CN108912929A - Fire-retardant, the aqueous nucleocapsid acrylic resin coating of antibiotic property and paint preparation method - Google Patents

Fire-retardant, the aqueous nucleocapsid acrylic resin coating of antibiotic property and paint preparation method Download PDF

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CN108912929A
CN108912929A CN201810665076.4A CN201810665076A CN108912929A CN 108912929 A CN108912929 A CN 108912929A CN 201810665076 A CN201810665076 A CN 201810665076A CN 108912929 A CN108912929 A CN 108912929A
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retardant
fire
added
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CN108912929B (en
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段小宁
何宏昌
赵玉真
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Liuzhou Andao Technology Co.,Ltd.
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段小宁
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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
    • C09D151/00Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
    • C09D151/003Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
    • 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
    • C08F265/00Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
    • C08F265/04Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
    • 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
    • C09D5/14Paints containing biocides, e.g. fungicides, insecticides or pesticides
    • 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
    • C09D5/185Intumescent paints

Abstract

The invention discloses the preparation methods of fire-retardant antibiotic property aqueous core shell acrylic esters resin coating and paint, 40 ~ 75 parts of water, 0.6 ~ 2.4 part of emulsifier, 1.6 ~ 3.0 parts of methacrylic acid are added into reaction vessel, it is warming up to 60 DEG C, stir 40min, A monomer is added, emulsification times are 30 ~ 40min;It is warming up to 70 DEG C and starts logical recirculation water, keep the temperature, be added dropwise 0.4 ~ 0.6 parts by weight of initiator A (with 5 parts by weight aqueous solvents), time for adding continues 1 ~ 2h, reacts 2h after dripping, and obtains stratum nucleare lotion after being warming up to 80 DEG C;B monomer is added dropwise simultaneously into gained stratum nucleare lotion, 3.6 parts by weight of initiator A and fire retardant of 0.3 ~ 0.6 parts by weight, time for adding continues 1 ~ 2h, it is kept the temperature after dripping and 0.4 parts by weight of antibacterial agent is added at 75 ~ 85 DEG C, it is stirred to react 2h, add 0.8 ~ 1.0 parts by weight of crosslinking agent, keep the temperature 75 ~ 85 DEG C of 1 ~ 2h of reaction time, cool to 50 DEG C, 0.4 parts by weight of emulsifier are added, reaction time 40min, add ammonium hydroxide tune pH value to 7 ~ 8, it is fire-retardant described in obtaining, antibiotic property aqueous core shell acrylic esters resin coating and paint, the material can be used for coating for internal and external wall, metallic finishes and anti-corrosion, make the paint of timber and its as leather finishing agent.

Description

Fire-retardant, the aqueous nucleocapsid acrylic resin coating of antibiotic property and paint preparation method
Technical field
It is especially fire-retardant, antibiotic property is aqueous the present invention relates to the preparation method of aqueous core shell acrylic esters resin The preparation method of hud typed acrylic resin coating and paint.
Background technique
Coating is to be applied to body surface to be formed with protection, decoration or property (such as insulation, anti-corrosion, mark) Solid coated film a kind of liquid or solid material general name, including oily (property) paint, water paint, powdery paints.Paint is flowable Liquid coating, including oily (property) paint and water paint.Paint is using organic solvent as medium or high solid, solvent-free oiliness Paint.Water paint is water-soluble or water-dispersible coating.Main material one of of the coating as house decoration, in decorations The large percentage accounted for, whether or not the purchased paint is qualified directly influence the environment in overall decoration effect and room, sometimes even meeting Greatly harm is generated to the health of human body.
World's coating variety structure develops towards the directions such as VOC are reduced, and water paint is wherein one of developing direction.China Traditional solvent based coating specific gravity is gradually reduced, and also quickly, but polyvinyl alcohol low grade kind is still for the development speed of water paint Account for larger specific gravity.Improving the quality of water paint, developing new kind is to consolidate and develop the important link of water paint.Emphasis Researching and developing should be with vinyl acetate-acrylate copolymer emulsion, Styrene And Chloroalkyl Acrylates copolymer emulsion and pure acrylic acid series Based on the latex paint of base-material, and strive for durability, paint film flatness, richness, application property, in terms of dashed forward It is broken, especially pay attention to aqueous research.
Acrylic resin has many advantages, such as compared with other materials, such as:Excellent adhesive force, film is tough and tensile, smooth, It is fast light, ageing-resistant simultaneously, water-resistance is stronger than casein, easy to use, but it also has the shortcomings that very important, i.e., heat sticks cold short, Limit it by weather to a certain extent in the use of leather surface.Since 1987, the Rohm and in the U.S. Hass company develops a large amount of new product in succession, wherein second generation acrylic resin, in terms of overcoming heat to stick cold short disadvantage There is breakthrough progress.Subsequent China is also successively achieving certain achievement to the research in terms of acryhic material modification.Mesh Preceding method of modifying is mostly to introduce functional monomer and acrylic molecules into system to be grafted or multi-component copolymer, using nucleocapsid Structure, or the method being blended are modified.
