CN113980179A - Modified water-based hydroxyl acrylic acid dispersoid and synthesis process thereof - Google Patents

Modified water-based hydroxyl acrylic acid dispersoid and synthesis process thereof Download PDF

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CN113980179A
CN113980179A CN202111205043.XA CN202111205043A CN113980179A CN 113980179 A CN113980179 A CN 113980179A CN 202111205043 A CN202111205043 A CN 202111205043A CN 113980179 A CN113980179 A CN 113980179A
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徐九华
蔡军
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Guanghan Costino New Material Technology Co ltd
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    • C08F230/04Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
    • C08F230/08Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
    • C08F230/085Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon the monomer being a polymerisable silane, e.g. (meth)acryloyloxy trialkoxy silanes or vinyl trialkoxysilanes
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Abstract

The invention provides a synthesis process of a modified aqueous hydroxyl acrylic acid dispersion, which comprises the following steps: (1) putting glycidyl methacrylate and hydroxysilane into a reaction kettle, heating to 60-80 ℃, preserving heat for 2-5 hours, and cooling to normal temperature to obtain an intermediate product; (2) uniformly stirring the intermediate product soft monomer, hard monomer, functional monomer, chain transfer agent and initiator obtained in the step (1) to obtain a mixed monomer; (3) adding an organic solvent into a reaction kettle, heating to 100-150 ℃, slowly dripping a mixed monomer, preserving heat, supplementing an initiator and then cooling; (4) cooling to 78-82 ℃, adding a neutralizing agent, stirring, adding water, and dispersing at high speed to obtain the modified water-based hydroxyl acrylic acid dispersoid. The process can increase the dosage of the hydroxyl silane, thereby improving the performance of the paint prepared from the aqueous hydroxyl acrylic acid dispersoid, and simultaneously, no gel appears in the synthesis process.

Description

Modified water-based hydroxyl acrylic acid dispersoid and synthesis process thereof
Technical Field
The invention belongs to the technical field of synthetic resin materials, and particularly relates to a modified aqueous hydroxy acrylic acid dispersoid and a synthesis process thereof.
Background
The water-based acrylic resin is an important resin for the coating, has simple process, multiple varieties, large formula change, convenient chemical modification and better performance; the paint made of the paint has the characteristics of good application property, good dryness and the like, and is widely applied to decoration and protection of steel structures, woodware, glass and the like. Compared with solvent-based acrylic resin, the water-based acrylic resin is totally or mostly diluted by water, has the characteristics of low VOC content, safety, environmental protection and safe transportation and construction, and is gradually replacing the solvent-based acrylic resin.
The wine bottle paint is used for decorating wine bottle glass, basically used for storing wine, has requirements on decoration effect and chemical resistance and water resistance, and is generally baked at high temperature to meet the required resistance requirement, wherein the baking temperature is generally 130-150 ℃, and the baking temperature is partially 170-190 ℃. In addition, the wine bottle paint has various colors, and a large part of the wine bottle paint is white, and the wine bottle paint is still gorgeous in color after being baked, namely, the wine bottle paint is required to have high gloss and no yellowing after being baked.
However, the paint prepared from the traditional water-based acrylic resin has poor alcohol resistance and water resistance of a coating film, is easy to fade after being baked at high temperature, and is easy to yellow particularly in white paint.
The organic silicon resin contains a large amount of Si-O-Si bonds, so that the bond energy is stable, the organic silicon resin is not easy to decompose at high temperature, and the organic silicon resin has good light and color retention and does not fade at high temperature. In order to improve the problems of the paint prepared from the water-based acrylic resin, the paint is prepared by modifying the water-based acrylic resin with organic silicon in the prior art, so that the performance is improved.
Disclosure of Invention
In the research of the organic silicon modified water-based acrylic resin, the invention discovers that the performance can be improved by introducing the organic silicon modification, but the invention also has the following problems: when the inventor expects to introduce more organosilicon modifier for modification to further improve the performance of the paint, climbing rod occurs in the synthesis process, and a large amount of gel particles occur in the filtered material, so that the quality of the synthesized waterborne hydroxy acrylic acid dispersoid is unqualified, and the possibility of further improving the performance of the paint by organosilicon modified waterborne acrylic resin is limited.
