CN106366318A - Production method of hydroxyl silicone oil - Google Patents
Production method of hydroxyl silicone oil Download PDFInfo
- Publication number
- CN106366318A CN106366318A CN201610737252.1A CN201610737252A CN106366318A CN 106366318 A CN106366318 A CN 106366318A CN 201610737252 A CN201610737252 A CN 201610737252A CN 106366318 A CN106366318 A CN 106366318A
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- CN
- China
- Prior art keywords
- production method
- silicon oil
- hydroxy silicon
- catalyst
- monomer
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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
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/16—Polysiloxanes containing silicon bound to oxygen-containing groups to hydroxyl groups
-
- 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
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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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 invention relates to a production method of hydroxyl silicone oil. The production method comprises the following steps that 1, in a reaction kettle, superacid is taken as a catalyst, an end capping agent is added into a monomer, and a polymerization reaction is conducted while stirring is conducted, wherein the monomer is dimethyl siloxane, and the end capping agent is deionized water; 2, after polymerization is finished, water washing is conducted, the catalyst is recycled, the obtained clear liquid is subjected to negative pressure dewatering at the temperature of 120 DEEG C to 140 DEG C, slow refluxing is kept, dewatering is conducted for 1-3 h, then the temperature is gradually increased to 140 DEG C to 205 DEG C, and low-boiling point substances are removed; 3, filtration is conducted, the obtained product is cooled to room temperature, and then the hydroxyl silicone oil is obtained. The whole preparation technology is simple, and the production cost is low.
Description
Technical field
The present invention relates to a kind of production method of hydroxy silicon oil, belong to the technical field of organosilicon macromolecule compound.
Background technology
In domestic prior art, the method for production hydroxy silicon oil, adopt acetic anhydride method more, with dimethicone be
Raw material, acetic anhydride are end-capping reagent, do catalyst, the silicone oil of synthesis of acetyl epoxide end-blocking using sulphuric acid, then acetoxyl group is blocked
Silicone oil hydrolyze in alkaline aqueous solution be obtained hydroxy silicon oil.Using the dmc after hydrolysate cracking as raw material, increased raw material
Cost；Single employing sulphuric acid, the conversion ratio of acetic anhydride is low, leads to produce the hydroxy silicon oil of same hydroxy radical content, required second
Anhydride cost increases；Above-mentioned preparation method is complicated, leads to production cost higher.
It is therefore desirable to designing a kind of production method of hydroxy silicon oil, to overcome the problems referred to above.
Content of the invention
It is an object of the invention to overcoming the defect of prior art, there is provided a kind of preparation process is simple, production cost are relatively
The production method of low hydroxy silicon oil.
The present invention is achieved in that
The present invention provides a kind of production method of hydroxy silicon oil, comprises the following steps: step one: in a kettle., with super acids
For catalyst, add end-capping reagent in monomer, while stirring, carry out polyreaction, wherein, described monomer is dimethyl silica
Alkane, described end-capping reagent is deionized water；Step 2: after polymerization finishes, washed, and reclaim catalyst, gained clear liquid is existed
120 ~ 140 DEG C of negative pressure dehydrations, keep slow and flow back, be dehydrated 1 ~ 3h, then gradually rise temperature to 140 ~ 205 DEG C, remove low boiling
Thing；Step 3, is filtered, and is cooled to room temperature, that is, obtain hydroxy silicon oil.
Further, in step one, the temperature of polyreaction is 40 ~ 100 DEG C, and polymerization reaction time is 5 ~ 720min.
Further, the consumption of described catalyst is the 10-12% of monomer gross mass.
Further, using sulphuric acid or phosphoric acid as catalyst.
The method have the advantages that
In a kettle., with super acids as catalyst, add end-capping reagent in monomer, while stirring, carry out polyreaction, gather
After conjunction finishes, washed, and reclaimed catalyst, gained clear liquid is dehydrated in 120 ~ 140 DEG C of negative pressure, keep slow and flow back, take off
Water 1 ~ 3h, then gradually rises temperature to 140 ~ 205 DEG C, removes low-boiling-point substance；Then filtered, be cooled to room temperature, that is, obtain
Hydroxy silicon oil.The production method of the hydroxy silicon oil that the present invention provides, the hydroxy silicon oil molecular weight of product of production can pass through end-capping reagent
Consumption, polymeric reaction temperature and time, to regulate and control well, can obtain from low-molecular-weight hydroxyl silicone oil to high molecular viscosity hydroxyl
A series of products of base silicone oil.Whole preparation process is simple, production cost is relatively low.
Specific embodiment
The enforcement it is clear that described will be clearly and completely described to the technical scheme in the embodiment of the present invention below
Example is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
All other embodiment that technical staff is obtained on the premise of not making creative work, broadly falls into present invention protection
Scope.
The embodiment of the present invention provides a kind of production method of hydroxy silicon oil, comprises the following steps:
Step one: in a kettle., with super acids as catalyst, add end-capping reagent in monomer, be polymerized while stirring
Reaction, wherein, described monomer is dimethyl siloxane, and described end-capping reagent is deionized water.
