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CN109337421A - A kind of aqueous polyurethane anti-flaming dope and preparation method - Google Patents

A kind of aqueous polyurethane anti-flaming dope and preparation method Download PDF

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Publication number
CN109337421A
CN109337421A CN201811118645.XA CN201811118645A CN109337421A CN 109337421 A CN109337421 A CN 109337421A CN 201811118645 A CN201811118645 A CN 201811118645A CN 109337421 A CN109337421 A CN 109337421A
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weight
parts
agent
aqueous polyurethane
flaming dope
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陈庆
曾军堂
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Chengdu New Keli Chemical Science Co Ltd
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Chengdu New Keli Chemical Science Co Ltd
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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
    • C09D4/00Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
    • C09D4/06Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
    • 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
    • C09D7/43Thickening agents
    • 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
    • C09D7/47Levelling agents
    • 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
    • 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
    • C09D7/65Additives macromolecular

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)
  • Fireproofing Substances (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention relates to paint field, a kind of aqueous polyurethane anti-flaming dope and preparation method are disclosed.Including following preparation process: (1) melting antimony under 1MPa air pressure at 1000-1300 DEG C and clashed with high pressure draught and micron silicon lime stone powder, deposit antimony oxide ultra-fine grain in particle surface, the composite particulate material with nucleocapsid structure is made;(2) it is compounded with decabromodiphenylethane, the synergistic fire retardant of halogen-sb system is made;(3) it is added in deionized water after mixing pentaerythritol triacrylate, high chlorinated polyethylene resin, polyurethane resin and methyl silicon resin, mixed liquor is made;(4) coalescing agent, thickener, levelling agent, dispersing agent, defoaming agent, synergistic fire retardant are added into mixed liquor, water flame-proof paint is made in agitation grinding.The composite particles for having increased core-shell structure of the anti-flaming dope that the present invention obtains, formation have bigger serface and higher activity, can effectively be compounded with bromide fire retardant, by the way of compound, be obviously improved the flame retarding efficiency of coating.

Description

A kind of aqueous polyurethane anti-flaming dope and preparation method
Technical field
The present invention relates to paint field, a kind of aqueous polyurethane anti-flaming dope and preparation method are disclosed.
Background technique
Fireproof flame-retardant coating is coated on flammable substrates surface, can reduce by the combustibility of painting material surface, block fire Rapid sprawling, or be coated on structural material surface, for improving the fire endurance of component;Fireproof coating generally by base-material, Decentralized medium, fire retardant, filler, auxiliary agent (plasticizer, stabilizer, waterproofing agent, anti-blushing agent etc.) composition, have been widely used in and have built It builds, the vehicles such as vehicle, aircraft, tire, historical relic's protection, electric appliance, cable, warehouse, military project, word boat etc..
Anti-flaming dope is generally divided into two class of intumescent and non-expansion type according to fire-retardant principle, and Non-expansive fireproof paint is to lean on Its own high fire retardant or noninflammability achievees the purpose that fire-retardant fireproof, and the flameproof effect to reach must apply very thick, Addition largely containing fire retardants such as halogen, nitrogen, phosphorus, generates a large amount of toxic gases, expanding fire-proof paint is exactly film expanded by heating Honeycomb charring layer is formed, flame heat regulating is isolated and reduces or slow down the transmitting to ground, while coating at high temperature Non-flammable compressive gas is decomposited, air is completely cut off and dilute, a series of physical and chemical reaction that in addition coating occurs in fire prevention are inhaled Amount of heat has been received to play fire-retardant and delay flame spread, sprawling, provides the time of fire extinguishing for people.
Research at present uses intensity of the inorganic resin for the fireproof coating of main binder to improve coating, but using inorganic Resin is that the fireproof coating high temperature of adhesive preparation is easy cracking, and adhesive strength is low.In aqueous polyurethane coating system hardly Containing organic solvent, there are the series of advantages such as nontoxic, environmentally friendly, easy to use, wear-resistant, high resiliency, high intensity, yield and Demand is all in sharp increase, but the fatal weakness of inflammability limits it in the application in many fields.Therefore, extinguishing waterborn is poly- Urethane coating becomes research hot topic project in recent years.
