CN108504318A - A kind of silane modified polyether elastic sealant and preparation method thereof of the high grade of transparency and high intensity - Google Patents
A kind of silane modified polyether elastic sealant and preparation method thereof of the high grade of transparency and high intensity Download PDFInfo
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- CN108504318A CN108504318A CN201810206325.3A CN201810206325A CN108504318A CN 108504318 A CN108504318 A CN 108504318A CN 201810206325 A CN201810206325 A CN 201810206325A CN 108504318 A CN108504318 A CN 108504318A
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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
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
- C09J171/02—Polyalkylene oxides
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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
- 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
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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
- 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
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses the silane modified polyether elastic sealants and preparation method thereof of a kind of high grade of transparency and high intensity.The silane modified polyether elastic sealant of this high grade of transparency and high intensity, is made of the raw material of following mass parts：100 parts of base polymer；10~40 parts of plasticizer；5~25 parts of white carbon；1~5 part of crosslinking agent；0.5~3 part of deicer；0.1~1 part of ultraviolet absorber；0.1~1 part of light stabilizer；0.2~3 part of adhesion promoter；0.2~1 part of catalyst；The preparation method of this silane modified polyether elastic sealant is also disclosed that simultaneously.The high grade of transparency of the present invention, high intensity silane modified polyether elastic sealant can be room-temperature moisture cured, the tensile strength tested after solidification>5MPa, light transmittance>80%, and have both elastic good, UV radiation, the features such as preparation process is simple, high-strength environment-friendly adhesives is can be used as a variety of industrial circles.
Description
Technical field
The present invention relates to the silane modified polyether elastic sealants and preparation method thereof of a kind of high grade of transparency and high intensity.
Background technology
Silicon-modified polyether fluid sealant has because of the special polyether backbone structure of its base polymer and silicon end group structure
The characteristic of moisture-curable, to have both polyurethane and silicone sealant feature performance benefit, have it is environmental-friendly, low it is staining,
Performances and the application characteristics such as covering with paint property is good, weather-proof and durability is good, adhesive property is good, sizing facilitates.Thus, building,
There is very extensive application in rail traffic, automobile, electronic apparatus and other industrial circles.
Conventional silicon-modified polyether fluid sealant is mostly opaque paste sizing material, and intensity is in contrast relatively low, this limit
It has made in its application in the occasion for requiring high-adhesive-strength, high tensile and the high grade of transparency, such as high-end residential room and has filled
Repair with the bonding field of windshield its still can not replace transparent silicone adhesive and high strength polyurethane sealant.
In current technology, CN106833321A discloses transparent mould proof silane modified polyether seal glue of one kind and preparation method thereof,
It is made of following component by weight：55~88 parts of base polymers, 0~12 part of plasticizer, 8~20 parts of fillers, 0.3~
2 parts of deicers, 0~1 part of ultraviolet absorber, 0~1 part of antioxidant, 0.2~2 part of catalyst, 0.2~5 part of coupling agent.This is close
Although sealing, agent anti-mold effect is good, and the surface drying time of 1~2h is still longer, appearance transparent, but specific light transmittance is unknown.
CN106634770A and CN107177340A successively discloses one-component transparent silicon modified polyether seal glue and waterproof mould-proof-type silicon
Alkane modified polyether seal glue and their own preparation method, although being prepared based on the Silante terminated modified polyether base polymers of α-
Seal sizing material have relatively short surface drying time (25-40min) and a degree of light transmittance (60-90%), but draw
It is relatively low to stretch intensity (0.9-1.8MPa).In general, clear silane modified polyether seal glue is asked there are still each performance is unbalanced
Topic, therefore, it is necessary to develop, a kind of surface drying time is suitable, silicon-modified polyether fluid sealant of the high grade of transparency, high intensity.
Invention content
The purpose of the present invention is to provide the silane modified polyether elastic sealant of a kind of high grade of transparency and high intensity and its
Preparation method.In the present invention, the high grade of transparency refers to that silane modified polyether elastic sealant is tested according to GB/T 2410-2008
Light transmittance>80%, high intensity refers to the tensile strength that silane modified polyether elastic sealant is tested according to GB/T 528-2009
>5MPa。
The technical solution used in the present invention is：
A kind of silane modified polyether elastic sealant of the high grade of transparency and high intensity, is the raw material group by following mass parts
At：
The base polymer is the Silante terminated polypropylene glycol of the degree of branching >=3, the silane of segment containing PolyTHF envelope
Hold at least one of embedding end polyethers.
