CN105368366A - Silane-terminated polyether sealant and preparation method thereof - Google Patents
Silane-terminated polyether sealant and preparation method thereof Download PDFInfo
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- CN105368366A CN105368366A CN201510937460.1A CN201510937460A CN105368366A CN 105368366 A CN105368366 A CN 105368366A CN 201510937460 A CN201510937460 A CN 201510937460A CN 105368366 A CN105368366 A CN 105368366A
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- C09K3/1006—Materials in mouldable or extrudable form for sealing or packing joints or covers characterised by the chemical nature of one of its constituents
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Abstract
The invention discloses silane-terminated polyether sealant. The sealant is prepared from silane-terminated polyether resin, plasticizer, a thixotropic agent, bonding accelerant, modified isocyanate polymer and the like, the main chain of the sealant is polyether, the end group of the sealant is hydrolysable silane, no bubble is generated in the curing process, no isocyanate group is contained, no contaminant is generated on the surface of the sealant, no contamination is caused to a substrate when the sealant is used, and the good adhesive property, good weatherability, high tensile strength and high shearing strength are achieved; the silane-terminated polyether sealant is good in elasticity, excellent in restoration property and applicable to a dynamic seam; by means of the silane-terminated polyether sealant, the problem that after existing sealant is cured, paintability is poor is particularly solved; the silane-terminated polyether sealant is few in preparation method procedure, the steps are easy to operate, and industrialized production is facilitated.
Description
Technical field
The present invention relates to seal gum technical field, is a kind of silane-terminated polyether seal gum and preparation method thereof specifically.
Background technology
Seal gum is generally used for first-class road, bridge, airstrips etc. have caulking sealing and the water drain of retractility seam, the connection sealing of the joint of low gas line, therefore very high requirement is proposed to the performance of seal gum, not only to there is high tensile strength, excellent elasticity, also require that its paintable is good, can be combined well with coating, the normally used seal gum of present people has the organosilicon sealant of self-vulcanizing and the polyurethane sealant of moisture-curable, organosilicon sealant temperature tolerance and having excellent weather resistance, but cohesive strength is lower and residual small molecules easily produces surface contaminant, ornamental difference, and polyurethane sealant cohesive strength is high, good springiness, low temperature resistant, oil resistant and anti-vibration but carbonic acid gas can be released when solidifying, very easily bubble and even crack, flame retardant resistance, temperature tolerance, wet-heat resisting are poor, and silane coupling agent is used to bonding needs of the material such as aluminium and glass, otherwise adhesiveproperties is poor, and isocyanate group free after solidification has fixed toxicity, thus affect its use.Silane-terminated polyether seal gum is as novel seal gum kind, combine the advantage of organosilicon sealant and polyurethane sealant, but the difference of polyethers, blocking modification material and synthesis technique of existing silane-terminated polyether seal gum owing to selecting, its agent structure causes its paintable poor.
Summary of the invention
For solving the problem, the object of this invention is to provide a kind of silane-terminated polyether seal gum and preparation method thereof.
The present invention for achieving the above object, is achieved through the following technical solutions:
A kind of silane-terminated polyether seal gum, with parts by weight, be made up of following raw material: silane-terminated polyether resin 25 ~ 50 parts, 10 ~ 20 parts, softening agent, water-removal agent 0.5 ~ 1.5 part, filler 25 ~ 35 parts, pigment 5 ~ 15 parts, thixotropic agent 0.5 ~ 5 part, adhesion promoters 0.5 ~ 1.5 part, modified isocyanate polymer 5 ~ 10 parts, photostabilizer 0.2 ~ 0.7 part, antioxidant 0.3 ~ 0.8 part and catalyzer 0.05 ~ 0.5 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 25000 ~ 35000; Described softening agent is DINP, DIDP, DOP or MESAMOLL; Described water-removal agent is molecular sieve, vinyltrimethoxy silane or tosic acid isocyanic ester; Described filler is light calcium carbonate, nano-calcium carbonate, kaolin or talcum powder; Described pigment is titanium dioxide or colour black; Described thixotropic agent is polyamide modified hydrogenated castor oil, polymeric amide or aerosil; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane or γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765, UV-1 or UV-326; Described antioxidant is 1076 or 1010; Described catalyzer is dibutyl tin laurate, dibutyl tin dichloride, isocaprylic acid lead or organic chelated tin; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing active group in isocyanic ester polymer, reacts 2 ~ 3 hours at 45 ~ 55 DEG C; Described silane containing active group and the polymeric mass ratio of isocyanic ester are 0.1 ~ 1:1; Described active group is amino or sulfydryl; Described isocyanic ester polymer is TDI tripolymer, HDI tripolymer, IPDI tripolymer or HDI biuret.
Preferred a kind of silane-terminated polyether seal gum, the silane containing active group is N-phenyl-γ-aminopropyltrimethoxysilane, ethyl-γ-ammonia trimethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyl triethoxysilane, γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane, γ-ureido-propyl Trimethoxy silane or γ-aminopropyltrimethoxysilane.
