CN104356287B - A kind of pure acrylic emulsion of stone-like coating and preparation method of the high water-whitening resistance of exterior crosslinked type - Google Patents

A kind of pure acrylic emulsion of stone-like coating and preparation method of the high water-whitening resistance of exterior crosslinked type Download PDF

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CN104356287B
CN104356287B CN201410607514.3A CN201410607514A CN104356287B CN 104356287 B CN104356287 B CN 104356287B CN 201410607514 A CN201410607514 A CN 201410607514A CN 104356287 B CN104356287 B CN 104356287B
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emulsion
stone
water
coating
pure acrylic
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CN104356287A (en
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孟伟康
徐健
冯中军
傅乐峰
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Nanjing Regal Polymer Co., Ltd.
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SHANGHAI SANRUI POLYMER MATERIAL CO Ltd
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Abstract

A kind of pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type, 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 are raw material, using semi-continuous seed emulsion polymerization method, synthesize a kind of pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type.The true mineral varnish emulsion of the present invention, by the composition and consumption that design soft or hard monomer in latex particle nucleocapsid, core, shell Tg are controlled respectively, so that emulsion is while good water resistance, film property is ensured, with good contaminated resistance, and pass through interior cross-linking monomer and outside cross-linking agent, realize that latex particle inside and outside dual is crosslinked, the water-whitening resistance energy of emulsion is substantially increased, and two weeks is soaked in applying film water not water-white.

Description

A kind of pure acrylic emulsion of stone-like coating and preparation method of the high water-whitening resistance of exterior crosslinked type
Technical field
The present invention relates to a kind of building coating polymer emulsion, more particularly to a kind of emulsion for configuring true mineral varnish.
Background technology
True mineral varnish, also known as stone similar paint, be a kind of principal polymeric emulsion with the natural stone-powder mixed preparing of shades of colour and Into building coating.The exterior wall of building is used it for, the decoration effect of the lithotomes such as class chrysodor, granite can be formed Really, and simple production process, easy construction, it is a kind of ideal material for substituting lithotome decorative cover effect.
True mineral varnish for outdoor, can frequently suffer from wind, drench with rain as a kind of building external paint, these families such as Exposure to Sunlight The test of external environment condition, therefore it is required which should have good resistance to water, weatherability and corrosion resistance.And currently use True mineral varnish, the bad problem of generally existing resistance to water, whenever the rainy day, after rain drop erosion, coating surface will whiten, paint Film further becomes loose or even peels off, and leverages the attractive in appearance of building appearance, and this performance with true mineral varnish emulsion itself There is direct relation, therefore should start with from emulsion, develop a true mineral varnish emulsion with good water-whitening resistance.
The content of the invention
It is an object of the present invention to be directed to the problems of existing true mineral varnish, there is provided a kind of exterior crosslinked type height is resistance to Pure acrylic emulsion of stone-like coating of water-white property and preparation method thereof, the emulsion good combination property are high to natural stone-powder adhesion strength, water-fast White property is good, and soaked two weeks is not water-white.
The implementation method of the object of the invention is:A kind of pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type, be with Hard monomer, soft monomer, compound emulsifying agent, interior cross-linking monomer, organo-silicon coupling agent, thermal decomposition initiating, pH adjusting agent, external crosslinking Agent is raw material, prepares the emulsion particle of soft core duricrust, controls nucleocapsid ratio for 1:1~9:1, using semi-continuous seed emulsion polymerization method;
The each raw materials quality percentage ratio for synthesizing the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of the exterior crosslinked type 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%, balance of deionized water.
