CN105238245A - Epoxy resin modified waterborne polyurethane flame retardant paint and preparation method thereof - Google Patents
Epoxy resin modified waterborne polyurethane flame retardant paint and preparation method thereof Download PDFInfo
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- CN105238245A CN105238245A CN201510667076.4A CN201510667076A CN105238245A CN 105238245 A CN105238245 A CN 105238245A CN 201510667076 A CN201510667076 A CN 201510667076A CN 105238245 A CN105238245 A CN 105238245A
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- epoxy resin
- aqueous polyurethane
- flaming dope
- resin modification
- diisocyanate
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Abstract
The invention relates to an epoxy resin modified waterborne polyurethane flame retardant paint, which is prepared from the following components by weight percentage: 25-35wt% of a waterborne polyurethane emulsion, 20-28wt% of a flame retardant, 15-23wt% of alcohol, and 20-34wt% of deionized water. The waterborne polyurethane flame retardant paint provided by the invention has the advantages of high film hardness and good water resistance, long fire resistance period, small smoke amount, good flame retardancy, no toxicity and no harm.
Description
Technical field
The present invention relates to chemical technology field, aqueous polyurethane anti-flaming dope being specifically related to a kind of epoxy resin modification and preparation method thereof.
Background technology
In China in recent ten years, every year on average because the catch fire fire that causes of buildings just about has 3 ~ 40,000, about death toll reaches 3,000 people, fire losses is more than 200,000,000 yuan.Therefore research and development have the significant and huge market outlook of flame retardant resistance coating.
Anti-flaming dope refers to that brushing is at substrate surface, stops propagation of flame to be propagated or isolation burning things which may cause a fire disaster, reduces by the combustibility being coated with material surface, stop the rapid spread of fire, improve a kind of functional coating of fire endurance.Anti-flaming dope comprises two portions: base-material and fire retardant matter.Divide by its fire prevention form and composition, non-expansion type and the large class of expanded polystyrene veneer two can be divided into.Current domestic and international the most widely used anti-flaming dope is intumescent paints; when having flame and high temperature; the cellular charring layer of nonflammable black of more dozens or even hundreds of than former thick coating times can be produced, effectively can completely cut off thermal source and enter the effect that protection base material is played in film inside further.Meanwhile, produce non-flammable gases, that reduce inflammable gas as gases such as carbonic acid gas, ammonia and water vapors with concentration that is oxygen in air, thus play fire prevention, fire retardation.It forms primarily of filmogen (resin binder), dehydration catalyst, char-forming agent, whipping agent, color stuffing, auxiliary agent and dispersion medium.And the intumescent paints of water-based and oiliness can be divided into by filmogen.
Compare the intumescent paints of oiliness, the intumescent paints of water-based is dispersion medium with water, has low VOC, nontoxic, safe, energy-conservation effect.Aqueous polyurethane has the performances such as levelling, good film-forming property, weather-proof, wear-resisting and snappiness, therefore selects urethane as the base-material of the intumescent paints of water-based.We select self-produced height to become the polypropylene carbonate esterdiol of carbon as the raw material of synthesis aqueous polyurethane, and himself oxygen index is conducive to the lifting of flame retardant effect at 24-26%.Compare oiliness urethane resin, in use still there is the shortcomings such as hardness of film is lower, surface gloss is not high, not water-fast in aqueous polyurethane, needs to carry out modification to it.We select epoxy resin and waterborne polyurethane prepolymer to carry out modification by copolymerization, are intended to improve its hardness, solvent resistant and water resistance.And for fire retardant, select ammonium polyphosphate as dewatering agent, trimeric cyanamide as whipping agent and tetramethylolmethane as carbon source, by the blended aqueous polyurethane anti-flaming dope preparing epoxy resin modification of epoxy resin modified water-based polyurethane emulsion of these fire retardants and synthesis.
Summary of the invention
Aqueous polyurethane anti-flaming dope that the invention provides a kind of epoxy resin modification and preparation method thereof, the hardness of film it solving aqueous polyurethane anti-flaming dope is lower, surface gloss is not high, the technical problem such as not water-fast, and it has fire resistance period length, good flame resistance, the advantage such as nontoxic, safe, energy-conservation.
An aqueous polyurethane anti-flaming dope for epoxy resin modification, it presses following weight percentage than formulated by following component:
Described aqueous polyurethane emulsion presses following weight percentage than formulated by following component:
Further, described hydrophilic chain extender is the one of the two hydroxymethyl propionic acid of second diamino sulfonic acid sodium (X506), adipic dihydrazide (ADH) or 2,2-.
