CN105623491A - High-flame-retardant heat-resistant polyurethane paint - Google Patents
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- C09D—COATING 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
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Abstract
The invention discloses high-flame-retardant heat-resistant polyurethane paint, which is prepared from the following raw materials including 4,4'-diphenyl methane diisocyanate, polytetramethylene etherglycol, alkynyl-containing polyhydric alcohols, borophenylic acid, 1,4-butanediol, azodiisobutyronitrile, antioxygen agents, graphene oxide, borate tri(2,3-dibromo) propyl ester, triethylamine, 3,3'-diamino-4,4'-dihydroxy diphenyl sulfone, 1-sulfolane-3-ethoxycarbonyl-5-hydroxypyazole, 1,4-bi(hydroxydimethylsilyl)benzene, a flatting agent, a defoaming agent, a moisturizing agent, benzoic acid and water. The high-flame-retardant heat-resistant polyurethane paint provided by the invention has the advantages that the flame-retardant performance is excellent; the thermal stability is good; the attaching force to base materials is high.
Description
Technical field
The present invention relates to polyurethane coating technical field, particularly relate to a kind of high fire-retardance thermal polyurethane coating.
Background technology
Polyurethane has the mechanical performance of wear-resisting, water-fast, solvent resistant and excellence preferably, is applied widely at present in elastomer, foam plastics, coating, adhesive and bio-medical material etc. Polyurethane coating method be generally applied to the fields such as leather finish, textile printing and dyeing, paper-making industry, building coating, adhesive, steel moulder's paint, involved in these areas nearly all have combustible material, these materials as not fire retardant treated, necessarily become the potential safety hazard of initiation fire in use. Polyurethane coating flame-retarded is one of urethane functionalized important directions. And there is defect relatively costly, that flame retardant effect is undesirable in the flame retardant polyurethane that China sells in the market, add the poor heat stability of polyurethane own, its mechanical performance substantially disappears in the environment of 80-90 DEG C, and on 200 DEG C, namely there is thermal degradation, therefore limit the application of polyurethane coating.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes a kind of high fire-retardance thermal polyurethane coating, its excellent fireproof performance, and Heat stability is good is strong with the adhesive force of base material.
A kind of high fire-retardance thermal polyurethane coating that the present invention proposes, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 30-50 part, polytetramethylene ether diol 5-15 part, containing alkynyl polyhydric alcohol 10-20 part, phenylboric acid 2-8 part, 1, 4-butanediol 1-5 part, azodiisobutyronitrile 0.1-0.5 part, antioxidant 0.1-0.5 part, graphene oxide 2-5 part, boric acid three (2, 3-dibromo) propyl ester 3-10 part, triethylamine 1-2.5 part, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 1-3.5 part, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 2-10 part, 1, double, two (dimethyl hydroxyl is silica-based) benzene 1-3.5 part of 4-, levelling agent 0.5-1 part, defoamer 0.2-0.8 part, wetting agent 0.1-0.6 part, benzoic acid 0.1-1 part, water 50-80 part.
Preferably, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 38-46 part, polytetramethylene ether diol 8-12 part, containing alkynyl polyhydric alcohol 13-17 part, phenylboric acid 3.2-4.5 part, 1, 4-butanediol 3.2-4 part, azodiisobutyronitrile 0.32-0.4 part, antioxidant 0.25-0.32 part, graphene oxide 3.5-4 part, boric acid three (2, 3-dibromo) propyl ester 6-7.2 part, triethylamine 1.6-2.1 part, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 1.9-2.5 part, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 4-5.6 part, 1, double, two (dimethyl hydroxyl is silica-based) benzene 1.7-3.1 part of 4-, levelling agent 0.65-0.8 part, defoamer 0.5-0.7 part, wetting agent 0.26-0.5 part, benzoic acid 0.65-0.72 part, water 62-70 part.
