CN108948994A - A kind of aqueous double-component is from delustring woodwork coating and preparation method thereof - Google Patents

A kind of aqueous double-component is from delustring woodwork coating and preparation method thereof Download PDF

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Publication number
CN108948994A
CN108948994A CN201810715265.8A CN201810715265A CN108948994A CN 108948994 A CN108948994 A CN 108948994A CN 201810715265 A CN201810715265 A CN 201810715265A CN 108948994 A CN108948994 A CN 108948994A
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delustring
monomer
hydroxy
aqueous
additive amount
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黄洪
胡天科
司徒粤
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South China University of Technology SCUT
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South China University of Technology SCUT
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
    • C08G18/6216—Polymers of alpha-beta ethylenically unsaturated carboxylic acids or of derivatives thereof
    • C08G18/622—Polymers of esters of alpha-beta ethylenically unsaturated carboxylic acids
    • C08G18/6225—Polymers of esters of acrylic or methacrylic acid
    • C08G18/6229—Polymers of hydroxy groups containing esters of acrylic or methacrylic acid with aliphatic polyalcohols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
    • C08G18/6216—Polymers of alpha-beta ethylenically unsaturated carboxylic acids or of derivatives thereof
    • C08G18/625—Polymers of alpha-beta ethylenically unsaturated carboxylic acids; hydrolyzed polymers of esters of these acids

Abstract

The invention discloses a kind of aqueous double-components from delustring woodwork coating and preparation method thereof.First reactor stirring is added in emulsifier and water by this method, and part acrylic acid esters monomer, initiator and function monomer mixed liquor is then added dropwise, is reacted to obtain stratum nucleare resin；When reactor solution blue light occurs and has obvious backflow phenomenon, remaining part propylene esters of gallic acid and hydroxy acids monomer mixed solution are added dropwise, reacted to obtain shell resin；Finally plus neutralizer and add distilled water high speed dispersion, obtain aqueous from delustring hydroxy acrylic acid secondary breakup body；Aqueous double-component is prepared from delustring woodwork coating with water-based polyurethane curing agent, auxiliary agent mixing again.Preparation method of the invention is simple, environmentally friendly, and coating storage stability obtained is high, and paint film extinction is good, and mechanical performance is stronger, and chemicals-resistant and contaminated resistance are more excellent.

Description

A kind of aqueous double-component is from delustring woodwork coating and preparation method thereof
Technical field
The invention belongs to water-borne wood coating fields, are related to a kind of aqueous double-component woodwork coating, in particular to a kind of water Property two-component is from delustring woodwork coating and preparation method thereof.
Background technique
It is increasingly stringent to the management of industry as domestic and international multiple laws, regulation gradually come into force, greatly limit tradition The production of solvent based coating and the use of product.And the gradually appearance of water paint, Environmentally friendly coatings standard, it implies new Opportunities and challenges.
The irreversible development trend of water paint will be one of the developing direction in coatings enterprises future.High-quality is aqueous It is even more an emphasis direction of furniture industry from delustring woodwork coating, indoor furniture has mostly used delustring face, has been covered in outside room The wooden boards in portion also delustring appearance substantially.When facing selection light or delustring effect, we are not limited solely to The demand of fashion and appearance.It was verified that the requirement of property, brightness effect and touch perception easy to clean etc. also affects us Selection, after film delustring to the good texture of people and it is comfortable feel, favored by people very much.In addition, economical and practical is also choosing Another key factor for selecting coating surface state, when certain substrates are scratched, have slight indentation and make dirty, using delustring Coating can cover up these defects, and coat polish lacquer and be difficult to cover such flaw.
The main delustering agent of addition in addition reaches extinction effect currently on the market, but the addition of delustering agent can make coating in drying Micro- rough surface is formed in the process, wherein most study is silica, it is modified by the way that silica flatting silica is added, it is closed At coating to be easy to appear dispersion uneven and cause varnish transparency not high, while the addition of flatting silica will lead to resistance to Jie of film Matter performance is decreased obviously.The matting resin then mainly delustring using the distinctive structure of organic matter and group absorptions light.Therefore, In order to obtain environmental-friendly and make it have good extinction, being synthesized using the semicontinuous dropwise addition mode of emulsion polymerization can be from delustring Water-based hydroxyl acrylic acid dispersion, in conjunction with the special construction of dumb light curing agent itself, to be generated from molecular structure good Delustring performance.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of system of two-component from delustring woodwork coating Preparation Method.
