone oil；And the patent makes
With adsorption filtration, ultrafiltration membrance filter, equipment investment is added, technological process is longer.
The content of the invention
It is an object of the invention to provide a kind of preparation technology of ultralow viscous dimethicone, raw material is made full use of, is being protected
Ultralow viscous the two of the high-end applications field that meets, particularly personal care industries purposes are prepared in the case of demonstrate,proving a good yield
Methyl-silicone oil.
A kind of preparation technology of ultra-low viscosity dimethicone, comprises the following steps：Methyl cyclosiloxane after metering and
Methyl blocking agent is further pulled out by being added to after adsorbent in reactor or flask in the case where heating up and being passed through nitrogen
Moisture in material, reaches and adds catalyst after reaction temperature into reactor or flask, maintenance reaction for a period of time, until mixed
The viscosity for closing liquid is not changing, and material is turned over rectifying still is moved to after filter, sets under rectifying condition, interception different temperatures
Cut, can obtain the ultra-low viscosity dimethicone wire body of different viscosities from the cut under different temperatures, and kettle liquid is viscous
The slightly higher ultra-low viscosity dimethicone of degree, sub-fraction wire body and ring body cut can return to continue in next batch reaction into
Row balanced reaction.
A kind of preparation technology of ultra-low viscosity dimethicone, described methyl cyclosiloxane and the quality of methyl blocking agent
Than for 1-10:1.
A kind of preparation technology of ultra-low viscosity dimethicone, described methyl cyclosiloxane is the silica of prestox ring four
Alkane, decamethylcyclopentaandoxane or dimethicone.
A kind of preparation technology of ultra-low viscosity dimethicone, described methyl blocking agent is that chemical general formula is Me3SiO
(Me2SiO)nSiMe3Compound, wherein n=1-100.
A kind of preparation technology of ultra-low viscosity dimethicone, described methyl blocking agent is that chemical general formula is Me3SiO
(Me2SiO)nSiMe3Compound and methyl cyclosiloxane mixture, wherein n=1-100.
A kind of preparation technology of ultra-low viscosity dimethicone, the adsorbent is adsorbent of molecular sieve.
A kind of preparation technology of ultra-low viscosity dimethicone, the drying nitrogen is nitrogen of the dew point below -40 DEG C.
A kind of preparation technology of ultra-low viscosity dimethicone, the reaction temperature is 50-100 degrees Celsius.
A kind of preparation technology of ultra-low viscosity dimethicone, the catalyst is Emathlite or large aperture cation acid
Property resin.
A kind of preparation technology of ultra-low viscosity dimethicone, the rectifying column be vacuum, separate the temperature difference 10 DEG C with
On component.
The advantage of the invention is that：
1st, present invention setting methyl cyclosiloxane and the mass ratio of methyl blocking agent, can prepare in the range of this and arbitrarily be less than
50mm2/ s ultralow viscous dimethicone, by feed change ratio, can adjust the yield of purpose product.
2nd, the present invention is inhaled before raw material methyl cyclosiloxane and methyl blocking agent are added into reactor by adsorbent
It is attached fall impurity therein, it is to avoid impurity, which is introduced in after reactor, can not remove clean, impurities accumulation be caused, to subsequent production
Impact.
3rd, the present invention uses rectifying mode to the low molecule separation in dimethicone, by setting rectifying condition,
Can farthest retain high boiling component and separation low boiling component, so better control over boiling point it is higher ultralow viscous two
Octamethylcy-clotetrasiloxane and decamethylcyclopentaandoxane etc. molecule content in methyl-silicone oil, allow it meeting some spies
The application requirement of different high-end applications field such as personal care industries, while can also be intercepted from rectifying cut, boiling point is lower to be surpassed
Low viscous linear dimethyl silicone oil, improves a yield of reaction.
4th, preparation technology of the invention can meet performance requirement of the high-end applications field to ultralow viscous dimethicone, obtain
The ultralow viscous dimethicone purity arrived is high, wherein the ring body content such as octamethylcy-clotetrasiloxane and decamethylcyclopentaandoxane
It is low, and the dimethicone of the more low viscosity of high added value can be obtained from rectifying cut simultaneously, improve the one of raw material
Secondary utilization rate, reduces energy consumption.
5th, the wire body and ring body that can not be directly utilized on a small quantity in the present invention can be recycled, and reach raw material availability
100%, zero-emission is reached, is a kind of and the environment-friendly environmental protection technique for efficiently preparing high-purity silicone oil with low viscosity, it is adaptable to
The production of ultralow low viscosity dimethyl silicone oil.
Embodiment
Below in conjunction with specific embodiment, the present invention is furture elucidated, but these embodiments are only used for explaining the present invention, without
It is to be used to limit the scope of the present invention.
