CN102241942A - Poly(propylene carbonate)-based polyurethane fireproof coating and preparation method thereof - Google Patents
Poly(propylene carbonate)-based polyurethane fireproof coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a poly(propylene carbonate)-based polyurethane fireproof coating and a preparation method thereof. The poly(propylene carbonate)-based polyurethane fireproof coating is prepared from 100 parts of poly(propylene carbonate) which is the polymer of carbon dioxide and propylene oxide, 15-30 parts of aromatic diisocyanate, 0.1-0.2 part of catalyst, 0-3 parts of non-ionic chain extender containing active hydrogen, 2-8 parts of active-hydrogen-containing ionic chain extender capable of forming a hydrophilic group, 1-6 parts of neutralizer, 1-10 parts of silane coupling agent, 200-350 parts of adjuvant, 40-140 parts of flame retardant, 10-50 parts of bentonite and 1-3 parts of dispersant. The fireproof coating has the advantages of good water resistance, strong adhesion force, flame retardance reaching one level, superior fireproof performance, strong integrated application capability and bright application prospect, and can be applied to the surface coating of wood, steel and other substrates.
Description
Technical field
The present invention relates to polytrimethylene carbonate aqueous polyurethane frie retardant coating and preparation method thereof, belong to field of fine chemical.
Technical background
Frie retardant coating is meant to be coated with and is contained in body surface, can prevent that fire from taking place, and stops fire spreading to be propagated or the isolation burning things which may cause a fire disaster, prolongs base material ignition time or increases heat-insulating property to postpone the class coating of structure deteriorate time.Along with science and technology development, industry to maximize and building to the development of clustered, high stratification, the application of frie retardant coating more and more widely, people are also more and more higher to its requirement, frie retardant coating can have more wide Application Areas and development prospect.
Can be divided into the different frie retardant coatings that use object by purposes: finishing fire retardant paint, cable fire-refractory coating, steel structure fire-proof paint etc.Perfect day by day at environmental regulation, today of people's environmental pollution and health of human body pay attention to day by day, the use of solvent based coating is subjected to more and more stricter restriction, so the exploitation aqueous fire-proof coating has great importance.
Aqueous fire-proof coating on the China market can be divided into following a few class based on finishing fire retardant paint and thick-slurry type frie retardant coating in nature substantially from film forming matter at present:
(1) polymer emulsion type, film forming matter are benzene emulsion, pure-acrylic emulsion, acetate emulsion etc., add expansion type flame retardant and other materials and make.This type of coating is used at present comparatively extensive, but water-borne coatings has been compared tangible deficiency with solvent based coating at aspects such as water tolerance, sticking power.
(2) water soluble resin type, wherein urea aldehyde-melamine resin is more representative, and it is good that it has over-all properties, and this resinoid is good through adding the fire retardant fire resistance, but be difficult to satisfy environmental requirement because its formaldehyde content is higher, so its development prospect is not expected.
(3) inorganic bond formulation, this class coating is base-material with silicate cement, magnesium hydroxide or other inorganic high-temp tackiness agents, add pearlstone, mineral wool and compositions such as other chemical assistants and water, based on non-expansion type, its shortcoming is that consumption is big, thick coating, and the physicochemical property of the coating deficiency that exists some to be difficult to overcome, its application is restricted.
Polyurethane coating has superior physical and mechanical properties, but its limited oxygen index low only be 17.3% to belong to combustible material, so it is big to develop polyurethane fireproof coating relative difficulty, polyurethane fireproof coating proportion is very low in the market.Has crucial value and significance so develop high performance aqueous polyurethane frie retardant coating.
Summary of the invention
The objective of the invention is to an object of the present invention is to provide a kind of in order to overcome the defective that above-mentioned prior art exists
Water-tolerant, strong adhesion, the polytrimethylene carbonate aqueous polyurethane frie retardant coating that fire resistance is superior, this coating comprises following component and mass fraction:
100 parts of poly (propylene carbonate) polyvalent alcohols
15～30 parts of vulcabond
0.1～0.2 part of catalyzer
0～3 part of nonionic chainextender
2～8 parts of ionic chainextenders
1～6 part of neutralizing agent
1～10 part of silane coupling agent
200～350 parts of auxiliary agents
40～140 parts of fire retardants
10～50 parts of calcium-base bentonites
1～3 part of dispersion agent IW.