Chinese invention patent application number 201610241148.3 discloses a kind of aqueous polyurethane anti-flaming dope, by following heavy The raw material of amount part is made: 30 ~ 80 parts of waterborne polyurethane resin, 10 ~ 20 parts of dispersion moisture agent, 1 ~ 5 part of defoaming agent, preservative 1 ~ 5 Part, 10 ~ 20 parts of coalescing agent, 1 ~ 10 part and 50 ~ 150 parts of water of fire retardant.Water flame-proof paint described in the invention has preferable Flameproof effect, have broad prospects in industrial application.
Chinese invention patent application number 201610735568.7 discloses a kind of high resistant burning coating material, and raw material includes: aqueous Acrylic acid ester emulsion, waterborne polyurethane resin, Aluminum sol, epoxy resin, dimethyl silicone polymer, zinc oxide, hollow glass are micro- Pearl, nano zircite, montmorillonite, nano silica, coalescing agent, defoaming agent, levelling agent, wetting agent, fire retardant, water;Institute Fire retardant is stated by boron oxide, dimethyl methyl phosphonate, phosphorus pentoxide, tricresyl phosphate (2- chloropropyl) ester, guanylurea phosphate, poly- phosphorus Sour ammonium, pentaerythrite, melamine, hexamethyldisiloxane mix, the high resistant burning coating material which proposes, water resistance Good, the excellent fireproof performance with wearability, and long service life.
According to above-mentioned, extinguishing waterborn polyurethane coating in existing scheme there are flame retarding efficiencies poor, fire-retardant at high cost, compounding Fire retardant significantly affects the defects of physicochemical property of coating, therefore, has good flame-retardance poly- with the extinguishing waterborn of physicochemical property Urethane coating becomes one of significant concern problem of paint field.
Summary of the invention
Poor, fire-retardant at high cost, the compounding resistance using the wider generally existing flame retarding efficiency of extinguishing waterborn polyurethane coating at present The defects of combustion agent significantly affects the physicochemical property of coating.
To solve the above problems, the invention adopts the following technical scheme:
A kind of preparation method of aqueous polyurethane anti-flaming dope, the detailed process of preparation are as follows:
(1) antimony is melted under 1MPa air pressure at 1000-1300 DEG C and is clashed with high pressure draught and micron silicon lime stone powder, Antimony oxide ultra-fine grain is deposited in particle surface, the composite particulate material with nucleocapsid structure is made;Antimony and micron silicon The mass ratio of lime stone powder is 1:3;
(2) composite particulate material made from step (1) is compounded with decabromodiphenylethane, the particle of antimony oxide cladding As the synergist of bromide fire retardant, the synergistic fire retardant of halogen-sb system is made;
(3) pentaerythritol triacrylate, high chlorinated polyethylene resin, polyurethane resin and methyl silicon resin are mixed, is added It in deionized water, stirs evenly, mixed liquor is made;
(4) addition coalescing agent, thickener, levelling agent, dispersing agent and defoaming agent into mixed liquor made from step (3), then plus Enter synergistic fire retardant made from step (2), stir evenly, grind, aqueous polyurethane anti-flaming dope is made.
Preferably, in step (2), composite particulate material 70-80 parts by weight, 20 ~ 30 parts by weight of decabromodiphenylethane.
Preferably, in step (3), 5 ~ 8 parts by weight of pentaerythritol triacrylate, 6 ~ 12 weight of high chlorinated polyethylene resin Part, 3 ~ 5 parts by weight of polyurethane resin, 5 ~ 10 parts by weight of methyl silicon resin, 65 ~ 81 parts by weight of deionized water.
Preferably, in step (4), 79 ~ 89 parts by weight of mixed liquor, 2 ~ 4 parts by weight of coalescing agent, 1 ~ 3 parts by weight of thickener, 1 ~ 2 parts by weight of levelling agent, 1 ~ 2 parts by weight of dispersing agent, 1 ~ 2 parts by weight of defoaming agent, 5 ~ 8 parts by weight of synergistic fire retardant.
Preferably, step (4) coalescing agent is 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates.
Preferably, step (4) thickener is methylcellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl At least one of cellulose.
Preferably, step (4) levelling agent is polymethylphenylsiloxane, dimethyl silicone polymer, polyether-modified has At least one of organic siloxane, polyester modified organic siloxane.
