CN106750310A - A kind of preparation technology of dimethicone - Google Patents
A kind of preparation technology of dimethicone Download PDFInfo
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- CN106750310A CN106750310A CN201611155620.8A CN201611155620A CN106750310A CN 106750310 A CN106750310 A CN 106750310A CN 201611155620 A CN201611155620 A CN 201611155620A CN 106750310 A CN106750310 A CN 106750310A
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- dimethicone
- weight portion
- sulfuric acid
- concentrated sulfuric
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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
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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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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention provides a kind of preparation technology of dimethicone, comprise the following steps：1）A certain proportion of methylsiloxane, octamethylcy-clotetrasiloxane, potassium hydroxide, dimethicone, HMDO are added to reactor, nitrogen is passed through, stirred；2）Continue to be passed through nitrogen, and add the concentrated sulfuric acid, it is 86 90 DEG C, the 3.2h of insulation reaction 2.8 to be warming up to reactor temperature；3）After reaction terminates, stratification releases the reacted concentrated sulfuric acid from reactor bottom valve；4）To adding sodium hydrate aqueous solution to stir in reactor, pH to 7.2 7.6 is adjusted；5）Add water filtering washing, obtains the upper strata oil crude product of neutrality；6）Water removal is stood, oily crude product is removed into low-boiling-point substance, obtain final product dimethicone.Present invention process is simple, improves the surface property of dimethicone, possesses reaction condition gently, and low production cost, catalysis activity is high, and stability is high, the advantage of non-environmental-pollution etc., is conducive to popularization and application on a large scale.
Description
Technical field
The present invention relates to chemical technology field, more particularly to a kind of preparation technology of dimethicone.
Background technology
Dimethicone is the transparency liquid of colorless and odorless, and its surface tension is low, and with surface-active high, excellent disappears
Bubble 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, have and intercept moist performance.Dimethicone is in width
Within the temperature range of viscosity B coefficent it is small.Heat resistance acid-proof.Stable chemical nature, boiling point is high, and freezing point is low, 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
Tension force is small.Anti-shear performance is excellent.The excellent property based on more than, dimethicone is widely used in machinery, electric, spinning
Knit, each department of national economy such as coating, medical science.In the production process of dimethicone, industrially generally use by
The dimethicone (D4 or DMC) of low molar mass gathers with the low molar mass dimethyl of trimethylsiloxy group end-blocking
Siloxanes (MDnM) is produced through equilibration reaction.
But existing dimethyl-silicon oil making technology has that technical requirements are high, cumbersome, production cost is high, and catalysis is lived
Low, the low defect of stability of property.
The content of the invention
In order to solve the above technical problems, the invention provides a kind of preparation technology of dimethicone, comprising the following steps：
1）By a certain proportion of methylsiloxane, octamethylcy-clotetrasiloxane, potassium hydroxide, dimethicone, hexamethyl two
Siloxanes is added to reactor, is passed through nitrogen, stirs；
2）Continue to be passed through nitrogen, and add the concentrated sulfuric acid, it is 86-90 DEG C, insulation reaction 2.8-3.2h to be warming up to reactor temperature；
3）After reaction terminates, stratification releases the reacted concentrated sulfuric acid from reactor bottom valve；
4）To adding sodium hydrate aqueous solution to stir in reactor, pH to 7.2-7.6 is adjusted；
5）Add water filtering washing, obtains the upper strata oil crude product of neutrality；
6）Water removal is stood, oily crude product is removed into low-boiling-point substance, obtain final product dimethicone.
Further, the step 1）In the weight portion of addition of each raw material be：The weight portion of methylsiloxane 35, prestox
Cyclotetrasiloxane 15-25 weight portions, potassium hydroxide 6-8 weight portions, dimethicone 7-9 weight portions, the silica of hexamethyl two
Alkane 5-7 weight portions.
Further, the step 2）Middle addition concentrated sulfuric acid quality feeds intake the 7% of quality for methylsiloxane.
Further, the step 1）In the weight portion of addition of each raw material be：The weight portion of methylsiloxane 35, prestox
The weight portion of cyclotetrasiloxane 20, the weight portion of potassium hydroxide 7, the weight portion of dimethicone 8, the weight of HMDO 6
Amount part.
Further, the concentrated sulfuric acid is the concentrated sulfuric acid that mass concentration is 95%.
