CN105061665A - Hydroxypolyacrylate emulsion, and preparation method and application thereof - Google Patents
Hydroxypolyacrylate emulsion, and preparation method and application thereof Download PDFInfo
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- C08F2/12—Polymerisation in non-solvents
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- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
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- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
- C08F220/283—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing one or more carboxylic moiety in the chain, e.g. acetoacetoxyethyl(meth)acrylate
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Abstract
The invention discloses a hydroxypolyacrylate emulsion, and a preparation method and an application thereof. The preparation method comprises the following steps: weighing an acrylate monomer and/or a metacrylate monomer, a hydroxyacrylate monomer, an acrylic monomer, an acrylate function monomer and a hydroxy oligomer, uniformly mixing to prepare a monomer mixture, weighing 10-15% of the monomer mixture, and emulsifying by using an emulsifier to prepare a seed pre-emulsion for later use; and adding the emulsifier, sodium bicarbonate and deionized water into a reaction kettle, stirring, rising the temperature of a reaction system, adding an initiator, stabilizing, adding the seed pre-emulsion in a dropwise manner, stabilizing, adding the remaining monomer mixture and the remaining initiator in a dropwise manner, heating, slaking, cooling, neutralizing, carrying out heat insulation, cooling, and discharging to obtain the hydroxypolyacrylate emulsion. A film made by using an aqueous dual-component polyurethane coating prepared from the hydroxypolyacrylate emulsion and an aqueous polyisocyanate curing agent has the advantages of high hardness, high luster and excellent chemical resistance.
Description
Technical field
The present invention relates to aqueous double-component polyurethane coating, be specifically related to a kind of hydroxy polyacrylate emulsion and preparation method thereof and application.
Background technology
Existing woodwork coating mostly is solvent based coating, and containing the organic solvent more than more than 50%, these solvents can evaporate into contaminate environment in air in construction process, also damage HUMAN HEALTH, and organic solvent itself can bring as potential safety hazards such as burning, blasts.Therefore, the Water-borne modification of woodwork coating is the trend of international coatings development.Water-borne wood coating comprises single-component and double-component aqueous woodwork coating.Wherein to comprise the aspects such as water tolerance, chemical-resistant and hardness bad for the paint film property of single-component water-based woodwork coating, comparatively large with oil paint gap, seriously limits applying of water-borne wood coating.Mechanical property, the water tolerance of double-component aqueous woodwork coating are suitable with solvent wood coatings with chemical-resistant, well can overcome the shortcoming of single-component water-based woodwork coating.In January, 2015, China issued the decree about imposing the excise to solvent based coating, made double-component aqueous woodwork coating to become the first-selection of high-grade water-borne wood coating.
Double-component waterborne polyurethane coating has excellent film performance and obtains investigation and application widely, and it is made up of waterborne polymeric polyvalent alcohol and aqueous polyisocyanate curing agent, and separately packaging, is mixed in proportion during use.Wherein waterborne polymeric polyvalent alcohol comprises water polyacrylic acid polyvalent alcohol, aqueous polyurethane polyvalent alcohol, waterborne polyester polyvalent alcohol and polyether glycol and polyol blend.Wherein water polyacrylic acid polyvalent alcohol has excellent guarantor's look, protects light and weathering resistance, low price, and molecular weight, second-order transition temperature (Tg) and hydroxy radical content are easy to the advantages such as adjustment, it is the first-selection of waterborne polymeric polyvalent alcohol in current double-component waterborne polyurethane coating.Adopt different polymerization technique can obtain emulsion-type and dispersion type two class polyacrylate polyol.The hydroxy radical content of water polyacrylic acid dispersion is higher, and the film of preparation has excellent water tolerance and chemical-resistant, deposits and uses a large amount of organic solvent in process of production, product solids content is lower, be generally 30%-40%, and the dry speed of paint film is slow, high in cost of production shortcoming.By contrast, emulsion-type polyacrylate polyol (also claiming hydroxy polyacrylate emulsion) production technique is simple, can up to more than 50% Gu contain, and cost is low, and dry speed is fast.Therefore, the double-component polyurethane coating of hydroxy polyacrylate emulsion preparation occupies the market space of larger aqueous double-component coating.
