CN105885051A - Hydroxyl silicone oil preparation method - Google Patents
Hydroxyl silicone oil preparation method Download PDFInfo
- Publication number
- CN105885051A CN105885051A CN201610394758.7A CN201610394758A CN105885051A CN 105885051 A CN105885051 A CN 105885051A CN 201610394758 A CN201610394758 A CN 201610394758A CN 105885051 A CN105885051 A CN 105885051A
- Authority
- CN
- China
- Prior art keywords
- parts
- preparation
- hydroxy silicon
- silicon oil
- oil
- 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.)
- Pending
Links
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
- 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
Abstract
The invention discloses a hydroxyl silicone oil preparation method. The method includes the following steps that S1, a dimethyl cyclosiloxane mixture, acetic anhydride and glacial acetic acid are mixed, stirred and heated to 100-115 DEG C, and temperature is preserved for 1.5-2.5 h and then reduced to 75-85 DEG C; S2, a soda ash aqueous solution is added, pH is adjusted to be 8.0, temperature is raised to 100 DEG C, preserved for 0.5-1.5 h and then reduced to 70-80 DEG C, the mixture stands still, water is separated, and oil is discharged. Viscosity of a hydroxyl silicone oil product prepared through the method is lower than 3 mPa.s (25 DEG C), the hydroxyl value content can reach 18-25%, and the product is high in purity and yield.
Description
Technical field
The present invention relates to hydroxy silicon oil synthesis technical field, particularly relate to the preparation method of a kind of hydroxy silicon oil.
Background technology
Hydroxy silicon oil, end group is the linear polydimethylsiloxane-of hydroxyl, oily liquids.There is the feature of methyl-silicone oil.Low viscous hydroxy silicon oil is the superior structural controlling agent in silicone rubber processing, can replace diphenyl silanediol, Simplified flowsheet, improve processing performance.Also serve as waterproof, the soft and release treatment agent of fabric, leather, paper.
At present, the synthetic method for hydroxy silicon oil has:
(1) formed by octamethylcy-clotetrasiloxane (D4) open loop degraded that adds water under acid or alkali effect；
(2) added water together at autoclave by silicone rubber, base catalysis degraded forms；
(3) by high molecular polydimethylsiloxane in high pressure with potassium hydroxide catalysed add water degraded and obtain；
(4) hydrolyzed under mild acid conditions by dimethyldialkylammonium TMOS and produce.
Typical hydroxy silicon oil viscosity≤40 mpas (25 DEG C) the most on the market, hydroxy radical content 4%～5%.
Summary of the invention
In view of this, the preparation method of the hydroxy silicon oil that the present invention proposes a kind of low viscosity, hydroxyl value content is high.
The technical scheme is that and be achieved in that: the preparation method of a kind of hydroxy silicon oil, comprise the following steps,
S1, mixes dimethicone mixture, acetic anhydride with glacial acetic acid, and stirring is warming up to 100-115 DEG C, is incubated 1.5～2.5 hours, is cooled to 75～85 DEG C；
S2, adds the aqueous solution of soda, regulates pH to 8.0, is warming up to 100 DEG C, is incubated 0.5～1.5 hour, cools to 70～80 DEG C, stands, and point water is drained the oil.
On the basis of above technical scheme, it is preferred that also include step S3, oil precipitation step S2 obtained filtered after 6 hours.It is further preferred that also bag step S3, adding activated carbon, be warmed up to 100 DEG C, evacuation removes low molecule and water, cooling, stirs and is filtrated to get final products in 4 hours.
On the basis of above technical scheme, it is preferred that in described dimethicone mixture, D3+D4+D5+D6 >=99.8%, D4 >=80%.
On the basis of above technical scheme, it is preferred that each constituent mass number is as follows,
DMC:1000～1400 parts
Acetic anhydride: 750～770 parts
Glacial acetic acid: 90～110 parts
Soda: 180～220 parts.
It is further preferred that each constituent mass number is as follows,
DMC:1200 part
Acetic anhydride: 760 parts
Glacial acetic acid: 100 parts
Soda: 200 parts.
The preparation method of the hydroxy silicon oil of the present invention has the advantages that relative to prior art
(1) product viscosity is less than 3 mpas (25 DEG C), and hydroxyl value content is up to 18%～25%；
(2) product purity is high, recovery rate is high.
