CN111040188A - Organic silicon emulsifier and preparation method thereof - Google Patents
Organic silicon emulsifier and preparation method thereof Download PDFInfo
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- CN111040188A CN111040188A CN201911205305.5A CN201911205305A CN111040188A CN 111040188 A CN111040188 A CN 111040188A CN 201911205305 A CN201911205305 A CN 201911205305A CN 111040188 A CN111040188 A CN 111040188A
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- emulsifier
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- organic silicon
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- 239000003995 emulsifying agent Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 15
- 229910052710 silicon Inorganic materials 0.000 title claims description 15
- 239000010703 silicon Substances 0.000 title claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 40
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 40
- 239000001257 hydrogen Substances 0.000 claims abstract description 40
- 229920002545 silicone oil Polymers 0.000 claims abstract description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 12
- -1 polyoxypropylene Polymers 0.000 claims abstract description 11
- 229920001451 polypropylene glycol Polymers 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 description 15
- 238000004945 emulsification Methods 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 4
- 239000012467 final product Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
Abstract
The invention discloses an organosilicon emulsifier and a preparation method thereof, the organosilicon emulsifier comprises a component A and/or a component B, wherein the component A comprises the following raw materials in parts by weight: 0.1-0.2% of low-hydrogen silicone oil with hydrogen content of 40-70%, 60-30% of allyl alcohol polyoxyethylene ether and 0.3% of isopropanol solution of chloroplatinic acid; the component B comprises the following raw materials in percentage by weight: 0.1-0.2% of low-hydrogen silicone oil with hydrogen content of 40-70%, 30-70% of allyl alcohol polyoxypropylene ether and 0.3% of isopropanol solution of chloroplatinic acid.
Description
Technical Field
The invention relates to the field of organic silicon emulsifiers, in particular to a high-efficiency composite organic silicon emulsifier and a preparation method thereof.
Background
An emulsifier is added to emulsify silicone oil in the process of producing the methyl silicone oil emulsion, common emulsifiers comprise span, tween, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether and the like, when the molecular weight of the methyl silicone oil is 800-50000, the emulsifier can be used for emulsifying a good effect, and when the molecular weight is more than 50000, phenomena such as oil floating and the like easily occur during emulsification.
Disclosure of Invention
The invention aims to provide an organosilicon emulsifier and a preparation method thereof, and the composite emulsifier can increase the affinity with methyl silicone oil, so as to achieve the purpose of emulsification and stability.
An organosilicon emulsifier comprises a component A and/or a component B, wherein the component A comprises the following raw materials in parts by weight: 0.1-0.2% of low-hydrogen silicone oil with hydrogen content of 40-70%, 60-30% of allyl alcohol polyoxyethylene ether and 0.3% of isopropanol solution of chloroplatinic acid; the component B comprises the following raw materials in percentage by weight: 0.1-0.2% of low-hydrogen silicone oil with low hydrogen content, 40-70% of allyl alcohol polyoxypropylene ether and 0.3% of isopropanol solution of chloroplatinic acid.
Preferably, the emulsifier is a composite organic silicon emulsifier which comprises a component A and a component B.
Preferably, the compound type organic silicon emulsifier is obtained by mixing the component A and the component B, wherein the component A and the component B are mixed according to the weight ratio of 1: 1 and mixing.
In the invention, the preparation method of the organic silicon emulsifier is also provided, and comprises the following steps: preparation of component A and/or component B.
Preferably, wherein component a comprises the following steps:
step (1), pumping 4 to 7 parts of low hydrogen silicone oil with hydrogen content of 0.1 to 0.2 percent and 3 to 6 parts of allyl alcohol polyoxyethylene ether into a reaction kettle in vacuum;
step (2), opening and stirring, heating to 100-120 ℃, and removing trace moisture in the raw materials with negative pressure for half an hour;
adding 0.3 per mill of isopropanol solution of chloroplatinic acid into the reaction kettle, and preserving the heat for 4 hours at the temperature of 120-140 ℃, wherein the materials in the kettle are changed into transparent and uniform liquid from turbid; cooling to below 50 deg.c to obtain the product.
