CN109233717A - A kind of preparation method of thermostable heat-conductive glue - Google Patents
A kind of preparation method of thermostable heat-conductive glue Download PDFInfo
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- CN109233717A CN109233717A CN201811104348.XA CN201811104348A CN109233717A CN 109233717 A CN109233717 A CN 109233717A CN 201811104348 A CN201811104348 A CN 201811104348A CN 109233717 A CN109233717 A CN 109233717A
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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
- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
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Abstract
The present invention relates to a kind of preparation methods of thermostable heat-conductive glue, belong to field of adhesive technology.Silver carp bone pyrohydrolysis is isolated collagen by the present invention, birch powder high temperature and high pressure hydrolysis is isolated to the lignin in wood powder, cellulose while furfural again can polymerize each organic molecule, the space structure density for improving heat-conducting glue, further strengthens the bond effect and mechanical performance of heat-conducting glue；Aluminium ion is introduced into lignin and plant fiber, is adsorbed on organic fiber using ionic bond by the present invention, and in plant fiber pipe, after peptide chain disconnection, peptide chain first and last is disconnected to form carboxyl and amino, aluminium ion can exchange to be bonded on peptide bond with hydrogen ion therein, aluminum ions introducing makes heat-conducting glue keep stability at high operating temperatures, when being decomposed by heat-flash, aluminium ion preferentially generates aluminium oxide with oxygen association reaction, these molecules are avoided to be oxidized decomposition, therefore there is good high temperature resistance, have a good application prospect.
Description
Technical field
The present invention relates to a kind of preparation methods of thermostable heat-conductive glue, belong to field of adhesive technology.
Background technique
Heat-conducting glue is one-component, heat-conducting type, room temperature curing organosilicon joint sealant.Moisture content through the air contracts
It closes reaction releasing low molecule and causes crosslinking curing, and be sulfided into high performance elastomer.Heat-conducting glue, also known as heat conductive silica gel.It is to have
Based on machine silica gel, the high molecular materials such as addition filler material, Heat Conduction Material, silica gel made of mixing has preferable thermally conductive, electric
Insulation performance is widely used in electronic component.Also known as: heat conductive silica gel, heat-conducting silicon rubber, thermally conductive silica gel, thermally conductive silicone.For
Transformer, transistor and other heater elements are adhered on printed circuit board assembly or radiator.Superhigh temperature can be divided into lead
Hot glue, organosilicon heat-conducting glue, epoxy resin AB glue, polyurethane adhesive, polyurethane guide thermal conducting glue, heat-conducting silicone grease.
Epoxy resin have excellent dielectric properties, mechanical property, adhesive property and corrosion resistance, cure shrinkage and
Thermal expansion coefficient is small, and production technology is mature, and cheap, this makes epoxy resin purposes very extensive.But epoxy resin
Heating conduction is poor, it is difficult to meet the needs of electronics industry.In addition, the electricity for electronic product, especially under high-voltage electricity application
Device equipment, is easy to happen fire incident, and the inflammability of organic material limits epoxy resin heat-conducting glue in high-power electrical equipment
On application.
With the development of science and technology, demand of the people to electronic product and require higher and higher, electronic product is towards collection
Become second nature, minimize, high-performance, energy-saving and environmental protection, safety direction develop.Highly integrated, the unit volume generation of electronic product
Heat be continuously increased.With to environmental protection pay attention to day by day and electronic component to the direction of densification, micromation send out
Exhibition, the requirement to electronic package material performance are also higher and higher.Heat conduction adhesive currently used in the market, it is most of for foreign countries
Imported material, cost is very high, and few high temperature resistant, caking property of can reaching simultaneously is good while having excellent heating conduction.
Therefore, inventing the heat-conducting glue that a kind of heat-resisting quantity is good and caking property is good has actively meaning to field of adhesive technology
Justice.
