CN103613702A - Aqueous multi-functional crylic acid extinction resin and preparation method thereof - Google Patents
Aqueous multi-functional crylic acid extinction resin and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an aqueous multi-functional crylic acid extinction resin and a preparation method thereof and belongs to the field of extinction type coatings. The preparation method of the aqueous multi-functional crylic acid extinction resin comprises the following steps: (1) preparing a crylic acid ester mixture monomer; (2) sufficiently mixing water, an emulsifier and a part of the crylic acid ester mixture monomer, heating to 70-90 DEG C, adding an initiator to react for 0.5-1 hour, dropwise adding the rest crylic acid ester mixture monomer within 3-5 hours, adding the rest initiator in different batches, performing heat preservation for 1-3 hours after the dropwise adding, cooling to 45 DEG C, sequentially adding modified silicon dioxide and an organic thermosetting polymethylurea resin with the particle size of 3.5mu m, uniformly stirring, cooling down and discharging so as to obtain the aqueous multi-functional crylic acid extinction resin. The aqueous multi-functional crylic acid extinction resin prepared by the preparation method disclosed by the invention is high in extinction efficiency, excellent in water resistance, acid resistance and alkali resistance, and good in abrasion resistance property.
Description
Technical field
The invention belongs to extinction type paint field, particularly a kind of water-soluble multifunctional acrylic matting resin and preparation method thereof.
Background technology
In recent years, along with scientific and technological development and the raising of people's living standard, people sharply increase having the coatings with low gloss finish demand of soft outward appearance, but the extinction type coating in producing adopts solvent type resin as carrier mostly, use the organic solvents such as a large amount of DMF, TOL and MEK, when coating drying and forming-film, solvent evaporates causes environmental pollution, harm human consumer, constructor's health, does not meet the current requirement to coating environmental protection.In addition, owing to containing a large amount of inflammable solvents, there is certain potential safety hazard in solvent type resin in the process that stores and transport.
Widespread demand water-based Flat paint in recent years, the water-based delustring paint that the acrylic resin of take is matrix resin, principal feature is that sticking power is good, yellowing resistance is excellent, has good avidity, low production cost with mineral filler; Yet, their anti-chemical, anti-scar, wear resistance and hardness of paint film, fullness ratio are poor, and over-all properties is general, and construction easily produces defect.
The shortcoming such as water-miscible paint clear finish in the market exists water tolerance, anti-chemical is poor, hardness is low, fullness ratio, feel, resistance to blocking are poor.
Summary of the invention
Primary and foremost purpose of the present invention is to overcome the deficiencies in the prior art, and a kind of water-soluble multifunctional acrylic matting resin is provided, and it can improve water-fast, acidproof, the alkali resistance of water-based Flat paint effectively; Improve chemical resistant properties and the wear resistance of filming, the silicon-dioxide of introducing and organic thermoset gather MU resin, can strengthen hardness and the non-melt character of coating, thereby strengthen the overall tolerance performance of coating; Organic thermoset gathers the hydroxyl generation etherification reaction in MU resin and acrylic resin simultaneously, improves physical strength and the surperficial erasibility of matting resin; Filming of obtaining has warm appearance effect, and eliminate optical property is excellent.
Another object of the present invention is to provide the preparation method of described water-soluble multifunctional acrylic matting resin.
