CN109762436A - A kind of low temperature resistant heat conductive insulating lacquer type organic coating and its preparation method and application suitable for superconducting insulation material - Google Patents
A kind of low temperature resistant heat conductive insulating lacquer type organic coating and its preparation method and application suitable for superconducting insulation material Download PDFInfo
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- CN109762436A CN109762436A CN201811516339.1A CN201811516339A CN109762436A CN 109762436 A CN109762436 A CN 109762436A CN 201811516339 A CN201811516339 A CN 201811516339A CN 109762436 A CN109762436 A CN 109762436A
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Abstract
The low temperature resistant heat conductive insulating lacquer type organic coating and its preparation method and application that the invention discloses a kind of suitable for superconducting insulation material, its raw material includes epoxy resin, polyether epoxy, epoxy hardener, polyurethane resin, acrylic resin, nbr carboxyl terminal and accounts for the nano level modified boron nitride that material quality percentage composition is 2-6.5%, epoxy resin, polyurethane resin, acrylic resin, nbr carboxyl terminal and nano level modified boron nitride the mass ratio that feeds intake be 5.5-17: 2-7: 0.8-2.5: 0.2-2.5: 1；Preparation: mixing epoxy resin with nano level modified boron nitride, and polyurethane resin reaction is added, polyether epoxy, nbr carboxyl terminal, epoxy hardener and acrylic resin is added, that is, is made；And its application in superconducting insulation material；Insulating resin paint of the present invention have both excellent electric property, processing performance, high thermal conductivity and preferably in a low temperature of mechanical property.
Description
Technical field
The invention belongs to superconducting insulation field more particularly to a kind of superconducting insulation materials, and in particular to one kind is suitable for super
Lead the low temperature resistant heat conductive insulating lacquer type organic coating and its preparation method and application of insulating materials.
Background technique
Epoxy resin due to excellent electrical insulation capability, excellent mechanical property and good processing performance,
It has been widely applied in superconducting insulation system.However as high-temperature superconductor insulating materials, need to be chronically under liquid nitrogen temperature
Work, it requires that epoxy resin must have excellent low temperature resistant mechanical property.In addition, to prevent from being obstructed due to heat transfer
And cause the phenomenon that losing superconductivity effects, the destruction to entire superconducting apparatus is caused, also requires epoxy resin that must have well
Heating conduction, but since conventional epoxies show brittleness feature at low temperature, and thermal conductivity at room temperature is lower, only
0.2W/mK or so, therefore be unable to satisfy superconducting device and insulating resin is wanted on cryogenic mechanics performance and insulation heat-conducting property
It asks.
It is big for brittleness existing for existing epoxy resin, it is not low temperature resistant the defects of, done in currently available technology some
It improves, such as Chinese invention patent CN 103740059B, it discloses a kind of low temperature resistant insulated impregnating resins, by weight, institute
The composition of raw materials for stating low temperature resistant insulated impregnating resin is as follows: 100 parts of epoxy resin, 40~90 parts of polyurethane-epoxy resin, number is equal
At 20~50 parts, 25 DEG C of end phenolic hydroxyl group low molecular weight polyphenylene ether resins of the molecular weight between 1500~2500 viscosity 50~
100~200 parts of low viscosity polyether epoxy between 100mPa.s, 10~30 parts of epoxy hardener, the low temperature resistant insulation
The curing molding temperature of impregnating resin is 120~160 DEG C；By weight, the polyurethane-epoxy resin is made of the following raw material:
100 parts of glycolylurea epoxide resin, poly- (tetramethylene-copolymerization-ethyleneether) glycol 15 that number-average molecular weight is 1000~2000~
30 parts, 1~3 part of 1,4-butanediol, 5~10 parts of hexa-methylene isocyanates；Although this patent realizes epoxy resin-matrix dipping
Paint has preferable resistance to low temperature, preferable electrical insulation properties, but it can not achieve good thermally conductive, be unable to satisfy
Requirement of the superconducting device to insulating resin on insulation heat-conducting property.