The object of the invention is also to provide a kind of two-components as made from above-mentioned preparation method from delustring woodwork coating.
The purpose of the present invention is achieved through the following technical solutions.
A kind of aqueous double-component includes the following steps: from the preparation method of delustring woodwork coating
(1) emulsifier and distilled water are added in the reaction vessel, insulated and stirred is uniform, then uniformly mixed acrylic acid is added dropwise Esters monomer, initiator and function monomer heat up and keep the temperature and reacted；
(2) step (1) after reaction, when mixed solution blue light occurs and has obvious backflow phenomenon, is added dropwise and is uniformly mixed Acrylic ester monomer and hydroxy acids monomer, heat preservation continue to react；
(3) step (2) after reaction, is added neutralizer and stirs evenly, add distilled water and dispersed, cool down, Filtering and discharging obtains aqueous from delustring hydroxy acrylic acid secondary breakup body；
(4) obtain it is aqueous from delustring hydroxy acrylic acid secondary breakup body be added defoaming agent, wetting agent, levelling agent and Deionized water is uniformly mixed, then is mixed evenly with water-based polyurethane curing agent, obtains the aqueous double-component from delustring wood Device coating.
Preferably, in step (1), the emulsifier is isomeric alcohol polyethenoxy ether, fatty alcohol polyoxyethylene ether ammonium sulfate With one kind of lauryl sodium sulfate, additive amount is that acrylic ester monomer total addition level and hydroxy acids monomer add The 1%~2% of the gross mass of amount.
It is furthermore preferred that the emulsifier is fatty alcohol polyoxyethylene ether ammonium sulfate in step (1).
Still more preferably, the preferred isomeric alcohol polyethenoxy ether ammonium sulfate of the fatty alcohol polyoxyethylene ether ammonium sulfate.
Preferably, in step (1), the additive amount of the distilled water is acrylic ester monomer total addition level and hydroxy The 20%~40% of the gross mass of acrylic monomer additive amount, more preferable 30%~40%.
Preferably, in step (1), the insulated and stirred is uniformly that insulated and stirred is uniform at 40~50 DEG C.
Preferably, in step (1), the acrylic ester monomer be methyl methacrylate, butyl methacrylate and One kind of butyl acrylate, the more preferably methyl methacrylate and butyl acrylate of mass ratio 1:0.43~0.80, add Dosage accounts for the 60%~75% of acrylic ester monomer total addition level.
Preferably, in step (1), the initiator is one kind of potassium peroxydisulfate and ammonium persulfate, and additive amount is propylene The 0.5%~1.1% of the gross mass of esters of gallic acid monomer total addition level and hydroxy acids monomer additive amount, more preferably 0.8%~1.1%.
It is furthermore preferred that the initiator is potassium peroxydisulfate in step (1).
Preferably, in step (1), the function monomer is isobornyl methacrylate, methyl propenoic acid glycidyl One of ester, hydroxyethyl methacrylate and hydroxypropyl acrylate, additive amount be acrylic ester monomer total addition level and The 2.6%~5.1% of the gross mass of hydroxy acids monomer additive amount, more preferably 3.5%~4.5%.
It is furthermore preferred that the function monomer is isobornyl methacrylate in step (1).
Preferably, in step (1), the used time of uniformly mixed acrylic ester monomer, initiator and function monomer is added dropwise It is 4~5 hours.
Preferably, in step (1), the heating is to be warming up to 70~75 DEG C.
Preferably, in step (1), the time of the reaction is 1~1.5 hour.
Hydrophobic stratum nucleare resin can be obtained by the reaction of step (1).
Preferably, in step (2), the acrylic ester monomer be methyl methacrylate, butyl methacrylate and One kind of butyl acrylate.Using the additive amount of the acrylic ester monomer in step (1) and step (2) as acrylic ester monomer Total addition level.
Preferably, in step (2), the hydroxy acids monomer be one of acrylic acid and methacrylic acid, Additive amount be acrylic ester monomer total addition level 1.2wt%~2.9wt%, more preferably 1.8%~2.7%.
It is furthermore preferred that the hydroxy acids monomer is acrylic acid in step (2).
Preferably, in step (2), uniformly mixed acrylic ester monomer and hydroxy acids monomer used time 3 is added dropwise ~4 hours.
Preferably, in step (2), it is that the reaction was continued is 1~2 small in 70~75 DEG C of heat preservations that the heat preservation, which continues reaction, When.
Hydrophilic shell resin can be obtained by the reaction of step (2).
