CN104356287A - Internal and external cross-linking real stone paint pure acrylic emulsion with high water whitening resistance and preparation method - Google Patents
Internal and external cross-linking real stone paint pure acrylic emulsion with high water whitening resistance and preparation method Download PDFInfo
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Abstract
The invention discloses an internal and external cross-linking real stone paint pure acrylic emulsion with high water whitening resistance. The real stone paint emulsion is synthesized from raw materials including hard monomers, soft monomers, a composite emulsifier, internal cross-linking monomers, an organic silicon coupling agent, a thermal decomposition initiator, a pH regulator and an external cross-linking agent by a semicontinuous seed emulsion polymerization method. According to the real stone paint emulsion, the components and ratios of the soft and hard monomers in cores and shells of emulsion particles are designed and the glass-transition temperatures (Tg) of the cores and the shells are controlled respectively, so that the emulsion is good in pollution resistance while good water resistance and film forming property are guaranteed; moreover, the emulsion particles are internally and externally cross-linked through the internal cross-linking monomers and the external cross-linking agent, so that the water whitening resistance of the emulsion is greatly improved and a coating film cannot cause the water whitening phenomenon after being soaked in water for half a month.
Description
Technical field
The present invention relates to a kind of building coating polymer emulsion, particularly relating to a kind of emulsion for configuring true mineral varnish.
Background technology
True mineral varnish, also known as stone similar paint, is the building coating of the natural stone-powder mixed preparing of a kind of principal polymeric emulsion and shades of colour.Use it for the exterior wall of buildings, can form class chrysodor, the decorative effect of the lithotomes such as grouan, and production technique is simple, easy construction is a kind of ideal material of alternative lithotome decorative cover effect.
True mineral varnish, as a kind of building external paint, for outdoor, often can suffer wind, drench with rain, the test of these outdoor environmental conditions such as Exposure to Sunlight, therefore requires that it should have good water tolerance, weathering resistance and erosion resistance.And the true mineral varnish used now, the problem that ubiquity water tolerance is bad, whenever the rainy day, after rain drop erosion, coating surface just can whiten, and paint film also can become loose and even peel off, greatly have impact on the attractive in appearance of building appearance, and the performance of this and true mineral varnish emulsion itself has direct relation, therefore should start with from emulsion, develops a true mineral varnish emulsion with good water-whitening resistance.
Summary of the invention
The object of the invention is to, for the problem existing for existing true mineral varnish, provide pure acrylic emulsion of stone-like coating of a kind of exterior crosslinked type height water-whitening resistance and preparation method thereof, this emulsion good combination property, high to natural stone-powder cohesive strength, water-whitening resistance is good, soaked two weeks not water-white.
The implementation method of the object of the invention is: a kind of pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance, with hard monomer, soft monomer, compound emulsifying agent, interior cross-linking monomer, organo-silicon coupling agent, thermal decomposition initiating, pH adjusting agent, outside cross-linking agent is raw material, prepare the emulsion particle of soft core duricrust, controlling nucleocapsid than being 1:1 ~ 9:1, adopting semi-continuous seed emulsion polymerization method;
The each raw materials quality per-cent synthesizing the pure acrylic emulsion of stone-like coating of this exterior crosslinked type height water-whitening resistance is as follows:
Hard monomer: 20% ~ 30%; Soft monomer: 15 ~ 25%; Compound emulsifying agent: 0.5% ~ 1.5%; Interior cross-linking monomer: 0.1 ~ 3%; Organo-silicon coupling agent: 0.1 ~ 5%; Thermal decomposition initiating: 0.1 ~ 0.4%, outside cross-linking agent: 0.5 ~ 3%, surplus is deionized water.
