CN114316113A - Water-based acrylic emulsion resin and preparation method thereof - Google Patents
Water-based acrylic emulsion resin and preparation method thereof Download PDFInfo
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- CN114316113A CN114316113A CN202210007644.8A CN202210007644A CN114316113A CN 114316113 A CN114316113 A CN 114316113A CN 202210007644 A CN202210007644 A CN 202210007644A CN 114316113 A CN114316113 A CN 114316113A
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Abstract
The invention discloses a water-based acrylic emulsion resin which comprises the following components in parts by weight: 0.05-0.1 part of sodium bicarbonate, 1-7 parts of acrylic monomers, 35-50 parts of styrene and acrylic monomers, 0.5-3 parts of special vinyl monomers, 0.02-0.5 part of first-stage initiators, 0.02-1 part of second-stage initiators, 0.1-1 part of first-stage emulsifiers, 0.1-1 part of second-stage emulsifiers, 0.1-3 parts of neutralizers and 40-60 parts of water. The coating prepared from the water-based acrylic emulsion resin can be dried at low temperature, has good adhesive force, high film hardness and simple preparation method of the product, and the obtained product can meet the requirements of related industries.
Description
Technical Field
The invention relates to the field of coatings, in particular to a water-based acrylic emulsion resin and a preparation method thereof.
Background
At present, with the increasing environmental protection requirement, the traditional oil paint is urgently required to be transformed into a low VOC paint. The water-based paint has the double advantages of safety and environmental protection, is the primary choice of the process of converting oil into water, but the development and application of domestic water-based resin are in the stage of starting, and have a lot of defects.
The existing water-based self-drying coating has the problems of poor drying and paint falling after replacing the prior oil paint product, if the baking coating is used, although the performance is qualified, the baking is required for more than 30 minutes at 140 ℃ for curing and drying, because the radiator workpiece is huge, the heating and cooling of the workpiece can cause the increase of energy consumption and the reduction of production takt.
The technical problems are solved by a water-based acrylic emulsion resin which can be dried at low temperature, has good adhesive force, high film hardness and qualified temperature change resistance and a preparation method thereof.
Disclosure of Invention
In order to solve the technical problems, the invention provides the water-based acrylic emulsion resin and the preparation method thereof, the coating prepared from the water-based acrylic emulsion resin can realize low-temperature drying, has better adhesive force, high film hardness and simple preparation method of the product, and the obtained product can meet the requirements of related industries.
The invention solves the technical problems by the following technical scheme:
the invention provides a water-based acrylic emulsion resin which comprises the following components in parts by weight: 0.05-0.1 part of sodium bicarbonate, 1-7 parts of acrylic monomers, 35-50 parts of styrene and acrylic monomers, 0.5-3 parts of special vinyl monomers, 0.02-0.5 part of first-stage initiators, 0.02-1 part of second-stage initiators, 0.1-1 part of first-stage emulsifiers, 0.1-1 part of second-stage emulsifiers, 0.1-3 parts of neutralizers and 40-60 parts of water.
In the present invention, preferably, the aqueous acrylic emulsion resin comprises the following components in parts by weight: 0.08 part of sodium bicarbonate, 1.21 parts of acrylic monomers, 38.34 parts of styrene and acrylic monomers, 0.72 part of special vinyl monomers, 0.21 part of first-stage initiator, 0.04 part of second-stage initiator, 0.28 part of first-stage emulsifier, 0.52 part of second-stage emulsifier, 0.6 part of neutralizer and 58 parts of water.
In the invention, the first-stage initiator and the second-stage initiator are conventional initiators in the field, and partial differences exist according to specific reaction processes and the effect requirements of the invention;
preferably, the first stage initiator is one or more of potassium persulfate, ammonium persulfate and azobisisobutylamidine hydrochloride;
preferably, the second stage initiator is tert-butyl peroxy-2-ethylhexanoate or tert-butyl hydroperoxide.