Object of the present invention is achieved through the following technical solutions: a kind of water-soluble multifunctional acrylic matting resin, comprises following by the component of mass parts:
Described acrylate mixing monomer is preferably by the unsaturated acrylic ester monomer of hydroxyl, carboxylic unsaturated acrylic ester monomer and free-radical polymerised acrylic ester monomer and forms; Wherein, in acrylate mixing monomer, the mass fraction of various monomers is preferably:
The unsaturated acrylic ester monomer of hydroxyl: 5-10 part
Carboxylic unsaturated acrylic ester monomer: 0.5-1.5 part
Free-radical polymerised acrylic ester monomer: 21.8-48.2 part
The unsaturated acrylic ester monomer of described hydroxyl is preferably at least one in (methyl) vinylformic acid-2-hydroxyl ethyl ester, (methyl) vinylformic acid 2-hydroxypropyl acrylate, (methyl) vinylformic acid 2-hydroxy butyl ester, polypropylene glycol monomethacrylate or polypropylene glycol mono acrylic ester;
Described carboxylic unsaturated acrylic ester monomer is preferably one or both in methacrylic acid or vinylformic acid;
Described free-radical polymerised acrylic ester monomer is preferably (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) butyl acrylate, (methyl) 2-EHA, (methyl) lauryl acrylate, (methyl) tridecyl acrylate, (methyl) stearyl acrylate ester, (methyl) cyclohexyl acrylate, the two or more monomers in acrylamide or vinylbenzene;
In described acrylate mixing monomer, the mass fraction of various monomers forms more preferably:
Described emulsifying agent is preferably the composite emulsifier that sodium lauryl sulphate and polyoxyethylene-8-octyl phenyl ether form for 3:1 ratio in mass ratio; Described emulsifying agent add-on is 3% of acrylate mixing monomer total amount;
Described initiator is preferably a kind of in Potassium Persulphate, Sodium Persulfate or ammonium persulphate;
The solution that described initiator is mixed with massfraction 5% is used;
Described basic cpd is a kind of in ethamine, propylamine, butylamine, benzylamine, monoethanolamine, neopentyl alcohol amine, 2-aminopropanol, 3-aminopropanol, diethylamine, triethylamine, Isopropylamine, Diisopropylamine, tri-isopropyl amine, diethanolamine, diisopropanolamine (DIPA), trolamine, dimethylethanolamine, diethylethanolamine, amine water, sodium hydroxide or potassium hydroxide; From over-all properties, consider, select sodium hydroxide best; By these alkaline matter regulation system pH to 8.0-10.0; Preferred 8.5-9.5.
Described improved silica dispersion liquid prepares by following method:
Tetraethoxy, ethanol, hydromassage that, than mixing for 1:4:8, are heated to 50～75 ℃, and with hydrochloric acid regulation system pH to 3～4, holding temperature sustained reaction 8～12h under churned mechanically condition, obtains SiO
2alcosol, the SiO making
2in alcosol, add silane coupling agent, condensing reflux 2～3h under 75～80 ℃ of condition of water bath heating, cooling, obtain organic-silicon-modified silica dispersions.
Described hydrochloric acid is preferably the hydrochloric acid of 0.1mol/L;
Described silane coupling agent is preferably vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane, 3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane, at least one in γ-aminopropyl triethoxysilane, γ-(the rare acyl-oxygen of methyl-prop) propyl trimethoxy silicane, γ-mercaptopropyl trimethoxysilane or γ-glycidyl ether Trimethoxy silane; Described silane coupling agent add-on is 10%～15% of tetraethoxy quality used; Described silane coupling agent is 3-(iso-butylene acyl-oxygen more preferably) propyl trimethoxy silicane;
The poly-MU resin of described organic thermoset is preferably particle diameter 3.5um;
Described water is deionized water;
The preparation method of above-mentioned water-soluble multifunctional acrylic matting resin, comprises the following steps:
(1) by hydroxyethyl methylacrylate, methyl methacrylate, acrylamide, methacrylic acid, butyl acrylate, styrene monomer mixes, and obtains acrylate mixing monomer, standby;
(2) under the protection of nitrogen, acrylate mixing monomer prepared by water intaking, 1/4 step (1), the aqueous solution and the emulsifying agent of 1/4 initiator, mix, and at 75～85 ℃ of reaction 0.5～1h, makes seed emulsion; Acrylate mixing monomer prepared by then dropping residue 3/4 step (1) and the aqueous solution of 3/4 initiator, time for adding is controlled at 3～5h, dropwise rear insulation 1～3h, after being cooled to room temperature, add basic cpd to regulate pH value of reaction system to 8.0～10.0, obtain water dispersible acrylate copolymer;
(3) by improved silica dispersion liquid, the poly-MU resin of organic thermoset adds in reactor, and mechanical stirring 1～2h under high-speed stirring condition, prepares water-soluble multifunctional acrylic matting resin.
