CN104497768B - The preparation method of anti-flammability and water proofing property acrylic resin coating - Google Patents

The preparation method of anti-flammability and water proofing property acrylic resin coating Download PDF

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CN104497768B
CN104497768B CN201410760259.6A CN201410760259A CN104497768B CN 104497768 B CN104497768 B CN 104497768B CN 201410760259 A CN201410760259 A CN 201410760259A CN 104497768 B CN104497768 B CN 104497768B
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water
add
monomer
flammability
reaction
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CN104497768A (en
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左广玲
叶红勇
曹英寒
李入林
薛刚
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NANTONG PUTHON CHEMICAL Co.,Ltd.
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Nanyang Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D133/00Coating compositions based on homopolymers or 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04Homopolymers or copolymers of esters
    • C09D133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09D133/08Homopolymers or copolymers of acrylic acid esters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/63Additives non-macromolecular organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00Adhesives based on homopolymers or 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04Homopolymers or copolymers of esters
    • C09J133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/08Homopolymers or copolymers of acrylic acid esters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate

Abstract

The present invention relates to anti-flammability and the preparation method of water proofing property acrylic resin coating and adhesive, water, dodecylbenzene sodium sulfonate and fatty alcohol-polyoxyethylene ether is added in reaction vessel, heat up stirring, add A monomer, emulsifying is warmed up to 70 DEG C and starts logical recirculation water, dropping initiator, stirring reaction, obtain stratum nucleare emulsion;It is simultaneously added dropwise B monomer and initiator in gained stratum nucleare emulsion, stirring reaction, cooling, add dodecylbenzene sodium sulfonate and fatty alcohol-polyoxyethylene ether, 70 DEG C of reaction 1h, add ammonia and adjust pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating and adhesive, this preparation method both can make acrylic resin anti-flammability and water proofing property be greatly improved, and can improve again the defect of acrylic resin emulsion film forming jaundice.

Description

The preparation method of anti-flammability and water proofing property acrylic resin coating
Technical field
The preparation method that the present invention relates to anti-flammability and preventing water coating, particularly to the preparation method of anti-flammability and water proofing property acrylic resin coating.
Background technology
Being sprayed at external and internal wall, furniture, the coating on ironware surface and paint, all the time all directly or indirectly contacting with the mankind, poisonous, harmful coating also moment threatens the health of people.Field owing to using often contacts sunlight, and owing to containing a large amount of ultraviolet lights that colored objects is harmful, its wavelength about 290~460nm in sunray, these harmful ultraviolet lights, by redox chemically, make the change of coating generation color.
The maximum market of acrylic resin coating is car paint, this external light industry, household electrical appliance, metal household implements, aluminum products, coiled material industry, instrument and meter, build, textile, plastic, woodwork, the industry such as papermaking are all widely used.The direction of acrylic resin coating hydrotropismization, multifunction and high function is developed.
Glued joint (bonding, bonding, cementing, gluing) and refer to that homogeneity or heterogeneous body surface stick with glue the technology that agent links together, there is stress distribution continuous, lightweight, or seal, the features such as most technological temperatures are low.Glued joint the connection being particularly well-suited to unlike material, different-thickness, ultra-thin specification and complex component.Glueing joint RECENT DEVELOPMENTS the fastest, application industry is extremely wide, and high-and-new science and technology progress and the improvement of people's daily life are had significant impact.Therefore, study, develop and produce all kinds of adhesive particularly significant.
But acrylic resin institute film forming plasticity is high, and fire-resistant, abrasion resisting poor performance, emulsion film forming somewhat do not turn to be yellow to cause it, it is therefore desirable to it is modified, the safety of protection lives and properties.