In the present invention, the acrylic monomer is conventional in the art;
preferably, the acrylic monomer is acrylic acid and/or methacrylic acid.
In the invention, the acrylate monomer is conventional in the field;
preferably, the acrylate monomer is one or more of styrene, methyl methacrylate, butyl acrylate, butyl methacrylate, isobornyl methacrylate, hydroxyethyl acrylate and hydroxyethyl methacrylate.
In the invention, the first-stage emulsifier and the second-stage emulsifier are conventional emulsifiers in the field, and the selection of the emulsifiers is slightly different according to the effect requirement and the reaction process;
preferably, the first-stage emulsifier is one or more of alkylphenol polyoxyethylene ether OP-7, OP-10, OP-15 and anionic emulsifier LA40SZ, which are all available from Solvay chemical (Shanghai) Co., Ltd;
preferably, the second-stage emulsifier is one or more of alkylphenol polyoxyethylene ether OP-10, sodium dodecyl benzene sulfonate Solvay DS-4AP, sulfosuccinic acid amine Aerosol EF-800 and anionic emulsifier LA40SZ, which are all available from Solvay chemical industry (Shanghai) Co.
In the invention, the special vinyl monomer is the key improvement of the invention, and the adhesive force to the surface of the metal substrate is increased by providing active groups which can be combined with the metal substrate, such as longer-chain carboxyl, carbamido, amido, phosphate and the like;
preferably, the special vinyl monomer is a mixture BCEA of acrylic acid dipolymer and oligomer, methacrylamide ethyl ethylene urea with the trade name of SolvaWAM-II, methacrylic acid alkoxy phosphate with the trade name of SolvaPAM 100 or PAM200, one or more of methacrylic acid phosphate with the trade name of SolvaPAM 4000 and vinyl phosphate with the trade name of SolvaPAM 5000; the above-mentioned special vinyl monomers are available from solvay chemical (Shanghai) Co., Ltd.
In the present invention, the neutralizing agent is conventional in the art;
preferably, the neutralizing agent is one or more of ammonia, triethylamine and n, n-dimethylethanolamine.
In the present invention, the water is conventional in the art;
preferably, the water is deionized water.
The invention also provides a preparation method of the waterborne acrylic emulsion resin, which comprises the following steps:
s1, putting 40-60% of water, sodium bicarbonate and the first-stage emulsifier into a reaction kettle in parts by weight, introducing nitrogen, and heating to 75-85 ℃;
s2, uniformly mixing an acrylic monomer, an acrylate monomer, a special vinyl monomer, a second-stage emulsifier and 40-50% of water in parts by weight to obtain a mixed monomer, and sufficiently and uniformly mixing the mixed monomer on an emulsifying machine to obtain a mixed solution M;
s3, uniformly mixing 15-30% of first-stage initiator and 1-3% of water, adding the mixture and 4-8% of mixed solution M into a reaction kettle, preserving heat for 25-35 minutes, and when emulsion seeds are formed, dripping the rest of first-stage initiator and the rest of mixed solution M into the reaction kettle when the solution in the kettle generates blue light, dripping into the reaction kettle for 3-5 hours, preserving heat for 1.5-2.5 hours after dripping is finished, supplementing second-stage initiator and 8-15% of water, and preserving heat for 1.8-2.5 hours at 80 ℃;
s4, cooling to 45-55 ℃, adding a neutralizing agent and the rest water, stirring uniformly, and detecting parameter indexes to obtain the water-based acrylic emulsion resin.
In the present invention, the temperature after the temperature rise in S1 is preferably 80 ℃.
In the present invention, in S3, it is preferable that the holding time after the addition of the first-stage initiator is 30 minutes, the dropping time of the remaining mixed solution M is 4 hours, the holding time after the dropping is 2 hours, and the holding time after the addition of the second-stage initiator is 2 hours.
In the present invention, the raw materials used are commercially available.
