CN111363104A - Preparation method of styrene-acrylic emulsion and water-based paint - Google Patents
Preparation method of styrene-acrylic emulsion and water-based paint Download PDFInfo
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- CN111363104A CN111363104A CN202010211511.3A CN202010211511A CN111363104A CN 111363104 A CN111363104 A CN 111363104A CN 202010211511 A CN202010211511 A CN 202010211511A CN 111363104 A CN111363104 A CN 111363104A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
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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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- 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
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F257/00—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00
- C08F257/02—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00 on to polymers of styrene or alkyl-substituted styrenes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/003—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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Abstract
The invention discloses a preparation method of styrene-acrylic emulsion, which comprises the following raw materials in parts by weight: preparing a hard core, wherein the raw materials of the hard core comprise 140-180 parts of hard monomers and 2-6 parts of acrylic acid; preparing a soft shell, wherein the raw materials of the soft shell comprise 70-90 parts of hard monomers and 30-50 parts of butyl acrylate; preparing an outer soft shell, wherein the raw materials of the outer soft shell comprise 30-50 parts of hard monomers, 70-90 parts of butyl acrylate, 2-7 parts of methyl methacrylate and 4-8 parts of diacetone acrylamide; the hard monomer consists of styrene and methyl methacrylate, and the mass ratio of the styrene to the methyl methacrylate is (10-180) to (0-160). The invention also discloses a water-based paint which comprises the following components in parts by weight: 93-96 parts of the styrene-acrylic emulsion, 0.1-0.8 part of a film-forming additive, 0.1-0.3 part of a defoaming agent and 0.1-0.7 part of a leveling additive. The mass part of the film forming additive added into the water-based paint is less than 0.8 percent, so that the water-based paint has excellent environmental protection property and high drying speed; the water-based paint has high hardness after being dried.
Description
Technical Field
The invention relates to the field of water-based paint, in particular to a preparation method of styrene-acrylic emulsion and water-based paint.
Background
In order to make the coating material have high hardness at room temperature, it is necessary to ensure that it is in a glassy state at room temperature, and the glass transition temperature of the coating material should be suitably higher than room temperature; in order to make the coating material form a film quickly, the minimum film-forming temperature needs to be lower than room temperature, otherwise the coating material generates whitening and cracking phenomena, and powder is seriously formed. The method for obtaining the acrylic coating with hard core and soft shell particles by adopting a seed emulsion polymerization method can obtain the styrene-acrylic emulsion with higher glass transition temperature and lower lowest film forming temperature, and is the popular research direction of the current water-based coating.
For the water-based paint, when the construction temperature is lower than the glass transition temperature, no film-forming assistant can form a film, the lowest film-forming temperature has a descending trend along with the increase of the dosage of the film-forming assistant, the film-forming assistant is the largest source of VOC (volatile organic compounds) (which refer to active volatile organic compounds, namely volatile organic compounds which can generate harm) in the water-based paint, and under the condition that the lowest film-forming temperature meets the construction requirement, the less the dosage of the film-forming assistant is, the better the environmental protection performance of the paint is, and the cost is also greatly reduced.
The problems existing in the prior art are as follows: the styrene-acrylic emulsion with hard-core soft-shell particles is obtained by adopting a seed emulsion polymerization method, has higher glass transition temperature and lower film-forming temperature, but a large amount of film-forming auxiliary agent needs to be added when the coating is prepared at the later stage, generally the mass fraction is more than two percent, the drying speed of the water-based coating is not as high as that of the oil-based coating due to the higher heat volatilization ratio of water, and the drying speed is further reduced after the film-forming auxiliary agent is added.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the styrene-acrylic emulsion with hard core and soft shell obtained by adopting a seed emulsion polymerization method needs to be added with a large amount of film-forming additives when preparing a coating at a later stage, so that the problems of low drying speed of the coating and high VOC content in the coating are caused.
