CN110157154A - A kind of electrical composition epoxy resin of low viscosity, fire resistant and preparation method thereof - Google Patents
A kind of electrical composition epoxy resin of low viscosity, fire resistant and preparation method thereof Download PDFInfo
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- CN110157154A CN110157154A CN201810222724.9A CN201810222724A CN110157154A CN 110157154 A CN110157154 A CN 110157154A CN 201810222724 A CN201810222724 A CN 201810222724A CN 110157154 A CN110157154 A CN 110157154A
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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
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of electrical composition epoxy resins of low viscosity, fire resistant, are made of the raw material below according to parts by weight: 100-105 parts of epoxy resin, 41-45 parts of curing agent, 34-38 parts of silicone resin, 12-16 parts of sillimanite, 1-2 parts of dibutyl phthalate, 18-22 parts of epoxy propane butyl ether, 0.5-0.9 parts of eucalyptol.The invention also discloses the preparation methods of the electrical composition epoxy resin of the low viscosity, fire resistant.Epoxy resin viscosity prepared by the present invention is low, is conducive to process, and has excellent high temperature resistance, is conducive to improve the service life of product under the high temperature conditions, is conducive to the application range for expanding the electric field of product, has a vast market foreground.
Description
Technical field
The present invention relates to electrical technical field of polymer materials, the electrical epoxy resin of specifically a kind of low viscosity, fire resistant
Composition and preparation method thereof.
Background technique
Epoxy resin refers to the general name of the quasi polymer containing more than two epoxy groups in molecule.It is epoxy chloropropionate
The polycondensation product of alkane and bisphenol-A or polyalcohol can be made due to the chemical activity of epoxy group with a variety of compounds containing active hydrogen
Its open loop, solidification crosslinking generates reticular structure, therefore it is a kind of thermosetting resin.Epoxy resin has good comprehensive mechanics
Performance, the electrical insulation capability that shrinking percentage is low, stability is good, excellent, as coating, adhesive, the matrix resin of composite material, electricity
Sub- encapsulating material etc. is widely used in fields such as aerospace, machinery, electronics, electric appliance, automobiles.
With the development of the times, in electric field, market proposes higher performance requirement, existing ring to epoxy resin
Performance of the oxygen resin in terms of high temperature resistance is gradually unable to satisfy the market demand, it would be highly desirable to improve.
Summary of the invention
The purpose of the present invention is to provide electrical composition epoxy resin of a kind of low viscosity, fire resistant and preparation method thereof,
To solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of electrical composition epoxy resin of low viscosity, fire resistant, is made: epoxy of the raw material below according to parts by weight
100-105 parts of resin, 41-45 parts of curing agent, 34-38 parts of silicone resin, 12-16 parts of sillimanite, dibutyl phthalate 1-2
Part, 18-22 parts of epoxy propane butyl ether, 0.5-0.9 parts of eucalyptol.
As a further solution of the present invention: it is made of the raw material below according to parts by weight: 101-104 parts of epoxy resin,
42-44 parts of curing agent, 35-37 parts of silicone resin, 13-15 parts of sillimanite, 1.3-1.7 parts of dibutyl phthalate, propylene oxide
19-21 parts of butyl ether, 0.6-0.8 parts of eucalyptol.
As further scheme of the invention: be made of the raw material below according to parts by weight: 102 parts of epoxy resin is consolidated
43 parts of agent, 36 parts of silicone resin, 14 parts of sillimanite, 1.5 parts of dibutyl phthalate, 20 parts of epoxy propane butyl ether, eucalyptus oil
0.7 part of essence.
As further scheme of the invention: the epoxy resin is by bisphenol A type epoxy resin and bisphenol S type epoxy tree
Rouge composition.
As further scheme of the invention: the epoxy resin is by bisphenol A type epoxy resin and bisphenol S type epoxy tree
Rouge is formed according to weight ratio 3:1.
As further scheme of the invention: the curing agent is hexahydrophthalic anhydride.
