CN107936470A - A kind of preparation method of epoxy resin-base composite material - Google Patents
A kind of preparation method of epoxy resin-base composite material Download PDFInfo
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- CN107936470A CN107936470A CN201711096574.3A CN201711096574A CN107936470A CN 107936470 A CN107936470 A CN 107936470A CN 201711096574 A CN201711096574 A CN 201711096574A CN 107936470 A CN107936470 A CN 107936470A
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/32—Epoxy compounds containing three or more epoxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5006—Amines aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
- C08G59/72—Complexes of boron halides
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08K2201/005—Additives being defined by their particle size in general
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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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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A kind of epoxy resin-base composite material of the present invention and preparation method thereof, belongs to technical field of composite materials.The present invention uses 4,4 diaminodiphenylmethane, four glycidyl amine, and heat resistance is good；Using T-shaped bimaleimide resin as toughener, using titanium dioxide, phlogopite as filler, strengthen its hardness, adjust its thermal coefficient of expansion, it is matched with stainless steel cavity, and improve its heat shock resistance and heat resistance；It is curing agent by accelerating agent, triethanolamine of Boron Trifluoride Ethylamine, adjusts its viscosity and cure crosslinking rate.It is rough that the present invention solves the epoxy fill-sealing materials embedding rear surface that ionic flame detector uses, the problems such as cracking, chip off-falling, its heat resistance brings up to 408 DEG C from original 361 DEG C, thermal coefficient of expansion matches with embedding impression material, material property meets auxiliary products requirement, the epoxy resin-base composite material has been successfully applied to the embedding of all kinds of aviation ionic flame detectors, packing material, very big economic benefit and social benefit.
Description
Technical field
A kind of epoxy resin-base composite material of the present invention and preparation method thereof, belongs to technical field of composite materials.
Background technology
Epoxy resin-base composite material is due to its good bonding, flexure, toughness, thermochemical property, good moisture resistance,
It is good to cure rear surface finish, is widely used in structural member filling, sealing.Particularly in aero-engine ion fire
Flame detector field, due to the characteristics of epoxy resin-base composite material heat resisting temperature is high, mechanical strength is high and resistance to pressure is good, can fill
The flame detecting working environment for meeting that aero-engine is harsh divided, as filling, fixed structure in ionic flame detector
Function is widely used.
Ionic flame detector uses existing short chain epoxy resin encapsulated material, and it is in cellular defect to cure rear surface,
Face checking, chip off-falling are mismatched mainly due to thermal coefficient of expansion, caused by curing cross-linking process is insufficient.Filled with epoxy resin
The impression material of closure material contact is stainless steel (1Cr18Ni9Ti), sealing alloy (4J34), aluminium oxide ceramics (A-95).Wherein
Sealing alloy is welded into contact pin component for electrode material and aluminium oxide ceramics, ceramics and epoxy resin encapsulated material area compared with
Small (about 63mm2), metal and larger (the about 2525mm of epoxy resin encapsulated material area2), mold cavity volume is larger
(15725mm3), mainly influenced when curing crosslinking by metal material thermal expansion, the thermal coefficient of expansion of epoxy resin encapsulated material
Metal is should be slightly bigger than, forms compression.
The epoxy resin-base composite material newly developed uses polyfunctional epoxy resin, and the viscosity of material being prepared into is low, easily
In embedding, cohesive force is strong, cures that cross-linking agent density is big, and shrinking percentage is low, has an excellent mechanical property, heat resistance and corrosion-resistant
Property.Verification result shows that all technical all meets associated specifications.
The content of the invention
The purpose of the present invention：After epoxy resin-base composite material cures crosslinking, its sealing-in gap can be effectively filled, it is fixed to insert
Pin and conducting wire, and insulating properties good between two contact pins can be kept, solve cracking, chip off-falling, linear expansion coefficient mismatch after sealing-in
And the problems such as cellular defect, improve the heat resistance that product uses, durability and security.
The prior art is using dicyclopentadiene as matrix, using dibutyl phthalate as toughener, with maleic anhydride
For curing agent, asbestos, silica flour, alumina powder are added to improve its hardness, shrinking percentage and thermal coefficient of expansion is reduced, improves impact
Intensity and heat resistance.The epoxy resin encapsulated material mechanical performance of prior art production is poor, and thermal coefficient of expansion is larger, during curing
Easily produce very big crackle, or even chip off-falling.In solidification process, since the viscosity of Embedding Material is big, the gas of secondary generation during heating
Bubble can not exclude, and the bubble to differ in size or cellular defect are formed on its surface.