Preferred a kind of silane-terminated polyether seal gum, isocyanic ester polymer is TDI tripolymer.
Preferred a kind of silane-terminated polyether seal gum, the particle diameter of polymeric amide is 1 ~ 16 μm, and activation temperature is 55 ~ 65 DEG C; Specific surface area 30 ~ the 70m of described aerosil
2/ g.
Further preferred a kind of silane-terminated polyether seal gum, with parts by weight, be made up of following raw material: silane-terminated polyether resin 40 parts, 15 parts, softening agent, water-removal agent 1.0 parts, filler 30 parts, pigment 10 parts, thixotropic agent 0.8 part, adhesion promoters 0.8 part, modified isocyanate polymer 8 parts, photostabilizer 0.5 part, antioxidant 0.6 part and catalyzer 0.1 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 30000; Described softening agent is DINP; Described water-removal agent is molecular sieve; Described filler is nano-calcium carbonate; Described pigment is titanium dioxide; Described thixotropic agent is specific surface area 50m
2the aerosil of/g; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765; Described antioxidant is 1076; Described catalyzer is dibutyl tin laurate; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing active group in isocyanic ester polymer, reacts 2.5 hours at 50 DEG C; Described silane containing active group and the polymeric mass ratio of isocyanic ester are 0.5:1; Described active group is amino; Described isocyanic ester polymer is TDI tripolymer.
The present invention also comprises the preparation method of silane-terminated polyether seal gum, comprises the following steps:
silane containing active group is added drop-wise in isocyanic ester polymer, reacts 2 ~ 3 hours at 45 ~ 55 DEG C, obtain modified isocyanate polymer; Described silane containing active group and the polymeric mass ratio of isocyanic ester are 0.1 ~ 1:1; Described active group is amino or sulfydryl; Described isocyanic ester polymer is TDI tripolymer, HDI tripolymer, IPDI tripolymer or HDI biuret;
with parts by weight, by silane-terminated polyether resin 25 ~ 50 parts, 10 ~ 20 parts, softening agent, filler 25 ~ 35 parts, pigment 5 ~ 15 parts and thixotropic agent 0.5 ~ 5 part add in reactor successively, 95 ~ 105 DEG C are heated under vacuum stirring, mix and be cooled to 45 ~ 55 DEG C after 2 hours, add water-removal agent 0.5 ~ 1.5 part dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 25000 ~ 35000; Described softening agent is DINP, DIDP, DOP or MESAMOLL; Described filler is light calcium carbonate, nano-calcium carbonate, kaolin or talcum powder; Described pigment is titanium dioxide or colour black; Described thixotropic agent is polyamide modified hydrogenated castor oil, polymeric amide or aerosil; Described water-removal agent is molecular sieve, vinyltrimethoxy silane or tosic acid isocyanic ester;
with parts by weight, by step
gained modified isocyanate polymer 5 ~ 10 parts joins step
in gained mixed solution, stir, add adhesion promoters 0.5 ~ 1.5 part, photostabilizer 0.2 ~ 0.7 part, antioxidant 0.3 ~ 0.8 part and catalyzer 0.05 ~ 0.5 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane or γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765, UV-1 or UV-326; Described antioxidant is 1076 or 1010; Described catalyzer is dibutyl tin laurate, dibutyl tin dichloride, isocaprylic acid lead or organic chelated tin.
The preparation method of preferred silane-terminated polyether seal gum, the silane containing active group is N-phenyl-γ-aminopropyltrimethoxysilane, ethyl-γ-ammonia trimethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyl triethoxysilane, γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane, γ-ureido-propyl Trimethoxy silane or γ-aminopropyltrimethoxysilane.
The preparation method of preferred silane-terminated polyether seal gum further, comprises the following steps:
the silane that 5 weight parts contain active group is added drop-wise in the isocyanic ester polymer of 10 weight parts, reacts 2.5 hours at 50 DEG C, obtain modified isocyanate polymer; Described containing with the polymeric mass ratio of isocyanic ester is 0.5:1; The described silane containing active group is ethyl-γ-ammonia trimethoxysilane; Described isocyanic ester polymer is TDI tripolymer;
with parts by weight, by silane-terminated polyether resin 40 parts, 15 parts, softening agent, filler 30 parts, pigment 10 parts and thixotropic agent 0.8 part add in reactor successively, are heated to 100 DEG C under vacuum stirring, mix and are cooled to 50 DEG C after 2 hours, add water-removal agent 1.0 parts dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 30000; Described softening agent is DINP; Described filler is nano-calcium carbonate; Described pigment is titanium dioxide; Described thixotropic agent is aerosil; Described water-removal agent is molecular sieve;
with parts by weight, by step
gained modified isocyanate polymer 8 parts joins step
in gained mixed solution, stir, add adhesion promoters 0.8 part, photostabilizer 0.5 part, antioxidant 0.6 part and catalyzer 0.1 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765; Described antioxidant is 1076; Described catalyzer is dibutyl tin laurate.
