CN110204858A - Low temperature resistant insulation high thermal conductivity impregnated material of one kind and preparation method thereof - Google Patents
Low temperature resistant insulation high thermal conductivity impregnated material of one kind and preparation method thereof Download PDFInfo
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- 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
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- C08K3/28—Nitrogen-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/282—Binary compounds of nitrogen with aluminium
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The present invention provides a kind of low temperature resistant insulation high thermal conductivity impregnated materials and preparation method thereof, which includes following components according to the mass fraction: epoxy resin 100, curing agent 60~90, heat filling 1~20, silane coupling agent 1~10.Impregnated material loading < 5wt% provided by the invention, tensile strength > 70MPa, disruptive field intensity > 70kV/mm, thermal conductivity > 0.2W/ (m*K), ensure that good mechanical property, electric property and heating conduction under low loading.Preparation method provided by the invention passes through the high-temperature process and modification to filler, effectively enhance interfacial effect, reduce the loss of mechanics, electric property, the method makes filler is more uniform to be distributed in entire resin system by ultrasonic disperse, the generation for preventing agglomeration is conducive to the foundation of passage of heat under low loading.
Description
Technical field
The present invention relates to a kind of insulation high thermal conductivity impregnated materials, in particular to a kind of to have excellent mechanical performances, electricity
The superconduction of performance and heating conduction low temperature resistant insulating heat-conductive impregnated material and preparation method.
Background technique
When substance reaches certain critical-temperature, the characteristic that resistance is zero is referred to as superconduction, not according to superconduction critical temperature
High-temperature superconductor (liquid nitrogen temperature, 77K) and cryogenic superconductor (liquid helium temperature, 4K) can be divided into superconductor.As electric device
Superconductor itself electrical insulating property it is most important.Epoxy resin as impregnating varnish is because of its excellent electrical insulating property and processability
Either layer insulation, turn-to-turn insulation or insulation against ground critical role can be occupied in entire superconductor, furthermore epoxy
Resin can also play the effects of support, bonding.Moreover epoxy insulation impregnating varnish will also have good heating conduction to keep away
Exempt to cause to quench the irreversible consequence of phenomenon bring because local temperature increases.
It is the main side for improving Heat Conduction Material heating conduction that heat filling and resin matrix, which are carried out compound blend method,
The main method of method.According to phonon thermal conduction theory, high filler loading capacity is building thermal conducting path, improves the necessary hand of thermal conductivity of material
Section can be strengthened to glue to lose support however as the intrinsic black brittleness of increase epoxy resin of heat filling itself therewith
Effect is connect, and high loading filler introduces more faults of construction often again to further decrease the electricity of epoxy resin
Insulation performance.
There are many researchs to the epoxy composite material with good heat conductive insulation performance both at home and abroad, it is most of more to stress
In the research of high temperature or room-temperature property, lack the research for Low-temperature epoxy composite material.Scholar Tanaka is in (IEEE
Transactions on Dielectrics and Electrical Insulation Vol.18,No.6；December
2011) disclosing a kind of can improve the room temperature thermal conductivity of insulating heat-conductive impregnating varnish to 2.91W/ (m* under 80wt% doping
K the report of superior isolation heat filling boron nitride (thermal conductivity is 180W/ (m*K))), however since highly doped amount results in tree
There are more defects, the breakdown strength of the insulating heat-conductive filler has dropped 45% in rouge.
Therefore, it need to provide a kind of while there is the superconduction of good low temperature mechanical property, electric property and heating conduction with resistance to
The thermally conductive impregnated material of low-temperature insulation.
Summary of the invention
For the defect for meeting the prior art, the present invention provides one kind to have simultaneously under low loading (loading < 5wt%)
Have excellent mechanical performances (tensile strength > 70MPa), electric property (breakdown strength > 70kV/mm) and heating conduction (thermal conductivity >
0.2W/ (m*K)) low-temperature superconducting insulating heat-conductive impregnated material and preparation method thereof.
Realize that the technical solution of the object of the invention is as follows:
A kind of low temperature resistant insulation high thermal conductivity impregnated material, the impregnated material includes following components according to the mass fraction:
Epoxy resin 100, curing agent 60~90, heat filling 1~20, silane coupling agent 1~10.
Preferably, the epoxy resin includes from glycidyl ether type epoxy, glycidol lipid epoxy, glycidyl amine
One or more mixtures that class epoxy, linear aliphatic same clan epoxy and alicyclic ring same clan epoxy are selected.