The preparation method of the electrical composition epoxy resin of the low viscosity, fire resistant, steps are as follows:
1) sillimanite is weighed, is put into ball mill, the water of 6-8 times of weight is added, ball milling mixing 2-3h discharges, and obtains
Sillimanite dispersion liquid；
2) dilute hydrochloric acid solution of concentration 15% is added into sillimanite dispersion liquid, is stirred 1- at 500-700rpm
2h is then fed into processor for ultrasonic wave, is ultrasonically treated 40-50min, and discharging obtains the first treatment fluid；
3) sodium hydroxide solution is added dropwise into the first treatment fluid under the stirring of 200-400rpm, adjusts pH to 7, stands 2-
3h obtains second processing liquid；
4) second processing liquid is filtered, and the solid matter that filtering obtains is dried at 50-60 DEG C to get modified sunset line
Mountain flour；
5) epoxy resin and silicone resin are weighed, is added into reaction kettle, is evacuated to 0.05Mpa, is warming up to 80-100 DEG C,
20-30min is kept the temperature, modified sillimanite powder and epoxy propane butyl ether is added, is stirred 50-60min, is cooled to 50-60 DEG C,
Dibutyl phthalate and eucalyptol is added, continues to be stirred 30-40min, obtains mixture A；
6) curing agent is weighed, is added into mixture A, 30-40min is stirred at 50-60 DEG C, obtains mixture B；
7) mixture B is poured into mold, keeps the temperature 2-3h at 65-70 DEG C, then heat to 125-130 DEG C, heat preservation
1-2h stops heating, after natural cooling, demoulding.
As further scheme of the invention: in step 2), the additional amount of the dilute hydrochloric acid solution is sillimanite dispersion
The 20-30% of liquid total volume.
As further scheme of the invention: in step 2), the ultrasonic treatment frequency is 40-60kHz.
The electrical composition epoxy resin of the low viscosity, fire resistant is preparing the purposes in epoxy resin product.
Compared with prior art, the beneficial effects of the present invention are:
Epoxy resin viscosity prepared by the present invention is low, is conducive to process, and has excellent high temperature resistance, has
Conducive to the service life of product under the high temperature conditions is improved, be conducive to the application range for expanding the electric field of product, have wide
Wealthy market prospects.
Specific embodiment
Technical solution of the present invention is described in more detail With reference to embodiment.
Embodiment 1
A kind of electrical composition epoxy resin of low viscosity, fire resistant, is made: epoxy of the raw material below according to parts by weight
100 parts of resin, 41 parts of curing agent, 34 parts of silicone resin, 12 parts of sillimanite, 1 part of dibutyl phthalate, epoxy propane butyl ether
18 parts, 0.5 part of eucalyptol.
Wherein, the epoxy resin is made of bisphenol A type epoxy resin and bisphenol-s epoxy resin according to weight ratio 3:1；
The curing agent is hexahydrophthalic anhydride.
The preparation method of the electrical composition epoxy resin of the low viscosity, fire resistant, steps are as follows:
1) sillimanite is weighed, is put into ball mill, the water of 6 times of weight, ball milling mixing 2h is added, discharging obtains sunset line
Stone dispersion liquid；
2) dilute hydrochloric acid solution of concentration 15% is added into sillimanite dispersion liquid, is stirred 1h at 500 rpm, then
It is sent into processor for ultrasonic wave, is ultrasonically treated 40min, discharging obtains the first treatment fluid, wherein the dilute hydrochloric acid solution adds
Enter 20% that amount is sillimanite dispersion liquid total volume, the ultrasonic treatment frequency is 40kHz；
3) sodium hydroxide solution is added dropwise into the first treatment fluid under the stirring of 200rpm, adjusts pH to 7, stands 2h, obtains
Obtain second processing liquid；
4) second processing liquid is filtered, and the solid matter that filtering obtains is dried at 50 DEG C to get modified sillimanite
Powder；
5) epoxy resin and silicone resin are weighed, is added into reaction kettle, is evacuated to 0.05Mpa, is warming up to 80 DEG C, heat preservation
20min is added modified sillimanite powder and epoxy propane butyl ether, is stirred 50min, be cooled to 50 DEG C, O-phthalic is added
Dibutyl phthalate and eucalyptol continue to be stirred 30min, obtain mixture A；
6) curing agent is weighed, is added into mixture A, 30min is stirred at 50 DEG C, obtains mixture B；
7) mixture B is poured into mold, keeps the temperature 2h at 65 DEG C, then heat to 125 DEG C, keep the temperature 1h, stop adding
Heat, after natural cooling, demoulding.
