CN109401710A - Dual-component silicane modified polyether seal glue and preparation method thereof - Google Patents

Dual-component silicane modified polyether seal glue and preparation method thereof Download PDF

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Publication number
CN109401710A
CN109401710A CN201811161591.5A CN201811161591A CN109401710A CN 109401710 A CN109401710 A CN 109401710A CN 201811161591 A CN201811161591 A CN 201811161591A CN 109401710 A CN109401710 A CN 109401710A
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component
parts
modified polyether
silane
dual
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杨苏邯
陈洋庆
陈建军
高敏华
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Guangzhou Baiyun Chemical Industry Co Ltd
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Guangzhou Baiyun Chemical Industry Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J171/00Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/221Oxides; Hydroxides of metals of rare earth metal
    • C08K2003/2213Oxides; Hydroxides of metals of rare earth metal of cerium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2272Ferric oxide (Fe2O3)
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K2201/00Specific properties of additives
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L2201/08Stabilised against heat, light or radiation or oxydation
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    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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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    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
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  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Sealing Material Composition (AREA)

Abstract

The present invention relates to a kind of dual-component silicane modified polyether seal glues and preparation method thereof.The dual-component silicane modified polyether seal glue includes component A and B component;Component A includes the raw material of following parts by weight: 0.5-5 parts of fiber, 0.5-5 parts of heat-resistant agent after silane treatment, 0.01-0.05 parts of water after 30-35 parts of silane modified polyether polymer, 50-90 parts of filler, 1.1-1.5 parts of carbon black, 10-40 parts of plasticizer, dispersion;B component includes the raw material of following parts by weight: 10-50 parts of filler, 25-30 parts of plasticizer, 1-10 parts of crosslinking agent, 0.1-5 parts of silane coupling agent, 1-5 parts of catalyst, 1-5 parts of co-catalyst.Compared with existing silane modified polyether seal glue, there is more preferably high-temperature stability, and intensity is high, can rapid curing, enable silane modified polyether seal glue heat resistant requirements are high, industrial circle that quickly produce uses.

Description

Dual-component silicane modified polyether seal glue and preparation method thereof
Technical field
The present invention relates to sealant fields, more particularly to a kind of dual-component silicane modified polyether seal glue and its preparation side Method.
Background technique
Sealant is widely used in the various fields such as building, building, bridge, container, ship, electrical, space flight, with The continuous improvement of industrial automation level, heat resistant type elastic sealant assembles in automobile component, the demand of electronic and electrical field It is gradually expanded.
Common high performance sealant mainly has currently on the market: polysulfide, silicone and polyurethane.Wherein polysulfide sealant holds Tend to age and harden, durability it is poor, and penetrating odor can be discharged, thus the scope of application gradually becomes smaller;Polyurethane sealant Intensity is high, corrosion resistance is strong, but-NCO group is very sensitive to moisture, deals with improperly and will affect storage stability, it is more difficult to when long Between store, there may be carbon dioxide gas when solidification forms bubble in sealant layer, reduce adhesive tape performance, weatherability itself and Heat resistance is less desirable;Silicone sealant is not blistering, and the heat-resisting weather resistance of glue-line is good, but surface cannot brush colouring, resistance to Oiliness is insufficient, and tearing strength is lower, and intolerant to puncture, glue-line is easy to appear oil dress object and pollution surrounding substrate is precipitated.
In recent years, silane modified polyether seal glue is a direction of domestic and international novel seal gum development.
Silane modified polyether seal glue is also referred to as MS sealant, has there is 40 years successful application history so far from invention, It is all widely used in Japan, Europe and the U.S..
The main chain of silane modified polyether polymer is polyether soft segments, has end-silicane-group group, main chain poly- in structure The characteristics of ether, the sealant prepared have both the overall merit of silicone adhesive and polyurethane adhesive;Silane modified polyether glue is free of solvent, With extensive caking property, good application property, durability and weatherability especially have paintability;Excellent technological operation Property and high elongation rate and high intensity.
