CN111848852A - Processing technology of organic silicon modified water-based acrylic resin - Google Patents
Processing technology of organic silicon modified water-based acrylic resin Download PDFInfo
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- CN111848852A CN111848852A CN202010720274.3A CN202010720274A CN111848852A CN 111848852 A CN111848852 A CN 111848852A CN 202010720274 A CN202010720274 A CN 202010720274A CN 111848852 A CN111848852 A CN 111848852A
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- 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
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
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Abstract
The invention relates to the technical field of high molecular polymers, in particular to a processing technology of organic silicon modified waterborne acrylic resin, which comprises the steps of premixing 70-120g of methyl methacrylate, 5-30g of butyl methacrylate, 60-100g of iso-neoacrylate, 3-10g of hydroxyethyl acrylate, 5-10g of butyl acrylate, 260g of styrene-acrylic acid, 55-70g of acrylic acid, 40-60g of silane coupling agent, 20-30g of benzoyl peroxide and 5-15g of ethylene glycol butyl ether, and adding the premixed materials into a dropping funnel to form a mixture; putting the four-mouth bottle into a heater, starting stirring and heating to a proper temperature, and then dropwise adding the mixture obtained in the step S2 for 2.5 hours; immediately adding 1-3g of benzoyl peroxide and 15-25g of ethylene glycol butyl ether after the completion of the step S3, finishing dropping within 30 minutes, and keeping the temperature at 155-165 ℃ for 1.5 hours after the completion of dropping; after the step S4 is completed, the temperature is reduced to 95-105 ℃, and 125g of ethylene glycol butyl ether is added to filter and store the finished product for later use.
Description
Technical Field
The invention relates to the technical field of high molecular polymers, in particular to a processing technology of organic silicon modified waterborne acrylic resin.
Background
In the organic polymer, Si-O bond energy (450kl/mol is far greater than C-C bond energy (345 kJ/mol and C-O bond energy (351kJ/mol, excellent high temperature resistance, ultraviolet radiation resistance, oxidative degradation resistance and chemical resistance) is greatly increased, an organosiloxane monomer is introduced into the main chain of the acrylic resin polymer by adopting a copolymerization method, and during film formation, organosiloxane is hydrolyzed and condensed to form Si-Si bonds with a cross-linking structure between polymer macromolecules and a polymer and a base material, so that the coating is endowed with excellent weather resistance, water resistance, stain resistance, light resistance and adhesive force, and the silicone-acrylic resin is widely applied to automobile finishing paint and industrial machinery, The resin is considered to be the resin variety with the most development prospect in the aspects of household appliances, metal furniture, plastics, building outer walls and the like, particularly in the aspect of building outer walls.
Therefore, how to design a processing technology of the organosilicon modified water-based acrylic resin is a problem to be solved by the application.
Disclosure of Invention
In order to solve the problems, the invention provides a processing technology of organic silicon modified waterborne acrylic resin, which has the characteristics of simple technology and high yield.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a processing technology of organic silicon modified waterborne acrylic resin, which comprises the following steps:
step S1, preparing a four-mouth bottle provided with a stirrer, a thermometer, a dropping funnel and a condenser tube, and adding a proper amount of ethylene glycol butyl ether into the four-mouth bottle;
step S2, pre-mixing 70-120g of methyl methacrylate, 5-30g of butyl methacrylate, 60-100g of iso-neoacrylate, 3-10g of hydroxyethyl acrylate, 5-10g of butyl acrylate, 350g of styrene 260-350g, 55-70g of acrylic acid, 40-60g of silane coupling agent, 20-30g of benzoyl peroxide and 5-15g of ethylene glycol butyl ether, and adding the pre-mixed materials into the dropping funnel to form a mixture;
step S3, putting the four-mouth bottle into a heater, starting stirring and heating to a proper temperature, and then dropwise adding the mixture obtained in the step S2 for 2.5 hours;
step S4, adding 1-3g of benzoyl peroxide and 15-25g of butyl cellosolve immediately after the step S3 is finished, dripping off within 30 minutes, and keeping the temperature at 155-165 ℃ for 1.5 hours after the dripping off is finished;
and S5, after the step S4 is finished, cooling to 95-105 ℃, adding 115 g of ethylene glycol butyl ether and 125g of ethylene glycol butyl ether, and filtering and storing the finished product for later use.
