CN109054712A - A kind of fire resistant epoxy gluing agent - Google Patents
A kind of fire resistant epoxy gluing agent Download PDFInfo
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- CN109054712A CN109054712A CN201811104013.8A CN201811104013A CN109054712A CN 109054712 A CN109054712 A CN 109054712A CN 201811104013 A CN201811104013 A CN 201811104013A CN 109054712 A CN109054712 A CN 109054712A
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- resistant epoxy
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of fire resistant epoxy gluing agent, belong to building material technical field.The present invention mixes silicon nitride crystal whisker with hydrofluoric acid 1:10~1:20 in mass ratio, filters, washing, silicon nitride crystal whisker must be pre-processed, according to parts by weight, by 20~30 parts of pretreatment silicon nitride crystal whiskers, 10~20 parts of lards, 2~3 parts of lipase, 5~8 parts of starch, 20~30 parts of ethylene glycol, 10~30 parts of ethyl orthosilicate mixing and ball millings, high-temperature stirring reaction, filtering, dry, pyroreaction is to get modified crystal whiskers；By epoxy resin, diluent, modified additive, rubber powder, modified crystal whiskers, cupric oxalate, manganese oxalate and coupling agent are stirred to get fire resistant epoxy gluing agent.Fire resistant epoxy gluing agent provided by the invention has excellent high temperature stability performance.
Description
Technical field
The invention discloses a kind of fire resistant epoxy gluing agent, belong to building material technical field.
Background technique
Based on molecular structure property, the application temperature of epoxy resin adhesive is usually less than 125 DEG C.It is higher in order to obtain
Following 4 kinds of methods are usually taken in heat resistance:
(1) heat resistance more high resin is added in epoxy resin and forms blend；
(2) high-temperature curing agent；
(3) heat resistant epoxide resin；
(4) combination of above-mentioned 3 kinds of methods.
Aromatic dicarboxylic anhydride is a kind of high-temperature curing agent, can be improved the heat resistance of epoxy adhesive.In epoxy-virtue
In fragrant race's anhydride system adhesive, Emerson&Cuming production ECCOBOND-104 adhesive it is most representative, it be by
Bisphenol A type epoxy resin is basic resin, and pyromellitic acid dianhydride is the Bi-component high-temperature resistant adhesive of curing agent composition, using temperature
Up to 230 DEG C of degree, the temperature of highest application in short-term is up to 290 DEG C.The glue practical many years in aircraft engine manufacture adhesive technology,
It is functional, securely and reliably.Traditional epoxy adhesive problem bad there is also high temperature stability performance at present, therefore also need pair
It is studied.
Summary of the invention
The present invention solves the technical problem of: for the bad problem of conventional epoxy adhesive high temperature stability performance,
Provide a kind of fire resistant epoxy gluing agent.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of fire resistant epoxy gluing agent, is made of the raw material of following parts by weight:
20~30 parts of epoxy resin
20~30 parts of diluent
5~8 parts of modified additive
3~5 parts of rubber powder
8~10 parts of modified crystal whiskers
3~5 parts of cupric oxalate
3~5 parts of ethylenediamine
3~5 parts of coupling agent
The preparation process of the fire resistant epoxy gluing agent are as follows: each raw material is weighed by raw material composition, by epoxy resin, diluent,
Modified additive, rubber powder, modified crystal whiskers, cupric oxalate, ethylenediamine and coupling agent are stirred to get fire resistant epoxy gluing agent.
The epoxy resin is epoxy resin E-42, any one in epoxy resin E-44 or epoxy resin E-52.
The diluent is acetone, ethyl alcohol, any one in dimethylbenzene or toluene.
The preparation process of the modified additive are as follows: sepiolite is mixed with casein solution 1:10~1:20 in mass ratio and is surpassed
Sound filters, dry, pretreatment sepiolite is obtained, according to parts by weight, by 20~30 parts of pretreatment sepiolites, 8~10 parts of carbomers
934P, 30~40 parts of deionized water constant temperature are stirred, filtering, dry to get modified additive.