Silane modified polyether seal glue is sealed for electric material, is polyurethane (PU) sealant currently on the market With the substitute of silicone (SR) sealant, have a vast market foreground.
Conventional method is related to a kind of one-component thermostable silicone sealant, and by introducing phenyl in main chain, resistance to height is added Warm filler, hence it is evident that improve the heat resistance of sealant.The invention improves the heat resistance of silicone sealant, can send out in automobile Bonding in motivation and chassis, but cannot fundamentally improve silicone sealant surface and cannot brush colouring, oil resistivity is insufficient, tears Resistance to spalling is lower, and intolerant to puncture, glue-line is easy to appear the shortcomings that pollution surrounding substrate is precipitated in oil dress object.
Separately there is conventional method to be related to a kind of single-component heat resistant type silane modified polyether sealant, by introducing benzene in main chain High temperature resistant filler is added, hence it is evident that improves the heat resistance of sealant in base.The invention improves the resistance to of silane modified polyether seal glue Hot property, can be used for the heating part assembly and sealing of electronic and electrical field, but the excessive of silane coupling agent is added and heat-resisting The addition of filler can sacrifice the intensity of sealant, and One component Sealant curing rate is slow, limits the shock processing of industrial products.
Summary of the invention
Based on this, it is necessary to provide a kind of dual-component silicane modified polyether seal glue.It is close with traditional silane modified polyether Sealing compares, and has more preferably high-temperature stability, and intensity is high, can rapid curing so that silane modified polyether seal glue It industrial circle that is high, quickly producing can be used in heat resistant requirements.
A kind of dual-component silicane modified polyether seal glue, component A and B component including weight ratio 2-4:1;
Component A includes the raw material of following parts by weight:
Wherein, the silane that the heat-resistant agent after the silane treatment uses is phenyltrimethoxysila,e and/or dimethyl benzene Base oxethyl silane, the weight percent that the silane accounts for the heat-resistant agent is 1-10%;
B component includes the raw material of following parts by weight:
The dual-component silicane modified polyether seal glue in one of the embodiments,
Component A includes the raw material of following parts by weight:
B component includes the raw material of following parts by weight:
It is 1-5% that the silane, which accounts for the weight percent of the heat-resistant agent, in one of the embodiments,.
The silane treatment heat-resistant agent processing method includes the following steps: in one of the embodiments,
100 parts of heat-resistant agent, 2-4 parts of silane, 0.5-1 parts of water are mixed by weight, and gained mixture is in inert gas shielding Under, in 100-110 DEG C of processing 1.5-2.5h.
The heat-resistant agent is gaseous oxidation aluminium, iron oxide, boric oxide glass powder, hydroxide in one of the embodiments, One of aluminium, zinc oxide, cerium oxide or multiple combinations.Preferably weight ratio be 1:0.8-1.2 boric oxide glass powder and hydrogen Aluminium oxide.
The fiber size is 200 μm -1000 μm in one of the embodiments,;The fiber is aramid fiber short fibre, benzene Support the combination of one or both of benzo dioxazole fiber.
The dispersing agent that the fiber after the dispersion uses in one of the embodiments, is water-soluble high-molecular compound, It can be selected from polyacrylate and its one of copolymer, polyvinyl alcohol and its derivative, modified natural polymer.
The silane modified polyether polymer is the silane modified polyether of trimethoxy sealing end in one of the embodiments, One of polymer or multiple combinations, viscosity is in 5000-20000mPa.s.
In one of the embodiments, the crosslinking agent be dimethoxydiphenylsilane, diphenyl diethoxy silane, One of triphenylpyridinium base phenyl triethoxysilane, tetraphenyl phenyl triethoxysilane or multiple combinations.Preferably Weight ratio is the tetraphenyl phenyl triethoxysilane and diphenyl diethoxy silane of 1:0.8-1.2.
The plasticizer is dibutyl phthalate, dioctyl terephthalate, molecule in one of the embodiments, One of polyether polyol that amount is 2000 or multiple combinations.
