CN112538141B - Preparation method of hydrophobically modified polymer - Google Patents
Preparation method of hydrophobically modified polymer Download PDFInfo
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- CN112538141B CN112538141B CN202011330138.XA CN202011330138A CN112538141B CN 112538141 B CN112538141 B CN 112538141B CN 202011330138 A CN202011330138 A CN 202011330138A CN 112538141 B CN112538141 B CN 112538141B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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Abstract
The invention belongs to the field of polymers, and provides a preparation method of a hydrophobic modified polymer for solving the problem of poor heavy feeling of a traditional product, which comprises the following steps of carrying out free radical polymerization on the following monomers in parts by weight: 100 parts by weight of acrylic acid; 10-15 parts of hard monomer; 5-10 parts of hydroxypropyl acrylate; 1-5 parts of hydrophobic association type monomer. The polymer prepared by the method has better massive feeling after being applied to hydrogel.
Description
Technical Field
The invention relates to the field of polymers, in particular to a preparation method of a hydrophobically modified polymer.
Background
Acrylic thickeners are lightly crosslinked acrylic polymers which provide excellent stability and thickening properties to the surfactant system and excellent suspendability even in low viscosity formulations, and insoluble and difficult to stabilize ingredients such as silicones can be co-emulsified and stabilized.
It is widely used in the field of daily chemicals, and is characterized in that:
excellent suspension and thickening performance, and improves the working efficiency of formulators;
the compatibility is strong, and the cationic polymer is almost compatible with all nonionic, anionic and amphoteric surfactants and various cationic polymers;
can be used for transparent products, is convenient to use and is an ideal matching of personal cleaning products.
The polymer hydrogel has a less-concerned performance, namely, the feeling of heaviness, which is detected by an effective scientific method and is represented by the following skin feeling of a human body: when the gel was uniformly applied to the skin, the spreading property feeling was more excellent and the tightening feeling of the gel layer was more noticeable.
After the performance is applied to daily chemical products, the use feeling of the daily chemical products, particularly daily chemicals for moisturizing and nursing is better.
The study of hydrogels with a thick feel is the direction of the present discussion.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a hydrophobic modified polymer, and the polymer prepared by the method has better heavy feeling.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a hydrophobic modified polymer comprises the following steps of carrying out free radical polymerization reaction on the following monomers in parts by weight:
further, the hard monomer is methyl methacrylate, styrene or ethyl methacrylate.
Further, the hydrophobic association type monomer is long-chain alkyl polyoxyethylene ether acrylate of C16-C22.
Further, the method specifically comprises the following steps: adding a mixture of ethyl acetate and cyclohexane serving as solvents, a monomer, a dispersing agent and a cross-linking agent into a reaction kettle, heating to 65-70 ℃, dropwise adding an initiator solution, reacting for 4-8 hours, finishing the reaction, and filtering and drying a product.
Further, the amount of the mixture of ethyl acetate and cyclohexane is 2 to 4 times of the total amount of the monomers. Generally, a weight ratio of cyclohexane to ethyl acetate of 2.5 to 3.
Further, the initiator accounts for 1-1.5% of the total weight of the monomers; the initiator is azobisisoheptonitrile.
Further, the dispersant is sodium dodecyl sulfate, and the dosage of the dispersant is 1.5 to 2 percent of the weight of the monomer.
Further, the crosslinking agent is one of N, N-methylene bisacrylamide, diallyl phthalate and ethylene glycol dimethacrylate, and the crosslinking agent accounts for 0.8-1.2% of the weight of the monomer.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts the combination of acrylic acid, hard monomer, hydroxyalkyl acrylate and hydrophobic association type monomer, can lead the hydrogel of the polymer to show better thick and heavy feeling, and can show more excellent spreading performance after being applied to daily chemicals.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the following embodiments, but the present invention is not limited thereto.
Example 1
A preparation method of a hydrophobic modified polymer comprises the steps of adding a solvent, a monomer, a dispersing agent and a cross-linking agent into a reaction kettle, heating to 65-70 ℃, dropwise adding an initiator solution, reacting for 6 hours, finishing the reaction, filtering and drying a product;
the components in the system are as follows:
wherein, the solvent is cyclohexane and ethyl acetate, the weight ratio is 3;
the monomer is as follows: acrylic acid, methyl methacrylate, hydroxypropyl acrylate, cetyl polyoxyethylene ether acrylate, in a ratio of 100.
Example 2
A preparation method of a hydrophobic modified polymer comprises the steps of adding a solvent, a monomer, a dispersant and a cross-linking agent into a reaction kettle, heating to 65-70 ℃, dropwise adding an initiator solution, reacting for 8 hours, finishing the reaction, filtering and drying a product;
the components in the system are as follows:
wherein, the solvent is cyclohexane and ethyl acetate, the weight ratio is 3;
the monomer is as follows: acrylic acid, methyl methacrylate, hydroxypropyl acrylate, octadecyl polyoxyethylene ether acrylate, in a ratio of 100.
Example 3
A preparation method of a hydrophobic modified polymer comprises the steps of adding a solvent, a monomer, a dispersant and a cross-linking agent into a reaction kettle, heating to 65-70 ℃, dropwise adding an initiator solution, reacting for 4 hours, finishing the reaction, filtering and drying a product;
the components in the system are as follows:
wherein, the solvent is cyclohexane and ethyl acetate, the weight ratio is 3;
the monomer is as follows: acrylic acid, methyl methacrylate, hydroxypropyl acrylate, eicosylpolyoxyethylene ether acrylate, in a ratio of 100.