Preferably, the glycidyl ether type epoxy includes bisphenol A-type or bisphenol-f type；
The glycidol esters epoxy include phthalic acid ethylene oxidic ester, tetrahydrophthalic acid ethylene oxidic ester or
Hexahydrophthalic acid ethylene oxidic ester；
The glycidol amine epoxy includes four glycidyl amine of diaminodiphenylmethane or diglycidyl to ammonia
Base phenol；
Linear aliphatic race epoxy includes polyethylene glycol di-epoxide；
The alicyclic epoxy includes poly- [(2- Oxyranyle) -1,2- cyclohexanediol] 2- ethyl -2- (methylol) -1,
3-propanediol ether.
Preferably, shrink curing agent includes solid from fatty amine curing agent, aromatic amine curing agent, anhydride curing agent and polymer
One or more mixtures that agent is selected.
Preferably, the fatty amine curing agent includes polyetheramine, diethylenetriamine or triethylene tetramine；
The aromatic amine curing agent includes m-phenylene diamine (MPD) or diamino diphenyl sulfone；
The anhydride curing agent includes methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride or benzophenone tetracarboxylic dianhydride；
The polymer curing agents include 400 type of 200 type of polyamide or polyamide.
Preferably, the heat filling includes aluminium nitride, boron nitride, silicon nitride, aluminium oxide or silica.
Preferably, the size of the heat filling is 1nm-200 μm；The crystal form of the heat filling includes six sides or stands
Side；The pattern of the heat filling includes spherical, sheet or rodlike.
Preferably, the silane coupling agent includes pressing γ-aminopropyl triethoxysilane (KH-550), γ-(2,3- rings
The third oxygen of oxygen) propyl trimethoxy silicane (KH-560), γ-methacryloxypropyl trimethoxy silane (KH-570) or N-
β-(aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane (KH-602).
Preferably, the loading<5wt% of the impregnated material, tensile strength>70MPa, breakdown strength>70KV/mm, lead
Heating rate > 0.2W/ (m*K)
A kind of preparation method of impregnated material as described in any one of the above embodiments, includes the following steps:
(1) heat filling is pre-processed:
It is molten in the ethyl alcohol of silane coupling agent after calcined heat filling in water ultrasonic wave dispersion, filtering and drying
The pretreated heat filling is heated to reflux to obtain in liquid；
(2) impregnated material is prepared:
After being ultrasonically treated 20~40min after the pretreated heat filling and epoxy resin stirring, add solid
Agent mixes dispersion, vacuum defoamation and solidifies to obtain the impregnated material.
Preferably, the step (1) calcining is 0.5~2h of calcining at 500 DEG C~1200 DEG C.
Preferably, the step (1) is dry for 6~12h dry in 100 DEG C~140 DEG C of vacuum oven.
Preferably, the step (1) is heated to reflux the time as 2~6h.
Preferably, step (2) the mixing dispersion includes mechanical stirring or ultrasonic disperse.
Preferably, the mechanical stirring magnetic stirring apparatus or mechanical agitator；The ultrasonic disperse ultrasonic dispersers
Or cell disruptor.
Preferably, step (2) solidification, which is included at 40~60 DEG C, solidifies 0~4h, solidifies 1- at 100-120 DEG C
8h, finally it is warming up to 150-180 DEG C of solidification 1-4 hours.
Preferably, described to be cured as 50 DEG C of solidification 2h, again 110 DEG C of solidification 4h, finally it is warming up to 150 DEG C of solidification 2h.
Compared with the latest prior art, technical solution provided by the invention has the advantages that
Loading < 5wt%, tensile strength > 70MPa, breakdown field of low temperature resistant superconduction impregnated material provided by the invention
Strong > 70kV/mm and thermal conductivity > 0.2W/ (m*K), ensure that good mechanical property, electric property and is led under low loading
Hot property.
Preparation method provided by the invention effectively enhances interfacial effect by high-temperature process and modification to filler,
Reduce the loss of mechanics, electric property, the method by ultrasonic disperse make filler it is more uniform be distributed in entire resin system
In, it is therefore prevented that the generation of agglomeration is conducive to the foundation of passage of heat under low loading.It is guided simultaneously by MOLECULE DESIGN
Structure-activity relationship, flexible siloxanes can improve the intrinsic low temperature tolerance ability of resin matrix, be conducive to composite material as collaboration curing agent
The promotion of low temperature resistant comprehensive performance.