Described hydrophilic chain extender is 2,2-two hydroxymethyl propionic acids preferably.
Further, described vulcabond is aromatic diisocyanate, aliphatic diisocyanate, alicyclic diisocyanate, tolylene diisocyanate (TDI), 4,4-diphenylmethanediisocyanates (MDI), vulcabond have one in isophorone diisocyanate (IPDI), hexamethylene diisocyanate (HDI).
The preferred hexamethylene diisocyanate of described isocyanate monomers (HDI).
Further, described small molecule chain extender is dibasic alcohol or diamine.Described dibasic alcohol is ethylene glycol, butyleneglycol, and described diamine is the one in quadrol, butanediamine.
The preferred butyleneglycol of described small molecule chain extender.
Further, described neutralizing agent is the one in triethylamine, ammoniacal liquor or sodium hydroxide.
The preferred triethylamine of described neutralizing agent.
Further, described epoxy resin is glycidyl ether or ethylene oxidic ester epoxy resin.
The preferred E-51 of described epoxy resin, 711 or TDE-85 in a kind of.
The preferred E-44 of described epoxy resin.
Further, described aqueous polyurethane emulsion is prepared as follows:
Agitator, thermometer, condensing works are being housed and are being connected with in five mouthfuls of flasks of nitrogen protection, add 7.5-17.5wt% polypropylene carbonate esterdiol, 50-60 DEG C is heated under stir speed (S.S.) is 300-500rmp, then 1-5wt% hydrophilic chain extender and 0.1-0.5wt% dibutyl tin laurate and 14-24.4wt% vulcabond is added, then 70-85 DEG C is warming up to, reaction 1.5-3h, slowly add the small molecule chain extender of 2-8wt%, keep 70-85 DEG C, reaction 0.5-1h, add 2-6wt% epoxy resin afterwards, keep 70-85 DEG C to react 0.5-1h; Be down to room temperature afterwards, with 15-30min by the neutralizing agent of 1-5wt% instillation reaction system, then add the water of 45-53wt% and the acetone of 2-6wt%, raise stir speed (S.S.) to 1000-1500rmp, stir 0.5-1h, last vacuum subtracts steaming and pumps acetone.
Further, described fire retardant by ammonium polyphosphate, trimeric cyanamide and tetramethylolmethane in mass ratio for 3-6:1-3:2-1 mixes.
A kind of preparation method of aqueous polyurethane anti-flaming dope of epoxy resin modification, it is characterized in that, comprise the following steps: in room temperature, stir speed (S.S.) is under 300-500rmp, fire retardant 20-28wt% is added in a mixing bowl, water 20-34wt% and alcohol 15-23wt%, after abundant stirring 30min-60min, again described aqueous polyurethane emulsion 25-35wt% is slowly joined in above-mentioned reaction system, then stir speed (S.S.) is raised to 1000-1500rmp, stir 50-70min, finally use emulsification pretreatment instrument emulsification 50-70min, obtained epoxy modified aqueous polyurethane flame-proof coating.
Principle of the present invention: utilize into the high poly (propylene carbonate) glycol of carbon value and isocyanate reaction, obtain polyurethane prepolymer, after prepare epoxide modified aqueous polyurethane emulsion through epoxy resin modification and neutralization reaction, by blended for the Intumscent Flame Retardant System formed with ammonium polyphosphate, trimeric cyanamide, tetramethylolmethane three in the aqueous polyurethane emulsion of synthesis, the aqueous polyurethane anti-flaming dope of obtained epoxy resin modification.
Advantage of the present invention is: not only hardness of film is high for aqueous polyurethane anti-flaming dope of the present invention, water-tolerant, and its fire resistance period is long, the amount of being fuming is few, good flame resistance, nontoxic.
Embodiment:
Below in conjunction with specific embodiment, the present invention will be further described.Each raw material in following examples is all commercially available raw materials, except aqueous polyurethane emulsion is prepared according to method of the present invention.