Embodiment 2
A kind of electrical composition epoxy resin of low viscosity, fire resistant, is made: epoxy of the raw material below according to parts by weight
100 parts of resin, 41 parts of curing agent, 38 parts of silicone resin, 16 parts of sillimanite, 1 part of dibutyl phthalate, epoxy propane butyl ether
22 parts, 0.5 part of eucalyptol.
Wherein, the epoxy resin is made of bisphenol A type epoxy resin and bisphenol-s epoxy resin according to weight ratio 3:1；
The curing agent is hexahydrophthalic anhydride.
The preparation method of the electrical composition epoxy resin of the low viscosity, fire resistant, steps are as follows:
1) sillimanite is weighed, is put into ball mill, the water of 6.5 times of weight, ball milling mixing 2h is added, discharging obtains sunset
Line stone dispersion liquid；
2) dilute hydrochloric acid solution of concentration 15% is added into sillimanite dispersion liquid, is stirred 1.5h at 500 rpm, so
It is sent into processor for ultrasonic wave afterwards, is ultrasonically treated 42min, discharging obtains the first treatment fluid, wherein the dilute hydrochloric acid solution
Additional amount is the 20% of sillimanite dispersion liquid total volume, and the ultrasonic treatment frequency is 50kHz；
3) sodium hydroxide solution is added dropwise into the first treatment fluid under the stirring of 200rpm, adjusts pH to 7, stands 2.5h,
Obtain second processing liquid；
4) second processing liquid is filtered, and the solid matter that filtering obtains is dried at 55 DEG C to get modified sillimanite
Powder；
5) epoxy resin and silicone resin are weighed, is added into reaction kettle, is evacuated to 0.05Mpa, is warming up to 80 DEG C, heat preservation
23min is added modified sillimanite powder and epoxy propane butyl ether, is stirred 55min, be cooled to 50 DEG C, O-phthalic is added
Dibutyl phthalate and eucalyptol continue to be stirred 30min, obtain mixture A；
6) curing agent is weighed, is added into mixture A, 32min is stirred at 50 DEG C, obtains mixture B；
7) mixture B is poured into mold, keeps the temperature 2h at 65 DEG C, then heat to 125 DEG C, keep the temperature 1.5h, stopped
It heats, after natural cooling, demoulding.
Embodiment 3
A kind of electrical composition epoxy resin of low viscosity, fire resistant, is made: epoxy of the raw material below according to parts by weight
101 parts of resin, 42 parts of curing agent, 37 parts of silicone resin, 15 parts of sillimanite, 1.3 parts of dibutyl phthalate, propylene oxide butyl
21 parts of ether, 0.6 part of eucalyptol.
Wherein, the epoxy resin is made of bisphenol A type epoxy resin and bisphenol-s epoxy resin according to weight ratio 3:1；
The curing agent is hexahydrophthalic anhydride.
The preparation method of the electrical composition epoxy resin of the low viscosity, fire resistant, steps are as follows:
1) sillimanite is weighed, is put into ball mill, the water of 7 times of weight, ball milling mixing 2h is added, discharging obtains sunset line
Stone dispersion liquid；
2) dilute hydrochloric acid solution of concentration 15% is added into sillimanite dispersion liquid, is stirred 1h at 600 rpm, then
It is sent into processor for ultrasonic wave, is ultrasonically treated 45min, discharging obtains the first treatment fluid, wherein the dilute hydrochloric acid solution adds
Enter 25% that amount is sillimanite dispersion liquid total volume, the ultrasonic treatment frequency is 40kHz；
3) sodium hydroxide solution is added dropwise into the first treatment fluid under the stirring of 300rpm, adjusts pH to 7, stands 2h, obtains
Obtain second processing liquid；
4) second processing liquid is filtered, and the solid matter that filtering obtains is dried at 50 DEG C to get modified sillimanite
Powder；
5) epoxy resin and silicone resin are weighed, is added into reaction kettle, is evacuated to 0.05Mpa, is warming up to 85 DEG C, heat preservation
23min is added modified sillimanite powder and epoxy propane butyl ether, is stirred 50min, be cooled to 55 DEG C, O-phthalic is added
Dibutyl phthalate and eucalyptol continue to be stirred 32min, obtain mixture A；
6) curing agent is weighed, is added into mixture A, 35min is stirred at 50 DEG C, obtains mixture B；
7) mixture B is poured into mold, keeps the temperature 2.5h at 65 DEG C, then heat to 125 DEG C, keep the temperature 1h, stopped
It heats, after natural cooling, demoulding.