Preferably, the amount of ethylene glycol butyl ether added in the step S1 is 120-140 g.
Preferably, the butyl cellosolve is 130 g.
Preferably, in the step S2, 70g of methyl methacrylate, 5g of butyl methacrylate, 60g of iso-neoacrylate, 3g of hydroxyethyl acrylate, 5g of butyl acrylate, 260g of styrene, 55g of acrylic acid, 40g of a silane coupling agent, 20g of benzoyl peroxide and 5g of ethylene glycol butyl ether are adopted.
Preferably, in the step S2, the content of methyl methacrylate is 120g, the content of butyl methacrylate is 30g, the content of iso-neoacrylate is 100g, the content of hydroxyethyl acrylate is 10g, the content of butyl acrylate is 10g, the content of styrene is 350g, the content of acrylic acid is 70g, the content of silane coupling agent is 60g, the content of benzoyl peroxide is 30g, and the content of ethylene glycol butyl ether is 15 g.
Preferably, in the step S2, 95g of methyl methacrylate, 20g of butyl methacrylate, 80g of iso-neoacrylate, 6g of hydroxyethyl acrylate, 8g of butyl acrylate, 300g of styrene, 60g of acrylic acid, 50g of a silane coupling agent, 25g of benzoyl peroxide and 10g of ethylene glycol butyl ether are adopted.
Preferably, the heating temperature in the step S3 is 160 ℃.
Preferably, in the step S4, benzoyl oxide 2g and butyl glycol ether 20g are used.
Preferably, the temperature in step S5 is decreased to 100 ℃.
Preferably, 120g of butyl cellosolve is adopted in the step S5.
The technical scheme of the invention has the following beneficial technical effects:
the processing technology of the invention is stable, the prepared resin with excellent water resistance and scrubbing resistance can be widely applied as water-based material, and the efficiency of the technology is greatly improved compared with the traditional technology.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easily understood, the invention is further described below with reference to the specific embodiments and the attached drawings, but the following embodiments are only the preferred embodiments of the invention, and not all embodiments. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Refer to fig. 1.
Example 1
The invention provides a processing technology of organic silicon modified waterborne acrylic resin, which comprises the following steps:
step S1, preparing a four-mouth bottle provided with a stirring device, a thermometer, a dropping funnel and a condensing tube, and adding 130 ethylene glycol butyl ether into the four-mouth bottle;
step S2, premixing 70g of methyl methacrylate, 5g of butyl methacrylate, 60g of iso-neoacrylate, 3g of hydroxyethyl acrylate, 5g of butyl acrylate, 260g of styrene, 55g of acrylic acid, 40g of silane coupling agent, 20g of benzoyl peroxide and 5g of ethylene glycol butyl ether, and adding the premixed materials into the dropping funnel to form a mixture;
step S3, putting the four-mouth bottle into a heater, starting stirring and heating to 160 ℃, and then dropwise adding the mixture obtained in the step S2 for 2.5 hours;
step S4, immediately adding 2g of benzoyl peroxide and 20g of butyl cellosolve after the step S3 is finished, dripping the mixture for 30 minutes, and keeping the temperature at 160 ℃ for 1.5 hours after the dripping is finished;
and step S5, after the step S4 is finished, cooling to 100 ℃, adding 120g of butyl cellosolve, and filtering and storing the finished product for later use.