Wherein, described poly (propylene carbonate) polyvalent alcohol is the poly (propylene carbonate) dibasic alcohol;
Described vulcabond comprises tolylene diisocyanate TDI, 4, any one among 4 '-diphenylmethanediisocyanate MDI, isophorone diisocyanate IPDI, hexamethylene diisocyanate HDI, the dicyclohexyl methane diisocyanate HMDI;
Described catalyzer be dibutyl tin laurate;
Described nonionic chainextender comprises 1,4-butyleneglycol, 1, any one in 6-hexylene glycol, quadrol, the diethylenetriamine;
Described ionic chainextender comprises dimethylol propionic acid or 1,2-dihydroxyl-3-N-morpholinopropanesulfonic acid;
Described neutralizing agent comprises triethylamine or ammoniacal liquor;
Described silane coupling agent comprises γ-An Bingjisanyiyangjiguiwan KH-550, N-β-ammonia any one among base-γ-aminopropyl methyl dimethoxysilane 602, the 3-glycidyl ether oxygen base propyl trimethoxy silicane KH-560;
Described auxiliary agent comprises organic solvent and deionized water, and described organic solvent comprises acetone or N methyl-2-pyrrolidone;
Described fire retardant comprises ammonium polyphosphate, trimeric cyanamide and tetramethylolmethane, and the ratio of three's quality is 2:1:1.
Another object of the present invention provides a kind of preparation method of polytrimethylene carbonate aqueous polyurethane frie retardant coating, and this method may further comprise the steps:
(1) Synthesis of Waterborne Polyurethane
(1) add the poly (propylene carbonate) polyvalent alcohol that measures in reactor, 100 ℃ vacuumize dehydration 30～60min, are cooled to 40 ℃;
(2) add ionic chainextender and the catalyzer that measures in reactor, logical nitrogen protection is warming up to 60 ℃ after stirring;
(3) add the vulcabond that measures in reactor, controlled temperature is 60～80
oC reacted 1～4 hour;
(4) add the non-ionic type chainextender that measures in reactor, controlled temperature is 65～85
oC reacted 1～3 hour;
(5) be cooled to room temperature, in reactor, add the silane coupling agent reaction 15～45min of metering;
(6) add the neutralizing agent stirring and emulsifying 15min that measures in reactor, add proper amount of deionized water and carry out violent stirring emulsification 10min, control emulsion solid content is 30～50%, and the adjusting ph value of emulsion is 7～8;
(7) discharging obtains the polytrimethylene carbonate aqueous polyurethane emulsion;
(2) preparation of frie retardant coating
(8) in the emulsification still, add proper amount of deionized water, be warming up to 50～70 ℃;
(9) in the emulsification still, add fire retardant, calcium-base bentonite, the dispersion agent IW that measures, stir 15～45min;
(10) in the emulsification still, add the above-mentioned polytrimethylene carbonate aqueous polyurethane emulsion that makes, stir 30～60min down for 50～70 ℃ in temperature;
(11) above-mentioned system is changed over to emulsification pretreatment machine or shredder and handle 45-75min;
(12) discharging is packaged to be polytrimethylene carbonate aqueous polyurethane frie retardant coating.
The present invention adopts and meets that fire is high to become the carbonic acid gas of carbon and the polymerisate poly (propylene carbonate) polyvalent alcohol of propylene oxide to prepare aqueous polyurethane coating, and adds the fire retardant preparation and have the superior polytrimethylene carbonate aqueous polyurethane frie retardant coating of fire resistance.Texacar PC base water polyurethane coating hydrolytic resistance is relatively poor, introducing the ammonium polyphosphate expansion type flame retardant in coating can cause the water resistance of frie retardant coating sharply to descend, after the aqueous polyurethane frie retardant coating is coated on the sheet glass oven dry film forming, 5 hours violent swellings of soaking at room temperature and split away off in water from sheet glass.Adopt γ-An Bingjisanyiyangjiguiwan KH-550, N-β-ammonia base-γ-silane coupling agents such as aminopropyl methyl dimethoxysilane 602 to the modification of polytrimethylene carbonate aqueous polyurethane or piece together to mix and use, significantly improve the hydrolytic resistance of product, prepared aqueous polyurethane frie retardant coating has excellent water tolerance: after the aqueous polyurethane frie retardant coating is coated in oven dry film forming on glass, in water, soak 72h, do not have obvious swelling, bounding force does not have considerable change.The big panel method test shows, this aqueous polyurethane frie retardant coating flame retardant resistance reaches one-level.The polytrimethylene carbonate aqueous polyurethane frie retardant coating that adopts the present invention to prepare is applied to the external coating of base materials such as timber, steel construction, and the integrated application performance is good.