The silane coupling agent is 3- aminopropyl trimethoxysilane, bis- [(tri- ethoxies of 3- in one of the embodiments, Base silicon substrate) propyl] combination of one or both of amine.
The filler is one of nanometer calcium carbonate, coarse whiting, fumed silica or more in one of the embodiments, Kind combination.
In one of the embodiments, in the component A, in terms of the parts by weight for accounting for the raw material, the filler includes:
35-50 parts of nanometer calcium carbonate,
15-25 parts of coarse whiting,
1-10 parts of fumed silica.
In the B component, in terms of the parts by weight for accounting for the raw material, the filler includes:
10-40 parts of coarse whiting,
0.5-5 parts of fumed silica.
The catalyst is that stannous octoate, dibutyl tin dilaurate, tin dilaurate two are pungent in one of the embodiments, One of base tin;The co-catalyst be lauryl amine, N, one of accelerine, low molecular polyamides or It is a variety of.
The present invention also provides the preparation methods of the dual-component silicane modified polyether seal glue, include the following steps:
The preparation of the component A: by fiber, the silane after the silane modified polyether polymer, filler, carbon black, dispersion Treated heat-resistant agent, plasticizer, water sequentially add in planet stirring kettle, stir 30-90min under room temperature, discharge to obtain the A group Point;
The preparation of the B component: the filler, plasticizer are added sequentially in planet stirring kettle, 105-115 is warming up to DEG C, it stirs 1.5-2.5 hours under vacuum state, is removed water after being cooled to room temperature, then sequentially add the crosslinking agent, silane coupled Agent, catalyst, co-catalyst stir 5-15min, and discharge to obtain the B component.
The principle of the present invention and advantage are as follows:
Dual-component silicane modified polyether seal glue of the invention, on the basis of reasonable preparation each raw material component, using double The mixed glue mode of component, and a small amount of water is added inside component A so that after mixed glue can rapid deep zone solidification, in conjunction with using passing through Phenyltrimethoxysila,e and/or the pretreated heat-resistant agent of 3,5-dimethylphenyl Ethoxysilane, a small amount of silane can be increased The compatibility of heat-resistant agent and silane modified polymer matrix, the fiber after cooperation dispersion, is improving the same of sealant thermal stability When keep its intensity.Thus obtained dual-component silicane modified polyether seal glue, with traditional silane modified polyether seal glue phase Compare, there is more preferably high-temperature stability, and intensity is high, can rapid curing, can in heat resistant requirements work that is high, quickly producing Industry field uses.
In addition, the component A of the dual-component silicane modified polyether seal glue is dehydrated without high-temperature vacuum, at room temperature, at a normal may be used Preparation, reduces production cost, is advantageously implemented large-scale production.
Further, fine using the aramid fiber short fibre containing phenyl ring or heterocycle structure of certain size, penylene benzo dioxazole Dimension, can optimize the heat resistance and intensity of sealant.
Further, using dimethoxydiphenylsilane, diphenyl diethoxy silane, triphenylpyridinium base phenyl three More phenyl groups can be introduced into silane and changed by more benzene cross-linking agents such as Ethoxysilane, tetraphenyl phenyl triethoxysilane Property polyether backbone on, improve the heat resistance of silane modified polyether main chain, and increase main polymer chain with containing phenyl ring or heterocycle knot The compatibility of structure staple fiber, and then the heat resistance of sealant is further increased, and improve the intensity of sealant.
The preparation method of dual-component silicane modified polyether seal glue of the present invention, step is simple, easily controllable, is applicable in In large-scale production.
Specific embodiment
Below in conjunction with specific embodiment to dual-component silicane modified polyether seal glue and preparation method thereof of the invention make into One step detailed description.
In the embodiment of the present invention, the processing method of the heat-resistant agent after the silane treatment is as follows:
By weight mix 100 parts of heat-resistant agent, 3 parts of silane, 0.7 part of water, gained mixture under inert gas protection, in 105 DEG C of processing 2h.