Preferably, in step (3), the neutralizer is triethylamine and N, one of N- dimethylethanolamine, addition Amount is the 0.9%~1.5% of the gross mass of acrylic ester monomer total addition level and hydroxy acids monomer additive amount.
It is furthermore preferred that in step (3), the neutralizer is N, N- dimethylethanolamine,
Preferably, in step (3), the time of the stirring is 30~50 minutes.
Preferably, in step (3), the time of the dispersion is 1~1.5 hour.
Preferably, in step (3), the distilled water and acrylic ester monomer total addition level and hydroxy acids monomer The mass ratio of the gross mass of additive amount is 0.8~0.9:1.
Preferably, in step (3), the aqueous solid content 47 ± 1.0% from delustring hydroxy acrylic acid secondary breakup body, Hydroxy radical content 4.0 ± 0.2%, viscosity 1200-2500mPas (25 DEG C), pH value 6.5-9, acid value≤20, Δ Tg50 DEG C of >, storage It is good to deposit stability.
Preferably, in step (4), the defoaming agent be the chemical Science and Technology Ltd.'s trade mark in firm gram of Shanghai be YCK-660 and One of defoaming agent of YCK-670, additive amount are aqueous from the 0.15% of delustring hydroxy acrylic acid secondary breakup weight ~0.2%.
Preferably, in step (4), the wetting agent is that firm gram of the Shanghai chemical Science and Technology Ltd. trade mark is YCK-1540's Wetting agent, additive amount are aqueous from the 0.3%~0.4% of delustring hydroxy acrylic acid secondary breakup weight.
Preferably, in step (4), the levelling agent be the chemical Science and Technology Ltd.'s trade mark in firm gram of Shanghai be YCK-2490 and One of levelling agent of YCK-1470, additive amount are aqueous from the 0.15% of delustring hydroxy acrylic acid secondary breakup weight ~0.25%.
Preferably, in step (4), the additive amount of the deionized water is aqueous from delustring hydroxy acrylic acid secondary breakup body The 11%~15% of quality.
Preferably, in step (4), the water-based polyurethane curing agent is that Bayer A.G's trade mark is XP2655 (- NCO Content 20.7%-21.7%, 3500 ± 1000mPas of viscosity, free isocyanate content is less than aqueous polyurethane 0.3%) Curing agent, additive amount are added according to-NCO/-OH molar ratio 1.4 (n (- NCO)/n (- OH)=1.4).
The aqueous double-component prepared by preparation method described in any of the above embodiments is from delustring woodwork coating.
Preferably, the aqueous double-component is sprayed on woodenware template from delustring woodwork coating and obtains film, room temperature is protected Deposit 7d and test performance, glossiness 20 ± 1%, 30 ± 1.5min of surface drying time does solid work 6 ± 0.5h of time, pencil hardness 3H, attached Put forth effort 0, impact resistance ± 50kgcm, water resistance >=165h, alcohol resistance is good, and transparency is good, working life >=3.8h.
First reactor is added in emulsifier aqueous solution by preparation method of the present invention, then by partial monosomy and initiator put into Row polymerization reaction, polymerization to a certain extent and then by remaining monomer in the case where continuous addition sustained response to whole Polymerization process is completed.Lotion synthesis is to use the double technologies of special self-crosslinking-nucleocapsid, and lotion is made to have special structure, because This has low film formation temperature, high intensity and good resistance to blocking energy, and core-shell structure also has extinction effect.It arranges in pairs or groups again dumb light Water-based polyurethane curing agent prepares dual-component coating, and surface forms one layer of close, non-flat and smooth film when film forming, works as light When line is radiated at film coated surface, due to film coated surface roughness with higher, light occurs diffusing reflection phenomenon on surface and reaches To delustring.
Compared with prior art, the present invention has the advantage that
(1) preparation method of the present invention has synthesized the hydroxy acrylic acid second level from delustring using semi-continuous emulsion polymerization Dispersion, operating method is easier, environmentally friendly, and polymerization reaction is also easier to control.
(2) present invention is a kind of special using the hydroxy acrylic acid secondary breakup body of the double technology synthesis of self-crosslinking-nucleocapsid Core-shell structure, nuclear structure have different T from shell structuregTemperature, the two difference DELTA TgAt 50 DEG C or more, thus have good Delustring performance.