The epoxy resin-base composite material newly developed uses 4,4- diaminodiphenylmethane, four glycidyl amine, heat resistance
It is good；Using T-shaped bimaleimide resin as toughener, using titanium dioxide, phlogopite as filler, strengthen its hardness, adjust its heat
The coefficient of expansion, makes it match with stainless steel cavity, and improves its heat shock resistance and heat resistance；Using boron triflouride-mono aminoethane as
Accelerating agent, triethanolamine are curing agent, adjust its viscosity and cure crosslinking rate.According to rational technological process during embedding, Gu
Using stringent temperature schedule during change, its surface is smooth after curing, flawless.Ionic flame detector carries out skill in factory after embedding
Art examination verification, items examination are qualified.
Technical scheme：A kind of epoxy resin-base composite material, the composition of the epoxy resin-base composite material
Component includes four glycidol of 4,4- diaminodiphenylmethane, T-shaped bimaleimide resin, titanium dioxide, phlogopite, trifluoro
Change boron-mono aminoethane, triethanolamine；The ratio of 4,4- diaminodiphenylmethane, four glycidol is 55%, T-shaped bismaleimide
The ratio of resin is 13.2%~15.5%, the ratio of titanium dioxide is 16.5%~22%, the ratio of phlogopite be 3.3%~
5.5%th, the ratio of boron triflouride-mono aminoethane is 0.34%~0.7%；The ratio of triethanolamine is 0.76%~1.3%.
A kind of preparation method of epoxy resin-base composite material, the method take following steps：
1) pretreatment of titanium dioxide
Titanium dioxide is placed in high-temperature resistant container, at least 2h is kept the temperature at 950 DEG C and is heat-treated, titanium dioxide is whole
Change into stable golden red type titanium dioxide；By golden red type titanium dioxide ball milling on ball mill through Overheating Treatment, make its grain
Degree reaches more than 200 mesh；
2) pretreatment of phlogopite
Phlogopite is soaked into 2~4h in 10% dilute hydrochloric acid solution, removes the impurity iron of phlogopite, fully washing immersion
Phlogopite afterwards, and it is dried, the ball milling on ball mill, makes its granularity reach more than 200 mesh, and the phlogopite of acquisition is bottled
It is spare；
3) preparation of epoxy resin-base composite material
By raw material according to 4,4- diaminodiphenylmethane, four glycidol ratio be 55%, T-shaped bismaleimide
The ratio of resin is 13.2%~15.5%, the ratio of titanium dioxide is 16.5%~22%, the ratio of phlogopite be 3.3%~
5.5%th, the ratio of boron triflouride-mono aminoethane is 0.34%~0.7%；The ratio of triethanolamine prepares for 0.76%~1.3%
After good, prepared according to following flow：
A) 4,4- diaminodiphenylmethane, four glycidyl amine is put into high-temperature resistant container, added in 70~80 DEG C of water-baths
It is in flow regime that heat, which arrives,；
B) add T-shaped span while being stirred to four glycidyl amine of liquid 4,4- diaminodiphenylmethane and carry out acyl
Imide resin, and be sufficiently stirred；
C) titanium dioxide, phlogopite are added in the mixture obtained to step b, and be sufficiently stirred；
D) boron triflouride-mono aminoethane, triethanolamine are added in the mixture obtained to step c, and be sufficiently stirred；
4) mixture finally obtained in step 3 is subjected to crosslinking curing
The mixture finally obtained in step 3 is put into drying box, the temperature in drying box is in room temperature between 60 DEG C
When, mixture freely heats up with drying box；At 60 DEG C~80 DEG C, the temperature of mixture raises temperature in drying box per hour
10℃；For temperature in drying box at 80 DEG C~100 DEG C, the temperature of mixture raises 20 DEG C per hour；Temperature in drying box
At 100 DEG C~150 DEG C, the temperature of mixture raises 50 DEG C per hour；Temperature in drying box is mixed at 150 DEG C~180 DEG C
The temperature of compound freely heats up with drying box；Temperature in drying box is at 180 DEG C, the temperature 2h of mixture, cures and hands over
After connection, mixture is taken out after being cooled down with drying box.