Detailed description of the invention
Below in conjunction with embodiment of the present invention, the technical scheme in embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, broadly fall into the scope of protection of the invention.
Embodiment 1
The preparation method of the hydroxy silicon oil of the present embodiment, each constituent mass number is as follows:
DMC:1000 part
Acetic anhydride: 750 parts
Glacial acetic acid: 90 parts
Soda: 180 parts.
Comprise the following steps,
S1, mixes dimethicone mixture, acetic anhydride with glacial acetic acid, and stirring is warming up to 100 DEG C, is incubated 1.5 hours, is cooled to 75 DEG C；
S2, adds the aqueous solution of soda, regulates pH to 8.0, is warming up to 100 DEG C, is incubated 0.5 hour, cools to 70 DEG C, stands, and point water is drained the oil；
S3, oil precipitation step S2 obtained filtered after 6 hours；
S3, adds activated carbon, is warmed up to 100 DEG C, and evacuation removes low molecule and water, cooling, stirs and is filtrated to get final products in 4 hours.
After testing, the hydroxy silicon oil that the present embodiment prepares,
Product viscosity is 2.9 mpas (25 DEG C)；
Hydroxyl value content is up to 18%；
Product purity reaches 80%；
Recovery rate reaches 60%.
Embodiment 2
The preparation method of the hydroxy silicon oil of the present embodiment, each constituent mass number is as follows:
DMC:1200 part
Acetic anhydride: 760 parts
Glacial acetic acid: 100 parts
Soda: 200 parts.
Comprise the following steps,
S1, mixes dimethicone mixture, acetic anhydride with glacial acetic acid, and stirring is warming up to 110 DEG C, is incubated 2 hours, is cooled to 80 DEG C；
S2, adds the aqueous solution of soda, regulates pH to 8.0, is warming up to 100 DEG C, is incubated 1 hour, cools to 75 DEG C, stands, and point water is drained the oil；
S3, oil precipitation step S2 obtained filtered after 6 hours；
S3, adds activated carbon, is warmed up to 100 DEG C, and evacuation removes low molecule and water, cooling, stirs and is filtrated to get final products in 4 hours.
After testing, the hydroxy silicon oil that the present embodiment prepares,
Product viscosity 2.3 mpas (25 DEG C)；
Hydroxyl value content is up to 25%；
Product purity reaches more than 93.2%；
Recovery rate reaches 68%.
Embodiment 3
The preparation method of the hydroxy silicon oil of the present embodiment, each constituent mass number is as follows:
DMC:1400 part
Acetic anhydride: 770 parts
Glacial acetic acid: 110 parts
Soda: 220 parts.
Comprise the following steps,
S1, mixes dimethicone mixture, acetic anhydride with glacial acetic acid, and stirring is warming up to 115 DEG C, is incubated 2.5 hours, is cooled to 85 DEG C；
S2, adds the aqueous solution of soda, regulates pH to 8.0, is warming up to 100 DEG C, is incubated 1.5 hours, cools to 80 DEG C, stands, and point water is drained the oil；
S3, oil precipitation step S2 obtained filtered after 6 hours；
S3, adds activated carbon, is warmed up to 100 DEG C, and evacuation removes low molecule and water, cooling, stirs and is filtrated to get final products in 4 hours.
After testing, the hydroxy silicon oil that the present embodiment prepares,
Product viscosity 2.5 mpas (25 DEG C)；
Hydroxyl value content is up to 20%；
Product purity reaches more than 86%；
Recovery rate reaches 63%.
The foregoing is only the better embodiment of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (6)
1. the preparation method of a hydroxy silicon oil, it is characterised in that: comprise the following steps,
S1, mixes dimethicone mixture, acetic anhydride with glacial acetic acid, and stirring is warming up to
100-115 DEG C, it is incubated 1.5～2.5 hours, is cooled to 75～85 DEG C；
S2, adds the aqueous solution of soda, regulates pH to 8.0, is warming up to 100 DEG C, is incubated 0.5～1.5 hour,
Cooling to 70～80 DEG C, stand, point water is drained the oil.
2. the preparation method of hydroxy silicon oil as claimed in claim 1, it is characterised in that: also include step S3,
Oil precipitation step S2 obtained filtered after 6 hours.