201711478310.4 the invention discloses a kind of antibiotic property acrylic resins, by the raw material of following mass fraction It is prepared:16-25 parts of silester, 35-42 parts of vinyltriethoxysilane, 2-6 parts of acetic acid, acrylics monomer 60-70 parts, 2-4 parts of initiator, 3-6 parts of n-butanol, 10-50 parts of acryloxyethyldimethyl ethyl phosphonium bromide ammonium.Of the invention Antibiotic property acrylic resin antibacterial effect is more significant, health environment-friendly, and performance reaches conventional criteria, and synthetic method is simple, easy to operate, It is at low cost to be suitable for promoting.
201610331925.3 fire-retardant, antibacterials, waterproof graphene modified acroleic acid esters resin preparation method for coating, will It is eluted with water after green peel of walnut removing, is placed in baking oven that drying to constant weight at a temperature of 40 ~ 70 DEG C, crushed and simultaneously cross 80 ~ 100 meshes, Green peel of walnut powder is obtained, green peel of walnut powder and water are weighed, allyl trimethyl ammonium chloride, 4- methoxyl group acetoacetate first is added Ester reflowing at a temperature of 80 ~ 100 DEG C filters decoction liquor, is concentrated under reduced pressure at a temperature of 60 ~ 70 DEG C, solution to be concentrated is at water content Stiff paste shape 15% ~ 20% obtains walnut peel extract concentrate to constant weight, and is used in acrylic resin, Gained acrylic resin has antibacterial, fire-retardant and good waterproof performance, and oxygen index (OI) can reach 26.6, and flaming combustion time is 2.2s, glowing time 0, antibiotic property(Golden yellow staphylococcus)Reach 97.
201510723163.7 are related to a kind of preparation method of antibiotic property acrylic resin coating, to stirring Water, neopelex, fatty alcohol polyoxyethylene ether, third are added in the 250ml three-necked flask of device, thermometer and condenser pipe Olefin(e) acid and formic acid are warming up to 45 DEG C, stir 40min, and A monomer is added, and emulsion reaction 90min is warming up to 50 DEG C and starts logical reflux Water is warming up to 60 DEG C, and potassium permanganate 3.6g is added, and reacts 2h, obtains stratum nucleare lotion;Potassium permanganate is added into gained stratum nucleare lotion 3.2g, formic acid 0.7g and B monomer, 60 DEG C are stirred to react 2h, cool to 50 DEG C, and neopelex 0.375g and rouge is added Vitamin C 7.8g, Gallic Acid 3.2g and mountain is added in fat alcohol polyoxyethylene ether 0.125g, reaction time 60min Pears sugar alcohol 0.6g, 60 DEG C of reaction 1h add ammonium hydroxide tune pH value to 7 ~ 8, obtain the antibiotic property acrylic resin coating, have Good antibiotic property, and the defect of acrylic resin emulsion film forming jaundice can be improved, golden yellow staphylococcus can reach 97.
Summary of the invention
Fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint the preparation method of the present invention, it is main Design is to synthesize a kind of fire retardant and antibacterial agent, the fire retardant and antibacterial agent are reacted with acrylic ester monomer, be can be changed fire-retardant Index is not high, the unabiding defect of antibacterial, is particularly synthesized in fire-retardant using dimethylphosphite, catalyst A, acrylamide Mesosome, used catalyst A replace traditional sodium methoxide, make products obtained therefrom without methanol smell, add pentaerythrite, substance A, 4-aminophenol makes have double bond generation in gained system(Be particularly due to substance A as entered), obtained flame-retardant agent have double bond, It reacts, can be integrated on the main chain of acrylic resin, 4-aminophenol is played with acrylic ester monomer subsequent in this way Raising substance A binding ability, while identical thinking synthetic antibacterial agents are also used, gefarnate, vinyl phosphonic acid, 2- is bromo- 2- nitro -1,3- propyl alcohol 1.2g, 2,5- dimethyl -3- hexin -2,5- glycol, ethanedioly chloride, borogen hybrid reaction, make institute Obtaining has double bond and three keys in antibacterial agent system, then reacts with acrylic ester monomer, improves the persistence of antibacterial agent, and passes It based on the antibacterial agent addition type of system, causes antibacterial not lasting, while improving the binding ability of unsaturated bond using borogen.
Fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint preparation method, preparation method are:
(1)40 ~ 75 parts of water, 0.6 ~ 2.4 part of emulsifier, 1.6 ~ 3.0 parts of methacrylic acid are added into reaction vessel, is warming up to 60 DEG C, 40min is stirred, A monomer is added, emulsification times are 30 ~ 40min;It is warming up to 70 DEG C and starts logical recirculation water, be warming up to 80 DEG C After keep the temperature 1h, 0.4 ~ 0.6 parts by weight of initiator A (being dissolved with 5 parts by weight aqueous solvents) is added dropwise, time for adding continues 1 ~ 2h, dropwise addition 2h is reacted after complete, obtains stratum nucleare lotion;
The A monomer be by:3 ~ 5 parts by weight of butyl acrylate, 2 ~ 7 parts by weight of methyl methacrylate, 3 ~ 6 weight of ethyl acrylate Amount part and 1 ~ 7 parts by weight of hydroxy-ethyl acrylate mix;
(2)To step(1)In gained stratum nucleare lotion simultaneously be added dropwise B monomer, 0.3 ~ 0.6 parts by weight initiator A (with 5 parts by weight Aqueous solvent dissolution) and 3.6 parts by weight of fire retardant, time for adding continue 1 ~ 2h, addition antibacterial agent 0.4 at 75 ~ 85 DEG C after dripping Parts by weight are stirred to react 2h, add 0.8 ~ 1.0 parts by weight of crosslinking agent, and 75 ~ 85 DEG C of 1 ~ 2h of reaction time cool to 50 DEG C, add Enter 0.4 parts by weight of emulsifier, reaction time 40min adds ammonium hydroxide tune pH value to 7 ~ 8, obtains fire-retardant, the aqueous nucleocapsid of antibiotic property Type acrylic resin coating and paint;
The B monomer be by:2 ~ 4 parts by weight of butyl acrylate, 2 ~ 8 parts by weight of methyl methacrylate, 3 ~ 7 weight of ethyl acrylate Amount part and 1 ~ 8 parts by weight of hydroxy-ethyl acrylate mix.
Dimethylphosphite 0.5mol is added in three-necked flask, catalyst A0.004mol and 0.5 ~ 0.8mol third is added Acrylamide, agitating paddle, condenser pipe and thermometer in connection, is slowly warming up to 70 ~ 90 DEG C, 2 ~ 5h of insulation reaction obtains light yellow liquid Body is 3-dimethoxy phosphoryl propionamides;Tetrakis hydroxymetyl phosphonium sulfuric is added into resulting 3-dimethoxy phosphoryl propionamide 0.2 ~ 0.6mol, 50 DEG C ~ 90 DEG C of reaction temperature, 2 ~ 3h of reaction time adds pentaerythrite 0.2mol, fills pentaerythrite Divide dissolution, be warming up to 70 ~ 90 DEG C, 2 ~ 3h of reaction time, adds substance A 0.1mol and 4-aminophenol 0.6mol, reaction temperature 70 ~ 90 DEG C, reaction time 2h of degree, cools to obtain fire retardant A.
Its catalyst A be diethyl maleate, dimethyl maleate, diacetyl monoxime, methyl benzilate it is any It is a kind of.
Its substance A is Linolenic Acid, 12,15- trienic acid, acetylene cyclohexanol, dimethylphosphite, dimethylformamide dimethyl oxygroup Any one of silane.
The preparation method of its antibacterial agent is:By gefarnate 1.2g, the bromo- 2- nitro -1,3- third of vinyl phosphonic acid 1.3g, 2- Alcohol 1.2g, 2,5- dimethyl -3- hexin -2,5- glycol 1.2g and 15g acetone are added in flask, and ethanedioly chloride 0.4g is being added 2 ~ 3h is reacted at 60 DEG C with borogen 0.7g, is removed acetone, is obtained the antibacterial agent.
Emulsifier is neopelex and fatty alcohol polyoxyethylene ether by weight 3:1 mixed mixture.
Initiator A is any one of ammonium persulfate, potassium peroxydisulfate.
Crosslinking agent is Diethylenetriamine, -2,5 di-t-butyl hexane peroxide of 2,5- dimethyl, trien, diformazan Any one of amido propylamine, diethyl amino propylamine.
Advantage of the invention is that:
(1)The fire retardant and antibacterial agent are reacted with acrylic ester monomer, can be changed that fire-retardant index is not high, and antibacterial is unabiding Defect particularly synthesizes fire-retardant intermediate, used catalyst A using dimethylphosphite, catalyst A, acrylamide Replace traditional sodium methoxide, makes products obtained therefrom without methanol smell, adding pentaerythrite, substance A, 4-aminophenol keeps institute proper There is double bond generation in system(Be particularly due to substance A as entered), obtained flame-retardant agent has double bond, in this way in subsequent and acrylate Class monomer reaction can be integrated on the main chain of acrylic resin, and 4-aminophenol, which plays, improves substance A binding ability,
(2)Identical thinking synthetic antibacterial agents are also used simultaneously, by gefarnate, vinyl phosphonic acid, the bromo- 2- nitro -1,3- third of 2- Alcohol 1.2g, 2,5- dimethyl -3- hexin -2,5- glycol, ethanedioly chloride, borogen hybrid reaction make gained antibacterial agent system In there are double bond and three keys, then reacted with acrylic ester monomer, improve the persistence of antibacterial agent, and traditional antibacterial agent adds It based on adding type, causes antibacterial not lasting, while improving the binding ability of unsaturated bond using borogen.