In order to solve the problems, the invention provides a synthesis process of a modified aqueous hydroxy acrylic acid dispersion, which is different from the prior art, the process adopts a method different from the prior art to introduce hydroxy silane, the method can improve the use amount of the hydroxy silane to further improve the performance of a paint prepared by improving the aqueous hydroxy acrylic acid dispersion, simultaneously, no gel appears in the synthesis process, the dispersion with guaranteed quality is synthesized, the problems of high-temperature yellowing, insufficient alcohol resistance and water resistance of glass wine bottle baking varnish can be better solved, the cost is low, and the process is simple.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the invention provides a synthesis process of a modified aqueous hydroxyl acrylic acid dispersion, which comprises the following steps:
(1) putting glycidyl methacrylate and hydroxysilane into a reaction kettle, heating to 60-80 ℃, continuously preserving heat for 2-5 hours, and cooling to normal temperature to obtain an intermediate product; in the step, boron trifluoride-diethyl ether solution is used as a catalyst to catalyze the ring opening of glycidyl methacrylate, and hydroxyl silane is grafted to the molecular chain of the glycidyl methacrylate after the ring opening;
(2) adding the intermediate product obtained in the step (1) into a monomer containing a soft monomer, a hard monomer, a functional monomer, a chain transfer agent and an initiator, and uniformly stirring to obtain a mixed monomer;
(3) adding an organic solvent into a reaction kettle, heating to 100-150 ℃, slowly dropwise adding a mixed monomer, finishing adding after about 3-8 hours, preserving heat for 1 hour, supplementing an initiator, preserving heat for 1 hour, supplementing the initiator again, preserving heat for 2 hours, and then cooling;
(4) cooling to 78-82 ℃, adding a neutralizing agent, stirring for 28-33min, and adding water for high-speed dispersion to obtain the modified aqueous hydroxyl acrylic acid dispersoid.
The structural formula of the glycidyl methacrylate is shown as the following formula (1)
Figure BDA0003306560530000021
The structural formula of the hydroxysilane is shown as the following formula (2):
Figure BDA0003306560530000022
Figure BDA0003306560530000023
wherein n is 4, R is (CH2)3, and R1 is (CH2) 4.
The organic silicon monomer adopted by the prior art contains double bonds, has high activity and instability, and is easy to cause gelation (a large amount of gel particles are formed in the synthesis) due to a large introduction amount, so that the synthesized water-based acrylic acid dispersion resin is unqualified; and the price of the organosilicon monomer is expensive; the hydroxyl silane of the invention is different from the organic silicon monomer in the prior art, does not contain double bonds, can improve the use amount to further improve the performance of the aqueous hydroxyl acrylic acid dispersoid, and does not generate gelation in the synthesis process.
Further, in the step (2), the soft monomer is one or more of butyl acrylate, isooctyl acrylate and laurate acrylate.
Further, in the step (2), the hard monomer is one or more of styrene, methyl methacrylate, isobornyl acrylate and the like.
Further, in the step (2), the functional monomer is one or more of acrylic acid, methacrylic acid, hydroxypropyl acrylate, hydroxyethyl methacrylate and hydroxyethyl acrylate.
Further, in the step (2), the chain transfer agent is one or two of dodecyl mercaptan and mercaptoethanol.
In the step (3), the organic solvent is one or more of ethylene glycol butyl ether, propylene glycol propyl ether, propylene glycol butyl ether, diethylene glycol dimethyl ether and diethylene glycol butyl ether;
further, in the step (3), the initiator is one or more of benzoyl peroxide, tert-butyl peroxybenzoate and isopropyl hydroperoxide.
Further, in the step (3), the neutralizing agent is dimethylethanolamine.
The modified aqueous hydroxy acrylic acid dispersion comprises the following components in parts by weight: 115 parts of glycidyl methacrylate 104-.