Embodiment 1
A kind of dual-component silicane modified polyether seal glue of the present embodiment, component A and B component including weight ratio 3:1:
Component A is made of the raw material of following parts by weight: the trimethoxy terminated silane modified polyether of viscosity 5000mPa.s is poly- Close 30 parts of object, 50 parts of nanometer calcium carbonate, 15 parts of coarse whiting, 1 part of fumed silica, 1.1 parts of carbon black, dibutyl phthalate 10 Part, 0.5 part of 200 μm of aramid fiber short fibres using after polyacrylate and its copolymer dispersion, 3,5-dimethylphenyl Ethoxysilane Handle 0.5 part of heat-resistant agent cerium oxide, 0.01 part of water;
B component is made of the raw material of following parts by weight: 40 parts of coarse whiting, 30 parts of dioctyl terephthalate, gas phase titanium dioxide 5 parts of silicon, 10 parts of dimethoxydiphenylsilane, 5 parts of 3- aminopropyl trimethoxysilane, 5 parts of dibutyl tin dilaurate, 12 5 parts of alkylamine.
Above-mentioned dual-component silicane modified polyether seal glue the preparation method is as follows:
Component A preparation: it by 30 parts of the trimethoxy terminated silane modified polyether polymer of the viscosity 5000mPa.s, receives 50 parts of calcium carbonate of rice, 1 part of fumed silica, 1.1 parts of carbon black, 10 parts of dibutyl phthalate, uses poly- third at 15 parts of coarse whiting 0.5 part of 200 μm of aramid fiber short fibres, 3,5-dimethylphenyl Ethoxysilane after olefin(e) acid ester and its copolymer dispersion handle heat-resistant agent oxygen Change 0.5 part of cerium, 0.01 part of water, sequentially add in planet stirring kettle, 30min is stirred under room temperature, discharging is packaged to be component A;
The preparation process of B component are as follows: by 40 parts of coarse whiting, 30 parts of plasticizer dioctyl terephthalate, fumed silica 5 Part is added sequentially in planet stirring kettle, is warming up under 110 DEG C of vacuum states and stirs 2 hours, ethylene is added after being cooled to room temperature Base trimethoxy silane water removal, after sequentially add 10 parts of crosslinking agent dimethoxydiphenylsilane, coupling agent 3- aminopropyl front three 5 parts of oxysilane, 5 parts of catalyst dibutyltin dilaurylate, 5 parts of co-catalyst lauryl amine stir 15min, discharging system Obtain B component.
In use, component A, B is mixed according to mass ratio 3:1.
Embodiment 2
A kind of dual-component silicane modified polyether seal glue of the present embodiment, component A and B component including weight ratio 3:1:
Component A is made of the raw material of following parts by weight:
35 parts of the trimethoxy terminated silane modified polyether polymer of viscosity 10000mPa.s, 35 parts of nanometer calcium carbonate, again 25 parts of calcium, 10 parts of fumed silica, 1.5 parts of carbon black, the polyether polyol and dioctyl terephthalate that molecular weight is 2000 Totally 40 parts, use polyvinyl alcohol and its derivative dispersion after 800 μm of 5 parts of penylene benzo dioxazole fiber staple fibers, phenyl three The heat-resistant agent boric oxide glass powder and 5 parts of alumag (weight ratio 1:1), 0.05 part of water of methoxy silane processing;
B component is made of the raw material of following parts by weight:
Totally 25 parts of 10 parts of coarse whiting, dibutyl phthalate and dioctyl terephthalate, 0.5 part of fumed silica, Tetraphenyl phenyl triethoxysilane and totally 1 part of diphenyl diethoxy silane mixture (weight ratio 1:1), bis- [(tri- ethoxies of 3- Base silicon substrate) propyl] one of amine 0.1 part, 1 part of stannous octoate, N, 1 part of accelerine.
