CN106753178A - Dual-component polyurethane fluid sealant and preparation method thereof - Google Patents

Dual-component polyurethane fluid sealant and preparation method thereof Download PDF

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Publication number
CN106753178A
CN106753178A CN201611236624.9A CN201611236624A CN106753178A CN 106753178 A CN106753178 A CN 106753178A CN 201611236624 A CN201611236624 A CN 201611236624A CN 106753178 A CN106753178 A CN 106753178A
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parts
component
fluid sealant
dual
component polyurethane
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CN106753178B (en
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毛俊轩
熊婷
潘林
李文辉
邹明晶
车国勇
王有治
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CHENGDU GUIBAO NEW MATERIAL Co.,Ltd.
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CHENGDU GUIBAO SCIENCE AND TECHNOLOGY INDUSTRIAL Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/08—Polyurethanes from polyethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
    • C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4804—Two or more polyethers of different physical or chemical nature
    • C08G18/4808—Mixtures of two or more polyetherdiols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02—Organic and inorganic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/544—Silicon-containing compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/06—Polyurethanes from polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets

Abstract

The invention discloses a kind of dual-component polyurethane fluid sealant, including mass ratio is 4~10：1 component A and B component；Described component A is by following mass parts into being grouped into：Polyhydric alcohol polymer, 100 parts；Plasticizer, 20~100 parts；Calcium carbonate, 50~500 parts；Tackifier, 0.5~2 part；Antioxidant, 1~5 part；Described B component is by following mass parts into being grouped into：Polyisocyanates, 100 parts；Polyhydric alcohol polymer, 50~300 parts；Plasticizer, 10~50 parts；Aerosil, 5~20 parts；Catalyst, 0.5~2.0 part.Polyurethane sealant mechanical strength of the invention is high, and ageing-resistant performance is good, and curing rate is fast, and volatile matter is low, will not pollute car light lampshade, is suitable to the adhering and sealing of automobile lamp.

Description

Dual-component polyurethane fluid sealant and preparation method thereof
Technical field
The invention belongs to polymeric material field, and in particular to a kind of preparation method of dual-component polyurethane fluid sealant, should Fluid sealant is mainly used in automobile lamp.
Background technology
The automobile lamp fluid sealant for using at present is broadly divided into PUR and the major class of vulcanized rubber at room temperature two.Wherein PUR Including Thermoplastic hot melt's glue and Reactive hot melt adhesive, vulcanized rubber at room temperature is divided into single-component room temperature vulcanized glue and double-component room temperature sulphur again Change glue.
PUR is needing heating melting using preceding, and melten gel then is coated in into abutting edge, and cooling and solidifying obtains preliminary viscous Effect is connect, one of its most prominent advantage is exactly fast curing rate, adapts to quick serialization industrial production.Additionally, hot melt Glue also has anti-moisture-permeability performance excellent, the advantages of shock resistance and strong resistance to low temperature.But, Thermoplastic hot melt's glue high temperature resistant Poor-performing, adhesive strength are low, partial picture need to be mechanically fixed while use, as Vehicle lamp structure is increasingly complicated, thermoplastic The reduction of hot melt glue usability.Though and Reactive hot melt adhesive excellent combination property, price is higher, and is moisture-curable, Packaging and storage aspect requirement are higher, and its application is limited to a certain extent.
The representative products of room temperature vulcanization adhesive are single, double component organosilicone sealant, with excellent high temperature resistant, weather-proof Performance, and the performance such as the good, nontoxic pollution-free of storage stability.But, it is most of at present with the fast development of auto industry Medium-to-high grade car uses fog-proof front light, and after organosilicon sealant is applied to fog-proof front light, its high volatile can cause antifog The failure of coating, limits its application.
For case above, exploitation is needed badly a kind of fast, right with good mechanical property, ageing-resistant performance, curing rate Antifogging coating is developed rapidly without destruction and the relatively low car light fluid sealant for being easy to market to receive of price, power-assisted car industry.