Preferably, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 42 parts, polytetramethylene ether diol 10 parts, containing alkynyl polyhydric alcohol 16 parts, phenylboric acid 4 parts, 1, 4-butanediol 3.5 parts, azodiisobutyronitrile 0.38 part, 0.3 part of antioxidant, graphene oxide 3.7 parts, boric acid three (2, 3-dibromo) propyl ester 6.5 parts, triethylamine 2 parts, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 2.1 parts, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 5.2 parts, 1, double, two (dimethyl hydroxyl the is silica-based) benzene 3 parts of 4-, levelling agent 0.7 part, defoamer 0.56 part, wetting agent 0.32 part, 0.7 part of benzoic acid, 68 parts of water.
Preferably, described it is prepared according to following technique containing alkynyl polyhydric alcohol: in reaction unit, pass into nitrogen, be subsequently adding 1-2 part 3,4,9,10-tetracarboxylic anhydride, 2-5 part D, L-phenylalanine, 15-25 part N,N-dimethylacetamide and 1-1.5 part pyridine, stirring reaction 5-12h after being warming up to 125-140 DEG C, reaction is poured in the hydrochloric acid that 50-80 part mass fraction is 8-10% after terminating, and filters after standing, dries and obtain material A after washing; By weight by 3-5 part material A and 15-25 part thionyl chloride mix homogeneously, reacting 3-6h at 70-75 DEG C, after reaction terminates, evaporation obtains material B; By weight by 15-20 part 1, double; two (2-the hydroxy ethoxy)-2-butyne of 4-, 1-2 part triethylamine and 25-35 part N, N-dimethyl acetylamide mix homogeneously, nitrogen is passed into when ice-water bath, it is subsequently adding 3-7 part material B, at room temperature reacting 15-22h, reaction adds in the hydrochloric acid that 300-450 part mass fraction is 10-15% after terminating, filter after standing, dry obtain described containing alkynyl polyhydric alcohol.
Preferably, in the preparation process containing alkynyl polyhydric alcohol, 3,4,9,10-tetracarboxylic anhydrides, D, the weight ratio of L-phenylalanine is 1.2-1.8:3.2-4.6.
Preferably, in the preparation process containing alkynyl polyhydric alcohol, material A, thionyl chloride weight ratio be 3.6-4.2:19-24.
Preferably, in the preparation process containing alkynyl polyhydric alcohol, Isosorbide-5-Nitrae-bis-(2-hydroxy ethoxy)-2-butyne, material B weight ratio be 16-19:4.5-6.5.
Preferably, described it is prepared according to following technique containing alkynyl polyhydric alcohol: in reaction unit, pass into nitrogen, be subsequently adding 1.6 part 3,4,9,10-tetracarboxylic anhydride, 3.8 parts of D, L-phenylalanine, 20 parts of N,N-dimethylacetamide and 1.2 parts of pyridines, stirring reaction 8h after being warming up to 135 DEG C, reaction is poured into after terminating in the hydrochloric acid that 72 parts of mass fractions are 9%, filters after standing, dry after washing obtains material A, by weight by 4 parts of material A and 21 parts of thionyl chloride mix homogeneously, reacting 4.6h at 73 DEG C, after reaction terminates, evaporation obtains material B, by weight by 18 part 1, double, two (2-the hydroxy ethoxy)-2-butyne of 4-, 1.3 parts of triethylamines and 30 parts of N, N-dimethyl acetylamide mix homogeneously, nitrogen is passed into when ice-water bath, it is subsequently adding 6 parts of material B, at room temperature reacting 20h, reaction adds after terminating in the hydrochloric acid that 420 parts of mass fractions are 13%, filter after standing, dry obtain described containing alkynyl polyhydric alcohol, in the preparation process containing alkynyl polyhydric alcohol, first have selected 3, 4, 9, 10-tetracarboxylic anhydride and D, L-phenylalanine is raw material, D is made by controlling the condition of reaction, amino and 3 in L-phenylalanine, 4, 9, oxygen in 10-tetracarboxylic anhydride there occurs reaction, generate the carboxylic acid containing imide ring, after adding thionyl chloride, chlorine in thionyl chloride instead of the hydrogen on carboxylic acid, generate the acyl chlorides containing imide ring, add 1, after double, two (2-the hydroxy ethoxy)-2-butyne of 4-, acyl chlorides and 1, hydroxyl in double, two (2-the hydroxy ethoxy)-2-butyne of 4-there occurs reaction, generate the polyhydric alcohol simultaneously containing imide ring and alkynyl, it is added in polyurethane coating, on the one hand, because of the increase of urethane group content in molecule, improve the rigidity of coating, improve hardness and the hot strength of coating, on the one hand, after introducing imide ring, improve the hydrogen bond between strand, strengthen the interaction force between strand, further increase hardness and the hot strength of coating, on the other hand, because molecule introduces imide ring and the alkynyl the two group of Heat stability is good, significantly improve the heat stability of coating, and imide ring is prone to into charcoal with alkynyl, further improve the anti-flammability of coating.