(3) prepared from delustring Hydroxylated acrylic resin and water-based polyurethane curing agent collocation double groups of the invention by synthesis Part coating delustring can be not necessarily to add flatting silica outside on molecular structure, and extinction effect is obvious, while having higher storage surely Qualitative, transparency, gloss uniformity, stronger mechanical performance, and also film chemicals-resistant and contaminated resistance are more excellent.
Specific embodiment
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment, but protection scope of the present invention It is without being limited thereto with embodiment.
Embodiment 1
A kind of preparation of aqueous double-component from delustring woodwork coating, comprising the following steps:
(1) in the four-hole boiling flask equipped with blender, constant pressure funnel, condenser pipe and thermometer, it is poly- that isomery alcohol is added Ethylene oxide ether ammonium sulfate 1.46g and distilled water 58.29g is maintained at 40 DEG C of stirrings；
(2) methyl methacrylate 75g and butyl acrylate 32.25g, potassium peroxydisulfate 1.16g and methyl-prop are accurately weighed Olefin(e) acid isobornyl thiocyanoacetate 5.09g is uniformly mixed, and is added drop-wise in step (1) reaction vessel and is warming up to 70 DEG C, time for adding 4h, heat preservation 1.5h is reacted, hydrophobic stratum nucleare resin is obtained；
(3) when solution blue light occurs and has obvious backflow phenomenon, remaining part methyl methyl acrylate is accurately weighed 25g, butyl acrylate 10.75g and acrylic acid 2.57g are uniformly mixed, and are added drop-wise in step (2) reaction vessel and are kept reaction temperature 70 DEG C, time for adding 3.5h, insulation reaction 1h, obtain hydrophilic shell resin；
(4) N is eventually adding to add after stirring 50min in N- dimethylethanolamine 1.31g to step (3) reaction such as distilled water 116.45g high speed dispersion 1h, filtering and discharging after cooling obtain aqueous from delustring hydroxy acrylic acid secondary breakup body, water obtained Property is from the performance parameter of delustring hydroxy acrylic acid secondary breakup body as shown in table 1A.
By table 1A it is found that gained is aqueous meets index from delustring hydroxy acrylic acid secondary breakup body various performance parameters and want Ask: the milky white blueing light of appearance, storage stability are high, admittedly contain, viscosity, hydroxy radical content, pH value, acid value are within the scope of parameter request, ΔTgThere is extinction greater than 50 DEG C.
(5) it accurately weighs aqueous from mat acrylic secondary breakup body 60g, addition 0.09g defoaming agent obtained by step (4) YCK-660,0.18g wetting agent YCK-1540,0.09g levelling agent YCK-2490 and 6.60g deionized water are uniformly mixed, then are weighed 2655 water-based polyurethane curing agent 14.57g of Bayer XP prepares woodcare paint to get two-component is arrived from delustring woodwork coating, and sprays Be applied on woodenware template, room temperature preservation 7d test performance, test paint film property index as shown in table 1B.
By table 1B it is found that obtained aqueous double-component meets finger with paint film performance indexes after paint from delustring woodwork coating Mark requires: dry speed is suitable for that hardness is high, and transparency and adhesive force are good, and impact resistance and patience are high, and glossiness is low, extinction It is good.
Embodiment 2
A kind of preparation of aqueous double-component from delustring woodwork coating, comprising the following steps:
(1) in the four-hole boiling flask equipped with blender, constant pressure funnel, condenser pipe and thermometer, it is poly- that isomery alcohol is added Ethylene oxide ether ammonium sulfate 2.30g and distilled water 53.55g is maintained at 50 DEG C of stirrings；
(2) methyl methacrylate 60g and butyl acrylate 30g, ammonium persulfate 1.53g and methacrylic acid are accurately weighed Ethylene oxidic ester 6.12g is uniformly mixed, and is added drop-wise in step (1) reaction vessel and is warming up to 75 DEG C, time for adding 4h, heat preservation is anti- 1h is answered, hydrophobic stratum nucleare resin is obtained；
(3) when solution blue light occurs and has obvious backflow phenomenon, remaining part methyl methyl acrylate is accurately weighed 40g, butyl acrylate 20g and methacrylic acid 3g are uniformly mixed, and are added drop-wise in step (2) reaction vessel and are kept reaction temperature 75 DEG C, time for adding 3.5h, insulation reaction 2h obtain hydrophilic shell resin；
(4) N is eventually adding to add after stirring 45min in N- dimethylethanolamine 1.53g to step (3) reaction such as distilled water 122.40g high speed dispersion 1.4h, filtering and discharging after cooling, obtain it is aqueous from delustring hydroxy acrylic acid secondary breakup body, it is obtained The aqueous performance parameter from delustring hydroxy acrylic acid secondary breakup body is as set forth in table 2.