In order to promote heating conduction, at present common practice first is that add heat filling into resin, however directly to
Heat filling is mixed or filled in resin matrix, and there is also following some technological difficulties: (1) increasing the same of interface resistance
When, the preferable of heat filling and polymeric matrix compatible is not easy to realize；(2) do not lose polymer good workability and it is low at
How this while realizes that the thermal conductivity for making polymer matrix composite with a small amount of heat filling additive amount improves；(3) exist
Under the premise of keeping polymer insulation, the thermal conductivity of polymer how is improved.And there are no one kind in the art can
Using epoxy resin as matrix resin and be provided simultaneously with high thermal conductivity and preferably in a low temperature of mechanical property insulating resin paint.
Summary of the invention
The technical problem to be solved by the present invention is to overcome deficiency in the prior art, provide a kind of suitable for superconducting insulation
The low temperature resistant heat conductive insulating lacquer type organic coating of material can have both excellent electric property, processing performance, high thermal conductivity and preferable low
Mechanical property under temperature.
The present invention also provides a kind of preparation methods of low temperature resistant heat conductive insulating lacquer type organic coating suitable for superconducting insulation material.
The present invention additionally provides a kind of low temperature resistant heat conductive insulating lacquer type organic coating suitable for superconducting insulation material in superconduction simultaneously
Application in insulating materials.
In order to solve the above technical problems, a kind of technical solution that the present invention takes is as follows:
A kind of low temperature resistant heat conductive insulating lacquer type organic coating suitable for superconducting insulation material, the raw material of the insulating resin paint include
Epoxy resin, polyether epoxy, epoxy hardener, the raw material further include polyurethane resin, acrylic resin, carboxyl end group fourth
Nitrile rubber and nano level modified boron nitride, the epoxy resin, the polyurethane resin, the acrylic resin, the end carboxylic
The mass ratio that feeds intake of base nitrile rubber and the nano level modified boron nitride is 5.5-17: 2-7: 0.8-2.5: 0.2-2.5: 1, with
Mass percentage meter, the mass percentage that the nano level modified boron nitride accounts for the raw material is 2-6.5%.
Some preferred aspects according to the present invention, the epoxy resin, the polyurethane resin, the acrylic resin,
The mass ratio that feeds intake of the nbr carboxyl terminal and the nano level modified boron nitride is 5.5-13: 2-5: 0.8-2: 0.5-2:
1.It is highly preferred that the epoxy resin, the polyurethane resin, the acrylic resin, the nbr carboxyl terminal and institute
The mass ratio that feeds intake for stating nano level modified boron nitride is 5.5-12.5: 2.1-5: 0.8-1.9: 0.5-1.5: 1.
More according to the present invention specific and preferred aspect, the nano level modified boron nitride are prepared via a method which
And obtain: modified boron nitride is made using alkaline hydrated oxide and hexagonal boron nitride hybrid reaction, then by the modified nitridation
Boron ultrasonic disperse and generate nano level modified boron nitride.
Some specific aspects according to the present invention, the shape of the nano level modified boron nitride are sheet.
More according to the present invention specific and preferred aspect, the alkaline hydrated oxide are sodium hydroxide and/or hydrogen-oxygen
Change potassium.
Some preferred aspects according to the present invention, the boron nitride are hexagonal boron nitride.
Some preferred aspects according to the present invention, the insulating resin paint are prepared via a method which and obtain: in 90-110
DEG C the epoxy resin is mixed with the nano level modified boron nitride, the polyurethane resin is then added, keeps temperature anti-
It answers, is cooled to 40-60 DEG C and the polyether epoxy mixing is added, the nbr carboxyl terminal mixing is added, adds ring
Oxygen curing agent and acrylic resin, mixing, are made the insulating resin paint.
Some preferred aspects according to the present invention, the epoxy resin are selected from bisphenol A type epoxy resin, Bisphenol F type ring
One of oxygen resin and hyperbranched epoxy resin or a variety of combinations.One according to the present invention specific and preferred aspect,
The epoxy resin is made of bisphenol A type epoxy resin, bisphenol f type epoxy resin and hyperbranched epoxy resin.Further preferably
Ground, the epoxy resin by feed intake mass ratio be 0.6-0.8: 0.6-0.8: 1 bisphenol A type epoxy resin, bisphenol F type epoxy tree
Rouge and hyperbranched epoxy resin are constituted.
Some preferred aspects according to the present invention, the epoxy hardener are selected from polyamide 6 50, diethyl toluene diamine
With one of methylnadic anhydride or a variety of combinations.