Summary of the invention
The technical problems to be solved by the invention: for the defect that current heat-conducting glue caking property is bad, heat-resisting ability is poor,
Provide a kind of preparation method of thermostable heat-conductive glue.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of thermostable heat-conductive glue, it is characterised in that specific preparation step are as follows:
(1) it weighs 500~800g silver carp bone to be placed in high-temperature high-pressure reaction kettle, with distillation water retting silver carp bone, increases temperature in furnace
Degree and air pressure, constant temperature and pressure are stood, and suction filtration obtains filtrate, and filtrate is poured into Rotary Evaporators, and concentration and evaporation is until product is permanent
Reaction glue is made in weight；
(2) birch powder is uniformly mixed with water 1:5 in mass ratio and mixed serum is made, mixed serum is placed in reaction kettle, risen
High temperature in the kettle and air pressure, constant temperature and pressure, which reacts, is made reaction solution, score meter by weight, weigh 15~18 parts of reaction solutions, 12~
14 parts of above-mentioned reaction glues, 3~5 parts of aluminium chloride crystal powders, 7~9 parts of deionized waters, 1~2 part of glycerol and 4~6 parts of propanedione
It puts into be mixed in high speed dispersion instrument and mixed liquor is made；
(3) it will be uniformly mixed in above-mentioned mixed liquor and proteolytic enzyme 30:1 in mass ratio investment beaker, place the beaker constant temperature
Constant temperature and humidity reacts in constant humidity cabinet, and enzymolysis liquid is made, and sodium carbonate liquor is added dropwise into beaker and adjusts pH value to 8~9, while with stirring
It mixes device and obtained akaline liquid is mixed；
(4) by above-mentioned akaline liquid and bisphenol A type epoxy resin 1:10 in mass ratio investment reaction kettle, temperature in the kettle is increased,
It is mixed with blender and mixed glue solution is made, the phosphoric acid of mixed glue solution quality 2~4% is added under constant temperature into reaction kettle
Triphenylmethyl methacrylate continuess to mix stirring and prefabricated glue is made；
(5) according to parts by weight, 50~55 parts of above-mentioned prefabricated glues, 5~7 parts of benzyl dimethylamines and 8~10 parts of γ-ammonia are weighed
It being mixed in propyl-triethoxysilicane investment reaction kettle, temperature in the kettle is increased after stirring, constant temperature is stood, it discharges after standing,
Thermostable heat-conductive glue is made in cooled to room temperature.
In-furnace temperature is increased to 230~240 DEG C in high-temperature high-pressure reaction kettle as described in step (1), and air pressure increases in furnace
To 2.0~2.8MPa, constant temperature and pressure time of repose is 40~50min, and the revolving speed of Rotary Evaporators is 300~330r/min, temperature
Degree is 65~75 DEG C.
Reactor temperature described in step (2) is increased to 220~240 DEG C, and air pressure is increased to 2.0~2.5MPa, permanent
The warm constant pressure reaction time is 60~80min, and the revolving speed in high speed dispersion instrument is 1100~1200r/min, and mixing time is
30~40min.
Temperature in climatic chamber described in step (3) is 35~38 DEG C, and relative air humidity is 70~90%, permanent
The constant temperature and humidity reaction time is 60~80min, and the mass fraction of sodium carbonate liquor is 8~12%, the revolving speed of blender is 300~
320r/min, mixing time are 100~120min.
Reactor temperature described in step (4) is increased to 75~80 DEG C, and the revolving speed of blender is 500~550r/
Min, mixing time are 30~40min.
Temperature in reaction kettle described in step (5) is 85~95 DEG C, and speed of agitator is 200~250r/min, mixing
Mixing time is 50~60min, and temperature in the kettle is increased to 130~150 DEG C, and constant temperature time of repose is 5~7h.
The method have the benefit that:
(1) present invention first reacts silver carp bone under conditions of high temperature and pressure with water, and reaction glue is made in concentration and evaporation after reaction
Liquid, then birch powder is blended under high-temperature and high-pressure conditions to react with water, reaction solution is made, then by reaction solution, aluminium chloride, glycerol
Equal organic solvents, which are mixed, is made mixed liquor, and proteolytic enzyme is added into mixed liquor and is digested, pH value is adjusted after enzymatic hydrolysis
To the obtained akaline liquid of alkalinity, then akaline liquid is successively mixed with resin solution, triphenyl phosphate, pre-prepared colloid is made
Prefabricated glue is finally mixed with silane coupling agent, benzyl dimethylamine heating, thermostable heat-conductive glue, this hair is made after cooling by liquid
It is bright that silver carp bone pyrohydrolysis is isolated into collagen, then birch powder high temperature and high pressure hydrolysis isolated lignin in wood powder,
The organic fibers such as cellulose, plant fiber, under high-temperature and high-pressure conditions, lignin, plant fiber etc. are decomposed to form carboxylic acid, furfural
Equal substances, while aluminium ion is added in conjunction with collagen and lignin, plant fiber, then pass through proteolytic enzyme enzyme
Solution, makes the Fragmentation in collagen, increases each group in peptide chain to the contact area of extraneous molecule, to reinforce heat-conducting glue
Caking property, while furfural can polymerize each organic molecule, improve the space structure density of heat-conducting glue, further strengthen heat-conducting glue
Bond effect and mechanical performance；
(2) aluminium ion is introduced into lignin and plant fiber, is adsorbed on organic fiber using ionic bond, Yi Jizhi by the present invention
In fibres pipe, after peptide chain disconnection, peptide chain first and last is disconnected to form carboxyl and amino, and aluminium ion can be exchanged with hydrogen ion therein
To be bonded on peptide bond, aluminum ions introducing makes heat-conducting glue keep stability at high operating temperatures, when being decomposed by heat-flash,
Aluminium ion preferentially generates aluminium oxide with oxygen association reaction, coats each molecule in heat-conducting glue, these molecules is avoided to be oxidized decomposition,
Therefore there is good high temperature resistance, have a good application prospect.
