CN115010867A - Water-based wood paint emulsion and preparation method thereof - Google Patents
Water-based wood paint emulsion and preparation method thereof Download PDFInfo
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- CN115010867A CN115010867A CN202210819833.5A CN202210819833A CN115010867A CN 115010867 A CN115010867 A CN 115010867A CN 202210819833 A CN202210819833 A CN 202210819833A CN 115010867 A CN115010867 A CN 115010867A
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- parts
- emulsion
- wood lacquer
- aqueous wood
- stirring
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- 239000000839 emulsion Substances 0.000 title claims abstract description 154
- 239000002023 wood Substances 0.000 title claims abstract description 81
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000004945 emulsification Methods 0.000 title claims description 10
- 239000003973 paint Substances 0.000 title description 20
- 239000000178 monomer Substances 0.000 claims abstract description 92
- 239000004922 lacquer Substances 0.000 claims abstract description 65
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 26
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 26
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003999 initiator Substances 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 13
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 11
- GTELLNMUWNJXMQ-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical class OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO GTELLNMUWNJXMQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 8
- WFVZQYQWGBYJRH-UHFFFAOYSA-N but-1-ene;2-methylprop-2-enamide;urea Chemical compound CCC=C.NC(N)=O.CC(=C)C(N)=O WFVZQYQWGBYJRH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 239000007800 oxidant agent Substances 0.000 claims abstract description 8
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 6
- 239000003899 bactericide agent Substances 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 16
- 238000004321 preservation Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 5
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 239000013530 defoamer Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000002480 mineral oil Substances 0.000 claims description 4
- 235000010446 mineral oil Nutrition 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 230000003115 biocidal effect Effects 0.000 claims description 2
- 239000003139 biocide Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- BIISIZOQPWZPPS-UHFFFAOYSA-N 2-tert-butylperoxypropan-2-ylbenzene Chemical compound CC(C)(C)OOC(C)(C)C1=CC=CC=C1 BIISIZOQPWZPPS-UHFFFAOYSA-N 0.000 claims 1
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 14
- 238000000576 coating method Methods 0.000 description 23
- 239000011248 coating agent Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 14
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- -1 allyloxy aromatic alcohol Chemical compound 0.000 description 3
- 239000011258 core-shell material Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000011534 incubation Methods 0.000 description 3
- 239000004816 latex Substances 0.000 description 3
- 229920000126 latex Polymers 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- KRDXTHSSNCTAGY-UHFFFAOYSA-N 2-cyclohexylpyrrolidine Chemical compound C1CCNC1C1CCCCC1 KRDXTHSSNCTAGY-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002211 L-ascorbic acid Substances 0.000 description 1
- 235000000069 L-ascorbic acid Nutrition 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- IBVAQQYNSHJXBV-UHFFFAOYSA-N adipic acid dihydrazide Chemical compound NNC(=O)CCCCC(=O)NN IBVAQQYNSHJXBV-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000012874 anionic emulsifier Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000003211 malignant effect Effects 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- 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
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
-
- 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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
Abstract
The invention provides an aqueous wood lacquer emulsion and a preparation method thereof, wherein the aqueous wood lacquer emulsion comprises the following raw materials in parts by weight: 400 portions and 800 portions of deionized water; 10-22 parts of an emulsifier; 50-150 parts of styrene; 190-400 parts of methyl methacrylate; 0-30 parts of butyl acrylate; 130-260 parts of isooctyl acrylate; 12-24 parts of methacrylic acid; 4-10 parts of an internal crosslinking agent; 10-20 parts of functional monomer; 1.2-3 parts of an initiator; 0.5-1 part of an oxidant; 0.5-1 part of reducing agent; 10-15 parts of a pH regulator; 1.5-2.5 parts of a defoaming agent; 5-10 parts of a bactericide; the internal crosslinking agent comprises ethoxylated trimethylolpropane triacrylate; the functional monomer comprises methacrylamide ethyl ethylene urea. The aqueous wood lacquer emulsion has high hardness, good film forming property, high drying speed and good flexibility.
Description
Technical Field
The invention belongs to the technical field of coatings, and relates to an aqueous wood lacquer emulsion and a preparation method thereof.