In the present invention, described high fire-retardance thermal polyurethane coating can polyurethane coating preparation technology conventionally be prepared from.
In molecular backbone, organic polymer containing alkynyl is due to the C �� C in its molecule can be reacted by heat cross-linking or photo-crosslinking makes intermolecular highly cross-linked formation more stable network structure, thus this base polymer has higher heat stability, in polyurethane coating of the present invention, have selected containing alkynyl polyhydric alcohol, 4, 4 '-methyl diphenylene diisocyanate, polytetramethylene ether diol, phenylboric acid and 1, 4-butanediol is raw material, thus by alkynyl introducing system, give the thermostability that coating is excellent, in system, introduce phenylboric acid simultaneously, improve anti-flammability and the thermostability of coating, in graphene oxide addition system, the hydroxyl on its surface, carboxyl isoreactivity group can with generation effects such as the isocyano in system, hydroxyls, improve the adhesion of itself and system, improve its dispersibility in system, further improve thermostability and the anti-flammability of coating, 3,3'-diaminourea-4, in 4'-dihydroxydiphenylsulisomer, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles, Isosorbide-5-Nitrae-bis-(dimethyl hydroxyl is silica-based) benzene addition system, because of in molecule containing activated hydroxyl, good with the associativity of system, system is uniformly dispersed, after collaborative with boric acid three (2,3-dibromo) propyl ester, excellent fireproof performance, and thing without dripping off during burning.
Detailed description of the invention
Below, by specific embodiment, technical scheme is described in detail.
Embodiment 1
The present invention proposes a kind of high fire-retardance thermal polyurethane coating, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 30 parts, polytetramethylene ether diol 15 parts, containing alkynyl polyhydric alcohol 10 parts, phenylboric acid 8 parts, 1, 4-butanediol 1 part, azodiisobutyronitrile 0.1 part, 0.5 part of antioxidant, graphene oxide 2 parts, boric acid three (2, 3-dibromo) propyl ester 10 parts, triethylamine 1 part, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 3.5 parts, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 2 parts, 1, double, two (dimethyl hydroxyl the is silica-based) benzene 3.5 parts of 4-, levelling agent 0.5 part, defoamer 0.8 part, wetting agent 0.1 part, 1 part of benzoic acid, 50 parts of water,
Wherein, described it is prepared according to following technique containing alkynyl polyhydric alcohol: in reaction unit, pass into nitrogen, be subsequently adding 1 part 3,4,9,10-tetracarboxylic anhydride, 5 parts of D, L-phenylalanine, 15 parts of N,N-dimethylacetamide and 1.5 parts of pyridines, stirring reaction 12h after being warming up to 125 DEG C, reaction is poured into after terminating in the hydrochloric acid that 50 parts of mass fractions are 10%, filters after standing, dry after washing obtains material A; By weight by 3 parts of material A and 25 parts of thionyl chloride mix homogeneously, reacting 6h at 70 DEG C, after reaction terminates, evaporation obtains material B; By weight by 15 part 1, double; two (2-the hydroxy ethoxy)-2-butyne of 4-, 2 parts of triethylamines and 25 parts of N, N-dimethyl acetylamide mix homogeneously, nitrogen is passed into when ice-water bath, it is subsequently adding 7 parts of material B, at room temperature reacting 15h, reaction adds after terminating in the hydrochloric acid that 450 parts of mass fractions are 10%, filter after standing, dry obtain described containing alkynyl polyhydric alcohol.