Embodiment 1：
Handle HMDO and dimethicone with molecular sieve in advance, by the HMDO handled well and
Dimethicone is with 2:3 mass ratio is added in 1000ml flask, starts heating, while being passed through drying into flask
Nitrogen, pulls out water half an hour, is warming up to 80 DEG C, adds and dries 602 resins, 8h is reacted at 80 DEG C, viscosity no longer changes, cooling drop
Warm to room temperature, filter, filtrate is transferred in the flask with rectifying column and carries out rectifying, cut under 91 DEG C/- 90KPa of interception, i.e.,
For octamethyltrisiloxane, yield reaches 8%, and it is 99.8% to analyze its purity；Cut under 127 DEG C/- 90KPa is intercepted, yield reaches
9%, it is 99.1% to analyze its purity；Cut under 158 DEG C/90KPa is intercepted, yield is 9%, it is 98.5% to analyze its purity；Exist again
Rectifying to no liquid flows out under 163/-90KPa, takes kettle liquid, yield is 63%, analyzes its viscosity for 5.1mm2/ s, prestox ring four
Content of siloxane is 0.067%, and decamethylcyclopentaandoxane content is 0.091%；Remaining 11% cut is left to lower batch reaction cycle
Use.
Embodiment 2：
HMDO and octamethylcy-clotetrasiloxane are delivered to adsorbent of molecular sieve cylinder from respective storage tank with pump, passed through
8000L enamel reaction stills are squeezed into after sorbent tube, the mass ratio control of HMDO and octamethylcy-clotetrasiloxane exists
35:65, total amount of feeding is 5000L, by low-pressure steam to reactor heat temperature raising, and is passed through by bottom insertion tank into kettle
Nitrogen, pulls out water 45 minutes, is warming up to 70 DEG C, adds and shifts to an earlier date dried catalyst, the balanced reaction 10h at 70 DEG C, and viscosity is not
Change again, be transferred to rectifying tower reactor after material is delivered into filter filtering, open vacuum system, rectification parameters are set,
Cut, as octamethyltrisiloxane under 91 DEG C/- 90KPa are intercepted, yield reaches 8%, it is 99.5% to analyze its purity；Interception 127
DEG C/- 90KPa under cut, yield reaches 8%, and it is 99.0% to analyze its purity；Cut under 158 DEG C/90KPa is intercepted, yield is 9%,
It is 98.3% to analyze its purity；Rectifying to no liquid flows out under 163/-90KPa again, takes kettle liquid, yield is 63%, analyzes it and glues
Spend for 6.2mm2/ s, octamethylcy-clotetrasiloxane content is 0.061%, and decamethylcyclopentaandoxane content is 0.093%；It is remaining
10% cut is left to lower batch reaction cycle and used.
Embodiment 3：
HMDO and octamethylcy-clotetrasiloxane are delivered to adsorbent of molecular sieve cylinder from respective storage tank with pump, passed through
Squeeze into 8000L enamel reaction stills after sorbent tube, HMDO and octamethylcy-clotetrasiloxane from mass ratio control
20:80, total amount of feeding is 5000L, by low-pressure steam to reactor heat temperature raising, and is led to by bottom insertion tank into kettle
Enter nitrogen, pull out water 45 minutes, be warming up to 60 DEG C, add catalyst dried in advance, balanced reaction 13h, viscosity at 60 DEG C
No longer change, be transferred to rectifying tower reactor after material is delivered into filter filtering, open vacuum system, set rectifying to join
Cut, as octamethyltrisiloxane under number, 91 DEG C/- 90KPa of interception, yield reach 6%, and it is 99.5% to analyze its purity；Interception
Cut under 127 DEG C/- 90KPa, yield reaches 7%, and it is 99.0% to analyze its purity；Cut under 158 DEG C/90KPa is intercepted, yield is
7%, it is 98.3% to analyze its purity；Rectifying to no liquid flows out under 163/-90KPa again, takes kettle liquid, yield is 74%, analyzes it
Viscosity is 10.1mm2/ s, octamethylcy-clotetrasiloxane content is 0.061%, and decamethylcyclopentaandoxane content is 0.093%；It is surplus
6% cut of remaininging is left to lower batch reaction cycle and used.
Claims (10)
1. a kind of preparation technology of ultra-low viscosity dimethicone, it is characterised in that：Comprise the following steps：Methyl ring after metering
Siloxanes and methyl blocking agent are entered by being added to after adsorbent in reactor or flask in the case where heating up and being passed through nitrogen
One step pulls out the moisture in material, reaches and adds catalyst after reaction temperature into reactor or flask, during one section of maintenance reaction
Between, until the viscosity of mixed liquor is not changing, material is turned over rectifying still is moved to after filter, rectifying condition is set, and interception is not
Cut under synthermal, can obtain the ultra-low viscosity dimethicone wire body of different viscosities from the cut under different temperatures, and
Kettle liquid is the slightly higher ultra-low viscosity dimethicone of viscosity, and it is anti-that sub-fraction wire body and ring body cut can return to next batch
Continue to be balanced reaction in answering.