Embodiment 4
A kind of electrical composition epoxy resin of low viscosity, fire resistant, is made: epoxy of the raw material below according to parts by weight
102 parts of resin, 43 parts of curing agent, 36 parts of silicone resin, 14 parts of sillimanite, 1.5 parts of dibutyl phthalate, propylene oxide butyl
20 parts of ether, 0.7 part of eucalyptol.
Wherein, the epoxy resin is made of bisphenol A type epoxy resin and bisphenol-s epoxy resin according to weight ratio 3:1；
The curing agent is hexahydrophthalic anhydride.
The preparation method of the electrical composition epoxy resin of the low viscosity, fire resistant, steps are as follows:
1) sillimanite is weighed, is put into ball mill, the water of 7 times of weight, ball milling mixing 2.5h is added, discharging obtains sunset
Line stone dispersion liquid；
2) dilute hydrochloric acid solution of concentration 15% is added into sillimanite dispersion liquid, is stirred 1.5h at 600 rpm, so
It is sent into processor for ultrasonic wave afterwards, is ultrasonically treated 45min, discharging obtains the first treatment fluid, wherein the dilute hydrochloric acid solution
Additional amount is the 25% of sillimanite dispersion liquid total volume, and the ultrasonic treatment frequency is 50kHz；
3) sodium hydroxide solution is added dropwise into the first treatment fluid under the stirring of 300rpm, adjusts pH to 7, stands 2.5h,
Obtain second processing liquid；
4) second processing liquid is filtered, and the solid matter that filtering obtains is dried at 55 DEG C to get modified sillimanite
Powder；
5) epoxy resin and silicone resin are weighed, is added into reaction kettle, is evacuated to 0.05Mpa, is warming up to 90 DEG C, heat preservation
25min is added modified sillimanite powder and epoxy propane butyl ether, is stirred 55min, be cooled to 55 DEG C, O-phthalic is added
Dibutyl phthalate and eucalyptol continue to be stirred 35min, obtain mixture A；
6) curing agent is weighed, is added into mixture A, 35min is stirred at 55 DEG C, obtains mixture B；
7) mixture B is poured into mold, keeps the temperature 2.5h at 70 DEG C, then heat to 125 DEG C, kept the temperature 1.5h, stop
Only heat, after natural cooling, demoulding.
Embodiment 5
A kind of electrical composition epoxy resin of low viscosity, fire resistant, is made: epoxy of the raw material below according to parts by weight
104 parts of resin, 44 parts of curing agent, 35 parts of silicone resin, 13 parts of sillimanite, 1.7 parts of dibutyl phthalate, propylene oxide butyl
19 parts of ether, 0.8 part of eucalyptol.
Wherein, the epoxy resin is made of bisphenol A type epoxy resin and bisphenol-s epoxy resin according to weight ratio 3:1；
The curing agent is hexahydrophthalic anhydride.
The preparation method of the electrical composition epoxy resin of the low viscosity, fire resistant, steps are as follows:
1) sillimanite is weighed, is put into ball mill, the water of 7 times of weight, ball milling mixing 3h is added, discharging obtains sunset line
Stone dispersion liquid；
2) dilute hydrochloric acid solution of concentration 15% is added into sillimanite dispersion liquid, is stirred 1.5h at 600 rpm, so
It is sent into processor for ultrasonic wave afterwards, is ultrasonically treated 50min, discharging obtains the first treatment fluid, wherein the dilute hydrochloric acid solution
Additional amount is the 30% of sillimanite dispersion liquid total volume, and the ultrasonic treatment frequency is 50kHz；
3) sodium hydroxide solution is added dropwise into the first treatment fluid under the stirring of 400rpm, adjusts pH to 7, stands 2.5h,
Obtain second processing liquid；
4) second processing liquid is filtered, and the solid matter that filtering obtains is dried at 60 DEG C to get modified sillimanite
Powder；
5) epoxy resin and silicone resin are weighed, is added into reaction kettle, is evacuated to 0.05Mpa, is warming up to 100 DEG C, is protected
Warm 25min is added modified sillimanite powder and epoxy propane butyl ether, is stirred 58min, is cooled to 60 DEG C, and adjacent benzene two is added
Formic acid dibutyl ester and eucalyptol continue to be stirred 35min, obtain mixture A；
6) curing agent is weighed, is added into mixture A, 40min is stirred at 60 DEG C, obtains mixture B；
7) mixture B is poured into mold, keeps the temperature 2.5h at 70 DEG C, then heat to 130 DEG C, keep the temperature 2h, stopped
It heats, after natural cooling, demoulding.