Beneficial effects of the present invention:
Present invention process is simple, improves the surface property of dimethicone, possesses reaction condition gently, and low production cost is urged
Change activity high, stability is high, and the advantage of non-environmental-pollution etc. is conducive to popularization and application on a large scale.
Specific embodiment
A kind of preparation technology of the dimethicone of embodiment 1
A kind of preparation technology of dimethicone, comprises the following steps：1）By a certain proportion of methylsiloxane, prestox ring four
Siloxanes, potassium hydroxide, dimethicone, HMDO are added to reactor, are passed through nitrogen, stir；
2）Continue to be passed through nitrogen, and add the concentrated sulfuric acid, it is 86 DEG C, insulation reaction 2.8h to be warming up to reactor temperature；
3）After reaction terminates, stratification releases the reacted concentrated sulfuric acid from reactor bottom valve；
4）To adding sodium hydrate aqueous solution to stir in reactor, pH to 7.2 is adjusted；
5）Add water filtering washing, obtains the upper strata oil crude product of neutrality；
6）Water removal is stood, oily crude product is removed into low-boiling-point substance, obtain final product dimethicone.
As preferred scheme of the invention, step 1 of the invention）In the weight portion of addition of each raw material be：Methyl silica
The weight portion of alkane 35, the weight portion of octamethylcy-clotetrasiloxane 15, the weight portion of potassium hydroxide 6, the weight portion of dimethicone 7, six
The weight portion of tetramethyldisiloxane 5.
As preferred scheme of the invention, step 2 of the invention）Middle addition concentrated sulfuric acid quality feeds intake matter for methylsiloxane
The 7% of amount.
Used as preferred scheme of the invention, the concentrated sulfuric acid of the invention is the concentrated sulfuric acid that mass concentration is 95%.
A kind of preparation technology of the dimethicone of embodiment 2
A kind of preparation technology of dimethicone, comprises the following steps：1）By a certain proportion of methylsiloxane, prestox ring four
Siloxanes, potassium hydroxide, dimethicone, HMDO are added to reactor, are passed through nitrogen, stir；
2）Continue to be passed through nitrogen, and add the concentrated sulfuric acid, it is 88 DEG C, insulation reaction 3h to be warming up to reactor temperature；
3）After reaction terminates, stratification releases the reacted concentrated sulfuric acid from reactor bottom valve；
4）To adding sodium hydrate aqueous solution to stir in reactor, pH to 7.4 is adjusted；
5）Add water filtering washing, obtains the upper strata oil crude product of neutrality；
6）Water removal is stood, oily crude product is removed into low-boiling-point substance, obtain final product dimethicone.
As preferred scheme of the invention, step 2 of the invention）Middle addition concentrated sulfuric acid quality feeds intake matter for methylsiloxane
The 7% of amount.
As preferred scheme of the invention, step 1 of the invention）In the weight portion of addition of each raw material be：Methyl silica
The weight portion of alkane 35, the weight portion of octamethylcy-clotetrasiloxane 20, the weight portion of potassium hydroxide 7, the weight portion of dimethicone 8,
The weight portion of HMDO 6.
Used as preferred scheme of the invention, the concentrated sulfuric acid of the invention is the concentrated sulfuric acid that mass concentration is 95%.
A kind of preparation technology of the dimethicone of embodiment 3
A kind of preparation technology of dimethicone, comprises the following steps：1）By a certain proportion of methylsiloxane, prestox ring four
Siloxanes, potassium hydroxide, dimethicone, HMDO are added to reactor, are passed through nitrogen, stir；
2）Continue to be passed through nitrogen, and add the concentrated sulfuric acid, it is 90 DEG C, insulation reaction 3.2h to be warming up to reactor temperature；
3）After reaction terminates, stratification releases the reacted concentrated sulfuric acid from reactor bottom valve；
4）To adding sodium hydrate aqueous solution to stir in reactor, pH to 7.6 is adjusted；
5）Add water filtering washing, obtains the upper strata oil crude product of neutrality；
6）Water removal is stood, oily crude product is removed into low-boiling-point substance, obtain final product dimethicone.
As preferred scheme of the invention, step 1 of the invention）In the weight portion of addition of each raw material be：Methyl silica
The weight portion of alkane 35, the weight portion of octamethylcy-clotetrasiloxane 25, the weight portion of potassium hydroxide 8, the weight portion of dimethicone 9,
The weight portion of HMDO 7.