Embodiment 2
The present invention proposes a kind of high fire-retardance thermal polyurethane coating, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 50 parts, polytetramethylene ether diol 5 parts, containing alkynyl polyhydric alcohol 20 parts, phenylboric acid 2 parts, 1, 4-butanediol 5 parts, azodiisobutyronitrile 0.5 part, 0.1 part of antioxidant, graphene oxide 5 parts, boric acid three (2, 3-dibromo) propyl ester 3 parts, triethylamine 2.5 parts, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 1 part, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 10 parts, 1, double, two (dimethyl hydroxyl the is silica-based) benzene 1 part of 4-, levelling agent 1 part, defoamer 0.2 part, wetting agent 0.6 part, 0.1 part of benzoic acid, 80 parts of water,
Wherein, described it is prepared according to following technique containing alkynyl polyhydric alcohol: in reaction unit, pass into nitrogen, be subsequently adding 2 part 3,4,9,10-tetracarboxylic anhydride, 2 parts of D, L-phenylalanine, 25 parts of N,N-dimethylacetamide and 1 part of pyridine, stirring reaction 5h after being warming up to 140 DEG C, reaction is poured into after terminating in the hydrochloric acid that 80 parts of mass fractions are 8%, filters after standing, dry after washing obtains material A; By weight by 5 parts of material A and 15 parts of thionyl chloride mix homogeneously, reacting 3h at 75 DEG C, after reaction terminates, evaporation obtains material B; By weight by 20 part 1, double; two (2-the hydroxy ethoxy)-2-butyne of 4-, 1 part of triethylamine and 35 parts of N, N-dimethyl acetylamide mix homogeneously, nitrogen is passed into when ice-water bath, it is subsequently adding 3 parts of material B, at room temperature reacting 22h, reaction adds after terminating in the hydrochloric acid that 300 parts of mass fractions are 15%, filter after standing, dry obtain described containing alkynyl polyhydric alcohol.
Embodiment 3
The present invention proposes a kind of high fire-retardance thermal polyurethane coating, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 38 parts, polytetramethylene ether diol 12 parts, containing alkynyl polyhydric alcohol 13 parts, phenylboric acid 4.5 parts, 1, 4-butanediol 3.2 parts, azodiisobutyronitrile 0.32 part, 0.32 part of antioxidant, graphene oxide 3.5 parts, boric acid three (2, 3-dibromo) propyl ester 6 parts, triethylamine 2.1 parts, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 1.9 parts, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 5.6 parts, 1, double, two (dimethyl hydroxyl the is silica-based) benzene 1.7 parts of 4-, levelling agent 0.8 part, defoamer 0.5 part, wetting agent 0.5 part, 0.65 part of benzoic acid, 62 parts of water,
Wherein, described it is prepared according to following technique containing alkynyl polyhydric alcohol: in reaction unit, pass into nitrogen, be subsequently adding 1.2 part 3,4,9,10-tetracarboxylic anhydride, 4.6 parts of D, L-phenylalanine, 17 parts of N,N-dimethylacetamide and 1.35 parts of pyridines, stirring reaction 10h after being warming up to 128 DEG C, reaction is poured into after terminating in the hydrochloric acid that 65 parts of mass fractions are 9%, filters after standing, dry after washing obtains material A; By weight by 3.6 material A and 24 parts of thionyl chloride mix homogeneously, reacting 5.2h at 73 DEG C, after reaction terminates, evaporation obtains material B; By weight by 16 part 1, double; two (2-the hydroxy ethoxy)-2-butyne of 4-, 1.7 parts of triethylamines and 28 parts of N, N-dimethyl acetylamide mix homogeneously, nitrogen is passed into when ice-water bath, it is subsequently adding 6.5 parts of material B, at room temperature reacting 18h, reaction adds after terminating in the hydrochloric acid that 420 parts of mass fractions are 12%, filter after standing, dry obtain described containing alkynyl polyhydric alcohol.