Embodiment 6
A kind of electrical composition epoxy resin of low viscosity, fire resistant, is made: epoxy of the raw material below according to parts by weight
104 parts of resin, 42 parts of curing agent, 38 parts of silicone resin, 13 parts of sillimanite, 1.6 parts of dibutyl phthalate, propylene oxide butyl
21 parts of ether, 0.8 part of eucalyptol.
Wherein, the epoxy resin is made of bisphenol A type epoxy resin and bisphenol-s epoxy resin according to weight ratio 3:1；
The curing agent is hexahydrophthalic anhydride.
The preparation method of the electrical composition epoxy resin of the low viscosity, fire resistant, steps are as follows:
1) sillimanite is weighed, is put into ball mill, the water of 8 times of weight, ball milling mixing 2.5h is added, discharging obtains sunset
Line stone dispersion liquid；
2) dilute hydrochloric acid solution of concentration 15% is added into sillimanite dispersion liquid, is stirred 1.5h at 600 rpm, so
It is sent into processor for ultrasonic wave afterwards, is ultrasonically treated 50min, discharging obtains the first treatment fluid, wherein the dilute hydrochloric acid solution
Additional amount is the 28% of sillimanite dispersion liquid total volume, and the ultrasonic treatment frequency is 60kHz；
3) sodium hydroxide solution is added dropwise into the first treatment fluid under the stirring of 300rpm, adjusts pH to 7, stands 2.5h,
Obtain second processing liquid；
4) second processing liquid is filtered, and the solid matter that filtering obtains is dried at 60 DEG C to get modified sillimanite
Powder；
5) epoxy resin and silicone resin are weighed, is added into reaction kettle, is evacuated to 0.05Mpa, is warming up to 100 DEG C, is protected
Warm 30min is added modified sillimanite powder and epoxy propane butyl ether, is stirred 56min, is cooled to 60 DEG C, and adjacent benzene two is added
Formic acid dibutyl ester and eucalyptol continue to be stirred 40min, obtain mixture A；
6) curing agent is weighed, is added into mixture A, 35min is stirred at 60 DEG C, obtains mixture B；
7) mixture B is poured into mold, keeps the temperature 2.5h at 70 DEG C, then heat to 130 DEG C, keep the temperature 2h, stopped
It heats, after natural cooling, demoulding.
Embodiment 7
A kind of electrical composition epoxy resin of low viscosity, fire resistant, is made: epoxy of the raw material below according to parts by weight
105 parts of resin, 45 parts of curing agent, 38 parts of silicone resin, 16 parts of sillimanite, 2 parts of dibutyl phthalate, epoxy propane butyl ether
22 parts, 0.9 part of eucalyptol.
Wherein, the epoxy resin is made of bisphenol A type epoxy resin and bisphenol-s epoxy resin according to weight ratio 3:1；
The curing agent is hexahydrophthalic anhydride.