The invention has the advantages and beneficial effects that:
Detailed Description
The following further describes embodiments of the present invention with reference to examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
This example provides an aqueous acrylic emulsion resin prepared by the following method:
s1, putting 25g of deionized water, 0.08g of sodium bicarbonate, 0.12g of OP10 emulsifier and 0.16g of LA40SZ emulsifier into a reaction kettle, introducing nitrogen, stirring and heating to 80 ℃;
s2, mixing 1.21g of methacrylic acid, 4.44g of methyl methacrylate, 17.76g of styrene, 16.14g of isooctyl acrylate, 0.72g of methacrylamide ethyl ethylene urea (Solvay WAM-II), 0.35g of OP10 emulsifier, 0.17g of LA40SZ emulsifier and 21.5g of deionized water uniformly to obtain a mixed monomer, and mixing the mixed monomer on an emulsifying machine sufficiently and uniformly to obtain a mixed solution M;
s3, uniformly mixing 0.05g of potassium persulfate as an initiator and 1.2g of deionized water, adding the mixture and a 5% mixed solution M into a reaction kettle, keeping the temperature for 30 minutes, and when the emulsion seeds are formed, starting to dropwise add the remaining 95% mixed solution M when the solution in the kettle appears blue light, simultaneously dropwise adding a mixed solution B of 0.16g of potassium persulfate and 6.5g of deionized water, keeping the temperature for 2 hours after dropwise adding, supplementing a mixed solution of 0.04g of tert-butyl hydroperoxide initiator and 1g of deionized water, and keeping the temperature for 2 hours at 80 ℃;
s4, cooling to 50 ℃, adding 0.6g of ammonia water and 2.8g of deionized water, and uniformly stirring to obtain the water-based acrylic emulsion resin.
Example 2
This example provides an aqueous acrylic emulsion resin prepared by the following method:
s1, putting 25g of deionized water, 0.08g of sodium bicarbonate, 0.12g of OP10 emulsifier and 0.16g of LA40SZ emulsifier into a reaction kettle, introducing nitrogen, stirring and heating to 80 ℃;
s2, uniformly mixing 1.21g of methacrylic acid, 4.44g of methyl methacrylate, 17.76g of styrene, 16.14g of isooctyl acrylate, 0.72g of methacrylic acid alkoxy phosphate (Solvapam 100), 0.35g of OP10 emulsifier, 0.17g of LA40SZ emulsifier and 21.5g of deionized water to obtain a mixed monomer, and sufficiently and uniformly mixing the mixed monomer on an emulsifying machine to obtain a mixed solution M;
s3, uniformly mixing 0.05g of potassium persulfate as an initiator and 1.2g of deionized water, adding the mixture and a 5% mixed solution M into a reaction kettle, keeping the temperature for 30 minutes, and when the emulsion seeds are formed, starting to dropwise add the remaining 95% mixed solution M when the solution in the kettle appears blue light, simultaneously dropwise adding a mixed solution B of 0.16g of potassium persulfate and 6.5g of deionized water, keeping the temperature for 2 hours after dropwise adding, supplementing a mixed solution of 0.04g of tert-butyl hydroperoxide initiator and 1g of deionized water, and keeping the temperature for 2 hours at 80 ℃;
s4, cooling to 50 ℃, adding 0.6g of ammonia water and 2.8g of deionized water, and uniformly stirring to obtain the water-based acrylic emulsion resin.
