CN101818039B - Single-component low-modulus polyurethane building sealant and preparation method thereof - Google Patents
Single-component low-modulus polyurethane building sealant and preparation method thereof Download PDFInfo
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Abstract
本发明涉及一种密封胶，尤其是单组份低模量聚氨酯建筑密封胶及其制备方法。单组份低模量聚氨酯建筑密封胶，包括聚氨酯预聚物A和聚氨酯预聚物B共30-60％，聚氨酯预聚物A与聚氨酯预聚物B的重量份比值为3～1，硅烷偶联剂0.25-2.5％，辛酸铝交联剂0.25-2.5％，潜伏型固化剂0.301-0.35％，增塑剂10-40％，填料10-60％，紫外线吸收剂和稳定剂0.1-3％，上述各个组份含量以质量百分含量计；聚氨酯预聚物A是二苯基甲烷二异氰酸酯与多元醇反应生成，聚氨酯预聚物B是1-6-己二异氰酸酯和多元醇在二丁基锡二月桂酸酯下反应生成。本发明伸长率好、耐黄变、环保，对陶瓷、玻璃有优异的粘接性能。The invention relates to a sealant, especially a one-component low-modulus polyurethane building sealant and a preparation method thereof. One-component low-modulus polyurethane building sealant, comprising 30-60% of polyurethane prepolymer A and polyurethane prepolymer B, the weight ratio of polyurethane prepolymer A to polyurethane prepolymer B is 3-1, silane Coupling agent 0.25-2.5%, aluminum octanoate crosslinking agent 0.25-2.5%, latent curing agent 0.301-0.35%, plasticizer 10-40%, filler 10-60%, ultraviolet absorber and stabilizer 0.1-3 %, the content of each of the above components is in mass percentage; polyurethane prepolymer A is produced by the reaction of diphenylmethane diisocyanate and polyol, polyurethane prepolymer B is 1-6-hexamethylene diisocyanate and polyol in two Under the reaction of butyl tin dilaurate. The invention has good elongation, yellowing resistance, environmental protection and excellent bonding performance to ceramics and glass.
Description
Technical field:
The present invention relates to a kind of seal gum, especially a kind of single-component low-modulus polyurethane building sealant and preparation method thereof.
Background technology:
The employed seal gum in domestic civil construction field mainly is silicone, esters of acrylic acid, this class seal gum bonding strength and elasticity are low, water-fast, weathering resistance is poor, to concrete corrosion, oil impregnate pollutes, easily tear, the defective such as can not paint, have at present the wet-solidifying single-component polyurethane seal gum that adopts take polyurethane prepolymer as major ingredient, polyurethane prepolymer wherein is to be generated by polyol compound and excessive isocyanic ester and polymer reaction thereof, and adding solvent, filler etc., this product modulus is high, elongation is lower, and weathering resistance is relatively poor, the solvent evaporates contaminate environment.
Summary of the invention:
Technical problem to be solved by this invention is the deficiency that overcomes the above-mentioned background technology, provide a kind of any solvent, free from environmental pollution, nonpoisonous and tasteless that do not add, the polyurethane building sealant of bonding strength height, low, the anti-xanthochromia of modulus, high elongation rate, good weatherability.
Technical scheme provided by the invention is:
Single-component low-modulus polyurethane building sealant, its composition comprises altogether 30-60% of polyurethane prepolymer A and polyurethane prepolymer B, the weight part ratio of polyurethane prepolymer A and polyurethane prepolymer B is 3～1, silane coupling agent 0.25-2.5%, aluminium octoate linking agent 0.25-2.5%, latent curing agent 0.301-0.35%, softening agent 10-40%, filler 10-60%, UV light absorber and stablizer 0.1-3%, the content of above-mentioned each component is in the quality percentage composition; Wherein polyurethane prepolymer A is that diphenylmethanediisocyanate and polyol compound reaction generate, and polyurethane prepolymer B is that 1-6-hexamethylene diisocyanate and polyol compound react generation under dibutyltin dilaurate.