The solution of the invention for solving the technical problem is as follows:
the preparation method of the styrene-acrylic emulsion comprises the following steps of:
s1, uniformly mixing 140-180 parts of hard monomer, 2-6 parts of acrylic acid and a proper amount of deionized water and emulsifier to prepare a first monomer mixed solution for later use; uniformly mixing 70-90 parts of hard monomer and 30-50 parts of butyl acrylate with a proper amount of deionized water and an emulsifier to prepare a second monomer mixed solution for later use; uniformly mixing 30-60 parts of hard monomer, 70-90 parts of butyl acrylate, 2-7 parts of methyl methacrylate and 4-8 parts of diacetone acrylamide with a proper amount of deionized water and an emulsifier to prepare a third monomer mixed solution for later use; the hard monomer consists of styrene and methyl methacrylate, and the mass ratio of the styrene to the methyl methacrylate is (10-180) to (0-160);
s2, taking 1-4 parts of emulsifier and 250-350 parts of deionized water, uniformly stirring, heating to 75-85 ℃, adding a proper amount of first monomer mixed solution, uniformly stirring, adding a proper amount of oxidant after 10-20 minutes, beginning to dropwise add the first monomer mixed solution within 5 minutes after the oxidant is added, finishing dropwise adding the first monomer mixed solution within 50-80 minutes, and preserving heat for 10-20 minutes to obtain a prepolymerization emulsion;
s3, adding 0.5-1 part of emulsifier into the pre-polymerization emulsion, dropwise adding a second monomer mixed solution, dropwise adding the second monomer mixed solution within 30-45 minutes, and keeping the temperature for 40-80 minutes to obtain an intermediate polymerization emulsion;
s4, 0.5-1 part of reducing agent and a proper amount of initiator are dripped into the intermediate polymerization emulsion, after 1-5 minutes, a third monomer mixed solution is dripped, after 3-5 hours, the third monomer mixed solution is dripped, and the temperature is kept for 1-2 hours; cooling to room temperature, and neutralizing with ammonia water until the pH value is 6-8; adding a proper amount of cross-linking agent, and uniformly stirring; filtering to obtain the styrene-acrylic emulsion.
In the invention, the monomer in the first monomer mixed solution is completely a monomer for synthesizing hard cores; the ratio of the soft monomer to the hard monomer in the second monomer mixed solution is about 1/2; the ratio of the soft monomer to the hard monomer in the third monomer mixed solution is about 2/1, and finally the styrene-acrylic emulsion with hard core and soft shell particles is synthesized. The hardness of the hard core and soft shell particles prepared from the raw materials according to the proportion is gradually reduced from inside to outside, compared with the traditional structure that a layer of soft shell is coated on the surface of a hard core, the contact area between the hard core and the soft shell in the structure is increased by multiple times, the hardness of the soft shell is higher, and the hardness of the prepared coating after drying is also improved.
In order to obtain the coating with higher hardness at room temperature after drying, the glass transition temperature of the styrene-acrylic emulsion is designed to be 40-50 ℃. According to the FOX equation:
wherein T isgIs the glass transition temperature, T, of the copolymerg1，Tg2Equal to the glass transition temperature, W, of the homopolymer of the monomer of each componentm1，Wm2And the like are the mass fractions of the component monomers in the total monomers. By TgFor example, at 45 ℃, the theoretical ratio of styrene to butyl acrylate is 75:25 by mass, and in the actual formulation, the functional monomers such as acrylic acid, methyl methacrylate, diacetone acrylamide and the like are also hard monomers, so the actual ratio of styrene to butyl acrylate is about 7:3 by mass.
Of course, the lowest film-forming temperature of the styrene-acrylic emulsion meets the condition below room temperature, specifically below 20 ℃.
The raw material in the step S4 comprises diacetone acrylamide, acrylamide double bond in the diacetone acrylamide can be homopolymerized by free radical and can be copolymerized with a plurality of monomers, ketone carbonyl can be introduced into a polymer, and the ketone carbonyl and α -H can carry out a plurality of reactions, such as cross-linking with hydrazine compounds, epoxy, l-aziridine and the like.