Example 3
This example provides an aqueous acrylic emulsion resin prepared by the following method:
s1, putting 25g of deionized water, 0.08g of sodium bicarbonate, 0.12g of OP10 emulsifier and 0.16g of LA40SZ emulsifier into a reaction kettle, introducing nitrogen, stirring and heating to 82 ℃;
s2, uniformly mixing 1.21g of methacrylic acid, 4.44g of methyl methacrylate, 17.76g of styrene, 16.14g of isooctyl acrylate, 0.72g of methacrylic acid phosphate PAM4000, 0.35g of OP10 emulsifier, 0.17g of LA40SZ emulsifier and 21.5g of deionized water to obtain a mixed monomer, and sufficiently and uniformly mixing the mixed monomer on an emulsifying machine to obtain a mixed solution M;
s3, uniformly mixing 0.05g of potassium persulfate as an initiator and 1.2g of deionized water, adding the mixture and a 5% mixed solution M into a reaction kettle, keeping the temperature for 30 minutes, and when the emulsion seeds are formed, starting to dropwise add the remaining 95% mixed solution M when the solution in the kettle appears blue light, simultaneously dropwise adding a mixed solution B of 0.16g of potassium persulfate and 6.5g of deionized water, keeping the temperature for 2 hours after dropwise adding, supplementing a mixed solution of 0.04g of tert-butyl hydroperoxide initiator and 1g of deionized water, and keeping the temperature for 2 hours at 80 ℃;
s4, cooling to 50 ℃, adding 0.6g of ammonia water and 2.8g of deionized water, and uniformly stirring to obtain the water-based acrylic emulsion resin.
The products of examples 1-3 were made into coatings in the following proportions as shown in table 1:
TABLE 1 coating formulations made from the products of examples 1-3
| Composition of | Ratio of |
| Aqueous acrylic resinOlefine acid emulsion | 65.00％ |
| Leveling agent | 0.50％ |
| Wetting agent | 2.00％ |
| Diethylene glycol butyl ether | 10.00％ |
| Aluminum powder | 15.00％ |
| Water (W) | 7.50％ |
| Total up to | 100.00％ |
The prepared coating is coated, and the construction conditions are shown in the following table 2:
TABLE 2 construction conditions for coatings prepared from the products of examples 1-3
| Item | Parameter(s) |
| Coating method | Air spraying |
| Diluent | Deionized water |
| Dilution ratio/% | Directly spraying or adding about 5% of water |
| Construction viscosity/coating-4, 25 deg.C, S | 25～50 |
| Leveling time/min before heating | 5～10 |
| Baking conditions | 80℃×15min |
The properties of the above-mentioned coating materials and those of commercially available coating materials were measured, and the method of measuring the coating film was as shown in the following Table 3:
TABLE 3 method for inspecting coating film
The results of the tests on the coating films of the coatings prepared from the products of examples 1 to 3 and the coating films of the commercial products are shown in Table 4 below:
TABLE 4 Properties of coating films of the coatings prepared from the products of examples 1 to 3 and of the coating films of the commercial products
Wherein the commercially available competitive product is a water-based paint (silver color) purchased from Qingdao Gechang environmental protection science and technology Limited.
The effect shows that the coating prepared from the water-based acrylic emulsion resin can realize low-temperature drying, has good adhesive force and high film hardness, and has obvious product advantages compared with conventional products sold in the market.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The water-based acrylic emulsion resin is characterized by comprising the following components in parts by weight: 0.05-0.1 part of sodium bicarbonate, 1-7 parts of acrylic monomers, 35-50 parts of styrene and acrylic monomers, 0.5-3 parts of special vinyl monomers, 0.02-0.5 part of first-stage initiators, 0.02-1 part of second-stage initiators, 0.1-1 part of first-stage emulsifiers, 0.1-1 part of second-stage emulsifiers, 0.1-3 parts of neutralizers and 40-60 parts of water.
2. The aqueous acrylic emulsion resin of claim 1, which comprises the following components in parts by weight: 0.08 part of sodium bicarbonate, 1.21 parts of acrylic monomers, 38.34 parts of styrene and acrylic monomers, 0.72 part of special vinyl monomers, 0.21 part of first-stage initiator, 0.04 part of second-stage initiator, 0.28 part of first-stage emulsifier, 0.52 part of second-stage emulsifier, 0.6 part of neutralizer and 58 parts of water.