In silane modified polyether elastic sealant, the number-average molecular weight of base polymer is 6000~30000 dalton.
In silane modified polyether elastic sealant, white carbon is vapor phase method hydrophabic silica, the specific surface area of white carbon
For 100m2/ g~400m2/g。
In silane modified polyether elastic sealant, crosslinking agent is made of the raw material of following mass percent：80~100%
Main crosslinking agent and 0~20% secondary crosslinking agent；
The general structure of the main crosslinking agent is：
Wherein, R1For-OCH2CH2O-、-OCH2CH2CH2O-、 -OCH2CH2OCH2CH2In O-
Any one；
R2ForIn any one；
R3For C1~C5Alkyl, methoxyl group, any one in ethyoxyl；
R4For methyl or ethyl；
The secondary crosslinking agent is methyl tributanoximo silane, vinyl tributyl ketoximyl silane, hexamethylene diamine ylmethyl
At least one of triethoxysilane, diethylin methyltriethoxysilane, aminopropyltriethoxysilane trimethoxy silane.
In silane modified polyether elastic sealant, plasticizer is the polyether polyols of 1000~4000 dalton of number-average molecular weight
Alcohol, didecyl phthalate, diethylene glycol dibenzoate, dipropylene glycol dibenzoate, triethylene-glycol dibenzoic acid
At least one of ester.
In silane modified polyether elastic sealant, deicer is hexamethyldisilazane, vinyltrimethoxysilane, second
At least one of alkenyl triethoxysilane.
In silane modified polyether elastic sealant, ultraviolet absorber is benzotriazole, benzophenone class, salicylic acid esters, takes
For at least one of vinyl cyanide, triazines absorbent；Light stabilizer is hindered amine light stabilizer.
In silane modified polyether elastic sealant, adhesion promoter is amino silicone, sulfydryl siloxanes, epoxy group silicon
At least one of oxygen alkane.
In silane modified polyether elastic sealant, catalyst is organo-tin compound.
The preparation method of the silane modified polyether elastic sealant of this high grade of transparency and high intensity, includes the following steps：
1) base polymer, plasticizer, white carbon, ultraviolet absorber and light stabilizer are added in blender, are warming up to
It 100 DEG C~110 DEG C, is stirred under vacuum, obtains mixed material；
2) wait for that the mixed material of step 1) is cooled to 50 DEG C hereinafter, deicer, crosslinking agent and adhesion promoter is added, after
It is continuous to be stirred under vacuum；
3) catalyst is added, is stirred under vacuum, obtains the silane modified polyether elastic sealant of the high grade of transparency and high intensity.
The beneficial effects of the invention are as follows：
The high grade of transparency of the present invention, high intensity silane modified polyether elastic sealant can be room-temperature moisture cured, after solidification
The tensile strength of test>5MPa, light transmittance>80%, and have both elastic good, UV radiation, preparation process is simple etc.
Feature can be used as high-strength environment-friendly adhesives for a variety of industrial circles.
Specifically：
1) present invention with the Silante terminated polypropylene glycol (degree of branching >=3) of branched structure, contain PolyTHF segment
Silane-terminated polyether or their compositions are prepolymer, by increasing base polymer crosslinking points or introducing PolyTHF chain
The mechanical strength of Duan Zengjia base rubbers；
2) present invention uses methyl tributanoximo with the silane of ether-containing key group and six hydrolyzable groups for main crosslinking agent
Silane, vinyl tributyl ketoximyl silane, methyltrimethoxysilane and methyltriethoxysilane etc. are as time crosslinking agent, really
While the high grade of transparency of secrecy sealing and suitable surface drying time, increase the crosslink density of fluid sealant, to improve fluid sealant
Mechanical strength；
3) for the present invention with hydrophobicity aerosil etc. for reinforcing filler, the mechanics for being obviously improved sealant material is strong
Degree；
4) mechanical strength and transparency are higher after sealing glue solidifying of the invention, according to GB/T 528-2009 and GB/T
The tensile strength that 2410- 2008 is tested>5MPa, light transmittance>80%, reach the silicon-modified polyether fluid sealant high grade of transparency and high-strength
The demand of degree.
Specific implementation mode
A kind of silane modified polyether elastic sealant of the high grade of transparency and high intensity, is the raw material group by following mass parts
At：
The base polymer is the Silante terminated polypropylene glycol of the degree of branching >=3, the silane of segment containing PolyTHF envelope
Hold at least one of embedding end polyethers.