The rubber powder is peach gum powder, jelly powder, any one in rubber powder or gelatine powder.
The preparation process of the modified crystal whiskers are as follows: silicon nitride crystal whisker is mixed with hydrofluoric acid 1:10~1:20 in mass ratio,
Filtering, washing, obtains pretreatment silicon nitride crystal whisker, according to parts by weight, by 20~30 parts of pretreatment silicon nitride crystal whiskers, 10~20 parts
Lard, 2~3 parts of lipase, 5~8 parts of starch, 20~30 parts of ethylene glycol, 10~30 parts of ethyl orthosilicate mixing and ball millings, high temperature stir
Reaction is mixed, is filtered, dry, pyroreaction is to get modified crystal whiskers.
The coupling agent is aluminate coupling agent, any one in silane coupling agent or titanate coupling agent.
The beneficial effects of the present invention are:
The present invention is by addition modified crystal whiskers and cupric oxalate, firstly, during the preparation process, silicon nitride crystal whisker passes through the place of hydrofluoric acid
Reason, so that there are a large amount of pits in whisker surface, meanwhile, so that the active group on whisker surface is exposed, it then will pretreatment
Silicon nitride crystal whisker, lard, lipase, glycerol, starch, ethylene glycol, ethyl orthosilicate mixing and ball milling, in mechanical milling process, fat
Enzymatic Hydrolysis of Lard generates fatty acid, and in high-temperature stirring reaction process, esterification occurs for fatty acid and ethylene glycol, raw
At water reacted with ethyl orthosilicate, generate nano silica, once generate nano silica it is recessed with regard to modified crystal whiskers surface
Hole absorption, so that the roughness of whisker table is improved, so that whisker skeleton is easily formed between whisker, then, in pyroreaction mistake
Cheng Zhong, the organic matter charing on silicon nitride crystal whisker surface constitute carbonaceous skeleton on whisker surface, meanwhile, it is generated in reaction process big
The tar of amount, as temperature gradually rises, charcoal in system, nitrogen and nanometer titanium dioxide pasc reaction generate silicon nitride, secondly,
In use, modified crystal whiskers constitute thermally conductive whisker network in system, and the tar exudation in system is conducive to improve being modified
The interface resistance between modified crystal whiskers and matrix resin is effectively reduced in interface cohesion between whisker and matrix resin, enables heat
Enough quickly to spread in system, so that the high-temperature stability of system gets a promotion, again, cupric oxalate is thermally decomposed, raw
At carbon dioxide and elemental copper, titanium dioxide Carbon diffusion accelerates the dissipation of heat in system, while can carry by single
Copper is dispersed in around thermally conductive whisker network, so that the heating conduction of whisker network gets a promotion, to further improve system
High temperature stability performance.