Still there is the problems such as appearance poor, chemical-resistant is poor, hardness is low in the paint film that existing hydroxy polyacrylate emulsion and aqueous polyisocyanate curing agent are prepared.The main manifestations of paint film appearance difference has the paint film transparency poor, and gloss is low, its major cause be hydroxy polyacrylate emulsion to the emulsion dispersion ability of solidifying agent and and the consistency of solidifying agent bad.During for ensureing that the Tg of the polyacrylic ester that paint film high rigidity designs is higher, poor with the bad paint film appearance that causes of the consistency of solidifying agent.The cross-linking density of paint film is higher, and its chemical-resistant is better, and the polyacrylic ester of high hydroxyl content can obtain the paint film of high crosslink density.But the polymerization stability of the polyacrylate dispersion of the high hydroxyl content of routine is poor, suitability for industrialized production is unstable.In addition, the excessive use emulsifying agent in letex polymerization or emulsifying agent mismatch can reduce gloss and the chemical-resistant of paint film.At present, aqueous double-component polyurethane hardness of paint film and chemical resistance is improved by the second-order transition temperature and hydroxy radical content that improve hydroxy polyacrylate emulsion, also can cause needing more organic molecule film coalescence aid and solidifying agent (normal containing a certain amount of solubility promoter in solidifying agent) joining in paint process, increase volatile organic compounds (VOC) content in coating, also can cause coating cost increase.Therefore, conventional method is more difficult improves the appearance poor of the two component paint film of hydroxy polyacrylate emulsion-type, the problem such as chemical-resistant is poor, hardness is low.
Chinese invention patent application CN103059210 carrys out modified hydroxyl polyacrylate dispersion by the fluoro-acrylate monomer adding 2%-5%, though water tolerance and the chemical-resistant of two component paint film can be improved a little, characteristic due to the hydrophobic oleophobic of fluorinated acrylate monomer makes the transformation efficiency of its polyreaction not high, easily cause a large amount of residual of fluorochemical monomer, also cause the problems such as the ply adhesion difference of paint film, and the expensive polymer emulsion cost that causes of fluorinated acrylate monomer sharply rises.
Summary of the invention
The object of the invention is to overcome prior art Problems existing, a kind of easy adjustment realizing hydroxy polyacrylate emulsion hydroxy radical content is provided, makes the multiple hydroxy resin and the solidifying agent hydroxy polyacrylate emulsion forming multiple cross-linked structure and preparation method thereof of different structure, different molecular weight, different glass temperature.
Another object of the present invention is to provide the application of described hydroxy polyacrylate emulsion in aqueous double-component polyurethane coating, the hardness of film of double-component polyurethane coating is made to reach H, gloss (60 °) reaches 83%, have excellent water-fast/alcohol performance, also there is good dry heat resistance.
The present invention is directed to the deficiencies in the prior art, adopt the technique of adding the oligopolymer of high hydroxyl content in hydroxy polyacrylate emulsion polymerization process China and foreign countries, prepare the hydroxy polyacrylate emulsion that hydroxy radical content is suitable, this technique not only realizes the easy adjustment of hydroxy polyacrylate emulsion hydroxy radical content, and makes different structure, different molecular weight, the multiple hydroxy resin of different Tg and solidifying agent form multiple cross-linked structure.With do not add hydroxyl oligomer identical hydroxy radical content conventional emulsions compared with, improve paint film appearance greatly, improve hardness of paint film, solve chemicals-resistant difference etc. a difficult problem.Meanwhile, under the prerequisite ensureing stability of emulsion polymerization and high monomer transformation efficiency, the variable range of the hydroxy radical content of hydroxy polyacrylate emulsion of the present invention is wider, makes the hydroxy polyacrylate emulsion of high hydroxyl content easily realize large-scale industrial production.In addition, the present invention adopts special acrylic monomers, as (methyl) isobornyl acrylate, improves the consistency of hydroxy polyacrylate emulsion and solidifying agent, thus improves paint film appearance.
Realize the technical scheme that object of the present invention adopts:
The preparation method of hydroxy polyacrylate emulsion, comprises following steps:
In mass fraction, take acrylate monomer and/or methacrylate monomer 30 ~ 45 parts, hydroxy-acrylate monomer 5 ~ 15 parts, Acrylic Acid Monomer 1.0 ~ 3.0 parts, acrylate functional monomer 0.5 ~ 3.0 part, hydroxyl oligomer 0.5 ~ 3 part, mix and prepare monomer mixture, it is for subsequent use that the monomer mixture 1-2 part emulsifier getting 10-15% prepares seed pre-emulsion;
By 1 ~ 2 part of emulsifying agent, 0.05-0.2 part sodium bicarbonate and 20 ~ 30 parts of deionized waters add in reactor, open and stir and raise the temperature of reaction system, the initiator of 10-15% is added after temperature reaches 78-83 DEG C, after stablizing 5-15 minute, seed pre-emulsion is dripped in 15-30 minute, stablize 15-30 minute, drip off in 3-4 hour by residual monomer mixture with 10 ~ 20 parts of remaining initiators of water dissolution, be warming up to 80-85 DEG C of slaking 1-2 hour, be cooled to 40-60 DEG C, with 3 ~ 10 parts of water dilutions, 0.3 ~ 0.6 part of neutralizing agent neutralization, be incubated cooling discharge after 15-30 minute and obtain hydroxy polyacrylate emulsion,
Described hydroxy-acrylate monomer is one or more of Hydroxyethyl acrylate, Propylene glycol monoacrylate, hydroxyethyl methylacrylate and Rocryl 410;
Described hydroxy-acrylate monomer is one or more of Hydroxyethyl acrylate, Propylene glycol monoacrylate, methacrylic hydroxyl ethyl ester and Rocryl 410.