Embodiment 1
1, the synthesis of epoxy resin modified aqueous polyurethane
Agitator is being housed, thermometer, condensing works and be connected with in five mouthfuls of flasks of nitrogen protection, add pretreated 7.5wt% polypropylene carbonate esterdiol, stirring is warming up to 50 DEG C, add 2wt% second diamino sulfonic acid sodium chainextender and 0.1wt% catalyst dibutyltin dilaurylate and 24.4wt% tolylene diisocyanate, after being warming up to 70 DEG C of reaction 1.5h, slowly add the ethylene glycol extender compounds of the quantitative 2wt% of meter, 80 DEG C are kept to react 0.5h, proceed to chain extension stage in reaction and complete a half, add meter 6wt% epoxy resin E-51, 70 DEG C are kept to react 0.5h, be down to room temperature afterwards, drip 3wt% ammoniacal liquor to neutralize, the acetone that titration time controls the water and 2wt% adding 53wt% after 15min in prepolymer carries out emulsification, violent stirring 30min, vacuum subtracts steaming and pumps acetone, obtained epoxy resin modified aqueous polyurethane coating.
2, the preparation of the aqueous polyurethane anti-flaming dope of epoxy resin modification
Preparation technology's formula of extinguishing waterborn polyurethane coating adhesive
Concrete technology is: in a mixing bowl, add meter quantitative fire retardant, water and alcohol, after abundant stirring 30min, the more quantitative aqueous polyurethane coating of meter is slowly added, violent stirring 50min, finally use emulsification pretreatment instrument emulsification 50min again, obtained epoxy modified aqueous polyurethane flame-proof coating.
Embodiment 2
1, the synthesis of epoxy resin modified aqueous polyurethane
Agitator is being housed, thermometer, condensing works and be connected with in five mouthfuls of flasks of nitrogen protection, add pretreated 17.5wt% polypropylene carbonate esterdiol, stirring is warming up to 55 DEG C, add 4 of 1wt% adipic dihydrazide chainextender and 0.5wt% catalyst dibutyltin dilaurylate and 14wt%, 4-diphenylmethanediisocyanate, after being warming up to 80 DEG C of reaction 3h, slowly add the chain expansion of succinic acid immunomodulator compounds of the quantitative 8wt% of meter, 70 DEG C are kept to react 0.8h, proceed to chain extension stage in reaction and complete a half, add 4wt% epoxy resin 711, 80 DEG C are kept to react 1h, be down to room temperature afterwards, drip 1wt% triethylamine to neutralize, the acetone that titration time controls the water and 5wt% adding 49wt% after 20 min in prepolymer carries out emulsification, violent stirring 30min, vacuum subtracts steaming and pumps acetone, obtained epoxy resin modified aqueous polyurethane coating.
2, the preparation of the aqueous polyurethane anti-flaming dope of epoxy resin modification
Preparation technology's formula of extinguishing waterborn polyurethane coating adhesive
Concrete technology is: in a mixing bowl, add meter quantitative fire retardant, water and alcohol, after abundant stirring 30min, the more quantitative aqueous polyurethane coating of meter is slowly added, violent stirring 50min, finally use emulsification pretreatment instrument emulsification 50min again, obtained epoxy modified aqueous polyurethane flame-proof coating.
Embodiment 3
1, the synthesis of epoxy resin modified aqueous polyurethane
Agitator is being housed, thermometer, condensing works and be connected with in five mouthfuls of flasks of nitrogen protection, add pretreated 13.5wt% poly (propylene carbonate) glycol, stirring is warming up to 60 DEG C, add 5wt%2, the two hydroxymethyl propionic acid chainextender of 2-and 0.3wt% catalyst dibutyltin dilaurylate and 19.2wt% vulcabond have isophorone diisocyanate, after being warming up to 85 DEG C of reaction 2h, slowly add the small molecule chain extender compound of the quantitative 4wt% of meter, 85 DEG C are kept to react 1h, proceed to chain extension stage in reaction and complete a half, add 2wt% epoxy resin, 85 DEG C are kept to react 0.8h, be down to room temperature afterwards, drip the agent of 5wt% ammonia neutralization to neutralize, the acetone that titration time controls the water and 6wt% adding 45wt% after 30min in prepolymer carries out emulsification, violent stirring 30min, vacuum subtracts steaming and pumps acetone, obtained epoxy resin modified aqueous polyurethane coating.
2, the preparation of the aqueous polyurethane anti-flaming dope of epoxy resin modification
Preparation technology's formula of extinguishing waterborn polyurethane coating adhesive
Concrete technology is: in a mixing bowl, add meter quantitative fire retardant, water and alcohol, after abundant stirring 30min, the more quantitative aqueous polyurethane coating of meter is slowly added, violent stirring 50min, finally use emulsification pretreatment instrument emulsification 50min again, obtained epoxy modified aqueous polyurethane flame-proof coating.