Specific embodiment
Example 1
Fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint preparation method, preparation method are:
(1)40 parts of water, 0.6 part of emulsifier, 1.6 parts of methacrylic acid are added into reaction vessel, is warming up to 60 DEG C, stirring 40min adds A monomer, emulsification times 30min;It is warming up to 70 DEG C and starts logical recirculation water, keep the temperature 1h after being warming up to 80 DEG C, 0.4 parts by weight of initiator A (being dissolved with 5 parts by weight aqueous solvents) is added dropwise, time for adding continues 1h, reacts 2h after dripping, obtains core Layer lotion;
The A monomer be by:3 parts by weight of butyl acrylate, 2 parts by weight of methyl methacrylate, 3 parts by weight of ethyl acrylate and 1 parts by weight of hydroxy-ethyl acrylate mix;
(2)To step(1)It is (water-soluble with 5 parts by weight that B monomer, the initiator A of 0.3 parts by weight is added dropwise simultaneously in gained stratum nucleare lotion Agent dissolution) and 3.6 parts by weight of fire retardant, time for adding continue 1h, drip addition 0.4 parts by weight of antibacterial agent at 75 DEG C afterwards, stir Reaction 2h is mixed, 0.8 parts by weight of crosslinking agent are added, 75 DEG C of reaction time 1h cool to 50 DEG C, 0.4 parts by weight of emulsifier are added, Reaction time 40min adds ammonium hydroxide tune pH value to 7 ~ 8, obtains fire-retardant, the antibiotic property aqueous core shell acrylic esters resin and apply Material and paint;
The B monomer be by:2 parts by weight of butyl acrylate, 2 parts by weight of methyl methacrylate, 3 parts by weight of ethyl acrylate and 1 parts by weight of hydroxy-ethyl acrylate mix.
Dimethylphosphite 0.5mol is added in three-necked flask, catalyst A0.004mol and 0.5mol acryloyl is added Amine, agitating paddle, condenser pipe and thermometer in connection, is slowly warming up to 70 DEG C, insulation reaction 2h, and obtaining weak yellow liquid is 3-two Methoxy phosphoryl propionamide;Tetrakis hydroxymetyl phosphonium sulfuric 0.2mol, reaction are added into resulting 3-dimethoxy phosphoryl propionamide Temperature 50 C, reaction time 2h add pentaerythrite 0.2mol, dissolve pentaerythrite sufficiently, are warming up to 70 DEG C, reaction Time 2h adds substance A 0.1mol and 4-aminophenol 0.6mol, and 70 DEG C of reaction temperature, reaction time 2h cools To fire retardant A.
Its catalyst A is diethyl maleate.
Its substance A is Linolenic Acid, 12,15- trienic acid.
The preparation method of its antibacterial agent is:By gefarnate 1.2g, the bromo- 2- nitro -1,3- third of vinyl phosphonic acid 1.3g, 2- Alcohol 1.2g, 2,5- dimethyl -3- hexin -2,5- glycol 1.2g and 15g acetone are added in flask, and ethanedioly chloride 0.4g is being added 2h is reacted at 60 DEG C with borogen 0.7g, is removed acetone, is obtained the antibacterial agent.
Emulsifier is neopelex and fatty alcohol polyoxyethylene ether by weight 3:1 mixed mixture.
Initiator A is ammonium persulfate.
Crosslinking agent is Diethylenetriamine.
Example 2
Fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint preparation method, preparation method are:
(1)75 parts of water, 2.4 parts of emulsifier, 3.0 parts of methacrylic acid are added into reaction vessel, is warming up to 60 DEG C, stirring 40min adds A monomer, emulsification times 40min;It is warming up to 70 DEG C and starts logical recirculation water, keep the temperature 1h after being warming up to 80 DEG C, 0.6 parts by weight of initiator A (being dissolved with 5 parts by weight aqueous solvents) is added dropwise, time for adding continues 2h, reacts 2h after dripping, obtains core Layer lotion;
The A monomer be by:5 parts by weight of butyl acrylate, 7 parts by weight of methyl methacrylate, 6 parts by weight of ethyl acrylate and 7 parts by weight of hydroxy-ethyl acrylate mix;
(2)To step(1)It is (water-soluble with 5 parts by weight that B monomer, the initiator A of 0.6 parts by weight is added dropwise simultaneously in gained stratum nucleare lotion Agent dissolution) and 3.6 parts by weight of fire retardant, time for adding continue 2h, drip addition 0.4 parts by weight of antibacterial agent at 85 DEG C afterwards, stir Reaction 2h is mixed, 1.0 parts by weight of crosslinking agent are added, 85 DEG C of reaction time 2h cool to 50 DEG C, and 0.4 weight of emulsifier is added Part, reaction time 40min adds ammonium hydroxide tune pH value to 7 ~ 8, obtains fire-retardant, the antibiotic property aqueous core shell acrylic esters tree Grease coating material and paint;
The B monomer be by:4 parts by weight of butyl acrylate, 8 parts by weight of methyl methacrylate, 7 parts by weight of ethyl acrylate and 8 parts by weight of hydroxy-ethyl acrylate mix.