Background
In recent years, with the improvement of the living standard of people and the enhancement of environmental awareness, people pay more attention to the hazard of solvent-based wood coatings, because organic solvents contained in paints have stronger volatility, volatile gases often contain a plurality of substances harmful to human bodies, and people can cause malignant diseases after long-term inhalation, and the water-based wood paint coating is an environment-friendly coating taking water as a dispersion medium, and along with the deepening of the understanding of people on health and environmental protection and the influence of various living environments, when the water-based wood paint coating is first seen in China in the 90 th century, the water-based wood paint coating is widely popular due to the environmental protection, simple production and good applicability.
The water-based wood paint coating on the market at present mainly takes water-based acrylic emulsion as a main film forming substance, and the proportion of the water-based acrylic emulsion in the water-based wood paint coating reaches more than 80%, so the quality of the water-based acrylic emulsion is directly related to the using effect of the water-based wood paint coating, the water-based wood paint emulsion mainly comprises single-component water-based acrylic emulsion and double-component water-based acrylic emulsion, the double-component water-based acrylic emulsion is better in performance compared with the single-component water-based acrylic emulsion, but when the double-component water-based acrylic emulsion is applied to the water-based wood paint coating, the coating is complex in construction, high in cost and contains a certain amount of solvent, the application of the water-based double-component emulsion in the wood paint is greatly limited due to the factors, so the film forming substance of the water-based wood paint coating mainly takes the single-component water-based propylene emulsion, but the hardness of the single-component water-based propylene emulsion is low, the wide application of the single-component water-based acrylic emulsion in the water-based wood paint is greatly influenced by the factors of poor film forming property, poor resistance and poor adhesion.
CN110964400A discloses an aqueous wood lacquer emulsion, which adopts a polymerization process of three-layer structure, limits Tg of each layer structure, and introduces a self-crosslinking system of diacetone acrylamide and adipic dihydrazide to synthesize a single-component aqueous propylene emulsion, the aqueous acrylic emulsion synthesized by the proposal has the characteristics of fast drying, high hardness, good film forming property, good resistance and good adhesive force when being applied to the aqueous wood lacquer coating, but the emulsion synthesis process is complex, the production efficiency and the production cost are higher in the actual production process, the aqueous acrylic emulsion synthesized by the proposal has poor flexibility, when the hardness of the aqueous wood lacquer coating is higher and the flexibility is poor in the actual application, the coating has obvious brittleness tendency, so the coating is easy to crack or even delaminate at corners and bending positions, and wood objects are transported or transported, when the collision phenomenon occurs, the coating is very easy to crack or even delaminate, the attractiveness of the woodware article is seriously influenced, and the popularization and normal use of the single-component water-based woodware paint can be greatly influenced.
Therefore, in the art, it is desired to develop an aqueous wood lacquer emulsion with high hardness, good film forming property, fast drying speed and good flexibility.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the water-based wood lacquer emulsion and the preparation method thereof. According to the invention, a core-shell process which is simpler than a three-layer process in CN110964400A is adopted in the emulsion synthesis process, and the high-Tg and low-film-forming-temperature water-based acrylic emulsion can be obtained by setting the Tg of a core monomer at 90-110 ℃ and the Tg of a shell monomer at-40-20 ℃, so that the water-based wood paint emulsion with high hardness, good film-forming property, high drying speed and good flexibility can be obtained.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides an aqueous wood lacquer emulsion, which comprises the following raw materials in parts by weight:
the internal crosslinking agent comprises ethoxylated trimethylolpropane triacrylate;
the functional monomer comprises methacrylamide ethyl ethylene urea.
According to the invention, by controlling the core-shell monomer dropping process, the Tg of the core monomer is controlled to be 90-110 ℃, and the Tg of the shell monomer is controlled to be-40-20 ℃, so that the water-based acrylic emulsion with high Tg and low film-forming temperature can be obtained; by introducing the internal crosslinking agent of ethoxylated trimethylolpropane triacrylate, on one hand, a flexible chain segment is introduced, so that the flexibility of the emulsion can be improved, and on the other hand, the structure of the emulsion is changed from a linear structure into a compact network structure, so that the drying speed and the resistance can be improved; by introducing the functional monomer of methacrylamide ethyl ethylene urea, the Tg of the emulsion can be improved on one hand, and the cohesive force of the emulsion can be improved on the other hand, so that the hardness and the adhesive force of the emulsion can be obviously improved. The three aspects act together to ensure that the synthesized aqueous wood lacquer emulsion has higher hardness, higher drying speed, better tolerance and better flexibility after film forming, better meets the requirement of the aqueous wood lacquer coating on the aqueous wood lacquer emulsion, and better expands the application range of the aqueous wood lacquer coating.