Example 2
The invention provides a processing technology of organic silicon modified waterborne acrylic resin, which comprises the following steps:
step S1, preparing a four-mouth bottle provided with a stirrer, a thermometer, a dropping funnel and a condenser tube, and adding 130g of ethylene glycol butyl ether into the four-mouth bottle;
step S2, pre-mixing 120g of methyl methacrylate, 30g of butyl methacrylate, 100g of iso-neoacrylate, 10g of hydroxyethyl acrylate, 10g of butyl acrylate, 350g of styrene, 70g of acrylic acid, 60g of silane coupling agent, 30g of benzoyl peroxide and 15g of butyl glycol ether, and adding the pre-mixed materials into the dropping funnel to form a mixture;
step S3, putting the four-mouth bottle into a heater, starting stirring and heating to 160 ℃, and then dropwise adding the mixture obtained in the step S2 for 2.5 hours;
step S4, immediately adding 2g of benzoyl peroxide and 20g of butyl cellosolve after the step S3 is finished, dripping the mixture for 30 minutes, and keeping the temperature at 160 ℃ for 1.5 hours after the dripping is finished;
and step S5, after the step S4 is finished, cooling to 100 ℃, adding 120g of butyl cellosolve, and filtering and storing the finished product for later use.
Example 3
The invention provides a processing technology of organic silicon modified waterborne acrylic resin, which comprises the following steps:
step S1, preparing a four-mouth bottle provided with a stirrer, a thermometer, a dropping funnel and a condenser tube, and adding a proper amount of ethylene glycol butyl ether into the four-mouth bottle;
step S2, pre-mixing 95g of methyl methacrylate, 20g of butyl methacrylate, 80g of iso-neoacrylate, 6g of hydroxyethyl acrylate, 8g of butyl acrylate, 300g of styrene, 60g of acrylic acid, 50g of silane coupling agent, 25g of benzoyl peroxide and 10g of butyl glycol ether, and adding the pre-mixed materials into the dropping funnel to form a mixture;
step S3, putting the four-mouth bottle into a heater, starting stirring and heating to 160 ℃, and then dropwise adding the mixture obtained in the step S2 for 2.5 hours;
step S4, immediately adding 2g of benzoyl peroxide and 20g of butyl cellosolve after the step S3 is finished, dripping the mixture for 30 minutes, and keeping the temperature at 160 ℃ for 1.5 hours after the dripping is finished;
and step S5, after the step S4 is finished, cooling to 100 ℃, adding 120g of butyl cellosolve, and filtering and storing the finished product for later use.
After using this process, the final product data obtained are as follows:
finished product | Solid content | Viscosity (Grignard second) | Acid value | Density of | Colour value |
Example 1 | 63% | 100-120 | 70-75 | 0.89 | <2 |
Example 2 | 65% | 100-130 | 65-70 | 0.96 | <2 |
Example 3 | 68% | 100-140 | 60-70 | 1 | <2 |
From the above table data, the present invention is preferred embodiment 3.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The processing technology of the organic silicon modified waterborne acrylic resin is characterized by comprising the following steps:
step S1, preparing a four-mouth bottle provided with a stirrer, a thermometer, a dropping funnel and a condenser tube, and adding a proper amount of ethylene glycol butyl ether into the four-mouth bottle;
step S2, pre-mixing 70-120g of methyl methacrylate, 5-30g of butyl methacrylate, 60-100g of iso-neoacrylate, 3-10g of hydroxyethyl acrylate, 5-10g of butyl acrylate, 350g of styrene 260-350g, 55-70g of acrylic acid, 40-60g of silane coupling agent, 20-30g of benzoyl peroxide and 5-15g of ethylene glycol butyl ether, and adding the pre-mixed materials into the dropping funnel to form a mixture;
step S3, putting the four-mouth bottle into a heater, starting stirring and heating to a proper temperature, and then dropwise adding the mixture obtained in the step S2 for 2.5 hours;
step S4, adding 1-3g of benzoyl peroxide and 15-25g of butyl cellosolve immediately after the step S3 is finished, dripping off within 30 minutes, and keeping the temperature at 155-165 ℃ for 1.5 hours after the dripping off is finished;
and S5, after the step S4 is finished, cooling to 95-105 ℃, adding 115 g of ethylene glycol butyl ether and 125g of ethylene glycol butyl ether, and filtering and storing the finished product for later use.
2. The processing technology of organosilicon modified waterborne acrylic resin as claimed in claim 1, wherein the amount of ethylene glycol butyl ether added in step S1 is 120-140 g.