Described hard monomer be methyl methacrylate, acrylic acid, methacrylic acid, the one kind or one kind in acrylonitrile with Upper mixture;
Described soft monomer be ethyl acrylate, butyl acrylate, in Isooctyl acrylate monomer one or more Mixture;
It is 0 ~ 22 DEG C that the emulsion structure of described soft core duricrust is core Tg, and shell Tg is 25 ~ 60 DEG C;
Described compound emulsifying agent is the compounding of response type anion emulsifier and nonionic emulsifier, and wherein response type is cloudy Ionic emulsifying agent is pi-allyl special type ether alcohol sulfate, the ether sulfosuccinates sodium salt of alcohol containing double bond, allyl ether hydroxy propane One or more mixture in sodium sulfonate, nonionic emulsifier are allyloxy nonylphenoxypolyoxyethylenes ether, One or more mixture in fatty alcohol-polyoxyethylene ether;
Described interior cross-linking monomer be ethyoxyl trimethylolpropane trimethacrylate, double pentaerythritol C5 methacrylate, In triallyl isocyanurate, trimethylolpropane trimethacrylate, pentaerythritol triacrylate, melamine acrylate One or more mixture;
Described organo-silicon coupling agent is VTES, vinyl silane triisopropoxide, pi-allyl three One or more mixture of methoxy silane;
Described thermal decomposition initiating is Ammonium persulfate., sodium peroxydisulfate, one or more mixed in potassium peroxydisulfate Compound;
Described pH adjusting agent be ammonia, dimethylethanolamine, 2-amino-2-methyl-1-propanol, in triethanolamine Plant or more than one mixture;
Described outside cross-linking agent be aziridine, vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan), adipic dihydrazide, carbodiimide, waterborne organic silicon cross-linking agent, aqueouss One or more mixture in isocyanates.
Present invention also offers a kind of preparation method of the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of above-mentioned exterior crosslinked type, This method is comprised the following steps:
(1)Take quantitative compound emulsifying agent and deionized water, configure three parts of emulsifier solution, respectively emulsifier solution I, Emulsifier solution II, emulsifier solution III;
(2)Quantitative initiator and deionized water are taken, three parts of initiator solution, respectively initiator solution I, initiation is configured Agent 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 into reaction In kettle, it is stirred vigorously 30 minutes, obtains homogeneous pre-emulsion I;
(4)By remaining hard monomer, soft monomer, interior cross-linking monomer, organo-silicon coupling agent and emulsifier solution III are added instead Kettle is answered, is stirred vigorously 30 minutes, obtain homogeneous pre-emulsion II;
(5)The core pre-emulsion I for taking emulsifier solution II, initiator solution I and 10% adds reactor, heated and stirred, 72~76 DEG C are to slowly warm up to, are reacted 15~30 minutes, is occurred blue light in reactor, obtain final product seed emulsion;
(6)Seed emulsion is to slowly warm up to into 80~85 DEG C, and by remaining pre-emulsion I and initiator solution II at the uniform velocity It is added drop-wise in seed emulsion, time for adding 1~2 hour, 0.5-2 hours is incubated after completion of dropping, nuclear polymer emulsion is obtained, so Afterwards pre-emulsion II and initiator solution III are at the uniform velocity dropped in nuclear polymer emulsion, time for adding is 1~2 hour,
(7)After completion of dropping be incubated 0.5-2 hours, be cooled to 45 DEG C addition pH adjusting agents, regulation system pH to 7~9, so After add outside cross-linking agent, filtering and discharging after stirring obtains final product the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type.
The present invention compared with prior art, with prominent resistance to water, while have adhesion strength high, filming performance and resistance to Stain performance it is good the advantages of, its reason have it is following some:
The special acrylic acid esters with three and more than three functional groups are introduced in the present invention as interior cross-linking monomer, pole Improve greatly intermolecular crosslink density in course of reaction so that polymer molecule forms compact network structure, so as to improve The water resistance of emulsion;
Outside cross-linking agent is introduced in the present invention, the crosslink density between emulsion particle is further improved, is formed more compact net Shape structure, so as to further improve the water-whitening resistance energy of emulsion;
Select the hydramine containing multiple hydroxyls as part PH regulators in the present invention, stable introduces more in system Crosslinking points;Reaction preferably can be crosslinked with outside cross-linking agent, is farthest improve between emulsion particle Crosslink density, so as to greatly improve the water-whitening resistance energy of emulsion;
By using response type composite emulsifying system in the present invention, hydrophilic component emulsifying agent and initiator system are reduced Consumption, so as to 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 so that latex particle is formed The nucleocapsid structure of soft core duricrust, so as to while emulsion water-whitening resistance energy is ensured, with good cohesive strength, filming performance and Contaminated resistance.