Advantages of the present invention：The present invention relates to a kind of High temperature epoxy resins based composites, its heatproof is more than 400 DEG C.This
The problems such as it is rough that invention solves the epoxy fill-sealing materials embedding rear surface that ionic flame detector uses, cracking, chip off-falling, its
Heat resistance brings up to 408 DEG C from original 361 DEG C, and thermal coefficient of expansion matches with embedding impression material, and material property meets to match somebody with somebody
Product requirement is covered, which has been successfully applied to the embedding of all kinds of aviation ionic flame detectors, has filled out
Material is filled, and generates very big economic benefit and social benefit.
Epoxy resin-base composite material according to the present invention, solves its formula design, material handling procedures, material
Preparation process and construction method.It is formulated and material requirements is shown in Table 1, and performance comparison is shown in Table 2.
Epoxy resin-base composite material of the present invention is applicable not only to the embedding of aviation particle flame detector, fills out
Fill, be also applied for other civilian flame detectors.
Brief description of the drawings
Fig. 1 fills schematic diagram for HTQ-17A/18A ionic flames detector.
Wherein, 1 is insulator, and 2 be stainless steel bushing, and 3 be housing unit, and 4 be the epoxy resin-matrix being filled into cavity
Composite material, 5 be metal cover board, and 6 be copper conductor, and 7 be sealing alloy contact pin, and 8 be insulator.
Embodiment
The present invention is described in more detail below in conjunction with the accompanying drawings.
A kind of epoxy resin-base composite material, the constituent of the epoxy resin-base composite material include 4,4- diaminourea
Four glycidol of diphenyl-methane, T-shaped bimaleimide resin, titanium dioxide, phlogopite, boron triflouride-mono aminoethane, three ethanol
Amine；The ratio of 4,4- diaminodiphenylmethane, four glycidol is 55%, and the ratio of T-shaped bimaleimide resin is 13.2%
~15.5%, the ratio of titanium dioxide is 16.5%~22%, the ratio of phlogopite is 3.3%~5.5%, boron trifluoride-mono-
The ratio of ethamine is 0.34%~0.7%；The ratio of triethanolamine is 0.76%~1.3%.
A kind of preparation method of epoxy resin-base composite material, the method take following steps：
1) pretreatment of titanium dioxide
Titanium dioxide is placed in high-temperature resistant container, at least 2h is kept the temperature at 950 DEG C and is heat-treated, titanium dioxide is whole
Change into stable golden red type titanium dioxide；By golden red type titanium dioxide ball milling on ball mill through Overheating Treatment, make its grain
Degree reaches more than 200 mesh；
2) pretreatment of phlogopite
Phlogopite is soaked into 2~4h in 10% dilute hydrochloric acid solution, removes the impurity iron of phlogopite, fully washing immersion
Phlogopite afterwards, and it is dried, the ball milling on ball mill, makes its granularity reach more than 200 mesh, and the phlogopite of acquisition is bottled
It is spare；
3) preparation of epoxy resin-base composite material
By raw material according to 4,4- diaminodiphenylmethane, four glycidol ratio be 55%, T-shaped bismaleimide
The ratio of resin is 13.2%~15.5%, the ratio of titanium dioxide is 16.5%~22%, the ratio of phlogopite be 3.3%~
5.5%th, the ratio of boron triflouride-mono aminoethane is 0.34%~0.7%；The ratio of triethanolamine prepares for 0.76%~1.3%
After good, prepared according to following flow：
A) 4,4- diaminodiphenylmethane, four glycidyl amine is put into high-temperature resistant container, added in 70~80 DEG C of water-baths
It is in flow regime that heat, which arrives,；
B) add T-shaped span while being stirred to four glycidyl amine of liquid 4,4- diaminodiphenylmethane and carry out acyl
Imide resin, and be sufficiently stirred；
C) titanium dioxide, phlogopite are added in the mixture obtained to step b, and be sufficiently stirred；
D) boron triflouride-mono aminoethane, triethanolamine are added in the mixture obtained to step c, and be sufficiently stirred；
4) mixture finally obtained in step 3 is subjected to crosslinking curing
The mixture finally obtained in step 3 is put into drying box, the temperature in drying box is in room temperature between 60 DEG C
When, mixture freely heats up with drying box；At 60 DEG C~80 DEG C, the temperature of mixture raises temperature in drying box per hour
10℃；For temperature in drying box at 80 DEG C~100 DEG C, the temperature of mixture raises 20 DEG C per hour；Temperature in drying box
At 100 DEG C~150 DEG C, the temperature of mixture raises 50 DEG C per hour；Temperature in drying box is mixed at 150 DEG C~180 DEG C
The temperature of compound freely heats up with drying box；Temperature in drying box is at 180 DEG C, the temperature 2h of mixture, cures and hands over
After connection, mixture is taken out after being cooled down with drying box.