Preferably, step (4) dispersing agent is that glyceryl monostearate, vinyl bis-stearamides, three stearic acid are sweet At least one of grease, oleic acid acyl.
Preferably, step (4) defoaming agent is polyoxyethylene polyoxypropylene pentaerythrite ether, polyoxyethylene polyoxy propyl alcohol At least one of amidogen ether, polypropylene glycerol aether.
A kind of aqueous polyurethane anti-flaming dope prepared by the above method, using deposition principle, silicon ash in the micron-scale Mountain flour body particle surface deposits antimony oxide ultra-fine grain, can not only modify micron silicon limestone particles pattern, is formed specific The composite particulate material of " core-shell structure copolymer " structure, and due to the cladding of antimony oxide, the surface-active of wollastonite fibre can be improved, Improve the flexibility and dispersibility of wollastonite fibre;Gained particle is compounded with decabromodiphenylethane, antimony oxide packet Cover particle as bromide fire retardant and obtain synergist, can formed halogen-antimony collaboration system, when antimony oxide particle and halogen system hinder When hydrogeneous bromide fire retardant in combustion agent is used in compounding, antimony oxide can generate three with reaction of hydrogen bromide in combustion Bromination antimony or bromine antimony oxide.And bromine antimony oxide can continue to be decomposed into antimonous bromide within the scope of very wide temperature, formation Antimonous bromide can effectively prevent the progress of combustion reaction, improve flame retarding efficiency;Again by pentaerythritol triacrylate, high chlorine Change polyvinyl resin, polyurethane resin and methyl silicon resin mixing, adds film forming after uniform stirring after addition deionized water and help Agent, continuously adds thickener, levelling agent, dispersing agent and defoaming agent and obtained flame-retardant agent, uniform stirring and after grinding.
It is compared with prior art, outstanding the present invention provides a kind of aqueous polyurethane anti-flaming dope and preparation method Feature and excellent effect are:
1, it proposes and compound preparation for aqueous resistance with the wollastonite composite particles of core-shell structure using decabromodiphenylethane The method of burning coating material.
2, by the way that superfine antimony trioxide particle is coated on micron silicon lime stone powder using the method for surface deposition The surface of grain, has increased bigger serface and has improved seed activity, improved the flexibility and dispersibility of wollastonite fibre.
3, by compounding the composite particles of the core-shell structure of formation with bromide fire retardant, using compound side Formula has been obviously improved the flame retarding efficiency of anti-flaming dope.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
(1) antimony is melted under 1MPa air pressure at 1200 DEG C and is clashed with high pressure draught and micron silicon lime stone powder, Grain surface deposits antimony oxide ultra-fine grain, and the composite particulate material with nucleocapsid structure is made;Antimony and micron silicon lime stone The mass ratio of powder is 1:3;
(2) composite particulate material made from step (1) is compounded with decabromodiphenylethane, the particle of antimony oxide cladding As the synergist of bromide fire retardant, the synergistic fire retardant of halogen-sb system is made;
Wherein, 75 parts by weight of composite particles, 25 parts by weight of decabromodiphenylethane;
(3) pentaerythritol triacrylate, high chlorinated polyethylene resin, polyurethane resin and methyl silicon resin are mixed, is added It in deionized water, stirs evenly, mixed liquor is made;
Wherein, 7 parts by weight of pentaerythritol triacrylate, 8 parts by weight of high chlorinated polyethylene resin, 4 parts by weight of polyurethane resin, 7 parts by weight of methyl silicon resin, 73 parts by weight of deionized water;
(4) addition coalescing agent, thickener, levelling agent, dispersing agent and defoaming agent into mixed liquor made from step (3), then plus Enter synergistic fire retardant made from step (2), stir evenly, grind, aqueous polyurethane anti-flaming dope is made;Coalescing agent is 2,2, 4- trimethyl -1,3- pentanediol mono isobutyrate;Thickener is methylcellulose;Levelling agent is polymethylphenylsiloxane;Point Powder is glyceryl monostearate;Defoaming agent is polyoxyethylene polyoxypropylene pentaerythrite ether;
Wherein, 85 parts by weight of mixed liquor, 3 parts by weight of coalescing agent, 2 parts by weight of thickener, 1 parts by weight of levelling agent, 2 weight of dispersing agent Measure part, 1 parts by weight of defoaming agent, 6 parts by weight of synergistic fire retardant.