Embodiment
Embodiment 1
(1) Synthesis of Waterborne Polyurethane
(1) the poly (propylene carbonate) dibasic alcohol with 100g molecular weight 3500 adds in the reactor, and 100 ℃ vacuumize dehydration 40min, are cooled to 40 ℃;
(2) 6g dimethylol propionic acid and 0.2g catalyzer dibutyl tin laurate are added under protection of nitrogen gas in the reactor, after stirring, be warming up to 60 ℃;
(3) add 20g tolylene diisocyanate TDI in reactor, reactor is warming up to 70 ℃, and insulation reaction 3 hours, reaction process can be replenished the viscosity of 15g acetone conditioned reaction system according to the viscosity of reaction system;
(4) in reactor, add 1 of 2g, the 4-chain expansion of succinic acid, reactor is warming up to 80
oC, insulation reaction 2 hours;
(5) be cooled to room temperature, in reactor, add the γ-An Bingjisanyiyangjiguiwan KH-550 reaction 30min of 5.2g;
(6) add the 3g triethylamine aqueous solution in reactor and carry out stirring and emulsifying 15min, add 200g deionized water violent stirring emulsification 10min again, control emulsion solid content is 30-50%, and the adjusting ph value of emulsion is 7-8;
(7) discharging obtains the polytrimethylene carbonate aqueous polyurethane emulsion;
(2) preparation of frie retardant coating
(8) in the emulsification still, add the 100g deionized water, be warming up to 60 ℃;
(9) in the emulsification still, add the 100g fire retardant, fire retardant comprises ammonium polyphosphate, trimeric cyanamide and tetramethylolmethane, and the ratio of three's quality is 2:1:1, the polymerization degree 1000 of ammonium polyphosphate, in the emulsification still, add 2g dispersion agent IW and 20g calcium-base bentonite, stir 30min;
(10) add the polytrimethylene carbonate aqueous polyurethane emulsion that step (7) obtains in the emulsification still, 60 ℃ are stirred 40min;
(11) step (10) gained system is changed over to the emulsification pretreatment machine and shear 60min;
(12) discharging, packing obtains polytrimethylene carbonate aqueous polyurethane frie retardant coating.
Embodiment 2
(1) Synthesis of Waterborne Polyurethane
(1) the poly (propylene carbonate) dibasic alcohol with 100g molecular weight 3500 adds in the reactor, and 100 ℃ vacuumize dehydration 60min, are cooled to 40 ℃;
(2) 8g dimethylol propionic acid and 0.2g catalyzer dibutyl tin laurate are added under protection of nitrogen gas in the reactor, after stirring, be warming up to 60 ℃;
(3) add 4 of 30g in reactor, 4 '-diphenylmethanediisocyanate MDI, reactor are warming up to 80 ℃, and insulation reaction 4 hours, reaction process can be replenished the viscosity of the N methyl-2-pyrrolidone conditioned reaction system of 20g according to the viscosity of reaction system;
(4) in reactor, add 1 of 3g, 6-hexylene glycol chain extension, reactor is warming up to 85
oC, insulation reaction 3 hours;
(5) be cooled to room temperature, the N-β-ammonia that adds 10g in reactor is base-γ-aminopropyl methyl dimethoxysilane 602 reaction 45min;
(6) add the 6g triethylamine aqueous solution in reactor and carry out stirring and emulsifying 15min, add 200g deionized water violent stirring emulsification 10min again, control emulsion solid content is 30-50%, and the adjusting ph value of emulsion is 7-8;
(7) discharging obtains the polytrimethylene carbonate aqueous polyurethane emulsion;
(2) preparation of frie retardant coating
(8) in the emulsification still, add the 130g deionized water, be warming up to 70 ℃;
(9) add the 140g fire retardant in the emulsification still, fire retardant comprises ammonium polyphosphate, trimeric cyanamide and tetramethylolmethane, and the ratio of three's quality is 2:1:1; In the emulsification still, add 3g dispersion agent IW and 50g calcium-base bentonite, stir 45min;
(10) add the polytrimethylene carbonate aqueous polyurethane emulsion that step (7) obtains in the emulsification still, 70 ℃ are stirred 60min;
(11) step (10) gained system is changed over to the emulsification pretreatment machine and shear 75min;
(12) discharging, packing obtains polytrimethylene carbonate aqueous polyurethane frie retardant coating.