The paint of the invention can be prepared according to the following formula, wherein the paint comprises the following components in parts by weight: 55 parts of modified aqueous hydroxy acrylic acid dispersoid and 10 parts of diethylene glycol butyl ether; 0.4 part of dimethylethanolamine; 10 parts of amino resin; 45 parts of titanium white paste; 0.2 part of defoaming agent; 4 parts of a dispersing agent; 0.3 part of anti-settling agent; 24.4 parts of water; can also be prepared according to the conventional formula.
The present invention has the following effects
Compared with the prior art, the method can further improve the performance of the paint prepared from the same aqueous hydroxyl acrylic acid dispersoid, particularly baking the paint in a wine bottle paint at 190 ℃ for 60 minutes, wherein the color difference is delta E (0.1), and the alcohol resistance is more than 3 hours, and the phenomenon of gelation can not occur when the modified aqueous hydroxyl acrylic acid dispersoid is synthesized by adopting the synthesis process, thereby effectively overcoming the problem that the performance of the paint prepared from the aqueous hydroxyl acrylic acid dispersoid can not be further improved by adopting the prior art through modification.
Practice proves that the modified water-based hydroxyl acrylic acid dispersoid coating film obtained by the process has good alcohol resistance and water resistance, high gloss, good heat resistance and yellowing resistance and good adhesive force.
Detailed Description
In order to better carry out the invention, the invention is illustrated in detail by the following examples.
Example 1
A synthesis process of an organosilicon modified waterborne hydroxyl acrylic dispersion comprises the following steps:
(1) putting 113g of glycidyl methacrylate and 150g of hydroxysilane into a reaction kettle, heating to 75 ℃, slowly dripping 3g of boron trifluoride-diethyl ether solution, continuously preserving the temperature for 2-5 hours, and cooling to normal temperature to obtain an intermediate product;
(2) adding the intermediate product in the step (1) into monomers containing 100g of soft monomer (60 g of butyl acrylate, 40g of lauryl methacrylate), 180g of hard monomer (110 g of methyl methacrylate and 70g of isobornyl methacrylate), 68g of functional monomer (20 g of acrylic acid, 18g of hydroxyethyl methacrylate and 30g of hydroxyethyl acrylate), 12g of chain transfer agent (dodecyl mercaptan) and 30g of initiator (benzoyl peroxide) and uniformly stirring to obtain a mixed monomer;
(3) adding 125g of organic solvent (60 g of ethylene glycol butyl ether and 65g of diethylene glycol dimethyl ether) into a reaction kettle, heating to 130 ℃, slowly dropwise adding the mixed monomer, finishing adding after about 3-4 hours, preserving heat for 1 hour, supplementing 3g of initiator (benzoyl peroxide) again, preserving heat for 2 hours, and then cooling;
(4) and cooling to 78 ℃, adding 20g of neutralizing agent dimethylethanolamine, stirring for 30min, slowly adding 630g of purified water, and dispersing at a high speed to obtain the modified aqueous hydroxyacrylic acid dispersion.
In this example, the hydroxysilane content was 24% of the solids.
Example 2
A synthesis process of an organosilicon modified waterborne hydroxyl acrylic acid dispersoid comprises the following process steps:
(1) putting 104g of glycidyl methacrylate and 152g of hydroxysilane into a reaction kettle, heating to 70 ℃, slowly dropping 2.8g of boron trifluoride-diethyl ether solution, continuously preserving the temperature for 2-5 hours, and cooling to normal temperature to obtain an intermediate product I;
(2) adding the intermediate product (i) in the step (1) into monomers containing 120g of soft monomer (60 g of butyl acrylate and 60g of methacrylic laurate), 160 g of hard monomer (95 g of methyl methacrylate and 65g of styrene), 80g of functional monomer (25 g of methacrylic acid, 25g of hydroxyethyl methacrylate and 30g of hydroxypropyl acrylate), 12g of chain transfer agent (dodecyl mercaptan) and 35g of initiator (benzoyl peroxide) and uniformly stirring to obtain a mixed monomer;
(3) adding 125g of organic solvent (60 g of diethylene glycol butyl ether and 65g of diethylene glycol dimethyl ether) into a reaction kettle, heating to 135 ℃, slowly dropwise adding the mixed monomer, finishing adding after about 3-4 hours, preserving heat for 1 hour, supplementing 3g of initiator (benzoyl peroxide) again, preserving heat for 2 hours, and then cooling;
(4) cooling to 80 ℃, adding 25g of neutralizing agent dimethylethanolamine, stirring for 28min, slowly adding 625g of purified water, and dispersing at high speed to obtain the modified aqueous hydroxyacrylic acid dispersoid.