The preparation method of the electrical composition epoxy resin of the low viscosity, fire resistant, steps are as follows:
1) sillimanite is weighed, is put into ball mill, the water of 8 times of weight, ball milling mixing 3h is added, discharging obtains sunset line
Stone dispersion liquid；
2) dilute hydrochloric acid solution of concentration 15% is added into sillimanite dispersion liquid, 2h is stirred at 700rpm, then
It is sent into processor for ultrasonic wave, is ultrasonically treated 50min, discharging obtains the first treatment fluid, wherein the dilute hydrochloric acid solution adds
Enter 30% that amount is sillimanite dispersion liquid total volume, the ultrasonic treatment frequency is 60kHz；
3) sodium hydroxide solution is added dropwise into the first treatment fluid under the stirring of 400rpm, adjusts pH to 7, stands 3h, obtains
Obtain second processing liquid；
4) second processing liquid is filtered, and the solid matter that filtering obtains is dried at 60 DEG C to get modified sillimanite
Powder；
5) epoxy resin and silicone resin are weighed, is added into reaction kettle, is evacuated to 0.05Mpa, is warming up to 100 DEG C, is protected
Warm 30min is added modified sillimanite powder and epoxy propane butyl ether, is stirred 60min, is cooled to 60 DEG C, and adjacent benzene two is added
Formic acid dibutyl ester and eucalyptol continue to be stirred 40min, obtain mixture A；
6) curing agent is weighed, is added into mixture A, 40min is stirred at 60 DEG C, obtains mixture B；
7) mixture B is poured into mold, keeps the temperature 3h at 70 DEG C, then heat to 130 DEG C, keep the temperature 2h, stop adding
Heat, after natural cooling, demoulding.
Comparative example 1
Compared with Example 4, sillimanite is free of, other are same as Example 4.
Comparative example 2
Compared with Example 4, eucalyptol is free of, other are same as Example 4.
Comparative example 3
Compared with Example 4, sillimanite and eucalyptol are free of, other are same as Example 4.
Performance detection is carried out to epoxy resin prepared by embodiment 4 and comparative example 1-3, test result is as follows shown in table.
1 performance test table of table
| Performance | Viscosity, cps (90 DEG C) | Glass transition temperature Tg, DEG C | Heat distortion temperature, DEG C |
| Embodiment 4 | 1325 | 245 | 218 |
| Comparative example 1 | 1421 | 213 | 201 |
| Comparative example 2 | 1337 | 221 | 205 |
| Comparative example 3 | 1463 | 203 | 193 |
As can be seen that epoxy resin viscosity prepared by the present invention is low from result above, be conducive to process, and have
There is excellent high temperature resistance, is conducive to improve the service life of product under the high temperature conditions, is conducive to expand the electrical of product
The application range in field, has a vast market foreground.
In addition, embodiment 4, compared with the performance of comparative example 1-3, the viscosity of embodiment 4 is suitable with the viscosity of comparative example 1-3,
The glass transition temperature and heat distortion temperature of embodiment 4 are superior to comparative example 1-3, therefore, it can be seen that the present invention by
Sillimanite and eucalyptol are added in formula, sillimanite and eucalyptol cooperate, and act synergistically with other components, are conducive to mention
The glass transition temperature and heat distortion temperature of high epoxy resin.
Better embodiment of the invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula within the knowledge of one of ordinary skill in the art can also be without departing from the purpose of the present invention
Various changes can be made.
Claims (10)
1. a kind of electrical composition epoxy resin of low viscosity, fire resistant, which is characterized in that by below according to the raw material of parts by weight
It is made: 100-105 parts of epoxy resin, 41-45 parts of curing agent, 34-38 parts of silicone resin, 12-16 parts of sillimanite, phthalic acid two
1-2 parts of butyl ester, 18-22 parts of epoxy propane butyl ether, 0.5-0.9 parts of eucalyptol.
2. the electrical composition epoxy resin of low viscosity, fire resistant according to claim 1, which is characterized in that by pressing below
It is made according to the raw material of parts by weight: 101-104 parts of epoxy resin, 42-44 parts of curing agent, 35-37 parts of silicone resin, sillimanite 13-15
Part, 1.3-1.7 parts of dibutyl phthalate, 19-21 parts of epoxy propane butyl ether, 0.6-0.8 parts of eucalyptol.
3. the electrical composition epoxy resin of low viscosity, fire resistant according to claim 2, which is characterized in that by pressing below
It is made according to the raw material of parts by weight: 102 parts of epoxy resin, 43 parts of curing agent, 36 parts of silicone resin, 14 parts of sillimanite, phthalic acid
1.5 parts of dibutyl ester, 20 parts of epoxy propane butyl ether, 0.7 part of eucalyptol.
4. the electrical composition epoxy resin of low viscosity, fire resistant according to claim 1, which is characterized in that the epoxy
Resin is made of bisphenol A type epoxy resin and bisphenol-s epoxy resin.