In some embodiments, the mass ratio of styrene to butyl acrylate in the raw material is (6.5-7.5): 2.5-3.5.
In some embodiments, the ratio of the mass of styrene in the first monomer to the sum of the mass of styrene and butyl acrylate in the feedstock is (3.5-4.5) to (9.5-10.5).
In some embodiments, the emulsifier is a mixture of OP-10 (polyoxyethylene octylphenol ether-10) and SDS (sodium dodecyl sulfate).
In some embodiments, the initiator is APS, the amount of initiator used in step S2 is 0.1 to 1 part, and the amount of initiator used in step S3 is 0.1 to 1 part.
In some embodiments, the oxidant is ammonium persulfate, the oxidant used in step S2 is 0.1-3 parts, and the reducing agent is sodium metabisulfite.
In some embodiments, the crosslinking agent is 10% adipic dihydrazide aqueous solution, and the amount of the crosslinking agent used in step S4 is 0.1-5%.
The invention also provides a water-based paint which comprises the following components in parts by weight: 93-96 parts of styrene-acrylic emulsion prepared by any one of the methods, 0.1-0.8 part of film-forming assistant, 0.1-0.3 part of defoaming agent and 0.1-0.7 part of leveling assistant.
In some embodiments, the liquid further comprises 3-4 parts of water, 0.03-0.06 part of mildew preventive, 0.01-0.2 part of thickener, 0.01-0.5 part of cosolvent and 0.01-0.1 part of essence.
In some embodiments, the coalescent is alcohol ester-12.
The invention has the beneficial effects that:
1. the glass transition temperature of the styrene-acrylic emulsion is 40-50 ℃, the styrene-acrylic emulsion is in a glass state at room temperature after being dried, and can naturally form a film at room temperature without adding a film-forming auxiliary agent, so that the construction requirement can be met;
2. the mass part of the film forming additive added into the water-based paint is less than 0.8 percent, so that the water-based paint has excellent environmental protection property and high drying speed;
3. the water-based paint has high hardness after being dried.
Detailed Description
The present invention is not limited to the embodiments described above, and those skilled in the art can make various equivalent modifications or substitutions without departing from the spirit of the present invention, and these equivalent modifications or substitutions are included in the scope defined by the claims of the present application.
Examples
TABLE 1
TABLE 2
Table 1 is a table of the formulation of the styrene-acrylic emulsion of the example, table 2 is a table of the formulation of the water-based paint of the first example, the first example includes the following steps, the raw materials in the following steps are calculated by weight:
uniformly mixing 140 parts of styrene, 24 parts of methyl methacrylate and 4 parts of acrylic acid with a proper amount of deionized water and an emulsifier to prepare a first monomer mixed solution for later use; uniformly mixing 20 parts of styrene, 24 parts of methyl methacrylate and 40 parts of butyl acrylate with a proper amount of deionized water and an emulsifier to prepare a second monomer mixed solution for later use; 40 parts of styrene, 80 parts of butyl acrylate, 4 parts of methyl methacrylate and 6 parts of diacetone acrylamide are taken and mixed evenly with a proper amount of deionized water and emulsifier to prepare a third monomer mixed solution for later use.
Adding 2.64 parts of emulsifier compounded by OP-10 and SDS and 308.5 parts of deionized water into 1000mL of a four-necked bottle provided with a thermometer, an electric stirrer, a condenser tube and a dropping funnel, heating the four-necked bottle by using an alcohol lamp, uniformly stirring, heating to 50 ℃, adding 0.8 part of APS (ammonium persulfate), uniformly stirring, adding a proper amount of APS after 15 minutes, immediately dropwise adding a first monomer mixed solution after adding the APS, completely dropping the first monomer mixed solution after 60 minutes, and preserving the temperature for 15 minutes to obtain a pre-emulsion; and adding 76 parts of deionized water into the pre-emulsion, uniformly stirring, adding 0.86 part of emulsifier compounded by OP-10 and SDS, dropwise adding the second monomer mixed solution after 40 minutes, and keeping the temperature for 60 minutes to obtain the intermediate emulsion.