Being applied as of described water-soluble multifunctional acrylic matting resin is coated to woodenware by water-soluble multifunctional acrylic matting resin finished product or drying and forming-film above metal device, can obtain the film coated surface of gloss below 30.
Reaction principle of the present invention is:
The 1st elementary reaction of the water-soluble multifunctional acrylic matting resin in the present invention, the unsaturated monomer that contains hydroxyl, the unsaturated monomer that contains carboxyl and other free-radical polymerised unsaturated acrylic ester monomer are carried out to letex polymerization, obtain water dispersible acrylate copolymer; The 2nd elementary reaction, obtains silicon-dioxide oligopolymer by tetraethoxy acid-catalyzed hydrolysis reaction in ethanol-water solution, then reacts with silane coupling agent, obtains organic-silicon-modified silica dispersions; The organic-silicon-modified silica dispersions then the 2nd stage being obtained, in the water dispersible acrylate copolymer that the poly-MU resin dispersion of organic thermoset obtained in the 1st stage, forms water-soluble multifunctional acrylic matting resin after stirring.
The present invention compared with prior art has following features:
1. the water-soluble multifunctional acrylic matting resin preparing is usingd water as dispersion medium, and VOC content is low, and smell is little, nontoxic pollution-free;
2. the water-soluble multifunctional acrylic matting resin extinction effect preparing is good, is uniformly dispersed, and stability in storage is good;
3. the water-soluble multifunctional acrylic matting resin preparing, has introduced the poly-MU resin of silicon-dioxide and organic thermoset, has strengthened hardness and the non-melt character of coating, thereby strengthens the overall tolerance performance of coating.
4. the water-soluble multifunctional acrylic matting resin water tolerance preparing, acidproof, alkaline resistance properties good, and paint film appearance effect is excellent.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
(1) prepare organosilicon improved silica dispersion liquid: by tetraethoxy, ethanol, hydromassage you than mixing for 1:4:8, be heated to 55 ℃, with 0.1mol/L hydrochloric acid regulation system pH to 3, under churned mechanically condition, holding temperature sustained reaction 8h, obtains SiO
2alcosol, the SiO making
2in alcosol, add 4.06 parts of 3-(iso-butylene acyl-oxygens) propyl trimethoxy silicane, condensing reflux 2h under 75 ℃ of condition of water bath heating, cooling, obtain organic-silicon-modified silica dispersions.
(2) by 5 mass parts hydroxyethyl methylacrylates, 5 mass parts methyl methacrylates, 0.8 mass parts acrylamide, 0.5 mass parts methacrylic acid, 12 mass parts butyl acrylates, 4 mass parts styrene monomers mix, and make acrylate mixing monomer standby.
(3) under the protection of nitrogen, get acrylate mixing monomer, 0.0410 mass parts initiator prepared by 102 mass parts water, 1/4 step (2), 0.6145 mass parts sodium lauryl sulphate and 0.2048 mass parts polyoxyethylene-8-octyl phenyl ether composite emulsifier, mix, at 80 ℃ of reaction 0.5h, make seed emulsion; Then drip remaining 3/4 acrylate mixing monomer and 0.1228 mass parts initiator, time for adding is controlled at 3h, dropwise rear insulation 1h, be cooled to after room temperature and add basic cpd to regulate pH value of reaction system to 9.0, obtain water dispersible acrylate copolymer.
(4) by 10 parts of improved silica dispersion liquids, 0.55 part of organic matting agent adds in reactor, and mechanical stirring 1h under high-speed stirring condition, prepares water-soluble multifunctional acrylic matting resin.
Embodiment 2
(1) preparation method of organic-silicon-modified silica dispersions is with embodiment 1 step (1).
(2) 6 mass parts hydroxyethyl methylacrylates, 7 mass parts methyl methacrylates, 2.6 mass parts acrylamides, 1.0 mass parts methacrylic acids, 18 mass parts butyl acrylates, 5 mass parts styrene monomers;
(3) under the protection of nitrogen, get acrylate mixing monomer, 0.05940 mass parts initiator prepared by 121 mass parts water, 1/4 step (1), 0.891 mass parts sodium lauryl sulphate and 0.297 mass parts polyoxyethylene-8-octyl phenyl ether composite emulsifier, mix, at 75～85 ℃ of reaction 0.5～1h, make seed emulsion; Then drip remaining 3/4 acrylate mixing monomer and 0.1782 mass parts initiator, time for adding is controlled at 4h, dropwise rear insulation 2h, be cooled to after room temperature and add basic cpd to regulate pH value of reaction system to 9.5, obtain water dispersible acrylate copolymer.