Summary of the invention
It is desirable to provide the preparation method of anti-flammability and water proofing property acrylic resin coating, with 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether, trifluoro vinyl phenylate, 1, 1, 2, 3, 3, 3-hexafluoro-1-propylene, 2, 2, 2-trifluoroethyl vinyl ether, Bei get Luo star makes acrylic resin not only have anti-flammability but also have water proofing property, and 2-chloro benzothiazole, cyprodinil, 3-amino quinine, oxygen cyclammonium phosphorus, cyclammonium sulphur is grand, Aminobutyric Acid makes the temperature that fluorine-containing material discharges reach the temperature that fire retardant is conventional, with apigenin, R-3-amino quinine ring dihydrochloride, 3-propyl group bicyclo-[2.2.1]-5-in heptan alkene-2-carboxylic aldehyde improves the defect of persulfate initiator emulsion film jaundice.
The present invention is by the following technical solutions:
1. the preparation method of anti-flammability and water proofing property acrylic resin coating, it is characterised in that:
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, water 75g, dodecylbenzene sodium sulfonate 1.5g, fatty alcohol-polyoxyethylene ether 0.5g and methacrylic acid 3.0g are added, it is warming up to 40 DEG C, stirring 30min, add A monomer, emulsifying 60min, it is warmed up to 70 DEG C and starts logical recirculation water, it is warmed up to 80 DEG C, the water-soluble ammonium persulfate solution 8.6g of dropping 8g, time for adding 2h, drips reaction 2h, adds 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether 3g, 2-chloro benzothiazole 0.15g, stirring reaction 2h, obtains stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 8g, methyl methacrylate 6g, ethyl acrylate 4g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble potassium monopersulfate solutions 8.7g of 8g, time for adding 2h, drip 80 DEG C of stirring reaction 2h, add apigenin 1.2g, 85 DEG C of response time 3h, cool to 50 DEG C, add dodecylbenzene sodium sulfonate 0.375g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add trifluoro vinyl phenylate 0.3g and cyprodinil 0.12g, 70 DEG C of reaction 1h, add ammonia and adjust pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating;
Described B monomer is made up of: butyl acrylate 4g, methyl methacrylate 3.0g, 2-(Acryloyloxy)ethanol 5.2g and styrene 0.7g mixing.
The preparation method of anti-flammability and water proofing property acrylic resin coating, it is characterised in that:
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, water 60g, dodecylbenzene sodium sulfonate 0.65g, fatty alcohol-polyoxyethylene ether 0.15g and acrylic acid 0.2g are added, it is warming up to 50 DEG C, stirring 40min, add A monomer, emulsifying 30min, it is warmed up to 70 DEG C and starts logical recirculation water, it is warmed up to 80 DEG C, the water-soluble potassium persulfate solution 7.2g of dropping 7g, time for adding 1h, drips reaction 1h, adds 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether 0.45g and 3-amino quinine 0.13g, stirring reaction 3h, obtains stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 3g, methyl methacrylate 2g, ethyl acrylate 2.0g and ethyl acrylate 3.5g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble potassium persulfate solution 9.2g of 9g, time for adding 0.5h, drip 80 DEG C of stirring reaction 2h, add R-3-amino quinine ring dihydrochloride 0.4g, 75 DEG C of reaction 1h, cool to 40 DEG C, add dodecylbenzene sodium sulfonate 0.25g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add 1,1,2,3,3,3-hexafluoro-1-propylene 0.01g and oxygen cyclammonium phosphorus 0.1g, 70 DEG C of reaction 1h, adding ammonia adjusts pH value to 7 ~ 8, obtains described anti-flammability and preventing water coating;
Described B monomer is made up of: butyl acrylate 3g, methyl methacrylate 4.0g, 2-(Acryloyloxy)ethanol 5.0g and styrene 0.5g mixing.