By table 2A it is found that gained is aqueous meets index from delustring hydroxy acrylic acid secondary breakup body various performance parameters and want Ask: the milky white blueing light of appearance, storage stability are high, admittedly contain, viscosity, hydroxy radical content, pH value, acid value are within the scope of parameter request, ΔTgThere is extinction greater than 50 DEG C.
(5) it accurately weighs aqueous from mat acrylic secondary breakup body 60.00g obtained by step (4), 0.10g is added and disappears Infusion YCK-670,0.20g wetting agent YCK-1540,0.11g levelling agent YCK-2490 and 7.80g deionized water is uniformly mixed, then 2655 water-based polyurethane curing agent 15.29g of Bayer XP is weighed, prepares woodcare paint to get to two-component from delustring woodwork coating, And be sprayed on woodenware template, room temperature preservation 7d test performance, test paint film property index as shown in table 2B.
Table 2B aqueous double-component is from delustring woodwork coating paint film physical and chemical performance parameter
By table 2B it is found that obtained aqueous double-component meets finger with paint film performance indexes after paint from delustring woodwork coating Mark requires: dry speed is suitable for that hardness is high, and transparency and adhesive force are good, and impact resistance and patience are high, and glossiness is low, extinction It is good.
Embodiment 3
A kind of preparation of aqueous double-component from delustring woodwork coating, comprising the following steps:
(1) in the four-hole boiling flask equipped with blender, constant pressure funnel, condenser pipe and thermometer, it is poly- that isomery alcohol is added Ethylene oxide ether 2.45g and distilled water 58.88g is maintained at 45 DEG C of stirrings；
(2) methyl methacrylate 65g and butyl acrylate 39g, potassium peroxydisulfate 1.47g and acrylic acid hydroxypropyl are accurately weighed Ester 6.21g is uniformly mixed, and is added drop-wise in step (1) reaction vessel and is warming up to 75 DEG C, time for adding 4.5h, insulation reaction 1.5h obtains hydrophobic stratum nucleare resin；
(3) when solution blue light occurs and has obvious backflow phenomenon, remaining part methyl methyl acrylate is accurately weighed 35g, butyl acrylate 21g and acrylic acid 3.52g are uniformly mixed, and are added drop-wise in step (2) reaction vessel and are kept reaction temperature 75 DEG C, time for adding 3h, insulation reaction 1.5h obtain hydrophilic shell resin；
(4) it is eventually adding triethylamine 1.96g and after stirring 35min, adds into step (3) reaction such as distilled water 147.17g high Speed dispersion 1.5h, filtering and discharging after cooling, obtain it is aqueous from delustring hydroxy acrylic acid secondary breakup body, it is obtained aqueous from delustring The performance parameter of hydroxy acrylic acid secondary breakup body is as shown in table 3A.
By table 3A it is found that gained is aqueous meets index from delustring hydroxy acrylic acid secondary breakup body various performance parameters and want Ask: the milky white blueing light of appearance, storage stability are high, admittedly contain, viscosity, hydroxy radical content, pH value, acid value are within the scope of parameter request, ΔTgThere is extinction greater than 50 DEG C.
(5) it accurately weighs aqueous from mat acrylic secondary breakup body 60g, addition 0.11g defoaming agent obtained by step (4) YCK-660,0.21g wetting agent YCK-1540,0.12g levelling agent YCK-1470 and 8.40g deionized water are uniformly mixed, then are weighed 2655 water-based polyurethane curing agent 13.84g of Bayer XP prepares woodcare paint to get two-component is arrived from delustring woodwork coating, and sprays Be applied on woodenware template, room temperature preservation 7d test performance, test paint film property index as shown in table 3B.
Table 3B aqueous double-component is from delustring woodwork coating paint film physical and chemical performance parameter
By table 3B it is found that obtained aqueous double-component meets finger with paint film performance indexes after paint from delustring woodwork coating Mark requires: dry speed is suitable for that hardness is high, and transparency and adhesive force are good, and impact resistance and patience are high, and glossiness is low, extinction It is good.