Embodiment 4 is best case study on implementation
1, the synthesis of epoxy resin modified aqueous polyurethane
Agitator is being housed, thermometer, condensing works and be connected with in five mouthfuls of flasks of nitrogen protection, add pretreated 14.5wt% poly (propylene carbonate) glycol, stirring is warming up to 60 DEG C, add 4.5wt%2, the two hydroxymethyl propionic acid of 2-and 0.4wt% catalyst dibutyltin dilaurylate, when temperature rises to 60 DEG C, add 17.2wt% hexamethylene diisocyanate, after being warming up to 85 DEG C of reaction 2h, slowly add the butanediamine extender compounds of the quantitative 4.5wt% of meter, 85 DEG C are kept to react 1h, proceed to chain extension stage in reaction and complete a half, add 3.5wt% epoxy resin E44, 85 DEG C are kept to react 0.8h, be down to room temperature afterwards, drip 3.5wt% triethylamine neutralizing agent to neutralize, the acetone that titration time controls the water and 3wt% adding 48.9wt% after 30min in prepolymer carries out emulsification, violent stirring 30min, vacuum subtracts steaming and pumps acetone, obtained epoxy resin modified aqueous polyurethane coating.
2, the preparation of the aqueous polyurethane anti-flaming dope of epoxy resin modification.
Preparation technology's formula of extinguishing waterborn polyurethane coating adhesive
Concrete technology is: in a mixing bowl, add meter quantitative fire retardant, water and alcohol, after abundant stirring 30min, the more quantitative aqueous polyurethane coating of meter is slowly added, violent stirring 50min, finally use emulsification pretreatment instrument emulsification 50min again, obtained epoxy modified aqueous polyurethane flame-proof coating.
Water-fast, the hardness of the viscosity of emulsion, stability and film and flame retardant properties are tested.
Emulsion viscosity: measure according to GB/T1723 – 1993.
Emulsion mechanical stability: test according to GB/T11175 – 2002.
Film is water-fast: test according to GB/T1733 – 1993.
Hardness of film: test according to GB/T6739-1996.
The test of flame retardant properties: be fixed on iron stand by the plank iron clamp to be measured scribbling anti-flaming dope, the vertical range between plank and operator's console is 16 ㎝, when flame temperature reaches top temperature, starts to test until test terminal plank to be measured.During test, with spirit lamp flame flame envelope heating plank, occur that charing is designated as duration of fire resistance (s) with the plank back side to be measured.
The test data of the aqueous polyurethane coating of table-epoxy resin modification
Above-mentioned embodiment is just explained in detail technical scheme of the present invention; the present invention has more than and is only confined to above-described embodiment; those skilled in the art should be understood that; every improvement on basis of the present invention according to above-mentioned principle and spirit, substitute, all should within protection scope of the present invention.
Claims (8)
1. an aqueous polyurethane anti-flaming dope for epoxy resin modification, is characterized in that: its by following component by following weight percentage than formulated:
2. the aqueous polyurethane anti-flaming dope of a kind of epoxy resin modification according to claim 1, is characterized in that: described aqueous polyurethane emulsion by following component by following weight percentage than formulated:
3. the aqueous polyurethane anti-flaming dope of a kind of epoxy resin modification according to claim 2, it is characterized in that: described vulcabond is aromatic diisocyanate, aliphatic diisocyanate, alicyclic diisocyanate, tolylene diisocyanate, 4,4-diphenylmethanediisocyanates, vulcabond have one in isophorone diisocyanate, hexamethylene diisocyanate.
4. the aqueous polyurethane anti-flaming dope of a kind of epoxy resin modification according to claim 2, is characterized in that: described small molecule chain extender is dibasic alcohol or diamine; Described hydrophilic chain extender is the one of the two hydroxymethyl propionic acid of second diamino sulfonic acid sodium, adipic dihydrazide or 2,2-; Described neutralizing agent is the one in triethylamine, ammoniacal liquor or sodium hydroxide.
5. the aqueous polyurethane anti-flaming dope of a kind of epoxy resin modification according to claim 2, is characterized in that: described epoxy resin is glycidyl ether or ethylene oxidic ester epoxy resin.