In the invention, the ethoxylated trimethylolpropane triacrylate (TMP3EOTA) is introduced in the emulsion synthesis process, and is a trifunctional internal crosslinking agent containing a flexible chain segment and provided with a plurality of reaction points, so that the flexible chain of the ethoxylated trimethylolpropane triacrylate can endow polymer molecules with good flexibility; on the other hand, in the emulsion polymerization process, the trifunctional internal crosslinking agent can be crosslinked with other monomers, so that the emulsion is changed into a more compact network structure from a linear structure, and the crosslinking density of the emulsion is increased, thereby increasing the drying speed, the emulsion paint film resistance and the hardness of the emulsion during film forming.
In the invention, methacrylamide ethyl ethylene urea (MAEEU) is introduced in the emulsion synthesis process, wherein the methacrylamide ethyl ethylene urea (MAEEU) is a high Tg functional monomer containing carbamido, the Tg of the monomer reaches 155 ℃, on one hand, the high Tg can endow polymer molecules with good rigidity, and can obviously improve the hardness of the polymer after film forming, and on the other hand, the carbamido has good cohesive force per se, and can obviously improve the adhesive force of the emulsion.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the amount of deionized water can be 400 parts, 450 parts, 500 parts, 550 parts, 600 parts, 650 parts, 700 parts, 750 parts or 800 parts and the like.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the amount of the emulsifier can be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts or 22 parts, etc.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the dosage of the styrene can be 50 parts, 60 parts, 70 parts, 80 parts, 90 parts, 100 parts, 110 parts, 120 parts, 130 parts, 140 parts or 150 parts and the like.
In the invention, in the raw material for preparing the aqueous wood lacquer emulsion, the amount of the methyl methacrylate can be 190 parts, 200 parts, 230 parts, 250 parts, 280 parts, 300 parts, 330 parts, 350 parts, 380 parts or 400 parts, etc.
In the invention, the amount of butyl acrylate in the raw materials for preparing the aqueous wood lacquer emulsion can be 0 part, 1 part, 3 parts, 5 parts, 8 parts, 10 parts, 13 parts, 15 parts, 18 parts, 20 parts, 23 parts, 25 parts, 28 parts or 30 parts, etc.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the dosage of the isooctyl acrylate can be 130 parts, 140 parts, 150 parts, 160 parts, 170 parts, 180 parts, 190 parts, 200 parts, 210 parts, 220 parts, 230 parts, 240 parts, 250 parts or 260 parts and the like.
In the invention, the amount of the methacrylic acid in the raw materials for preparing the aqueous wood lacquer emulsion can be 12 parts, 15 parts, 18 parts, 20 parts, 22 parts or 24 parts.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the amount of the internal cross-linking agent can be 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts or 10 parts.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the amount of the functional monomer can be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts or 20 parts, etc.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the amount of the initiator can be 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, 2.2 parts, 2.5 parts, 2.8 parts or 3 parts, etc.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the amount of the oxidant can be 0.5 part, 0.8 part or 1 part, etc.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the amount of the reducing agent can be 0.5 part, 0.8 part or 1 part, etc.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the amount of the pH regulator can be 10 parts, 13 parts or 15 parts.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the dosage of the defoaming agent can be 1.5 parts, 2 parts or 2.5 parts, etc.
In the invention, in the raw materials for preparing the aqueous wood lacquer emulsion, the amount of the bactericide can be 5 parts, 8 parts or 10 parts.
Preferably, the ratio of the parts by weight of isooctyl acrylate to the sum of the parts by weight of styrene and methyl methacrylate is 1 (1-3), such as 1:1, 1:2 or 1:3, etc.
Preferably, the emulsifier is a reactive emulsifier, and the reactive group of the reactive anionic emulsifier can be firmly combined with the latex particles, so that the stability of the system is improved, and the water resistance of the film-forming material can be effectively improved. The reactive emulsifier comprises any one of SR-10, AR-10 or LR-10 or the combination of at least two of the SR-10, the AR-10 or the LR-10.
The reactive emulsifier is characterized in that emulsifier molecules can be copolymerized with monomers and permanently bonded to latex molecules, and the chemical bonding has the following advantages: (1) the molecules of the emulsifier can not migrate to cause latex agglomeration, and the molecules of the emulsifier are still attached to the surfaces of particles after the emulsion is formed into a film or is prepared into solid powder, so that the particles can be re-dispersed in water; (2) when the dosage of the reactive emulsifier is proper, the reactivity is improved, and emulsifier molecules do not exist in the polymerized water phase, so that the film forming speed is accelerated; (3) the water resistance of the adhesive film can be improved.