The present invention has the following advantages compared to existing technology:
Seal gum prepared by silane-terminated polyether seal gum of the present invention polymkeric substance based on silane modified polymer, its main chain is polyethers, end group is hydrolyzable silane, non-foaming during solidification, not isocyanato group containing group, surface can not produce pollutent, uses base material pollution-free, and there is good cementability, weathering resistance, high tensile strength, high shearing resistance; Silane-terminated polyether seal gum good springiness of the present invention, has excellent Restoration, can be used for dynamic juncture; Silane-terminated polyether seal gum of the present invention especially solves the poor problem of paintable after existing sealing glue solidifying; Preparation method's flow process of silane-terminated polyether seal gum of the present invention is few, and step easy handling is with short production cycle, is convenient to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the detection figure of embodiment 5 gained silane-terminated polyether seal gum paintable;
Fig. 2 is the detection figure of certain polyurethane sealant paintable on market.
Embodiment
The object of this invention is to provide a kind of heat-resisting water-resisting type high strength polyurethane adhesive and preparation method thereof, be achieved through the following technical solutions:
A kind of silane-terminated polyether seal gum, with parts by weight, be made up of following raw material: silane-terminated polyether resin 25 ~ 50 parts, 10 ~ 20 parts, softening agent, water-removal agent 0.5 ~ 1.5 part, filler 25 ~ 35 parts, pigment 5 ~ 15 parts, thixotropic agent 0.5 ~ 5 part, adhesion promoters 0.5 ~ 1.5 part, modified isocyanate polymer 5 ~ 10 parts, photostabilizer 0.2 ~ 0.7 part, antioxidant 0.3 ~ 0.8 part and catalyzer 0.05 ~ 0.5 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 25000 ~ 35000; Described softening agent is DINP, DIDP, DOP or MESAMOLL; Described water-removal agent is molecular sieve, vinyltrimethoxy silane or tosic acid isocyanic ester; Described filler is light calcium carbonate, nano-calcium carbonate, kaolin or talcum powder; Described pigment is titanium dioxide or colour black; Described thixotropic agent is polyamide modified hydrogenated castor oil, polymeric amide or aerosil; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane or γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765, UV-1 or UV-326; Described antioxidant is 1076 or 1010; Described catalyzer is dibutyl tin laurate, dibutyl tin dichloride, isocaprylic acid lead or organic chelated tin; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing active group in isocyanic ester polymer, reacts 2 ~ 3 hours at 45 ~ 55 DEG C; Described silane containing active group and the polymeric mass ratio of isocyanic ester are 0.1 ~ 1:1; Described active group is amino or sulfydryl; Described isocyanic ester polymer is TDI tripolymer, HDI tripolymer, IPDI tripolymer or HDI biuret.
Preferred a kind of silane-terminated polyether seal gum, the silane containing active group is N-phenyl-γ-aminopropyltrimethoxysilane, ethyl-γ-ammonia trimethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyl triethoxysilane, γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane, γ-ureido-propyl Trimethoxy silane or γ-aminopropyltrimethoxysilane.
Preferred a kind of silane-terminated polyether seal gum, isocyanic ester polymer is TDI tripolymer.
Preferred a kind of silane-terminated polyether seal gum, the particle diameter of polymeric amide is 1 ~ 16 μm, and activation temperature is 55 ~ 65 DEG C; Specific surface area 30 ~ the 70m of described aerosil
2/ g.
Further preferred a kind of silane-terminated polyether seal gum, with parts by weight, be made up of following raw material: silane-terminated polyether resin 40 parts, 15 parts, softening agent, water-removal agent 1.0 parts, filler 30 parts, pigment 10 parts, thixotropic agent 0.8 part, adhesion promoters 0.8 part, modified isocyanate polymer 8 parts, photostabilizer 0.5 part, antioxidant 0.6 part and catalyzer 0.1 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 30000; Described softening agent is DINP; Described water-removal agent is molecular sieve; Described filler is nano-calcium carbonate; Described pigment is titanium dioxide; Described thixotropic agent is specific surface area 50m
2the aerosil of/g; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765; Described antioxidant is 1076; Described catalyzer is dibutyl tin laurate; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing active group in isocyanic ester polymer, reacts 2.5 hours at 50 DEG C; Described silane containing active group and the polymeric mass ratio of isocyanic ester are 0.5:1; Described active group is amino; Described isocyanic ester polymer is TDI tripolymer.
