CN111205388A - Chlorine-containing fluorocarbon water-proof and oil-proof agent copolymer emulsion and polymerization method thereof - Google Patents
Chlorine-containing fluorocarbon water-proof and oil-proof agent copolymer emulsion and polymerization method thereof Download PDFInfo
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Abstract
The invention discloses a copolymer emulsion of fluorine-carbon water-proof and oil-proof agent containing chlorine and its polymerization method, which comprises the following components, emulsifier, four to six kinds of surface active agents with different hydrophile-lipophile balance (HLB value); at least one of a polymerized monomer, perfluoroalkyl ethyl acrylate (methyl), perfluoro octyl ethyl acrylate, perfluoro octyl methyl ethyl acrylate, perfluoro hexyl ethyl acrylate and perfluoro hexyl methyl ethyl acrylate; from the general formula CH2＝CCl(C＝O)‑O‑CnH2n+1Chloroacrylates of formula (I) wherein n is 12, 14, 16, 18, 20, 22; a functional monomer. The copolymer emulsion of the fluorine-containing fluorocarbon waterproof and oil-proof agent utilizes the characteristic of strong electronegativity of chlorine-containing groups to improve the adsorption of the waterproof agent to fabrics and improve the waterproof effect and the water washing resistance, the long-chain chloroacrylate has little influence on the waterproof and oil-proof effects relative to the short-chain polyethylene, and no toxic substances such as vinyl chloride are required to be pressurized in the reaction process.
Description
The technical field is as follows:
the invention relates to the field of waterproof and oil-proof agents, in particular to a chlorine-containing fluorocarbon waterproof and oil-proof agent copolymer emulsion and a polymerization method thereof.
Background art:
the existing copolymer emulsion of perfluoroalkyl ethyl acrylate (methyl) containing chlorine on the market generally adopts vinyl chloride as a reaction monomer to carry out reaction. The characteristic of strong electronegativity of the chlorine-containing group is utilized to improve the adsorption of the waterproof agent to the fabric, thereby improving the waterproof effect. This reaction has the following problems: 1. vinyl chloride forms an explosive mixture with air, the explosion limit is 3.6-33% (volume), and the mixture is more explosive under pressurization, and the reaction process needs pressurization and has certain danger. 2. Vinyl chloride is a toxic substance and can cause liver cancer by long-term inhalation and contact. 3. Short-chain vinyl chloride affects the water-repellent properties.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a novel chlorine-containing fluorocarbon waterproof and oil-proof agent copolymer emulsion synthesized by replacing a part of long-chain acrylic ester with long-chain chloroacrylic ester on the basis of the traditional waterproof and oil-proof agent (perfluoroalkyl ethyl acrylate (methyl) copolymer emulsion) for fabrics, wherein the chlorine-containing fluorocarbon waterproof and oil-proof agent copolymer emulsion utilizes the characteristic of strong electronegativity of a chlorine-containing group to improve the adsorption of a waterproof agent to fabrics and improve the waterproof effect and the washing resistance, the long-chain chloroacrylic ester has little influence on the waterproof and oil-proof effects relative to short-chain polyethylene, and the chlorine-containing fluorocarbon waterproof and oil-proof agent copolymer emulsion does not need pressurization and does not contain toxic substances such as chloroethylene in the reaction process, thereby being a safer normal-pressure emulsion polymerization reaction.
The technical scheme of the invention is to provide a copolymer emulsion containing chlorine fluorocarbon waterproof and oil-proof agents, which is characterized in that: which comprises the following components in percentage by weight,
an emulsifier consisting of four to six surfactants of different hydrophilic-lipophilic balance (HLB value);
at least one of a polymerized monomer, perfluoroalkyl ethyl acrylate (methyl), perfluoro octyl ethyl acrylate, perfluoro octyl methyl ethyl acrylate, perfluoro hexyl ethyl acrylate and perfluoro hexyl methyl ethyl acrylate;
from the general formula CH2＝CCl(C＝O)-O-CnH2n+1Chloroacrylates of formula (I) wherein n is 12, 14, 16, 18, 20, 22;
at least one of a functional monomer, octadecyl acrylate, octadecyl methacrylate, hexadecyl acrylate, hexadecyl methacrylate, docosyl acrylate, docosyl methacrylate, lauryl acrylate, lauryl methacrylate, hydroxyethyl acrylate, hydroxymethyl acrylamide, hydroxypropyl acrylate, hydroxybutyl acrylate, hydroxypropyl methacrylate, hydroxybutyl methacrylate, N-isobutoxy acrylamide, N-methylolacrylamide, hydroxyoctyl acrylate, isocyanato acrylate, acetoacetoxyethyl methacrylate, glycidyl methacrylate;
initiator, 2, 2' -azobis (2-aminopropane) dihydrochloride;
cosolvent, at least one of tripropylene glycol TPG, propylene glycol methyl ether PM, dipropylene glycol methyl ether DPM, polyethylene glycol PEG, dipropylene glycol DPG and diethylene glycol methyl ether DEM;
at least one of a chain transfer agent, dodecyl mercaptan and octyl mercaptan;
pH value regulator: at least one of acetic acid, citric acid and nitric acid.