Described hard monomer is methyl methacrylate, vinylformic acid, methacrylic acid, one or more mixtures in vinyl cyanide;
Described soft monomer is ethyl propenoate, butyl acrylate, one or more the mixture in Isooctyl acrylate monomer;
The emulsion structure of described soft core duricrust is core Tg is 0 ~ 22 DEG C, and shell Tg is 25 ~ 60 DEG C;
Described compound emulsifying agent is the composite of response type anionic emulsifier and nonionic emulsifying agent, wherein response type anionic emulsifier be the extraordinary ether alcohol sulfate of allyl group, containing one or more the mixture in double bond alcohol ether sulfosuccinates sodium salt, allyl ethers hydroxypropanesulfonic acid sodium, nonionic emulsifying agent is allyloxy nonylphenoxypolyoxyethylenes ether, one or more the mixture in fatty alcohol-polyoxyethylene ether;
Described interior cross-linking monomer is one or more the mixture in oxyethyl group Viscoat 295, double pentaerythritol C5 methacrylate, triallyl isocyanurate, Viscoat 295, pentaerythritol triacrylate, melamine acrylate;
Described organo-silicon coupling agent is one or more mixture of vinyltriethoxysilane, vinyl silane triisopropoxide, allyltrimethoxysilanis;
Described thermal decomposition initiating is ammonium persulphate, Sodium Persulfate, one or more the mixture in Potassium Persulphate;
Described pH adjusting agent is ammoniacal liquor, dimethylethanolamine, 2-amino-2-methyl-1-propanol, one or more the mixture in trolamine;
Described outside cross-linking agent is aziridine, vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan), adipic dihydrazide, carbodiimide, waterborne organic silicon linking agent, one or more the mixture in water-based isocyanate.
Present invention also offers a kind of preparation method of pure acrylic emulsion of stone-like coating of above-mentioned exterior crosslinked type height water-whitening resistance, present method comprises the following steps:
(1) get quantitative compound emulsifying agent and deionized water, configuration emulsifier solution three parts, is respectively emulsifier solution I, emulsifier solution II, emulsifier solution III;
(2) get quantitative initiator and deionized water, configuration initiator solution three parts, is respectively initiator solution I, initiator solution II, initiator solution III;
(3) quantitative hard monomer, soft monomer, interior cross-linking monomer, organo-silicon coupling agent and emulsifier solution I are added in reactor, vigorous stirring 30 minutes, obtain homogeneous pre-emulsion I;
(4) by remaining hard monomer, soft monomer, interior cross-linking monomer, organo-silicon coupling agent and emulsifier solution III add reactor, vigorous stirring 30 minutes, obtain homogeneous pre-emulsion II;
(5) get emulsifier solution II, initiator solution I and 10% core pre-emulsion I add in reactor, heated and stirred, is slowly warming up to 72 ~ 76 DEG C, reacts 15 ~ 30 minutes, until there is blue light in reactor, obtains seed emulsion;
(6) seed emulsion is slowly warming up to 80 ~ 85 DEG C, and remaining pre-emulsion I and initiator solution II are at the uniform velocity added drop-wise in seed emulsion, time for adding 1 ~ 2 hour, dropwise rear insulation 0.5-2 hour, obtain nuclear polymer emulsion, then at the uniform velocity drop in nuclear polymer emulsion by pre-emulsion II and initiator solution III, time for adding is 1 ~ 2 hour
(7) dropwise rear insulation 0.5-2 hour, be cooled to 45 DEG C and add pH adjusting agent, regulation system pH to 7 ~ 9, then add outside cross-linking agent, filter discharging after stirring, and obtain the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance.
The present invention compared with prior art, has outstanding water tolerance, has cohesive strength high simultaneously, film forming properties and the advantage such as contaminated resistance is good, its reason have following some:
In the present invention, introducing has the Specialty Acrylates class of more than three and three functional groups as interior cross-linking monomer, greatly improve the cross-linking density between reaction process Middle molecule, make polymer molecule form compact reticulated structure, thus improve the water resistance of emulsion;
Introduce outside cross-linking agent in the present invention, improve the cross-linking density between emulsion particle further, form more compact reticulated structure, thus improve the water-whitening resistance energy of emulsion further;
Select the hydramine containing multiple hydroxyl as part PH conditioning agent in the present invention, stable introduces more cross-linking set in system; Can better with outside cross-linking agent generation crosslinking reaction, farthest improve the cross-linking density between emulsion particle, thus improve the water-whitening resistance energy of emulsion greatly;
By using response type composite emulsifying system in the present invention, decreasing the consumption of hydrophilic component emulsifying agent and initiator system, thus improve the water-whitening resistance of emulsion;
By the monomer composition of design latex particle, core Tg, shell Tg and nucleocapsid ratio in the present invention, latex particle is made to form the nucleocapsid structure of soft core duricrust, thus while guarantee emulsion water-whitening resistance energy, there is good cohesive strength, film forming properties and contaminated resistance.