Preferably, in silane modified polyether elastic sealant, the number-average molecular weight of base polymer is 6000~30000
Er Dun；It is further preferred that the number-average molecular weight of base polymer is 10000~20000 dalton.
Preferably, in silane modified polyether elastic sealant, white carbon is vapor phase method hydrophabic silica, the ratio of white carbon
Surface area is 100m2/ g~400m2/g。
Preferably, in silane modified polyether elastic sealant, crosslinking agent is made of the raw material of following mass percent：80~
100% main crosslinking agent and 0~20% secondary crosslinking agent；
The general structure of the main crosslinking agent is：
Wherein, R1For-OCH2CH2O-、-OCH2CH2CH2O-、 -OCH2CH2OCH2CH2In O-
Any one；
R2ForIn any one；
R3For C1~C5Alkyl, methoxyl group, any one in ethyoxyl；
R4For methyl or ethyl；
It is further preferred that the main crosslinking agent is the α containing six hydrolyzable groups-degree of functionality coupling agent, structure
Formula is：
Preferably, the secondary crosslinking agent is methyl tributanoximo silane, vinyl tributyl ketoximyl silane, hexamethylene diamine
At least one in ylmethyl triethoxysilane, diethylin methyltriethoxysilane, aminopropyltriethoxysilane trimethoxy silane
Kind.
Preferably, in silane modified polyether elastic sealant, plasticizer is 1000~4000 dalton of number-average molecular weight
Polyether polyol, didecyl phthalate, diethylene glycol dibenzoate, dipropylene glycol dibenzoate, triethylene-glycol
At least one of dibenzoate.
Preferably, in silane modified polyether elastic sealant, deicer is hexamethyldisilazane, vinyl trimethoxy
At least one of silane, vinyltriethoxysilane.
Preferably, in silane modified polyether elastic sealant, ultraviolet absorber is benzotriazole, benzophenone class, salicylic acid
At least one of esters, group-substituted acrylonitrile, triazines absorbent.
Preferably, in silane modified polyether elastic sealant, light stabilizer is hindered amine light stabilizer；Further preferably
, hindered amine light stabilizer is selected from 770,944,622,783,791, at least one of HS-508.
Preferably, in silane modified polyether elastic sealant, adhesion promoter be amino silicone, sulfydryl siloxanes,
At least one of epoxy radical siloxane；It is further preferred that adhesion promoter is aminopropyl trimethoxysilane, aminopropyl
Triethoxysilane, ureidopropyltriethoxysilane, N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, N- (β-ammonia
Ethyl)-gamma-aminopropyl-triethoxy-silane, diethylenetriamine base propyl trimethoxy silicane, γ-glycidyl ether oxygen propyl
At least one of trimethoxy silane；Still further preferably, adhesion promoter is aminopropyl trimethoxysilane, N-
At least one of (β-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane.
Preferably, in silane modified polyether elastic sealant, catalyst is organo-tin compound；It is further preferred that urging
Agent is stannous octoate, dibutyl tin laurate, the just pungent tin of tin dilaurate two, dibutyltin diacetate, two (dodecyls
At least one of sulphur) dibutyl tin；Still further preferably, catalyst is in stannous octoate, dibutyl tin laurate
It is at least one.
The preparation method of the silane modified polyether elastic sealant of this high grade of transparency and high intensity, includes the following steps：
1) base polymer, plasticizer, white carbon, ultraviolet absorber and light stabilizer are added in blender, are warming up to
It 100 DEG C~110 DEG C, is stirred under vacuum, obtains mixed material；
2) wait for that the mixed material of step 1) is cooled to 50 DEG C hereinafter, deicer, crosslinking agent and adhesion promoter is added, after
It is continuous to be stirred under vacuum；
3) catalyst is added, is stirred under vacuum, obtains the silane modified polyether elastic sealant of the high grade of transparency and high intensity.
Preferably, in the step 1) of preparation method, the time of vacuum stirring is 2h~3h；In the step 2) of preparation method,
The time of vacuum stirring is 10min~30min；In the step 3) of preparation method, the time of vacuum stirring is 10min~30min.
Preferably, the vacuum stirring described in preparation method, vacuum degree are 0.09MPa~0.095MPa.
Present disclosure is described in further detail below by way of specific embodiment.It is former used in embodiment
Material unless otherwise specified, can be obtained from routine business approach.