Water flame-proof paint made from embodiment 1, big plate combustion test test plate (panel) burn through time, combustion phenomena such as 1 institute of table Show.
Embodiment 2
(1) antimony is melted under 1MPa air pressure at 1200 DEG C and is clashed with high pressure draught and micron silicon lime stone powder, Grain surface deposits antimony oxide ultra-fine grain, and the composite particulate material with nucleocapsid structure is made;Antimony and micron silicon lime stone The mass ratio of powder is 1:3;
(2) composite particulate material made from step (1) is compounded with decabromodiphenylethane, the particle of antimony oxide cladding As the synergist of bromide fire retardant, the synergistic fire retardant of halogen-sb system is made;
Wherein, 77 parts by weight of composite particles, 23 parts by weight of decabromodiphenylethane;
(3) pentaerythritol triacrylate, high chlorinated polyethylene resin, polyurethane resin and methyl silicon resin are mixed, is added It in deionized water, stirs evenly, mixed liquor is made;
Wherein, 6 parts by weight of pentaerythritol triacrylate, 7 parts by weight of high chlorinated polyethylene resin, 4 parts by weight of polyurethane resin, 6 parts by weight of methyl silicon resin, 74 parts by weight of deionized water;
(4) addition coalescing agent, thickener, levelling agent, dispersing agent and defoaming agent into mixed liquor made from step (3), then plus Enter synergistic fire retardant made from step (2), stir evenly, grind, aqueous polyurethane anti-flaming dope is made;Coalescing agent is 2,2, 4- trimethyl -1,3- pentanediol mono isobutyrate;Thickener is carboxymethyl cellulose;Levelling agent is dimethyl silicone polymer;Point Powder is vinyl bis-stearamides;Defoaming agent is polyoxyethylene polyoxy propyl alcohol amidogen ether;
Wherein, 86 parts by weight of mixed liquor, 2 parts by weight of coalescing agent, 2 parts by weight of thickener, 1 parts by weight of levelling agent, 1 weight of dispersing agent Measure part, 2 parts by weight of defoaming agent, 6 parts by weight of synergistic fire retardant.
Water flame-proof paint made from embodiment 2, big plate combustion test test plate (panel) burn through time, combustion phenomena such as 1 institute of table Show.
Embodiment 3
(1) antimony is melted under 1MPa air pressure at 1200 DEG C and is clashed with high pressure draught and micron silicon lime stone powder, Grain surface deposits antimony oxide ultra-fine grain, and the composite particulate material with nucleocapsid structure is made;Antimony and micron silicon lime stone The mass ratio of powder is 1:3;
(2) composite particulate material made from step (1) is compounded with decabromodiphenylethane, the particle of antimony oxide cladding As the synergist of bromide fire retardant, the synergistic fire retardant of halogen-sb system is made;
Wherein, 73 parts by weight of composite particles, 27 parts by weight of decabromodiphenylethane;
(3) pentaerythritol triacrylate, high chlorinated polyethylene resin, polyurethane resin and methyl silicon resin are mixed, is added It in deionized water, stirs evenly, mixed liquor is made;
Wherein, 7 parts by weight of pentaerythritol triacrylate, 11 parts by weight of high chlorinated polyethylene resin, 5 weight of polyurethane resin Part, 9 parts by weight of methyl silicon resin, 68 parts by weight of deionized water;
(4) addition coalescing agent, thickener, levelling agent, dispersing agent and defoaming agent into mixed liquor made from step (3), then plus Enter synergistic fire retardant made from step (2), stir evenly, grind, aqueous polyurethane anti-flaming dope is made;Coalescing agent is 2,2, 4- trimethyl -1,3- pentanediol mono isobutyrate;Thickener is hydroxyethyl cellulose;Levelling agent is organic silicon modified by polyether oxygen Alkane;Dispersing agent is glyceryl tristearate;Defoaming agent is polypropylene glycerol aether;
Wherein, 82 parts by weight of mixed liquor, 4 parts by weight of coalescing agent, 2 parts by weight of thickener, 2 parts by weight of levelling agent, 1 weight of dispersing agent Measure part, 2 parts by weight of defoaming agent, 7 parts by weight of synergistic fire retardant.