The preparation method of anti-flammability and water proofing property acrylic resin coating, it is characterised in that:
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, add water 75g, DBSA 2.5g, fatty alcohol-polyoxyethylene ether 1.5g and acrylic acid 3.0g, be warming up to 40 DEG C, stir 30min, add A monomer, emulsifying 60min, is warmed up to 70 DEG C and starts logical recirculation water, be warmed up to 80 DEG C, the water-soluble ammonium persulfate solution 9.6g of dropping 9g, time for adding 1h, drips reaction 2h, adds Bei get Luo star 3g and the grand 0.11g of cyclammonium sulphur, stirring reaction 2h, obtains stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 8g, methyl methacrylate 6g, ethyl acrylate 4g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble ammonium persulfate solution 8.7g of 8g, time for adding 2h, drip 80 DEG C of stirring reaction 2h, add 3-propyl group bicyclo-[2.2.1]-5-in heptan alkene-2-carboxylic aldehyde 0.35g, 85 DEG C of response time 3h, cool to 50 DEG C, add dodecylbenzene sodium sulfonate 0.375g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add 2, 2, 2-trifluoroethyl vinyl ether 0.3g and Aminobutyric Acid 0.13g, 70 DEG C of reaction 1h, adding ammonia adjusts pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating;
Described B monomer by: butyl acrylate 5g, methyl methacrylate 5.5g, 2-(Acryloyloxy)ethanol 6.5g, styrene 1.5g mixing form.
The beneficial effects of the present invention is:
(1) 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether, trifluoro vinyl phenylate, 1,1,2,3,3,3-hexafluoro-1-propylene, 2,2,2-trifluoroethyl vinyl ether, Bei get Luo star not only have anti-flammability but also have water proofing property;
(2) 2-chloro benzothiazole, cyprodinil, 3-amino quinine, oxygen cyclammonium phosphorus, cyclammonium sulphur is grand, Aminobutyric Acid improves the temperature making fluorine-containing material discharge and reaches the temperature of fire retardant routine;
(3) apigenin, R-3-amino quinine ring dihydrochloride, 3-propyl group bicyclo-[2.2.1]-5-in heptan alkene-2-carboxylic aldehyde improve the defect of the jaundice of the acrylic resin film that persulfate initiator causes;
(4) under stratum nucleare and shell combined effect, the fire-retardant of acrylic resin and water proofing property are improved.
Detailed description of the invention
In order to be more fully understood that and implement the present invention, further illustrate the present invention below in conjunction with specific embodiment.
Example 1
(1) to agitator, the 250mL there-necked flask of thermometer and condensing tube adds water 75g, dodecylbenzene sodium sulfonate 1.5g, fatty alcohol-polyoxyethylene ether 0.5g and methacrylic acid 3.0g, it is warming up to 40 DEG C, stirring 30min, add A monomer, emulsifying 60min, it is warmed up to 70 DEG C and starts logical recirculation water, it is warmed up to 80 DEG C, the water-soluble ammonium persulfate solution 8.6g of dropping 8g, time for adding 2h, drip reaction 2h, add 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether 3g, 2-chloro benzothiazole 0.15g, drip stirring reaction 2h, obtain stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 8g, methyl methacrylate 6g, ethyl acrylate 4g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble potassium monopersulfate solutions 8.7g of 8g, time for adding 2h, drip 80 DEG C of stirring reaction 2h, add apigenin 1.2g, 85 DEG C of response time 3h, cool to 50 DEG C, add dodecylbenzene sodium sulfonate 0.375g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add trifluoro vinyl phenylate 0.3g and cyprodinil 0.12g, 70 DEG C of reaction 1h, add ammonia and adjust pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating;
Described B monomer is made up of: butyl acrylate 4g, methyl methacrylate 3.0g, 2-(Acryloyloxy)ethanol 5.2g and styrene 0.7g mixing.