The preparation method of fire retardant A:Dimethylphosphite 0.5mol is added in three-necked flask, catalyst is added A0.004mol and 0.8mol acrylamide, agitating paddle, condenser pipe and thermometer in connection, is slowly warming up to 90 DEG C, insulation reaction 5h, obtaining weak yellow liquid is 3-dimethoxy phosphoryl propionamides;Four are added into resulting 3-dimethoxy phosphoryl propionamide Methylol sulfuric acid phosphorus 0.6mol, 90 DEG C of reaction temperature, reaction time 3h adds pentaerythrite 0.2mol, fills pentaerythrite Divide dissolution, is warming up to 90 DEG C, reaction time 3h, adds substance A 0.1mol and 4-aminophenol 0.6mol, reaction temperature 90 DEG C, reaction time 2h cools to obtain fire retardant A.
Its catalyst A is dimethyl maleate.
Its substance A is acetylene cyclohexanol.
The preparation method of its antibacterial agent is:By gefarnate 1.2g, the bromo- 2- nitro -1,3- third of vinyl phosphonic acid 1.3g, 2- Alcohol 1.2g, 2,5- dimethyl -3- hexin -2,5- glycol 1.2g and 15g acetone are added in flask, and ethanedioly chloride 0.4g is being added 3h is reacted at 60 DEG C with borogen 0.7g, is removed acetone, is obtained the antibacterial agent.
Emulsifier is neopelex and fatty alcohol polyoxyethylene ether by weight 3:1 mixed mixture.
Initiator A is potassium peroxydisulfate.
Crosslinking agent is -2,5 di-t-butyl hexane peroxide of 2,5- dimethyl.
Example 3
Fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint preparation method, preparation method are:
(1)58 parts by weight of water, 1.5 parts by weight of emulsifier, 2.4 parts by weight of methacrylic acid are added into reaction vessel, are warming up to 60 DEG C, 40min is stirred, A monomer, emulsification times 35min are added;It is warming up to 70 DEG C and starts logical recirculation water, be warming up to 80 DEG C After keep the temperature 1h, 0.5 parts by weight of initiator A (with the dissolution of 5 parts by weight aqueous solvents) is added dropwise, time for adding continues 1.5h, after dripping 2h is reacted, stratum nucleare lotion is obtained;
The A monomer be by:4 parts by weight of butyl acrylate, 4.5 parts by weight of methyl methacrylate, 4.5 weight of ethyl acrylate Part and 4 parts by weight of hydroxy-ethyl acrylate mix;
(2)To step(1)It is (water-soluble with 5 parts by weight that B monomer, the initiator A of 0.45 parts by weight is added dropwise simultaneously in gained stratum nucleare lotion Agent dissolution) and 3.6 parts by weight of fire retardant, time for adding continue 1.5h, drip addition 0.4 parts by weight of antibacterial agent at 80 DEG C afterwards, It is stirred to react 2h, adds 0.9 parts by weight of crosslinking agent, 80 DEG C of reaction time 1.5h cool to 50 DEG C, and 0.4 weight of emulsifier is added Part is measured, reaction time 40min adds ammonium hydroxide tune pH value to 7 ~ 8, obtains fire-retardant, the antibiotic property aqueous core shell acrylic esters Cold coating and paint;
The B monomer be by:3 parts by weight of butyl acrylate, 5 parts by weight of methyl methacrylate, 5 parts by weight of ethyl acrylate and 4.5 parts by weight of hydroxy-ethyl acrylate mix.
The preparation method of fire retardant A:Dimethylphosphite 0.5mol is added in three-necked flask, catalyst is added A0.004mol and 0.65mol acrylamide, agitating paddle, condenser pipe and thermometer in connection are slowly warming up to 80 DEG C, and heat preservation is anti- 3.5h is answered, obtaining weak yellow liquid is 3-dimethoxy phosphoryl propionamides;Add into resulting 3-dimethoxy phosphoryl propionamide Enter tetrakis hydroxymetyl phosphonium sulfuric 0.4mol, 70 DEG C of reaction temperature, reaction time 2.5h adds pentaerythrite 0.2mol, makes season penta Tetrol sufficiently dissolves, and is warming up to 80 DEG C, reaction time 2.5h, adds substance A 0.1mol and 4-aminophenol 0.6mol, reaction 80 DEG C of temperature, reaction time 2h cools to obtain fire retardant A.
Its catalyst A is diacetyl monoxime.
Its substance A is dimethylphosphite.
The preparation method of its antibacterial agent is:By gefarnate 1.2g, the bromo- 2- nitro -1,3- third of vinyl phosphonic acid 1.3g, 2- Alcohol 1.2g, 2,5- dimethyl -3- hexin -2,5- glycol 1.2g and 15g acetone are added in flask, and ethanedioly chloride 0.4g is being added 2.5h is reacted at 60 DEG C with borogen 0.7g, is removed acetone, is obtained the antibacterial agent.
Emulsifier is neopelex and fatty alcohol polyoxyethylene ether by weight 3:1 mixed mixture.
Initiator A is ammonium persulfate.
Crosslinking agent is trien.