Water flame-proof paint made from embodiment 3, big plate combustion test test plate (panel) burn through time, combustion phenomena such as 1 institute of table Show.
Embodiment 4
(1) antimony is melted under 1MPa air pressure at 1300 DEG C and is clashed with high pressure draught and micron silicon lime stone powder, Grain surface deposits antimony oxide ultra-fine grain, and the composite particulate material with nucleocapsid structure is made;Antimony and micron silicon lime stone The mass ratio of powder is 1:3;
(2) composite particulate material made from step (1) is compounded with decabromodiphenylethane, the particle of antimony oxide cladding As the synergist of bromide fire retardant, the synergistic fire retardant of halogen-sb system is made;
Wherein, 70 parts by weight of composite particles, 30 parts by weight of decabromodiphenylethane;
(3) pentaerythritol triacrylate, high chlorinated polyethylene resin, polyurethane resin and methyl silicon resin are mixed, is added It in deionized water, stirs evenly, mixed liquor is made;
Wherein, 8 parts by weight of pentaerythritol triacrylate, 12 parts by weight of high chlorinated polyethylene resin, 5 weight of polyurethane resin Part, 10 parts by weight of methyl silicon resin, 65 parts by weight of deionized water;
(4) addition coalescing agent, thickener, levelling agent, dispersing agent and defoaming agent into mixed liquor made from step (3), then plus Enter synergistic fire retardant made from step (2), stir evenly, grind, aqueous polyurethane anti-flaming dope is made;Coalescing agent is 2,2, 4- trimethyl -1,3- pentanediol mono isobutyrate;Thickener is hydroxypropyl cellulose;Levelling agent is polyester resin change properties of organic silicon oxygen Alkane;Dispersing agent is oleic acid acyl;Defoaming agent is polyoxyethylene polyoxypropylene pentaerythrite ether;
Wherein, 79 parts by weight of mixed liquor, 4 parts by weight of coalescing agent, 3 parts by weight of thickener, 2 parts by weight of levelling agent, 2 weight of dispersing agent Measure part, 2 parts by weight of defoaming agent, 8 parts by weight of synergistic fire retardant.
Water flame-proof paint made from embodiment 4, big plate combustion test test plate (panel) burn through time, combustion phenomena such as 1 institute of table Show.
Embodiment 5
(1) antimony is melted under 1MPa air pressure at 1300 DEG C and is clashed with high pressure draught and micron silicon lime stone powder, Grain surface deposits antimony oxide ultra-fine grain, and the composite particulate material with nucleocapsid structure is made;Antimony and micron silicon lime stone The mass ratio of powder is 1:3;
(2) composite particulate material made from step (1) is compounded with decabromodiphenylethane, the particle of antimony oxide cladding As the synergist of bromide fire retardant, the synergistic fire retardant of halogen-sb system is made;
Wherein, 80 parts by weight of composite particles, 20 parts by weight of decabromodiphenylethane;
(3) pentaerythritol triacrylate, high chlorinated polyethylene resin, polyurethane resin and methyl silicon resin are mixed, is added It in deionized water, stirs evenly, mixed liquor is made;
Wherein, 5 parts by weight of pentaerythritol triacrylate, 6 parts by weight of high chlorinated polyethylene resin, 3 parts by weight of polyurethane resin, 5 parts by weight of methyl silicon resin, 81 parts by weight of deionized water;
(4) addition coalescing agent, thickener, levelling agent, dispersing agent and defoaming agent into mixed liquor made from step (3), then plus Enter synergistic fire retardant made from step (2), stir evenly, grind, aqueous polyurethane anti-flaming dope is made;Coalescing agent is 2,2, 4- trimethyl -1,3- pentanediol mono isobutyrate;Thickener is methylcellulose;Levelling agent is polymethylphenylsiloxane;Point Powder is glyceryl monostearate;Defoaming agent is polyoxyethylene polyoxy propyl alcohol amidogen ether;
Wherein, 89 parts by weight of mixed liquor, 2 parts by weight of coalescing agent, 1 parts by weight of thickener, 1 parts by weight of levelling agent, 1 weight of dispersing agent Measure part, 1 parts by weight of defoaming agent, 5 parts by weight of synergistic fire retardant.