Preferably, the initiator comprises any one of potassium persulfate, sodium persulfate or ammonium persulfate or a combination of at least two thereof.
Preferably, the oxidizing agent comprises tert-butyl hydroperoxide and/or tert-butyl cumyl peroxide.
Preferably, the reducing agent comprises sodium bisulfite or ascorbic acid.
Preferably, the pH regulator comprises 25% ammonia water, and the ammonia water has high neutralization efficiency and low price.
Preferably, the defoamer comprises a mineral oil type defoamer.
Preferably, the biocide comprises cason and/or BIT.
In a second aspect, the present invention provides a method for preparing the aqueous wood lacquer emulsion according to the first aspect, wherein the method comprises the following steps:
(a) preparing a kettle bottom solution: adding 200 and 400 parts of deionized water and 4-8 parts of emulsifier into the reactor, and stirring to obtain a kettle bottom solution;
(b) preparation of nuclear monomer pre-emulsion: adding 100-200 parts of deionized water and 3-7 parts of an emulsifier into a pre-emulsification cylinder, stirring, then adding 50-150 parts of styrene, 150-320 parts of methyl methacrylate, 5-9 parts of methacrylic acid, 0-30 parts of butyl acrylate, 1-3 parts of an internal crosslinking agent, 4-8 parts of a functional monomer and 0.4-1 part of an initiator, and continuously stirring to obtain a nuclear monomer pre-emulsion;
(c) heating the reactor in the step (a), adding 2-5 parts of the nuclear monomer pre-emulsion obtained in the step (b) into the reactor, adding 0.4-1 part of an initiator, and preserving heat;
(d) dropwise adding the residual nuclear monomer pre-emulsion into a reactor, and preserving heat after dropwise adding is finished to obtain nuclear monomer emulsion;
(e) preparing a shell monomer pre-emulsion: adding 100-200 parts of deionized water and 3-7 parts of an emulsifier into a pre-emulsification cylinder, stirring, then adding 40-80 parts of methyl methacrylate, 130-260 parts of isooctyl acrylate, 7-15 parts of methacrylic acid, 3-7 parts of an internal crosslinking agent, 6-12 parts of a functional monomer and 0.4-1 part of an initiator, and continuously stirring to obtain a shell monomer pre-emulsion;
(f) dropwise adding the shell monomer pre-emulsion obtained in the step (e) into the core monomer emulsion obtained in the step (d), and preserving heat after dropwise adding;
(g) after the heat preservation in the step (f) is finished, cooling, then adding 0.5-1 part of oxidant, preserving heat for 20-30min, adding 0.5-1 part of reducing agent, and preserving heat for 30-60 min;
(h) and (g) after the heat preservation is finished, cooling, adding 10-15 parts of a pH regulator, then adding 1.5-2.5 parts of a defoaming agent and 5-10 parts of a bactericide, preserving heat, and stirring to obtain the aqueous wood lacquer emulsion.
Preferably, the stirring in step (b) is continued for 20-60min, such as 20min, 30min, 40min, 50min or 60 min.
Preferably, the temperature increase in step (c) is to 85-90 ℃, such as 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃ or 90 ℃ and the like.
Preferably, the incubation time in step (c) is 10-30min, such as 10min, 20min or 30 min.
Preferably, the dropwise addition of the remaining nuclear monomer pre-emulsion in the step (d) is completed within 90-180min (e.g., 90min, 120min, 150min, 180min, etc.) at 85-90 ℃ (e.g., 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃, or 90 ℃, etc.).
Preferably, the incubation time in step (d) is 30-60min, such as 30min, 40min, 50min or 60 min.
Preferably, the stirring in step (e) is continued for 20-60min, such as 20min, 30min, 40min, 50min or 60 min.
Preferably, the step (f) of adding dropwise the shell monomer pre-emulsion obtained in the step (e) to the core monomer emulsion obtained in the step (d) is completed within 90-180min (e.g. 90min, 120min, 150min or 180min, etc.) at 85-90 ℃ (e.g. 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃ or 90 ℃, etc.).
Preferably, the incubation time in step (f) is 60-120min, such as 60min, 80min, 100min or 120 min.