Described Acrylic Acid Monomer be vinylformic acid, methacrylic acid one or more.
Described acrylate functional monomer be acrylamide, isobornyl methacrylate, glycidyl methacrylate, acetoacetoxyethyl methacrylate one or more.
Described hydroxyl oligomer is the urea formaldehyde A81 of BASF AG, the aldehyde ketone resin KR-80F of Changsha Chang Tai Industrial Co., Ltd., KR-120, KR120B, KR-120W, one or more of YHKR-1210, YHKR-1218 of UK-100, UK-300, UK-500, Ba Ling petrochemical industry aldehyde ketone resin of Weng Kaier company aldehyde ketone resin.
Described emulsifying agent is one or more in isomeric alcohol polyethenoxy ether (EH-9), the Chinese mugwort ADEKAREASOAP series non-ionic (ER-30) of Dicon A/S and negatively charged ion (SR-10) emulsifying agent, 2-acrylamide-2-methylpro panesulfonic acid sodium (COPS-2), AESA (KL-525), sodium lauryl sulphate (SDS).
Described initiator be Potassium Persulphate, ammonium persulphate one or more.
A kind of hydroxy polyacrylate emulsion, is obtained by above-mentioned preparation method.The hydroxy polyacrylate emulsion particle diameter < 300nm of gained, solids content 45-52%, hydroxyl value is 40-150mgKOH/g, Tg is 10-80 DEG C.
Hydroxy polyacrylate emulsion of the present invention is mainly used in prepares aqueous double-component polyurethane coating.
Hydroxy polyacrylate emulsion is joined in stirring tank, in mass fraction, add 1-10 part film coalescence aid, 0.05-1.5 part defoamer, 0.05-0.2 part thickening material, 0.05-0.3 part wetting agent and 0.05-0.1 part neutralizing agent, dispersion 10-30 minute, filter discharging, the coating of hydroxy polyacrylate emulsion preparation;
Described film coalescence aid be in propylene glycol monomethyl ether, propandiol butyl ether, dipropylene glycol methyl ether, dipropylene one or more.
Described defoamer be the modified polyorganosiloxane interpolymer solution B YK-019 of polyether siloxane copolymer defoamer TEGO-800, TEGO-805, TEGO-815, TEGO-825 and BYK company of TEGO company, BYK-020 one or more.
Described thickening material is one or more of non-ionic associative type thickening material TEGOViscoPlus3000, TEGOViscoPlus3030, TEGOViscoPlus3060 of non-ionic polyurethane associative thickener RM-8W, the hydrophobically-modified alkali swelling associative thickener TT-935 of DOW company, the swelling non-associative thickener ASE-60 of alkali and TEGO company.
Described wetting agent is one or more of polyether siloxane copolymer TEGO-245, the nonionic organic surfactant TEGO-500 of TEGO company and the Siloxane-Oxyalkylene Copolymers solution B YK-346 of BYK company.
Tell neutralizing agent be triethylamine, dimethylethanolamine one or more.
Described polyisocyanate curing agent comprise sulfonate, carboxylate salt and alkoxyl group hydrophilic modifying hexa-methylene two vulcabond (HDI) one or more.
Gained aqueous double-component polyurethane film has high gloss, high-clarity, water-fast and excellent chemical resistance, high crosslink density and high rigidity, anti scuffing and the advantage such as wear-resisting.Can be applicable to high-grade woodwork coating, car paint, metal anti-corrosive paint and other industrial protection coating.