Example 2
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, water 60g, dodecylbenzene sodium sulfonate 0.65g, fatty alcohol-polyoxyethylene ether 0.15g and acrylic acid 0.2g are added, it is warming up to 50 DEG C, stirring 40min, add A monomer, emulsifying 30min, it is warmed up to 70 DEG C and starts logical recirculation water, it is warmed up to 80 DEG C of water-soluble potassium persulfate solution 7.2g of dropping 7g, time for adding 1h, drip reaction 1h, add 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether 0.45g and 3-amino quinine 0.13g, stirring reaction 3h, obtain stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 3g, methyl methacrylate 2g, ethyl acrylate 2.0g and ethyl acrylate 3.5g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble potassium persulfate solution 9.2g of 9g, time for adding 0.5h, drip 80 DEG C of stirring reaction 2h, add R-3-amino quinine ring dihydrochloride 0.4g, 75 DEG C of reaction 1h, cool to 40 DEG C, add dodecylbenzene sodium sulfonate 0.25g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add 1,1,2,3,3,3-hexafluoro-1-propylene 0.01g and oxygen cyclammonium phosphorus 0.1g, 70 DEG C of reaction 1h, adding ammonia adjusts pH value to 7 ~ 8, obtains described anti-flammability and preventing water coating;
Described B monomer is made up of: butyl acrylate 3g, methyl methacrylate 4.0g, 2-(Acryloyloxy)ethanol 5.0g and styrene 0.5g mixing.
Example 3
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, add water 75g, DBSA 2.5g, fatty alcohol-polyoxyethylene ether 1.5g and acrylic acid 3.0g, be warming up to 40 DEG C, stir 30min, add A monomer, emulsifying 60min, is warmed up to 70 DEG C and starts logical recirculation water, be warmed up to 80 DEG C, the water-soluble ammonium persulfate solution 9.6g of dropping 9g, time for adding 1h, drips reaction 2h, adds Bei get Luo star 3g and the grand 0.11g of cyclammonium sulphur, stirring reaction 2h, obtains stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 8g, methyl methacrylate 6g, ethyl acrylate 4g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble ammonium persulfate solution 8.7g of 8g, time for adding 2h, drip 80 DEG C of stirring reaction 2h, add 3-propyl group bicyclo-[2.2.1]-5-in heptan alkene-2-carboxylic aldehyde 0.35g, 85 DEG C of response time 3h, cool to 50 DEG C, add dodecylbenzene sodium sulfonate 0.375g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add 2, 2, 2-trifluoroethyl vinyl ether 0.3g and Aminobutyric Acid 0.13g, 70 DEG C of reaction 1h, adding ammonia adjusts pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating;
Described B monomer is made up of: butyl acrylate 5g, methyl methacrylate 5.5g, 2-(Acryloyloxy)ethanol 6.5g and styrene 1.5g mixing.
Example 4
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, water 75g, dodecylbenzene sodium sulfonate 1.5g, fatty alcohol-polyoxyethylene ether 0.5g and methacrylic acid 3.0g are added, it is warming up to 40 DEG C, stirring 30min, add A monomer, emulsifying 60min, it is warmed up to 70 DEG C and starts logical recirculation water, it is warmed up to 80 DEG C, the water-soluble ammonium persulfate solution 8.6g of dropping 8g, time for adding 2h, drips reaction 2h, adds 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether 3g, 2-chloro benzothiazole 0.15g, stirring reaction 2h, obtains stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 8g, methyl methacrylate 6g, ethyl acrylate 4g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble potassium monopersulfate solutions 8.7g of 8g, time for adding 2h, drip 80 DEG C of stirring reaction 2h, add apigenin 1.2g and 3-hydroxy-n, N-diethylaniline 1.6g, 85 DEG C of response time 3h, cool to 50 DEG C, add dodecylbenzene sodium sulfonate 0.375g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, adds trifluoro vinyl phenylate 0.3g and cyprodinil 0.12g, 70 DEG C of reaction 1h, adding ammonia adjusts pH value to 7 ~ 8, obtains described anti-flammability and preventing water coating;
Described B monomer is made up of: butyl acrylate 3g, methyl methacrylate 3.0g, 2-(Acryloyloxy)ethanol 5.2g and styrene 0.7g mixing.