Specific embodiment
Embodiment 1:
1st, true mineral varnish emulsion formulations
2nd, the preparation method of true mineral varnish emulsion
(1)Compound emulsifying agent is pressed into 21:9:5 points is three parts, deionized water configuration emulsifier solution, respectively emulsifying agent Solution I, emulsifier solution II, emulsifier solution III;
(2)Initiator is pressed into 4:3:1 point is three parts, and deionized water configuration initiator solution, and respectively initiator is molten Liquid I, initiator solution II, initiator solution III;
(3)By 15.4 parts of methyl methacrylate, 0.3 part of acrylic acid, 18.5 parts of butyl acrylate, 0.3 part During hydroxyethyl methylacrylate, 0.7 vinyl silane triisopropoxide and emulsifier solution I add reactor, 30 are stirred vigorously Minute, obtain homogeneous core pre-emulsion I;
(4)By 6.5 parts of methyl methacrylate, 0.5 part of methacrylic acid, 4.7 parts of butyl acrylate, 0.1 part Hydroxyethyl methylacrylate, 0.2 part of vinyl silane triisopropoxide and emulsifier solution III add reactor, acutely stir Mix 30 minutes, obtain homogeneous shell pre-emulsion II;
(5)The core pre-emulsion I for taking emulsifier solution II, initiator solution I and 10% adds reactor, heated and stirred, 72~76 DEG C are to slowly warm up to, are reacted 15~30 minutes, is occurred blue light in reactor, obtain final product seed emulsion;
(6)Seed emulsion is to slowly warm up to into 80~85 DEG C, and by remaining pre-emulsion I and initiator solution II at the uniform velocity It is added drop-wise in seed emulsion, time for adding 1~2 hour, 0.5-2 hours is incubated after completion of dropping, nuclear polymer emulsion is obtained, so Afterwards pre-emulsion II and initiator solution III are at the uniform velocity dropped in nuclear polymer emulsion, time for adding is 1~2 hour,
(7)After completion of dropping be incubated 0.5-2 hours, be cooled to 45 DEG C addition pH adjusting agents, regulation system pH to 7~9, so After add outside cross-linking agent, filtering and discharging after stirring obtains final product the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type.
Embodiment 2:
1st, true mineral varnish emulsion formulations
2nd, true mineral varnish emulsion preparation method
(1)Compound emulsifying agent is pressed into 21:9:5 points is three parts, deionized water configuration emulsifier solution, respectively emulsifying agent Solution I, emulsifier solution II, emulsifier solution III;
(2)Initiator is pressed into 4:3:1 point is three parts, and deionized water configuration initiator solution, and respectively initiator is molten Liquid I, initiator solution II, initiator solution III;
(3)By 19.5 parts of methyl methacrylate, 0.5 part of acrylic acid, 14 parts of butyl acrylate, the three of 0.8 part It is during hydroxymethyl-propane triacrylate, 0.5 part of vinyl silane triisopropoxide and emulsifier solution I add reactor, acute Strong stirring 30 minutes, obtains homogeneous core pre-emulsion I;
(4)By 8.4 parts of methyl methacrylate, 0.3 part of methacrylic acid, 2.3 parts of butyl acrylate, 0.4 part Trimethylolpropane trimethacrylate, 0.3 part of vinyl silane triisopropoxide and emulsifier solution III add reactor, It is stirred vigorously 30 minutes, obtains homogeneous shell pre-emulsion II;
(5)The core pre-emulsion I for taking emulsifier solution II, initiator solution I and 10% adds reactor, heated and stirred, 72~76 DEG C are to slowly warm up to, are reacted 15~30 minutes, is occurred blue light in reactor, obtain final product seed emulsion;
(6)Seed emulsion is to slowly warm up to into 80~85 DEG C, and by remaining pre-emulsion I and initiator solution II at the uniform velocity It is added drop-wise in seed emulsion, time for adding 1~2 hour, 0.5-2 hours is incubated after completion of dropping, nuclear polymer emulsion is obtained, so Afterwards pre-emulsion II and initiator solution III are at the uniform velocity dropped in nuclear polymer emulsion, time for adding is 1~2 hour,
(7)After completion of dropping be incubated 0.5-2 hours, be cooled to 45 DEG C addition pH adjusting agents, regulation system pH to 7~9, so After add outside cross-linking agent, filtering and discharging after stirring obtains final product the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type.