Preferably, it contains the following components in percentage by mass,
preferably, it contains the following components in percentage by mass,
preferably, it contains the following components in percentage by mass,
the invention also provides a polymerization method of the copolymer emulsion containing the chlorine fluorocarbon waterproof and oil-proof agent, which is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
step 1, preparing a liquid, namely preparing a pre-emulsion from components except an initiator and dilution water of the initiator in a formula according to a proportion, placing the pre-emulsion in a water bath at 60 ℃, and stirring and preserving heat for 30 minutes at 300 revolutions per minute;
step 2, homogenizing the pre-emulsion for three times by using a high-pressure homogenizer or an ultrasonic homogenizer;
step 3, pouring the homogenized pre-emulsion into a reactor with a thermometer, a stirrer, a condenser pipe and a protective gas through pipe, setting the temperature in the reactor to be 60-75 ℃, introducing nitrogen N into the reactor at the rotating speed of the stirrer according to 100 revolutions per minute2Stopping introducing air after three minutes, increasing the rotating speed of the stirrer to 200 revolutions per minute, slowly dripping 5 percent aqueous solution of the initiator when the temperature of the thermometer reaches 58 ℃, and finishing dripping within half an hour;
and 4, maintaining the temperature at 60-75 ℃, adding an initiator until the reaction is finished, then cooling, filtering (a 100-mesh filter screen with 200 meshes) and bottling.
Preferably, when the chlorine-containing fluorine-free water repellent copolymer emulsion component contains a water-soluble monomer, the water-soluble monomer and the diluting water for diluting the water-soluble monomer are removed in addition to the initiator and the diluting water for diluting the initiator in the solution preparation in step 1, and the aqueous solution of the water-soluble monomer is continuously added dropwise at a concentration of 10 to 20% in the latter half hour after the completion of the addition of the initiator, and the addition is completed in two hours.
Further, the method comprises the following steps of,
step 1, preparing a pre-emulsion from 1.5g of octadecyl trimethyl ammonium chloride, 1.2g of Tween 40, 4.8g of lauryl polyoxyethylene ether 30, 2.4g of polyoxyethylene dioleate, 0.3g of dodecyl mercaptan, 18g of octadecyl acrylate, 24g of octadecyl chloroacrylate, 42g of perfluorohexylethyl methacrylate, 0.3g of lauryl methacrylate, 3g of methyl methacrylate, 1.5g of N-hydroxymethyl acrylamide, 21g of dipropylene glycol methyl ether, 2.1g of glacial acetic acid and 150g of deionized water, placing the pre-emulsion in a water bath at the temperature of 60 ℃, and stirring and preserving heat for 30 minutes at 300 revolutions per minute;
step 2, homogenizing the pre-emulsion for three times by using a high-pressure homogenizer or an ultrasonic homogenizer, and cooling by using cold water at the temperature of 20 ℃ during homogenization;
step 3, pouring the homogenized pre-emulsion into a reactor with a thermometer, a stirrer, a condenser pipe and a protective gas through pipe, setting the temperature in the reactor to be 70 ℃, introducing nitrogen N into the reactor at the rotating speed of the stirrer according to 100 revolutions per minute2Stopping ventilation after three minutes, increasing the rotating speed of the stirrer to 200 revolutions per minute, slowly dripping 1.2g of (2, 2' -azobis (2-aminopropane) dihydrochloride into an initiator aqueous solution prepared by dissolving 15.8g of deionized water when the thermometer reaches 58 ℃, finishing dripping within half an hour, continuously dripping 0.9g of hydroxypropyl acrylate aqueous solution prepared by dissolving 10g of deionized water after the initiator is dripped, and finishing dripping within two hours;
and 4, maintaining the water bath at 72 ℃ until the reaction is finished, cooling to below 40 ℃ after the reaction is finished, filtering by using a 200-mesh filter screen, and bottling.