(4) by 20 parts of improved silica dispersion liquids, 0.79 part of organic matting agent is put into reactor, and mechanical stirring 1h under high-speed stirring condition, prepares multifunctional water-soluble acrylic matting resin.
Embodiment 3
(1) prepare organosilicon improved silica dispersion liquid: by tetraethoxy, ethanol, hydromassage you than mixing for 1:4:8, be heated to 70 ℃, with 0.1mol/L hydrochloric acid regulation system pH to 4, under churned mechanically condition, holding temperature sustained reaction 12h, obtains SiO
2alcosol, the SiO making
2in alcosol, add 4.69 parts of 3-(iso-butylene acyl-oxygens) propyl trimethoxy silicane, condensing reflux 3h under 80 ℃ of condition of water bath heating, cooling, obtain organic-silicon-modified silica dispersions.
(2) 10 mass parts hydroxyethyl methylacrylates, 8 mass parts methyl methacrylates, 3.2 mass parts acrylamides, 1.5 mass parts methacrylic acids, 30 mass parts butyl acrylates, 7 mass parts styrene monomers;
(3) under the protection of nitrogen, get acrylate mixing monomer, 0.090 mass parts initiator prepared by 186 mass parts water, 1/4 step (2), 1.3432 mass parts sodium lauryl sulphate and 0.4478 mass parts polyoxyethylene-8-octyl phenyl ether composite emulsifier, mix, at 85 ℃ of reaction 1h, make seed emulsion; Then drip remaining 3/4 acrylate mixing monomer and 0.2682 mass parts initiator, time for adding is controlled at 5h, dropwise rear insulation 3h, be cooled to after room temperature and add basic cpd to regulate pH value of reaction system to 9.5, obtain water dispersible acrylate copolymer.
(4) by 25 parts of improved silica dispersion liquids, 1.80 parts of organic matting agents are put into reactor, and mechanical stirring 1.5h under high-speed stirring condition, prepares multifunctional water-soluble acrylic matting resin.
The matting resin that embodiment 1-3 is obtained is placed in glassware seasoning seven days, in the baking oven of 50 ℃, be dried again 24h, filming of obtaining has following performance: water tolerance 10 days is unchanged, alkali resistance (3%NaOH) 7 days is unchanged, acidproof (hydrochloric acid soln of pH=4) 7 days is unchanged, washable Shua≤10000 time, glossiness (60 °) is respectively 30%, 23%, 28%.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (10)
1. a water-soluble multifunctional acrylic matting resin, is characterized in that comprising following by the component of mass parts:
2. water-soluble multifunctional acrylic matting resin according to claim 1, is characterized in that: described acrylate mixing monomer is for to be comprised of the unsaturated acrylic ester monomer of hydroxyl, carboxylic unsaturated acrylic ester monomer and free-radical polymerised acrylic ester monomer; Wherein, in acrylate mixing monomer, the mass fraction of various monomers is:
The unsaturated acrylic ester monomer of hydroxyl: 5-10 part
Carboxylic unsaturated acrylic ester monomer: 0.5-1.5 part
Free-radical polymerised acrylic ester monomer: 21.8-48.2 part.
3. water-soluble multifunctional acrylic matting resin according to claim 2, is characterized in that: the unsaturated acrylic ester monomer of described hydroxyl is at least one in (methyl) vinylformic acid-2-hydroxyl ethyl ester, (methyl) vinylformic acid 2-hydroxypropyl acrylate, (methyl) vinylformic acid 2-hydroxy butyl ester, polypropylene glycol monomethacrylate or polypropylene glycol mono acrylic ester;
Described carboxylic unsaturated acrylic ester monomer is one or both in methacrylic acid or vinylformic acid;
Described free-radical polymerised acrylic ester monomer is the two or more monomers in (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) butyl acrylate, (methyl) 2-EHA, (methyl) lauryl acrylate, (methyl) tridecyl acrylate, (methyl) stearyl acrylate ester, (methyl) cyclohexyl acrylate, acrylamide or vinylbenzene.