Embodiment 4
The present invention proposes a kind of high fire-retardance thermal polyurethane coating, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 46 parts, polytetramethylene ether diol 8 parts, containing alkynyl polyhydric alcohol 17 parts, phenylboric acid 3.2 parts, 1, 4-butanediol 4 parts, azodiisobutyronitrile 0.4 part, 0.25 part of antioxidant, graphene oxide 4 parts, boric acid three (2, 3-dibromo) propyl ester 7.2 parts, triethylamine 1.6 parts, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 2.5 parts, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 4 parts, 1, double, two (dimethyl hydroxyl the is silica-based) benzene 3.1 parts of 4-, levelling agent 0.65 part, defoamer 0.7 part, wetting agent 0.26 part, 0.72 part of benzoic acid, 62 parts of water,
Wherein, described it is prepared according to following technique containing alkynyl polyhydric alcohol: in reaction unit, pass into nitrogen, be subsequently adding 1.8 part 3,4,9,10-tetracarboxylic anhydride, 3.2 parts of D, L-phenylalanine, 22 parts of N,N-dimethylacetamide and 1.2 parts of pyridines, stirring reaction 7.5h after being warming up to 136 DEG C, reaction is poured into after terminating in the hydrochloric acid that 70 parts of mass fractions are 8.5%, filters after standing, dry after washing obtains material A; By weight by 4.2 material A and 19 parts of thionyl chloride mix homogeneously, reacting 3.8h at 72 DEG C, after reaction terminates, evaporation obtains material B; By weight by 19 part 1, double; two (2-the hydroxy ethoxy)-2-butyne of 4-, 1.3 parts of triethylamines and 33 parts of N, N-dimethyl acetylamide mix homogeneously, nitrogen is passed into when ice-water bath, it is subsequently adding 4.5 parts of material B, at room temperature reacting 20h, reaction adds after terminating in the hydrochloric acid that 380 parts of mass fractions are 13.5%, filter after standing, dry obtain described containing alkynyl polyhydric alcohol.
Embodiment 5
The present invention proposes a kind of high fire-retardance thermal polyurethane coating, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 42 parts, polytetramethylene ether diol 10 parts, containing alkynyl polyhydric alcohol 16 parts, phenylboric acid 4 parts, 1, 4-butanediol 3.5 parts, azodiisobutyronitrile 0.38 part, 0.3 part of antioxidant, graphene oxide 3.7 parts, boric acid three (2, 3-dibromo) propyl ester 6.5 parts, triethylamine 2 parts, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 2.1 parts, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 5.2 parts, 1, double, two (dimethyl hydroxyl the is silica-based) benzene 3 parts of 4-, levelling agent 0.7 part, defoamer 0.56 part, wetting agent 0.32 part, 0.7 part of benzoic acid, 68 parts of water,
Wherein, described it is prepared according to following technique containing alkynyl polyhydric alcohol: in reaction unit, pass into nitrogen, be subsequently adding 1.6 part 3,4,9,10-tetracarboxylic anhydride, 3.8 parts of D, L-phenylalanine, 20 parts of N,N-dimethylacetamide and 1.2 parts of pyridines, stirring reaction 8h after being warming up to 135 DEG C, reaction is poured into after terminating in the hydrochloric acid that 72 parts of mass fractions are 9%, filters after standing, dry after washing obtains material A; By weight by 4 parts of material A and 21 parts of thionyl chloride mix homogeneously, reacting 4.6h at 73 DEG C, after reaction terminates, evaporation obtains material B; By weight by 18 part 1, double; two (2-the hydroxy ethoxy)-2-butyne of 4-, 1.3 parts of triethylamines and 30 parts of N, N-dimethyl acetylamide mix homogeneously, nitrogen is passed into when ice-water bath, it is subsequently adding 6 parts of material B, at room temperature reacting 20h, reaction adds after terminating in the hydrochloric acid that 420 parts of mass fractions are 13%, filter after standing, dry obtain described containing alkynyl polyhydric alcohol.