3. The processing technology of organosilicon modified waterborne acrylic resin as claimed in claim 2, wherein the butyl glycol ether is 130 g.
4. The processing technology of the organosilicon modified waterborne acrylic resin as claimed in claim 1, wherein in the step S2, methyl methacrylate is 70g, butyl methacrylate is 5g, iso-neoacrylate is 60g, hydroxyethyl acrylate is 3g, butyl acrylate is 5g, styrene is 260g, acrylic acid is 55g, silane coupling agent is 40g, benzoyl peroxide is 20g, and ethylene glycol butyl ether is 5 g.
5. The processing technology of the organosilicon modified waterborne acrylic resin as claimed in claim 1, wherein in the step S2, the processing technology comprises 120g of methyl methacrylate, 30g of butyl methacrylate, 100g of iso-neoacrylate, 10g of hydroxyethyl acrylate, 10g of butyl acrylate, 350g of styrene, 70g of acrylic acid, 60g of silane coupling agent, 30g of benzoyl peroxide and 15g of ethylene glycol butyl ether.
6. The processing technology of the organosilicon modified waterborne acrylic resin as claimed in claim 1, wherein in the step S2, the processing technology comprises 95g of methyl methacrylate, 20g of butyl methacrylate, 80g of iso-neoacrylate, 6g of hydroxyethyl acrylate, 8g of butyl acrylate, 300g of styrene, 60g of acrylic acid, 50g of silane coupling agent, 25g of benzoyl peroxide and 10g of ethylene glycol butyl ether.
7. The processing technology of silicone-modified aqueous acrylic resin according to claim 1, wherein the heating temperature in step S3 is 160 ℃.
8. The processing technology of the organosilicon modified waterborne acrylic resin as claimed in claim 1, wherein in step S4, benzoyl oxide 2g and butyl glycol ether 20g are added.
9. The processing technology of the organosilicon modified waterborne acrylic resin as claimed in claim 1, wherein the temperature in step S5 is decreased to 100 ℃.
10. The processing technology of organosilicon modified waterborne acrylic resin as claimed in claim 1, wherein in step S5, 120g of butyl glycol ether is used.
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Citations (5)
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US20020156174A1 (en) * | 1999-07-29 | 2002-10-24 | Robson Mafoti | Moisture curable acrylic sealants |
CN105330784A (en) * | 2014-08-01 | 2016-02-17 | 阜阳师范学院 | Method for preparing waterborne acrylic resin |
CN106905468A (en) * | 2017-03-26 | 2017-06-30 | 沈阳宣伯新材料科技有限公司 | Extra-weather-proof type aqueous, environmental protective resin and its preparation technology |
CN109796555A (en) * | 2019-01-08 | 2019-05-24 | 江西省科学院应用化学研究所 | A kind of preparation method of high-performance water-based acrylic resin |
CN111217955A (en) * | 2018-11-26 | 2020-06-02 | 阜阳师范学院 | Water-based acrylic resin and preparation method thereof |
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2020
- 2020-07-24 CN CN202010720274.3A patent/CN111848852A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20020156174A1 (en) * | 1999-07-29 | 2002-10-24 | Robson Mafoti | Moisture curable acrylic sealants |
CN105330784A (en) * | 2014-08-01 | 2016-02-17 | 阜阳师范学院 | Method for preparing waterborne acrylic resin |
CN106905468A (en) * | 2017-03-26 | 2017-06-30 | 沈阳宣伯新材料科技有限公司 | Extra-weather-proof type aqueous, environmental protective resin and its preparation technology |
CN111217955A (en) * | 2018-11-26 | 2020-06-02 | 阜阳师范学院 | Water-based acrylic resin and preparation method thereof |
CN109796555A (en) * | 2019-01-08 | 2019-05-24 | 江西省科学院应用化学研究所 | A kind of preparation method of high-performance water-based acrylic resin |
Non-Patent Citations (2)
Title |
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杨玉玮: "有机硅改性丙烯酸树脂的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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