Embodiment 3
(1) Synthesis of Waterborne Polyurethane
(1) the poly (propylene carbonate) dibasic alcohol with 100g molecular weight 3500 adds in the reactor, and 100 ℃ vacuumize dehydration 30min, are cooled to 40 ℃;
(2) with 1 of 2g, 2-dihydroxyl-3-N-morpholinopropanesulfonic acid and 0.1g catalyzer dibutyl tin laurate add under protection of nitrogen gas in the reactor, after stirring, are warming up to 60 ℃;
(3) add 15g isophorone diisocyanate IPDI in reactor, reactor is warming up to 60 ℃, and insulation reaction 1 hour, reaction process can be replenished the viscosity of 10g acetone conditioned reaction system according to the viscosity of reaction system;
(4) the quadrol chain extension of adding 1g in reactor, reactor is warming up to 65
oC, insulation reaction 1 hour;
(5) be cooled to room temperature, in reactor, add the 3-glycidyl ether oxygen base propyl trimethoxy silicane KH-560 reaction 15min of 1g;
(6) add 1g ammoniacal liquor in reactor and carry out stirring and emulsifying 15min, add 120g deionized water violent stirring emulsification 10min again, control emulsion solid content is 30-50%, and the adjusting ph value of emulsion is 7-8;
(7) discharging obtains the polytrimethylene carbonate aqueous polyurethane emulsion;
(2) preparation of frie retardant coating
(8) in the emulsification still, add the 70g deionized water, be warming up to 50 ℃;
(9) add the 40g fire retardant in the emulsification still, fire retardant comprises ammonium polyphosphate, trimeric cyanamide and tetramethylolmethane, and the ratio of three's quality is 2:1:1; In the emulsification still, add 1g dispersion agent IW and 10g calcium-base bentonite, stir 15min;
(10) add the polytrimethylene carbonate aqueous polyurethane emulsion that step (7) obtains in the emulsification still, 50 ℃ are stirred 30min;
(11) step (10) gained system is changed over to the emulsification pretreatment machine and shear 45min;
(12) discharging, packing obtains polytrimethylene carbonate aqueous polyurethane frie retardant coating.
Embodiment 4
(1) Synthesis of Waterborne Polyurethane
(1) the poly (propylene carbonate) dibasic alcohol with 100g molecular weight 3500 adds in the reactor, and 100 ℃ vacuumize dehydration 60min, are cooled to 40 ℃;
(2) 6g dimethylol propionic acid and 0.2g catalyzer dibutyl tin laurate are added under protection of nitrogen gas in the reactor, after stirring, be warming up to 60 ℃;
(3) the hexamethylene diisocyanate HDI of adding 20g in reactor, reactor is warming up to 70 ℃, and insulation reaction 3 hours, reaction process can be replenished the viscosity of 15g acetone conditioned reaction system according to the viscosity of reaction system;
(4) the diethylenetriamine chain extension of adding 2g in reactor, reactor is warming up to 80
oC, insulation reaction 2 hours;
(5) be cooled to room temperature, in reactor, add the γ-An Bingjisanyiyangjiguiwan KH-550 reaction 30min of 5.2g;
(6) add the 3g triethylamine aqueous solution in reactor and carry out stirring and emulsifying 15min, add 200g deionized water violent stirring emulsification 10min again, control emulsion solid content is 30-50%, and the adjusting ph value of emulsion is 7-8;
(7) discharging obtains the polytrimethylene carbonate aqueous polyurethane emulsion;
(2) preparation of frie retardant coating
(8) in the emulsification still, add the 100g deionized water, be warming up to 60 ℃;
(9) in the emulsification still, add the 100g fire retardant, fire retardant comprises ammonium polyphosphate, trimeric cyanamide and tetramethylolmethane, and the ratio of three's quality is 2:1:1, the polymerization degree 1000 of ammonium polyphosphate, in the emulsification still, add 2g dispersion agent IW and 20g calcium-base bentonite, stir 30min;
(10) add the polytrimethylene carbonate aqueous polyurethane emulsion that step (7) obtains in the emulsification still, 60 ℃ are stirred 30min;
(11) step (10) gained system is changed over to the emulsification pretreatment machine and shear 75min;
(12) discharging, packing obtains polytrimethylene carbonate aqueous polyurethane frie retardant coating.