4. water-soluble multifunctional acrylic matting resin according to claim 3, is characterized in that: in described acrylate mixing monomer, the mass fraction of various monomers consists of:
5. water-soluble multifunctional acrylic matting resin according to claim 1, is characterized in that: described emulsifying agent is that sodium lauryl sulphate and polyoxyethylene-8-octyl phenyl ether are 3:1 ratio composition composite emulsifier in mass ratio; Described emulsifying agent add-on is 3% of acrylate mixing monomer total amount.
6. water-soluble multifunctional acrylic matting resin according to claim 1, is characterized in that: described initiator is a kind of in Potassium Persulphate, Sodium Persulfate or ammonium persulphate;
The solution that described initiator is mixed with massfraction 5% is used;
Described basic cpd is a kind of in ethamine, propylamine, butylamine, benzylamine, monoethanolamine, neopentyl alcohol amine, 2-aminopropanol, 3-aminopropanol, diethylamine, triethylamine, Isopropylamine, Diisopropylamine, tri-isopropyl amine, diethanolamine, diisopropanolamine (DIPA), trolamine, dimethylethanolamine, diethylethanolamine, amine water, sodium hydroxide or potassium hydroxide;
The poly-MU resin of described organic thermoset is particle diameter 3.5um;
Described water is deionized water.
7. water-soluble multifunctional acrylic matting resin according to claim 1, is characterized in that: described improved silica dispersion liquid prepares by following method:
Tetraethoxy, ethanol, hydromassage that, than mixing for 1:4:8, are heated to 50～75 ℃, and with hydrochloric acid regulation system pH to 3～4, holding temperature sustained reaction 8～12h under churned mechanically condition, obtains SiO
2alcosol, the SiO making
2in alcosol, add silane coupling agent, condensing reflux 2～3h under 75～80 ℃ of condition of water bath heating, cooling, obtain organic-silicon-modified silica dispersions.
8. water-soluble multifunctional acrylic matting resin according to claim 7, is characterized in that:
Described hydrochloric acid is the hydrochloric acid of 0.1mol/L;
Described silane coupling agent is vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane, 3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane, at least one in γ-aminopropyl triethoxysilane, γ-(the rare acyl-oxygen of methyl-prop) propyl trimethoxy silicane, γ-mercaptopropyl trimethoxysilane or γ-glycidyl ether Trimethoxy silane; Described silane coupling agent add-on is 10%～15% of tetraethoxy quality used.
9. the preparation method of the water-soluble multifunctional acrylic matting resin described in claim 1～8 any one, is characterized in that comprising the following steps:
(1) by hydroxyethyl methylacrylate, methyl methacrylate, acrylamide, methacrylic acid, butyl acrylate, styrene monomer mixes, and obtains acrylate mixing monomer, standby;
(2) under nitrogen protection, acrylate mixing monomer prepared by water intaking, 1/4 step (1), 1/4 initiator and emulsifying agent, mix, and at 75～85 ℃ of reaction 0.5～1h, makes seed emulsion; Then drip acrylate mixing monomer prepared by remaining 3/4 step (1) and 3/4 initiator, time for adding is controlled at 3～5h, dropwise rear insulation 1～3h, after being cooled to room temperature, add basic cpd to regulate pH value of reaction system to 8.0～10.0, obtain water dispersible acrylate copolymer;
(3) by improved silica dispersion liquid, the poly-MU resin of organic thermoset is put into reactor, and mechanical stirring 1～2h under high-speed stirring condition, prepares water-soluble multifunctional acrylic matting resin.
10. the application of the water-soluble multifunctional acrylic matting resin described in claim 1～8 any one, is characterized in that water-soluble multifunctional acrylic matting resin finished product is coated to woodenware or drying and forming-film above metal device, obtains the film coated surface of gloss below 30.
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