Adding 169 parts of deionized water into the intermediate emulsion, uniformly stirring, dropwise adding 0.76 part of sodium metabisulfite and a proper amount of APS, dropwise adding a third monomer mixed solution after 3 minutes, dropwise adding the third monomer mixed solution after 3.5 hours, and keeping the temperature for 1.5 hours; cooling to room temperature, and neutralizing with ammonia water to pH 7.5; adding a proper amount of 10% adipic dihydrazide, and uniformly stirring; filtering to obtain the styrene-acrylic emulsion.
Taking 94.4 parts of the styrene-acrylic emulsion, 0.05 part of A26, 3.73 parts of water, 0.2 part of BYK037, 0.6 part of Hydropalat140, 0.02 part of WB811, 0.1 part of SN-612 and 0.3 part of diethylene glycol butyl ether, and uniformly stirring and mixing to obtain the water-based paint.
Comparative example
TABLE 3
Table 3 is a table of the formulation of a styrene-acrylic emulsion of comparative examples, which includes the following steps, the raw materials in the following steps are in parts by weight:
uniformly mixing 100 parts of styrene, 82 parts of methyl methacrylate, 13 parts of butyl acrylate, 7 parts of acrylic acid and 14 parts of 10% adipic dihydrazide to obtain an inner core monomer; uniformly mixing 40 parts of styrene, 10 parts of methyl methacrylate, 115 parts of butyl acrylate and 7 parts of acrylic acid to obtain a shell monomer; adding 560 parts of water, 8 parts of emulsifier compounded by OP-10 and SDS into a polymerization kettle, starting stirring, heating to 80 ℃, adding 1 part of ammonium persulfate, immediately beginning to dropwise add the core monomer, finishing dropwise adding within 2.5 hours, and preserving heat for 1 hour;
adding 1 part of ammonium persulfate into a reaction kettle, beginning to dropwise add a shell monomer, after dropwise adding is completed within 3.5 hours, adding 0.7 part of ammonium persulfate, preserving heat for 1 hour, cooling to 60 ℃, adding 0.35 part of sodium formaldehyde sulfoxylate after 10 minutes, adding 0.35 part of sodium formaldehyde sulfoxylate after 20 minutes, preserving heat for 30 minutes, cooling to room temperature, adjusting the pH value to 7.5 by ammonia water, and filtering to obtain the styrene-acrylic emulsion.
Taking 94.4 parts of the styrene-acrylic emulsion, 0.05 part of A26, 3.73 parts of water, 0.2 part of BYK037, 0.6 part of alcohol ester-12, 0.4 part of Hydropalat140, 0.02 part of WB811, 0.1 part of SN-612 and 0.3 part of diethylene glycol butyl ether, and uniformly stirring and mixing to obtain the water-based paint.
Tests show that the glass transition temperature of the styrene-acrylic emulsion in the embodiment is 45 ℃ and the lowest film forming temperature is 15 ℃; the glass transition temperature of the styrene-acrylic emulsion of the comparative example is 55 ℃, and the lowest film forming temperature is 10 ℃, which all meet the requirements.
Selecting a density board adhered with a veneer, treating the density board with a sealing primer, polishing, spraying the water-based paint, constructing twice, naturally drying for 7 days, and performing performance test, wherein the test results are shown in table 4:
TABLE 4
The results show that the water-based paint prepared from the styrene-acrylic emulsion prepared by the preparation method of the styrene-acrylic emulsion has high hardness, and can achieve excellent film-forming performance by only needing a small amount of film-forming additive.