Specific embodiment
Casein solution 1:10~1:20 in mass ratio that sepiolite and mass concentration are 2.6mg/mL is placed in No. 1 beaker
In, No. 1 beaker is then placed in ultrasonic disperse instrument, under the conditions of supersonic frequency is 55~75kHz, mixes 40~60min of ultrasound,
Dispersion liquid, then dispersion liquid is filtered, obtains No. 1 filter cake, then No. 1 filter cake is placed in baking oven, in temperature be 105~110 DEG C
Under the conditions of, it is dry to constant weight, pretreatment sepiolite is obtained, according to parts by weight, and by 20~30 parts of pretreatment sepiolites, 8~10 parts
Carbomer940,30~40 parts of deionized waters are placed in No. 2 beakers, and No. 2 beakers are then placed in the digital display constant temperature magnetic force that tests the speed and are stirred
It mixes in device, is 40~60 DEG C in temperature, under the conditions of revolving speed is 300~500r/min, constant temperature is stirred 40~60min, obtains mixed
Close slurries, then mixed serum is filtered, obtains No. 2 filter cakes, then No. 2 filter cakes are placed in baking oven, in temperature be 105~110
Under the conditions of DEG C, drying is to constant weight to get modified additive；The hydrofluoric acid that silicon nitride crystal whisker is 30~35% with mass fraction is pressed
Mass ratio 1:10~1:20 is placed in mixing kettle, under the conditions of revolving speed is 300~500r/min, is stirred 40~60min, is obtained
Mixed liquor then filters mixed liquor, obtains No. 1 filter residue, and the ammonium hydroxide for being then 20~30% with mass fraction is by No. 1 filter residue
Washing to cleaning solution is neutrality, obtains pretreatment silicon nitride crystal whisker, according to parts by weight, 20~30 parts of pretreatments is nitrogenized silicon wafer
Palpus, 10~20 parts of lards, 2~3 parts of lipase, 5~8 parts of starch, 20~30 parts of ethylene glycol, 10~30 parts of ethyl orthosilicates are placed in
40~60min of mixing and ball milling in ball mill obtains ball milling material, and then ball milling material is placed in reaction kettle, in temperature be 140~160
Under the conditions of DEG C, high-temperature stirring reaction obtains mixed slurry, then filters mixed slurry, obtain No. 2 filter residues, then sets No. 2 filter residues
It is dry to constant weight under the conditions of temperature is 105~110 DEG C in baking oven, No. 2 filter residues must be dried, then by dry No. 2 filter residues
Be placed in tube furnace, nitrogen be then filled with into tube furnace with the rate of 60~90mL/min, in temperature be 1400~1550 DEG C
Under the conditions of, 2~3h of pyroreaction is to get modified crystal whiskers；According to parts by weight, by 20~30 parts of epoxy resin, 20~30 parts dilute
Release agent, 5~8 parts of modified additives, 3~5 parts of rubber powders, 8~10 parts of modified crystal whiskers, 3~5 parts of cupric oxalates, 3~5 parts of ethylenediamines and 3
~5 parts of coupling agents are placed in batch mixer, in revolving speed be 1100~1200r/min under the conditions of, be stirred 40~60min to get
Fire resistant epoxy gluing agent.The epoxy resin is epoxy resin E-42, appointing in epoxy resin E-44 or epoxy resin E-52
It anticipates one kind.The diluent is acetone, ethyl alcohol, any one in dimethylbenzene or toluene.The rubber powder is peach gum powder, gelatin
Any one in powder, rubber powder or gelatine powder.The coupling agent is aluminate coupling agent, silane coupling agent or titanate esters coupling
Any one in agent.
The casein solution 1:20 in mass ratio that sepiolite and mass concentration are 2.6mg/mL is placed in No. 1 beaker, then
No. 1 beaker is placed in ultrasonic disperse instrument, under the conditions of supersonic frequency is 75kHz, mixes ultrasound 60min, obtains dispersion liquid, then will divide
Dispersion liquid filtering, obtains No. 1 filter cake, then No. 1 filter cake is placed in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains
Sepiolite is pre-processed, according to parts by weight, by 30 parts of pretreatment sepiolites, 10 parts of carbomer940s, 40 parts of deionized waters are placed in 2
In number beakers, No. 2 beakers are then placed in digital display and are tested the speed in constant temperature blender with magnetic force, in temperature be 60 DEG C, revolving speed 500r/