In this example, the silane content was 24.2% of the solids.
Example 3
The process of preparing organosilicon modified water-thinned hydroxy acrylic acid dispersion includes the following steps:
1) putting 115g of glycidyl methacrylate and 153g of hydroxysilane into a reaction kettle, heating to 80 ℃, slowly dropping 3g of boron trifluoride-diethyl ether solution, continuously preserving heat for 2-5 hours, and cooling to normal temperature to obtain an intermediate product;
(2) adding the intermediate product in the step (1) into monomers containing 80g of soft monomer (35 g of isooctyl acrylate, 45g of lauryl methacrylate), 180g of hard monomer (150 g of methyl methacrylate, 30g of isobornyl methacrylate), 100g of functional monomer (28 g of acrylic acid, 22g of hydroxyethyl methacrylate and 50g of hydroxyethyl acrylate), 16g of chain transfer agent (dodecyl mercaptan) and 34g of initiator (tert-butyl peroxybenzoate) and uniformly stirring to obtain a mixed monomer;
(3) adding 140g of organic solvent (60 g of propylene glycol butyl ether and 80g of propylene glycol propyl ether) into a reaction kettle, heating to 140 ℃, slowly dropwise adding the mixed monomer, finishing adding after about 3-4 hours, preserving heat for 1 hour, supplementing 3g of initiator (tert-butyl peroxybenzoate) again, preserving heat for 2 hours, cooling, and supplementing
(4) And cooling to 82 ℃, adding 28g of neutralizing agent, stirring for 33min, slowly adding 650g of purified water, and dispersing at a high speed to obtain the modified aqueous hydroxy acrylic acid dispersoid.
In this example, the silane content was 23.7% of the solids.
Example 4
An organosilicon modified water-based hydroxyl acrylic acid dispersoid and a preparation method thereof are disclosed, wherein the preparation process comprises the following steps:
(1) putting 106g of glycidyl methacrylate and 155g of hydroxysilane into a reaction kettle, heating to 75 ℃, slowly dropping 2.9g of boron trifluoride-diethyl ether solution, continuously preserving the heat for 2-5 hours, and cooling to normal temperature to obtain an intermediate product;
(2) adding the intermediate product in the step (1) into a monomer containing 115g of soft monomer (80 g of butyl acrylate and 35g of isooctyl acrylate), 200g of hard monomer (100 g of methyl methacrylate, 70g of styrene and 30g of isobornyl methacrylate), 60g of functional monomer (20 g of acrylic acid and 40g of hydroxypropyl acrylate), 20g of chain transfer agent (dodecyl mercaptan) and 40g of initiator (18g of benzoyl peroxide and 22g of tert-butyl peroxybenzoate) and uniformly stirring to obtain a mixed monomer;
(3) adding 145g of organic solvent (65 g of ethylene glycol butyl ether and 80g of diethylene glycol butyl ether) into a reaction kettle, heating to 128 ℃, slowly dropwise adding the mixed monomer, finishing adding after about 3-4 hours, preserving heat for 1 hour, supplementing 3g of initiator (tert-butyl peroxybenzoate) again, preserving heat for 2 hours, and then cooling;
(4) cooling to 80 ℃, adding 20g of neutralizing agent, stirring for half an hour, slowly adding 640g of purified water, and dispersing at high speed to obtain the modified aqueous hydroxyl acrylic acid dispersoid.