Claims (10)
1. The preparation method of the styrene-acrylic emulsion is characterized by comprising the following steps of:
s1, uniformly mixing 140-180 parts of hard monomer, 2-6 parts of acrylic acid and a proper amount of deionized water and emulsifier to prepare a first monomer mixed solution for later use; uniformly mixing 70-90 parts of hard monomer and 30-50 parts of butyl acrylate with a proper amount of deionized water and an emulsifier to prepare a second monomer mixed solution for later use; uniformly mixing 30-60 parts of hard monomer, 70-90 parts of butyl acrylate, 2-7 parts of methyl methacrylate and 4-8 parts of diacetone acrylamide with a proper amount of deionized water and an emulsifier to prepare a third monomer mixed solution for later use; the hard monomer consists of styrene and methyl methacrylate, and the mass ratio of the styrene to the methyl methacrylate is (10-180) to (0-160);
s2, taking 1-4 parts of emulsifier and 250-350 parts of deionized water, uniformly stirring, heating to 75-85 ℃, adding a proper amount of first monomer mixed solution, uniformly stirring, adding a proper amount of oxidant after 10-20 minutes, beginning to dropwise add the first monomer mixed solution within 5 minutes after the oxidant is added, finishing dropwise adding the first monomer mixed solution within 50-80 minutes, and preserving heat for 10-20 minutes to obtain a prepolymerization emulsion;
s3, adding 0.5-1 part of emulsifier into the pre-polymerization emulsion, dropwise adding a second monomer mixed solution, dropwise adding the second monomer mixed solution within 30-45 minutes, and keeping the temperature for 40-80 minutes to obtain an intermediate polymerization emulsion;
s4, 0.5-1 part of reducing agent and a proper amount of initiator are dripped into the intermediate polymerization emulsion, after 1-5 minutes, a third monomer mixed solution is dripped, after 3-5 hours, the third monomer mixed solution is dripped, and the temperature is kept for 1-2 hours; cooling to room temperature, and neutralizing with ammonia water until the pH value is 6-8; adding a proper amount of cross-linking agent, and uniformly stirring; filtering to obtain the styrene-acrylic emulsion.
2. The method for preparing styrene-acrylic emulsion according to claim 1, wherein: the mass ratio of the hard monomer to the butyl acrylate in the raw materials is (6.5-7.5) to (2.5-3.5).
3. The method for preparing styrene-acrylic emulsion according to claim 1, wherein: the ratio of the mass of the hard monomer in the first monomer to the sum of the mass of the hard monomer and the mass of the butyl acrylate in the raw material is (3.5-4.5) to (9.5-10.5).
4. The method for preparing styrene-acrylic emulsion according to claim 1, wherein: the emulsifier is a mixture of a nonionic surfactant and an anionic surfactant.
5. The method for preparing styrene-acrylic emulsion according to claim 1, wherein: the initiator is APS, and the using amount of the initiator in the step S4 is 0.1-1 part.
6. The method for preparing styrene-acrylic emulsion according to claim 1, wherein: the oxidant is ammonium persulfate, and the using amount of the oxidant in the step S2 is 0.1-1 part; the reducing agent is sodium metabisulfite.
7. The method for preparing styrene-acrylic emulsion according to claim 1, wherein: the cross-linking agent is 10% adipic dihydrazide aqueous solution, and the dosage of the cross-linking agent in the step S4 is 0.1-5%.
8. The water-based paint is characterized by comprising the following components in parts by weight: 93-96 parts of styrene-acrylic emulsion prepared by the preparation method of the styrene-acrylic emulsion according to any one of claims 1-7, 0.1-0.8 part of film-forming assistant, 0.1-0.3 part of defoaming agent and 0.1-0.7 part of leveling assistant.
9. The aqueous coating of claim 8, wherein: the preservative also comprises 3-4 parts of water, 0.03-0.06 part of mildew preventive, 0.01-0.2 part of thickening agent, 0.01-0.5 part of cosolvent and 0.01-0.1 part of essence.
10. The aqueous coating of claim 8, wherein: the film-forming auxiliary agent is DPM and DPNB.
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| CN112724765A (en) * | 2021-01-23 | 2021-04-30 | 台州市万胜涂料有限公司 | Styrene-acrylic emulsion water-based paint for plastics |
| CN117487428A (en) * | 2023-11-02 | 2024-02-02 | 广州芯联化工产品有限公司 | Functional natural latex glove inner coating and preparation process thereof |
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