Preferably, wherein component B comprises the following steps:
step (1): pumping 4 to 7 parts of 0.1 to 0.2 percent hydrogen-containing low-hydrogen silicone oil and 3 to 6 parts of allyl alcohol polyoxypropylene ether into a reaction kettle by vacuum;
step (2): opening the stirrer, heating to 100-120 ℃, and removing trace moisture in the raw materials with negative pressure for half an hour;
and (3): adding 0.3 per mill isopropanol solution of chloroplatinic acid into the reaction kettle, preserving the heat for 4 hours at 120-140 ℃, changing the material in the kettle from turbid into transparent and uniform liquid, and cooling to below 50 ℃ to obtain the finished product.
Preferably, the finished product of the component A and the finished product of the component B are mixed according to the proportion of 1: 1, and then the mixture is mixed evenly to obtain the compound organic silicon emulsifier.
Compared with the prior art, the invention has the following beneficial effects:
1. the composite emulsifier prepared by the invention can increase the affinity with methyl silicone oil, and achieves the purpose of emulsification and stability; and no by-product is generated in the preparation process; and in the organosilicon emulsification process, the reaction condition is lower, and the phenomenon of layering can not occur after long-time standing after emulsification.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Embodiment 1, an organosilicon emulsifier, comprising a component a and/or a component B, wherein the component a comprises the following raw materials in parts by weight: 0.1-0.2% of low-hydrogen silicone oil with hydrogen content of 40-70%, 60-30% of allyl alcohol polyoxyethylene ether and 0.3% of isopropanol solution of chloroplatinic acid; the component B comprises the following raw materials in percentage by weight: 0.1-0.2% of low-hydrogen silicone oil with low hydrogen content, 40-70% of allyl alcohol polyoxypropylene ether and 0.3% of isopropanol solution of chloroplatinic acid.
Embodiment 2, an organosilicon emulsifier, comprising a component a and a component B, wherein the component a comprises the following raw materials in parts by weight: 0.1-0.2% of low-hydrogen silicone oil with hydrogen content of 40-70%, 60-30% of allyl alcohol polyoxyethylene ether and 0.3% of isopropanol solution of chloroplatinic acid; the component B comprises the following raw materials in percentage by weight: 0.1-0.2% of low-hydrogen silicone oil with hydrogen content of 40-70%, 30-70% of allyl alcohol polyoxypropylene ether and 0.3% of isopropanol solution of chloroplatinic acid, wherein the component A and the component B are prepared according to the weight ratio of 1: 1 and mixing.
Example 3, a method of preparing an organosilicon emulsifier, wherein component a comprises the steps of:
step (1), pumping 4 to 7 parts of low hydrogen silicone oil with hydrogen content of 0.1 to 0.2 percent and 3 to 6 parts of allyl alcohol polyoxyethylene ether into a reaction kettle in vacuum;
step (2), opening and stirring, heating to 100-120 ℃, and removing trace moisture in the raw materials with negative pressure for half an hour;
adding 0.3 per mill of isopropanol solution of chloroplatinic acid into the reaction kettle, and preserving the heat for 4 hours at the temperature of 120-140 ℃, wherein the materials in the kettle are changed into transparent and uniform liquid from turbid; cooling to below 50 deg.C to obtain the final product;
wherein the component B comprises the following steps:
step (1): pumping 4 to 7 parts of 0.1 to 0.2 percent hydrogen-containing low-hydrogen silicone oil and 3 to 6 parts of allyl alcohol polyoxypropylene ether into a reaction kettle by vacuum;
step (2): opening the stirrer, heating to 100-120 ℃, and removing trace moisture in the raw materials with negative pressure for half an hour;
and (3): adding 0.3 per mill isopropanol solution of chloroplatinic acid into the reaction kettle, preserving the heat for 4 hours at 120-140 ℃, changing the material in the kettle from turbid into transparent and uniform liquid, and cooling to below 50 ℃ to obtain a finished product;
and (3) mixing the finished product of the component A and the finished product of the component B according to the ratio of 1: 1, and then the mixture is mixed evenly to obtain the compound organic silicon emulsifier.