Above-mentioned dual-component silicane modified polyether seal glue the preparation method is as follows:
Component A preparation: by 35 parts of the trimethoxy terminated silane modified polyether polymer of viscosity 10000mPa.s, nano-sized carbon 35 parts of sour calcium, 25 parts of coarse whiting, 10 parts of fumed silica, 1.5 parts of carbon black, molecular weight be 2000 polyether polyol and to benzene two Totally 40 parts of formic acid dioctyl ester uses the 800um penylene benzo dioxazole fiber staple fiber 5 after polyvinyl alcohol and its derivative dispersion The heat-resistant agent boric oxide glass powder and 5 parts of alumag, 0.05 part of water that part, phenyltrimethoxysila,e are handled, successively It is added in planet stirring kettle, 90min is stirred under room temperature, discharging is packaged to be component A;
The preparation process of B component are as follows: by 10 parts of coarse whiting, plasticizer phthalic acid dibutyl ester and dioctyl terephthalate Totally 25 parts, 0.5 part of fumed silica are added sequentially in planet stirring kettle, and it is small to be warming up to stirring 2 under 110 DEG C of vacuum states When, after being cooled to room temperature be added vinyltrimethoxysilane water removal, after sequentially add crosslinking agent tetraphenyl phenyl triethoxy Silane and bis- [(3- triethoxy silicon substrate) propyl] 0.1 part of the amine of totally 1 part of diphenyl diethoxy silane, coupling agent, catalyst are pungent 1 part of sour stannous, 1 part of co-catalyst n,N-Dimethylaniline stir 5min, discharge and B component is made.
In use, component A, B is mixed according to mass ratio 3:1.
Embodiment 3
A kind of dual-component silicane modified polyether seal glue of the present embodiment, component A and B component including weight ratio 3:1:
Component A is made of the raw material of following parts by weight:
33 parts of the trimethoxy terminated silane modified polyether polymer of viscosity 20000mPa.s, 40 parts of nanometer calcium carbonate, again 20 parts of calcium, 1.3 parts of carbon black, 30 parts of dioctyl terephthalate, uses modified natural polymer point at 5 parts of fumed silica 1000 μm of aramid fiber short fibres and 3 parts of penylene benzo dioxazole fibre blend (weight ratio 2:1), phenyl trimethoxy silicon after dissipating The heat-resistant agent gaseous oxidation aluminium and 3 parts of iron oxide mixture (weight ratio 2:1), 0.02 part of water of alkane processing;
B component is made of the raw material of following parts by weight:
25 parts of coarse whiting, 28 parts of the polyether polyol that molecular weight is 2000,2 parts of fumed silica, triphenylpyridinium base benzene 5 parts of ethyl triethoxy silicane alkane, 3- aminopropyl trimethoxysilane and bis- [(3- triethoxy silicon substrate) propyl] amine blends (weight Than 1:2) totally 3 parts, 2 parts of tin dilaurate dioctyl tin, 2 parts of low molecular polyamides.
Above-mentioned dual-component silicane modified polyether seal glue the preparation method is as follows:
Component A preparation: silane modified polyether polymer 33 part, nanometer that the trimethoxy of viscosity 20000mPa.s is blocked 40 parts of calcium carbonate, 5 parts of fumed silica, 1.3 parts of carbon black, 30 parts of dioctyl terephthalate, uses natural height at 20 parts of coarse whiting 1000 μm of aramid fiber short fibres and 3 parts of penylene benzo dioxazole fibre blend, phenyl trimethoxy after molecule derivant dispersion 3 parts of heat-resistant agent gaseous oxidation aluminium and iron oxide mixture, 0.02 part of the water of silane treatment, sequentially add in planet stirring kettle, often Temperature is lower to stir 50min, and discharging is packaged to be component A;
The preparation process of B component are as follows: by 25 parts of coarse whiting, 28 parts of the polyether polyol that plasticizer molecule amount is 2000, gas phase 2 parts of silica are added sequentially in planet stirring kettle, are warming up under 110 DEG C of vacuum states and stir 2 hours, after being cooled to room temperature Vinyltrimethoxysilane water removal is added, after sequentially add 5 parts of crosslinking agent triphenylpyridinium base phenyl triethoxysilane, even Join agent 3- aminopropyl trimethoxysilane and bis- [(3- triethoxy silicon substrate) propyl] totally 3 parts of amine blends, catalyst dibutyltin osmanthus 2 parts of sour dioctyl tin, 2 parts of co-catalyst low molecular polyamides stir 10min, discharge and B component is made;By component A, B according to Mass ratio 3:1 is mixed.