Under the conditions of min, constant temperature is stirred 60min, obtains mixed serum, then filters mixed serum, obtains No. 2 filter cakes, then by No. 2
Filter cake is placed in baking oven, and under the conditions of temperature is 110 DEG C, drying is to constant weight to get modified additive；By silicon nitride crystal whisker and matter
The hydrofluoric acid 1:20 in mass ratio that amount score is 35% is placed in mixing kettle, under the conditions of revolving speed is 500r/min, is stirred
60min obtains mixed liquor, then filters mixed liquor, obtains No. 1 filter residue, and the ammonium hydroxide for being then 30% with mass fraction is by No. 1
Residue washing to cleaning solution is neutrality, obtains pretreatment silicon nitride crystal whisker, according to parts by weight, 30 parts of pretreatments is nitrogenized silicon wafer
Palpus, 20 parts of lards, 3 parts of lipase, 8 parts of starch, 30 parts of ethylene glycol, 30 parts of ethyl orthosilicates are placed in mixing and ball milling in ball mill
60min obtains ball milling material, and then ball milling material is placed in reaction kettle, and under the conditions of temperature is 160 DEG C, high-temperature stirring reaction is obtained mixed
Close slurry, then mixed slurry is filtered, obtains No. 2 filter residues, then No. 2 filter residues are placed in baking oven, in temperature be 110 DEG C of conditions
Under, it is dry to constant weight, No. 2 filter residues must be dried, then dry No. 2 filter residues are placed in tube furnace, then with the speed of 90mL/min
Rate is filled with nitrogen into tube furnace, and under the conditions of temperature is 1550 DEG C, pyroreaction 3h is to get modified crystal whiskers；In parts by weight
Meter, by 30 parts of epoxy resin, 30 parts of diluents, 8 parts of modified additives, 5 parts of rubber powders, 10 parts of modified crystal whiskers, 5 parts of cupric oxalates, 5 parts
Ethylenediamine and 5 parts of coupling agents are placed in batch mixer, under the conditions of revolving speed is 1200r/min, are stirred 60min to get resistance to height
Temperature epoxy adhesive.The epoxy resin is epoxy resin E-42.The diluent is acetone.The rubber powder is peach gum powder.Institute
Stating coupling agent is aluminate coupling agent.
The hydrofluoric acid 1:20 in mass ratio that silicon nitride crystal whisker and mass fraction are 35% is placed in mixing kettle, is in revolving speed
Under the conditions of 500r/min, it is stirred 60min, mixed liquor is obtained, then filters mixed liquor, No. 1 filter residue is obtained, then uses matter
No. 1 residue washing to cleaning solution is neutrality by the ammonium hydroxide that amount score is 30%, obtains pretreatment silicon nitride crystal whisker, according to parts by weight,
By 30 parts of pretreatment silicon nitride crystal whiskers, 20 parts of lards, 3 parts of lipase, 8 parts of starch, 30 parts of ethylene glycol, 30 parts of ethyl orthosilicates are set
The mixing and ball milling 60min in ball mill obtains ball milling material, and then ball milling material is placed in reaction kettle, in temperature be 160 DEG C of conditions
Under, high-temperature stirring reaction obtains mixed slurry, then filters mixed slurry, obtain No. 2 filter residues, No. 2 filter residues are then placed in baking oven
In, it is dry to constant weight under the conditions of temperature is 110 DEG C, No. 2 filter residues must be dried, dry No. 2 filter residues are then placed in tube furnace
In, nitrogen is then filled with into tube furnace with the rate of 90mL/min, under the conditions of temperature is 1550 DEG C, pyroreaction 3h, i.e.,
Obtain modified crystal whiskers；According to parts by weight, by 30 parts of epoxy resin, 30 parts of diluents, 5 parts of rubber powders, 10 parts of modified crystal whiskers, 5 parts of grass
Sour copper, 5 parts of ethylenediamines and 5 parts of coupling agents are placed in batch mixer, under the conditions of revolving speed is 1200r/min, are stirred 60min,
Up to fire resistant epoxy gluing agent.The epoxy resin is epoxy resin E-42.The diluent is acetone.The rubber powder is peach
Rubber powder.The coupling agent is aluminate coupling agent.