Embodiment 4, a method for preparing a silicone emulsifier, comprising component a, comprising the steps of:
step (1), pumping 6 parts of low hydrogen silicone oil with hydrogen content of 0.1-0.2% and 4 parts of allyl alcohol polyoxyethylene ether into a reaction kettle in vacuum;
step (2), opening stirring, heating to 110 ℃, and removing trace moisture in the raw materials under negative pressure for half an hour;
adding 0.3 per mill of isopropanol solution of chloroplatinic acid into the reaction kettle, and preserving the temperature for 4 hours at 130 ℃, wherein the materials in the kettle are changed into transparent and uniform liquid from turbid; cooling to below 50 deg.c to obtain the product.
Example 5, a method of preparing an organosilicon emulsifier, wherein component B, comprises the steps of:
step (1): pumping 6 parts of 0.1-0.2% hydrogen-containing low-hydrogen silicone oil and 4 parts of allyl alcohol polyoxypropylene ether into a reaction kettle in vacuum;
step (2): opening stirring, heating to 110 deg.C, and removing trace water in the raw materials under negative pressure for half an hour;
and (3): adding 0.3 per mill isopropanol solution of chloroplatinic acid into the reaction kettle, preserving the temperature for 4 hours at 130 ℃, changing the material in the kettle from turbid state into transparent and uniform liquid, and cooling to below 50 ℃ to obtain the finished product.
Example 6, a method of preparing a silicone emulsifier, wherein component a comprises the steps of:
step (1), pumping 6 parts of low hydrogen silicone oil with hydrogen content of 0.1-0.2% and 4 parts of allyl alcohol polyoxyethylene ether into a reaction kettle in vacuum;
step (2), opening stirring, heating to 110 ℃, and removing trace moisture in the raw materials under negative pressure for half an hour;
adding 0.3 per mill of isopropanol solution of chloroplatinic acid into the reaction kettle, and preserving the temperature for 4 hours at 130 ℃, wherein the materials in the kettle are changed into transparent and uniform liquid from turbid; cooling to below 50 deg.C to obtain the final product;
wherein the component B comprises the following steps:
step (1): pumping 6 parts of 0.1-0.2% hydrogen-containing low-hydrogen silicone oil and 4 parts of allyl alcohol polyoxypropylene ether into a reaction kettle in vacuum;
step (2): opening stirring, heating to 110 deg.C, and removing trace water in the raw materials under negative pressure for half an hour;
and (3): adding 0.3 per mill isopropanol solution of chloroplatinic acid into the reaction kettle, preserving the heat for 4 hours at 130 ℃, changing the materials in the kettle from turbid to transparent and uniform liquid, and cooling to below 50 ℃ to obtain a finished product;
and (3) mixing the finished product of the component A and the finished product of the component B according to the ratio of 1: 1, and then the mixture is mixed evenly to obtain the compound organic silicon emulsifier.
The products prepared in examples 4 to 6 were emulsified into hydroxyl-terminated polymethylphenylsiloxane, respectively, with a molecular weight of 30000, and an emulsification mode: the silicone emulsions were emulsified by dropping at 5000 rpm and stored for 15 days in a 30 ℃ environment, and then dispersed at 3000 rpm, and the silicone emulsions prepared by the products of examples 4 and 5 both showed creaming and floating, while the silicone emulsion prepared by the product of example 6 showed no change.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (7)
1. The organic silicon emulsifier is characterized by comprising a component A and/or a component B, wherein the component A comprises the following raw materials in parts by weight: 0.1-0.2% of low-hydrogen silicone oil with hydrogen content of 40-70%, 60-30% of allyl alcohol polyoxyethylene ether and 0.3% of isopropanol solution of chloroplatinic acid; the component B comprises the following raw materials in percentage by weight: 0.1-0.2% of low-hydrogen silicone oil with low hydrogen content, 40-70% of allyl alcohol polyoxypropylene ether and 0.3% of isopropanol solution of chloroplatinic acid.