Preparation method provided by the invention simple, lower-price characteristic with process, can be in industrialized production extensively
Using.
Detailed description of the invention:
Fig. 1: boron nitride transmission electron microscope picture after modification；
Fig. 2: the profile scanning Electronic Speculum for the impregnated material that the embodiment of the present invention 1 provides.
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to embodiments, but the present invention is not limited to these
Embodiment.
Filler boron nitride used is that product number is 20063778 purchased from Sinopharm Chemical Reagent Co., Ltd.；Institute
Filler boron nitride is that product number is 200637611 purchased from Aladdin；Filler silicon nitride used is that product number is
20073762 are purchased from Sinopharm Chemical Reagent Co., Ltd.；Filler aluminium nitride used is that product number is 20075870 to be purchased from
Sinopharm Chemical Reagent Co., Ltd.；
Epoxy resin used is that product number is GY282 purchased from Huntsman Corporation；Epoxy resin used is product
Number is E-51 purchased from Wuxi resin processing plant；
Curing agent used is that polyetheramine product number is D-230 purchased from Tianjin Heowns Biochemical Technology Co., Ltd.；
Curing agent used is that methyl hexahydrophthalic anhydride product number is 668670 purchased from lark prestige Science and Technology Ltd.；Solidification used
Agent is that bis- (3- the aminopropyl) -1,1,3,3- tetramethyl disiloxane product numbers of 1,3- are W830187 purchased from An Naijike
Skill Co., Ltd.
Embodiment 1
The preparation of low temperature resistant insulation high thermal conductivity impregnated material:
(1) heat filling is pre-processed:
By the ultrasonic wavelength-division in water of 100 μm of the sheet hexagonal boron nitride in Muffle furnace after 1000 DEG C are calcined 1h
It dissipates, filter to obtain boron nitride particle, the 10g boron nitride particle, 0.5g silane in 120 DEG C of vacuum oven after dry 8h are even
Connection agent KH-560 is heated to reflux 4h in 400ml ethanol solution and obtains pretreated heat filling；
(2) impregnated material is prepared:
It will be ultrasonically treated after the pretreated boron nitride particle uniform stirring of 50g glycidyl ether resin GY282 and 1.5g
30min, be eventually adding 18g polyethers amine hardener D-230 magnetic agitation uniformly, vacuum defoamation, finally solidification is 2 small at 50 DEG C
When, solidify 4 hours at 110 DEG C, after be warming up to 150 DEG C of solidifications 2 hours up to the impregnated material.
Embodiment 2
The preparation of low temperature resistant insulation high thermal conductivity impregnated material:
(1) heat filling is pre-processed:
By the ultrasonic wavelength-division in water of the spherical cubic silicon nitride of the 1nm in Muffle furnace after 1200 DEG C are calcined 0.5h
It dissipates, filter to obtain silicon nitride particle, the 10g silicon nitride particle, 0.5g silane in 100 DEG C of vacuum oven after dry 6h are even
Connection agent KH-550 is heated to reflux 2h in 400ml ethanol solution and obtains pretreated heat filling；
(2) impregnated material is prepared:
It will be ultrasonically treated after 50g phthalic acid ethylene oxidic ester and the pretreated silicon nitride particle uniform stirring of 0.5g
20min, be eventually adding 30g m-phenylene diamine (MPD) curing agent ultrasonic disperse uniformly, vacuum defoamation, finally solidify at 40 DEG C 1 hour,
Solidify 1 hour at 100 DEG C, after be warming up to 160 DEG C of solidifications 1 hour up to the impregnated material.
Embodiment 3
The preparation of low temperature resistant insulation high thermal conductivity impregnated material:
(1) heat filling is pre-processed:
By in Muffle furnace by 500 DEG C calcine 2h after 200 μm of rodlike cubic oxide aluminium in water ultrasonic wave dispersion,
Alumina particle is filtered to obtain, 20g alumina particle, 5g silane coupling agent in 140 DEG C of vacuum oven after dry 12h
KH-570 is heated to reflux 6h in 400ml ethanol solution and obtains pretreated heat filling；
(2) impregnated material is prepared:
It will surpass after four glycidyl amine of 50g diaminodiphenylmethane and the pretreated alumina particle uniform stirring of 10g
Sonication 40min, be eventually adding 45g methyl hexahydrophthalic anhydride be uniformly dispersed with cell disruptor, vacuum defoamation, finally at 120 DEG C
Lower solidification 8 hours, after be warming up to 180 DEG C of solidifications 4 hours up to the impregnated material.