The content of the invention
It is an object of the invention to provide it is a kind of with good mechanical property, ageing-resistant performance, curing rate it is fast, to antifog Coating is without destruction and the relatively low car light dual-component polyurethane fluid sealant for being easy to market to receive of price.
It is a further object to provide a kind of preparation method of dual-component polyurethane fluid sealant.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme：
A kind of dual-component polyurethane fluid sealant, including mass ratio is 4~10：1 component A and B component；
Described component A is by following mass parts into being grouped into：
Polyhydric alcohol polymer, 100 parts；
Plasticizer, 20~100 parts；
Calcium carbonate, 50~500 parts；
Tackifier, 0.5~2 part；
Antioxidant, 1~5 part；
Described B component is by following mass parts into being grouped into：
Polyisocyanates, 100 parts；
Polyhydric alcohol polymer, 50~300 parts；
Plasticizer, 10~50 parts；
Aerosil, 5~20 parts；
Catalyst, 0.5~2.0 part.
Further technical scheme is, described polyhydric alcohol polymer is selected from PPG, PEPA extremely Few one kind.
Further technical scheme is that described polyisocyanates is the compound that formula is OCN-R-NCO, wherein, R is C1~20Alkylidene, arlydene, cycloalkylidene, alkylidene aryl, alkylene cycloalkyl, arlydene alkyl, arlydene cycloalkyl, Cycloalkylidene alkyl, cycloalkylidene aryl.
Further technical scheme is that described polyisocyanates is selected from toluene di-isocyanate(TDI), the isocyanic acid of tetramethyl two Ester, benzhydryl -4,4 '-diisocyanate, 1, hexamethylene-diisocyanate, IPDI, dimethylenebenzene Diisocyanate, 4,4 '-diphenylmethane diisocyanate, to phenyl diisocyanate and its isomers, the isocyanide of 1,5- naphthalenes two Acid esters, benzhydryl -4 of halogen substitution, at least one in 4 '-diisocyanate.
Further technical scheme is that described calcium carbonate is that mass ratio is 1~10：10~1 precipitated calcium carbonate and weight The mixture of matter calcium carbonate.
Further technical scheme is that described plasticizer is selected from commercially available alkane oil, aromatic naphtha, phthalic acid ester At least one.
Further technical scheme is that described tackifier are selected from aminopropyl trimethoxysilane, aminopropyl-triethoxy Silane, aminopropyltriethoxy dimethoxysilane, aminoethylaminopropyl trimethoxy silane, aminoethylaminopropyl triethoxysilicane Alkane, aminoethyl aminomethyl triethoxysilane, 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicanes and urea propyl trimethoxy At least one in silane.
Further technical scheme is that described antioxidant is selected from least one in Hinered phenols, aromatic amine class.
Further technical scheme is that described catalyst is selected from dibutyl tin laurate, dibutyl tin acetate, two At least one in the maleic acid tin of butyl two, dibutyl tin dioctoate, stannous octoate.
Present invention also offers the preparation method of described dual-component polyurethane fluid sealant, comprise the following steps：
Step A：By the polyhydric alcohol polymer of 100 weight portions, the calcium carbonate of 50~500 weight portions, 20~100 weight portions Plasticizer, the tackifier of 0.5~2 weight portion, the antioxidant of 1~5 weight portion are well mixed in adding vacuum kneader in 80 DEG C； Then under the conditions of 100~150 DEG C of temperature, 0.06~0.09MPa of vacuum, dehydration blending 30~200 minutes obtains double-component The component A of polyurethane sealant；
Step B：By the polyisocyanates of 100 weight portions, the polyhydric alcohol polymer of 50~300 weight portions, 10~50 weight The plasticizer of part is added in mixer, and is stirred 60~200 minutes under nitrogen protective condition；It is subsequently adding 5~20 parts of gas Aerosil, 0.5~2.0 part of catalyst, under the conditions of 0.06~0.09MPa of vacuum, stir 5~10 minutes, obtain Dual-component polyurethane fluid sealant B component；
Step C：At room temperature, by component A and B component according to mass ratio 4~10：1 is well mixed, then in vacuum 0.06 Deaeration 3~10 minutes under the conditions of~0.09MPa, obtain final product dual-component polyurethane fluid sealant.