The casein solution 1:20 in mass ratio that sepiolite and mass concentration are 2.6mg/mL is placed in No. 1 beaker, then
No. 1 beaker is placed in ultrasonic disperse instrument, under the conditions of supersonic frequency is 75kHz, mixes ultrasound 60min, obtains dispersion liquid, then will divide
Dispersion liquid filtering, obtains No. 1 filter cake, then No. 1 filter cake is placed in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains
Sepiolite is pre-processed, according to parts by weight, by 30 parts of pretreatment sepiolites, 10 parts of carbomer940s, 40 parts of deionized waters are placed in 2
In number beakers, No. 2 beakers are then placed in digital display and are tested the speed in constant temperature blender with magnetic force, in temperature be 60 DEG C, revolving speed 500r/
Under the conditions of min, constant temperature is stirred 60min, obtains mixed serum, then filters mixed serum, obtains No. 2 filter cakes, then by No. 2
Filter cake is placed in baking oven, and under the conditions of temperature is 110 DEG C, drying is to constant weight to get modified additive；By silicon nitride crystal whisker and matter
The hydrofluoric acid 1:20 in mass ratio that amount score is 35% is placed in mixing kettle, under the conditions of revolving speed is 500r/min, is stirred
60min obtains mixed liquor, then filters mixed liquor, obtains No. 1 filter residue, and the ammonium hydroxide for being then 30% with mass fraction is by No. 1
Residue washing to cleaning solution is neutrality, obtains pretreatment silicon nitride crystal whisker, according to parts by weight, 30 parts of pretreatments is nitrogenized silicon wafer
Palpus, 20 parts of lards, 3 parts of lipase, 8 parts of starch, 30 parts of ethylene glycol, 30 parts of ethyl orthosilicates are placed in mixing and ball milling in ball mill
60min obtains ball milling material, and then ball milling material is placed in reaction kettle, and under the conditions of temperature is 160 DEG C, high-temperature stirring reaction is obtained mixed
Close slurry, then mixed slurry is filtered, obtains No. 2 filter residues, then No. 2 filter residues are placed in baking oven, in temperature be 110 DEG C of conditions
Under, it is dry to constant weight, No. 2 filter residues must be dried, then dry No. 2 filter residues are placed in tube furnace, then with the speed of 90mL/min
Rate is filled with nitrogen into tube furnace, and under the conditions of temperature is 1550 DEG C, pyroreaction 3h is to get modified crystal whiskers；In parts by weight
Meter, by 30 parts of epoxy resin, 30 parts of diluents, 8 parts of modified additives, 10 parts of modified crystal whiskers, 5 parts of cupric oxalates, 5 parts of ethylenediamines and
5 parts of coupling agents are placed in batch mixer, under the conditions of revolving speed is 1200r/min, are stirred 60min to get high temperature resistant epoxy
Glutinous agent.The epoxy resin is epoxy resin E-42.The diluent is acetone.The coupling agent is aluminate coupling agent.
The casein solution 1:20 in mass ratio that sepiolite and mass concentration are 2.6mg/mL is placed in No. 1 beaker, then
No. 1 beaker is placed in ultrasonic disperse instrument, under the conditions of supersonic frequency is 75kHz, mixes ultrasound 60min, obtains dispersion liquid, then will divide
Dispersion liquid filtering, obtains No. 1 filter cake, then No. 1 filter cake is placed in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains
Sepiolite is pre-processed, according to parts by weight, by 30 parts of pretreatment sepiolites, 10 parts of carbomer940s, 40 parts of deionized waters are placed in 2
In number beakers, No. 2 beakers are then placed in digital display and are tested the speed in constant temperature blender with magnetic force, in temperature be 60 DEG C, revolving speed 500r/
Under the conditions of min, constant temperature is stirred 60min, obtains mixed serum, then filters mixed serum, obtains No. 2 filter cakes, then by No. 2
Filter cake is placed in baking oven, and under the conditions of temperature is 110 DEG C, drying is to constant weight to get modified additive；According to parts by weight, will
30 parts of epoxy resin, 30 parts of diluents, 8 parts of modified additives, 5 parts of rubber powders, 5 parts of cupric oxalates, 5 parts of ethylenediamines and 5 parts of coupling agents
It is placed in batch mixer, under the conditions of revolving speed is 1200r/min, is stirred 60min to get fire resistant epoxy gluing agent.It is described
Epoxy resin is epoxy resin E-42.The diluent is acetone.The rubber powder is peach gum powder.The coupling agent is that Aluminate is even
Join agent.