Embodiment 4
The preparation of low temperature resistant insulation high thermal conductivity impregnated material:
(1) heat filling is pre-processed:
By the ultrasonic wavelength-division in water of 100 μm of six side's aluminium nitride of sheet in Muffle furnace after 1000 DEG C are calcined 1h
It dissipates, filter to obtain aluminum nitride particle, the 10g aluminum nitride particle, 0.5g silane in 120 DEG C of vacuum oven after dry 8h are even
Connection agent KH-602 is heated to reflux 4h in 400ml ethanol solution and obtains pretreated heat filling；
(2) impregnated material is prepared:
It will be ultrasonically treated after 50g polyethylene glycol di-epoxide and the pretreated alumina particle uniform stirring of 1.5g
30min, be eventually adding 18g methyl tetrahydro phthalic anhydride curing agent magnetic agitation uniformly, vacuum defoamation, finally solidification is 2 small at 50 DEG C
When, solidify 4 hours at 110 DEG C, after be warming up to 150 DEG C of solidifications 2 hours up to the impregnated material.
Embodiment 5
The preparation of low temperature resistant insulation high thermal conductivity impregnated material:
(1) heat filling is pre-processed:
By the ultrasonic wavelength-division in water of 100 μm of six side's silica of sheet in Muffle furnace after 1000 DEG C are calcined 1h
It dissipates, filter to obtain silica dioxide granule, 10g silica dioxide granule, 0.5g silicon in 120 DEG C of vacuum oven after dry 8h
Alkane coupling agent KH-602 is heated to reflux 4h in 400ml ethanol solution and obtains pretreated heat filling；
(2) impregnated material is prepared:
It will be ultrasonically treated after 50g polyethylene glycol di-epoxide and the pretreated alumina particle uniform stirring of 1.5g
30min, be eventually adding 18g methyl tetrahydro phthalic anhydride curing agent magnetic agitation uniformly, vacuum defoamation, finally solidification is 2 small at 50 DEG C
When, solidify 4 hours at 110 DEG C, after be warming up to 150 DEG C of solidifications 2 hours up to the impregnated material.
Reference examples:
By 50g phthalic acid ethylene oxidic ester and 30g m-phenylene diamine (MPD) curing agent is uniformly mixed and vacuum defoamation, finally 40
Solidify 1 hour at solidifying 1 hour, 100 DEG C at DEG C, after be warming up to 160 DEG C of solidifications 1 hour up to the reference examples impregnated material.
To the above various embodiments and reference examples resulting superconduction insulating heat-conductive impregnating varnish under liquid nitrogen temperature (- 196 DEG C)
It carries out tensile strength, breakdown voltage and thermal conductivity test, test result and is shown in Table 1:
Table 1: the low temperature resistant insulation high thermal conductivity impregnated material of each embodiment provided by the invention and reference examples impregnated material
Property:
| Tensile strength/MPa | Breakdown strength/kV/mm | Thermal conductivity/W/ (m*K) | |
| Embodiment 1 | 142 | 83 | 0.24 |
| Embodiment 2 | 135 | 79 | 0.23 |
| Embodiment 3 | 141 | 82 | 0.26 |
| Embodiment 4 | 146 | 84 | 0.25 |
| Embodiment 5 | 132 | 76 | 0.24 |
| Reference examples | 78 | 80 | 0.12 |
The above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited, the common skill of fields
Art personnel should be appreciated that referring to above-described embodiment can with modifications or equivalent substitutions are made to specific embodiments of the invention,
These are applying for pending claim protection model without departing from any modification of spirit and scope of the invention or equivalent replacement
Within enclosing.
Claims (17)
1. a kind of low temperature resistant insulation high thermal conductivity impregnated material, which is characterized in that the impregnated material includes according to the mass fraction
Following components: epoxy resin 100, curing agent 60~90, heat filling 1~20 and silane coupling agent 1~10.