The present invention will be further explained below.
In fluid sealant of the invention, polyhydric alcohol polymer is selected from least one in PPG, PEPA. In a particular embodiment of the present invention, the molecular weight of PPG is 2000~5000；The molecular weight of PEPA is 2000~3000.Preferably, polyhydric alcohol polymer is that mass ratio is 1~9：9~1 PPG, PEPA Mixture；It is further preferred that it is 2~8 that polyhydric alcohol polymer is mass ratio：8~2 PPG, PEPA it is mixed Compound.
In fluid sealant of the invention, the polyisocyanates in B component is the compound for OCN-R-NCO with formula, Wherein, R is C1~20Alkylidene, arlydene, cycloalkylidene, alkylidene aryl, alkylene cycloalkyl, arlydene alkyl, sub- virtue Basic ring alkyl, cycloalkylidene alkyl, cycloalkylidene aryl.In the present invention, the purpose from polyisocyanates is to be prepared into It is-the performed polymer of NCO group to end group, with-OH the reactions in component A, realizes the crosslinking curing of dual-component polyurethane fluid sealant. Preferably, described polyisocyanates be selected from toluene di-isocyanate(TDI), benzhydryl -4,4 '-diisocyanate, 1,6- oneself two At least one in isocyanates, IPDI, dimethylenebenzene diisocyanate；It is further preferred that institute The polyisocyanates stated is selected from toluene di-isocyanate(TDI), dimethylenebenzene diisocyanate.
In the present invention, calcium carbonate is that mass ratio is 1~10：10~1 precipitated calcium carbonate and the mixing of powdered whiting Thing, it is to adjust fluid sealant mechanical property within the specific limits from the purpose of precipitated calcium carbonate and the mixture of powdered whiting And workability, prepare cost performance fluid sealant product higher.Preferably, the matter of precipitated calcium carbonate and powdered whiting Amount is than being 1~10:5:1；It is further preferred that mass ratio is 1~5:1.
In the present invention, tackifier are preferable over aminopropyl triethoxysilane, aminoethylaminopropyl triethoxysilane, 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicane, urea propyl trimethoxy silicane.
The performance test methods of fluid sealant are as follows：
The surface drying time of fluid sealant is tested by GB/T 13477.
The shore hardness of fluid sealant is tested by GB/T 531.
Tested respectively by GB/T528 fluid sealant, fluid sealant placed 24 hours at 120 DEG C and fluid sealant UV300 shine The tensile strength and elongation at break penetrated after 24 hours.
The bond failure area of fluid sealant is tested by SAEJ 1525-1985.
The volatile matter of fluid sealant is tested by PV 2015.
The present invention compared with prior art, with following beneficial effect：
1st, dual-component polyurethane sealing glue solidifying speed of the invention is fast, can meet automobile lamp quickly continuous chemical industry Production needs.
2nd, dual-component polyurethane fluid sealant of the invention improves cementability of the polyurethane sealant to PP and PC materials, carries Resistance to ag(e)ing high, meets the requirement of automobile lamp fluid sealant.
3rd, dual-component polyurethane fluid sealant of the invention is processed by the pre-polymerization of isocyanates, hence it is evident that reduce fluid sealant Volatile matter, after being applied to automobile lamp, volatilizees without small molecule substantially, not only avoid destruction of the volatile matter to antifogging coating, carries Without small molecule isocyanates residual, environmental protection in high travel safety, and colloid.
4th, dual-component polyurethane fluid sealant preparation process is simple of the invention and cost is relatively low, for automobile lamp industry is provided A kind of combination property more excellent adhering and sealing material.
Specific embodiment
With reference to embodiments of the invention, the invention will be further elaborated.
" part " of each material refers to mass parts in following examples.
Embodiment 1：
By PEPA that PPG that 80 parts of molecular weight are 5000,20 parts of molecular weight are 2800,150 parts light Calcium, 50 parts of coarse whitings, 50 parts of diisobutyl phthalates, 0.5 part of 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicane, 0.5 Part urea propyl trimethoxy silicane, 3 parts of Hinered phenols antioxidants are well mixed in adding vacuum kneaders in 80 DEG C；Then in temperature Under the conditions of 120 DEG C of degree, vacuum 0.09MPa, dehydration blending 100 minutes obtains dual-component polyurethane fluid sealant component A.