Preferably, silane coupling agent is selected N-phenyl γ-aminopropyltrimethoxysilane, latent curing agent is selected the mixture of ketoimine and dibutyltin dilaurate, softening agent is selected dioctyl phthalate (DOP), filler is selected talcum powder, active calcium oxide, light calcium carbonate, polyvinyl chloride resin, aerosil, vacuum glass microballoon, UV light absorber is selected Tinuvin329, and stablizer is selected Tinuvin5050; The single-component low-modulus polyurethane building sealant compositing formula is: polyurethane prepolymer A28kg, polyurethane prepolymer B14kg, talcum powder 5kg, light calcium carbonate 9kg, active calcium oxide 1kg, polyvinyl chloride resin 15kg, aerosil 3kg, vacuum glass microballoon 5kg, dioctyl phthalate (DOP) 19kg, Tinuvin329 is 0.2kg, Tinuvin5050 is 0.2kg, N-phenyl γ-aminopropyltrimethoxysilane 0.3kg, aluminium octoate linking agent 0.38kg, ketoimine 0.58kg, dibutyltin dilaurate 0.08kg.
Preferably, polyol compound is to choose any one kind of them or several combination from polyether glycol, polyester polyol and other main chains contain the end carboxylic compound of C-C.
Preferably, silane coupling agent is from gamma-methyl allyl acyloxypropyl trimethylammonium TMOS, N-(B-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-sulfenyl propyl trimethoxy silicane choose any one kind of them or several combination in γ-aminopropyltrimethoxysilane, the N-phenyl γ-aminopropyltrimethoxysilane.
Preferably, latent curing agent adopts ketoimine, dibutyltin dilaurate mixing cpd, wherein ketoimine content is the 0.3%-3% of single-component low-modulus polyurethane building sealant total mass, and the content of dibutyltin dilaurate is the 0.001%-0.5% of single-component low-modulus polyurethane building sealant total mass.
Preferably, softening agent is to choose any one kind of them from phthalate, alkyl sulfonates, clorafin or several combination.
Preferably, UV light absorber be from salicylic acid, benzophenone class, benzotriazole category, triazines is chosen any one kind of them or several combination, stablizer is selected hindered amine light stabilizer.
Preferably, select and choose any one kind of them in active calcium oxide, silicon powder, carbon black, talcum powder, titanium dioxide, the kaolin or several and vacuum glass microballoon and polyvinyl chloride resin are mixed into filler.
The preparation process of described single-component low-modulus polyurethane building sealant:
1) getting polyol compound adds in the vacuum reaction still, allow polyol compound under 110 ℃ vacuum environment, dewater 2 hours, make the moisture in the polyol compound be not more than 0.01%, then after the temperature of charge in the vacuum reaction still being down to 50 ℃, add diphenylmethanediisocyanate, under nitrogen protection, stir, be heated to 82 ℃, allow polyol compound and diphenylmethanediisocyanate react 4 hours, obtain polyurethane prepolymer A;
2) get polyol compound and put into the vacuum reaction still, allow polyol compound under 110 ℃ vacuum environment, dewater 2 hours, make the moisture content in the polyol compound be not more than 0.01%, then the temperature of charge in the vacuum reaction still is down to 50 ℃, in the vacuum reaction still, add the 1-6-hexamethylene diisocyanate, stir, add dibutyltin dilaurate, under nitrogen protection, temperature in the vacuum reaction still is risen to 92 ℃, allow polyol compound and 1-6-hexamethylene diisocyanate react 6 hours, obtain polyurethane prepolymer B;
3) at room temperature the order in the double-planet reactor adds softening agent, filler, polyurethane prepolymer A, polyurethane prepolymer B, silane coupling agent, aluminium octoate linking agent, UV light absorber, stablizer and mixes under vacuum protection; be warming up to 68 ℃; reacted 2 hours; be cooled to 40 ℃; add latent curing agent; stir, can obtain thixotropic single-component low-modulus polyurethane building sealant.