In this example, the silane content was 23.6% of the solids.
Comparative example 1
The present invention provides a conventional acrylate dispersion synthesized by this company as comparative example 1, which was prepared as follows:
firstly, adding 130 parts of butyl cellosolve serving as a bottoming solvent into a reaction kettle, and heating to 125-130 ℃;
adding 75 parts of butyl acrylate monomer, 45 parts of isooctyl acrylate, 95 parts of methyl methacrylate, 120 parts of styrene, 105 parts of hydroxypropyl acrylate, 20 parts of acrylic acid, 10 parts of dodecyl mercaptan, 9 parts of benzoyl peroxide and 16 parts of tert-butyl peroxybenzoate into a dropping tank, stirring and uniformly mixing;
thirdly, when the temperature of the reaction kettle reaches 125-130 ℃, dropwise adding the mixed material obtained in the step II, dropwise adding the mixed material within 3-4 hours, preserving heat for 1 hour after dropwise adding, supplementing 1.5 parts of tert-butyl peroxybenzoate, continuously preserving heat for 1 hour, supplementing 1 part of tert-butyl peroxybenzoate, and continuously preserving heat for 2 hours;
and fourthly, after the heat preservation is finished, cooling to 80 ℃, adding 22 parts of dimethyl ethanolamine serving as a neutralizing agent, stirring for half an hour to increase the stirring speed and slowly adding 550 parts of deionized water, after the dispersion is finished, continuing stirring for half an hour, reducing the stirring speed and cooling, filtering and discharging to obtain the water-based acrylic acid dispersoid resin.
Comparative example 2
The invention provides an acrylate dispersion prepared by using a conventional silane monomer, which is synthesized by the company, wherein the organosilicon used is KH570(3- (methacryloyloxy) propyl trimethoxy silane), and the preparation process is as follows:
adding 150 portions of butyl cellosolve serving as a priming solvent into a reaction kettle, heating the solution to 125-130 DEG C
Adding 75 parts of butyl acrylate monomer, 45 parts of isooctyl acrylate, 95 parts of methyl methacrylate, 120 parts of styrene, 105 parts of hydroxypropyl acrylate, 20 parts of acrylic acid, 50 parts of KH570(3- (methacryloyloxy) propyl trimethoxy silane), 10 parts of dodecyl mercaptan, 9 parts of benzoyl peroxide and 16 parts of tert-butyl peroxybenzoate into a dripping tank, stirring and uniformly stirring to obtain a mixed monomer;
thirdly, when the temperature of the reaction kettle reaches 125-130 ℃, the mixed monomer obtained in the second step is dripped in 3-4 hours, the temperature is kept for 1 hour after dripping, 1.5 parts of tert-butyl peroxybenzoate is added, the temperature is kept for 1 hour, 1 part of tert-butyl peroxybenzoate is added again, and the temperature is kept for 2 hours;
and fourthly, after the heat preservation is finished, cooling to 80 ℃, adding 22 parts of dimethyl ethanolamine serving as a neutralizing agent, stirring for half an hour to increase the stirring speed and slowly adding 670 parts of deionized water, after the dispersion is finished, continuing stirring for half an hour, reducing the stirring speed and cooling, filtering and discharging to obtain the water-based acrylic acid dispersoid resin.
The silane content in this comparative example was 9.6% of the solids.