By 60 parts of toluene di-isocyanate(TDI)s, 20 part 1, hexamethylene-diisocyanate, 20 parts of dimethylenebenzene diisocyanate, PPG that PPG that 120 parts of molecular weight are 2000,80 parts of molecular weight are 5000,50 parts of alkane oils add stirring In machine, and stirred 120 minutes under nitrogen protective condition；It is subsequently adding 20 parts of aerosils, 1 part of di lauric dibutyl Tin, under the conditions of vacuum 0.08MPa, stirs 10 minutes, obtains dual-component polyurethane fluid sealant B component.
At room temperature, by component A and B component according to mass ratio 6:1 is well mixed, then under the conditions of vacuum 0.08MPa Deaeration 5 minutes, obtains dual-component polyurethane fluid sealant, and the test result details of properties of product are shown in Table 1.
Embodiment 2：
PEPA that 100 parts of molecular weight are 3000,20 parts of fine particle calcium carbonates, 60 parts of coarse whitings, 20 parts of phthalic acids two are different Monooctyl ester, 1 part of aminoethylaminopropyl trimethoxy silane, 2 parts of Hinered phenols antioxidants mix in adding vacuum kneader in 80 DEG C Uniformly；Then under the conditions of 100 DEG C of temperature, vacuum 0.06MPa, dehydration blending 60 minutes obtains dual-component polyurethane sealing Glue component A.
By 50 parts of benzhydryl -4,4 '-diisocyanate, 50 part 1, hexamethylene-diisocyanate, 200 parts of molecular weight are 2000 PPG, during the PEPA that 100 parts of molecular weight are 2800,40 parts of aromatic naphtha add mixers, and protected in nitrogen Stirred 200 minutes under the conditions of shield；10 parts of aerosils, 0.5 part of maleic acid tin of dibutyl two are subsequently adding, in vacuum Under the conditions of 0.09MPa, stir 7 minutes, obtain dual-component polyurethane fluid sealant B component.
At room temperature, by component A and B component according to mass ratio 4:1 is well mixed, then under the conditions of vacuum 0.06MPa Deaeration 10 minutes, obtains dual-component polyurethane fluid sealant, and the test result details of properties of product are shown in Table 1.
Embodiment 3：
By PPG that PPG that 60 parts of molecular weight are 3000,40 parts of molecular weight are 5000,300 parts light Calcium, 200 parts of coarse whitings, 50 parts of alkane oils, 30 parts of diisooctyl phthalates, 0.5 part of aminoethylaminopropyl triethoxysilane, 3 parts of Hinered phenols antioxidants, 2 parts of aromatic amine kind antioxidants are well mixed in adding vacuum kneader in 80 DEG C；Then exist Under the conditions of 150 DEG C of temperature, vacuum 0.09MPa, dehydration blending 200 minutes obtains dual-component polyurethane fluid sealant component A.
Polyethers that 80 parts of toluene di-isocyanate(TDI)s, 20 parts of IPDIs, 50 parts of molecular weight are 3000 is more First alcohol, 50 parts of alkane oils are added in mixer, and are stirred 60 minutes under nitrogen protective condition；It is subsequently adding 5 parts of gas phase dioxies SiClx, 1 part of dibutyl tin laurate, 0.5 part of stannous octoate, under the conditions of vacuum 0.08MPa, stir 5 minutes, obtain double Component polyurethane fluid sealant B component.
At room temperature, by component A and B component according to mass ratio 10:1 is well mixed, then under the conditions of vacuum 0.08MPa Deaeration 5 minutes, obtains dual-component polyurethane fluid sealant, and the test result details of properties of product are shown in Table 1.