Example 4
Fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint preparation method, preparation method are:
(1)50 parts by weight of water, 1 parts by weight of emulsifier, 2.7 parts of methacrylic acid are added into reaction vessel, is warming up to 60 DEG C, stirs 40min is mixed, A monomer, emulsification times 35min are added;It is warming up to 70 DEG C and starts logical recirculation water, kept the temperature after being warming up to 80 DEG C 0.4 parts by weight of initiator A (being dissolved with 5 parts by weight aqueous solvents) is added dropwise in 1h, and time for adding continues 1h, reacts 2h after dripping, obtains Stratum nucleare lotion;
The A monomer be by:5 parts by weight of butyl acrylate, 4 parts by weight of methyl methacrylate, 4 parts by weight of ethyl acrylate and 5 parts by weight of hydroxy-ethyl acrylate mix;
(2)To step(1)It is (water-soluble with 5 parts by weight that B monomer, the initiator A of 0.4 parts by weight is added dropwise simultaneously in gained stratum nucleare lotion Agent dissolution) and 3.6 parts by weight of fire retardant, time for adding continue 1h, drip addition 0.4 parts by weight of antibacterial agent at 75 DEG C afterwards, stir Reaction 2h is mixed, 0.8 parts by weight of crosslinking agent are added, 75 DEG C of reaction time 1h cool to 50 DEG C, 0.4 parts by weight of emulsifier are added, Reaction time 40min adds ammonium hydroxide tune pH value to 7 ~ 8, obtains fire-retardant, the antibiotic property aqueous core shell acrylic esters resin and apply Material and paint;
The B monomer be by:2 parts by weight of butyl acrylate, 2 parts by weight of methyl methacrylate, 7 parts by weight of ethyl acrylate and 8 parts by weight of hydroxy-ethyl acrylate mix.
The preparation method of fire retardant A:Dimethylphosphite 0.5mol is added in three-necked flask, catalyst is added A0.004mol and 0.5mol acrylamide, agitating paddle, condenser pipe and thermometer in connection, is slowly warming up to 70 DEG C, insulation reaction 5h, obtaining weak yellow liquid is 3-dimethoxy phosphoryl propionamides;Four are added into resulting 3-dimethoxy phosphoryl propionamide Methylol sulfuric acid phosphorus 0.6mol, 90 DEG C of reaction temperature, reaction time 3h adds pentaerythrite 0.2mol, fills pentaerythrite Divide dissolution, is warming up to 90 DEG C, reaction time 3h, adds substance A 0.1mol and 4-aminophenol 0.6mol, reaction temperature 90 DEG C, reaction time 2h cools to obtain fire retardant A.
Its catalyst A is methyl benzilate.
Its substance A is dimethyldimethoxysil,ne.
The preparation method of its antibacterial agent is:By gefarnate 1.2g, the bromo- 2- nitro -1,3- third of vinyl phosphonic acid 1.3g, 2- Alcohol 1.2g, 2,5- dimethyl -3- hexin -2,5- glycol 1.2g and 15g acetone are added in flask, and ethanedioly chloride 0.4g is being added 2h is reacted at 60 DEG C with borogen 0.7g, is removed acetone, is obtained the antibacterial agent.
Emulsifier is neopelex and fatty alcohol polyoxyethylene ether by weight 3:1 mixed mixture.
Initiator A is ammonium persulfate.
Crosslinking agent is dimethylamine propylamine.
Example 5
Fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint preparation method, preparation method are:
(1)40 parts of water, 1.2 parts of emulsifier, 1.6 parts of methacrylic acid are added into reaction vessel, is warming up to 60 DEG C, stirring 40min adds A monomer, emulsification times 30min;It is warming up to 70 DEG C and starts logical recirculation water, keep the temperature 1h after being warming up to 80 DEG C, 0.4 parts by weight of initiator A (being dissolved with 5 parts by weight aqueous solvents) is added dropwise, time for adding continues 1h, reacts 2h after dripping, obtains core Layer lotion;
The A monomer be by:3.5 parts by weight of butyl acrylate, 4 parts by weight of methyl methacrylate, 4 parts by weight of ethyl acrylate It is mixed with 3 parts by weight of hydroxy-ethyl acrylate;
(2)To step(1)It is (water-soluble with 5 parts by weight that B monomer, the initiator A of 0.3 parts by weight is added dropwise simultaneously in gained stratum nucleare lotion Agent dissolution) and 3.6 parts by weight of fire retardant, time for adding continue 1h, drip addition 0.4 parts by weight of antibacterial agent at 75 DEG C afterwards, stir Reaction 2h is mixed, 1.0 parts by weight of crosslinking agent are added, 85 DEG C of reaction time 1h cool to 50 DEG C, 0.4 parts by weight of emulsifier are added, Reaction time 40min adds ammonium hydroxide tune pH value to 7 ~ 8, obtains fire-retardant, the antibiotic property aqueous core shell acrylic esters resin and apply Material and paint;
The B monomer be by:4 parts by weight of butyl acrylate, 6 parts by weight of methyl methacrylate, 4 parts by weight of ethyl acrylate and 3 parts by weight of hydroxy-ethyl acrylate mix.