Claims (10)
1. polytrimethylene carbonate aqueous polyurethane frie retardant coating, this coating comprises following component and mass fraction:
100 parts of poly (propylene carbonate) polyvalent alcohols
15～30 parts of vulcabond
0.1～0.2 part of catalyzer
0～3 part of nonionic chainextender
2～8 parts of ionic chainextenders
1～6 part of neutralizing agent
1～10 part of silane coupling agent
200～350 parts of auxiliary agents
40～140 parts of fire retardants
10～50 parts of wilkinites
1～3 part of dispersion agent.
2. a kind of polytrimethylene carbonate aqueous polyurethane frie retardant coating according to claim 1, it is characterized in that: described poly (propylene carbonate) polyvalent alcohol is the poly (propylene carbonate) dibasic alcohol.
3. a kind of polytrimethylene carbonate aqueous polyurethane frie retardant coating according to claim 1, it is characterized in that: described vulcabond comprises tolylene diisocyanate TDI, 4, among 4 '-diphenylmethanediisocyanate MDI, isophorone diisocyanate IPDI, hexamethylene diisocyanate HDI, the dicyclohexyl methane diisocyanate HMDI any one.
4. a kind of polytrimethylene carbonate aqueous polyurethane frie retardant coating according to claim 1, it is characterized in that: described catalyzer is a dibutyl tin laurate.
5. a kind of polytrimethylene carbonate aqueous polyurethane frie retardant coating according to claim 1, it is characterized in that: described nonionic chainextender comprises 1,4-butyleneglycol, 1, any one in 6-hexylene glycol, quadrol, the diethylenetriamine; Described ionic chainextender comprises dimethylol propionic acid or 1,2-dihydroxyl-3-N-morpholinopropanesulfonic acid.
6. a kind of polytrimethylene carbonate aqueous polyurethane frie retardant coating according to claim 1, it is characterized in that: described neutralizing agent comprises triethylamine or ammoniacal liquor.
7. a kind of polytrimethylene carbonate aqueous polyurethane frie retardant coating according to claim 1 is characterized in that: described silane coupling agent comprises γ-An Bingjisanyiyangjiguiwan KH-550, N-β-ammonia any one among base-γ-aminopropyl methyl dimethoxysilane 602, the 3-glycidyl ether oxygen base propyl trimethoxy silicane KH-560.
8. a kind of polytrimethylene carbonate aqueous polyurethane frie retardant coating according to claim 1, it is characterized in that: described auxiliary agent comprises organic solvent and deionized water, described organic solvent comprises acetone or N methyl-2-pyrrolidone.
9. a kind of polytrimethylene carbonate aqueous polyurethane frie retardant coating according to claim 1, it is characterized in that: described fire retardant comprises ammonium polyphosphate, trimeric cyanamide and tetramethylolmethane, the ratio of three's quality is 2:1:1.
10. the preparation method of a polytrimethylene carbonate aqueous polyurethane frie retardant coating is characterized in that, this method may further comprise the steps:
(1) Synthesis of Waterborne Polyurethane
(1) add the poly (propylene carbonate) polyvalent alcohol that measures in reactor, 100 ℃ vacuumize dehydration 30～60min, are cooled to 40 ℃;
(2) add ionic chainextender and the catalyzer that measures in reactor, logical nitrogen protection is warming up to 60 ℃ after stirring;
(3) add the vulcabond that measures in reactor, controlled temperature is 60～80oC, reacts 1～4 hour;
(4) add the non-ionic type chainextender that measures in reactor, controlled temperature is 65～85oC, reacts 1～3 hour;
(5) be cooled to room temperature, in reactor, add the silane coupling agent reaction 15～45min of metering;
(6) add the neutralizing agent stirring and emulsifying 15min that measures in reactor, add proper amount of deionized water and carry out violent stirring emulsification 10min, control emulsion solid content is 30～50%, and the adjusting ph value of emulsion is 7～8;
(7) discharging obtains the polytrimethylene carbonate aqueous polyurethane emulsion;
(2) preparation of frie retardant coating
(8) in the emulsification still, add proper amount of deionized water, be warming up to 50～70 ℃;
(9) in the emulsification still, add fire retardant, calcium-base bentonite, the dispersion agent IW that measures, stir 15～45min;
(10) in the emulsification still, add the above-mentioned polytrimethylene carbonate aqueous polyurethane emulsion that makes, stir 30～60min down for 50～70 ℃ in temperature;
(11) above-mentioned system is changed over to emulsification pretreatment machine or shredder and handle 45-75min;
(12) discharging is packaged to be polytrimethylene carbonate aqueous polyurethane frie retardant coating.
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