Embodiment
Embodiment 1:
1, true mineral varnish emulsion formulations
2, the preparation method of true mineral varnish emulsion
(1) compound emulsifying agent is divided into three parts by 21:9:5, configures emulsifier solution with deionized water, be respectively emulsifier solution I, emulsifier solution II, emulsifier solution III;
(2) initiator is divided into three parts by 4:3:1, and configures initiator solution with deionized water, be respectively initiator solution I, initiator solution II, initiator solution III;
(3) by the methyl methacrylate of 15.4 parts, the vinylformic acid of 0.3 part, the butyl acrylate of 18.5 parts, hydroxyethyl methylacrylate, 0.7 vinyl silane triisopropoxide and the emulsifier solution I of 0.3 part add in reactor, vigorous stirring 30 minutes, obtains homogeneous core pre-emulsion I;
(4) by the methyl methacrylate of 6.5 parts, the methacrylic acid of 0.5 part, the butyl acrylate of 4.7 parts, the hydroxyethyl methylacrylate of 0.1 part, vinyl silane triisopropoxide and the emulsifier solution III of 0.2 part add reactor, vigorous stirring 30 minutes, obtains homogeneous shell pre-emulsion II;
(5) get emulsifier solution II, initiator solution I and 10% core pre-emulsion I add in reactor, heated and stirred, is slowly warming up to 72 ~ 76 DEG C, reacts 15 ~ 30 minutes, until there is blue light in reactor, obtains seed emulsion;
(6) seed emulsion is slowly warming up to 80 ~ 85 DEG C, and remaining pre-emulsion I and initiator solution II are at the uniform velocity added drop-wise in seed emulsion, time for adding 1 ~ 2 hour, dropwise rear insulation 0.5-2 hour, obtain nuclear polymer emulsion, then at the uniform velocity drop in nuclear polymer emulsion by pre-emulsion II and initiator solution III, time for adding is 1 ~ 2 hour
(7) dropwise rear insulation 0.5-2 hour, be cooled to 45 DEG C and add pH adjusting agent, regulation system pH to 7 ~ 9, then add outside cross-linking agent, filter discharging after stirring, and obtain the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance.
Embodiment 2:
1, true mineral varnish emulsion formulations
2, true mineral varnish emulsion preparation method
(1) compound emulsifying agent is divided into three parts by 21:9:5, configures emulsifier solution with deionized water, be respectively emulsifier solution I, emulsifier solution II, emulsifier solution III;
(2) initiator is divided into three parts by 4:3:1, and configures initiator solution with deionized water, be respectively initiator solution I, initiator solution II, initiator solution III;
(3) by the methyl methacrylate of 19.5 parts, the vinylformic acid of 0.5 part, the butyl acrylate of 14 parts, the Viscoat 295 of 0.8 part, the vinyl silane triisopropoxide of 0.5 part and emulsifier solution I add in reactor, vigorous stirring 30 minutes, obtains homogeneous core pre-emulsion I;
(4) by the methyl methacrylate of 8.4 parts, the methacrylic acid of 0.3 part, the butyl acrylate of 2.3 parts, the Viscoat 295 of 0.4 part, vinyl silane triisopropoxide and the emulsifier solution III of 0.3 part add reactor, vigorous stirring 30 minutes, obtains homogeneous shell pre-emulsion II;
(5) get emulsifier solution II, initiator solution I and 10% core pre-emulsion I add in reactor, heated and stirred, is slowly warming up to 72 ~ 76 DEG C, reacts 15 ~ 30 minutes, until there is blue light in reactor, obtains seed emulsion;
(6) seed emulsion is slowly warming up to 80 ~ 85 DEG C, and remaining pre-emulsion I and initiator solution II are at the uniform velocity added drop-wise in seed emulsion, time for adding 1 ~ 2 hour, dropwise rear insulation 0.5-2 hour, obtain nuclear polymer emulsion, then at the uniform velocity drop in nuclear polymer emulsion by pre-emulsion II and initiator solution III, time for adding is 1 ~ 2 hour
(7) dropwise rear insulation 0.5-2 hour, be cooled to 45 DEG C and add pH adjusting agent, regulation system pH to 7 ~ 9, then add outside cross-linking agent, filter discharging after stirring, and obtain the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance.