Some preferred aspects according to the present invention, the epoxy hardener is by polyamide 6 50, diethyl toluene diamine and first
Base carbic anhydride is constituted, and the mass ratio that feeds intake of the polyamide 6 50, diethyl toluene diamine and methylnadic anhydride is
0.8-1.2∶0.8-1.2∶1。
Some preferred aspects according to the present invention, in terms of mass fraction, in the raw material, 100 parts of epoxy resin, polyurethane
30-50 parts of resin, 90-110 parts of polyether epoxy, 10-20 parts of acrylic resin, 5-15 parts of nbr carboxyl terminal, nanometer
Grade is boron nitride 6-18 parts, 10-20 parts of epoxy hardener modified.
According to the present invention, the polyurethane resin is commercially available conventional polyurethanes resin, is including but not limited to purchased from Dongguan
The FR-C609 of Jing Ze resin Co., Ltd, city.
According to the present invention, the polyether epoxy is commercially available conventional polyether epoxy resin, is including but not limited to purchased from
Fly upward the E208 of Jun Yan new material limited liability company in Shenzhen.
According to the present invention, the acrylic resin is commercially available conventional propylene acid resin, is including but not limited to purchased from same moral
The AC10331 of resin.
Another technical solution provided by the invention: a kind of described above to be suitable for the low temperature resistant thermally conductive of superconducting insulation material
The preparation method of insulating resin paint, the preparation method include the following steps:
(1) each raw material is weighed by formula, epoxy resin is added in reaction vessel, 90-110 DEG C is warming up to, vacuumizes；
(2) nano level modified boron nitride, mixing is added；
(3) polyurethane resin is added and keeps 90-110 DEG C of temperature reaction；
(4) it is cooled to 40-60 DEG C, polyether epoxy, mixing is added；
(5) nbr carboxyl terminal is added at 40-60 DEG C, mixes；
(6) epoxy hardener and acrylic resin is added, mixing is made described suitable for the low temperature resistant of superconducting insulation material
Heat conductive insulating lacquer type organic coating.
Another technical solution provided by the invention: a kind of described above to be suitable for the low temperature resistant thermally conductive of superconducting insulation material
Application of the insulating resin paint in superconducting insulation material.
Due to the use of above technical scheme, the invention has the following advantages over the prior art:
Insulating resin paint of the invention is by using polyurethane resin, acrylic resin and carboxyl end group butyl rubber and epoxy
Resin and polyether epoxy compound and form modified epoxy resin-matrix insulating resin paint, do not give only insulating resin paint
Fabulous resistance to low temperature, at the same by selecting specific heat filling, i.e., nano level modified boron nitride, and controller adds
Amount also overcomes on the basis of imparting insulating resin paint fabulous heating conduction because adding heat filling due to bring pair
The adverse effect of electric property, mechanical mechanics property and processing performance, so that insulating resin paint of the invention can have both
Excellent high thermal conductivity, resistance to low temperature, excellent electric property and processing performance, to make it particularly suitable for superconducting insulation
In material.
Specific embodiment
Above scheme is described further below in conjunction with specific embodiment；It should be understood that these embodiments are for illustrating
The basic principles, principal features and advantages of the present invention, and the present invention is not by the scope limitation of following embodiment；It is used in embodiment
Implementation condition further adjustment can be done according to specific requirement, the implementation condition being not specified is usually the item in routine experiment
Part.
In following, unless otherwise specified, all raw materials are both from conventional method system commercially available or by this field
It is standby and obtain.Bisphenol A type epoxy resin (is purchased from Ba Ling petrochemical industry E-44)；Bisphenol f type epoxy resin (is purchased from Taiwan South Asia NPEF-
170)；Hyperbranched epoxy resin (is purchased from Wuhan hyperbranched resin Science and Technology Ltd. HyPer E102)；Polyurethane resin (is purchased from
Dongguan City Jing Ze resin Co., Ltd FR-C609)；Polyether epoxy (flies upward fine horse purchased from Shenzhen and grinds the limited public affairs of new material share
Take charge of E208)；Acrylic resin (purchased from moral Resin A C10331)；Nbr carboxyl terminal (it is limited to lead to high chemical industry purchased from Jingjiang City
Company's T L910).