6. the aqueous polyurethane anti-flaming dope of a kind of epoxy resin modification according to claim 2, is characterized in that: described aqueous polyurethane emulsion is prepared as follows:
Agitator, thermometer, condensing works are being housed and are being connected with in five mouthfuls of flasks of nitrogen protection, add 7.5-17.5wt% polypropylene carbonate esterdiol, 50-60 DEG C is heated under stir speed (S.S.) is 300-500rmp, then 1-5wt% hydrophilic chain extender, 0.1-0.5wt% dibutyl tin laurate and 14-24.4wt% vulcabond is added, then 70-85 DEG C is warming up to, after reaction 1.5-3h, slowly add the small molecule chain extender of 2-8wt%, keep 70-85 DEG C, reaction 0.5-1h, add 2-6wt% epoxy resin afterwards, keep 70-85 DEG C to react 0.5-1h;
Be down to room temperature afterwards, by the neutralizing agent of 1-5wt% instillation reaction system, the time of described instillation neutralizing agent is 15-30min, then the water of 45-53wt% and the acetone of 2-6wt% is added, raise stir speed (S.S.) to 1000-1500rmp, stir 0.5-1h, last vacuum subtracts steaming and pumps acetone.
7. the aqueous polyurethane anti-flaming dope of a kind of epoxy resin modification according to claim 1, is characterized in that: described fire retardant by ammonium polyphosphate, trimeric cyanamide and tetramethylolmethane in mass ratio for 3-6:1-3:2-1 mixes.
8. according to the preparation method of the aqueous polyurethane anti-flaming dope of a kind of epoxy resin modification in claim 1-7 described in any one, it is characterized in that: comprise the following steps, in room temperature, stir speed (S.S.) is under 300-500rmp, fire retardant 20-28wt% is added in a mixing bowl, water 20-34wt% and alcohol 15-23wt%, after abundant stirring 30min-60min, again described aqueous polyurethane emulsion 25-35wt% is slowly joined in above-mentioned reaction system, then stir speed (S.S.) is raised to 1000-1500rmp, stir 50-70min, finally use emulsification pretreatment instrument emulsification 50-70min, obtained epoxy modified aqueous polyurethane flame-proof coating.
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Cited By (6)
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| CN105885660A (en) * | 2016-05-30 | 2016-08-24 | 福建盈浩工艺制品有限公司 | Flame-retardant environment-friendly paint and preparation method thereof |
| CN105925168A (en) * | 2016-05-20 | 2016-09-07 | 武汉工程大学 | Microencapsulated water-based fire retardant coating and preparation method thereof |
| CN106221346A (en) * | 2016-07-29 | 2016-12-14 | 武汉工程大学 | A kind of self-repair type fire-resistant coating for steel structure and preparation method thereof |
| CN106634530A (en) * | 2016-12-13 | 2017-05-10 | 苏州赛斯德工程设备有限公司 | Waterborne polyurethane coating and preparation process |
| CN108441100A (en) * | 2018-03-30 | 2018-08-24 | 天长市巨龙车船涂料有限公司 | A kind of high-ductility flame retardant polyurethane coating |
| CN111057216A (en) * | 2019-12-31 | 2020-04-24 | 安徽三棵树涂料有限公司 | Single-component non-flammable polyurethane fireproof coating and preparation method thereof |
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Cited By (8)
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| CN105925168A (en) * | 2016-05-20 | 2016-09-07 | 武汉工程大学 | Microencapsulated water-based fire retardant coating and preparation method thereof |
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| CN106221346A (en) * | 2016-07-29 | 2016-12-14 | 武汉工程大学 | A kind of self-repair type fire-resistant coating for steel structure and preparation method thereof |
| CN106221346B (en) * | 2016-07-29 | 2019-06-11 | 武汉工程大学 | A kind of self-repair type fire-resistant coating for steel structure and preparation method thereof |
| CN106634530A (en) * | 2016-12-13 | 2017-05-10 | 苏州赛斯德工程设备有限公司 | Waterborne polyurethane coating and preparation process |
| CN108441100A (en) * | 2018-03-30 | 2018-08-24 | 天长市巨龙车船涂料有限公司 | A kind of high-ductility flame retardant polyurethane coating |
| CN111057216A (en) * | 2019-12-31 | 2020-04-24 | 安徽三棵树涂料有限公司 | Single-component non-flammable polyurethane fireproof coating and preparation method thereof |
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