The present invention also comprises the preparation method of silane-terminated polyether seal gum, comprises the following steps:
silane containing active group is added drop-wise in isocyanic ester polymer, reacts 2 ~ 3 hours at 45 ~ 55 DEG C, obtain modified isocyanate polymer; Described silane containing active group and the polymeric mass ratio of isocyanic ester are 0.1 ~ 1:1; Described active group is amino or sulfydryl; Described isocyanic ester polymer is TDI tripolymer, HDI tripolymer, IPDI tripolymer or HDI biuret;
with parts by weight, by silane-terminated polyether resin 25 ~ 50 parts, 10 ~ 20 parts, softening agent, filler 25 ~ 35 parts, pigment 5 ~ 15 parts and thixotropic agent 0.5 ~ 5 part add in reactor successively, 95 ~ 105 DEG C are heated under vacuum stirring, mix and be cooled to 45 ~ 55 DEG C after 2 hours, add water-removal agent 0.5 ~ 1.5 part dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 25000 ~ 35000; Described softening agent is DINP, DIDP, DOP or MESAMOLL; Described filler is light calcium carbonate, nano-calcium carbonate, kaolin or talcum powder; Described pigment is titanium dioxide or colour black; Described thixotropic agent is polyamide modified hydrogenated castor oil, polymeric amide or aerosil; Described water-removal agent is molecular sieve, vinyltrimethoxy silane or tosic acid isocyanic ester;
with parts by weight, by step
gained modified isocyanate polymer 5 ~ 10 parts joins step
in gained mixed solution, stir, add adhesion promoters 0.5 ~ 1.5 part, photostabilizer 0.2 ~ 0.7 part, antioxidant 0.3 ~ 0.8 part and catalyzer 0.05 ~ 0.5 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane or γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765, UV-1 or UV-326; Described antioxidant is 1076 or 1010; Described catalyzer is dibutyl tin laurate, dibutyl tin dichloride, isocaprylic acid lead or organic chelated tin.
The preparation method of preferred silane-terminated polyether seal gum, the silane containing active group is N-phenyl-γ-aminopropyltrimethoxysilane, ethyl-γ-ammonia trimethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyl triethoxysilane, γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane, γ-ureido-propyl Trimethoxy silane or γ-aminopropyltrimethoxysilane.
The preparation method of preferred silane-terminated polyether seal gum further,
the silane that 5 weight parts contain active group is added drop-wise in the isocyanic ester polymer of 10 weight parts, reacts 2.5 hours at 50 DEG C, obtain modified isocyanate polymer; Described containing with the polymeric mass ratio of isocyanic ester is 0.5:1; The described silane containing active group is ethyl-γ-ammonia trimethoxysilane; Described isocyanic ester polymer is TDI tripolymer;
with parts by weight, by silane-terminated polyether resin 40 parts, 15 parts, softening agent, filler 30 parts, pigment 10 parts and thixotropic agent 0.8 part add in reactor successively, are heated to 100 DEG C under vacuum stirring, mix and are cooled to 50 DEG C after 2 hours, add water-removal agent 1.0 parts dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 30000; Described softening agent is DINP; Described filler is nano-calcium carbonate; Described pigment is titanium dioxide; Described thixotropic agent is aerosil; Described water-removal agent is molecular sieve;
with parts by weight, by step
gained modified isocyanate polymer 8 parts joins step
in gained mixed solution, stir, add adhesion promoters 0.8 part, photostabilizer 0.5 part, antioxidant 0.6 part and catalyzer 0.1 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765; Described antioxidant is 1076; Described catalyzer is dibutyl tin laurate.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of silane-terminated polyether seal gum, with parts by weight, be made up of following raw material: silane-terminated polyether resin 25 parts, 10 parts, softening agent, water-removal agent 0.5 part, filler 25 parts, pigment 5 parts, thixotropic agent 0.5 part, adhesion promoters 0.5 part, modified isocyanate polymer 5 parts, photostabilizer 0.2 part, antioxidant 0.3 part and catalyzer 0.05 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 25000; Described softening agent is DINP; Described water-removal agent is molecular sieve; Described filler is light calcium carbonate; Described pigment is titanium dioxide; Described thixotropic agent is polyamide modified hydrogenated castor oil; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765; Described antioxidant is 1076; Described catalyzer is dibutyl tin laurate; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing amino active group in isocyanic ester polymer, reacts 2 hours at 45 DEG C; Described silane containing amino active group and the polymeric mass ratio of isocyanic ester are 0.1:1; Described isocyanic ester polymer is TDI tripolymer, and the described silane containing amino active group is N-phenyl-γ-aminopropyltrimethoxysilane.
Embodiment 2
A kind of silane-terminated polyether seal gum, with parts by weight, be made up of following raw material: silane-terminated polyether resin 50 parts, 20 parts, softening agent, water-removal agent 1.5 parts, filler 35 parts, pigment 15 parts, thixotropic agent 5 parts, adhesion promoters 1.5 parts, modified isocyanate polymer 10 parts, photostabilizer 0.7 part, antioxidant 0.8 part and catalyzer 0.5 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 35000; Described softening agent is DIDP; Described water-removal agent is vinyltrimethoxy silane; Described filler is nano-calcium carbonate; Described pigment is colour black; Described thixotropic agent is polymeric amide; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-1; Described antioxidant is 1010; Described catalyzer is dibutyl tin dichloride; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing sulfhydryl reactive group in isocyanic ester polymer, reacts 3 hours at 55 DEG C; Described silane containing sulfhydryl reactive group and the polymeric mass ratio of isocyanic ester are 1:1; The described silane containing sulfhydryl reactive group is γ-mercaptopropyl trimethoxysilane; Described isocyanic ester polymer is HDI tripolymer.