Preferably, the temperature reduction in step (g) is to be reduced to 65-75 ℃, such as 65 ℃, 68 ℃, 70 ℃, 73 ℃ or 75 ℃ and the like.
Preferably, the temperature reduction in step (h) is to be below 50 ℃, such as 50 ℃, 45 ℃, 40 ℃ or 35 ℃ and the like.
Preferably, the stirring time in step (h) is 10-20min, such as 10min, 13min, 15min, 18min or 20min, etc.
As a preferred technical scheme, the preparation method of the aqueous wood lacquer emulsion comprises the following steps:
(a) preparing a kettle bottom solution: adding 200 and 400 parts of deionized water and 4-8 parts of emulsifier into the reactor, and stirring to obtain a kettle bottom solution;
(b) preparation of nuclear monomer pre-emulsion: adding 100-200 parts of deionized water and 3-7 parts of emulsifier into a pre-emulsification cylinder, stirring, then adding 50-150 parts of styrene, 150-320 parts of methyl methacrylate, 5-9 parts of methacrylic acid, 0-30 parts of butyl acrylate, 1-3 parts of internal crosslinking agent, 4-8 parts of functional monomer and 0.4-1 part of initiator, and continuing stirring for 20-60min to obtain nuclear monomer pre-emulsion;
(c) heating the reactor in the step (a) to 85-90 ℃, adding 2-5 parts of the nuclear monomer pre-emulsion obtained in the step (b) into the reactor, adding 0.4-1 part of an initiator, and preserving heat for 10-30 min;
(d) dropwise adding the rest nuclear monomer pre-emulsion into a reactor, dropwise adding for 90-180min at 85-90 ℃, and after dropwise adding, preserving heat for 30-60min at 85-90 ℃ to obtain nuclear monomer emulsion;
(e) preparing a shell monomer pre-emulsion: adding 100-200 parts of deionized water and 3-7 parts of an emulsifier into a pre-emulsification cylinder, stirring, then adding 40-80 parts of methyl methacrylate, 130-260 parts of isooctyl acrylate, 7-15 parts of methacrylic acid, 3-7 parts of an internal crosslinking agent, 6-12 parts of a functional monomer and 0.4-1 part of an initiator, and continuously stirring for 20-60min to obtain a shell monomer pre-emulsion;
(f) dropwise adding the shell monomer pre-emulsion obtained in the step (e) into the core monomer emulsion obtained in the step (d), dropwise adding for 90-180min at the temperature of 85-90 ℃, and preserving heat for 60-120min at the temperature of 85-90 ℃ after dropwise adding;
(g) and (3) post-treatment: after the heat preservation in the step (f) is finished, cooling to 65-75 ℃, then adding 0.5-1 part of oxidant, preserving heat for 20-30min, then adding 0.5-1 part of reducing agent, and preserving heat for 30-60 min;
(h) post-addition: and (g) after the heat preservation is finished, cooling to below 50 ℃, adding 10-15 parts of pH regulator, then adding 1.5-2.5 parts of defoaming agent and 5-10 parts of bactericide, preserving heat, and stirring for 10-20min to obtain the aqueous wood lacquer emulsion.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the invention, the core monomer Tg is controlled to be 90-110 ℃ and the shell monomer Tg is controlled to be-40-20 ℃ by controlling the core-shell monomer dropping process, so that the water-based acrylic emulsion with high Tg and low film forming temperature can be obtained; by introducing the internal crosslinking agent of ethoxylated trimethylolpropane triacrylate, on one hand, a flexible chain segment is introduced, so that the flexibility of the emulsion can be improved, and on the other hand, the emulsion structure is changed from a linear structure into a compact net structure, so that the drying speed and the resistance can be improved; by introducing the functional monomer of methacrylamide ethyl ethylene urea, the Tg of the emulsion can be improved on one hand, and the cohesive force of the emulsion can be improved on the other hand, so that the hardness and the adhesive force of the emulsion can be obviously improved. The three aspects act together to ensure that the synthesized aqueous wood lacquer emulsion has higher hardness, faster drying speed (surface drying time is 10-15min), better tolerance and better flexibility after being formed into a film, better meets the requirement of the aqueous wood lacquer coating on the aqueous wood lacquer emulsion and better expands the application range of the aqueous wood lacquer coating.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Examples 1 to 5
In examples 1-5, an aqueous wood lacquer emulsion is provided, wherein the raw materials and the amount of the aqueous wood lacquer emulsion are shown in table 1.