Embodiment 4
A kind of preparation of aqueous double-component from delustring woodwork coating, comprising the following steps:
(1) in the four-hole boiling flask equipped with blender, constant pressure funnel, condenser pipe and thermometer, it is poly- that isomery alcohol is added Ethylene oxide ether ammonium sulfate 3.49g and distilled water 66.22g is maintained at 45 DEG C of stirrings；
(2) methyl methacrylate 70g and butyl acrylate 49g, potassium peroxydisulfate 2.09g and methacrylic acid are accurately weighed Isobornyl thiocyanoacetate 7.32g is uniformly mixed, and is added drop-wise in step (1) reaction vessel and is warming up to 70 DEG C, time for adding 5h, insulation reaction 1h obtains hydrophobic stratum nucleare resin；
(3) when solution blue light occurs and has obvious backflow phenomenon, remaining part methyl methyl acrylate is accurately weighed 30g, butyl acrylate 21g and acrylic acid 4.25g are uniformly mixed, and are added drop-wise in step (2) reaction vessel and are kept reaction temperature 70 DEG C, time for adding 3h, insulation reaction 1h obtain hydrophilic shell resin；
(4) it is eventually adding triethylamine 2.61g and after stirring 40min, adds into step (3) reaction such as distilled water 148.11g high Speed dispersion 1.2h, filtering and discharging after cooling, obtain it is aqueous from delustring hydroxy acrylic acid secondary breakup body, it is obtained aqueous from delustring The performance parameter of hydroxy acrylic acid secondary breakup body is as shown in table 4A.
By table 4A it is found that gained is aqueous meets index from delustring hydroxy acrylic acid secondary breakup body various performance parameters and want Ask: the milky white blueing light of appearance, storage stability are high, admittedly contain, viscosity, hydroxy radical content, pH value, acid value are within the scope of parameter request, ΔTgThere is extinction greater than 50 DEG C.
(5) it accurately weighs aqueous from mat acrylic secondary breakup body 60g, addition 0.12g defoaming agent obtained by step (4) YCK-670,0.22g wetting agent YCK-1540,0.12g levelling agent YCK-1470 and 7.8g deionized water are uniformly mixed, then are weighed 2655 water-based polyurethane curing agent 14.75g of Bayer XP prepares woodcare paint to get two-component is arrived from delustring woodwork coating, and sprays Be applied on woodenware template, room temperature preservation 7d test performance, test paint film property index as shown in table 4B.
By table 4B it is found that obtained aqueous double-component meets finger with paint film performance indexes after paint from delustring woodwork coating Mark requires: dry speed is suitable for that hardness is high, and transparency and adhesive force are good, and impact resistance and patience are high, and glossiness is low, extinction It is good.
Embodiment 5
A kind of preparation of aqueous double-component from delustring woodwork coating, comprising the following steps:
(1) in the four-hole boiling flask equipped with blender, constant pressure funnel, condenser pipe and thermometer, dodecyl is added Sodium sulphate 3.32g and distilled water 55.46g is maintained at 50 DEG C of stirrings；
(2) methyl methacrylate 75g and butyl acrylate 60g, potassium peroxydisulfate 1.85g and methacrylic acid are accurately weighed Hydroxyl ethyl ester 8.31g is uniformly mixed, and is added drop-wise in step (1) reaction vessel and is warming up to 75 DEG C, time for adding 5h, insulation reaction 1.5h obtains hydrophobic stratum nucleare resin；
(3) when solution blue light occurs and has obvious backflow phenomenon, remaining part methyl methyl acrylate is accurately weighed 25g, butyl acrylate 20g and methacrylic acid 4.86g are uniformly mixed, and are added drop-wise in step (2) reaction vessel and are kept reaction temperature 75 DEG C, time for adding 4h, insulation reaction 2h of degree, obtains hydrophilic shell resin；
(4) N is eventually adding to add after stirring 30min in N- dimethylethanolamine 2.77g to step (3) reaction such as distilled water 168.17g high speed dispersion 1.5h, filtering and discharging after cooling, obtain it is aqueous from delustring hydroxy acrylic acid secondary breakup body, it is obtained The aqueous performance parameter from delustring hydroxy acrylic acid secondary breakup body is as shown in table 5A.
By table 5A it is found that gained is aqueous meets index from delustring hydroxy acrylic acid secondary breakup body various performance parameters and want Ask: the milky white blueing light of appearance, storage stability are high, admittedly contain, viscosity, hydroxy radical content, pH value, acid value are within the scope of parameter request, ΔTgThere is extinction greater than 50 DEG C.