2. The organic silicon emulsifier is characterized by being a composite organic silicon emulsifier which comprises a component A and a component B.
3. A silicone emulsifier according to claim 1, characterized in that; and mixing the component A and the component B to obtain the compound organic silicon emulsifier, wherein the component A and the component B are mixed according to the weight ratio of 1: 1 and mixing.
4. A preparation method of an organosilicon emulsifier is characterized by comprising the following steps: preparation of component A and/or component B.
5. The method for preparing the silicone emulsifier according to claim 4, wherein the component A comprises the following steps:
step (1), pumping 4 to 7 parts of low hydrogen silicone oil with hydrogen content of 0.1 to 0.2 percent and 3 to 6 parts of allyl alcohol polyoxyethylene ether into a reaction kettle in vacuum;
step (2), opening and stirring, heating to 100-120 ℃, and removing trace moisture in the raw materials with negative pressure for half an hour;
adding 0.3 per mill of isopropanol solution of chloroplatinic acid into the reaction kettle, and preserving the heat for 4 hours at the temperature of 120-140 ℃, wherein the materials in the kettle are changed into transparent and uniform liquid from turbid; cooling to below 50 deg.c to obtain the product.
6. The method for preparing a silicone emulsifier according to claim 4, wherein component B comprises the steps of:
step (1): pumping 4 to 7 parts of 0.1 to 0.2 percent hydrogen-containing low-hydrogen silicone oil and 3 to 6 parts of allyl alcohol polyoxypropylene ether into a reaction kettle by vacuum;
step (2): opening the stirrer, heating to 100-120 ℃, and removing trace moisture in the raw materials with negative pressure for half an hour;
and (3): adding 0.3 per mill isopropanol solution of chloroplatinic acid into the reaction kettle, preserving the heat for 4 hours at 120-140 ℃, changing the material in the kettle from turbid into transparent and uniform liquid, and cooling to below 50 ℃ to obtain the finished product.
7. The method for preparing a silicone emulsifier according to claim 4, wherein the ratio of the finished component A to the finished component B is 1: 1, and then the mixture is mixed evenly to obtain the compound organic silicon emulsifier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911205305.5A CN111040188B (en) | 2019-11-29 | 2019-11-29 | Organic silicon emulsifier and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911205305.5A CN111040188B (en) | 2019-11-29 | 2019-11-29 | Organic silicon emulsifier and preparation method thereof |
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| CN111040188A true CN111040188A (en) | 2020-04-21 |
| CN111040188B CN111040188B (en) | 2022-09-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113004529A (en) * | 2021-03-05 | 2021-06-22 | 无锡龙驰氟硅新材料有限公司 | Self-emulsifying self-curing fluorine-containing polysiloxane and synthesis method thereof |
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| CN113004529A (en) * | 2021-03-05 | 2021-06-22 | 无锡龙驰氟硅新材料有限公司 | Self-emulsifying self-curing fluorine-containing polysiloxane and synthesis method thereof |
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| CN111040188B (en) | 2022-09-02 |
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Effective date of registration: 20230117 Address after: 441000 south of Taoyuan road and west of the fourth West Ring Road, Zaoyang City, Xiangyang City, Hubei Province (Zaoyang Chemical Industrial Park) Patentee after: Hubei Longsheng Sihai New Material Co.,Ltd. Address before: 441000 building 3, group 5, neighborhood committee, Nancheng Wangjiawan community, Zaoyang City, Xiangyang City, Hubei Province Patentee before: HUBEI NEW SIHAI CHEMICAL INDUSTRY CO.,LTD. |
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Denomination of invention: A silicone emulsifier and its preparation method Granted publication date: 20220902 Pledgee: Bank of China Limited Xiangyang Branch Pledgor: Hubei Longsheng Sihai New Material Co.,Ltd. Registration number: Y2024980006288 |