The casein solution 1:20 in mass ratio that sepiolite and mass concentration are 2.6mg/mL is placed in No. 1 beaker, then
No. 1 beaker is placed in ultrasonic disperse instrument, under the conditions of supersonic frequency is 75kHz, mixes ultrasound 60min, obtains dispersion liquid, then will divide
Dispersion liquid filtering, obtains No. 1 filter cake, then No. 1 filter cake is placed in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains
Sepiolite is pre-processed, according to parts by weight, by 30 parts of pretreatment sepiolites, 10 parts of carbomer940s, 40 parts of deionized waters are placed in 2
In number beakers, No. 2 beakers are then placed in digital display and are tested the speed in constant temperature blender with magnetic force, in temperature be 60 DEG C, revolving speed 500r/
Under the conditions of min, constant temperature is stirred 60min, obtains mixed serum, then filters mixed serum, obtains No. 2 filter cakes, then by No. 2
Filter cake is placed in baking oven, and under the conditions of temperature is 110 DEG C, drying is to constant weight to get modified additive；By silicon nitride crystal whisker and matter
The hydrofluoric acid 1:20 in mass ratio that amount score is 35% is placed in mixing kettle, under the conditions of revolving speed is 500r/min, is stirred
60min obtains mixed liquor, then filters mixed liquor, obtains No. 1 filter residue, and the ammonium hydroxide for being then 30% with mass fraction is by No. 1
Residue washing to cleaning solution is neutrality, obtains pretreatment silicon nitride crystal whisker, according to parts by weight, 30 parts of pretreatments is nitrogenized silicon wafer
Palpus, 20 parts of lards, 3 parts of lipase, 8 parts of starch, 30 parts of ethylene glycol, 30 parts of ethyl orthosilicates are placed in mixing and ball milling in ball mill
60min obtains ball milling material, and then ball milling material is placed in reaction kettle, and under the conditions of temperature is 160 DEG C, high-temperature stirring reaction is obtained mixed
Close slurry, then mixed slurry is filtered, obtains No. 2 filter residues, then No. 2 filter residues are placed in baking oven, in temperature be 110 DEG C of conditions
Under, it is dry to constant weight, No. 2 filter residues must be dried, then dry No. 2 filter residues are placed in tube furnace, then with the speed of 90mL/min
Rate is filled with nitrogen into tube furnace, and under the conditions of temperature is 1550 DEG C, pyroreaction 3h is to get modified crystal whiskers；In parts by weight
Meter, by 30 parts of epoxy resin, 30 parts of diluents, 8 parts of modified additives, 5 parts of rubber powders, 10 parts of modified crystal whiskers, 5 parts of ethylenediamines and 5
Part coupling agent is placed in batch mixer, under the conditions of revolving speed is 1200r/min, is stirred 60min to get fire resistant epoxy gluing
Agent.The epoxy resin is epoxy resin E-42.The diluent is acetone.The rubber powder is peach gum powder.The coupling agent is
Aluminate coupling agent.
Comparative example: the epoxy adhesive of Guangzhou Industrial Co., Ltd. production.
1 to 5 gained adhesive of example and comparative example product are subjected to performance detection, the specific detection method is as follows:
Room temperature shear strength is executed by GB/T7124, and shear at high temperature intensity is executed by GJB/444, and test piece material is the conjunction of LY12CZ aluminium
Gold, specification 60mm × 20mm × 3mm, splicing area: 20mm × 15mm.TGA analysis, room temperature~230 DEG C, air atmosphere, heating
10 DEG C/min of rate.
Table 1
By 1 testing result of table it is found that present invention gained fire resistant epoxy gluing agent has excellent high temperature stability performance.