Embodiment 1
The present embodiment provides a kind of nano level modified boron nitride, preparation method is as follows:
Step 1) first weighs 3 parts of hexagonal boron nitrides and is added in 50 parts of ethanol solution, and it is standby that dispersion obtains milky white liquid
With.Then 100 parts of NaOH aqueous solution (mass fraction 16.7%) for configuring 5mol/L (0.2g/ml) is spare, will be above two
Solution is added in three-necked flask, under 100 DEG C of oil baths magnetic agitation and carry out be condensed back 18 hours, then by acquired solution
Filtering and washing is carried out to neutrality, is then dried to get modified h-BN (i.e. modified boron nitride) is arrived.
50 parts of deionized waters are blended step 2) with 50 parts of isopropanols, (deionized water: isopropanol=1:1), by 2 parts of modifications
Boron nitride is added in blend solution, forms milky white solution.The milky white solution is subjected to ultrasonic disperse and handles 4h (JY92-
2D ultrasonic cell disrupte machine), obtain the dispersion solution of modified boron nitride, then to its dispersion liquid carry out centrifugal treating (4000r,
Unstripped modification boron nitride 10min) is removed, supernatant liquor is collected, continues centrifugal treating (10000r, 10min) and finally obtains
The nano level modified boron nitride (BNNS-OH) of the sheet of removing.
Embodiment 2
The present embodiment provides a kind of low temperature resistant heat conductive insulating lacquer type organic coatings suitable for superconducting insulation material, with mass fraction
Meter, raw material include:
Wherein, epoxy resin is by 30 parts of bisphenol A type epoxy resin, 30 parts of bisphenol f type epoxy resin and hyperbranched asphalt mixtures modified by epoxy resin
40 parts of rouge compositions；
Curing agent is made of 5 parts of polyamide 6s, 50,5 parts of diethyl toluene diamines and 5 parts of methylnadic anhydrides.
The preparation method of the above-mentioned low temperature resistant heat conductive insulating lacquer type organic coating suitable for superconducting insulation material includes the following steps:
(1) each raw material is weighed by formula, epoxy resin is added in reaction vessel, 100 DEG C is warming up to, vacuumizes 30min；
(2) nano level modified boron nitride is added, 2h is mixed；
(3) polyurethane resin is added and keeps 100 DEG C of temperature reactions；
(4) 50 DEG C are cooled to, polyether epoxy is added, 1h is mixed；
(5) nbr carboxyl terminal is added at 40-60 DEG C, 1h is mixed；
(6) epoxy hardener and acrylic resin is added, mixing is made described suitable for the resistance to low of superconducting insulation material
Warm heat conductive insulating lacquer type organic coating.
Embodiment 3
The present embodiment provides a kind of low temperature resistant heat conductive insulating lacquer type organic coatings suitable for superconducting insulation material, with mass fraction
Meter, raw material include:
The other the same as in Example 2.
Embodiment 4
The present embodiment provides a kind of low temperature resistant heat conductive insulating lacquer type organic coatings suitable for superconducting insulation material, with mass fraction
Meter, raw material include:
The other the same as in Example 2.
Embodiment 5
The present embodiment provides a kind of low temperature resistant heat conductive insulating lacquer type organic coatings suitable for superconducting insulation material, with mass fraction
Meter, raw material include:
The other the same as in Example 2.
Comparative example 1
Substantially with embodiment 2, difference, which is only that in raw material, is not added acrylic resin, corresponding to adjust containing for epoxy resin
Amount.
Comparative example 2
Substantially with embodiment 2, difference, which is only that in raw material, is not added nbr carboxyl terminal, corresponding adjustment epoxy resin
Content.
Comparative example 3
Substantially with embodiment 2, difference is only that the silicon rubber that nbr carboxyl terminal is replaced with to equal quality.
Comparative example 4
Substantially with embodiment 2, difference is only that, as follows in preparation method: by epoxy resin, nano level modified nitridation
It is kept stirring 2h at 80 DEG C after boron, polyurethane resin, polyether epoxy, acrylic resin, nbr carboxyl terminal mixing,
Then epoxy hardener is added, mixes and is made.
Performance test
After insulating resin paint film-forming obtained by above-described embodiment 2-5 and comparative example 1-4, consolidating of being formed is measured
The performance parameter for changing film is as shown in table 1.Liquid nitrogen environment in following is circulation > 40 times.