As preferred scheme of the invention, step 2 of the invention）Middle addition concentrated sulfuric acid quality feeds intake matter for methylsiloxane
The 7% of amount.
Used as preferred scheme of the invention, the concentrated sulfuric acid of the invention is the concentrated sulfuric acid that mass concentration is 95%.
The above, is only presently preferred embodiments of the present invention, is not the limitation for making other forms to the present invention, is appointed
What those skilled in the art changed possibly also with the technology contents of the disclosure above or be modified as equivalent variations etc.
Effect embodiment.But it is every without departing from technical solution of the present invention content, according to technical spirit of the invention to above example institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection domain of technical solution of the present invention.
Claims (5)
1. a kind of preparation technology of dimethicone, it is characterised in that:Comprise the following steps：
1）By a certain proportion of methylsiloxane, octamethylcy-clotetrasiloxane, potassium hydroxide, dimethicone, pregnancy
Base disiloxane is added to reactor, is passed through nitrogen, stirs；
2）Continue to be passed through nitrogen, and add the concentrated sulfuric acid, it is 86-90 DEG C, insulation reaction 2.8-3.2h to be warming up to reactor temperature；
3）After reaction terminates, stratification releases the reacted concentrated sulfuric acid from reactor bottom valve；
4）To adding sodium hydrate aqueous solution to stir in reactor, pH to 7.2-7.6 is adjusted；
5）Add water filtering washing, obtains the upper strata oil crude product of neutrality；
6）Water removal is stood, oily crude product is removed into low-boiling-point substance, obtain final product dimethicone.
2. a kind of preparation technology of dimethicone as claimed in claim 1, it is characterised in that：The step 1）In each raw material
The weight portion of addition be：The weight portion of methylsiloxane 35, octamethylcy-clotetrasiloxane 15-25 weight portions, potassium hydroxide 6-8
Weight portion, dimethicone 7-9 weight portions, HMDO 5-7 weight portions.
3. a kind of preparation technology of dimethicone as claimed in claim 1, it is characterised in that：Step 2）The middle addition concentrated sulfuric acid
Quality feeds intake the 7% of quality for methylsiloxane.
4. a kind of preparation technology of dimethicone as claimed in claim 2, it is characterised in that：The step 1）In each raw material
The weight portion of addition be：The weight portion of methylsiloxane 35, the weight portion of octamethylcy-clotetrasiloxane 20, the weight of potassium hydroxide 7
Part, the weight portion of dimethicone 8, the weight portion of HMDO 6.
5. a kind of preparation technology of dimethicone as claimed in claim 3, it is characterised in that：The concentrated sulfuric acid is that quality is dense
Spend the concentrated sulfuric acid for 95%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611155620.8A CN106750310A (en) | 2016-12-14 | 2016-12-14 | A kind of preparation technology of dimethicone |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611155620.8A CN106750310A (en) | 2016-12-14 | 2016-12-14 | A kind of preparation technology of dimethicone |
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| CN106750310A true CN106750310A (en) | 2017-05-31 |
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| CN201611155620.8A Withdrawn CN106750310A (en) | 2016-12-14 | 2016-12-14 | A kind of preparation technology of dimethicone |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569489A (en) * | 2018-12-05 | 2019-04-05 | 江西华昊化工有限公司 | A kind of process units and its preparation process of high boiling point silicon oil |
| CN112779786A (en) * | 2021-02-05 | 2021-05-11 | 浙江好派服饰有限公司 | Preparation method of high-elasticity anti-wrinkle silk shirt fabric |
-
2016
- 2016-12-14 CN CN201611155620.8A patent/CN106750310A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569489A (en) * | 2018-12-05 | 2019-04-05 | 江西华昊化工有限公司 | A kind of process units and its preparation process of high boiling point silicon oil |
| CN109569489B (en) * | 2018-12-05 | 2021-07-30 | 江西华昊化工有限公司 | Production device and preparation process of high-boiling silicone oil |
| CN112779786A (en) * | 2021-02-05 | 2021-05-11 | 浙江好派服饰有限公司 | Preparation method of high-elasticity anti-wrinkle silk shirt fabric |
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Application publication date: 20170531 |