Claims (7)
1. a kind of fire resistant epoxy gluing agent, it is characterised in that: be made of the raw material of following parts by weight:
20~30 parts of epoxy resin
20~30 parts of diluent
5~8 parts of modified additive
3~5 parts of rubber powder
8~10 parts of modified crystal whiskers
3~5 parts of cupric oxalate
3~5 parts of ethylenediamine
3~5 parts of coupling agent
The preparation process of the fire resistant epoxy gluing agent are as follows: each raw material is weighed by raw material composition, by epoxy resin, diluent,
Modified additive, rubber powder, modified crystal whiskers, cupric oxalate, manganese oxalate and coupling agent are stirred to get fire resistant epoxy gluing agent.
2. a kind of fire resistant epoxy gluing agent according to claim 1, it is characterised in that: the epoxy resin is epoxy resin
Any one in E-42, epoxy resin E-44 or epoxy resin E-52.
3. a kind of fire resistant epoxy gluing agent according to claim 1, it is characterised in that: the diluent be acetone, ethyl alcohol,
Any one in dimethylbenzene or toluene.
4. a kind of fire resistant epoxy gluing agent according to claim 1, it is characterised in that: the preparation of the modified additive
Journey are as follows: sepiolite is mixed into ultrasound with casein solution 1:10~1:20 in mass ratio, is filtered, it is dry, pretreatment sepiolite is obtained, is pressed
Parts by weight meter, by 20~30 parts of pretreatment sepiolites, 8~10 parts of carbomer940s, 30~40 parts of deionized water constant temperature stirrings
Mixing, filtering are dry to get modified additive.
5. a kind of fire resistant epoxy gluing agent according to claim 1, it is characterised in that: the rubber powder is peach gum powder, gelatin
Any one in powder, rubber powder or gelatine powder.
6. a kind of fire resistant epoxy gluing agent according to claim 1, it is characterised in that: the preparation process of the modified crystal whiskers
Are as follows: silicon nitride crystal whisker is mixed with hydrofluoric acid 1:10~1:20 in mass ratio, is filtered, washing obtains pretreatment silicon nitride crystal whisker, presses
Parts by weight meter, by 20~30 parts of pretreatment silicon nitride crystal whiskers, 10~20 parts of lards, 2~3 parts of lipase, 5~8 parts of starch, 20
~30 parts of ethylene glycol, 10~30 parts of ethyl orthosilicate mixing and ball millings, high-temperature stirring reaction are filtered, dry, pyroreaction to get
Modified crystal whiskers.
7. a kind of fire resistant epoxy gluing agent according to claim 1, it is characterised in that: the coupling agent is Aluminate coupling
Any one in agent, silane coupling agent or titanate coupling agent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109929235A (en) * | 2019-03-03 | 2019-06-25 | 姜丽丽 | A kind of electric-conductivity heat-conductivity high carbon nano-complex and preparation method thereof |
| CN110184008A (en) * | 2019-05-20 | 2019-08-30 | 秦臻 | A kind of preparation method of epoxy group heat conductive insulating compound cutan |
| CN110746917A (en) * | 2019-10-18 | 2020-02-04 | 李志兴 | Preparation method of high-temperature-resistant epoxy resin adhesive |
Citations (2)
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| CN110184008A (en) * | 2019-05-20 | 2019-08-30 | 秦臻 | A kind of preparation method of epoxy group heat conductive insulating compound cutan |
| CN110746917A (en) * | 2019-10-18 | 2020-02-04 | 李志兴 | Preparation method of high-temperature-resistant epoxy resin adhesive |
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Application publication date: 20181221 |