2. a kind of impregnated material as described in claim 1, which is characterized in that the epoxy resin includes from glycidol ethers
It is selected in epoxy, glycidol lipid epoxy, glycidol amine epoxy, linear aliphatic same clan epoxy and alicyclic ring same clan epoxy
One or more mixtures.
3. a kind of impregnated material as claimed in claim 2, which is characterized in that the glycidyl ether type epoxy includes bisphenol-A
Type or bisphenol-f type；
The glycidol esters epoxy includes phthalic acid ethylene oxidic ester, tetrahydrophthalic acid ethylene oxidic ester or hexahydro
O-phthalic acid glycidyl ester；
The glycidol amine epoxy includes four glycidyl amine of diaminodiphenylmethane or diglycidyl p-aminophenyl
Phenol；
Linear aliphatic race epoxy includes polyethylene glycol di-epoxide；
The alicyclic epoxy includes poly- [(2- Oxyranyle) -1,2- cyclohexanediol] 2- ethyl -2- (methylol) -1,3- third
Glycol ethers.
4. a kind of impregnated material as described in claim 1, which is characterized in that shrink curing agent include from fatty amine curing agent,
One or more mixtures that aromatic amine curing agent, anhydride curing agent and polymer curing agents are selected.
5. a kind of impregnated material as claimed in claim 4, which is characterized in that the fatty amine curing agent includes polyetheramine, two
Ethylene triamine or triethylene tetramine；
The aromatic amine curing agent includes m-phenylene diamine (MPD) or diamino diphenyl sulfone；
The anhydride curing agent includes methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride or benzophenone tetracarboxylic dianhydride；
The polymer curing agents include 400 type of 200 type of polyamide or polyamide.
6. a kind of impregnated material as described in claim 1, which is characterized in that the heat filling include aluminium nitride, boron nitride,
Silicon nitride, aluminium oxide or silica.
7. a kind of impregnated material as claimed in claim 6, which is characterized in that the size of the heat filling is 1nm-200 μm；
The crystal form of the heat filling include six sides or cube；The pattern of the heat filling includes spherical, sheet or rodlike.
8. a kind of impregnated material as described in claim 1, which is characterized in that the silane coupling agent includes pressing γ-aminopropyl
Triethoxysilane (KH-550), γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane (KH-560), γ-methacryl
Oxygroup propyl trimethoxy silicane (KH-570) or N- β-(aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane (KH-602).
9. a kind of impregnated material as described in claim 1, which is characterized in that loading < 5wt% of the impregnated material, drawing
Stretch intensity > 70MPa, breakdown strength > 70kV/mm, thermal conductivity > 0.2W/ (m*K).
10. a kind of preparation method of impregnated material as described in any one of claims 1 to 9, which is characterized in that including walking as follows
It is rapid:
(1) heat filling is pre-processed:
After calcined heat filling in water ultrasonic wave dispersion, filtering and drying, in the ethanol solution of silane coupling agent
It is heated to reflux to obtain the pretreated heat filling；
(2) impregnated material is prepared:
After being ultrasonically treated 20~40min after the pretreated heat filling and epoxy resin stirring, curing agent is added
It mixes dispersion, vacuum defoamation and solidifies to obtain the impregnated material.
11. preparation method as claimed in claim 10, which is characterized in that step (1) calcining is 500 DEG C~1200
0.5~2h is calcined at DEG C.
12. preparation method as claimed in claim 10, which is characterized in that the step (1) is dry at 100 DEG C~140 DEG C
Dry 6~12h in vacuum oven.
13. preparation method as claimed in claim 10, which is characterized in that the step (1) is heated to reflux the time as 2~6h.
14. preparation method as claimed in claim 10, which is characterized in that the step (2) mixing dispersion include mechanical stirring or
Ultrasonic disperse.
15. preparation method as claimed in claim 14, which is characterized in that the mechanical stirring magnetic stirring apparatus or mechanical stirring
Device；The ultrasonic disperse ultrasonic dispersers or cell disruptor.
16. preparation method as claimed in claim 10, which is characterized in that step (2) solidification is included at 40~60 DEG C solid
0~4h of change, solidify 1-8h at 100-120 DEG C, be finally warming up to 150-180 DEG C of solidification 1-4 hours.
17. preparation method as claimed in claim 16, which is characterized in that described to be cured as 50 DEG C of solidification 2h, again 110 DEG C of solidifications
4h is finally warming up to 150 DEG C of solidification 2h.
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