Compared with the prior art, the invention has the following advantages after adopting the scheme: a novel chlorine-containing fluorocarbon waterproof and oil-proof agent copolymer emulsion is synthesized by replacing a part of long-chain acrylic ester with long-chain chloroacrylic ester on the basis of the traditional waterproof and oil-proof agent for fabrics (perfluoroalkyl ethyl acrylate (methyl) copolymer emulsion).
The specific implementation mode is as follows:
the invention is further illustrated with respect to specific embodiments below:
example 1
A copolymer emulsion of fluorine-carbon water-proof and oil-proof agent contains the following components by mass percent,
the polymerization method comprises the following steps,
comprises the following steps of (a) carrying out,
step 1, preparing a pre-emulsion from 1.5g of octadecyl trimethyl ammonium chloride, 1.2g of Tween 40, 4.8g of lauryl polyoxyethylene ether 30, 2.4g of polyoxyethylene dioleate, 0.3g of dodecyl mercaptan, 18g of octadecyl acrylate, 24g of octadecyl chloroacrylate, 42g of perfluorohexylethyl methacrylate, 0.3g of lauryl methacrylate, 3g of methyl methacrylate, 1.5g of N-hydroxymethyl acrylamide, 21g of dipropylene glycol methyl ether, 2.1g of glacial acetic acid and 150g of deionized water, placing the pre-emulsion in a water bath at the temperature of 60 ℃, and stirring and preserving heat for 30 minutes at 300 revolutions per minute;
step 2, homogenizing the pre-emulsion for three times by using a high-pressure homogenizer or an ultrasonic homogenizer, and cooling by using cold water at the temperature of 20 ℃ during homogenization;
step 3, pouring the homogenized pre-emulsion into a reactor with a thermometer, a stirrer, a condenser pipe and a protective gas through pipe, setting the temperature in the reactor to be 70 ℃, introducing nitrogen N into the reactor at the rotating speed of the stirrer according to 100 revolutions per minute2Stopping ventilation after three minutes, increasing the rotating speed of the stirrer to 200 revolutions per minute, slowly dripping 1.2g of (2, 2' -azobis (2-aminopropane) dihydrochloride into an initiator aqueous solution prepared by dissolving 15.8g of deionized water when the thermometer reaches 58 ℃, finishing dripping within half an hour, continuously dripping 0.9g of hydroxypropyl acrylate aqueous solution prepared by dissolving 10g of deionized water after the initiator is dripped, and finishing dripping within two hours;
and 4, maintaining the water bath at 72 ℃ until the reaction is finished, cooling to below 40 ℃ after the reaction is finished, filtering by using a 200-mesh filter screen, and bottling.
Example 2
A copolymer emulsion of fluorine-carbon water-proof and oil-proof agent contains the following components by mass percent,
the polymerization method comprises the following steps,
step 1, preparing a pre-emulsion from raw materials (1.5 g of octadecyl trimethyl ammonium chloride, 1.2g of Tween 40, 4.8g of lauryl polyoxyethylene ether 30, 2.4g of polyoxyethylene dioleate, 0.3g of dodecyl mercaptan, 24g of octadecyl acrylate, 18g of octadecyl chloroacrylate, 42g of perfluorohexylethyl methacrylate, 0.3g of lauryl methacrylate, 3g of methyl methacrylate, 1.5g of N-hydroxymethyl acrylamide, 21g of dipropylene glycol methyl ether, 2.1g of glacial acetic acid and 150g of deionized water) in a formula, placing the pre-emulsion in a water bath at 60 ℃, stirring (300 revolutions per minute) and preserving heat for 30 minutes;
step 2, homogenizing the pre-emulsion for three times by using a high-pressure homogenizer or an ultrasonic homogenizer (cooling by using cold water at the temperature of 20 ℃ during homogenization);
and 3, pouring the homogenized pre-emulsion into a reactor with a thermometer, a stirrer, a condenser pipe and a protective gas through pipe, setting the temperature in the reactor to be 70 ℃, introducing nitrogen N2 for three minutes at the stirrer rotating speed of 100 revolutions per minute, stopping introducing the nitrogen, increasing the stirrer rotating speed to 200 revolutions per minute, slowly dropwise adding 1.2g of initiator aqueous solution (2, 2' -azobis (2-aminopropane) dihydrochloride dissolved in 15.8g of deionized water) when the thermometer reaches 58 ℃, and completing dripping within half an hour. Continuously dropwise adding a hydroxypropyl acrylate aqueous solution (0.9 g of hydroxypropyl acrylate is dissolved in 10g of deionized water and the dropping is finished within two hours) after the initiator is dropped;
and 4, maintaining the water bath at 72 ℃ until the reaction is finished (the total time from the beginning of the initiator dropwise addition to the end of the reaction is maintained at 5 hours, cooling to below 40 ℃ after the reaction is finished, filtering (a 200-mesh filter screen), and bottling.