Example 5
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, water 60g, dodecylbenzene sodium sulfonate 0.65g, fatty alcohol-polyoxyethylene ether 0.15g, acrylic acid 0.2g are added, it is warming up to 50 DEG C, stirring 40min, add A monomer, emulsifying 30min, it is warmed up to 70 DEG C and starts logical recirculation water, it is warmed up to 80 DEG C of water-soluble potassium persulfate solution 7.2g of dropping 7g, time for adding 1h, drip reaction 1h, add 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether 0.45g and 3-amino quinine 0.13g, stirring reaction 3h, obtain stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 3g, methyl methacrylate 2g, ethyl acrylate 2.0g and ethyl acrylate 3.5g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble potassium persulfate solution 9.2g of 9g, time for adding 0.5h, drip 80 DEG C of stirring reaction 2h, add R-3-amino quinine ring dihydrochloride 0.4g and 5-amino isophthalic acid dimethyl ester 1.2g, 75 DEG C of reaction 1h, cool to 40 DEG C, add dodecylbenzene sodium sulfonate 0.25g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add 1, 1, 2, 3, 3, 3-hexafluoro-1-propylene 0.01g and oxygen cyclammonium phosphorus 0.1g, 70 DEG C of reaction 1h, adding ammonia adjusts pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating;
Described B monomer is made up of: butyl acrylate 3g, methyl methacrylate 4.0g, 2-(Acryloyloxy)ethanol 5.0g and styrene 0.5g mixing.
Example 6
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, add water 75g, DBSA 2.5g, fatty alcohol-polyoxyethylene ether 1.5g and acrylic acid 3.0g, be warming up to 40 DEG C, stir 30min, add A monomer, emulsifying 60min, is warmed up to 70 DEG C and starts logical recirculation water, be warmed up to 80 DEG C, the water-soluble ammonium persulfate solution 9.6g of dropping 9g, time for adding 1h, drips reaction 2h, adds Bei get Luo star 3g and the grand 0.11g of cyclammonium sulphur, stirring reaction 2h, obtains stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 8g, methyl methacrylate 6g, ethyl acrylate 4g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble ammonium persulfate solution 8.7g of 8g, time for adding 2h, drip 80 DEG C of stirring reaction 2h, add 3-propyl group bicyclo-[2.2.1]-5-in heptan alkene-2-carboxylic aldehyde 0.35g and chlorpromazine 0.4g, 85 DEG C of response time 3h, cool to 50 DEG C, add dodecylbenzene sodium sulfonate 0.375g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add 2, 2, 2-trifluoroethyl vinyl ether 0.3g and Aminobutyric Acid 0.13g, 70 DEG C of reaction 1h, adding ammonia adjusts pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating;
Described B monomer by: butyl acrylate 5g, methyl methacrylate 5.5g, 2-(Acryloyloxy)ethanol 6.5g, styrene 1.5g mixing form.
Example 7
(1) to agitator, the 250mL there-necked flask of thermometer and condensing tube adds water 75g, dodecylbenzene sodium sulfonate 1.5g, fatty alcohol-polyoxyethylene ether 0.5g and methacrylic acid 3.0g, it is warming up to 40 DEG C, stirring 30min, add A monomer, emulsifying 60min, it is warmed up to 70 DEG C and starts logical recirculation water, it is warmed up to 80 DEG C, the water-soluble ammonium persulfate solution 8.6g of dropping 8g, time for adding 2h, drip reaction 2h, add 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether 3g, 2-chloro benzothiazole 0.15g, drip stirring reaction 2h, obtain stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 8g, methyl methacrylate 6g, ethyl acrylate 4g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble potassium monopersulfate solutions 8.7g of 8g, time for adding 2h, drip 80 DEG C of stirring reaction 2h, add apigenin 1.2g and carbachol 0.21g, 85 DEG C of response time 3h, cool to 50 DEG C, add dodecylbenzene sodium sulfonate 0.375g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add trifluoro vinyl phenylate 0.3g, cyprodinil 0.12g and 2-(3, 4-dihydroxy phenyl) ethamine 0.54g, 70 DEG C of reaction 1h, adding ammonia adjusts pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating;
Described B monomer by: butyl acrylate 4.6g, methyl methacrylate 3.0g, 2-(Acryloyloxy)ethanol 5.2g, styrene 0.7g mixing form.