Embodiment 4：
By PEPA that PPG that 40 parts of molecular weight are 2000,60 parts of molecular weight are 2800,30 parts of fine particle calcium carbonates, 300 parts of coarse whitings, 50 parts of aromatic naphtha, 50 diisononyl phthalates, 1.5 parts of 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicon Alkane, 0.5 part of aminopropyl trimethoxysilane, 3 parts of aromatic amine kind antioxidants mix equal in adding vacuum kneader in 80 DEG C It is even；Then under the conditions of 110 DEG C of temperature, vacuum 0.085MPa, dehydration blending 30 minutes obtains dual-component polyurethane fluid sealant Component A.
Polyethers that 60 parts of tetramethyl group diisocyanates, 40 parts of 1,5- naphthalene diisocyanates, 100 parts of molecular weight are 2000 is more First alcohol, 10 parts of alkane oils are added in mixer, and are stirred 100 minutes under nitrogen protective condition；It is subsequently adding 10 parts of gas phases two Silica, 2 parts of dibutyl tin dioctoates, under the conditions of vacuum 0.085MPa, stir 8 minutes, obtain dual-component polyurethane close Sealing B component.
At room temperature, by component A and B component according to mass ratio 5:1 is well mixed, then under the conditions of vacuum 0.09MPa Deaeration 3 minutes, obtains dual-component polyurethane fluid sealant, and the test result details of properties of product are shown in Table 1.
Embodiment 5：
PPG that 100 parts of molecular weight are 5000,100 parts of fine particle calcium carbonates, 10 parts of coarse whitings, 50 parts of phthalic acids two are different Monooctyl ester, 0.8 part of urea propyl trimethoxy silicane, 1 part of Hinered phenols antioxidant, 1 part of aromatic amine kind antioxidant add vacuum It is well mixed in 80 DEG C in kneader；Then under the conditions of 150 DEG C of temperature, vacuum 0.06MPa, dehydration blending 180 minutes is obtained To dual-component polyurethane fluid sealant component A.
It is 5000 by PPG that 100 parts of toluene di-isocyanate(TDI)s, 100 parts of molecular weight are 2000,50 parts of molecular weight PPG, during 30 parts of alkane oils add mixers, and stirred 120 minutes under nitrogen protective condition；It is subsequently adding 15 Part aerosil, 1 part of dibutyl tin laurate, under the conditions of vacuum 0.07MPa, stir 10 minutes, obtain double groups Part polyurethane sealant B component.
At room temperature, by component A and B component according to mass ratio 6:1 is well mixed, then under the conditions of vacuum 0.09MPa Deaeration 5 minutes, obtains dual-component polyurethane fluid sealant, and the test result details of properties of product are shown in Table 1.
Embodiment 6：
By PEPA that PPG that 50 parts of molecular weight are 5000,50 parts of molecular weight are 2000,30 parts of fine particle calcium carbonates, 20 parts of coarse whitings, 30 parts of diisobutyl phthalates, 0.5 part of 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicane, 0.5 part of ammonia Ethylaminopropyl triethoxysilane, 1 part of Hinered phenols antioxidant are well mixed in adding vacuum kneader in 80 DEG C；Then exist Under the conditions of 120 DEG C of temperature, vacuum 0.08MPa, dehydration blending 120 minutes obtains dual-component polyurethane fluid sealant component A.
By 80 parts of toluene di-isocyanate(TDI)s, 20 parts of dimethylenebenzene diisocyanate, 100 parts of molecular weight be 5000 it is poly- During ethoxylated polyhydric alcohol, 100 parts of molecular weight are 2000 PPG, 40 parts of alkane oils add mixers, and in nitrogen ceiling Stirred 90 minutes under part；10 parts of aerosils, 1 part of dibutyl tin laurate, 1 part of stannous octoate are subsequently adding, true Under the conditions of reciprocal of duty cycle 0.09MPa, stir 8 minutes, obtain dual-component polyurethane fluid sealant B component.
At room temperature, by component A and B component according to mass ratio 5:1 is well mixed, then under the conditions of vacuum 0.09MPa Deaeration 10 minutes, obtains dual-component polyurethane fluid sealant, and the test result details of properties of product are shown in Table 1.