Embodiment 1：
The high grade of transparency and high intensity silane modified polyether elastic sealant, preparation method of embodiment 1 are as follows：
1) branched polypropylene glycol (degree of branching 3, the number-average molecular weight 10000 for blocking 2kg trimethoxy propyl silanes
Er Dun), (specific surface area is for 200g polypropylene glycols (4000 dalton of number-average molecular weight), 240g hydrophobicity aerosils
300m2/ g), 10g ultraviolet absorbers UV-326 (2- (2- hydroxyl -3- tertiary butyl -5- aminomethyl phenyls) -5- chlorinated benzotriazoles) and
Planet is added in 10g hindered amine light stabilizers Tinuvin 770 (bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate)
Blender makes material be warming up to 100~110 DEG C, is stirred under vacuum 3h；
2) wait for that the mixed material temperature of step 1) is down to 50 DEG C hereinafter, 60g vinyltrimethoxysilanes are added, 20g is handed over
Join agent I and 20g N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane, continues to be stirred under vacuum 20min；
3) 20g dibutyl tin laurates are added, are stirred under vacuum 20min, it is silane-modified poly- to obtain the high grade of transparency, high intensity
Ether elastic sealant.
Cross-linking agents Ⅰ structural formula described in step 2) is as follows：
Embodiment 2：
The high grade of transparency and high intensity silane modified polyether elastic sealant, preparation method of embodiment 2 are as follows：
1) branched polypropylene glycol (degree of branching 4, the number-average molecular weight 16000 for blocking 2kg trimethoxy propyl silanes
Er Dun), (specific surface area is for 400g polypropylene glycols (3000 dalton of number-average molecular weight), 200g hydrophobicity aerosils
300m2/ g), 2g ultraviolet absorbers UV-326 (2- (2- hydroxyl -3- tertiary butyl -5- aminomethyl phenyls) -5- chlorinated benzotriazoles) and
Planet is added in 20g hindered amine light stabilizers Tinuvin 770 (bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate)
Blender makes material be warming up to 100~110 DEG C, is stirred under vacuum 2.5h；
2) wait for that the mixed material temperature of step 1) is down to 50 DEG C hereinafter, 30g vinyltrimethoxysilanes are added, 40g is handed over
Join agent I (identical as the cross-linking agents Ⅰ used in embodiment 1) and 20g N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane, after
It is continuous to be stirred under vacuum 30min；
3) 20g dibutyl tin laurates are added, is stirred under vacuum 20min, it is close to obtain high intensity silane modified polyether elasticity
Sealing.
Embodiment 3：
The high grade of transparency and high intensity silane modified polyether elastic sealant, preparation method of embodiment 3 are as follows：
1) by 2kg triethoxy methyl silicanes sealing end block polyether prepolymer (16000 dalton of number-average molecular weight, including
The PolyTHF of 4000 dalton of polyethylene glycol block and a hop count average molecular weight of two hop count average molecular weights, 6000 dalton
Block), 600g polypropylene glycols (2000 dalton of number-average molecular weight), (specific surface area is 160g hydrophobicity aerosils
200m2/ g), 10g ultraviolet absorbers UV-327 (2- (2 '-hydroxyls -3 ', 5 '-di-tert-butyl-phenyls) -5- chlorinated benzotriazoles)
Planet is added with 8g hindered amine light stabilizers Tinuvin 770 (bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate)
Blender makes material be warming up to 100~110 DEG C, is stirred under vacuum 2h；
2) wait for that the mixed material temperature of step 1) is down to 50 DEG C hereinafter, 20g vinyltrimethoxysilanes are added, 54g is handed over
Join agent II, 6g hexamethylene diamine ylmethyl triethoxysilanes and 10g N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane, after
It is continuous to be stirred under vacuum 30min；
3) 4g stannous octoates are added, is stirred under vacuum 30min, obtains high intensity silane modified polyether elastic sealant.