Specific embodiment
It weighs 500~800g silver carp bone to be placed in high-temperature high-pressure reaction kettle, with distillation water retting silver carp bone, increases temperature in furnace
Degree is to 230~240 DEG C, and increasing air pressure in furnace, to 2.0~2.8MPa, constant temperature and pressure stands 40~50min, and suction filtration obtains filtrate,
Filtrate is poured into Rotary Evaporators, concentration and evaporation is straight under conditions of revolving speed is 300~330r/min, temperature is 65~75 DEG C
To product constant weight, reaction glue is made；Birch powder is uniformly mixed with water 1:5 in mass ratio, mixed serum is made, by mixing slurry
Liquid is placed in reaction kettle, increases in-furnace temperature to 220~240 DEG C, air pressure is increased to 2.0~2.5MPa, constant temperature and pressure reaction 60
~80min is made reaction solution, by weight score meter, weighs 15~18 parts of reaction solutions, 12~14 parts of above-mentioned reaction glues, 3~5
In part aluminium chloride crystal powder, 7~9 parts of deionized waters, 1~2 part of glycerol and 4~6 parts of propanedione investment high speed dispersion instrument with
The revolving speed of 1100~1200r/min is mixed 30~40min and mixed liquor is made；Above-mentioned mixed liquor and proteolytic enzyme are pressed into matter
Amount places the beaker in climatic chamber than being uniformly mixed in 30:1 investment beaker, is 35~38 DEG C in temperature, air is relatively wet
Degree reacts 60~80min for constant temperature and humidity under conditions of 70~90%, and enzymolysis liquid is made, be added dropwise into beaker mass fraction be 8~
12% sodium carbonate liquor adjusts pH value to 8~9, at the same with blender with the revolving speed mixing 100 of 300~320r/min~
Akaline liquid is made in 120min；By in above-mentioned akaline liquid and bisphenol A type epoxy resin 1:10 in mass ratio investment reaction kettle, rise
30~40min is mixed to 75~80 DEG C, with blender with the revolving speed of 500~550r/min in high temperature in the kettle, and mixing is made
The triphenyl phosphate of mixed glue solution quality 2~4% is added under constant temperature into reaction kettle for glue, continues with 500~550r/
The revolving speed of min is mixed 20~30min and prefabricated glue is made；According to parts by weight, weigh 50~55 parts of above-mentioned prefabricated glues,
In the reaction kettle that 5~7 parts of benzyl dimethylamines and 8~10 parts of γ-aminopropyl triethoxysilane investment temperature are 85~95 DEG C,
50~60min is mixed with the revolving speed of 200~250r/min, temperature in the kettle is increased after stirring to 130~150 DEG C, constant temperature is quiet
5~7h is set, is discharged after standing, thermostable heat-conductive glue is made in cooled to room temperature.