Example 4
A preparation method of a hydrophobic modified polymer comprises the steps of adding a solvent, a monomer, a dispersant and a cross-linking agent into a reaction kettle, heating to 65-70 ℃, dropwise adding an initiator solution, reacting for 4 hours, finishing the reaction, filtering and drying a product;
the components in the system are as follows:
wherein, the solvent is cyclohexane and ethyl acetate, the weight ratio is 3;
the monomer is as follows: acrylic acid, methyl methacrylate, hydroxypropyl acrylate, eicosylpolyoxyethylene ether acrylate, in a ratio of 100.
Comparative example 1
With reference to example 1, the different experimental conditions were: the monomer does not contain hydroxypropyl acrylate.
Test items
The test items were viscosity, light transmittance, and a feeling of heaviness test with the addition amount of the polymer thickener powder of 0.5% of the hydrogel.
The viscosity was measured as follows: viscosity measured at 20 revolutions per minute with a Brookfield DV-II viscometer;
the light transmittance test instrument is as follows: (model 725 ultraviolet-visible spectrophotometer, shanghai prism technology Co., ltd.).
The method for testing the heaviness comprises the following steps: 0.5% strength hydrogel from example 1, comparative example 1 and a commercially available acrylic thickener a 0.5% strength hydrogel was blinded by volunteers and evaluated for heaviness of friction between thumb and forefinger, spreadability on the arm and firmness, with the evaluation being scored on a 1-5 point scale, with higher scores indicating more pronounced feel.
TABLE 1 test results of examples and comparative examples
TABLE 2 Thick weight test results
| Serial number | Feeling of heaviness | Spreadability | Compactness |
| Example 1 | 5 | 5 | 5 |
| Comparative example 1 | 2 | 3 | 2 |
| Commercially available product | 4 | 4 | 4 |
Claims (7)
1. The preparation method of the hydrophobic modified polymer is characterized in that the following monomers in parts by weight are subjected to free radical polymerization:
100 parts by weight of acrylic acid;
10-15 parts of hard monomer;
5-10 parts of hydroxypropyl acrylate;
1-5 parts of hydrophobic association type monomer;
the hydrophobic association type monomer is long-chain alkyl polyoxyethylene ether acrylate of C16-C22.
2. The method of claim 1, wherein: the hard monomer is methyl methacrylate, styrene or ethyl methacrylate.
3. The production method according to claim 1, characterized in that: the method specifically comprises the following steps: adding a mixture of solvents of ethyl acetate and cyclohexane, a monomer, a dispersant and a cross-linking agent into a reaction kettle, heating to 65-70 ℃, dropwise adding an initiator solution, reacting for 4-8h, finishing the reaction, filtering and drying a product.
4. The production method according to claim 3, characterized in that: the amount of the mixture of ethyl acetate and cyclohexane is 2-4 times of the total amount of the monomers.
5. The production method according to claim 3, characterized in that: the initiator accounts for 1-1.5% of the total weight of the monomers; the initiator is azobisisoheptonitrile.
6. The production method according to claim 3, characterized in that: the dispersant is sodium dodecyl sulfate, and the dosage of the dispersant is 1.5 to 2 percent of the weight of the monomer.
7. The production method according to claim 3, characterized in that: the crosslinking agent is one of N, N-methylene bisacrylamide, diallyl phthalate and ethylene glycol dimethacrylate, and the weight of the crosslinking agent is 0.8-1.2% of that of the monomer.
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| JPH0610220B2 (en) * | 1986-08-27 | 1994-02-09 | 大阪有機化学工業株式会社 | Super absorbent resin manufacturing method |
| AU6169598A (en) * | 1997-02-12 | 1998-08-26 | K B Technologies Ltd. | Composition and method for a dual-function soil-grouting excavating or boring fluid |
| CN1934206A (en) * | 2004-03-17 | 2007-03-21 | 西巴特殊化学品控股有限公司 | Liquid dispersion polymer thickeners for aqueous systems |
| EP2287216A1 (en) * | 2009-08-06 | 2011-02-23 | Basf Se | Water soluble associative polymers |
| KR101072371B1 (en) * | 2010-09-20 | 2011-10-11 | 주식회사 엘지화학 | Adhesive for polarizing plate and polarizing plate comprising the same |
| CN103788283B (en) * | 2014-01-17 | 2016-01-20 | 广州市东雄化工有限公司 | A kind of hydrophobically modified associative thickener and preparation method thereof |
| CN107099001B (en) * | 2017-04-19 | 2019-08-02 | 广州天赐高新材料股份有限公司 | A kind of polymers of carboxylic acid thickener and preparation method thereof |
| CN107641167A (en) * | 2017-09-14 | 2018-01-30 | 上海优卡化工科技有限公司 | A kind of hydrophobically modified acrylic compounds association thickener and preparation method thereof |
| WO2019188795A1 (en) * | 2018-03-30 | 2019-10-03 | 株式会社マンダム | Gel cosmetic |
| CN111592865B (en) * | 2020-04-11 | 2022-04-22 | 北京宏勤石油助剂有限公司 | Hydroxyl film forming agent for drilling fluid and preparation method thereof |
| CN111533850A (en) * | 2020-04-20 | 2020-08-14 | 天津中油渤星工程科技有限公司 | Method for preparing tackifier by soap-free method, tackifier and drilling fluid |
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Denomination of invention: A Preparation Method of Hydrophobically Modified Polymer Effective date of registration: 20230810 Granted publication date: 20230203 Pledgee: Bank of Guiyang Limited by Share Ltd. Danzhai branch Pledgor: GUIZHOU XINZIHONG PHARMACEUTIC ADJUVANT Co.,Ltd. Registration number: Y2023980051498 |