Relative to prior art, tool of the present invention has the following advantages:
The chemical resistance of aqueous double-component polyurethane coating film is determined by film cross-linking density, by OH base content and the regulation and control of NCO and OH mol ratio of hydroxy polyacrylate emulsion; Appearance of film and decorate properties are determined by group partition inter-capacitive, the structure of consistency and water-based hydroxyl resin, particle structure and form, to the emulsifying capacity of solidifying agent and emulsifier content relevant.Hydroxy polyacrylate emulsion of the present invention is main components with polyacrylate polyol, and hydroxyl oligomer is auxiliary components.First with the hydroxyl oligomer that monomer dissolved mixture is appropriate, with appropriate emulsifying agent, pre-emulsification is carried out to it, get some or all of pre-emulsion and prepare seed, adopt the technique of pre-emulsification seeded emulsion polymerization can obtain hydroxy polyacrylate emulsion.Present invention obviates the problem that the excessive polymerization stability caused of hydroxy-acrylate monomer addition sharply reduces, therefore kind and addition by adjusting hydroxyl oligomer significantly can improve emulsion hydroxyl value and adjustment hydroxyl structure, thus improve machinery and the chemical property of two component film.Meanwhile, the hydroxyl oligomer of introducing itself has the feature such as high gloss, high-clarity, can improve outward appearance and the decorate properties of film further.The film of the aqueous double-component polyurethane coating that hydroxy polyacrylate emulsion of the present invention and aqueous polyisocyanate curing agent are prepared has the chemical resistance of high rigidity, high gloss and excellence, solve a difficult problem for paint film machinery that traditional hydroxy polyacrylate emulsion causes because hydroxyl value is low and chemical property difference, overcome the problems such as the supporting obtained gloss of film with aqueous polyisocyanate curing agent is low, poor transparency.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described, but embodiments of the present invention are not limited thereto, and for the processing parameter do not indicated especially, can refer to routine techniques and carry out.
Embodiment related detection method is as follows below:
Fundamental property test comprises: hydroxy polyacrylate emulsion is tested with reference to GB/T11175-2002 " synthetic resin emulsion test method ", outward appearance, pH, solids content, the viscosity of test emulsion.Paint film property is tested with reference to GB/T23999-2009 " indoor decorating use woodwork coating ", test gloss, hardness, water tolerance, dry heat resistance, alcohol resistance.The median size of emulsion adopts nano-particle size analysis instrument (ZSNanoS) to measure.
Embodiment 1
(1) preparation of hydroxy polyacrylate emulsion: (hydroxyl value=65mgKOH/g) formula of hydroxy polyacrylate emulsion is as table 1a:
Table 1a
Preparation technology: 1-9 is mixed with monomer mixture, gets 10% monomer mixture, 0.05 part of emulsifying agent (wherein 0.025 part of KL-525 and 0.025 part COPS-2) and 2.75 parts of water to its pre-emulsification as seed pre-emulsion.Residual emulsifier, sodium bicarbonate, 0.1 part of initiator (Potassium Persulphate), 25 parts of deionized waters are added in reactor, be warming up to 78 DEG C, stir 15 minutes, seed pre-emulsion was at the uniform velocity dripped off in 20 minutes, treat emulsion-stabilizing half an hour to obtain seed emulsion.Temperature of reaction system is kept to be 80 DEG C.Mix monomer will be remained mix with all the other monomers, then drip in seed emulsion, and drip the aqueous solution with 15 parts of water dissolution, 0.15 part of initiator (Potassium Persulphate) simultaneously, drip off at about 3.5h.85 DEG C are warming up to, insulation 1.5h after dripping.Be cooled to 55 DEG C, add neutralization by after 5.5 parts of water and the mixing of neutralizing agent triethylamine, insulation 0.25h, cooling discharge obtains milky white semi-transparent hydroxy polyacrylate emulsion.
(2) performance of hydroxy polyacrylate emulsion: the emulsion median size 128nm prepared, viscosity: 535cps, pH=7.0, solids content: 48.3%.
(3) preparation of high-performance water-based double-component polyurethane coating: formula is as table 1b:
Table 1b
The wherein mol ratio 1.8:1 of OH group in NCO group and hydroxy polyacrylate emulsion in solidifying agent.
Preparation method is as follows: emulsion joined in stirring tank, and rotating speed is 700 turns/min, by adding in emulsion after 10 parts of water and film coalescence aid premix, adds 5-9 raw material successively, disperses 20 minutes, filters discharging.During construction, aqueous polyisocyanate curing agent is joined in the coating of above-mentioned hydroxy polyacrylate emulsion preparation, stir 6 minutes, obtain aqueous double-component polyurethane coating.