Comparative example 1：
By PPG that PPG that 60 parts of molecular weight are 3000,40 parts of molecular weight are 5000,300 parts light Calcium, 200 parts of coarse whitings, 50 parts of alkane oils, 30 parts of diisooctyl phthalates, 0.5 part of methacryloxypropyl trimethoxy Base silane, 3 parts of Hinered phenols antioxidants, 2 parts of aromatic amine kind antioxidants are well mixed in adding vacuum kneader in 80 DEG C； Then under the conditions of 150 DEG C of temperature, vacuum 0.09MPa, dehydration blending 200 minutes obtains dual-component polyurethane fluid sealant A groups Point.
Polyethers that 80 parts of toluene di-isocyanate(TDI)s, 20 parts of IPDIs, 50 parts of molecular weight are 3000 is more First alcohol, 50 parts of alkane oils are added in mixer, and are stirred 60 minutes under nitrogen protective condition；It is subsequently adding 5 parts of gas phase dioxies SiClx, 1 part of dibutyl tin laurate, 0.5 part of stannous octoate, under the conditions of vacuum 0.08MPa, stir 5 minutes, obtain double Component polyurethane fluid sealant B component.
At room temperature, by component A and B component according to mass ratio 10:1 is well mixed, then under the conditions of vacuum 0.08MPa Deaeration 5 minutes, obtains dual-component polyurethane fluid sealant, and the test result details of properties of product are shown in Table 1.
Comparative example 2：
By PEPA that PPG that 50 parts of molecular weight are 5000,50 parts of molecular weight are 2000,30 parts of fine particle calcium carbonates, 20 parts of coarse whitings, 30 parts of diisobutyl phthalates, 0.5 part of 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicane, 0.5 part of ammonia Ethylaminopropyl triethoxysilane, 1 part of Hinered phenols antioxidant are well mixed in adding vacuum kneader in 80 DEG C；Then exist Under the conditions of 120 DEG C of temperature, vacuum 0.08MPa, dehydration blending 120 minutes obtains dual-component polyurethane fluid sealant component A.
By 80 parts of toluene di-isocyanate(TDI)s, 20 parts of dimethylenebenzene diisocyanate, 40 parts of alkane oils, 10 parts of gas phases two Silica, 1 part of dibutyl tin laurate, 1 part of stannous octoate, under the conditions of vacuum 0.09MPa, stir 8 minutes, obtain double Component polyurethane fluid sealant B component.
At room temperature, by component A and B component according to mass ratio 5:1 is well mixed, then under the conditions of vacuum 0.09MPa Deaeration 10 minutes, obtains dual-component polyurethane fluid sealant, and the test result details of properties of product are shown in Table 1.
The automobile lamp of table 1 dual-component polyurethane fluid sealant the performance test results
Polyurethane sealant mechanical strength of the invention is high, and ageing-resistant performance is good, and curing rate is fast, and volatile matter is low, comprehensive Excellent performance, will not pollute car light lampshade, be suitable to the adhering and sealing of automobile lamp.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair Bright preferably implementation method, embodiments of the present invention are simultaneously not restricted to the described embodiments, it should be appreciated that people in the art Member can be designed that a lot of other modification and implementation methods, and these modifications and implementation method will fall in principle disclosed in the present application Within scope and spirit.

Claims (10)

1. a kind of dual-component polyurethane fluid sealant, it is characterised in that including mass ratio be 4~10：1 component A and B component；
Described component A is by following mass parts into being grouped into：
Polyhydric alcohol polymer, 100 parts；
Plasticizer, 20~100 parts；
Calcium carbonate, 50~500 parts；
Tackifier, 0.5~2 part；
Antioxidant, 1~5 part；
Described B component is by following mass parts into being grouped into：
Polyisocyanates, 100 parts；
Polyhydric alcohol polymer, 50~300 parts；
Plasticizer, 10~50 parts；
Aerosil, 5~20 parts；
Catalyst, 0.5~2.0 part.
2. dual-component polyurethane fluid sealant according to claim 1, it is characterised in that described polyhydric alcohol polymer is selected from At least one in PPG, PEPA.