Embodiment 3
A kind of silane-terminated polyether seal gum, with parts by weight, be made up of following raw material: silane-terminated polyether resin 30 parts, 14 parts, softening agent, water-removal agent 0.9 part, filler 28 parts, pigment 7 parts, thixotropic agent 2 parts, adhesion promoters 0.8 part, modified isocyanate polymer 9 parts, photostabilizer 0.6 part, antioxidant 0.4 part and catalyzer 0.2 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 28000; Described softening agent is DOP; Described water-removal agent is tosic acid isocyanic ester; Described filler is kaolin; Described pigment is titanium dioxide; Described thixotropic agent is aerosil; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-326; Described antioxidant is 1010; Described catalyzer is that isocaprylic acid is plumbous; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing amino active group in isocyanic ester polymer, reacts 2.5 hours at 48 DEG C; Described silane containing amino active group and the polymeric mass ratio of isocyanic ester are 0.6:1; The silane of described amino active group is ethyl-γ-ammonia trimethoxysilane; Described isocyanic ester polymer is IPDI tripolymer.
Embodiment 4
A kind of silane-terminated polyether seal gum, with parts by weight, be made up of following raw material: silane-terminated polyether resin 40 parts, 16 parts, softening agent, water-removal agent 1.2 parts, filler 32 parts, pigment 12 parts, thixotropic agent 4 parts, adhesion promoters 1.2 parts, modified isocyanate polymer 8 parts, photostabilizer 0.6 part, antioxidant 0.4 part and catalyzer 0.3 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 32000; Described softening agent is MESAMOLL; Described water-removal agent is molecular sieve; Described filler is talcum powder; Described pigment is colour black; Described thixotropic agent is specific surface area is 30m
2the aerosil of/g; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-326; Described antioxidant is 1076; Described catalyzer is organic chelated tin; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing sulfhydryl reactive group in isocyanic ester polymer, reacts 2.5 hours at 52 DEG C; Described silane containing sulfhydryl reactive group and the polymeric mass ratio of isocyanic ester are 0.8:1; The described silane containing sulfhydryl reactive group is γ-mercaptopropyl trimethoxysilane; Described isocyanic ester polymer is HDI biuret.
Embodiment 5
A kind of silane-terminated polyether seal gum, with parts by weight, be made up of following raw material: silane-terminated polyether resin 40 parts, 15 parts, softening agent, water-removal agent 1.0 parts, filler 30 parts, pigment 10 parts, thixotropic agent 0.8 part, adhesion promoters 0.8 part, modified isocyanate polymer 8 parts, photostabilizer 0.5 part, antioxidant 0.6 part and catalyzer 0.1 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 30000; Described softening agent is DINP; Described water-removal agent is molecular sieve; Described filler is nano-calcium carbonate; Described pigment is titanium dioxide; Described thixotropic agent is specific surface area 50m
2the aerosil of/g; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765; Described antioxidant is 1076; Described catalyzer is dibutyl tin laurate; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing active group in isocyanic ester polymer, reacts 2.5 hours at 50 DEG C; Described silane containing active group and the polymeric mass ratio of isocyanic ester are 0.5:1; Described active group is amino; Described isocyanic ester polymer is TDI tripolymer.
Embodiment 6
The preparation method of the silane-terminated polyether seal gum described in embodiment 1, comprises the following steps:
silane containing amino active group is added drop-wise in isocyanic ester polymer, reacts 2 hours at 45 DEG C; Described silane containing amino active group and the polymeric mass ratio of isocyanic ester are 0.1:1; Described isocyanic ester polymer is TDI tripolymer, and the described silane containing amino active group is N-phenyl-γ-aminopropyltrimethoxysilane;
with parts by weight, by silane-terminated polyether resin 25 parts, 10 parts, softening agent, filler 25 parts, pigment 5 parts and thixotropic agent 0.5 part add in reactor successively, are heated to 95 DEG C under vacuum stirring, mix and are cooled to 45 DEG C after 2 hours, add water-removal agent 0.5 part dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 25000; Described softening agent is DINP; Described filler is light calcium carbonate; Described pigment is titanium dioxide; Described thixotropic agent is polyamide modified hydrogenated castor oil; Described water-removal agent is molecular sieve;
with parts by weight, by step
gained modified isocyanate polymer 5 parts joins step
in gained mixed solution, stir, add adhesion promoters 0.5 part, photostabilizer 0.2 part, antioxidant 0.3 part and catalyzer 0.05 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765; Described antioxidant is 1076; Described catalyzer is dibutyl tin laurate.