(4) film performance: aqueous double-component polyurethane coating is obtained paint film and solidify dry 7 days at normal temperatures, its performance is as follows:
The over-all properties of the high-performance water-based double-component polyurethane coating of table 1c
The present embodiment adds hydroxyl oligomer A81 in the hydroxy polyacrylate emulsion of lower hydroxy radical content, is dissolved by monomer, and pre-emulsification, preparation emulsification seed emulsion, the basis of seed emulsion is prepared hydroxy polyacrylate emulsion.This method ensures that hydroxyl oligomer stable dispersion is in hydroxy polyacrylate emulsion, mainly be present in latex particle inside, acrylate monomer is polymerized in hydroxyl oligomer, form the interpenetrating polymer networks of polyacrylic ester and hydroxyl oligomer, ensure that hydroxyl oligomer fully mixes with between acrylate copolymer on the one hand, on the other hand, may there is a small amount of acrylate copolymer and be grafted on hydroxyl oligomer, graftomer provides the bridge of polymer-compatible.The interpolation of hydroxyl oligomer, improve the hydroxy radical content of hydroxy polyacrylate emulsion, ensure the polymerization stability of hydroxy polyacrylate emulsion, two component hardness of film is made to reach H, gloss (60 °) is 83%, have excellent water-fast/alcohol performance, also have good dry heat resistance, hydroxy polyacrylate emulsion prepared by the method overcomes the shortcoming that traditional hydroxy polyacrylate emulsion prepares double-component polyurethane coating.
Embodiment 2
(1) preparation of hydroxy polyacrylate emulsion: hydroxy polyacrylate emulsion (hydroxyl value=65mgKOH/g) formula is as table 2a:
Table 2a
Preparation method: 1-8 is mixed with monomer mixture, gets the molten use of 15% monomer mixture 0.1 part of emulsifying agent (being each 0.05 part of SR-10 and ER-30) and 3 parts of water to its pre-emulsification as seed pre-emulsion.Residual emulsifier, sodium bicarbonate, 0.1 part of initiator (ammonium persulphate), 30 parts of deionized waters are added in reactor, be warming up to 80 DEG C, stir 30 minutes, seed pre-emulsion was at the uniform velocity dripped off in 30 minutes, treat emulsion-stabilizing half an hour to obtain seed emulsion.Temperature of reaction system is kept to be 80 DEG C.Residual monomer mixture is dripped in seed emulsion, drips the aqueous solution with 20 parts of water dissolution, 0.2 part of initiator (ammonium persulphate) simultaneously, drip off at about 4h.82 DEG C are warming up to, insulation 2h after dripping.Be cooled to 45 DEG C, add neutralization by after 10 parts of water and the mixing of N, N-dimethylethanolamine, insulation 0.25h, cooling discharge obtains milky white semi-transparent hydroxy polyacrylate emulsion.
(2) performance of hydroxy polyacrylate emulsion: the emulsion median size 135nm prepared, viscosity: 573cps, pH=7.0, solids content: 48.5%.
(3) preparation of high-performance water-based double-component polyurethane coating: formula is as table 2b:
Table 2b
The wherein mol ratio 1.5:1 of OH group in NCO group and hydroxy polyacrylate emulsion in solidifying agent.
Preparation method is as follows: emulsion joined in stirring tank, and rotating speed is 700 turns/min, by adding in emulsion after 10 parts of water and film coalescence aid premix, adds 5-9 raw material successively, disperses 10 minutes, filters discharging.During construction, aqueous polyisocyanate curing agent is joined in the coating of above-mentioned hydroxy polyacrylate emulsion preparation, stir 5 minutes, obtain aqueous double-component polyurethane coating.
(4) dual-component coating performance: aqueous double-component polyurethane coating is obtained paint film and solidify dry 7 days at normal temperatures, its performance is as follows:
The over-all properties of the high-performance water-based double-component polyurethane coating of table 2c
Embodiment 3
(1) preparation of hydroxy polyacrylate emulsion: hydroxy polyacrylate emulsion (hydroxyl value=70mgKOH/g) formula is as table 3a:
Table 3a
Preparation technology: 1-8 is mixed with monomer mixture, gets 12% monomer mixture, 0.1 part of emulsifying agent (two kinds emulsifying agent each 0.05 part) and 3 parts of water to its pre-emulsification as seed pre-emulsion.Residual emulsifier, sodium bicarbonate, 0.1 part of initiator (KPS), 20 parts of deionized waters are added in reactor, be warming up to 82 DEG C, stir 15 minutes, seed pre-emulsion was at the uniform velocity dripped off in 15 minutes, treat emulsion-stabilizing half an hour to obtain seed emulsion.Temperature of reaction system is kept to be 82 DEG C.Residual monomer mixture is mixed with all the other monomers, then drips in seed emulsion, drip the aqueous solution with 10 parts of water dissolution, 0.2 part of initiator (KPS) simultaneously, drip off at about 3h.85 DEG C are warming up to, insulation 1h after dripping.Be cooled to 60 DEG C, add neutralization by after 5.9 parts of water and triethylamine mixing, insulation 30min, cooling discharge obtains milky white semi-transparent hydroxy polyacrylate emulsion.