Comparative example 3
The comparative example, which is a prior art dispersion prepared, increases the amount of silicone based on comparative example 2, and the process is as follows:
190 portions of butyl cellosolve serving as a priming solvent are put into a reaction kettle and heated to 125-130 DEG C
Adding 75 parts of monomer butyl acrylate, 35 parts of isooctyl acrylate, 110 parts of methyl methacrylate, 90 parts of styrene, 95 parts of hydroxypropyl acrylate, 20 parts of acrylic acid, 80 parts of KH570(3- (methacryloyloxy) propyl trimethoxy silane), 10 parts of dodecyl mercaptan, 9 parts of benzoyl peroxide and 16 parts of tert-butyl peroxybenzoate into a dropping tank, stirring and uniformly stirring to obtain a mixed monomer;
thirdly, when the temperature of the reaction kettle reaches 125-130 ℃, the mixed monomer obtained in the second step is dripped in 3 to 4 hours, the temperature is kept for 1 hour after the dripping, 1.5 parts of tert-butyl peroxybenzoate is added, the temperature is kept for 1 hour, 1 part of tert-butyl peroxybenzoate is added, the temperature is kept for 2 hours
And fourthly, after the heat preservation is finished, cooling to 80 ℃, adding 22 parts of dimethyl ethanolamine serving as a neutralizing agent, stirring for half an hour to increase the stirring speed and slowly adding 630 parts of deionized water, after the dispersion is finished, continuing stirring for half an hour, reducing the stirring speed and cooling, filtering, and discharging to obtain the water-based acrylic acid dispersoid resin.
In this comparative example, it was found that there was a slight gel-climbing phenomenon during the reaction and a large amount of gel particles after filtration. Therefore, in the prior art, after the usage amount of organic silicon is increased, a gel phenomenon occurs, a large number of gel particles are filtered, and the quality of the synthesized aqueous acrylic acid dispersion resin cannot be guaranteed.
The silane content in this comparative example 3 was 15.5% of the solids.
Comparative example 4
The comparative example increases the dosage of the organic silicon on the basis of the comparative example 3, and the process flow is as follows:
190 portions of butyl cellosolve serving as a priming solvent are put into a reaction kettle and heated to 125-130 DEG C
Adding 75 parts of monomer butyl acrylate, 35 parts of isooctyl acrylate, 110 parts of methyl methacrylate, 90 parts of styrene, 95 parts of hydroxypropyl acrylate, 20 parts of acrylic acid, 120 parts of KH570(3- (methacryloyloxy) propyl trimethoxy silane), 10 parts of dodecyl mercaptan, 9 parts of benzoyl peroxide and 16 parts of tert-butyl peroxybenzoate into a dropping tank, stirring and uniformly stirring to obtain a mixed monomer;
thirdly, when the temperature of the reaction kettle reaches 125-130 ℃, the mixed monomer obtained in the second step is dripped in 3-4 hours, the temperature is kept for 1 hour after dripping, 1.5 parts of tert-butyl peroxybenzoate is added, the temperature is kept for 1 hour, 1 part of tert-butyl peroxybenzoate is added, and the temperature is kept for 2 hours;
fourthly, after the heat preservation is finished, the temperature is reduced, the viscosity is high, the resin is gelatinized by climbing a rod and is difficult to stir, and the resin cannot be stirred gradually along with the reduction of the temperature and is poured out.
In this comparative example, it was found that the gelling was severe during the reaction. Therefore, the subsequent neutralization and dispersion processes cannot be carried out after the dosage of the organic silicon is increased in the prior art. This comparative example, the silane content was 21% of the solids.
As can be seen from comparative examples 2-4, in the prior art organosilicon modified acrylic acid process, the product performance is not significantly improved by increasing the amount of organosilicon to about 15%, gelation also occurs, and the process cannot be synthesized when the amount is about 20%.
55 parts of the aqueous hydroxy acrylic acid dispersoid prepared in the examples 1 to 4 and the comparative examples 1 to 3 are added into the components in the paint preparation proportioning table in the following table 1 to respectively prepare paint samples 1 to 7, the paint samples are sprayed on a glass wine bottle, the glass wine bottle is put into an oven after being dried, and the glass wine bottle is baked at 190 ℃ for 20 minutes and then taken out. After cooling, testing related indexes according to national standards or industry experience; the test results are shown in Table 2, and it can be seen from the test results that the aqueous organosilicon modified acrylic dispersion prepared has good alcohol resistance and water resistance, high gloss, good heat resistance and yellowing resistance, and good adhesion.