The above; it is only the present invention preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; any those familiar with the art is in the technical scope that the invention discloses; it is equal to replacement according to technical scheme and inventive concept thereof or is changed, all should be encompassed within protection scope of the present invention.
Claims (8)
1. a high fire-retardance thermal polyurethane coating, it is characterized in that, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 30-50 part, polytetramethylene ether diol 5-15 part, containing alkynyl polyhydric alcohol 10-20 part, phenylboric acid 2-8 part, 1, 4-butanediol 1-5 part, azodiisobutyronitrile 0.1-0.5 part, antioxidant 0.1-0.5 part, graphene oxide 2-5 part, boric acid three (2, 3-dibromo) propyl ester 3-10 part, triethylamine 1-2.5 part, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 1-3.5 part, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 2-10 part, 1, double, two (dimethyl hydroxyl is silica-based) benzene 1-3.5 part of 4-, levelling agent 0.5-1 part, defoamer 0.2-0.8 part, wetting agent 0.1-0.6 part, benzoic acid 0.1-1 part, water 50-80 part.
2. high fire-retardance thermal polyurethane coating according to claim 1, it is characterized in that, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 38-46 part, polytetramethylene ether diol 8-12 part, containing alkynyl polyhydric alcohol 13-17 part, phenylboric acid 3.2-4.5 part, 1, 4-butanediol 3.2-4 part, azodiisobutyronitrile 0.32-0.4 part, antioxidant 0.25-0.32 part, graphene oxide 3.5-4 part, boric acid three (2, 3-dibromo) propyl ester 6-7.2 part, triethylamine 1.6-2.1 part, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 1.9-2.5 part, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 4-5.6 part, 1, double, two (dimethyl hydroxyl is silica-based) benzene 1.7-3.1 part of 4-, levelling agent 0.65-0.8 part, defoamer 0.5-0.7 part, wetting agent 0.26-0.5 part, benzoic acid 0.65-0.72 part, water 62-70 part.
3. high fire-retardance thermal polyurethane coating according to claim 1 or claim 2, it is characterized in that, its raw material includes following components by weight: 4, 4 '-methyl diphenylene diisocyanate 42 parts, polytetramethylene ether diol 10 parts, containing alkynyl polyhydric alcohol 16 parts, phenylboric acid 4 parts, 1, 4-butanediol 3.5 parts, azodiisobutyronitrile 0.38 part, 0.3 part of antioxidant, graphene oxide 3.7 parts, boric acid three (2, 3-dibromo) propyl ester 6.5 parts, triethylamine 2 parts, 3, 3'-diaminourea-4, 4'-dihydroxydiphenylsulisomer 2.1 parts, 1-sulfolane-3-carbethoxyl group-5-hydroxypyrazoles 5.2 parts, 1, double, two (dimethyl hydroxyl the is silica-based) benzene 3 parts of 4-, levelling agent 0.7 part, defoamer 0.56 part, wetting agent 0.32 part, 0.7 part of benzoic acid, 68 parts of water.