(2) performance of hydroxy polyacrylate emulsion: the emulsion median size 123nm prepared, viscosity: 617cps, pH=7.0, solids content: 48.0%.
(3) preparation of high-performance water-based double-component polyurethane coating: formula is as table 3b:
Table 3b
The wherein mol ratio 1.2:1 of OH group in NCO group and hydroxy polyacrylate emulsion in solidifying agent.
Preparation method is as follows: emulsion joined in stirring tank, and rotating speed is 700 turns/min, by adding in emulsion after 10 parts of water and film coalescence aid premix, adds 5-9 raw material successively, disperses 10 minutes, filters discharging.During construction, aqueous polyisocyanate curing agent is joined in the coating of above-mentioned hydroxy polyacrylate emulsion preparation, stir 8 minutes, obtain aqueous double-component polyurethane coating.
(4) by the paint film property of aqueous double-component polyurethane coating: obtained paint film solidifies dry 7 days at normal temperatures, and its performance is as follows:
The over-all properties of the high-performance water-based double-component polyurethane coating of table 3c
Embodiment 4
(1) preparation of hydroxy polyacrylate emulsion: hydroxy polyacrylate emulsion (hydroxyl value=79mgKOH/g) formula is as table 4a:
Table 4a
Preparation technology: mixed by 1-8 and prepare monomer mixture, gets 14 parts of monomer mixtures, 0.1 part of emulsifying agent (two kinds emulsifying agent each 0.05 part) and 3.35 parts of water to its pre-emulsification as seed pre-emulsion.Residual emulsifier, sodium bicarbonate, 0.1 part of initiator, 25 parts of deionized waters are added in reactor, is warming up to 75 DEG C, stirs 15 minutes, seed pre-emulsion was at the uniform velocity dripped off in 20 minutes, treat emulsion-stabilizing half an hour to obtain seed emulsion.Temperature of reaction system is kept to be 80 DEG C.Residual monomer mixture is dripped in seed emulsion, drips the aqueous solution with 15 parts of water dissolution, 0.2 part of initiator simultaneously, drip off at about 3.5h.85 DEG C are warming up to, insulation 1.5h after dripping.Be cooled to 55 DEG C, add neutralization by after 6 parts of water and N, N-dimethylethanolamine mixing, insulation 0.25h, cooling discharge obtains milky white semi-transparent hydroxy polyacrylate emulsion.
(2) performance of hydroxy polyacrylate emulsion: the emulsion median size 119nm prepared, viscosity: 820cps, pH=7.0, solids content: 47.7%.
(3) preparation of high-performance water-based double-component polyurethane coating: formula is as table 4b:
Table 4b
The wherein mol ratio 1.8:1 of OH group in NCO group and hydroxy polyacrylate emulsion in solidifying agent.
Preparation method is as follows: emulsion joined in stirring tank, and rotating speed is 700 turns/min, by adding in emulsion after 10 parts of water and film coalescence aid premix, adds 5-9 raw material successively, disperses 25 minutes, filters discharging.During construction, aqueous polyisocyanate curing agent is joined in the coating of above-mentioned hydroxy polyacrylate emulsion preparation, stir 7 minutes, obtain aqueous double-component polyurethane coating.
(4) film performance of aqueous double-component polyurethane coating: aqueous double-component polyurethane coating is obtained paint film and solidify dry 7 days at normal temperatures, its performance is as follows:
The over-all properties of the high-performance water-based double-component polyurethane coating of table 4c
Embodiment 5
(1) preparation of hydroxy polyacrylate emulsion: hydroxy polyacrylate emulsion (hydroxyl value=95mgKOH/g) formula is as table 5a:
Table 5a
Preparation technology: mixed by 1-7 and prepare monomer mixture, gets 13 parts of monomer mixtures, 0.1 part of emulsifying agent (two kinds emulsifying agent each 0.05 part) and 4 parts of water to its pre-emulsification as seed pre-emulsion.Residual emulsifier, sodium bicarbonate, 0.1 part of initiator, 25 parts of deionized waters are added in reactor, is warming up to 75 DEG C, stirs 15 minutes, seed pre-emulsion was at the uniform velocity dripped off in 20 minutes, treat emulsion-stabilizing half an hour to obtain seed emulsion.Temperature of reaction system is kept to be 80 DEG C.Residual monomer mixture is dripped in seed emulsion, drips the aqueous solution with 15 parts of water dissolution, 0.2 part of initiator simultaneously, drip off at about 3.5h.85 DEG C are warming up to, insulation 1.5h after dripping.Be cooled to 55 DEG C, add neutralization by after 5.9 parts of water and triethylamine mixing, insulation 0.25h, cooling discharge obtains milky white semi-transparent hydroxy polyacrylate emulsion.