Example 3
A copolymer emulsion of fluorine-carbon water-proof and oil-proof agent contains the following components by mass percent,
the polymerization method comprises the following steps,
step 1, preparing a pre-emulsion from raw materials (1.5 g of octadecyl trimethyl ammonium chloride, 1.2g of Tween 40, 4.8g of lauryl polyoxyethylene ether 30, 2.4g of polyoxyethylene dioleate, 0.3g of dodecyl mercaptan, 30g of octadecyl acrylate, 12g of octadecyl chloroacrylate, 42g of perfluorohexylethyl methacrylate, 0.3g of lauryl methacrylate, 3g of methyl methacrylate, 1.5g of N-hydroxymethyl acrylamide, 21g of dipropylene glycol methyl ether, 2.1g of glacial acetic acid and 150g of deionized water) in a formula, placing the pre-emulsion in a water bath at the temperature, stirring (300 revolutions per minute) and preserving heat for 30 minutes;
step 2, homogenizing the sheared pre-emulsion for three times by using a high-pressure homogenizer or an ultrasonic homogenizer, and cooling by using cold water at the temperature of 20 ℃ during homogenization;
step 3, pouring the homogenized pre-emulsion into a reactor with a thermometer, a stirrer, a condenser pipe and a protective gas through pipe, setting the temperature in the reactor to be 70 ℃, introducing nitrogen N into the reactor at the rotating speed of the stirrer according to 100 revolutions per minute2After three minutes, the aeration was stopped, the stirrer speed was increased to 200 rpm, and an aqueous initiator solution (1.2 g of 2, 2' -azobis (2-aminopropane) dihydrochloride dissolved in 15.8g of deionized water) was slowly added dropwise over half an hour after the temperature reached 58 ℃. Continuously dropwise adding a hydroxypropyl acrylate aqueous solution (0.9 g of hydroxypropyl acrylate is dissolved in 10g of deionized water and the dropping is finished within two hours) after the initiator is dropped;
and 4, maintaining the water bath at 72 ℃ until the reaction is finished (the total time from the beginning of the initiator dropwise addition to the end of the reaction is maintained at 5 hours, cooling to below 40 ℃ after the reaction is finished, filtering (a 200-mesh filter screen), and bottling.
Comparative example:
the prior art product comprises the following components,
the polymerization method is as follows,
step 1, preparing a pre-emulsion from raw materials (1.5 g of octadecyl trimethyl ammonium chloride, 1.2g of Tween 40, 4.8g of lauryl polyoxyethylene ether 30, 2.4g of polyoxyethylene dioleate, 0.3g of dodecyl mercaptan, 42g of octadecyl acrylate, 42g of perfluorohexyl ethyl methacrylate, 0.3g of lauryl methacrylate, 3g of methyl methacrylate, 1.5g of N-hydroxymethyl acrylamide, 21g of dipropylene glycol methyl ether, 2.1g of glacial acetic acid and 150g of deionized water) in a formula, placing the pre-emulsion in a water bath at 60 ℃, stirring (300 revolutions per minute) and keeping the temperature for 30 minutes;
step 2, homogenizing the sheared pre-emulsion for three times by using a high-pressure homogenizer or an ultrasonic homogenizer;
step 3, homogenizing the pre-emulsionPouring into a reactor with a thermometer, a stirrer, a condenser pipe and a protective gas through pipe, setting the temperature in the reactor at 70 ℃, and introducing nitrogen N into the reactor at the rotating speed of the stirrer of 100 revolutions per minute2After three minutes, the aeration was stopped, the stirrer speed was increased to 200 rpm, and an aqueous initiator solution (1.2 g of 2, 2' -azobis (2-aminopropane) dihydrochloride dissolved in 15.8g of deionized water) was slowly added dropwise over half an hour after the temperature reached 58 ℃. Continuously dropwise adding a hydroxypropyl acrylate aqueous solution (0.9 g of hydroxypropyl acrylate is dissolved in 10g of deionized water and the dropping is finished within two hours) after the initiator is dropped;
and 4, maintaining the water bath at 72 ℃ until the reaction is finished (the total time from the beginning of the initiator dropwise addition to the end of the reaction is maintained at 5 hours, cooling to below 40 ℃ after the reaction is finished, filtering (a 200-mesh filter screen), and bottling.