Water flame-proof paint made from embodiment 5, big plate combustion test test plate (panel) burn through time, combustion phenomena such as 1 institute of table Show.
Embodiment 6
(1) antimony is melted under 1MPa air pressure at 1300 DEG C and is clashed with high pressure draught and micron silicon lime stone powder, Grain surface deposits antimony oxide ultra-fine grain, and the composite particulate material with nucleocapsid structure is made;Antimony and micron silicon lime stone The mass ratio of powder is 1:3;
(2) composite particulate material made from step (1) is compounded with decabromodiphenylethane, the particle of antimony oxide cladding As the synergist of bromide fire retardant, the synergistic fire retardant of halogen-sb system is made;
Wherein, 75 parts by weight of composite particles, 25 parts by weight of decabromodiphenylethane;
(3) pentaerythritol triacrylate, high chlorinated polyethylene resin, polyurethane resin and methyl silicon resin are mixed, is added It in deionized water, stirs evenly, mixed liquor is made;
Wherein, 6 parts by weight of pentaerythritol triacrylate, 9 parts by weight of high chlorinated polyethylene resin, 4 parts by weight of polyurethane resin, 8 parts by weight of methyl silicon resin, 73 parts by weight of deionized water;
(4) addition coalescing agent, thickener, levelling agent, dispersing agent and defoaming agent into mixed liquor made from step (3), then plus Enter synergistic fire retardant made from step (2), stir evenly, grind, aqueous polyurethane anti-flaming dope is made;Coalescing agent is 2,2, 4- trimethyl -1,3- pentanediol mono isobutyrate;Thickener is carboxymethyl cellulose;Levelling agent is polyester resin change properties of organic silicon oxygen Alkane;Dispersing agent is vinyl bis-stearamides;Defoaming agent is polypropylene glycerol aether;
Wherein, 84 parts by weight of mixed liquor, 3 parts by weight of coalescing agent, 2 parts by weight of thickener, 1 parts by weight of levelling agent, 2 weight of dispersing agent Measure part, 2 parts by weight of defoaming agent, 6 parts by weight of synergistic fire retardant.
Water flame-proof paint made from embodiment 6, big plate combustion test test plate (panel) burn through time, combustion phenomena such as 1 institute of table Show.
Comparative example 1
Comparative example 1 does not use micron silicon lime stone powder granule to be loaded, but directly by antimony oxide ultra-fine grain It is compounded with decabromodiphenylethane, other conditions are same as Example 6, water flame-proof paint obtained, big plate burning examination It is as shown in table 1 to test test plate (panel) burn through time.
The test method of above-mentioned performance indicator are as follows:
Combustion testing is carried out referring to GB15442.2-1995, takes the plank with a thickness of 5mm, test plate (panel) having a size of 5mm × 10mm, it will be to Water flame-proof paint even application is surveyed on plank, average thickness 1mm is placed in 25 DEG C, adjusts under conditions of relative humidity 50% To constant mass, flammability test is carried out according to the big panel method in GB15442.2-1995, using alcolhol burner to test plate (panel) Calcination is carried out, using alcolhol burner flame flame envelope contact coating as standard, the time burnt with stopwatch record test plate (panel), and it is existing to observe burning As.
Table 1:
Performance indicator Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Comparative example 1
Big plate combustion test test plate (panel) burn through time (s) 545 565 556 558 562 564 404
Combustion phenomena A small amount of cigarette A small amount of cigarette A small amount of cigarette A small amount of cigarette A small amount of cigarette A small amount of cigarette Smoke amount is larger

Claims (10)

1. a kind of preparation method of aqueous polyurethane anti-flaming dope, which is characterized in that the detailed process of preparation are as follows:
(1) antimony is melted under 1MPa air pressure at 1000-1300 DEG C and is clashed with high pressure draught and micron silicon lime stone powder, Antimony oxide ultra-fine grain is deposited in particle surface, the composite particulate material with nucleocapsid structure is made;Antimony and micron silicon The mass ratio of lime stone powder is 1:3;
(2) composite particulate material made from step (1) is compounded with decabromodiphenylethane, the collaboration of halogen-sb system is made Fire retardant;
(3) pentaerythritol triacrylate, high chlorinated polyethylene resin, polyurethane resin and methyl silicon resin are mixed, is added It in deionized water, stirs evenly, mixed liquor is made;
(4) addition coalescing agent, thickener, levelling agent, dispersing agent and defoaming agent into mixed liquor made from step (3), then plus Enter synergistic fire retardant made from step (2), stir evenly, grind, aqueous polyurethane anti-flaming dope is made.