(2) performance of hydroxy polyacrylate emulsion: the emulsion median size 132nm prepared, viscosity: 673cps, pH=7.0, solids content: 48.2%.
(3) preparation of high-performance water-based double-component polyurethane coating: formula is as table 5b:
Table 5b
The wherein mol ratio 1.5:1 of OH group in NCO group and hydroxy polyacrylate emulsion in solidifying agent.
Preparation method is as follows: emulsion joined in stirring tank, and rotating speed is 700 turns/min, by adding in emulsion after 10 parts of water and film coalescence aid premix, adds 5-9 raw material successively, disperses 30 minutes, filters discharging.During construction, aqueous polyisocyanate curing agent is joined in the coating of above-mentioned hydroxy polyacrylate emulsion preparation, stir 6 minutes, obtain aqueous double-component polyurethane coating.
(4) film performance of aqueous double-component polyurethane coating: aqueous double-component polyurethane coating is obtained paint film and solidify dry 7 days at normal temperatures, its performance is as follows:
The over-all properties of the high-performance water-based double-component polyurethane coating of table 5c
Embodiment 6
(1) preparation of hydroxy polyacrylate emulsion: hydroxy polyacrylate emulsion (hydroxyl value=110mgKOH/g) formula is as table 6a:
Table 6a
Preparation technology: mixed by 1-7 and prepare monomer mixture, gets 10% monomer mixture, 0.1 part of emulsifying agent (two kinds emulsifying agent each 0.05 part) and 4.5 parts of water to its pre-emulsification as seed pre-emulsion.Residual emulsifier, sodium bicarbonate, 0.1 part of initiator, 25 parts of deionized waters are added in reactor, is warming up to 75 DEG C, stirs 15 minutes, seed pre-emulsion was at the uniform velocity dripped off in 20 minutes, treat emulsion-stabilizing half an hour to obtain seed emulsion.Temperature of reaction system is kept to be 80 DEG C.Residual monomer blend mixture is dripped in seed emulsion, drips the aqueous solution with 15 parts of water dissolution, 0.2 part of initiator simultaneously, drip off at about 3.5h.85 DEG C are warming up to, insulation 1.5h after dripping.Be cooled to 55 DEG C, add neutralization by after 5.55 parts of water and N, N-dimethylethanolamine mixing, insulation 0.25h, cooling discharge obtains milky white semi-transparent hydroxy polyacrylate emulsion.
(2) performance of hydroxy polyacrylate emulsion: the emulsion median size 125nm prepared, viscosity: 725cps, pH=7.0, solids content: 47.6%.
(3) preparation of high-performance water-based double-component polyurethane coating: formula is as table 6b:
Table 6b
The wherein mol ratio 1.0:1 of OH group in NCO group and hydroxy polyacrylate emulsion in solidifying agent.
Preparation method is as follows: emulsion joined in stirring tank, and rotating speed is 700 turns/min, by adding in emulsion after 10 parts of water and film coalescence aid premix, adds 5-9 raw material successively, disperses 20 minutes, filters discharging.During construction, aqueous polyisocyanate curing agent is joined in the coating of above-mentioned hydroxy polyacrylate emulsion preparation, stir 5 minutes, obtain aqueous double-component polyurethane coating.