Embodiment 7
The preparation method of the silane-terminated polyether seal gum described in embodiment 2, comprises the following steps:
silane containing sulfhydryl reactive group is added drop-wise in isocyanic ester polymer, reacts 3 hours at 55 DEG C; Described silane containing sulfhydryl reactive group and the polymeric mass ratio of isocyanic ester are 1:1; The described silane containing sulfhydryl reactive group is γ-mercaptopropyl trimethoxysilane; Described isocyanic ester polymer is HDI tripolymer;
with parts by weight, by silane-terminated polyether resin 50 parts, 20 parts, softening agent, filler 35 parts, pigment 15 parts and thixotropic agent 5 parts add in reactor successively, are heated to 105 DEG C under vacuum stirring, mix and are cooled to 55 DEG C after 2 hours, add water-removal agent 1.5 parts dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 35000; Described softening agent is DIDP; Described filler is nano-calcium carbonate; Described pigment is colour black; Described thixotropic agent is polymeric amide; Described water-removal agent is vinyltrimethoxy silane;
with parts by weight, by step
gained modified isocyanate polymer 10 parts joins step
in gained mixed solution, stir, add adhesion promoters 1.5 parts, photostabilizer 0.7 part, antioxidant 0.8 part and catalyzer 0.5 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-1; Described antioxidant is 1010; Described catalyzer is dibutyl tin dichloride.
Embodiment 8
The preparation method of the silane-terminated polyether seal gum described in embodiment 3, comprises the following steps:
silane containing amino active group is added drop-wise in isocyanic ester polymer, reacts 2.5 hours at 48 DEG C; Described silane containing amino active group and the polymeric mass ratio of isocyanic ester are 0.6:1; The silane of described amino active group is ethyl-γ-ammonia trimethoxysilane; Described isocyanic ester polymer is IPDI tripolymer;
with parts by weight, by silane-terminated polyether resin 30 parts, 14 parts, softening agent,, filler 28 parts, pigment 7 parts and thixotropic agent 2 parts add in reactor successively, are heated to 100 DEG C under vacuum stirring, mix and be cooled to 48 DEG C after 2 hours, add water-removal agent 0.9 part dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 28000; Described softening agent is DOP; Described water-removal agent is tosic acid isocyanic ester; Described filler is kaolin; Described pigment is titanium dioxide; Described thixotropic agent is aerosil;
with parts by weight, by step
gained modified isocyanate polymer 9 parts joins step
in gained mixed solution, stir, add adhesion promoters 0.8 part, photostabilizer 0.6 part, antioxidant 0.4 part and catalyzer 0.2 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-326; Described antioxidant is 1010; Described catalyzer is that isocaprylic acid is plumbous.
Embodiment 9
The preparation method of the silane-terminated polyether seal gum described in embodiment 4, comprises the following steps:
silane containing sulfhydryl reactive group is added drop-wise in isocyanic ester polymer, reacts 2.5 hours at 52 DEG C; Described silane containing sulfhydryl reactive group and the polymeric mass ratio of isocyanic ester are 0.8:1; The described silane containing sulfhydryl reactive group is γ-mercaptopropyl trimethoxysilane; Described isocyanic ester polymer is HDI biuret;
with parts by weight, by silane-terminated polyether resin 40 parts, 16 parts, softening agent, filler 32 parts, pigment 12 parts and thixotropic agent 4 parts add in reactor successively, are heated to 98 DEG C under vacuum stirring, mix and are cooled to 52 DEG C after 2 hours, add water-removal agent 1.2 parts dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 32000; Described softening agent is DINP, DIDP, DOP or MESAMOLL; Described softening agent is MESAMOLL; Described water-removal agent is molecular sieve; Described filler is talcum powder; Described pigment is colour black; Described thixotropic agent is specific surface area is 30m
2the aerosil of/g; ;
with parts by weight, by step
gained modified isocyanate polymer 8 parts joins step
in gained mixed solution, stir, add adhesion promoters 1.2 parts, photostabilizer 0.6 part, antioxidant 0.4 part and catalyzer 0.3 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-326; Described antioxidant is 1076; Described catalyzer is organic chelated tin.
Embodiment 10
The preparation method of the silane-terminated polyether seal gum described in embodiment 5, comprises the following steps:
the silane that 5 weight parts contain active group is added drop-wise in the isocyanic ester polymer of 10 weight parts, reacts 2.5 hours at 50 DEG C, obtain modified isocyanate polymer; Described containing with the polymeric mass ratio of isocyanic ester is 0.5:1; The described silane containing active group is ethyl-γ-ammonia trimethoxysilane; Described isocyanic ester polymer is TDI tripolymer;
with parts by weight, by silane-terminated polyether resin 40 parts, 15 parts, softening agent, filler 30 parts, pigment 10 parts and thixotropic agent 0.8 part add in reactor successively, are heated to 100 DEG C under vacuum stirring, mix and are cooled to 50 DEG C after 2 hours, add water-removal agent 1.0 parts dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 30000; Described softening agent is DINP; Described filler is nano-calcium carbonate; Described pigment is titanium dioxide; Described thixotropic agent is aerosil; Described water-removal agent is molecular sieve;
with parts by weight, by step
gained modified isocyanate polymer 8 parts joins step
in gained mixed solution, stir, add adhesion promoters 0.8 part, photostabilizer 0.5 part, antioxidant 0.6 part and catalyzer 0.1 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765; Described antioxidant is 1076; Described catalyzer is dibutyl tin laurate.