TABLE 1
The materials represented by the abbreviations of the raw materials in Table 1 and the manufacturers are as follows:
AR-10: allyloxy aromatic alcohol ethoxylate ammonium sulfate, first pharmaceutical of manufacturer japan;
SR-10: ammonium vinyl polyoxyethylene alkyl thionate, ledike, manufacturer;
LR-10: fatty alcohol reaction type emulsifier, made by Nanjing chess of manufacturer;
KPS: potassium persulfate, a good fortune establishing minor of the manufacturer;
NPS: sodium persulfate, a good fortune establishing minor of the manufacturer;
APS: ammonium persulfate, manufacturer Fujian Ming Lin;
TMP3 EOTA: ethoxylated trimethylolpropane triacrylate, commercially available Navigator Biotech Ltd;
MAEEU: methacrylamide ethyl ethylene urea, manufacturer solvi;
ST: styrene, a commercial shanghai friendship;
BA: butyl acrylate, manufacturer basf;
MMA: methyl methacrylate, manufactured by shanghai friendship;
MAA: methacrylic acid, shanghai friendship of the manufacturer;
2-EHA: isooctyl acrylate, a shanghai friendship from the manufacturer;
TBHP: t-butyl hydroperoxide, Pestar chemical Co., Ltd;
LQ-TBCP: tert-butyl cumyl peroxide, manufactured by hand-in-hand, by the scientific and technological Limited;
NaHSO 3: sodium bisulfite, a manufacturer Zhentai chemical industry;
VC: l-ascorbic acid, manufacturer gold, Rich source Biotech limited;
WBA: mineral oil antifoam, manufacturer basf;
NXZ: mineral oil antifoam, manufacturer nopopucace.
C, loosening: 1.5, manufacturer Hoffman;
the BIT: 5% content, manufacturer Hoffman.
The preparation method of the aqueous wood lacquer emulsion in the embodiments 1 to 5 comprises the following steps:
(a) preparing a kettle bottom solution: adding deionized water and an emulsifier into a reactor according to the formula of the bottom of the kettle in the table 1, and uniformly stirring to obtain a kettle bottom solution;
(b) preparation of nuclear monomer pre-emulsion: adding deionized water and an emulsifier into a pre-emulsification cylinder according to the formula of the nuclear monomer pre-emulsion in the table 1, stirring, then adding styrene, methyl methacrylate, methacrylic acid, butyl acrylate, an internal crosslinking agent, a functional monomer and an initiator, and continuously stirring for 40min to obtain the nuclear monomer pre-emulsion;
(c) heating the reactor in the step (a) to 90 ℃, adding 5 parts of the nuclear monomer pre-emulsion obtained in the step (b) into the reactor, adding an initiator according to the amount of the bottom of the kettle in the table 1, and keeping the temperature for 20 min;
(d) dropwise adding the rest nuclear monomer pre-emulsion into a reactor, dropwise adding for 120min at 90 ℃, and after dropwise adding, preserving heat for 40min at 90 ℃ to obtain a nuclear monomer emulsion;
(e) preparation of a shell monomer pre-emulsion: adding deionized water and an emulsifier into a pre-emulsification cylinder according to the formula of the shell monomer pre-emulsion in the table 1, stirring, then adding methyl methacrylate, isooctyl acrylate, methacrylic acid, an internal crosslinking agent, a functional monomer and an initiator, and continuously stirring for 40min to obtain a shell monomer pre-emulsion;
(f) dropwise adding the shell monomer pre-emulsion obtained in the step (e) into the core monomer emulsion obtained in the step (d), dropwise adding for 120min at the temperature of 90 ℃, and after dropwise adding, keeping the temperature for 100min at the temperature of 90 ℃;
(g) and (3) post-treatment: after the heat preservation in the step (f) is finished, cooling to 65 ℃, adding an oxidant according to the formula of the post-treatment agent in the table 1, preserving the heat for 30min, adding a reducing agent, and preserving the heat for 30-60 min;
(h) post-addition: and (g) after the heat preservation is finished, cooling to below 50 ℃, adding a pH regulator according to the formula of the later additive in the table 1, then adding a defoaming agent and a bactericide, preserving the heat, and stirring for 15min to obtain the water-based wood lacquer emulsion.
Comparative example 1
The difference between the comparative example and the example 1 is that the internal crosslinking agent in the raw materials for preparing the aqueous wood lacquer emulsion is 3 parts by weight, that is, the internal crosslinking agent is not added in the preparation process of the core monomer pre-emulsion, and the internal crosslinking agent is added in the preparation process of the shell monomer pre-emulsion.