4. high fire-retardance thermal polyurethane coating according to any one of claim 1-3, it is characterized in that, described it is prepared according to following technique containing alkynyl polyhydric alcohol: in reaction unit, pass into nitrogen, it is subsequently adding 1-2 part 3,4,9,10-tetracarboxylic anhydride, 2-5 part D, L-phenylalanine, 15-25 part N, N-dimethyl acetylamide and 1-1.5 part pyridine, stirring reaction 5-12h after being warming up to 125-140 DEG C, reaction is poured in the hydrochloric acid that 50-80 part mass fraction is 8-10% after terminating, filter after standing, dry after washing and obtain material A; By weight by 3-5 part material A and 15-25 part thionyl chloride mix homogeneously, reacting 3-6h at 70-75 DEG C, after reaction terminates, evaporation obtains material B; By weight by 15-20 part 1, double; two (2-the hydroxy ethoxy)-2-butyne of 4-, 1-2 part triethylamine and 25-35 part N, N-dimethyl acetylamide mix homogeneously, nitrogen is passed into when ice-water bath, it is subsequently adding 3-7 part material B, at room temperature reacting 15-22h, reaction adds in the hydrochloric acid that 300-450 part mass fraction is 10-15% after terminating, filter after standing, dry obtain described containing alkynyl polyhydric alcohol.
5. high fire-retardance thermal polyurethane coating according to claim 4, it is characterised in that in the preparation process containing alkynyl polyhydric alcohol, 3,4,9,10-tetracarboxylic anhydrides, D, the weight ratio of L-phenylalanine is 1.2-1.8:3.2-4.6.
6. high fire-retardance thermal polyurethane coating according to claim 4 or 5, it is characterised in that in the preparation process containing alkynyl polyhydric alcohol, material A, thionyl chloride weight ratio be 3.6-4.2:19-24.
7. high fire-retardance thermal polyurethane coating according to any one of claim 4-6, it is characterised in that in the preparation process containing alkynyl polyhydric alcohol, Isosorbide-5-Nitrae-bis-(2-hydroxy ethoxy)-2-butyne, material B weight ratio be 16-19:4.5-6.5.
8. high fire-retardance thermal polyurethane coating according to any one of claim 1-7, it is characterised in that described be prepared according to following technique containing alkynyl polyhydric alcohol: pass into nitrogen in reaction unit, it is subsequently adding 1.6 part 3,4,9,10-tetracarboxylic anhydrides, 3.8 parts of D, L-phenylalanine, 20 parts of N, N-dimethyl acetylamide and 1.2 parts of pyridines, stirring reaction 8h after being warming up to 135 DEG C, reaction is poured in the hydrochloric acid that 72 parts of mass fractions are 9% after terminating, filter after standing, dry after washing and obtain material A; By weight by 4 parts of material A and 21 parts of thionyl chloride mix homogeneously, reacting 4.6h at 73 DEG C, after reaction terminates, evaporation obtains material B; By weight by 18 part 1, double; two (2-the hydroxy ethoxy)-2-butyne of 4-, 1.3 parts of triethylamines and 30 parts of N, N-dimethyl acetylamide mix homogeneously, nitrogen is passed into when ice-water bath, it is subsequently adding 6 parts of material B, at room temperature reacting 20h, reaction adds after terminating in the hydrochloric acid that 420 parts of mass fractions are 13%, filter after standing, dry obtain described containing alkynyl polyhydric alcohol.
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| CN106478915A (en) * | 2016-10-09 | 2017-03-08 | 合肥广能新材料科技有限公司 | Polyurethane rigid foam exterior wall thermal insulation material and preparation method thereof |
| CN106497021A (en) * | 2016-10-09 | 2017-03-15 | 合肥广能新材料科技有限公司 | Polyurethane rigid foam exterior wall flame-retardant thermal insulation material and preparation method thereof |
| CN107778451A (en) * | 2017-11-02 | 2018-03-09 | 合众（佛山）化工有限公司 | A kind of low free high rigidity boron modification polyurethane curing agent |
| CN110563909A (en) * | 2019-09-03 | 2019-12-13 | 四川睿铁科技有限责任公司 | restrictive pouring modified polyurethane resin for guide rail of guide rail electric car and preparation method thereof |
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Application publication date: 20160601 |