3. The aqueous acrylic emulsion resin of claim 1 wherein the first stage initiator is one or more of potassium persulfate, ammonium persulfate, and azobisisobutylamidine hydrochloride;
and/or the second stage initiator is tert-butyl peroxy-2-ethylhexanoate or tert-butyl hydroperoxide.
4. The aqueous acrylic emulsion resin according to claim 1 wherein the acrylic monomer is acrylic acid and/or methacrylic acid;
and/or the acrylate monomer is one or more of styrene, methyl methacrylate, butyl acrylate, butyl methacrylate, isobornyl methacrylate, hydroxyethyl acrylate and hydroxyethyl methacrylate.
5. The aqueous acrylic emulsion resin of claim 1 wherein the first stage emulsifier is one or more of alkylphenol polyoxyethylene ethers OP-7, OP-10, OP-15 and anionic emulsifier LA40SZ, all available from solvay chemical (shanghai) ltd;
and/or the second-stage emulsifier is one or more of alkylphenol polyoxyethylene ether OP-10, sodium dodecyl benzene sulfonate Solvay DS-4AP, sulfosuccinic acid amine Aerosol EF-800 and an anionic emulsifier LA40SZ, which are all purchased from Solvay chemical industry (Shanghai) Co.
6. The aqueous acrylic emulsion resin of claim 1 wherein the specific vinyl monomer is a mixture of acrylic acid dimer and oligomer BCEA, methacrylamido ethyl ethylene urea having a designation of SolvaWAM-II, methacrylic acid alkoxy phosphate having a designation of SolvaPAM 100 or PAM200, one or more of methacrylic acid phosphate having a designation of SolvaPAM 4000 and vinyl phosphate having a designation of SolvaPAM 5000; the above-mentioned special vinyl monomers are available from solvay chemical (Shanghai) Co., Ltd.
7. The aqueous acrylic emulsion resin of claim 1 wherein the neutralizing agent is one or more of ammonia, triethylamine and n, n-dimethylethanolamine;
and/or the water is deionized water.
8. The aqueous acrylic emulsion resin according to any one of claims 1 to 7, comprising the steps of:
s1, putting 40-60% of water, sodium bicarbonate and the first-stage emulsifier into a reaction kettle in parts by weight, introducing nitrogen, and heating to 75-85 ℃;
s2, uniformly mixing an acrylic monomer, an acrylate monomer, a special vinyl monomer, a second-stage emulsifier and 40-50% of water in parts by weight to obtain a mixed monomer, and sufficiently and uniformly mixing the mixed monomer on an emulsifying machine to obtain a mixed solution M;
s3, uniformly mixing 15-30% of first-stage initiator and 1-3% of water, adding the mixture and 4-8% of mixed solution M into a reaction kettle, preserving heat for 25-35 minutes, and when emulsion seeds are formed, dripping the rest of first-stage initiator and the rest of mixed solution M into the reaction kettle when the solution in the kettle generates blue light, dripping into the reaction kettle for 3-5 hours, preserving heat for 1.5-2.5 hours after dripping is finished, supplementing second-stage initiator and 8-15% of water, and preserving heat for 1.8-2.5 hours at 80 ℃;
s4, cooling to 45-55 ℃, adding a neutralizing agent and the rest water, stirring uniformly, and detecting parameter indexes to obtain the water-based acrylic emulsion resin.
9. The aqueous acrylic emulsion resin according to claim 8, wherein the temperature after the temperature rise in S1 is 80 ℃.
10. The aqueous acrylic emulsion resin according to claim 8, wherein in S3, the holding time after the addition of the first stage initiator is 30 minutes, the dropping time of the remaining mixed solution M is 4 hours, the holding time after the dropping is 2 hours, and the holding time after the addition of the second stage initiator is 2 hours.
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| CN117106127A (en) * | 2023-08-08 | 2023-11-24 | 南京科工煤炭科学技术研究有限公司 | Acrylate emulsion for polymer cement under coal mine and preparation method thereof |
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