Example 8
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, water 60g, dodecylbenzene sodium sulfonate 0.65g, fatty alcohol-polyoxyethylene ether 0.15g, acrylic acid 0.2g are added, it is warming up to 50 DEG C, stirring 40min, add A monomer, emulsifying 30min, it is warmed up to 70 DEG C and starts logical recirculation water, it is warmed up to 80 DEG C of water-soluble potassium persulfate solution 7.2g of dropping 7g, time for adding 1h, drip reaction 1h, add 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether 0.45g and 3-amino quinine 0.13g, stirring reaction 3h, obtain stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 3g, methyl methacrylate 2g, ethyl acrylate 2.0g and ethyl acrylate 3.5g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble potassium persulfate solution 9.2g of 9g, time for adding 0.5h, drip 80 DEG C of stirring reaction 2h, add R-3-amino quinine ring dihydrochloride 0.4g and penicillamine 0.13g, 75 DEG C of reaction 1h, cool to 40 DEG C, add dodecylbenzene sodium sulfonate 0.25g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add 1, 1, 2, 3, 3, 3-hexafluoro-1-propylene 0.01g, oxygen cyclammonium phosphorus 0.1g and 2, 3, 4, 5, 6-penta hydroxy group-2-hexenoic acid-4-lactone 0.14g, 70 DEG C of reaction 1h, adding ammonia adjusts pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating;
Described B monomer by: butyl acrylate 3g, methyl methacrylate 4.0g, 2-(Acryloyloxy)ethanol 5.0g, styrene 0.5g mixing form.
Beneficial effects of the present invention is further illustrated below by relevant experimental data:
Water proofing property adopts and takes appropriate emulsion and be evenly applied on glass plate, is put into by glass plate in deionized water and soak under uniform temperature after drying and forming-film, observes film and becomes blue, turns white, bubbles, sends out the situation wrinkled, come off.
Table 1 anti-flammability and water proofing property acrylic resin coating institute filming performance
Experimental group Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8
Film outward appearance (resistance to water 48h) Transparent Transparent Transparent Transparent Transparent Transparent Transparent Transparent
Hardness B B B B B B B B
Adhesive force/level 2 2 2 3 2 2 2 3
Pliability/mm 2 2 2 2 2 2 2 2
As can be found from Table 1, from film outward appearance, hardness, adhesive force, flexibility better performances.
Anti-flammability is to be weighed by smoke density method (maximum smoke density, reach the maximum smoke density time), oxygen index (OI), vertical combustion index (flaming combustion time, glowing time), and elongation at break characterizes its mechanical property.
The anti-flammability of table 2 anti-flammability and water proofing property acrylic resin coating gained film
Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8
Maximum smoke density 12 11 13 15 13 14 17 21
Reach maximum smoke density time/s 165 165 180 215 175 185 185 225
Oxygen index (OI) 24.5 24.7 24.8 24.8 26.5 26.7 26.8 26.8
Flaming combustion time/s 32.4 31.4 32.3 32.8 32.4 31.6 32.5 31.9
Glowing time/s 0 0 0 0 0 0 0 0
The detection of table 2 indices is respectively according to following standard: smoke density measures according to GB8323-2008, and oxygen index (OI) adopts GB/T5454-1997 " textile combustion performance test-oxygen index method " to measure;Flaming combustion time and glowing time are to be measured by GB/T5455-1997 " textile combustion energy test-normal beam technique ".
As shown in Table 2, when anti-flammability of the present invention and the burning of water proofing property acrylic resin coating gained film, maximum smoke density significantly reduces, and reaches the maximum smoke density time and significantly extends, and oxygen index (OI) significantly improves, and burning time substantially shortens.
Table 3 anti-flammability and water proofing property acrylic resin coating gained film elongation at break and outward appearance
Experimental group Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8
Elongation at break/% 139.77 122.53 116.69 167.38 199.25 126.69 177.38 199.25
Film outward appearance Water white transparency Water white transparency Water white transparency Water white transparency Water white transparency Water white transparency Water white transparency Water white transparency
Table 3 middle finger object detection method reference: Jiang Weiqi. leather finish physical and chemical inspection [M]. China Light Industry Press, 1999,82-96.Employ lightfast coating material film of the present invention, elongation at break be improved significantly.
