CN112480391A - Silicon-containing polyether polyol and preparation method thereof - Google Patents
Silicon-containing polyether polyol and preparation method thereof Download PDFInfo
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- CN112480391A CN112480391A CN202011347392.0A CN202011347392A CN112480391A CN 112480391 A CN112480391 A CN 112480391A CN 202011347392 A CN202011347392 A CN 202011347392A CN 112480391 A CN112480391 A CN 112480391A
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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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/336—Polymers modified by chemical after-treatment with organic compounds containing silicon
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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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/321—Polymers modified by chemical after-treatment with inorganic compounds
- C08G65/328—Polymers modified by chemical after-treatment with inorganic compounds containing other elements
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Abstract
The invention belongs to the technical field of chemical synthesis, and particularly relates to silicon-containing polyether polyol and a preparation method thereof. DX-505S is used as an initiator, reacts with sodium hydroxide to generate sodium alkoxide, and then reacts with a dimethyldichlorosilane monomer to prepare the silicon-containing polyether polyol, so that the silicon-containing polyether polyol has excellent thermal oxidation stability, viscosity-temperature performance, flexibility, proper freezing point and smaller surface tension, and can be applied to additives of cosmetics and daily chemicals and the like. The preparation method is scientific, reasonable, simple and feasible.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to silicon-containing polyether polyol and a preparation method thereof.
Background
In the market, the common silicone oil is mainly used as high-grade lubricating oil, shockproof oil, insulating oil, defoaming agent, release agent, polishing agent, vacuum diffusion pump oil and the like. Among various silicone oils, methyl silicone oil is most widely used, and is the most important variety of silicone oils, and methyl phenyl silicone oil is the second choice. Further, ethyl silicone oil, methylphenyl silicone oil, nitrile-containing silicone oil and the like are also available. However, the silicone oil has the defects of small surface tension, high gas solubility, high thermal expansion coefficient, poor lubricating property and the like.
Disclosure of Invention
Aiming at the defects of the performance of the existing silicone oil, the invention aims to provide the silicon-containing polyether polyol and the preparation method thereof, and the prepared silicon-containing polyether polyol has excellent thermal oxidation stability, viscosity-temperature performance, flexibility, proper freezing point and smaller surface tension, and can be applied to additives of cosmetics and daily chemicals and the like.
The silicon-containing polyether polyol is prepared from the following raw materials in parts by weight:
500 portions of initiator DX-505S 100-;
4.5-21.5 parts of sodium hydroxide;
8.7-43.2 parts of dimethyldichlorosilane.
The starter DX-505S is a product of Zibode Xin Federal chemical industries, Ltd. The structure is as follows: adopts glycerin as an initiator and KOH as a catalyst, EO is polymerized to the molecular weight of about 1500-. The modified product is mainly used as cosmetic and daily chemical product additives and the like after being modified by the dimethyldichlorosilane.
Furthermore, the feed is prepared from the following raw materials in parts by mass:
350 parts of initiator DX-505S;
15 parts of sodium hydroxide;
30.2 parts of dimethyldichlorosilane.
The preparation method of the silicon-containing polyether polyol comprises the following steps:
(1) putting an initiator DX-505S and sodium hydroxide into a reaction kettle, replacing with nitrogen, heating to 60-80 ℃, carrying out polymerization reaction, and degassing for 4-6h until no bubbles are generated;
(2) keeping the temperature at 70-80 ℃, dripping dimethyl dichlorosilane, curing, removing monomers in vacuum, washing with water, neutralizing, adsorbing, drying and filtering to obtain the silicon-containing polyether polyol.
The catalyst in the above step can be one or more of sodium hydroxide, potassium hydroxide, sodium methoxide, sodium hydride, etc.;
further, the polymerization time in the step (1) is 1 to 4 hours.
Furthermore, the curing in the step (2) is carried out for 7 hours at the curing temperature of 60 ℃, and the monomers are removed in vacuum for 2 hours after the curing is finished.
Further, the water washing in the step (2) is carried out at 90 ℃, pure water is added, and the stirring is carried out for 0.5 h.
Further, the neutralization in the step (2) is to add inorganic acid and stir for 1 h.