It weighs 500g silver carp bone to be placed in high-temperature high-pressure reaction kettle, with distillation water retting silver carp bone, increases in-furnace temperature extremely
230 DEG C, increasing air pressure in furnace, to 2.0MPa, constant temperature and pressure stands 40min, and suction filtration obtains filtrate, filtrate is poured into rotary evaporation
In instrument, reaction glue is made until product constant weight in concentration and evaporation under conditions of revolving speed is 300r/min, temperature is 65 DEG C；It will
Birch powder is uniformly mixed with water 1:5 in mass ratio is made mixed serum, and mixed serum is placed in reaction kettle, in-furnace temperature is increased
To 220 DEG C, air pressure is increased to 2.0MPa, and constant temperature and pressure reacts 60min, and reaction solution, by weight score meter is made, and weighs 15 parts instead
Answer liquid, 12 parts of above-mentioned reaction glues, 3 parts of aluminium chloride crystal powders, 7 parts of deionized waters, 1 part of glycerol and 4 parts of propanedione investments high
30min is mixed with the revolving speed of 1100r/min in fast separating apparatus, mixed liquor is made；Above-mentioned mixed liquor is pressed with proteolytic enzyme
Mass ratio 30:1 puts into beaker and is uniformly mixed, and places the beaker in climatic chamber, is 35 DEG C in temperature, relative air humidity
Constant temperature and humidity reacts 60min under conditions of being 70%, and enzymolysis liquid is made, and it is molten that the sodium carbonate that mass fraction is 8% is added dropwise into beaker
Liquid adjusts pH value to 8, while the obtained akaline liquid of 100min is mixed with the revolving speed of 300r/min with blender；By above-mentioned alkali
Property liquid and bisphenol A type epoxy resin 1:10 in mass ratio investment reaction kettle in, increase temperature in the kettle to 75 DEG C, with blender with
30min is mixed in the revolving speed of 500r/min, and mixed glue solution is made, mixed glue solution quality is added into reaction kettle under constant temperature
2% triphenyl phosphate continues that prefabricated glue is made with the revolving speed mixing 20min of 500r/min；According to parts by weight, claim
Taking 50 parts of above-mentioned prefabricated glues, 5 parts of benzyl dimethylamines and 8 parts of γ-aminopropyl triethoxysilane investment temperature is 85 DEG C anti-
It answers in kettle, 50min is mixed with the revolving speed of 200r/min, temperature in the kettle is increased after stirring to 130 DEG C, constant temperature stands 5h, quiet
Discharging is postponed, thermostable heat-conductive glue is made in cooled to room temperature.
It weighs 700g silver carp bone to be placed in high-temperature high-pressure reaction kettle, with distillation water retting silver carp bone, increases in-furnace temperature extremely
235 DEG C, increasing air pressure in furnace, to 2.4MPa, constant temperature and pressure stands 45min, and suction filtration obtains filtrate, filtrate is poured into rotary evaporation
In instrument, reaction glue is made until product constant weight in concentration and evaporation under conditions of revolving speed is 315r/min, temperature is 70 DEG C；It will
Birch powder is uniformly mixed with water 1:5 in mass ratio is made mixed serum, and mixed serum is placed in reaction kettle, in-furnace temperature is increased
To 230 DEG C, air pressure is increased to 2.2MPa, and constant temperature and pressure reacts 70min, and reaction solution, by weight score meter is made, and weighs 17 parts instead
Answer liquid, 13 parts of above-mentioned reaction glues, 4 parts of aluminium chloride crystal powders, 8 parts of deionized waters, 1 part of glycerol and 5 parts of propanedione investments high
35min is mixed with the revolving speed of 1150r/min in fast separating apparatus, mixed liquor is made；Above-mentioned mixed liquor is pressed with proteolytic enzyme
Mass ratio 30:1 puts into beaker and is uniformly mixed, and places the beaker in climatic chamber, is 37 DEG C in temperature, relative air humidity
Constant temperature and humidity reacts 70min under conditions of being 80%, and enzymolysis liquid is made, and it is molten that the sodium carbonate that mass fraction is 10% is added dropwise into beaker
Liquid adjusts pH value to 8, while the obtained akaline liquid of 110min is mixed with the revolving speed of 310r/min with blender；By above-mentioned alkali
Property liquid and bisphenol A type epoxy resin 1:10 in mass ratio investment reaction kettle in, increase temperature in the kettle to 77 DEG C, with blender with
35min is mixed in the revolving speed of 525r/min, and mixed glue solution is made, mixed glue solution quality is added into reaction kettle under constant temperature
3% triphenyl phosphate continues that prefabricated glue is made with the revolving speed mixing 25min of 520r/min；According to parts by weight, claim
Take 52 parts of above-mentioned prefabricated glues, 6 parts of benzyl dimethylamines and 9 parts of γ-aminopropyl triethoxysilane investment at a temperature of 90 °C anti-
It answers in kettle, 55min is mixed with the revolving speed of 220r/min, temperature in the kettle is increased after stirring to 140 DEG C, constant temperature stands 6h, quiet
Discharging is postponed, thermostable heat-conductive glue is made in cooled to room temperature.