Preferably, the preparation process of described single-component low-modulus polyurethane building sealant:
1) gets in the polyether-tribasic alcohol adding vacuum reaction still of 85kg, allow polyether-tribasic alcohol under 110 ℃ vacuum environment, dewater 2 hours, make the moisture in the polyether-tribasic alcohol be not more than 0.01%, then after the temperature of charge in the vacuum reaction still being down to 50 ℃, add the 15kg diphenylmethanediisocyanate, under nitrogen protection, stir, be heated to 82 ℃, allow polyether-tribasic alcohol and diphenylmethanediisocyanate react 4 hours, obtain polyurethane prepolymer A;
2) polyether Glycols of getting 90kg is put into the vacuum reaction still, allow polyether Glycols under 110 ℃ vacuum environment, dewater 2 hours, make the moisture content in the polyether Glycols be not more than 0.01%, then the temperature of charge in the vacuum reaction still is down to 50 ℃, in the vacuum reaction still, add 10kg 1-6-hexamethylene diisocyanate, stir, add the 10g dibutyltin dilaurate, under nitrogen protection, temperature in the vacuum reaction still is risen to 92 ℃, allow polyether Glycols and 1-6-hexamethylene diisocyanate react 6 hours, get polyurethane prepolymer B;
3) at room temperature in the double-planet stirring tank, sequentially add 28kg polyurethane prepolymer A; 14kg polyurethane prepolymer B; the 5kg talcum powder; the 9kg light calcium carbonate; the 1kg active calcium oxide; the 15kgPVC resin; the 3kg aerosil; 5kg vacuum glass microballoon; the 9kg dioctyl phthalate (DOP); 0.2kg Tinuvin329; 0.2kg Tinuvin 5050; 0.3kg N-phenyl γ-aminopropyltrimethoxysilane; 0.3kg aluminium octoate linking agent; under vacuum protection, mix; be warming up to 68 ℃; reacted 2 hours; be cooled to 40 ℃; the ketoimine and the 80g dibutyltin dilaurate that add 0.5kg; stir, can obtain thixotropic single-component low-modulus polyurethane building sealant.
It is good to the seal gum thickening effectiveness that polyvinyl chloride resin can reach the maximum swelling coefficient at 70 degree, and its effective ingredient glass tiny balloon can reduce the modulus of seal gum.
Good, the anti-xanthochromia of elongation of the present invention, good weatherability, low, solvent-free, the environmental protection of modulus, to pottery, glass, concrete structure, timber, plastic-steel, painted steel sheet, aluminium alloy possess excellent adhesiveproperties, the roofing, exterior wall, vault, the seam of toilet, the sealing of waterproofing node that can be used for buildings, the insert windowpane, the expansion joint of concrete structure, the sealing of settlement joint construction joint, and motorway, bridge tunnel, the filleting of the civil engineering works such as subway, airfield runway.
Embodiment
Polyurethane prepolymer A is that diphenylmethanediisocyanate and polyether-tribasic alcohol reaction generate, and polyurethane prepolymer B is that 1-6-hexamethylene diisocyanate and polyether Glycols react generation under dibutyltin dilaurate.
Polyurethane prepolymer A28kg, polyurethane prepolymer B14kg, talcum powder 5kg, light calcium carbonate 9kg, active calcium oxide 1kg, polyvinyl chloride resin 15kg, aerosil 3kg, vacuum glass microballoon 5kg, dioctyl phthalate (DOP) 19kg, Tinuvin329 are that 0.2kg, Tinuvin5050 are 0.2kg, N-phenyl γ-aminopropyltrimethoxysilane 0.3kg, aluminium octoate linking agent 0.38kg, ketoimine 0.58kg, dibutyltin dilaurate 0.08kg.
The preparation process of described single-component low-modulus polyurethane building sealant:
1) gets in the polyether-tribasic alcohol adding vacuum reaction still of 85kg, allow polyether-tribasic alcohol under 110 ℃ vacuum environment, dewater 2 hours, make the moisture in the polyether-tribasic alcohol be not more than 0.01%, then after the temperature of charge in the vacuum reaction still being down to 50 ℃, add the 15kg diphenylmethanediisocyanate, under nitrogen protection, stir, be heated to 82 ℃, allow polyether-tribasic alcohol and diphenylmethanediisocyanate react 4 hours, obtain polyurethane prepolymer A;
2) polyether Glycols of getting 90kg is put into the vacuum reaction still, allow polyether Glycols under 110 ℃ vacuum environment, dewater 2 hours, make the moisture content in the polyether Glycols be not more than 0.01%, then the temperature of charge in the vacuum reaction still is down to 50 ℃, in the vacuum reaction still, add 10kg 1-6-hexamethylene diisocyanate, stir, add the 10g dibutyltin dilaurate, under nitrogen protection, temperature in the vacuum reaction still is risen to 92 ℃, allow polyether Glycols and 1-6-hexamethylene diisocyanate react 6 hours, get polyurethane prepolymer B;
3) at room temperature in the double-planet stirring tank, sequentially add 28kg polyurethane prepolymer A; 14kg polyurethane prepolymer B; the 5kg talcum powder; the 9kg light calcium carbonate; the 1kg active calcium oxide; the 15kgPVC resin; the 3kg aerosil; 5kg vacuum glass microballoon; the 9kg dioctyl phthalate (DOP); 0.2kg Tinuvin329; 0.2kg Tinuvin 5050; 0.3kg N-phenyl γ-aminopropyltrimethoxysilane; 0.3kg aluminium octoate linking agent; under vacuum protection, mix; be warming up to 68 ℃; reacted 2 hours; be cooled to 40 ℃; the ketoimine and the 80g dibutyltin dilaurate that add 0.5kg; stir, can obtain thixotropic single-component low-modulus polyurethane building sealant.