The experimental control table is as follows:
| example 1 | Example 2 | Example 3 | Comparative example 1 | |
| Water-proof property after 0 time washing | 100 | 90+ | 90+ | 90 |
| 0-time washing oil repellency | 5 | 5 | 5 | 5 |
| Water-proof performance after 5 times of washing | 90 | 80+ | 80+ | 70+ |
| 5-time washing oil repellency | 4 | 4 | 4 | 3 |
The method for comparing the performances of the water-proof and oil-proof agent comprises the following steps:
diluting the above prepared water-and oil-repellent agent sample with 5% water to obtain a treatment solution, and collecting 130g/M2After the polyester cotton fabric with gram weight is soaked (the liquid absorption rate is controlled to be 50-60%), and after the polyester cotton fabric is dried (the drying condition is that the polyester cotton fabric is baked for 100 seconds at 180 ℃), the water resistance and the oil resistance of the fabric are tested according to the following standards.
And (4) testing standard: waterproof AATCC-22
Oil-proof AATCC-118
Washing with water standard AATCC-135.
Therefore, on the basis of the traditional fabric waterproof and oil-proof agent (perfluoroalkyl ethyl acrylate (methyl) copolymer emulsion), a part of long-chain acrylic ester is replaced by long-chain chloroacrylic ester to synthesize a novel chlorine-containing fluorocarbon waterproof and oil-proof agent copolymer emulsion, the chlorine-containing fluorocarbon waterproof and oil-proof agent copolymer emulsion utilizes the characteristic of strong electronegativity of chlorine-containing groups to improve the adsorption of a waterproof agent to the fabric and improve the waterproof effect and the water washing resistance, the long-chain chloroacrylic ester has little influence on the waterproof and oil-proof effects relative to short-chain polyethylene, and toxic substances such as pressurized vinyl chloride are not needed in the reaction process, so that the chlorine-containing fluorocarbon waterproof and oil-proof agent copolymer emulsion is a safer normal-pressure emulsion polymerization reaction.
The foregoing is illustrative of the preferred embodiments of the present invention only and is not to be construed as limiting the claims. All equivalent process changes made by the present specification are included in the scope of the present invention.
Claims (7)
1. A copolymer emulsion of fluorine-containing fluorocarbon water and oil proofing agent is characterized in that: which comprises the following components in percentage by weight,
the emulsifier consists of four to six surfactants with different hydrophilic-lipophilic balance values;
at least one of a polymerized monomer, perfluoroalkyl ethyl acrylate (methyl), perfluoro octyl ethyl acrylate, perfluoro octyl methyl ethyl acrylate, perfluoro hexyl ethyl acrylate and perfluoro hexyl methyl ethyl acrylate;
from the general formula CH2＝CCl(C＝O)-O-CnH2n+1Chloroacrylates of formula (I) wherein n is 12, 14, 16, 18, 20, 22;
at least one of a functional monomer, octadecyl acrylate, octadecyl methacrylate, hexadecyl acrylate, hexadecyl methacrylate, docosyl acrylate, docosyl methacrylate, lauryl acrylate, lauryl methacrylate, hydroxyethyl acrylate, hydroxymethyl acrylamide, hydroxypropyl acrylate, hydroxybutyl acrylate, hydroxypropyl methacrylate, hydroxybutyl methacrylate, N-isobutoxy acrylamide, N-methylolacrylamide, hydroxyoctyl acrylate, isocyanato acrylate, acetoacetoxyethyl methacrylate, glycidyl methacrylate;
initiator, 2, 2' -azobis (2-aminopropane) dihydrochloride;
cosolvent, at least one of tripropylene glycol TPG, propylene glycol methyl ether PM, dipropylene glycol methyl ether DPM, polyethylene glycol PEG, dipropylene glycol DPG and diethylene glycol methyl ether DEM;
at least one of a chain transfer agent, dodecyl mercaptan and octyl mercaptan;
pH value regulator: at least one of acetic acid, citric acid and nitric acid.