II structural formula of crosslinking agent described in step 2) is as follows：
Embodiment 4：
The high grade of transparency and high intensity silane modified polyether elastic sealant, preparation method of embodiment 4 are as follows：
1) by 2kg trimethoxymethylsila,es sealing end block polyether prepolymer (20000 dalton of number-average molecular weight, including
The PolyTHF of 2000 dalton of polyethylene glycol block and two hop count average molecular weights of two hop count average molecular weights, 8000 dalton
Block), 800g polypropylene glycols (2000 dalton of number-average molecular weight), (specific surface area is 100g hydrophobicity aerosils
130m2/ g), 20g ultraviolet absorbers UV-327 (2- (2 '-hydroxyls -3 ', 5 '-di-tert-butyl-phenyls) -5- chlorinated benzotriazoles)
Planet is added with 2g hindered amine light stabilizers Tinuvin 770 (bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate)
Blender makes material be warming up to 100~110 DEG C, is stirred under vacuum 2h；
2) wait for that the mixed material temperature of step 1) is down to 50 DEG C hereinafter, 20g vinyltrimethoxysilanes are added, 80g is handed over
Join agent II (identical as the crosslinking agent II used in embodiment 3) and 60g γ-glycidyl ether oxygen propyl trimethoxy silicane, continues
It is stirred under vacuum 30min；
3) 5g stannous octoates are added, is stirred under vacuum 30min, obtains high intensity silane modified polyether elastic sealant.
Embodiment 5：
The high grade of transparency and high intensity silane modified polyether elastic sealant, preparation method of embodiment 5 are as follows：
1) branched polypropylene glycol (degree of branching 4, the number-average molecular weight 16000 for blocking 1kg trimethoxy propyl silanes
Er Dun), 1kg trimethoxymethylsila,es block block polyether prepolymer (20000 dalton of number-average molecular weight, including two sections of sections
Number-average molecular weight is the polypropylene glycol segment of 8000 dalton and the PolyTHF that two hop count average molecular weights are 2000 dalton
Segment), 800g polypropylene glycols (1000 dalton of number-average molecular weight), (specific surface area is 100g hydrophobicity aerosils
100m2/ g), 10g ultraviolet absorbers UV-327 (2- (2 '-hydroxyls -3 ', 5 '-di-tert-butyl-phenyls) -5- chlorinated benzotriazoles) and
Planet is added in 10g hindered amine light stabilizers Tinuvin 770 (bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate)
Blender makes material be warming up to 100~110 DEG C, is stirred under vacuum 2h；
2) wait for that the mixed material temperature of step 1) is down to 50 DEG C hereinafter, 20g vinyltrimethoxysilanes are added, 80g is handed over
Join agent II (identical as the crosslinking agent II used in embodiment 3), 20g methyl tributanoximo silanes and 20g γ-glycidyl ether oxygen
Propyl trimethoxy silicane continues to be stirred under vacuum 25min；
3) 6g stannous octoates are added, is stirred under vacuum 30min, it is close to obtain the high grade of transparency, high intensity silane modified polyether elasticity
Sealing.
Comparative example：
The polyether seal glue of comparative example 1, preparation method are as follows：
1) by 2kg dimethoxy-methyl propyl Terminated Polyether Prepolymer, (Japanese Zhong Yuan chemical companies MS-S203H, number are divided equally
Son amount be more than 8000 dalton), 200g polypropylene glycols (2000 dalton of number-average molecular weight), 240g hydrophobicity aerosils
(specific surface area 300m2/ g), 10g ultraviolet absorbers UV-327 (2- (2 '-hydroxyls -3 ', 5 '-di-tert-butyl-phenyls) -5- chloros
Benzotriazole) and 10g hindered amine light stabilizers Tinuvin770 (bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate)
Planetary mixer is added, material is made to be warming up to 100~110 DEG C, is stirred under vacuum 3h；
2) wait for that the mixed material temperature of step 1) is down to 50 DEG C hereinafter, 40g vinyltrimethoxysilanes, 60g ammonia is added
Propyl trimethoxy silicane and 60g N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane continue to be stirred under vacuum 30min；
3) 20g dibutyl tin laurates are added, is stirred under vacuum 30min, obtains silane modified polyether seal glue.
Test case：
Standard batten is made in fluid sealant in Examples 1 to 5 and comparative example, in 25 DEG C, the environment of 50% relative humidity
Middle solidification 7 days, then be tested for the property, test result is as shown in table 1.
The performance test results of the fluid sealant of 1 Examples 1 to 5 of table and comparative example
Note：It tensile strength and is tested according to national standard GB/T 528-2009 with elongation at break, shear strength is according to state
Mark GB/T 7124-2008 are tested, and transparency is indicated with light transmittance, is tested according to GB/T 2410-2008.