1. embodiment 1 ~ 5 gained silane-terminated polyether seal gum is carried out physical and mechanical property test, result is as shown in table 1.
Tensile strength and elongation at break press the mensuration of GB/T528-2009 vulcanized rubber and thermoplastic elastomer tensile stress-strain performance.
The physical and mechanical property test result of table 1 embodiment 1 ~ 5 gained silane-terminated polyether seal gum
Test item | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 |
Surface drying time/min | 35 | 32 | 25 | 30 | 20 |
Curing speed mm/24h | 3.5 | 3.6 | 3.8 | 3.8 | 4.1 |
Hardness/A | 45 | 41 | 40 | 38 | 35 |
Shearing resistance/MPa | 5.8 | 5.9 | 6.4 | 6.5 | 6.8 |
Tensile strength/MPa | 6.2 | 6.7 | 6.6 | 7.2 | 7.4 |
Elongation at break/% | 526 | 521 | 532 | 556 | 585 |
Paintable/(after solidification) | Good | Good | Good | Good | Good |
Weathering resistance | Good | Good | Good | Good | Good |
Cementability | Good | Good | Good | Good | Good |
2. embodiment 5 gained silane-terminated polyether seal gum is carried out the detection of paintable, method is as follows: by seal gum smear, after solidification, deployed component paint is coated in seal gum surface, overlay on the adhesive surface of scotch tape after film curing on the paint film on seal gum surface, strike off by identical dynamics, paint film is bonded together with scotch tape as far as possible, then takes scotch tape off and overlay on clean blank sheet of paper.Fig. 1 is the detection figure of embodiment 5 gained silane-terminated polyether seal gum paintable, Fig. 2 is the detection figure of certain polyurethane sealant paintable on market, black shade in Fig. 2 is glued by scotch tape the component paint got off, can find out that silane-terminated polyether seal gum of the present invention is not glued by scotch tape substantially by the contrast of Fig. 1 and Fig. 2, paintable is good.
Claims (8)
1. a silane-terminated polyether seal gum, it is characterized in that: with parts by weight, be made up of following raw material: silane-terminated polyether resin 25 ~ 50 parts, 10 ~ 20 parts, softening agent, water-removal agent 0.5 ~ 1.5 part, filler 25 ~ 35 parts, pigment 5 ~ 15 parts, thixotropic agent 0.5 ~ 5 part, adhesion promoters 0.5 ~ 1.5 part, modified isocyanate polymer 5 ~ 10 parts, photostabilizer 0.2 ~ 0.7 part, antioxidant 0.3 ~ 0.8 part and catalyzer 0.05 ~ 0.5 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 25000 ~ 35000; Described softening agent is DINP, DIDP, DOP or MESAMOLL; Described water-removal agent is molecular sieve, vinyltrimethoxy silane or tosic acid isocyanic ester; Described filler is light calcium carbonate, nano-calcium carbonate, kaolin or talcum powder; Described pigment is titanium dioxide or colour black; Described thixotropic agent is polyamide modified hydrogenated castor oil, polymeric amide or aerosil; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane or γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765, UV-1 or UV-326; Described antioxidant is 1076 or 1010; Described catalyzer is dibutyl tin laurate, dibutyl tin dichloride, isocaprylic acid lead or organic chelated tin; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing active group in isocyanic ester polymer, reacts 2 ~ 3 hours at 45 ~ 55 DEG C; Described silane containing active group and the polymeric mass ratio of isocyanic ester are 0.1 ~ 1:1; Described active group is amino or sulfydryl; Described isocyanic ester polymer is TDI tripolymer, HDI tripolymer, IPDI tripolymer or HDI biuret.
2. a kind of silane-terminated polyether seal gum according to claim 1, is characterized in that: the silane containing active group is N-phenyl-γ-aminopropyltrimethoxysilane, ethyl-γ-ammonia trimethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyl triethoxysilane, γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane, γ-ureido-propyl Trimethoxy silane or γ-aminopropyltrimethoxysilane.
3. a kind of silane-terminated polyether seal gum according to claim 1, is characterized in that: described isocyanic ester polymer is TDI tripolymer.
4. a kind of silane-terminated polyether seal gum according to claim 1, is characterized in that: the particle diameter of described polymeric amide is 1 ~ 16 μm, and activation temperature is 55 ~ 65 DEG C; Specific surface area 30 ~ the 70m of described aerosil
2/ g.