Comparative example 2
The difference between the comparative example and the example 1 is that the weight part of the internal crosslinking agent in the raw materials for preparing the aqueous wood lacquer emulsion is 1 part, namely, the internal crosslinking agent is added in the preparation process of the core monomer pre-emulsion, and the internal crosslinking agent is not added in the preparation process of the shell monomer pre-emulsion.
Comparative example 3
The difference between the comparative example and the example 1 is that the raw materials for preparing the aqueous wood lacquer emulsion do not include the internal cross-linking agent, i.e., the internal cross-linking agent is not added in the preparation process of the core monomer pre-emulsion and the shell monomer pre-emulsion.
Comparative example 4
The difference between the comparative example and the example 1 is only that the weight part of the functional monomer in the raw material for preparing the aqueous wood lacquer emulsion is 6 parts, namely, the functional monomer is not added in the preparation process of the core monomer pre-emulsion, and the functional monomer is added in the preparation process of the shell monomer pre-emulsion.
Comparative example 5
The difference between the comparative example and the example 1 is only that the weight part of the functional monomer in the raw material for preparing the aqueous wood lacquer emulsion is 4 parts, namely, the functional monomer is added in the preparation process of the core monomer pre-emulsion, and the functional monomer is not added in the preparation process of the shell monomer pre-emulsion.
Comparative example 6
The difference between the comparative example and the example 1 is that the raw materials for preparing the aqueous wood lacquer emulsion do not include functional monomers, i.e., the functional monomers are not added in the preparation process of the core monomer pre-emulsion and the shell monomer pre-emulsion.
Comparative example 7
This comparative example differs from example 1 only in that the internal crosslinking agent ethoxylated trimethylolpropane triacrylate was replaced with an equal amount of trimethylolpropane triacrylate.
Comparative example 8
This comparative example differs from example 1 only in that the functional monomer methacrylamide ethylethyleneurea was replaced by an equal amount of acrylamide.
Comparative example 9
Wood lacquer emulsion prepared according to CN110964400A example 1.
The water-based wood lacquer emulsion prepared in the embodiment and the proportion is subjected to performance test, wherein the flexibility is tested according to the method of GB/T1731-1993 and is scored according to 1-5, and the higher the score is, the better the flexibility is; other performances are tested by adopting a paint film testing method in GB/T23999-2009 waterborne wood paint for interior decoration.
The results of the performance tests are shown in table 2.
TABLE 2
As can be seen from Table 2, when the aqueous wood lacquer emulsion provided by the embodiments 1-5 of the invention is applied to an aqueous wood lacquer coating, the drying speed is high (the surface drying time is 10-15min), the paint film hardness is high, the adhesion to a base material is good (0-1 level), and the water resistance and the alcohol resistance are good. The combination property of the embodiment 4 is the best, the surface drying time is only 10min, and the adhesive force is 0 grade.
Compared with the embodiment 1, when the aqueous wood lacquer emulsion provided by the comparative examples 1 to 8 is applied to the aqueous wood lacquer coating, the drying speed is obviously slowed down, the hardness of the lacquer film is deteriorated, the adhesive force to the base material is deteriorated, and the flexibility is deteriorated.
Although comparative example 9 provided an aqueous wood lacquer emulsion that dried faster than example 1, it was significantly less flexible.
The applicant states that the present invention is illustrated by the above examples and the preparation method of the aqueous wood lacquer emulsion of the present invention, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must rely on the above examples to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
2. The aqueous wood lacquer emulsion according to claim 1, wherein the emulsifier is a reactive emulsifier comprising any one of SR-10, AR-10 or LR-10 or a combination of at least two thereof.
3. The aqueous wood lacquer emulsion according to claim 1 or 2, wherein the initiator comprises any one of potassium persulfate, sodium persulfate, or ammonium persulfate, or a combination of at least two thereof.
4. The aqueous wood lacquer emulsion according to any one of claims 1 to 3, wherein the oxidizing agent comprises t-butyl hydroperoxide and/or t-butyl cumyl peroxide.
5. The aqueous wood lacquer emulsion according to any one of claims 1 to 4, wherein the reducing agent comprises sodium bisulfite or ascorbic acid.
6. The aqueous wood lacquer emulsion according to any one of claims 1-5, wherein the pH regulator comprises 25% strength ammonia.