Table 4 anti-flammability and water proofing property acrylic resin coating gained film abrasion performance
Experimental group Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8
Abrasion loss/mg 27 25 20 18 18 22 13 7
Note: use 120# sand round
The data of table 4 are to carry out under GB1768-89 paint film abrasion performance assay method, and wear-resisting those at least is best, and the abrasivity of example is all better.

Claims (2)

1. the preparation method of anti-flammability and water proofing property acrylic resin coating, it is characterised in that:
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, water 75g, dodecylbenzene sodium sulfonate 1.5g, fatty alcohol-polyoxyethylene ether 0.5g and methacrylic acid 3.0g are added, it is warming up to 40 DEG C, stirring 30min, add A monomer, emulsifying 60min, it is warmed up to 70 DEG C and starts logical recirculation water, it is warmed up to 80 DEG C, the water-soluble ammonium persulfate solution 8.6g of dropping 8g, time for adding 2h, drips reaction 2h, adds 2-perfluor propoxyl group perfluoro propyl trifluoro vinyl ether 3g, 2-chloro benzothiazole 0.15g, stirring reaction 2h, obtains stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 8g, methyl methacrylate 6g, ethyl acrylate 4g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble potassium monopersulfate solutions 8.7g of 8g, time for adding 2h, drip 80 DEG C of stirring reaction 2h, add apigenin 1.2g, 85 DEG C of response time 3h, cool to 50 DEG C, add dodecylbenzene sodium sulfonate 0.375g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add trifluoro vinyl phenylate 0.3g and cyprodinil 0.12g, 70 DEG C of reaction 1h, add ammonia and adjust pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating;
Described B monomer is made up of: butyl acrylate 4g, methyl methacrylate 3.0g, 2-(Acryloyloxy)ethanol 5.2g and styrene 0.7g mixing.
2. the preparation method of anti-flammability and water proofing property acrylic resin coating, it is characterised in that:
(1) in the 250mL there-necked flask with agitator, thermometer and condensing tube, add water 75g, DBSA 2.5g, fatty alcohol-polyoxyethylene ether 1.5g and acrylic acid 3.0g, be warming up to 40 DEG C, stir 30min, add A monomer, emulsifying 60min, is warmed up to 70 DEG C and starts logical recirculation water, be warmed up to 80 DEG C, the water-soluble ammonium persulfate solution 9.6g of dropping 9g, time for adding 1h, drips reaction 2h, adds Bei get Luo star 3g and the grand 0.11g of cyclammonium sulphur, stirring reaction 2h, obtains stratum nucleare emulsion;
Described A monomer be by: butyl acrylate 8g, methyl methacrylate 6g, ethyl acrylate 4g mix;
(2) in step (1) gained stratum nucleare emulsion, B monomer it is simultaneously added dropwise and with the water-soluble ammonium persulfate solution 8.7g of 8g, time for adding 2h, drip insulation 80 DEG C, stirring reaction 2h, add 3-propyl group bicyclo-[2.2.1]-5-in heptan alkene-2-carboxylic aldehyde 0.35g, 85 DEG C of response time 3h, cool to 50 DEG C, add dodecylbenzene sodium sulfonate 0.375g and fatty alcohol-polyoxyethylene ether 0.125g, response time 60min, add 2, 2, 2-trifluoroethyl vinyl ether 0.3g and Aminobutyric Acid 0.13g, 70 DEG C of reaction 1h, adding ammonia adjusts pH value to 7 ~ 8, obtain described anti-flammability and preventing water coating;
Described B monomer by: butyl acrylate 5g, methyl methacrylate 5.5g, 2-(Acryloyloxy)ethanol 6.5g, styrene 1.5g mixing form.
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CN105176290A (en) * 2015-10-29 2015-12-23 南阳理工学院 Method for preparing antibacterial acrylate resin coating
CN105153355A (en) * 2015-10-29 2015-12-16 南阳理工学院 Preparation method of acrylic resin coating with antibacterial property and light resistance for building
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