Step 2: after polymerization finishes, washed, and reclaim catalyst, gained clear liquid is taken off in 120 ~ 140 DEG C of negative pressure
Water, keeps slow and flows back, be dehydrated 1 ~ 3h, then gradually rise temperature to 140 ~ 205 DEG C, remove low-boiling-point substance.In dehydration,
Gasification dimethicone and water, condensed after, enter phase separator；Split-phase in phase separator, upper strata is organic faciess-two
Methyl cyclosiloxane, lower floor is water, the dimethicone on upper strata, all passes back into dehydrating kettle, continues to participate in dehydration.
Step 3, is filtered, and is cooled to room temperature, that is, obtain hydroxy silicon oil.
Further, in step one, the temperature of polyreaction is 40 ~ 100 DEG C, and polymerization reaction time is 5 ~ 720min.
Further, the consumption of described catalyst is the 10-12% of monomer gross mass.
Further, using sulphuric acid or phosphoric acid as catalyst.
The method have the advantages that
In a kettle., with super acids as catalyst, add end-capping reagent in monomer, while stirring, carry out polyreaction, gather
After conjunction finishes, washed, and reclaimed catalyst, gained clear liquid is dehydrated in 120 ~ 140 DEG C of negative pressure, keep slow and flow back, take off
Water 1 ~ 3h, then gradually rises temperature to 140 ~ 205 DEG C, removes low-boiling-point substance；Then filtered, be cooled to room temperature, that is, obtain
Hydroxy silicon oil.The production method of the hydroxy silicon oil that the present invention provides, the hydroxy silicon oil molecular weight of product of production can pass through end-capping reagent
Consumption, polymeric reaction temperature and time, to regulate and control well, can obtain from low-molecular-weight hydroxyl silicone oil to high molecular viscosity hydroxyl
A series of products of base silicone oil.Whole preparation process is simple, production cost is relatively low.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement made etc., should be included within the scope of the present invention.
Claims (4)
1. a kind of production method of hydroxy silicon oil is it is characterised in that comprise the following steps:
Step one: in a kettle., with super acids as catalyst, add end-capping reagent in monomer, be polymerized while stirring
Reaction, wherein, described monomer is dimethyl siloxane, and described end-capping reagent is deionized water；
Step 2: after polymerization finishes, washed, and reclaim catalyst, gained clear liquid is dehydrated in 120 ~ 140 DEG C of negative pressure, protect
Hold slow backflow, be dehydrated 1 ~ 3h, then gradually rise temperature to 140 ~ 205 DEG C, remove low-boiling-point substance；
Step 3, is filtered, and is cooled to room temperature, that is, obtain hydroxy silicon oil.
2. hydroxy silicon oil as claimed in claim 1 production method it is characterised in that: in step one, the temperature of polyreaction
For 40 ~ 100 DEG C, polymerization reaction time is 5 ~ 720min.
3. hydroxy silicon oil as claimed in claim 1 or 2 production method it is characterised in that: the consumption of described catalyst is
The 10-12% of monomer gross mass.
4. hydroxy silicon oil as claimed in claim 1 or 2 production method it is characterised in that: using sulphuric acid or phosphoric acid as urging
Agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610737252.1A CN106366318A (en) | 2016-08-29 | 2016-08-29 | Production method of hydroxyl silicone oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610737252.1A CN106366318A (en) | 2016-08-29 | 2016-08-29 | Production method of hydroxyl silicone oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106366318A true CN106366318A (en) | 2017-02-01 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610737252.1A Pending CN106366318A (en) | 2016-08-29 | 2016-08-29 | Production method of hydroxyl silicone oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106366318A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110606953A (en) * | 2019-09-26 | 2019-12-24 | 唐山三友硅业有限责任公司 | Low-viscosity hydroxyl-terminated vinyl methyl silicone oil and continuous preparation method thereof |
| CN111116919A (en) * | 2019-12-31 | 2020-05-08 | 枣阳市金鹏化工有限公司 | Novel dimethyl-terminated hydroxyl silicone oil and preparation method thereof |
| CN111333842A (en) * | 2020-04-29 | 2020-06-26 | 苏州歌诗夫新材料有限公司 | Synthesis method of hydroxyl silicone oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781401A (en) * | 2009-01-20 | 2010-07-21 | 扬州宏远化工新材料有限公司 | Novel method for producing hydroxy silicone oil |
| CN102408567A (en) * | 2011-11-11 | 2012-04-11 | 杭州师范大学 | Preparation method for hydroxyl silicone oil |
-
2016
- 2016-08-29 CN CN201610737252.1A patent/CN106366318A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781401A (en) * | 2009-01-20 | 2010-07-21 | 扬州宏远化工新材料有限公司 | Novel method for producing hydroxy silicone oil |
| CN102408567A (en) * | 2011-11-11 | 2012-04-11 | 杭州师范大学 | Preparation method for hydroxyl silicone oil |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110606953A (en) * | 2019-09-26 | 2019-12-24 | 唐山三友硅业有限责任公司 | Low-viscosity hydroxyl-terminated vinyl methyl silicone oil and continuous preparation method thereof |
| CN111116919A (en) * | 2019-12-31 | 2020-05-08 | 枣阳市金鹏化工有限公司 | Novel dimethyl-terminated hydroxyl silicone oil and preparation method thereof |
| CN111333842A (en) * | 2020-04-29 | 2020-06-26 | 苏州歌诗夫新材料有限公司 | Synthesis method of hydroxyl silicone oil |
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Application publication date: 20170201 |
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