5. the electrical composition epoxy resin of low viscosity, fire resistant according to claim 4, which is characterized in that the epoxy
Resin is made of bisphenol A type epoxy resin and bisphenol-s epoxy resin according to weight ratio 3:1.
6. the electrical composition epoxy resin of low viscosity, fire resistant according to claim 1, which is characterized in that the solidification
Agent is hexahydrophthalic anhydride.
7. a kind of preparation method of the electrical composition epoxy resin of the low viscosity, fire resistant as described in claim 1-6 is any,
It is characterized in that, steps are as follows:
1) sillimanite is weighed, is put into ball mill, the water of 6-8 times of weight, ball milling mixing 2-3h is added, discharging obtains sunset line
Stone dispersion liquid；
2) dilute hydrochloric acid solution of concentration 15% is added into sillimanite dispersion liquid, 1-2h is stirred at 500-700rpm, so
It is sent into processor for ultrasonic wave afterwards, is ultrasonically treated 40-50min, discharging obtains the first treatment fluid；
3) sodium hydroxide solution is added dropwise into the first treatment fluid under the stirring of 200-400rpm, adjusts pH to 7, stands 2-3h,
Obtain second processing liquid；
4) second processing liquid is filtered, and the solid matter that filtering obtains is dried at 50-60 DEG C to get modified sillimanite
Powder；
5) epoxy resin and silicone resin are weighed, is added into reaction kettle, is evacuated to 0.05Mpa, is warming up to 80-100 DEG C, heat preservation
20-30min is added modified sillimanite powder and epoxy propane butyl ether, is stirred 50-60min, be cooled to 50-60 DEG C, is added
Dibutyl phthalate and eucalyptol continue to be stirred 30-40min, obtain mixture A；
6) curing agent is weighed, is added into mixture A, 30-40min is stirred at 50-60 DEG C, obtains mixture B；
7) mixture B is poured into mold, keeps the temperature 2-3h at 65-70 DEG C, then heat to 125-130 DEG C, keep the temperature 1-2h,
Stop heating, after natural cooling, demoulding.
8. the preparation method of the electrical composition epoxy resin of low viscosity, fire resistant according to claim 7, feature exist
In in step 2), the additional amount of the dilute hydrochloric acid solution is the 20-30% of sillimanite dispersion liquid total volume.
9. the preparation method of the electrical composition epoxy resin of low viscosity, fire resistant according to claim 7, feature exist
In in step 2), the ultrasonic treatment frequency is 40-60kHz.
10. a kind of electrical composition epoxy resin of the low viscosity, fire resistant as described in claim 1-6 is any is preparing epoxy
Purposes in naval stores.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810222724.9A CN110157154A (en) | 2018-03-19 | 2018-03-19 | A kind of electrical composition epoxy resin of low viscosity, fire resistant and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810222724.9A CN110157154A (en) | 2018-03-19 | 2018-03-19 | A kind of electrical composition epoxy resin of low viscosity, fire resistant and preparation method thereof |
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Citations (3)
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|---|---|---|---|---|
| CN102732209A (en) * | 2012-07-06 | 2012-10-17 | 郑州大学 | High-temperature-resistant flexible adhesive cured at normal temperature and preparation method thereof |
| CN104804693A (en) * | 2015-05-20 | 2015-07-29 | 叶芳 | Novel high temperature-resistant epoxy resin structure adhesive and preparation method thereof |
| CN105482293A (en) * | 2015-12-11 | 2016-04-13 | 中冠电缆有限公司 | Modified fibrolite for high-temperature-resistant polyvinyl chloride cable material and preparing method of thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732209A (en) * | 2012-07-06 | 2012-10-17 | 郑州大学 | High-temperature-resistant flexible adhesive cured at normal temperature and preparation method thereof |
| CN104804693A (en) * | 2015-05-20 | 2015-07-29 | 叶芳 | Novel high temperature-resistant epoxy resin structure adhesive and preparation method thereof |
| CN105482293A (en) * | 2015-12-11 | 2016-04-13 | 中冠电缆有限公司 | Modified fibrolite for high-temperature-resistant polyvinyl chloride cable material and preparing method of thereof |
Non-Patent Citations (1)
| Title |
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| 田磊: ""萜类和挥发油"", 《中药学专业知识（一）》 * |
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Application publication date: 20190823 |