It weighs 800g silver carp bone to be placed in high-temperature high-pressure reaction kettle, with distillation water retting silver carp bone, increases in-furnace temperature extremely
240 DEG C, increasing air pressure in furnace, to 2.8MPa, constant temperature and pressure stands 50min, and suction filtration obtains filtrate, filtrate is poured into rotary evaporation
In instrument, reaction glue is made until product constant weight in concentration and evaporation under conditions of revolving speed is 330r/min, temperature is 75 DEG C；It will
Birch powder is uniformly mixed with water 1:5 in mass ratio is made mixed serum, and mixed serum is placed in reaction kettle, in-furnace temperature is increased
To 240 DEG C, air pressure is increased to 2.5MPa, and constant temperature and pressure reacts 80min, and reaction solution, by weight score meter is made, and weighs 18 parts instead
Answer liquid, 14 parts of above-mentioned reaction glues, 5 parts of aluminium chloride crystal powders, 9 parts of deionized waters, 2 parts of glycerol and 6 parts of propanedione investments high
40min is mixed with the revolving speed of 1200r/min in fast separating apparatus, mixed liquor is made；Above-mentioned mixed liquor is pressed with proteolytic enzyme
Mass ratio 30:1 puts into beaker and is uniformly mixed, and places the beaker in climatic chamber, is 38 DEG C in temperature, relative air humidity
Constant temperature and humidity reacts 80min under conditions of being 90%, and enzymolysis liquid is made, and it is molten that the sodium carbonate that mass fraction is 12% is added dropwise into beaker
Liquid adjusts pH value to 9, while the obtained akaline liquid of 120min is mixed with the revolving speed of 320r/min with blender；By above-mentioned alkali
Property liquid and bisphenol A type epoxy resin 1:10 in mass ratio investment reaction kettle in, increase temperature in the kettle to 80 DEG C, with blender with
40min is mixed in the revolving speed of 550r/min, and mixed glue solution is made, mixed glue solution quality is added into reaction kettle under constant temperature
4% triphenyl phosphate continues that prefabricated glue is made with the revolving speed mixing 30min of 550r/min；According to parts by weight, claim
Taking 55 parts of above-mentioned prefabricated glues, 7 parts of benzyl dimethylamines and 10 parts of γ-aminopropyl triethoxysilane investment temperature is 95 DEG C
In reaction kettle, 60min is mixed with the revolving speed of 250r/min, temperature in the kettle is increased after stirring to 150 DEG C, constant temperature stands 7h,
It discharges after standing, thermostable heat-conductive glue is made in cooled to room temperature.
The thermostable heat-conductive glue that comparative example is produced with Shenzhen company as a comparison case leads high temperature resistant produced by the present invention
Thermostable heat-conductive glue in hot glue and comparative example carries out performance detection, and testing result is as shown in table 1:
Test method:
According to 2007 standard of GB/T15022.2-, the thermal conductivity of material is measured.
Adhesion strength test is detected using adhesive strength tester.
Glass transition temperature test is detected using glass transition temperature tester.
Heat-resisting quantity test: the heat-conducting glue in example 1~3 and comparative example is toasted to a period of time in 260 DEG C of baking oven
After measure adhesion strength.
1 heat-conducting glue performance measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example |
| Thermal conductivity coefficient (W/mk) | 2.30 | 2.32 | 2.35 | 1.82 |
| Adhesion strength (MPa) | 26.2 | 26.4 | 26.5 | 15.6 |
| Glass transition temperature (DEG C) | 162 | 163 | 165 | 120 |
| Adhesion strength (MPa) after 260 DEG C of bakings | 24.0 | 24.0 | 24.2 | 10.3 |
High according to above-mentioned detection data thermostable heat-conductive glue thermal conductivity produced by the present invention, thermal conductivity is good, and adhesion strength is high,
Caking property is good, and glass transition temperature is high, and adhesion strength is high after toasting at a high temperature of 260 DEG C, and heat-resisting quantity is good, has wide
Application prospect.