In use, component A, B is mixed according to mass ratio 3:1.
Comparative example 1
This comparative example is traditional silane modified polyether seal glue, is prepared according to the following recipe with technique:
By 50 parts of the silane modified polyether polymer of viscosity 15000mPa.s, 70 parts of nanometer calcium carbonate, 30 parts of coarse whiting, gas phase 6 parts of silica, 1.5 parts of carbon black, 60 parts of dioctyl terephthalate be added sequentially in planet stirring kettle, be warming up to 110 DEG C It is stirred 2 hours under vacuum state, vinyltrimethoxysilane water removal is added after being cooled to room temperature, 3- aminopropyl three is then added 2 parts of methoxy silane, 2 parts of dibutyl tin dilaurate stir 15min discharging and conventional silanes modified polyether are made under vacuum state Sealant.
Comparative example 2
A kind of silane modified polyether seal glue of this comparative example is prepared by following formulas and technique:
SPT type nm-class active calcium carbonate 41kg, R972 type fumed silica 1kg, R902 type is weighed respectively by formula White powder 4kg, PFZ type gas phase titanium dioxide is admired 1.8kg, 1010 type anti-aging agent 0.5kg, fumed titanium dioxide 1kg, N-220 charcoal by the emperor himself Black 0.4kg, Tinuvin 326 type ultraviolet absorber 0.3kg, Tinuvin 770 type light stabilizer 0.3kg be put into togerther double-planet Blender is heated to 110 DEG C, is slowly stirred (25-50rpm) 100 minutes;Addition S3O3H type silane modified polyether resin 35kg, DOP plasticizer 15kg vacuumizes and is heated to 1100C, and high-speed stirred (l000rpm) 150 minutes is cooled to 40 DEG C, is added VTMO silane 0.6kg, is slowly stirred (250rpm) 25 minutes, and phenyltrimethoxysila,e 1.2kg is added, is slowly stirred (250rpm) 25 minutes is added 1146 type silane attaches power promotor 0.4kg, is slowly stirred (250rpm) 25 minutes, be added two Dibutyl tin laurate 0.6kg, is slowly stirred (250rpm) 25 minutes, discharging.
Comparative example 3
A kind of dual-component silicane modified polyether seal glue of this comparative example, raw material and the preparation method is the same as that of Example 1, difference exist In: 200 μm of aramid fiber short fibres using after polyacrylate and its copolymer dispersion are not added.
Comparative example 4
A kind of dual-component silicane modified polyether seal glue of this comparative example, raw material and the preparation method is the same as that of Example 1, difference exist In: the water is not added.
It is tested by following experiment, by the dual-component silicane modified polyether seal glue of embodiment 1-3 with comparative example 1-4's The performance of silane modified polyether glue compares.
It is tested in following manner:
A surface drying time: under the conditions of 25 DEG C of 55%RH, the dry time is touched in test;
The b deep cure time: under the conditions of 25 DEG C of 55%RH, the time used in sealing glue solidifying depth >=4mm;
The test of c tensile strength: target product is coated uniformly on the mold of thickness 2mm after mixed glue, normal temperature cure 7d is pressed GB/T 528-2009 test;
The test piece being cured is placed 7d under the conditions of 180 DEG C by d, is then placed 1d at normal temperature and is tested tensile strength.