Embodiment 3:
1, true mineral varnish emulsion formulations
2, true mineral varnish emulsion preparation method
(1) compound emulsifying agent is divided into three parts by 21:9:5, configures emulsifier solution with deionized water, be respectively emulsifier solution I, emulsifier solution II, emulsifier solution III;
(2) initiator is divided into three parts by 4:3:1, and configures initiator solution with deionized water, be respectively initiator solution I, initiator solution II, initiator solution III;
(3) by the methyl methacrylate of 17.2 parts, the vinylformic acid of 0.7 part, the butyl acrylate of 16.2 parts, nitrogen n-methylolacrylamide, 0.4 vinyl silane triisopropoxide and the emulsifier solution I of 0.4 part add in reactor, vigorous stirring 30 minutes, obtains homogeneous core pre-emulsion I;
(4) by the methyl methacrylate of 6.8 parts, the methacrylic acid of 0.3 part, the butyl acrylate of 3.8 parts, the nitrogen n-methylolacrylamide of 0.2 part, vinyl silane triisopropoxide and the emulsifier solution III of 0.3 part add reactor, vigorous stirring 30 minutes, obtains homogeneous shell pre-emulsion II;
(5) get emulsifier solution II, initiator solution I and 10% core pre-emulsion I add in reactor, heated and stirred, is slowly warming up to 72 ~ 76 DEG C, reacts 15 ~ 30 minutes, until there is blue light in reactor, obtains seed emulsion;
(6) seed emulsion is slowly warming up to 80 ~ 85 DEG C, and remaining pre-emulsion I and initiator solution II are at the uniform velocity added drop-wise in seed emulsion, time for adding 1 ~ 2 hour, dropwise rear insulation 0.5-2 hour, obtain nuclear polymer emulsion, then at the uniform velocity drop in nuclear polymer emulsion by pre-emulsion II and initiator solution III, time for adding is 1 ~ 2 hour
(7) dropwise rear insulation 0.5-2 hour, be cooled to 45 DEG C and add pH adjusting agent, regulation system pH to 7 ~ 9, then add outside cross-linking agent, filter discharging after stirring, and obtain the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance.
Embodiment 4:
1, true mineral varnish emulsion formulations
2, true mineral varnish emulsion preparation method
(1) compound emulsifying agent is divided into three parts by 21:9:5, configures emulsifier solution with deionized water, be respectively emulsifier solution I, emulsifier solution II, emulsifier solution III;
(2) initiator is divided into three parts by 4:3:1, and configures initiator solution with deionized water, be respectively initiator solution I, initiator solution II, initiator solution III;
(3) by the methyl methacrylate of 20 parts, the vinylformic acid of 0.7 part, the butyl acrylate of 18.5 parts, nitrogen n-methylolacrylamide, 0.7 vinyl silane triisopropoxide and the emulsifier solution I of 0.5 part add in reactor, vigorous stirring 30 minutes, obtains homogeneous core pre-emulsion I;
(4) by the methyl methacrylate of 3.6 parts, the methacrylic acid of 0.2 part, the butyl acrylate of 1.5 parts, the nitrogen n-methylolacrylamide of 0.1 part, vinyl silane triisopropoxide and the emulsifier solution III of 0.1 part add reactor, vigorous stirring 30 minutes, obtains homogeneous shell pre-emulsion II;
(5) get emulsifier solution II, initiator solution I and 10% core pre-emulsion I add in reactor, heated and stirred, is slowly warming up to 72 ~ 76 DEG C, reacts 15 ~ 30 minutes, until there is blue light in reactor, obtains seed emulsion;
(6) seed emulsion is slowly warming up to 80 ~ 85 DEG C, and remaining pre-emulsion I and initiator solution II are at the uniform velocity added drop-wise in seed emulsion, time for adding 1 ~ 2 hour, dropwise rear insulation 0.5-2 hour, obtain nuclear polymer emulsion, then at the uniform velocity drop in nuclear polymer emulsion by pre-emulsion II and initiator solution III, time for adding is 1 ~ 2 hour
(7) dropwise rear insulation 0.5-2 hour, be cooled to 45 DEG C and add pH adjusting agent, regulation system pH to 7 ~ 9, then add outside cross-linking agent, filter discharging after stirring, and obtain the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance.