2. a kind of preparation technology of ultra-low viscosity dimethicone as claimed in claim 1, it is characterised in that：Described methyl
Cyclosiloxane and the mass ratio of methyl blocking agent are 1-10:1.
3. a kind of preparation technology of ultra-low viscosity dimethicone as claimed in claim 1, it is characterised in that：Described methyl
Cyclosiloxane is octamethylcy-clotetrasiloxane, decamethylcyclopentaandoxane or dimethicone.
4. a kind of preparation technology of ultra-low viscosity dimethicone as claimed in claim 1, it is characterised in that：Described methyl
End-capping reagent is that chemical general formula is Me3SiO(Me2SiO)nSiMe3Compound, wherein n=1-100.
5. a kind of preparation technology of ultra-low viscosity dimethicone as claimed in claim 1, it is characterised in that：Described methyl
End-capping reagent is that chemical general formula is Me3SiO(Me2SiO)nSiMe3Compound and methyl cyclosiloxane mixture, wherein n=1-
100。
6. a kind of preparation technology of ultra-low viscosity dimethicone as claimed in claim 1, it is characterised in that：The adsorbent
For adsorbent of molecular sieve.
7. a kind of preparation technology of ultra-low viscosity dimethicone as claimed in claim 1, it is characterised in that：The dry nitrogen
Gas is nitrogen of the dew point below -40 DEG C.
8. a kind of preparation technology of ultra-low viscosity dimethicone as claimed in claim 1, it is characterised in that：The reaction temperature
Spend for 50-100 degrees Celsius.
9. a kind of preparation technology of ultra-low viscosity dimethicone as claimed in claim 1, it is characterised in that：The catalyst
For Emathlite or large aperture cation acidic resins.
10. a kind of preparation technology of ultra-low viscosity dimethicone as claimed in claim 1, it is characterised in that：The rectifying
Tower is vacuum, separates component of the temperature difference more than 10 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611079203.XA CN107033351B (en) | 2016-11-30 | 2016-11-30 | Preparation process of ultralow-viscosity dimethyl silicone oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611079203.XA CN107033351B (en) | 2016-11-30 | 2016-11-30 | Preparation process of ultralow-viscosity dimethyl silicone oil |
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| Publication Number | Publication Date |
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| CN107033351A true CN107033351A (en) | 2017-08-11 |
| CN107033351B CN107033351B (en) | 2020-09-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611079203.XA Active CN107033351B (en) | 2016-11-30 | 2016-11-30 | Preparation process of ultralow-viscosity dimethyl silicone oil |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110687228A (en) * | 2019-11-14 | 2020-01-14 | 湖南九典制药股份有限公司 | Method for detecting related substances in simethicone |
| CN110804185A (en) * | 2019-11-29 | 2020-02-18 | 湖北新海鸿化工有限公司 | Production process of 201 methyl silicone oil |
| CN110878141A (en) * | 2019-11-29 | 2020-03-13 | 湖北新海鸿化工有限公司 | Production process of room-temperature vulcanized methyl silicone rubber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040082850A (en) * | 2003-03-20 | 2004-09-30 | 주식회사 금강고려화학 | A method for preparing polydimethylsiloxane having low viscosity |
| CN203408486U (en) * | 2013-07-09 | 2014-01-29 | 浙江合盛硅业有限公司 | Device for rectifying and purifying decamethylcyclopentasiloxane from organic silicon high-boiling-point ring body mixture |
| CN104059229A (en) * | 2014-06-18 | 2014-09-24 | 湖北兴发化工集团股份有限公司 | Preparation method for synthesizing methyl silicone oil under catalytic action of solid acid |
-
2016
- 2016-11-30 CN CN201611079203.XA patent/CN107033351B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040082850A (en) * | 2003-03-20 | 2004-09-30 | 주식회사 금강고려화학 | A method for preparing polydimethylsiloxane having low viscosity |
| CN203408486U (en) * | 2013-07-09 | 2014-01-29 | 浙江合盛硅业有限公司 | Device for rectifying and purifying decamethylcyclopentasiloxane from organic silicon high-boiling-point ring body mixture |
| CN104059229A (en) * | 2014-06-18 | 2014-09-24 | 湖北兴发化工集团股份有限公司 | Preparation method for synthesizing methyl silicone oil under catalytic action of solid acid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110687228A (en) * | 2019-11-14 | 2020-01-14 | 湖南九典制药股份有限公司 | Method for detecting related substances in simethicone |
| CN110804185A (en) * | 2019-11-29 | 2020-02-18 | 湖北新海鸿化工有限公司 | Production process of 201 methyl silicone oil |
| CN110878141A (en) * | 2019-11-29 | 2020-03-13 | 湖北新海鸿化工有限公司 | Production process of room-temperature vulcanized methyl silicone rubber |
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| CN107033351B (en) | 2020-09-04 |
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