Embodiment 3:
1st, true mineral varnish emulsion formulations
2nd, true mineral varnish emulsion preparation method
(1)Compound emulsifying agent is pressed into 21:9:5 points is three parts, deionized water configuration emulsifier solution, respectively emulsifying agent Solution I, emulsifier solution II, emulsifier solution III;
(2)Initiator is pressed into 4:3:1 point is three parts, and deionized water configuration initiator solution, and respectively initiator is molten Liquid I, initiator solution II, initiator solution III;
(3)By 17.2 parts of methyl methacrylate, 0.7 part of acrylic acid, 16.2 parts of butyl acrylate, 0.4 part During nitrogen n-methylolacrylamide, 0.4 vinyl silane triisopropoxide and emulsifier solution I add reactor, 30 are stirred vigorously Minute, obtain homogeneous core pre-emulsion I;
(4)By 6.8 parts of methyl methacrylate, 0.3 part of methacrylic acid, 3.8 parts of butyl acrylate, 0.2 part Nitrogen n-methylolacrylamide, 0.3 part of vinyl silane triisopropoxide and emulsifier solution III add reactor, acutely stir Mix 30 minutes, obtain homogeneous shell pre-emulsion II;
(5)The core pre-emulsion I for taking emulsifier solution II, initiator solution I and 10% adds reactor, heated and stirred, 72~76 DEG C are to slowly warm up to, are reacted 15~30 minutes, is occurred blue light in reactor, obtain final product seed emulsion;
(6)Seed emulsion is to slowly warm up to into 80~85 DEG C, and by remaining pre-emulsion I and initiator solution II at the uniform velocity It is added drop-wise in seed emulsion, time for adding 1~2 hour, 0.5-2 hours is incubated after completion of dropping, nuclear polymer emulsion is obtained, so Afterwards pre-emulsion II and initiator solution III are at the uniform velocity dropped in nuclear polymer emulsion, time for adding is 1~2 hour,
(7)After completion of dropping be incubated 0.5-2 hours, be cooled to 45 DEG C addition pH adjusting agents, regulation system pH to 7~9, so After add outside cross-linking agent, filtering and discharging after stirring obtains final product the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type.
Embodiment 4:
1st, true mineral varnish emulsion formulations
2nd, true mineral varnish emulsion preparation method
(1)Compound emulsifying agent is pressed into 21:9:5 points is three parts, deionized water configuration emulsifier solution, respectively emulsifying agent Solution I, emulsifier solution II, emulsifier solution III;
(2)Initiator is pressed into 4:3:1 point is three parts, and deionized water configuration initiator solution, and respectively initiator is molten Liquid I, initiator solution II, initiator solution III;
(3)By 20 parts of methyl methacrylate, 0.7 part of acrylic acid, 18.5 parts of butyl acrylate, 0.5 part of nitrogen During n-methylolacrylamide, 0.7 vinyl silane triisopropoxide and emulsifier solution I add reactor, 30 points are stirred vigorously Clock, obtains homogeneous core pre-emulsion I;
(4)By 3.6 parts of methyl methacrylate, 0.2 part of methacrylic acid, 1.5 parts of butyl acrylate, 0.1 part Nitrogen n-methylolacrylamide, 0.1 part of vinyl silane triisopropoxide and emulsifier solution III add reactor, acutely stir Mix 30 minutes, obtain homogeneous shell pre-emulsion II;
(5)The core pre-emulsion I for taking emulsifier solution II, initiator solution I and 10% adds reactor, heated and stirred, 72~76 DEG C are to slowly warm up to, are reacted 15~30 minutes, is occurred blue light in reactor, obtain final product seed emulsion;
(6)Seed emulsion is to slowly warm up to into 80~85 DEG C, and by remaining pre-emulsion I and initiator solution II at the uniform velocity It is added drop-wise in seed emulsion, time for adding 1~2 hour, 0.5-2 hours is incubated after completion of dropping, nuclear polymer emulsion is obtained, so Afterwards pre-emulsion II and initiator solution III are at the uniform velocity dropped in nuclear polymer emulsion, time for adding is 1~2 hour,
(7)After completion of dropping be incubated 0.5-2 hours, be cooled to 45 DEG C addition pH adjusting agents, regulation system pH to 7~9, so After add outside cross-linking agent, filtering and discharging after stirring obtains final product the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type.