(5) it accurately weighs aqueous from mat acrylic secondary breakup body 60g, addition 0.10g defoaming agent obtained by step (4) YCK-660,0.24g wetting agent YCK-1540,0.11g levelling agent YCK-2490 and 9g deionized water are uniformly mixed, then are weighed and visitd 2655 water-based polyurethane curing agent 14.93g of ear XP prepares woodcare paint to get two-component is arrived from delustring woodwork coating, and sprays In on woodenware template, room temperature preservation 7d test performance, test paint film property index as shown in table 5B.
By table 5B it is found that obtained aqueous double-component meets finger with paint film performance indexes after paint from delustring woodwork coating Mark requires: dry speed is suitable for that hardness is high, and transparency and adhesive force are good, and impact resistance and patience are high, and glossiness is low, extinction It is good.
Above embodiments are only preferred embodiment of the invention, are only that further detailed to technical solution of the present invention work Description, but do not limit the scope of the invention, any change made without departing from spirit of the invention, modification, replacement, Deletion or combination etc. are included in protection scope of the present invention.

Claims (10)

1. a kind of aqueous double-component is from the preparation method of delustring woodwork coating, which comprises the steps of:
(1) emulsifier and distilled water are added in the reaction vessel, insulated and stirred is uniform, then uniformly mixed esters of acrylic acid is added dropwise Monomer, initiator and function monomer heat up and keep the temperature and reacted；
(2) after reaction, when mixed solution blue light occurs and has obvious backflow phenomenon, uniformly mixed third is added dropwise in step (1) Olefin(e) acid esters monomer and hydroxy acids monomer, heat preservation continue to react；
(3) step (2) after reaction, is added neutralizer and stirs evenly, add distilled water and dispersed, cool down, filtering Discharging, obtains aqueous from delustring hydroxy acrylic acid secondary breakup body；
(4) obtain it is aqueous from delustring hydroxy acrylic acid secondary breakup body be added defoaming agent, wetting agent, levelling agent and go from Sub- water is uniformly mixed, then is mixed evenly with water-based polyurethane curing agent, obtains the aqueous double-component and applies from delustring woodenware Material.
2. preparation method according to claim 1, which is characterized in that in step (1), the emulsifier is isomery alcohol polyoxy One kind of vinethene, fatty alcohol polyoxyethylene ether ammonium sulfate and lauryl sodium sulfate, additive amount are acrylic ester monomer The 1% ~ 2% of the gross mass of total addition level and hydroxy acids monomer additive amount；The additive amount of the distilled water is acrylate The 20% ~ 40% of the gross mass of class monomer total addition level and hydroxy acids monomer additive amount；The insulated and stirred be uniformly Insulated and stirred is uniform at 40 ~ 50 DEG C；The used time that uniformly mixed acrylic ester monomer, initiator and function monomer is added dropwise is 4 ~ 5 hours；The heating is to be warming up to 70 ~ 75 DEG C；The time of the reaction is 1 ~ 1.5 hour.
3. preparation method according to claim 1, which is characterized in that in step (1), the acrylic ester monomer is first One kind of base methyl acrylate, butyl methacrylate and butyl acrylate, additive amount account for acrylic ester monomer and always add The 60% ~ 75% of amount.
4. preparation method according to claim 1, which is characterized in that in step (1), the initiator be potassium peroxydisulfate and One kind of ammonium persulfate, additive amount are total matter of acrylic ester monomer total addition level and hydroxy acids monomer additive amount The 0.5% ~ 1.1% of amount；The function monomer is isobornyl methacrylate, glycidyl methacrylate, metering system One of sour hydroxyl ethyl ester and hydroxypropyl acrylate, additive amount are acrylic ester monomer total addition level and hydroxy acids The 2.6% ~ 5.1% of the gross mass of monomer additive amount.
5. preparation method according to claim 1, which is characterized in that in step (2), the acrylic ester monomer is first One kind of base methyl acrylate, butyl methacrylate and butyl acrylate；The hydroxy acids monomer be acrylic acid and One of methacrylic acid, additive amount are 1.2wt% ~ 2.9wt% of acrylic ester monomer total addition level；It is equal that mixing is added dropwise Even acrylic ester monomer and 3 ~ 4 hours acids monomer used times of hydroxy；It is 70 ~ 75 that the heat preservation, which continues reaction, DEG C heat preservation the reaction was continued 1 ~ 2 hour.
6. preparation method according to claim 1, which is characterized in that in step (3), the neutralizer be triethylamine and N, One of N- dimethylethanolamine, additive amount are that acrylic ester monomer total addition level and hydroxy acids monomer add The 0.9% ~ 1.5% of the gross mass of amount；The distilled water adds with acrylic ester monomer total addition level and hydroxy acids monomer The mass ratio of the gross mass of dosage is 0.8 ~ 0.9:1.
