CN106750310A - A kind of preparation technology of dimethicone - Google Patents
A kind of preparation technology of dimethicone Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- dimethicone
- weight portion
- sulfuric acid
- concentrated sulfuric
- reactor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 229940008099 dimethicone Drugs 0.000 title claims abstract description 45
- 239000004205 dimethyl polysiloxane Substances 0.000 title claims abstract description 45
- 235000013870 dimethyl polysiloxane Nutrition 0.000 title claims abstract description 45
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 39
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 27
- -1 methylsiloxane Chemical class 0.000 claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 9
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000012467 final product Substances 0.000 claims abstract description 6
- 238000009413 insulation Methods 0.000 claims abstract description 6
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 6
- 238000013517 stratification Methods 0.000 claims abstract description 6
- 238000010792 warming Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 7
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims 1
- 230000035935 pregnancy Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- DDJSWKLBKSLAAZ-UHFFFAOYSA-N cyclotetrasiloxane Chemical compound O1[SiH2]O[SiH2]O[SiH2]O[SiH2]1 DDJSWKLBKSLAAZ-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000003254 anti-foaming effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
Landscapes
- 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 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 |
Applications Claiming Priority (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 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106750310A true CN106750310A (en) | 2017-05-31 |
Family
ID=58888812
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611155620.8A Withdrawn CN106750310A (en) | 2016-12-14 | 2016-12-14 | A kind of preparation technology of dimethicone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106750310A (en) |
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 | A kind of production device of high boiling silicone oil and preparation process thereof |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105688452B (en) | A kind of emulsion-type organic silicon defoamer and preparation method thereof | |
| CN103613765B (en) | A kind of preparation method of dimethicone with controllable viscosity | |
| CN103665380A (en) | Preparation method for low hydrogen-containing silicon oil | |
| CN108623832B (en) | Polysilsesquioxane aerogel and preparation method thereof | |
| CN102643431A (en) | Method for preparing low viscosity dimethyl silicone oil | |
| CN105418933A (en) | Preparation method of long-chain alkyl polyether co-modified silicone oil | |
| CN102408723A (en) | Silicone rubber, silicone rubber manufacturing method and feeding bottle manufactured by silicone rubber | |
| CN106750310A (en) | A kind of preparation technology of dimethicone | |
| CN100396715C (en) | Branched benzene siliconic oil | |
| CN104109244A (en) | Long-chain fluorine-containing alkyl silicone oil and synthetic method thereof | |
| CN106928267B (en) | The preparation method of quaternary ammonium salt type trisiloxane gemini surfactant | |
| CN107537185A (en) | A kind of self-emulsifying type defoamer and preparation method thereof | |
| CN106750309A (en) | A kind of technique for preparing dimethyl-silicon oil formulation | |
| CN104031392B (en) | A kind of add-on type silica gel and its production and use | |
| CN103804834B (en) | A kind of silicon composition and preparation method thereof | |
| CN102604101B (en) | Synthesis method for phenyl organosilicon copolymer with uniformly distributed phenyl units | |
| CN104927056B (en) | A kind of preparation method of double-component catalyst system synthesis of vinyl fluorosilicon oil | |
| CN102516971A (en) | Block polyether zwitterionic heavy oil emulsified viscosity reducer and preparation method thereof | |
| CN117535061A (en) | Polyether amine nonionic surfactant and preparation process thereof | |
| CN111139138A (en) | Synthetic method of modified grease ethoxylate | |
| CN104071857B (en) | A kind of preparation method of oil field low temperature viscous crude oily water treatment water cleaning agent | |
| US9175138B2 (en) | Method for producing organopolysiloxanes | |
| CN103408587A (en) | Preparation method of silica-based phosphate ester | |
| CN106564905A (en) | Method for large-scale preparation of low-cost silicon dioxide composite aerogel | |
| CN106117277A (en) | A kind of method that alkyl polyglucoside is prepared in ionic liquid compound system concerted catalysis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170531 |