5. a kind of silane-terminated polyether seal gum according to claim 1, it is characterized in that: with parts by weight, be made up of following raw material: silane-terminated polyether resin 40 parts, 15 parts, softening agent, water-removal agent 1.0 parts, filler 30 parts, pigment 10 parts, thixotropic agent 0.8 part, adhesion promoters 0.8 part, modified isocyanate polymer 8 parts, photostabilizer 0.5 part, antioxidant 0.6 part and catalyzer 0.1 part; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 30000; Described softening agent is DINP; Described water-removal agent is molecular sieve; Described filler is nano-calcium carbonate; Described pigment is titanium dioxide; Described thixotropic agent is specific surface area 50m
2the aerosil of/g; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765; Described antioxidant is 1076; Described catalyzer is dibutyl tin laurate; Described modified isocyanate polymer is obtained by following steps: be added drop-wise to by the silane containing active group in isocyanic ester polymer, reacts 2.5 hours at 50 DEG C; Described silane containing active group and the polymeric mass ratio of isocyanic ester are 0.5:1; Described active group is amino; Described isocyanic ester polymer is TDI tripolymer.
6. the preparation method of a kind of silane-terminated polyether seal gum according to claim 1, is characterized in that: comprise the following steps:
silane containing active group is added drop-wise in isocyanic ester polymer, reacts 2 ~ 3 hours at 45 ~ 55 DEG C, obtain modified isocyanate polymer; Described silane containing active group and the polymeric mass ratio of isocyanic ester are 0.1 ~ 1:1; Described active group is amino or sulfydryl; Described isocyanic ester polymer is TDI tripolymer, HDI tripolymer, IPDI tripolymer or HDI biuret;
with parts by weight, by silane-terminated polyether resin 25 ~ 50 parts, 10 ~ 20 parts, softening agent, filler 25 ~ 35 parts, pigment 5 ~ 15 parts and thixotropic agent 0.5 ~ 5 part add in reactor successively, 95 ~ 105 DEG C are heated under vacuum stirring, mix and be cooled to 45 ~ 55 DEG C after 2 hours, add water-removal agent 0.5 ~ 1.5 part dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 25000 ~ 35000; Described softening agent is DINP, DIDP, DOP or MESAMOLL; Described filler is light calcium carbonate, nano-calcium carbonate, kaolin or talcum powder; Described pigment is titanium dioxide or colour black; Described thixotropic agent is polyamide modified hydrogenated castor oil, polymeric amide or aerosil; Described water-removal agent is molecular sieve, vinyltrimethoxy silane or tosic acid isocyanic ester;
with parts by weight, by step
gained modified isocyanate polymer 5 ~ 10 parts joins step
in gained mixed solution, stir, add adhesion promoters 0.5 ~ 1.5 part, photostabilizer 0.2 ~ 0.7 part, antioxidant 0.3 ~ 0.8 part and catalyzer 0.05 ~ 0.5 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane or γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765, UV-1 or UV-326; Described antioxidant is 1076 or 1010; Described catalyzer is dibutyl tin laurate, dibutyl tin dichloride, isocaprylic acid lead or organic chelated tin.
7. the preparation method of a kind of silane-terminated polyether seal gum according to claim 6, is characterized in that: the silane containing active group is N-phenyl-γ-aminopropyltrimethoxysilane, ethyl-γ-ammonia trimethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyl triethoxysilane, γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane, γ-ureido-propyl Trimethoxy silane or γ-aminopropyltrimethoxysilane.
8. the preparation method of a kind of silane-terminated polyether seal gum according to claim 6, is characterized in that: comprise the following steps:
the silane that 5 weight parts contain active group is added drop-wise in the isocyanic ester polymer of 10 weight parts, reacts 2.5 hours at 50 DEG C, obtain modified isocyanate polymer; Described containing with the polymeric mass ratio of isocyanic ester is 0.5:1; The described silane containing active group is ethyl-γ-ammonia trimethoxysilane; Described isocyanic ester polymer is TDI tripolymer;
with parts by weight, by silane-terminated polyether resin 40 parts, 15 parts, softening agent, filler 30 parts, pigment 10 parts and thixotropic agent 0.8 part add in reactor successively, are heated to 100 DEG C under vacuum stirring, mix and are cooled to 50 DEG C after 2 hours, add water-removal agent 1.0 parts dehydration 30 minutes, obtain mixed solution; The silane-terminated polyether resin of described silane-terminated polyether resin to be end group be trimethoxy, molecular weight 30000; Described softening agent is DINP; Described filler is nano-calcium carbonate; Described pigment is titanium dioxide; Described thixotropic agent is aerosil; Described water-removal agent is molecular sieve;
with parts by weight, by step
gained modified isocyanate polymer 8 parts joins step
in gained mixed solution, stir, add adhesion promoters 0.8 part, photostabilizer 0.5 part, antioxidant 0.6 part and catalyzer 0.1 part, stir, obtain silane-terminated polyether seal gum; Described adhesion promoters is N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane; Described photostabilizer is UV-765; Described antioxidant is 1076; Described catalyzer is dibutyl tin laurate.
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