Fire retardant A:Will dimethylphosphite 0.5mol be added three-necked flask in, be added catalyst A0.004mol and 0.5mol acrylamide, agitating paddle, condenser pipe and thermometer in connection, is slowly warming up to 90 DEG C, insulation reaction 5h is obtained faint yellow Liquid is 3-dimethoxy phosphoryl propionamides;Tetrakis hydroxymetyl phosphonium sulfuric is added into resulting 3-dimethoxy phosphoryl propionamide 0.6mol, 90 DEG C of reaction temperature, reaction time 2h adds pentaerythrite 0.2mol, dissolves pentaerythrite sufficiently, heating To 70 DEG C, reaction time 3h, substance A 0.1mol and 4-aminophenol 0.6mol are added, 70 DEG C of reaction temperature, the reaction time 2h cools to obtain fire retardant A.
Its catalyst A is methyl benzilate.
Its substance A is dimethylphosphite.
The preparation method of its antibacterial agent is:By gefarnate 1.2g, the bromo- 2- nitro -1,3- third of vinyl phosphonic acid 1.3g, 2- Alcohol 1.2g, 2,5- dimethyl -3- hexin -2,5- glycol 1.2g and 15g acetone are added in flask, and ethanedioly chloride 0.4g is being added 2.5h is reacted at 60 DEG C with borogen 0.7g, is removed acetone, is obtained the antibacterial agent.
Emulsifier is neopelex and fatty alcohol polyoxyethylene ether by weight 3:1 mixed mixture.
Initiator A is ammonium persulfate.
Crosslinking agent is diethyl amino propylamine.
Anti-flammability is measured by oxygen index (OI), flaming combustion time, antibiotic property using Escherichia coli, golden yellow staphylococcus and Yellow inulinase bacterium measures.
Table 1 is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint test performance
Example 1 Example 2 Example 3 Example 4 Example 5
Oxygen index (OI)/% 29.5 29.9 29.6 29.7 29.6
Flaming combustion time/s 2.1 3.3 1.3 1.8 2.6
As it can be seen from table 1 this is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint are superior to background skill The performance of patent of invention mentioned in art, since length is limited, 201610331925.3 oxygen index (OI) can reach 26.6, there is flame Burning time is 2.2s, and glowing time 0, the present invention is better than documents.
Table 2 is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint test performance(Not plus fire retardant)
Example 1 Example 2 Example 3 Example 4 Example 5
Oxygen index (OI)/% 24.2 21.8 22.1 23.2 22.8
Flaming combustion time/s 11.8 21.7 22.8 24.8 32.8
From table 2 it can be seen that this is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint do not add fire retardant, Its oxygen index (OI) and flaming combustion time greatly improve.
Table 3 is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint test performance(Add fire retardant, not Add catalyst A)
Example 1 Example 2 Example 3 Example 4 Example 5
Oxygen index (OI)/% 26.3 24.3 23.4 24.9 25.1
Flaming combustion time/s 10.3 12.5 13.6 19.7 14.2
From table 3 it can be seen that this is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint plus fire retardant and not Add catalyst A, oxygen index (OI) does not add fire retardant high than, and flaming combustion time is greatly reduced.
Table 4 is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint test performance(Add fire retardant, not Add substance A)
Example 1 Example 2 Example 3 Example 4 Example 5
Oxygen index (OI)/% 25.8 25.1 24.9 25.4 25.7
Flaming combustion time/s 12.6 6.8 4.5 4.9 9.5
Apply resistance from table 4, it can be seen that this is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating compares with paint Oxygen index (OI) declines when firing agent, and flaming combustion time improves.
Table 5 is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint(%)The same day
Example 1 Example 2 Example 3 Example 4 Example 5
Escherichia coli 97 99 98 96 97
Golden yellow staphylococcus 96 96 98 98 99
Yellow inulinase 97 97 97 98 99
As can be seen from Table 5, which has preferable antibacterial effect.
Table 6 is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint(%)360 days
Example 1 Example 2 Example 3 Example 4 Example 5
Escherichia coli 78 79 81 78 78
Golden yellow staphylococcus 77 76 71 74 76
Yellow inulinase 68 69 68 71 75
As can be seen from Table 6, which has good Durability of antimicrobial effect.
Table 7 is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint(%)The same day, not plus(Gefarnate)
Example 1 Example 2 Example 3 Example 4 Example 5
Escherichia coli 82 81 79 81 83
Golden yellow staphylococcus 83 85 76 78 84
Yellow inulinase 72 74 79 81 73
As can be found from Table 7, gefarnate in the antibacterial agent plays the effect for improving antibiotic property.
Table 8 is fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint(%)The same day, not plus(Boric acid second Ester)
Example 1 Example 2 Example 3 Example 4 Example 5
Escherichia coli 81 77 74 72 76
Golden yellow staphylococcus 73 87 79 76 74
Yellow inulinase 65 77 69 73 72
As can be seen from Table 8, borogen improves its antibiotic property.