7. preparation method according to claim 1, which is characterized in that described aqueous from delustring hydroxy in step (3) The solid content 47 ± 1.0% of sour secondary breakup body, hydroxy radical content 4.0 ± 0.2%, viscosity 1200-2500 mPa s(25 DEG C), pH value 6.5-9, acid value≤20, Δ Tg50 DEG C of >.
8. preparation method according to claim 1, which is characterized in that in step (4), the defoaming agent is that the trade mark is YCK- One of the defoaming agent of 660 and YCK-670, additive amount are aqueous from delustring hydroxy acrylic acid secondary breakup weight 0.15%~0.2%；The wetting agent is the wetting agent that the trade mark is YCK-1540, and additive amount is aqueous from delustring hydroxy acrylic acid The 0.3% ~ 0.4% of secondary breakup weight；The levelling agent be the trade mark be YCK-2490 and the levelling agent of YCK-1470 in one Kind, additive amount is aqueous from the 0.15% ~ 0.25% of delustring hydroxy acrylic acid secondary breakup weight.
9. preparation method according to claim 1, which is characterized in that in step (4), the additive amount of the deionized water is It is aqueous from the 11% ~ 15% of delustring hydroxy acrylic acid secondary breakup weight；The water-based polyurethane curing agent is that the trade mark is XP 2655 water-based polyurethane curing agent, additive amount are added according to-NCO/-OH molar ratio 1.4.
10. by the aqueous double-component of claim 1 ~ 9 described in any item preparation methods preparation from delustring woodwork coating.
CN201810715265.8A 2018-06-29 2018-06-29 A kind of aqueous double-component is from delustring woodwork coating and preparation method thereof Pending CN108948994A (en)

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CN109912766A (en) * 2019-03-04 2019-06-21 江西省龙海化工有限公司 It is a kind of aqueous from ester modified polyurethane resin of mat acrylic and preparation method thereof
CN110903436A (en) * 2019-12-04 2020-03-24 东胜化学(上海)有限公司 Solution containing self-extinction acrylic polymer particles and preparation method thereof
CN110964152A (en) * 2019-11-13 2020-04-07 广州化工研究设计院有限公司 Quick-drying core-shell structure hydroxyl acrylic emulsion and preparation method and application thereof
WO2020125714A1 (en) * 2018-12-21 2020-06-25 广东华润涂料有限公司 Two-component aqueous polyurethane coating composition and low-gloss coating formed thereby
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CN114195948A (en) * 2021-11-25 2022-03-18 上海展辰涂料有限公司 Acrylic acid aqueous dispersion for anti-collapse woodware and preparation method thereof

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WO2020125714A1 (en) * 2018-12-21 2020-06-25 广东华润涂料有限公司 Two-component aqueous polyurethane coating composition and low-gloss coating formed thereby
CN109912766A (en) * 2019-03-04 2019-06-21 江西省龙海化工有限公司 It is a kind of aqueous from ester modified polyurethane resin of mat acrylic and preparation method thereof
CN109912766B (en) * 2019-03-04 2021-08-10 江西省龙海化工有限公司 Waterborne self-extinction acrylic ester modified polyurethane resin and preparation method thereof
CN110964152A (en) * 2019-11-13 2020-04-07 广州化工研究设计院有限公司 Quick-drying core-shell structure hydroxyl acrylic emulsion and preparation method and application thereof
CN110903436A (en) * 2019-12-04 2020-03-24 东胜化学(上海)有限公司 Solution containing self-extinction acrylic polymer particles and preparation method thereof
CN113372778A (en) * 2020-03-09 2021-09-10 上海沪正实业有限公司 Preparation method of high-matte wood floor coating and nano-silica modified high-matte resin prepolymer
CN113136135A (en) * 2021-04-16 2021-07-20 广东金涂宝新材料股份有限公司 Double-component polyurethane self-extinction velvet-feel finish coating and preparation method thereof
CN114195948A (en) * 2021-11-25 2022-03-18 上海展辰涂料有限公司 Acrylic acid aqueous dispersion for anti-collapse woodware and preparation method thereof
CN114195948B (en) * 2021-11-25 2024-04-05 上海展辰涂料有限公司 Acrylic acid aqueous dispersion for collapse-preventing wood device and preparation method thereof

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