3. dual-component polyurethane fluid sealant according to claim 1, it is characterised in that described polyisocyanates is formula It is the compound of OCN-R-NCO, wherein, R is C1~20Alkylidene, arlydene, cycloalkylidene, alkylidene aryl, alkylene basic ring Alkyl, arlydene alkyl, arlydene cycloalkyl, cycloalkylidene alkyl, cycloalkylidene aryl.
4. dual-component polyurethane fluid sealant according to claim 3, it is characterised in that described polyisocyanates is selected from first Phenylene diisocyanate, tetramethyl group diisocyanate, benzhydryl -4,4 '-diisocyanate, 1, hexamethylene-diisocyanate, different Buddhist Your ketone diisocyanate, dimethylenebenzene diisocyanate, 4,4 '-diphenylmethane diisocyanate, to the isocyanide of phenyl two Acid esters and its isomers, 1,5- naphthalene diisocyanates, benzhydryl -4 of halogen substitution, in 4 '-diisocyanate at least one Kind.
5. dual-component polyurethane fluid sealant according to claim 1, it is characterised in that described calcium carbonate is that mass ratio is 1 ~10：10~1 precipitated calcium carbonate and the mixture of powdered whiting.
6. dual-component polyurethane fluid sealant according to claim 1, it is characterised in that described plasticizer be selected from alkane oil, At least one in aromatic naphtha, phthalic acid ester.
7. dual-component polyurethane fluid sealant according to claim 1, it is characterised in that described tackifier are selected from aminopropyl Trimethoxy silane, aminopropyl triethoxysilane, aminopropyltriethoxy dimethoxysilane, aminoethylaminopropyl trimethoxy silicon Alkane, aminoethylaminopropyl triethoxysilane, aminoethyl aminomethyl triethoxysilane, 3- (oxygen of 2,3- epoxies third) propyl group front three At least one in TMOS and urea propyl trimethoxy silicane.
8. dual-component polyurethane fluid sealant according to claim 1, it is characterised in that described antioxidant is selected from hindered phenol At least one in class, aromatic amine class.
9. dual-component polyurethane fluid sealant according to claim 1, it is characterised in that described catalyst is selected from two bays In sour dibutyl tin, dibutyl tin acetate, the maleic acid tin of dibutyl two, dibutyl tin dioctoate, stannous octoate at least one Kind.
10. the preparation method of the dual-component polyurethane fluid sealant according to claim any one of 1-9, it is characterised in that including Following steps：
Step A：By the polyhydric alcohol polymer of 100 weight portions, the calcium carbonate of 50~500 weight portions, 20~100 weight portions plasticising Agent, the tackifier of 0.5~2 weight portion, the antioxidant of 1~5 weight portion are well mixed in adding vacuum kneader in 80 DEG C；Then Under the conditions of 100~150 DEG C of temperature, 0.06~0.09MPa of vacuum, dehydration blending 30~200 minutes obtains the poly- ammonia of double-component The component A of ester fluid sealant；
Step B：By the polyisocyanates of 100 weight portions, the polyhydric alcohol polymer of 50~300 weight portions, 10~50 weight portions Plasticizer is added in mixer, and is stirred 60~200 minutes under nitrogen protective condition；It is subsequently adding 5~20 parts of gas phase two Silica, 0.5~2.0 part of catalyst, under the conditions of 0.06~0.09MPa of vacuum, stir 5~10 minutes, obtain double groups Part polyurethane sealant B component；
Step C：At room temperature, by component A and B component according to mass ratio 4~10：1 be well mixed, then vacuum 0.06~ Deaeration 3~10 minutes under the conditions of 0.09MPa, obtain final product dual-component polyurethane fluid sealant.
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CN110791249A (en) * 2019-11-21 2020-02-14 上海康达化工新材料集团股份有限公司 Two-component polyurethane sealant
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CN110791249A (en) * 2019-11-21 2020-02-14 上海康达化工新材料集团股份有限公司 Two-component polyurethane sealant
CN111534266A (en) * 2020-05-20 2020-08-14 天津鼎鑫防火材料科技有限公司 Two-component polyurethane foaming adhesive

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