Claims (8)
1. a pure acrylic emulsion of stone-like coating for exterior crosslinked type height water-whitening resistance, is characterized in that,
Described pure acrylic emulsion of stone-like coating is with hard monomer, soft monomer, compound emulsifying agent, interior cross-linking monomer, organo-silicon coupling agent, thermal decomposition initiating, pH adjusting agent, and outside cross-linking agent is raw material, prepares the emulsion particle of soft core duricrust;
Described pure acrylic emulsion of stone-like coating, interior cross-linking monomer is one or more the mixture in oxyethyl group Viscoat 295, double pentaerythritol C5 methacrylate, triallyl isocyanurate, Viscoat 295, pentaerythritol triacrylate, melamine acrylate;
Described pure acrylic emulsion of stone-like coating, outside cross-linking agent is aziridine, vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan), adipic dihydrazide, carbodiimide, waterborne organic silicon linking agent, one or more the mixture in water-based isocyanate;
Described pure acrylic emulsion of stone-like coating pH adjusting agent is ammoniacal liquor, dimethylethanolamine, 2-amino-2-methyl-1-propanol, one or more the mixture in trolamine;
Described pure acrylic emulsion of stone-like coating, nucleocapsid, than being 1:1 ~ 9:1, adopts semi-continuous seed emulsion polymerization method to obtain;
Described pure acrylic emulsion of stone-like coating, shared by each component, mass percent is: hard monomer: 20% ~ 30%; Soft monomer: 15 ~ 25%; Compound emulsifying agent: 0.5% ~ 1.5%; Interior cross-linking monomer: 0.1 ~ 3%; Organo-silicon coupling agent: 0.1 ~ 5%; Thermal decomposition initiating: 0.1 ~ 0.4%, outside cross-linking agent: 0.5 ~ 3%, surplus is deionized water.
2. the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance according to claim 1, is characterized in that, described hard monomer is methyl methacrylate, vinylformic acid, methacrylic acid, one or more mixtures in vinyl cyanide.
3. the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance according to claim 1, is characterized in that, described soft monomer is ethyl propenoate, butyl acrylate, one or more the mixture in Isooctyl acrylate monomer.
4. the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance according to claim 1, is characterized in that, the emulsion structure of soft core duricrust is core Tg is 0 ~ 22 DEG C, and shell Tg is 25 ~ 60 DEG C.
5. the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance according to claim 1, it is characterized in that, compound emulsifying agent is the composite of response type anionic emulsifier and nonionic emulsifying agent, described response type anionic emulsifier is the extraordinary ether alcohol sulfate of allyl group, containing one or more the mixture in double bond alcohol ether sulfosuccinates sodium salt, allyl ethers hydroxypropanesulfonic acid sodium, described nonionic emulsifying agent is allyloxy nonylphenoxypolyoxyethylenes ether, one or more the mixture in fatty alcohol-polyoxyethylene ether.
6. the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance according to claim 1, it is characterized in that, described organo-silicon coupling agent is one or more mixture of vinyltriethoxysilane, vinyl silane triisopropoxide, allyltrimethoxysilanis.
7. the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance according to claim 1, is characterized in that, described thermal decomposition initiating is ammonium persulphate, Sodium Persulfate, one or more the mixture in Potassium Persulphate.
8. prepare a method for the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance according to claim 1, it is characterized in that this method comprises the following steps:
(1) get quantitative compound emulsifying agent and deionized water, configuration emulsifier solution three parts, is respectively emulsifier solution I, emulsifier solution II, emulsifier solution III;
(2) get quantitative initiator and deionized water, configuration initiator solution three parts, is respectively initiator solution I, initiator solution II, initiator solution III;
(3) quantitative hard monomer, soft monomer, interior cross-linking monomer, organo-silicon coupling agent and emulsifier solution I are added in reactor, vigorous stirring 30 minutes, obtain homogeneous pre-emulsion I;
(4) by remaining hard monomer, soft monomer, interior cross-linking monomer, organo-silicon coupling agent and emulsifier solution III add reactor, vigorous stirring 30 minutes, obtain homogeneous pre-emulsion II;
(5) get emulsifier solution II, initiator solution I and 10% core pre-emulsion I add in reactor, heated and stirred, is slowly warming up to 72 ~ 76 DEG C, reacts 15 ~ 30 minutes, until there is blue light in reactor, obtains seed emulsion;
(6) seed emulsion is slowly warming up to 80 ~ 85 DEG C, and remaining pre-emulsion I and initiator solution II are at the uniform velocity added drop-wise in seed emulsion, time for adding 1 ~ 2 hour, dropwise rear insulation 0.5-2 hour, obtain nuclear polymer emulsion, then at the uniform velocity drop in nuclear polymer emulsion by pre-emulsion II and initiator solution III, time for adding is 1 ~ 2 hour;
(7) dropwise rear insulation 0.5-2 hour, be cooled to 45 DEG C and add pH adjusting agent, regulation system pH to 7 ~ 9, then add outside cross-linking agent, filter discharging after stirring, and obtain the pure acrylic emulsion of stone-like coating of exterior crosslinked type height water-whitening resistance.
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