2. A chlorine-containing fluorocarbon water and oil repellent copolymer emulsion as set forth in claim 1, characterized in that: the composite material comprises the following components in percentage by mass,
3. a chlorine-containing fluorocarbon water and oil repellent copolymer emulsion as set forth in claim 1, characterized in that: the composite material comprises the following components in percentage by mass,
4. a chlorine-containing fluorocarbon water and oil repellent copolymer emulsion as set forth in claim 1, characterized in that: the composite material comprises the following components in percentage by mass,
5. a polymerization method of copolymer emulsion containing chlorine fluorocarbon waterproof and oil-proof agent is characterized in that: comprises the following steps of (a) carrying out,
step 1, preparing a liquid, namely preparing a pre-emulsion from components except an initiator and dilution water of the initiator in a formula according to a proportion, placing the pre-emulsion in a water bath at 60 ℃, and stirring and preserving heat for 30 minutes at 300 revolutions per minute;
step 2, homogenizing the pre-emulsion for three times by using a high-pressure homogenizer or an ultrasonic homogenizer;
step 3, pouring the homogenized pre-emulsion into a reactor with a thermometer, a stirrer, a condenser pipe and a protective gas through pipe, setting the temperature in the reactor to be 60-75 ℃, introducing nitrogen N into the reactor at the rotating speed of the stirrer according to 100 revolutions per minute2Stopping introducing air after three minutes, increasing the rotating speed of the stirrer to 200 revolutions per minute, slowly dripping 5 percent aqueous solution of the initiator when the temperature of the thermometer reaches 58 ℃, and finishing dripping within half an hour;
and 4, maintaining the temperature of 60-75 ℃, adding an initiator until the reaction is finished, then cooling, filtering and bottling.
6. The polymerization method of copolymer emulsion containing chlorine-containing fluorocarbon water and oil repellent according to claim 5, characterized in that: if the water-soluble monomer is contained in the components of the copolymer emulsion of the fluorocarbon water-and oil-repellent agent containing chlorine, the water-soluble monomer and the dilution water for diluting the water-soluble monomer are removed in addition to the initiator and the dilution water for diluting the initiator when the solution is prepared in the step 1, and the aqueous solution of the water-soluble monomer is continuously dripped after the half hour after the initiator is dripped, wherein the concentration is 10-20 percent and the dripping is finished for two hours.
7. The polymerization method of copolymer emulsion containing chlorine-containing fluorocarbon water and oil repellent according to claim 2, characterized in that: comprises the following steps of (a) carrying out,
step 1, preparing a pre-emulsion from 1.5g of octadecyl trimethyl ammonium chloride, 1.2g of Tween 40, 4.8g of lauryl polyoxyethylene ether 30, 2.4g of polyoxyethylene dioleate, 0.3g of dodecyl mercaptan, 18g of octadecyl acrylate, 24g of octadecyl chloroacrylate, 42g of perfluorohexylethyl methacrylate, 0.3g of lauryl methacrylate, 3g of methyl methacrylate, 1.5g of N-hydroxymethyl acrylamide, 21g of dipropylene glycol methyl ether, 2.1g of glacial acetic acid and 150g of deionized water, placing the pre-emulsion in a water bath at the temperature of 60 ℃, and stirring and preserving heat for 30 minutes at 300 revolutions per minute;
step 2, homogenizing the pre-emulsion for three times by using a high-pressure homogenizer or an ultrasonic homogenizer, and cooling by using cold water at the temperature of 20 ℃ during homogenization;
step 3, pouring the homogenized pre-emulsion into a reactor with a thermometer, a stirrer, a condenser pipe and a protective gas through pipe, setting the temperature in the reactor to be 70 ℃, introducing nitrogen N into the reactor at the rotating speed of the stirrer according to 100 revolutions per minute2Stopping ventilation after three minutes, increasing the rotating speed of the stirrer to 200 revolutions per minute, slowly dripping 1.2g of (2, 2' -azobis (2-aminopropane) dihydrochloride into an initiator aqueous solution prepared by dissolving 15.8g of deionized water when the thermometer reaches 58 ℃, finishing dripping within half an hour, continuously dripping 0.9g of hydroxypropyl acrylate aqueous solution prepared by dissolving 10g of deionized water after the initiator is dripped, and finishing dripping within two hours;
and 4, maintaining the water bath at 72 ℃ until the reaction is finished, cooling to below 40 ℃ after the reaction is finished, filtering by using a 200-mesh filter screen, and bottling.
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