TABLE 1 paint compounding ratio table
Figure BDA0003306560530000081
Figure BDA0003306560530000091
TABLE 2 test results of examples and comparative examples
Figure BDA0003306560530000092
As can be seen from the results in Table 2 in examples 1-4 and comparative examples 1-4, the process for preparing the waterborne hydroxyacrylic acid dispersion by the process modification of the invention is reliable, the dosage of the hydroxysilane is 23-24.5%, the color difference of the wine bottle paint prepared from the dispersion is kept at 0.1 as delta E, the alcohol resistance is more than 3 hours, and no gelation occurs. Compared with the prior art, the lifting device has larger lifting.

Claims (10)

1. A synthetic process of a modified aqueous hydroxy acrylic acid dispersoid is characterized in that: the method comprises the following steps:
(1) preparing a matrix: putting glycidyl methacrylate and hydroxysilane into a reaction kettle, heating to 60-80 ℃, continuously preserving heat for 2-5 hours, and cooling to obtain an intermediate product;
(2) mixing monomers: adding the intermediate product obtained in the step (1) into a monomer containing a soft monomer, a hard monomer, a functional monomer, a chain transfer agent and an initiator, and uniformly stirring to obtain a mixed monomer;
(3) dropwise addition polymerization: adding an organic solvent into a reaction kettle, heating to 100-150 ℃, slowly dropwise adding the mixed monomer, completing the addition within about 3-4 hours, then carrying out heat preservation, adding an initiator, carrying out heat preservation and then cooling;
(4) neutralization and dispersion: cooling to 78-82 ℃, adding a neutralizing agent, stirring for 28-33min, adding water, and dispersing at high speed to obtain the organic silicon modified water-based hydroxyl acrylic acid dispersoid.
2. The process of claim 1 for the synthesis of a modified aqueous hydroxyacrylic dispersion, characterized in that: the structural formula of the glycidyl methacrylate is shown as the following formula (1)
Figure FDA0003306560520000011
The structural formula of the hydroxyl silane is shown as the following formula (2),
Figure FDA0003306560520000012
wherein n is 4, R is (CH2)3, and R1 is (CH2) 4.
3. The process of claim 1 for the synthesis of a modified aqueous hydroxyacrylic dispersion, characterized in that: the soft monomer comprises one or more of butyl acrylate, isooctyl acrylate and acrylic laurate.
4. The process of claim 1 for the synthesis of a modified aqueous hydroxyacrylic dispersion, characterized in that: the hard monomer comprises one or more of styrene, methyl methacrylate and isobornyl acrylate.
5. The process of claim 1 for the synthesis of a modified aqueous hydroxyacrylic dispersion, characterized in that: the functional monomer comprises one or more of acrylic acid, methacrylic acid, hydroxypropyl acrylate, hydroxyethyl methacrylate and hydroxyethyl acrylate.
6. The process of claim 1 for the synthesis of a modified aqueous hydroxyacrylic dispersion, characterized in that: the chain transfer agent comprises one or two of dodecyl mercaptan and mercaptoethanol.
7. The process of claim 1 for the synthesis of a modified aqueous hydroxyacrylic dispersion, characterized in that: the organic solvent comprises one or more of ethylene glycol butyl ether, propylene glycol propyl ether, propylene glycol butyl ether, diethylene glycol dimethyl ether and diethylene glycol butyl ether.
8. The process of claim 1 for the synthesis of a modified aqueous hydroxyacrylic dispersion, characterized in that: the initiator comprises one or more of benzoyl peroxide, tert-butyl peroxybenzoate and isopropyl hydrogen peroxide.
9. The process of claim 1 for the synthesis of a modified aqueous hydroxyacrylic dispersion, characterized in that: the neutralizing agent is dimethylethanolamine.
10. The process for the synthesis of a modified aqueous hydroxyacrylic dispersion according to claim 1 or 2, characterized in that: the modified aqueous hydroxy acrylic acid dispersion comprises the following components in parts by weight: 115 parts of glycidyl methacrylate 104-.
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Citations (5)

* Cited by examiner, † Cited by third party
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