Claims (8)
1. single-component low-modulus polyurethane building sealant, it is characterized in that, its composition comprises altogether 30-60% of polyurethane prepolymer A and polyurethane prepolymer B, and the weight part ratio of polyurethane prepolymer A and polyurethane prepolymer B is 3～1, silane coupling agent 0.25-2.5%, aluminium octoate linking agent 0.25-2.5%, latent curing agent 0.301-0.35%, softening agent 10-40%, filler 10-60%, UV light absorber and stablizer 0.1-3%, the content of above-mentioned each component is in the quality percentage composition; Wherein polyurethane prepolymer A is that diphenylmethanediisocyanate and polyol compound reaction generate, and polyurethane prepolymer B is that 1-6-hexamethylene diisocyanate and polyol compound react generation under dibutyltin dilaurate.
2. described single-component low-modulus polyurethane building sealant according to claim 1, it is characterized in that, silane coupling agent is selected N-phenyl-γ-aminopropyltrimethoxysilane, latent curing agent is selected the mixture of ketoimine and dibutyltin dilaurate, softening agent is selected dioctyl phthalate (DOP), filler is selected talcum powder, active calcium oxide, light calcium carbonate, polyvinyl chloride resin, aerosil, vacuum glass microballoon, UV light absorber is selected Tinuvin329, and stablizer is selected Tinuvin5050.
3. described single-component low-modulus polyurethane building sealant according to claim 1 is characterized in that polyol compound is to choose any one kind of them or several combination from polyether glycol, polyester polyol.
4. described single-component low-modulus polyurethane building sealant according to claim 1, it is characterized in that, silane coupling agent is from gamma-methyl allyl acyloxypropyl trimethylammonium TMOS, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-sulfenyl propyl trimethoxy silicane is chosen any one kind of them or several combination in γ-aminopropyltrimethoxysilane, the N-phenyl-γ-aminopropyltrimethoxysilane.
5. described single-component low-modulus polyurethane building sealant according to claim 1 is characterized in that softening agent is to choose any one kind of them or several combination from phthalate, alkyl sulfonates, clorafin.
6. described single-component low-modulus polyurethane building sealant according to claim 1 is characterized in that, UV light absorber be from Whitfield's ointment, benzophenone class, benzotriazole category, triazines is chosen any one kind of them or several combination, stablizer is selected hindered amine light stabilizer.
7. described single-component low-modulus polyurethane building sealant according to claim 1, it is characterized in that, select and choose any one kind of them in active calcium oxide, silicon powder, carbon black, talcum powder, titanium dioxide, the kaolin or several and vacuum glass microballoon and polyvinyl chloride resin are mixed into filler.
8. the preparation process of described single-component low-modulus polyurethane building sealant according to claim 1 is characterized in that:
1) getting polyol compound adds in the vacuum reaction still, allow polyol compound under 110 ℃ vacuum environment, dewater 2 hours, make the moisture in the polyol compound be not more than 0.01%, then after the temperature of charge in the vacuum reaction still being down to 50 ℃, add diphenylmethanediisocyanate, under nitrogen protection, stir, be heated to 82 ℃, allow polyol compound and diphenylmethanediisocyanate react 4 hours, obtain polyurethane prepolymer A;
2) get polyol compound and put into the vacuum reaction still, allow polyol compound under 110 ℃ vacuum environment, dewater 2 hours, make the moisture content in the polyol compound be not more than 0.01%, then the temperature of charge in the vacuum reaction still is down to 50 ℃, in the vacuum reaction still, add the 1-6-hexamethylene diisocyanate, stir, add dibutyltin dilaurate, under nitrogen protection, temperature in the vacuum reaction still is risen to 92 ℃, allow polyol compound and 1-6-hexamethylene diisocyanate react 6 hours, obtain polyurethane prepolymer B;
3) at room temperature the order in the double-planet reactor adds softening agent, filler, polyurethane prepolymer A, polyurethane prepolymer B, silane coupling agent, aluminium octoate linking agent, UV light absorber, stablizer and mixes under vacuum protection; be warming up to 68 ℃; reacted 2 hours; be cooled to 40 ℃; add latent curing agent; stir, can obtain thixotropic single-component low-modulus polyurethane building sealant.
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