3. the preparation method of hydroxy silicon oil as claimed in claim 2, it is characterised in that: also bag step S3,
Adding activated carbon, be warmed up to 100 DEG C, evacuation removes low molecule and water, cooling, stirs and filters for 4 hours
To final products.
4. the preparation method of hydroxy silicon oil as claimed in claim 1, it is characterised in that: described diformazan basic ring
In mixture of siloxanes, D3+D4+D5+D6 >=99.8%, D4 >=80%.
5. the preparation method of hydroxy silicon oil as claimed in claim 1, it is characterised in that: each constituent mass part
Number is as follows,
DMC:1000～1400 parts
Acetic anhydride: 750～770 parts
Glacial acetic acid: 90～110 parts
Soda: 180～220 parts.
6. the preparation method of hydroxy silicon oil as claimed in claim 5, it is characterised in that: each constituent mass part
Number is as follows,
DMC:1200 part
Acetic anhydride: 760 parts
Glacial acetic acid: 100 parts
Soda: 200 parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610394758.7A CN105885051A (en) | 2016-06-06 | 2016-06-06 | Hydroxyl silicone oil preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610394758.7A CN105885051A (en) | 2016-06-06 | 2016-06-06 | Hydroxyl silicone oil preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105885051A true CN105885051A (en) | 2016-08-24 |
Family
ID=56711559
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610394758.7A Pending CN105885051A (en) | 2016-06-06 | 2016-06-06 | Hydroxyl silicone oil preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105885051A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818901A (en) * | 2019-11-29 | 2020-02-21 | 湖北新海鸿化工有限公司 | Preparation method of hydroxyl silicone oil |
| CN111458453A (en) * | 2020-05-12 | 2020-07-28 | 万华化学集团股份有限公司 | Method for testing hydroxyl value in lactide-containing polylactic acid and application thereof |
| CN111690138A (en) * | 2020-07-16 | 2020-09-22 | 江西蓝星星火有机硅有限公司 | Low-viscosity vinyl hydroxyl silicone oil and preparation method thereof |
| CN112010887A (en) * | 2019-05-28 | 2020-12-01 | 赢创运营有限公司 | Method for preparing siloxane with acetoxy group |
| CN112010888A (en) * | 2019-05-28 | 2020-12-01 | 赢创运营有限公司 | Method for preparing siloxane with acetoxy group |
| CN112011054A (en) * | 2019-05-28 | 2020-12-01 | 赢创运营有限公司 | Acetoxy system |
| CN112119111A (en) * | 2018-05-17 | 2020-12-22 | 赢创运营有限公司 | Linear polydimethylsiloxane-polyoxyalkylene block copolymers of the ABA structure type |
| EP4119597A1 (en) * | 2021-07-14 | 2023-01-18 | Evonik Operations GmbH | Molecular weight structure of low-molecular alpha, omega-polysiloxane diols |
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 |
| CN102766261A (en) * | 2012-08-04 | 2012-11-07 | 山东东岳有机硅材料有限公司 | Preparation method of hydroxyl silicone oil |
-
2016
- 2016-06-06 CN CN201610394758.7A patent/CN105885051A/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 |
| CN102766261A (en) * | 2012-08-04 | 2012-11-07 | 山东东岳有机硅材料有限公司 | Preparation method of hydroxyl silicone oil |
Non-Patent Citations (2)
| Title |
|---|
| 戴传波 李建桥 王华 陶军: "羟甲基硅油的合成研究", 《吉林化工学院学报》 * |
| 杨安明 刘娜: "小分子端羟基硅油的制备及表征", 《染整技术》 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112119111A (en) * | 2018-05-17 | 2020-12-22 | 赢创运营有限公司 | Linear polydimethylsiloxane-polyoxyalkylene block copolymers of the ABA structure type |
| EP3744755A1 (en) * | 2019-05-28 | 2020-12-02 | Evonik Operations GmbH | Method for producing siloxanes bearing acetoxy groups |
| US11286351B2 (en) | 2019-05-28 | 2022-03-29 | Evonik Operations Gmbh | Process for producing acetoxy-bearing siloxanes |
| CN112010887A (en) * | 2019-05-28 | 2020-12-01 | 赢创运营有限公司 | Method for preparing siloxane with acetoxy group |
| CN112010888A (en) * | 2019-05-28 | 2020-12-01 | 赢创运营有限公司 | Method for preparing siloxane with acetoxy group |