Claims (8)

1. the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of a kind of exterior crosslinked type, it is characterised in that
Described pure acrylic emulsion of stone-like coating is the interior cross-linking monomer with hard monomer, soft monomer, compound emulsifying agent, organo-silicon coupling agent, Thermal decomposition initiating, pH adjusting agent, outside cross-linking agent are raw material, prepare the emulsion particle of soft core duricrust,
Described pure acrylic emulsion of stone-like coating, interior cross-linking monomer are ethyoxyl trimethylolpropane trimethacrylate, Bis(pentaerythritol) Five acrylate, triallyl isocyanurate, trimethylolpropane trimethacrylate, pentaerythritol triacrylate, melamine One or more mixture in amine 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 Cross-linking agent, one or more the mixture in water-based isocyanate;
Described pure acrylic emulsion of stone-like coating pH adjusting agent be ammonia, dimethylethanolamine, 2-amino-2-methyl-1-propanol, three second One or more mixture in hydramine;
Described pure acrylic emulsion of stone-like coating, nucleocapsid mass ratio are 1:1~9:1, obtained using semi-continuous seed emulsion polymerization method;
Described pure acrylic emulsion of stone-like coating, mass percent shared by each component 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%, balance of deionized water.
2. the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type according to claim 1, it is characterised in that hard single Body is methyl methacrylate, acrylic acid, one or more mixture in methacrylic acid.
3. the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type according to claim 1, it is characterised in that soft list Body is ethyl acrylate, butyl acrylate, one or more the mixture in Isooctyl acrylate monomer.
4. the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type according to claim 1, it is characterised in that soft core It is 0 ~ 22 DEG C that the emulsion structure of duricrust is core Tg, and shell Tg is 25 ~ 60 DEG C.
5. the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type according to claim 1, it is characterised in that compound Emulsifying agent is the compounding of response type anion emulsifier and nonionic emulsifier, and wherein response type anion emulsifier is pi-allyl One kind or two in extraordinary ether alcohol sulfate, the ether sulfosuccinates sodium salt of alcohol containing double bond, allyl ether hydroxypropanesulfonic acid sodium The mixture of the above is planted, nonionic emulsifier is allyloxy nonylphenoxypolyoxyethylenes ether, in fatty alcohol-polyoxyethylene ether One or more mixture.
6. the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type according to claim 1, it is characterised in that organic Silicone couplet be VTES, vinyl silane triisopropoxide, one kind of allyltrimethoxysilanis or Two or more mixture.
7. the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type according to claim 1, it is characterised in that heat point Solution initiator be Ammonium persulfate., sodium peroxydisulfate, one or more the mixture in potassium peroxydisulfate.
8. the method for the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of a kind of exterior crosslinked type prepared described in claim 1, which is special Levy is that the method is comprised the following steps:
(1)Compound emulsifying agent and deionized water are taken, three parts of emulsifier solution is configured, respectively emulsifier solution I, emulsifying agent is molten Liquid II, emulsifier solution III;
(2)Initiator and deionized water are taken, three parts of initiator solution, respectively initiator solution I, initiator solution II is configured, Initiator solution III;
(3)Hard monomer, soft monomer, interior cross-linking monomer, organo-silicon coupling agent and emulsifier solution I are added in reactor, acutely Stirring 30 minutes, obtains homogeneous pre-emulsion I;
(4)By remaining hard monomer, soft monomer, interior cross-linking monomer, organo-silicon coupling agent and the addition reactor of emulsifier solution III, It is stirred vigorously 30 minutes, obtains homogeneous pre-emulsion II;
(5)The pre-emulsion I for taking emulsifier solution II, initiator solution I and 10% adds reactor, and heated and stirred is slow to rise Temperature is reacted 15~30 minutes, blue light occurs, obtain final product seed emulsion in reactor to 72~76 DEG C;
(6)Seed emulsion is to slowly warm up to into 80~85 DEG C, and by remaining pre-emulsion I and the at the uniform velocity Deca of initiator solution II To in seed emulsion, time for adding 1~2 hour is incubated 0.5-2 hours, obtains nuclear polymer emulsion after completion of dropping, then will Pre-emulsion II and initiator solution III are at the uniform velocity dropped in nuclear polymer emulsion, and time for adding is 1~2 hour;
(7)0.5-2 hours are incubated after completion of dropping, 45 DEG C of addition pH adjusting agents, regulation system pH to 7~9, Ran Houjia is cooled to Enter outside cross-linking agent, filtering and discharging after stirring obtains final product the pure acrylic emulsion of stone-like coating of the high water-whitening resistance of exterior crosslinked type.
CN201410607514.3A 2014-11-03 2014-11-03 A kind of pure acrylic emulsion of stone-like coating and preparation method of the high water-whitening resistance of exterior crosslinked type Active CN104356287B (en)

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