7. The aqueous wood lacquer emulsion according to any one of claims 1-6, wherein the defoamer comprises a mineral oil defoamer;
preferably, the biocide comprises cason and/or BIT.
8. The method for preparing the aqueous wood lacquer emulsion according to any one of claims 1 to 7, wherein the method comprises the following steps:
(a) preparing a kettle bottom solution: adding 200 and 400 parts of deionized water and 4-8 parts of emulsifier into the reactor, and stirring to obtain a kettle bottom solution;
(b) preparation of nuclear monomer pre-emulsion: adding 100-200 parts of deionized water and 3-7 parts of an emulsifier into a pre-emulsification cylinder, stirring, then adding 50-150 parts of styrene, 150-320 parts of methyl methacrylate, 5-9 parts of methacrylic acid, 0-30 parts of butyl acrylate, 1-3 parts of an internal crosslinking agent, 4-8 parts of a functional monomer and 0.4-1 part of an initiator, and continuing stirring to obtain a nuclear monomer pre-emulsion;
(c) heating the reactor in the step (a), adding 2-5 parts of the nuclear monomer pre-emulsion obtained in the step (b) into the reactor, adding 0.4-1 part of an initiator, and preserving heat;
(d) dropwise adding the rest nuclear monomer pre-emulsion into the reactor, and preserving heat after dropwise adding to obtain nuclear monomer emulsion;
(e) preparation of a shell monomer pre-emulsion: adding 100-200 parts of deionized water and 3-7 parts of an emulsifier into a pre-emulsification cylinder, stirring, then adding 40-80 parts of methyl methacrylate, 130-260 parts of isooctyl acrylate, 7-15 parts of methacrylic acid, 3-7 parts of an internal crosslinking agent, 6-12 parts of a functional monomer and 0.4-1 part of an initiator, and continuously stirring to obtain a shell monomer pre-emulsion;
(f) dropwise adding the shell monomer pre-emulsion obtained in the step (e) into the core monomer emulsion obtained in the step (d), and preserving heat after dropwise adding;
(g) after the heat preservation in the step (f) is finished, cooling, then adding 0.5-1 part of oxidant, preserving heat for 20-30min, then adding 0.5-1 part of reducing agent, preserving heat for 30-60 min;
(h) and (g) after the heat preservation is finished, cooling, adding 10-15 parts of a pH regulator, then adding 1.5-2.5 parts of a defoaming agent and 5-10 parts of a bactericide, preserving heat, and stirring to obtain the aqueous wood lacquer emulsion.
9. The method of claim 8, wherein the stirring of step (b) is continued for 20-60 min;
preferably, the temperature rise in the step (c) is to 85-90 ℃;
preferably, the time for the heat preservation in the step (c) is 10-30 min;
preferably, the dropwise addition of the remaining nuclear monomer pre-emulsion in the step (d) is completed within 90-180min at 85-90 ℃;
preferably, the time for the heat preservation in the step (d) is 30-60 min;
preferably, the stirring of step (e) is continued for a period of 20-60 min.
10. The process according to claim 8 or 9, wherein the step (f) of adding dropwise the shell monomer pre-emulsion obtained in step (e) to the core monomer emulsion obtained in step (d) is carried out at 85 ℃ to 90 ℃ within 90 to 180 min;
preferably, the time for the heat preservation in the step (f) is 60-120 min;
preferably, the temperature reduction of the step (g) is to be reduced to 65-75 ℃;
preferably, the temperature reduction in the step (h) is to be reduced to below 50 ℃;
preferably, the stirring time of step (h) is 10-20 min.
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EP3115846A1 (en) * | 2015-07-06 | 2017-01-11 | Betek Boya ve Kimya Sanayi A.S. | Core-shell type binder and a method for preparation thereof |
CN111944103A (en) * | 2020-07-29 | 2020-11-17 | 中国科学院化学研究所 | Water-based acrylic emulsion and preparation method and application thereof |
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EP3115846A1 (en) * | 2015-07-06 | 2017-01-11 | Betek Boya ve Kimya Sanayi A.S. | Core-shell type binder and a method for preparation thereof |
CN106243273A (en) * | 2016-07-29 | 2016-12-21 | 肇庆浩城树脂科技有限公司 | A kind of hydroxyl acrylic emulsion with nucleocapsid structure and preparation method and application |
CN111944103A (en) * | 2020-07-29 | 2020-11-17 | 中国科学院化学研究所 | Water-based acrylic emulsion and preparation method and application thereof |
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