From the comparison of test results of table 1 it is found that compared with comparative example, after the sealing glue solidifying obtained by Examples 1 to 5
Mechanical strength and transparency significantly improve, and have reached the demand of the silicon-modified polyether fluid sealant high grade of transparency and high intensity, i.e. basis
The tensile strength of GB/T 528-2009 tests>5MPa, according to the light transmittance of GB/T 2410-2008 tests>80%.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. the silane modified polyether elastic sealant of a kind of high grade of transparency and high intensity, it is characterised in that：By following mass parts
Raw material forms：
The base polymer is that Silante terminated polypropylene glycol, the segment containing PolyTHF of the degree of branching >=3 are Silante terminated embedding
Hold at least one of polyethers.
2. the silane modified polyether elastic sealant of a kind of high grade of transparency according to claim 1 and high intensity, feature
It is：The number-average molecular weight of base polymer is 6000~30000 dalton.
3. the silane modified polyether elastic sealant of a kind of high grade of transparency according to claim 1 and high intensity, feature
It is：White carbon is vapor phase method hydrophabic silica, and the specific surface area of white carbon is 100m2/ g~400m2/g。
4. the silane modified polyether elastic sealant of a kind of high grade of transparency according to claim 1 and high intensity, feature
It is：Crosslinking agent is made of the raw material of following mass percent：80~100% main crosslinking agent and 0~20% secondary crosslinking agent；
The general structure of the main crosslinking agent is：
Wherein, R1For-OCH2CH2O-、-OCH2CH2CH2O-、-OCH2CH2OCH2CH2It is arbitrary in O-
It is a kind of；
R2ForIn any one；
R3For C1~C5Alkyl, methoxyl group, any one in ethyoxyl；
R4For methyl or ethyl；
The secondary crosslinking agent is methyl tributanoximo silane, vinyl tributyl ketoximyl silane, three second of hexamethylene diamine ylmethyl
At least one of oxysilane, diethylin methyltriethoxysilane, aminopropyltriethoxysilane trimethoxy silane.
5. the silane modified polyether elastic sealant of a kind of high grade of transparency according to claim 1 and high intensity, feature
It is：Plasticizer is the polyether polyol of 1000~4000 dalton of number-average molecular weight, didecyl phthalate, diethylene glycol (DEG) two
At least one of benzoic ether, dipropylene glycol dibenzoate, triethylene-glycol dibenzoate.
6. the silane modified polyether elastic sealant of a kind of high grade of transparency according to claim 1 and high intensity, feature
It is：Deicer is at least one in hexamethyldisilazane, vinyltrimethoxysilane, vinyltriethoxysilane
Kind.
7. the silane modified polyether elastic sealant of a kind of high grade of transparency according to claim 1 and high intensity, feature
It is：Ultraviolet absorber be benzotriazole, benzophenone class, salicylic acid esters, group-substituted acrylonitrile, in triazines absorbent extremely
Few one kind；Light stabilizer is hindered amine light stabilizer.
8. the silane modified polyether elastic sealant of a kind of high grade of transparency according to claim 1 and high intensity, feature
It is：Adhesion promoter is at least one of amino silicone, sulfydryl siloxanes, epoxy radical siloxane.
9. the silane modified polyether elastic sealant of a kind of high grade of transparency according to claim 1 and high intensity, feature
It is：Catalyst is organo-tin compound.
10. the silane modified polyether elastic sealant of a kind of high grade of transparency of claim 1~9 any one of them and high intensity
Preparation method, it is characterised in that：Include the following steps：
1) base polymer, plasticizer, white carbon, ultraviolet absorber and light stabilizer are added in blender, are warming up to 100 DEG C
It~110 DEG C, is stirred under vacuum, obtains mixed material；
2) wait for that the mixed material of step 1) is cooled to 50 DEG C hereinafter, deicer, crosslinking agent and adhesion promoter is added, continuation is true
Sky stirring；
3) catalyst is added, is stirred under vacuum, obtains the silane modified polyether elastic sealant of the high grade of transparency and high intensity.
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| CN112029467B (en) * | 2020-09-16 | 2021-11-30 | 深圳市安伯斯科技有限公司 | High-transparency MS glue with pencil hardness reaching 3H and preparation method thereof |
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Address after: 510665 Guangzhou, Guangdong, Tianhe District Province Road West, No. 318 Patentee after: Institute of chemical engineering, Guangdong Academy of Sciences Address before: 510665 Guangzhou, Guangdong, Tianhe District Province Road West, No. 318 Patentee before: GUANGDONG RESEARCH INSTITITUTE OF PETROCHEMICAL AND FINE CHEMICAL ENGINEERING |