Claims (6)
1. a kind of preparation method of thermostable heat-conductive glue, it is characterised in that specific preparation step are as follows:
(1) it weighs 500~800g silver carp bone to be placed in high-temperature high-pressure reaction kettle, with distillation water retting silver carp bone, increases temperature in furnace
Degree and air pressure, constant temperature and pressure are stood, and suction filtration obtains filtrate, and filtrate is poured into Rotary Evaporators, and concentration and evaporation is until product is permanent
Reaction glue is made in weight；
(2) birch powder is uniformly mixed with water 1:5 in mass ratio and mixed serum is made, mixed serum is placed in reaction kettle, risen
High temperature in the kettle and air pressure, constant temperature and pressure, which reacts, is made reaction solution, score meter by weight, weigh 15~18 parts of reaction solutions, 12~
14 parts of above-mentioned reaction glues, 3~5 parts of aluminium chloride crystal powders, 7~9 parts of deionized waters, 1~2 part of glycerol and 4~6 parts of propanedione
It puts into be mixed in high speed dispersion instrument and mixed liquor is made；
(3) it will be uniformly mixed in above-mentioned mixed liquor and proteolytic enzyme 30:1 in mass ratio investment beaker, place the beaker constant temperature
Constant temperature and humidity reacts in constant humidity cabinet, and enzymolysis liquid is made, and sodium carbonate liquor is added dropwise into beaker and adjusts pH value to 8~9, while with stirring
It mixes device and obtained akaline liquid is mixed；
(4) by above-mentioned akaline liquid and bisphenol A type epoxy resin 1:10 in mass ratio investment reaction kettle, temperature in the kettle is increased,
It is mixed with blender and mixed glue solution is made, the phosphoric acid of mixed glue solution quality 2~4% is added under constant temperature into reaction kettle
Triphenylmethyl methacrylate continuess to mix stirring and prefabricated glue is made；
(5) according to parts by weight, 50~55 parts of above-mentioned prefabricated glues, 5~7 parts of benzyl dimethylamines and 8~10 parts of γ-ammonia are weighed
It being mixed in propyl-triethoxysilicane investment reaction kettle, temperature in the kettle is increased after stirring, constant temperature is stood, it discharges after standing,
Thermostable heat-conductive glue is made in cooled to room temperature.
2. a kind of preparation method of thermostable heat-conductive glue according to claim 1, it is characterised in that: described in step (1)
High-temperature high-pressure reaction kettle in in-furnace temperature be increased to 230~240 DEG C, air pressure is increased to 2.0~2.8MPa, constant temperature and pressure in furnace
Time of repose is 40~50min, and the revolving speed of Rotary Evaporators is 300~330r/min, temperature is 65~75 DEG C.
3. a kind of preparation method of thermostable heat-conductive glue according to claim 1, it is characterised in that: described in step (2)
Reactor temperature be increased to 220~240 DEG C, air pressure is increased to 2.0~2.5MPa, the constant temperature and pressure reaction time is 60~
80min, the revolving speed in high speed dispersion instrument are 1100~1200r/min, and mixing time is 30~40min.
4. a kind of preparation method of thermostable heat-conductive glue according to claim 1, it is characterised in that: described in step (3)
Climatic chamber in temperature be 35~38 DEG C, relative air humidity be 70~90%, the constant temperature and humidity reaction time be 60~
80min, the mass fraction of sodium carbonate liquor are 8~12%, and the revolving speed of blender is 300~320r/min, and mixing time is
100~120min.
5. a kind of preparation method of thermostable heat-conductive glue according to claim 1, it is characterised in that: described in step (4)
Reactor temperature be increased to 75~80 DEG C, the revolving speed of blender is 500~550r/min, mixing time is 30~
40min。
6. a kind of preparation method of thermostable heat-conductive glue according to claim 1, it is characterised in that: described in step (5)
Reaction kettle in temperature be 85~95 DEG C, speed of agitator be 200~250r/min, mixing time be 50~60min, kettle
Interior temperature is increased to 130~150 DEG C, and constant temperature time of repose is 5~7h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811104348.XA CN109233717A (en) | 2018-09-21 | 2018-09-21 | A kind of preparation method of thermostable heat-conductive glue |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811104348.XA CN109233717A (en) | 2018-09-21 | 2018-09-21 | A kind of preparation method of thermostable heat-conductive glue |
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| CN109233717A true CN109233717A (en) | 2019-01-18 |
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| CN201811104348.XA Pending CN109233717A (en) | 2018-09-21 | 2018-09-21 | A kind of preparation method of thermostable heat-conductive glue |
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| CN110183999A (en) * | 2019-05-30 | 2019-08-30 | 刘丹 | A kind of preparation method of ageing-resistant glue spraying |
| CN112795140A (en) * | 2021-01-04 | 2021-05-14 | 中变集团上海变压器有限公司 | Epoxy resin coil for transformer and processing technology thereof |
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| CN112795140A (en) * | 2021-01-04 | 2021-05-14 | 中变集团上海变压器有限公司 | Epoxy resin coil for transformer and processing technology thereof |
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