2. a kind of preparation method of aqueous polyurethane anti-flaming dope according to claim 1, it is characterised in that: in step (2), Composite particulate material 70-80 parts by weight, 20 ~ 30 parts by weight of decabromodiphenylethane.
3. a kind of preparation method of aqueous polyurethane anti-flaming dope according to claim 1, it is characterised in that: in step (3), 5 ~ 8 parts by weight of pentaerythritol triacrylate, 6 ~ 12 parts by weight of high chlorinated polyethylene resin, 3 ~ 5 parts by weight of polyurethane resin, first 5 ~ 10 parts by weight of base silicone resin, 65 ~ 81 parts by weight of deionized water.
4. a kind of preparation method of aqueous polyurethane anti-flaming dope according to claim 1, it is characterised in that: in step (4), 79 ~ 89 parts by weight of mixed liquor, 2 ~ 4 parts by weight of coalescing agent, 1 ~ 3 parts by weight of thickener, 1 ~ 2 parts by weight of levelling agent, dispersing agent 1 ~ 2 Parts by weight, 1 ~ 2 parts by weight of defoaming agent, 5 ~ 8 parts by weight of synergistic fire retardant.
5. a kind of preparation method of aqueous polyurethane anti-flaming dope according to claim 1, it is characterised in that: step (4) institute Stating coalescing agent is 2,2,4- trimethyl -1,3- pentanediol mono isobutyrate.
6. a kind of preparation method of aqueous polyurethane anti-flaming dope according to claim 1, it is characterised in that: step (4) institute Stating thickener is at least one of methylcellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose.
7. a kind of preparation method of aqueous polyurethane anti-flaming dope according to claim 1, it is characterised in that: step (4) institute Stating levelling agent is polymethylphenylsiloxane, dimethyl silicone polymer, organic silicon modified by polyether oxygen alkane, polyester resin change properties of organic silicon oxygen At least one of alkane.
8. a kind of preparation method of aqueous polyurethane anti-flaming dope according to claim 1, it is characterised in that: step (4) institute Stating dispersing agent is at least one of glyceryl monostearate, vinyl bis-stearamides, glyceryl tristearate, oleic acid acyl.
9. a kind of preparation method of aqueous polyurethane anti-flaming dope according to claim 1, it is characterised in that: step (4) institute Defoaming agent is stated as in polyoxyethylene polyoxypropylene pentaerythrite ether, polyoxyethylene polyoxy propyl alcohol amidogen ether, polypropylene glycerol aether It is at least one.
10. a kind of aqueous polyurethane anti-flaming dope that any one of claim 1 ~ 9 the method is prepared.
CN201811118645.XA 2018-09-26 2018-09-26 A kind of aqueous polyurethane anti-flaming dope and preparation method Withdrawn CN109337421A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113308014A (en) * 2021-06-07 2021-08-27 安徽杰蓝特新材料有限公司 Double-wall corrugated pipe with good flame retardance and preparation method thereof
CN114015269A (en) * 2021-11-25 2022-02-08 称意科技研发园(江苏)有限公司 Environment-friendly flame-retardant coating and preparation method thereof
CN115109315A (en) * 2022-06-22 2022-09-27 中国科学院福建物质结构研究所 A kind of spray-type core-shell structure flame retardant and its preparation method and application

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113308014A (en) * 2021-06-07 2021-08-27 安徽杰蓝特新材料有限公司 Double-wall corrugated pipe with good flame retardance and preparation method thereof
CN114015269A (en) * 2021-11-25 2022-02-08 称意科技研发园(江苏)有限公司 Environment-friendly flame-retardant coating and preparation method thereof
CN115109315A (en) * 2022-06-22 2022-09-27 中国科学院福建物质结构研究所 A kind of spray-type core-shell structure flame retardant and its preparation method and application

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Application publication date: 20190215