Embodiment
With a certain product (HTQ-17A) for embodiment, after Product processing forms the cavity such as attached drawing 1, by epoxy resin-matrix
Composite material is filled into cavity, is welded on after curing crosslinking with by cover board 5 on housing unit, cover board has with composite material surface
The cavity of about 7mm.The preparation of its epoxy resin-base composite material and construction method are as follows：
1. the pretreatment of titanium dioxide.
Titanium dioxide is kept the temperature 2h at 950 DEG C in corundum crucible to be heat-treated, heat treatment temperature system is as follows：Room
Temperature~600 DEG C, 200 DEG C/h；600 DEG C~800 DEG C, 150 DEG C/h；800 DEG C~950 DEG C, 80 DEG C/h；950+10DEG C, keep the temperature 2h.
Golden red type titanium dioxide ball milling 1h on planetary ball mill through Overheating Treatment, makes its granularity reach 200 mesh sieves
Nothing tails over.
2. the pretreatment of phlogopite
Phlogopite is soaked into 4h in 10% dilute hydrochloric acid solution, removes hydrochloric acid solution, it is dry after distillation water washing 3 times,
The ball milling 0.5h on planetary ball mill, crosses 200 mesh sieves without tailing over, it is spare to load wide-mouth bottle labeling.
The preparation of 3.TiO2/ epoxy resin-base composite materials (K-400)
1) component formula
1 TiO of table2/ epoxy resin-base composite material formula table
2) weigh
After raw material are ready to, every part of dispensing presses 4,4- diaminodiphenylmethane, four glycidyl amine 100g, T-shaped span
Bismaleimide resin 20g, titanium dioxide 30g, phlogopite 7.5g, boron triflouride-mono aminoethane 0.5g, triethanolamine 1.6 weigh.Tool
Antibody Production Techniques flow is as follows：
3) 4,4- diaminodiphenylmethane, four glycidyl amine is put into porcelain crucible, is heated in 80 DEG C of water-baths in stream
Dynamic state；
4) T-shaped bimaleimide resin is added while stirring is not stopped, be sufficiently stirred；
5) a certain amount of titanium dioxide of uniformly rear addition to be mixed, phlogopite continue to stir 30min；
6) boron triflouride-mono aminoethane, triethanolamine are added and is sufficiently stirred, in case construction is used.
In the above process, 4,4- diaminodiphenylmethane, four glycidyl amine has good ductility and toughness, anti-impact
Hit power, dielectric properties and very strong cohesive force, add T-shaped bimaleimide resin be in order to improve the bonding of epoxy resin,
Flexure, toughness, moisture resistance and surface smoothness, addition titanium dioxide, phlogopite are filled into the gap of epoxy resin, improve it
Intensity, reduces its thermal coefficient of expansion, adds boron triflouride-mono aminoethane, triethanolamine is accelerated to cure as accelerating agent, curing agent
Flow, saves the construction time, which is no more than a hour.
3. mixture construction flow.
The manufactured mixture with mobility is entered in the cavity for being injected into and needing to fill.
4. crosslinking curing.
The good product of embedding is put into drying box, by certain temperature schedule crosslinking, is cured, is made it have required strong
Degree, surface smoothness.After curing crosslinking, power supply is closed, less than 35 DEG C taking-ups are cooled to drying box.Specific crosslinking is solid
It is as follows to change temperature schedule：Room temperature~60 DEG C, freely heat up with drying box；60 DEG C~80 DEG C, 20 DEG C/2h；80 DEG C~100 DEG C, 20
℃/1h；100 DEG C~150 DEG C, 50 DEG C/1h；150 DEG C~180 DEG C, freely heat up with drying box；180+10DEG C, keep the temperature 2h.