Further, after the pH value of the adsorption in the step (2) is qualified, adding a silicate adsorbent.
Further, the drying in the step (2) is performed by vacuum drum nitrogen for 6 hours at 120 ℃ until the moisture is less than or equal to 0.03.
Further, the filtration in the step (2) is vacuum filtration under reduced pressure.
Compared with the prior art, the invention has the following beneficial effects:
(1) DX-505S is used as an initiator, reacts with sodium hydroxide to generate sodium alkoxide, and then reacts with a dimethyldichlorosilane monomer to prepare the silicon-containing polyether polyol, so that the silicon-containing polyether polyol has excellent thermal oxidation stability, viscosity-temperature performance, flexibility, proper freezing point and smaller surface tension, and can be applied to additives of cosmetics and daily chemicals and the like.
(2) The preparation method is scientific, reasonable, simple and feasible.
Detailed Description
The present invention will be further described with reference to the following examples.
All the starting materials used in the examples are commercially available, except where otherwise indicated.
Example 1:
the silicon-containing polyether polyol is prepared from the following raw materials in parts by weight:
350 parts of initiator DX-505S;
15 parts of sodium hydroxide;
30.2 parts of dimethyldichlorosilane.
The preparation method comprises the following steps:
(1) putting an initiator DX-505S and sodium hydroxide into a reaction kettle, replacing with nitrogen, heating to 70 ℃, carrying out polymerization reaction for 2 hours, and degassing for 5 hours until no bubbles are generated;
(2) keeping the temperature at 70 ℃, dropwise adding dimethyldichlorosilane, curing for 7 hours at 60 ℃, removing the monomers in vacuum for 2 hours after curing, heating to 90 ℃, adding pure water, stirring for 0.5 hour for washing, adding inorganic acid after washing, stirring for 1 hour for neutralization, adding a silicate adsorbent for adsorption after the pH is qualified, then blowing nitrogen in vacuum at 120 ℃ for 6 hours until the water content is less than or equal to 0.03, and finally carrying out vacuum reduced pressure filtration to obtain the silicon-containing polyether polyol.
Example 2:
the silicon-containing polyether polyol is prepared from the following raw materials in parts by weight:
100 parts of initiator DX-505S;
4.5 parts of sodium hydroxide;
8.7 parts of dimethyldichlorosilane.
The preparation method comprises the following steps:
(1) putting an initiator DX-505S and sodium hydroxide into a reaction kettle, replacing with nitrogen, heating to 60 ℃, carrying out polymerization reaction for 4 hours, and degassing for 6 hours until no bubbles are generated;
(2) keeping the temperature at 80 ℃, dropwise adding dimethyldichlorosilane, curing for 7 hours at 60 ℃, removing monomers in vacuum for 2 hours after curing, heating to 90 ℃, adding pure water, stirring for 0.5 hour for washing, adding inorganic acid after washing, stirring for 1 hour for neutralization, adding a silicate adsorbent for adsorption after the pH is qualified, then blowing nitrogen in vacuum at 120 ℃ for 6 hours until the water content is less than or equal to 0.03, and finally carrying out vacuum reduced pressure filtration to obtain the silicon-containing polyether polyol.
Example 3:
the silicon-containing polyether polyol is prepared from the following raw materials in parts by weight:
500 parts of initiator DX-505S;
10.7 parts of sodium hydroxide;
43 parts of dimethyldichlorosilane.
The preparation method comprises the following steps:
(1) putting an initiator DX-505S and sodium hydroxide into a reaction kettle, replacing with nitrogen, heating to 80 ℃, carrying out polymerization reaction for 1.5 hours, and degassing for 4 hours until no bubbles are generated;
(2) keeping the temperature at 70 ℃, dropwise adding dimethyldichlorosilane, curing for 7 hours at 60 ℃, removing the monomers in vacuum for 2 hours after curing, heating to 90 ℃, adding pure water, stirring for 0.5 hour for washing, adding inorganic acid after washing, stirring for 1 hour for neutralization, adding a silicate adsorbent for adsorption after the pH is qualified, then blowing nitrogen in vacuum at 120 ℃ for 6 hours until the water content is less than or equal to 0.03, and finally carrying out vacuum reduced pressure filtration to obtain the silicon-containing polyether polyol.