| CN112011054A (en) * | 2019-05-28 | 2020-12-01 | 赢创运营有限公司 | Acetoxy system |
| CN112011054B (en) * | 2019-05-28 | 2023-09-29 | 赢创运营有限公司 | Acetoxygen systems |
| EP3744754A1 (en) * | 2019-05-28 | 2020-12-02 | Evonik Operations GmbH | Method for producing siloxanes bearing acetoxy groups |
| US11066429B2 (en) | 2019-05-28 | 2021-07-20 | Evonik Operations Gmbh | Process for producing acetoxy-bearing siloxanes |
| CN110818901B (en) * | 2019-11-29 | 2021-11-30 | 湖北新海鸿化工有限公司 | Preparation method of hydroxyl silicone oil |
| CN110818901A (en) * | 2019-11-29 | 2020-02-21 | 湖北新海鸿化工有限公司 | Preparation method of hydroxyl silicone oil |
| CN111458453A (en) * | 2020-05-12 | 2020-07-28 | 万华化学集团股份有限公司 | Method for testing hydroxyl value in lactide-containing polylactic acid and application thereof |
| CN111458453B (en) * | 2020-05-12 | 2022-07-12 | 万华化学(四川)有限公司 | Method for testing hydroxyl value in lactide-containing polylactic acid and application thereof |
| CN111690138A (en) * | 2020-07-16 | 2020-09-22 | 江西蓝星星火有机硅有限公司 | Low-viscosity vinyl hydroxyl silicone oil and preparation method thereof |
| EP4119597A1 (en) * | 2021-07-14 | 2023-01-18 | Evonik Operations GmbH | Molecular weight structure of low-molecular alpha, omega-polysiloxane diols |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105885051A (en) | Hydroxyl silicone oil preparation method | |
| CN109011726A (en) | Acidproof resistance to high temperature resistant type defoaming agent with high salt of one kind and preparation method thereof | |
| CN1657687A (en) | Hydrophilic ammonia hydrocarbon base polystoxane softening agent and its preparation method | |
| CN106279668B (en) | A kind of acetyl blocked polyethers and preparation method thereof | |
| CN105147568A (en) | Active grape wine lees mask and production method thereof | |
| CN106279620A (en) | A kind of modified aqueous polyurethane resin for woodcare paint and preparation method thereof | |
| CN106902008A (en) | A kind of facial mask and its production technology with refrigerant sense | |
| RU2012122207A (en) | METHOD FOR PRODUCING UTERINE MIXTURE OF DIENE ELASTOMER AND SILICON OXIDE | |
| CN110818901B (en) | Preparation method of hydroxyl silicone oil | |
| CN102987484A (en) | Chinese wolfberry fruit vinegar beverage | |
| CN108424530A (en) | A kind of preparation method of Cortex Eucommiae latex | |
| JP4571575B2 (en) | Proanthocyanidin-containing tea beverage and method for producing the same | |
| EP0346375A1 (en) | Plant gum material and use thereof in food products. | |
| CN103333497A (en) | Two-component RTV (Room Temperature Vulcanization) mould gel and preparation method thereof | |
| CN103214674B (en) | Method for efficiently producing an organic silicone resin microsphere | |
| CA2560432A1 (en) | Pseudo-thermosetting neutralized chitosan composition forming a hydrogel and a process for producing the same | |
| CN113368543A (en) | Organic silicon polyether emulsion type defoaming agent and preparation method and application thereof | |
| CN108623858B (en) | Acid coagulation preparation method of medical gloves | |
| CN102805156A (en) | Brain-enriching medlar soya-bean milk | |
| CN113957721B (en) | Anti-wrinkle elastic silicone oil and preparation method thereof | |
| CN108586749A (en) | A kind of additional organosilicon resin and preparation method thereof | |
| CN106380596A (en) | Heat-resisting and damping polyether type polyurethane sponge | |
| CN106946717B (en) | Benzalkonium chloride monomer synthesis technology | |
| CN105801863A (en) | Preparation method of hydroxyl-terminated poly(diethyldimethyl)siloxane | |
| CN102659953B (en) | A kind of molecular weight is the preparation method of the hydroxyethylamyle of 5,500,000 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160824 |