5. performance detection
Test the TiO after crosslinking curing2The insulation resistance of/epoxy resin-base composite material, heat-resisting, heatproof, ageing properties,
And routine test examination is carried out with ionic flame detector, routine test includes antivibration kinetic force, thermal shock and life test etc.,
To examine its durability, reliability.On this basis, it is also necessary to carry out growing examination examination with supporting engine.
Epoxy resin embedding adhesive (existing Embedding Material), epoxy resin-base composite material (newly developing material) property are tested respectively
Can, it is shown in Table 2.
Table 2 newly develops TiO2/ epoxy resin-base composite material and existing Embedding Material performance comparison table
Claims (2)
1. a kind of epoxy resin-base composite material, it is characterised in that the constituent of the epoxy resin-base composite material includes
Four glycidol of 4,4- diaminodiphenylmethane, T-shaped bimaleimide resin, titanium dioxide, phlogopite, boron trifluoride-mono-
Ethamine, triethanolamine；The ratio of 4,4- diaminodiphenylmethane, four glycidol is 55%, T-shaped bimaleimide resin
Ratio is 13.2%~15.5%, the ratio of titanium dioxide is 16.5%~22%, the ratio of phlogopite is 3.3%~5.5%,
The ratio of boron triflouride-mono aminoethane is 0.34%~0.7%；The ratio of triethanolamine is 0.76%~1.3%.
2. a kind of preparation method of epoxy resin-base composite material, it is characterised in that the method takes following steps：
1) pretreatment of titanium dioxide
Titanium dioxide is placed in high-temperature resistant container, at least 2h is kept the temperature at 950 DEG C and is heat-treated, titanium dioxide is totally converted
Into stable golden red type titanium dioxide；By golden red type titanium dioxide ball milling on ball mill through Overheating Treatment, reach its granularity
To more than 200 mesh；
2) pretreatment of phlogopite
Phlogopite is soaked into 2~4h in 10% dilute hydrochloric acid solution, removes the impurity iron of phlogopite, fully after washing immersion
Phlogopite, and it is dried, the ball milling on ball mill, makes its granularity reach more than 200 mesh, and the phlogopite bottling of acquisition is standby
With；
3) preparation of epoxy resin-base composite material
By raw material according to 4,4- diaminodiphenylmethane, four glycidol ratio be 55%, T-shaped bimaleimide resin
Ratio be 13.2%~15.5%, the ratio of titanium dioxide is 16.5%~22%, the ratio of phlogopite be 3.3%~
5.5%th, the ratio of boron triflouride-mono aminoethane is 0.34%~0.7%；The ratio of triethanolamine prepares for 0.76%~1.3%
After good, prepared according to following flow：
A) 4,4- diaminodiphenylmethane, four glycidyl amine is put into high-temperature resistant container, is heated in 70~80 DEG C of water-baths
In flow regime；
B) T-shaped bismaleimide is added while being stirred to four glycidyl amine of liquid 4,4- diaminodiphenylmethane
Resin, and be sufficiently stirred；
C) titanium dioxide, phlogopite are added in the mixture obtained to step b, and be sufficiently stirred；
D) boron triflouride-mono aminoethane, triethanolamine are added in the mixture obtained to step c, and be sufficiently stirred；
4) mixture finally obtained in step 3 is subjected to crosslinking curing
The mixture finally obtained in step 3 is put into drying box, the temperature in drying box is mixed when room temperature is between 60 DEG C
Compound freely heats up with drying box；For temperature in drying box at 60 DEG C~80 DEG C, the temperature of mixture raises 10 DEG C per hour；
For temperature in drying box at 80 DEG C~100 DEG C, the temperature of mixture raises 20 DEG C per hour；Temperature in drying box is 100
DEG C~150 DEG C when, the temperature of mixture raises 50 DEG C per hour；Temperature in drying box is at 150 DEG C~180 DEG C, mixture
Temperature freely heat up with drying box；Temperature in drying box is at 180 DEG C, the temperature 2h of mixture, cures crosslinking knot
Shu Hou, takes out mixture after being cooled down with drying box.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112898931A (en) * | 2021-03-22 | 2021-06-04 | 深圳市汇北川电子技术有限公司 | High-temperature epoxy resin potting material for preventing cold and hot alternating cracking after curing and use method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112898931A (en) * | 2021-03-22 | 2021-06-04 | 深圳市汇北川电子技术有限公司 | High-temperature epoxy resin potting material for preventing cold and hot alternating cracking after curing and use method thereof |
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