Test result is as shown in table 1:
Table 1
As shown in Table 1, under same experimental enviroment, the heat-resistance type rapid curing of preparation of the embodiment of the present invention is high-intensitive double Component silane modified polyether seal glue is compared with the common silane modified polyether glue of comparative example, surface drying time, deep cure time It greatly shortens, the process time can be reduced, greatly improve efficiency, the tensile strength after solidification significantly improves, and passes through high temperature resistant Aging after, tensile strength does not have significant change.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (10)

1. a kind of dual-component silicane modified polyether seal glue, which is characterized in that component A and B component including weight ratio 2-4:1;
Component A includes the raw material of following parts by weight:
Wherein, the silane that the heat-resistant agent after the silane treatment uses is phenyltrimethoxysila,e and/or 3,5-dimethylphenyl second Oxysilane, the weight percent that the silane accounts for the heat-resistant agent is 1-10%;
B component includes the raw material of following parts by weight:
2. dual-component silicane modified polyether seal glue according to claim 1, which is characterized in that
Component A includes the raw material of following parts by weight:
B component includes the raw material of following parts by weight:
3. dual-component silicane modified polyether seal glue according to claim 1, which is characterized in that the silane treatment is heat-resisting The method of agent includes the following steps:
By weight mix 100 parts of heat-resistant agent, 2-4 parts of silane, 0.5-1 parts of water, gained mixture under inert gas protection, in 100-110 DEG C of processing 1.5-2.5h.
4. dual-component silicane modified polyether seal glue according to claim 1, which is characterized in that the heat-resistant agent is gas phase One of aluminium oxide, iron oxide, boric oxide glass powder, aluminium hydroxide, zinc oxide, cerium oxide or multiple combinations.
5. dual-component silicane modified polyether seal glue according to claim 1, which is characterized in that the size of the fiber is 200μm-1000μm;The fiber is the combination of one or both of aramid fiber short fibre, penylene benzo dioxazole fiber.
6. dual-component silicane modified polyether seal glue according to claim 1, which is characterized in that the silane modified polyether Polymer is one of silane modified polyether polymer of trimethoxy sealing end or multiple combinations, and viscosity is in 5000- 20000mPa.s。
7. dual-component silicane modified polyether seal glue according to claim 1-6, which is characterized in that the crosslinking Agent is dimethoxydiphenylsilane, diphenyl diethoxy silane, triphenylpyridinium base phenyl triethoxysilane, tetraphenyl One of phenyl triethoxysilane or multiple combinations.
8. dual-component silicane modified polyether seal glue according to claim 1-6, which is characterized in that the plasticising Agent is dibutyl phthalate, dioctyl terephthalate, molecular weight are one of 2000 polyether polyol or a variety of Combination;The silane coupling agent is one of 3- aminopropyl trimethoxysilane, bis- [(3- triethoxy silicon substrate) propyl] amine Or two kinds of combinations;The filler is one of nanometer calcium carbonate, coarse whiting, fumed silica or multiple combinations.
9. dual-component silicane modified polyether seal glue according to claim 1-6, which is characterized in that the catalysis Agent is one of stannous octoate, dibutyl tin dilaurate, tin dilaurate dioctyl tin;The co-catalyst is dodecyl Amine, N, one of accelerine, low molecular polyamides or a variety of.
10. the preparation method of the described in any item dual-component silicane modified polyether seal glues of claim 1-9, which is characterized in that Include the following steps:
The preparation of the component A: by the fiber after the silane modified polyether polymer, filler, carbon black, dispersion, silane treatment Heat-resistant agent, plasticizer, water afterwards sequentially adds in planet stirring kettle, stirs 30-90min under room temperature, and discharge to obtain the component A;
The preparation of the B component: the filler, plasticizer being added sequentially in planet stirring kettle, are warming up to 105-115 DEG C, Stir 1.5-2.5 hours under vacuum state, removed water after being cooled to room temperature, then sequentially add the crosslinking agent, silane coupling agent, Catalyst, co-catalyst stir 5-15min, and discharge to obtain the B component.
CN201811161591.5A 2018-09-30 2018-09-30 Dual-component silicane modified polyether seal glue and preparation method thereof Pending CN109401710A (en)

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Application publication date: 20190301