Claims (8)

1. the preparation method of fire-retardant antibiotic property aqueous core shell acrylic esters resin coating and paint, preparation method are:
(1)40 ~ 75 parts of water, 0.6 ~ 2.4 part of emulsifier, 1.6 ~ 3.0 parts of methacrylic acid are added into reaction vessel, is warming up to 60 DEG C, 40min is stirred, A monomer is added, emulsification times are 30 ~ 40min;It is warming up to 70 DEG C and starts logical recirculation water, be warming up to 80 DEG C After keep the temperature 1h, 0.4 ~ 0.6 parts by weight of initiator A (being dissolved with 5 parts by weight aqueous solvents) is added dropwise, time for adding continues 1 ~ 2h, dropwise addition 2h is reacted after complete, obtains stratum nucleare lotion;
The A monomer be by:3 ~ 5 parts by weight of butyl acrylate, 2 ~ 7 parts by weight of methyl methacrylate, 3 ~ 6 weight of ethyl acrylate Amount part and 1 ~ 7 parts by weight of hydroxy-ethyl acrylate mix;
(2)To step(1)In gained stratum nucleare lotion simultaneously be added dropwise B monomer, 0.3 ~ 0.6 parts by weight initiator A (with 5 parts by weight Aqueous solvent dissolution) and 3.6 parts by weight of fire retardant, time for adding continue 1 ~ 2h, addition antibacterial agent 0.4 at 75 ~ 85 DEG C after dripping Parts by weight are stirred to react 2h, add 0.8 ~ 1.0 parts by weight of crosslinking agent, and 75 ~ 85 DEG C of 1 ~ 2h of reaction time cool to 50 DEG C, add Enter 0.4 parts by weight of emulsifier, reaction time 40min adds ammonium hydroxide tune pH value to 7 ~ 8, obtains fire-retardant, the aqueous nucleocapsid of antibiotic property Type acrylic resin coating and paint;
The B monomer be by:2 ~ 4 parts by weight of butyl acrylate, 2 ~ 8 parts by weight of methyl methacrylate, 3 ~ 7 weight of ethyl acrylate Amount part and 1 ~ 8 parts by weight of hydroxy-ethyl acrylate mix.
2. fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint the preparation method as described in right 1, The preparation method of fire retardant is:Will dimethylphosphite 0.5mol be added three-necked flask in, be added catalyst A0.004mol and 0.5 ~ 0.8mol acrylamide, agitating paddle, condenser pipe and thermometer in connection are slowly warming up to 70 ~ 90 DEG C, and insulation reaction 2 ~ 5h, obtaining weak yellow liquid is 3-dimethoxy phosphoryl propionamides;Four are added into resulting 3-dimethoxy phosphoryl propionamide Methylol sulfuric acid 0.2 ~ 0.6mol of phosphorus, 50 DEG C ~ 90 DEG C of reaction temperature, 2 ~ 3h of reaction time adds pentaerythrite 0.2mol, It dissolves pentaerythrite sufficiently, is warming up to 70 ~ 90 DEG C, 2 ~ 3h of reaction time adds substance A 0.1mol and 4-aminophenol 0.6mol, 70 ~ 90 DEG C of reaction temperature, reaction time 2h cools to obtain fire retardant A.
3. fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint the preparation method as described in right 2, Catalyst A is any one of diethyl maleate, dimethyl maleate, diacetyl monoxime, methyl benzilate.
4. fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint the preparation method as described in right 2, Substance A is Linolenic Acid, 12,15- trienic acid, acetylene cyclohexanol, dimethylphosphite, dimethyldimethoxysil,ne it is any It is a kind of.
5. fire-retardant, antibiotic property aqueous core shell acrylic esters resin coating and paint the preparation method as described in right 1, The preparation method of antibacterial agent is:By gefarnate 1.2g, bromo- 2- nitro -1,3- propyl alcohol 1.2g, the 2,5- of vinyl phosphonic acid 1.3g, 2- Dimethyl -3- hexin -2,5- glycol 1.2g and 15g acetone is added in flask, and ethanedioly chloride 0.4g and borogen is being added 0.7g reacts 2 ~ 3h at 60 DEG C, removes acetone, obtains the antibacterial agent.
6. a kind of preparation method of the core-shell type aqueous acrylic resin coating of anti-flammability as described in claim 1, special Sign is that emulsifier is neopelex and fatty alcohol polyoxyethylene ether by weight 3:1 mixed mixture.
7. fire-retardant, waterproof aqueous core shell acrylic esters resin coating and paint the preparation method as described in right 1, described Initiator A be ammonium persulfate, potassium peroxydisulfate any one.
8. fire-retardant, waterproof aqueous core shell acrylic esters resin coating and paint the preparation method as described in right 1, described Crosslinking agent be Diethylenetriamine, -2,5 di-t-butyl hexane peroxide of 2,5- dimethyl, trien, dimethylamino third Any one of amine, diethyl amino propylamine.
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