Test example:
and (3) performance testing:
by comparing conventional silicone oils, the patent provides silicon-containing polyethers with comparable performance to conventional silicone oils, as shown in the table:
Claims (10)
1. a silicon-containing polyether polyol characterized by: the feed is prepared from the following raw materials in parts by mass:
500 portions of initiator DX-505S 100-;
4.5-21.5 parts of sodium hydroxide;
8.7-43.2 parts of dimethyldichlorosilane.
2. The silicon-containing polyether polyol according to claim 1, wherein: the feed is prepared from the following raw materials in parts by mass:
350 parts of initiator DX-505S;
15 parts of sodium hydroxide;
30.2 parts of dimethyldichlorosilane.
3. A preparation method of silicon-containing polyether polyol is characterized by comprising the following steps:
(1) putting an initiator DX-505S and sodium hydroxide into a reaction kettle, replacing with nitrogen, heating to 60-80 ℃, carrying out polymerization reaction, and degassing for 4-6h until no bubbles are generated;
(2) keeping the temperature at 70-80 ℃, dripping dimethyl dichlorosilane, curing, removing monomers in vacuum, washing with water, neutralizing, adsorbing, drying and filtering to obtain the silicon-containing polyether polyol.
4. The process according to claim 3 for preparing a silicon-containing polyether polyol, wherein: the polymerization reaction time in the step (1) is 1 to 4 hours.
5. The process according to claim 3 for preparing a silicon-containing polyether polyol, wherein: curing in the step (2) is carried out for 7 hours at the curing temperature of 60 ℃, and monomers are removed in vacuum for 2 hours after curing.
6. The process according to claim 3 for preparing a silicon-containing polyether polyol, wherein: and (3) washing with water in the step (2), adding pure water at 90 ℃, and stirring for 0.5 h.
7. The process according to claim 3 for preparing a silicon-containing polyether polyol, wherein: and (3) the neutralization in the step (2) is to add inorganic acid and stir for 1 h.
8. The process according to claim 3 for preparing a silicon-containing polyether polyol, wherein: and (3) adding a silicate adsorbent after the adsorption in the step (2) is that the PH is qualified.
9. The process according to claim 3 for preparing a silicon-containing polyether polyol, wherein: and (3) drying in the step (2) by vacuum blowing nitrogen for 6 hours at 120 ℃ until the water content is less than or equal to 0.03.
10. The process according to claim 3 for preparing a silicon-containing polyether polyol, wherein: the filtration in the step (2) is vacuum reduced pressure filtration.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343358A (en) * | 2008-08-20 | 2009-01-14 | 南京德美世创化工有限公司 | End capping polyether prepared with end hydroxyl radical polyether and preparation thereof |
| CN101884852A (en) * | 2010-06-30 | 2010-11-17 | 南京四新科技应用研究所有限公司 | Method for improving properties of polyether defoaming agent |
| CN102604070A (en) * | 2012-03-02 | 2012-07-25 | 衢州学院 | Synthesis method for polyether polyol flame retardant |
| CN108047452A (en) * | 2017-12-20 | 2018-05-18 | 山东东岳有机硅材料股份有限公司 | A kind of levelling agent super high molecular weight Siloxane-Oxyalkylene Copolymers and preparation method and application |
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- 2020-11-26 CN CN202011347392.0A patent/CN112480391B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343358A (en) * | 2008-08-20 | 2009-01-14 | 南京德美世创化工有限公司 | End capping polyether prepared with end hydroxyl radical polyether and preparation thereof |
| CN101884852A (en) * | 2010-06-30 | 2010-11-17 | 南京四新科技应用研究所有限公司 | Method for improving properties of polyether defoaming agent |
| CN102604070A (en) * | 2012-03-02 | 2012-07-25 | 衢州学院 | Synthesis method for polyether polyol flame retardant |
| CN108047452A (en) * | 2017-12-20 | 2018-05-18 | 山东东岳有机硅材料股份有限公司 | A kind of levelling agent super high molecular weight Siloxane-Oxyalkylene Copolymers and preparation method and application |
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