(4) film performance of aqueous double-component polyurethane coating: aqueous double-component polyurethane coating is obtained paint film and solidify dry 7 days at normal temperatures, its performance is as follows:
The over-all properties of the high-performance water-based double-component polyurethane coating of table 6c
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (8)
1. a preparation method for hydroxy polyacrylate, is characterized in that comprising following steps,
1) in mass fraction, take acrylate monomer and/or methacrylate monomer 30 ~ 45 parts, hydroxy-acrylate monomer 5 ~ 15 parts, Acrylic Acid Monomer 1.0 ~ 3.0 parts, acrylate functional monomer 0.5 ~ 3.0 part, hydroxyl oligomer 0.5 ~ 3 part, mix and prepare monomer mixture, it is for subsequent use that the monomer mixture 1-2 part emulsifier getting 10-15% prepares seed pre-emulsion;
2) in mass fraction, by 1 ~ 2 part of emulsifying agent, 0.05-0.2 part sodium bicarbonate and 20 ~ 30 parts of deionized waters add in reactor, open and stir and raise the temperature of reaction system, the initiator of 10-15% is added after temperature reaches 78-83 DEG C, after stablizing 5-15 minute, seed pre-emulsion is dripped in 15-30 minute, stablize 15-30 minute, drip off in 3-4 hour by residual monomer mixture with 10 ~ 20 parts of remaining initiators of water dissolution, be warming up to 80-85 DEG C of slaking 1-2 hour, be cooled to 40-60 DEG C, with 3 ~ 10 parts of water dilutions, 0.3 ~ 0.6 part of neutralizing agent neutralization, be incubated cooling discharge after 15-30 minute and obtain hydroxy polyacrylate emulsion,
Described acrylate monomer and/or methacrylate monomer be methyl methacrylate, methyl acrylate, ethyl propenoate, butyl methacrylate, butyl acrylate and cinnamic one or more;
Described hydroxy-acrylate monomer is one or more of Hydroxyethyl acrylate, Propylene glycol monoacrylate, hydroxyethyl methylacrylate and Rocryl 410;
Described Acrylic Acid Monomer is vinylformic acid and/or methacrylic acid;
Described acrylate functional monomer be acrylamide, isobornyl methacrylate, glycidyl methacrylate, acetoacetoxyethyl methacrylate one or more;
Described hydroxyl oligomer is one or more of YHKR-1210 and YHKR-1218 of urea formaldehyde A81, aldehyde ketone resin KR-80F, KR-120, KR120B, KR-120W, aldehyde ketone resin UK-100, UK-300, UK-500, aldehyde ketone resin;
Described emulsifying agent be isomeric alcohol polyethenoxy ether, polymerisable emulsifier ADEKAREASOAP series non-ionic ER-30 and negatively charged ion SR-10 emulsifying agent, 2-acrylamide-2-methylpro panesulfonic acid sodium, AESA and sodium lauryl sulphate one or more;
Described initiator be Potassium Persulphate, ammonium persulphate one or more.
2. the preparation method of hydroxy polyacrylate emulsion according to claim 1, is characterized in that, described neutralizing agent is one or more in triethylamine, ammoniacal liquor and dimethylethanolamine.
3. the preparation method of hydroxy polyacrylate emulsion according to claim 1, is characterized in that, the hydroxyl value of described hydroxy polyacrylate emulsion is 40-150mgKOH/g (in solid resin).
4. the preparation method of hydroxy polyacrylate emulsion according to claim 1, is characterized in that, the glass transition temp of described hydroxy polyacrylate emulsion is 10-80 DEG C.
5. a hydroxy polyacrylate emulsion, is characterised in that described in it, and it is obtained by preparation method described in any one of claim 1-4.
6. the application of hydroxy polyacrylate emulsion in aqueous double-component polyurethane coating described in claim 5.
7. the application of hydroxy polyacrylate emulsion in aqueous double-component polyurethane coating according to 6, is characterized in that comprising the steps:
1) hydroxy polyacrylate emulsion is joined in stirring tank, in mass fraction, add 1-10 part film coalescence aid, 0.05-1.5 part defoamer, 0.05-0.2 part thickening material, 0.05-0.3 part wetting agent and 0.05-0.1 part neutralizing agent, dispersion 10-30 minute, filter discharging, the coating of hydroxy polyacrylate emulsion preparation;
2) construction time, by aqueous polyisocyanate curing agent according to NCO/OH mol ratio be 1.0-1.8 join described hydroxy polyacrylate emulsion preparation coating in, stir 5-8 minute, obtain aqueous double-component polyurethane coating.
8. the application of hydroxy polyacrylate emulsion in aqueous double-component polyurethane coating according to 7, is characterized in that, described film coalescence aid is one or more of propylene glycol monomethyl ether, propandiol butyl ether, dipropylene glycol methyl ether and dipropylene;
Described defoamer be polyether siloxane copolymer defoamer TEGO-800, TEGO-805, TEGO-815, TEGO-825, modified polyorganosiloxane interpolymer solution B YK-019 and BYK-020 one or more;
Described thickening material be non-ionic polyurethane associative thickener RM-8W, hydrophobically-modified alkali swelling associative thickener TT-935, the swelling non-associative thickener ASE-60 of alkali, non-ionic associative type thickening material TEGOViscoPlus3000, TEGOViscoPlus3030 and TEGOViscoPlus3060 one or more;
Described wetting agent is one or more of polyether siloxane copolymer TEGO-245, nonionic organic surfactant TEGO-500 and Siloxane-Oxyalkylene Copolymers solution B YK-346.
Described neutralizing agent is one or more in triethylamine, ammoniacal liquor and dimethylethanolamine.
Described polyisocyanate curing agent comprise in the hexamethylene diisocyanate of sulfonate, carboxylate salt and alkoxyl group hydrophilic modifying one or more.
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