Table 1
Continued 1
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention, it is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of low temperature resistant heat conductive insulating lacquer type organic coating suitable for superconducting insulation material, the raw material of the insulating resin paint includes ring
Oxygen resin, polyether epoxy, epoxy hardener, which is characterized in that the raw material further includes polyurethane resin, acrylic acid tree
Rouge, nbr carboxyl terminal and nano level modified boron nitride, the epoxy resin, the polyurethane resin, the acrylic acid tree
The mass ratio that feeds intake of rouge, the nbr carboxyl terminal and the nano level modified boron nitride is 5.5-17: 2-7: 0.8-2.5:
0.2-2.5: 1, in terms of mass percentage, the mass percentage that the nano level modified boron nitride accounts for the raw material is 2-
6.5%。
2. the low temperature resistant heat conductive insulating lacquer type organic coating according to claim 1 suitable for superconducting insulation material, which is characterized in that
The nano level modified boron nitride is prepared via a method which and obtains: using alkaline hydrated oxide and hexagonal boron nitride hybrid reaction
And modified boron nitride is made, the modified boron nitride ultrasonic disperse is then generated into nano level modified boron nitride.
3. the low temperature resistant heat conductive insulating lacquer type organic coating according to claim 2 suitable for superconducting insulation material, which is characterized in that
The shape of the nano level modified boron nitride is sheet；And/or the alkaline hydrated oxide is sodium hydroxide and/or hydroxide
Potassium；And/or the boron nitride is hexagonal boron nitride.
4. the low temperature resistant heat conductive insulating lacquer type organic coating according to claim 1 suitable for superconducting insulation material, which is characterized in that
The insulating resin paint is prepared via a method which and obtains: at 90-110 DEG C by the epoxy resin and the nano level modified nitrogen
Change boron mixing, the polyurethane resin is then added, keep thermotonus, is cooled to 40-60 DEG C and the polyethers asphalt mixtures modified by epoxy resin is added
Rouge mixing is added the nbr carboxyl terminal mixing, adds epoxy hardener and acrylic resin, mix, is made described
Insulating resin paint.
5. the low temperature resistant heat conductive insulating lacquer type organic coating according to claim 1 suitable for superconducting insulation material, which is characterized in that
The epoxy resin is selected from one of bisphenol A type epoxy resin, bisphenol f type epoxy resin and hyperbranched epoxy resin or more
The combination of kind.
6. the low temperature resistant heat conductive insulating lacquer type organic coating according to claim 1 suitable for superconducting insulation material, which is characterized in that
The epoxy hardener is selected from one of polyamide 6 50, diethyl toluene diamine and methylnadic anhydride or a variety of
Combination.
7. the low temperature resistant heat conductive insulating lacquer type organic coating according to claim 6 suitable for superconducting insulation material, which is characterized in that
The epoxy hardener is made of polyamide 6 50, diethyl toluene diamine and methylnadic anhydride, the polyamide 6 50, two
The mass ratio that feeds intake of ethyltoluene diamines and methylnadic anhydride is 0.8-1.2: 0.8-1.2: 1.
8. the low temperature resistant heat conductive insulating lacquer type organic coating according to claim 1 suitable for superconducting insulation material, which is characterized in that
In terms of mass fraction, in the raw material, 100 parts of epoxy resin, 30-50 parts of polyurethane resin, 90-110 parts of polyether epoxy,
10-20 parts of acrylic resin, 5-15 parts of nbr carboxyl terminal, boron nitride 6-18 parts nano level modified, epoxy hardener 10-20
Part.
9. being suitable for the low temperature resistant heat conductive insulating of superconducting insulation material described in a kind of any one of claim 1-8 claim
The preparation method of lacquer type organic coating, which is characterized in that the preparation method includes the following steps:
(1) each raw material is weighed by formula, epoxy resin is added in reaction vessel, 90-110 DEG C is warming up to, vacuumizes；
(2) nano level modified boron nitride, mixing is added；
(3) polyurethane resin is added and keeps 90-110 DEG C of temperature reaction；
(4) it is cooled to 40-60 DEG C, polyether epoxy, mixing is added；
(5) nbr carboxyl terminal is added at 40-60 DEG C, mixes；
(6) epoxy hardener and acrylic resin is added, mixing is made described suitable for the low temperature resistant thermally conductive of superconducting insulation material
Insulating resin paint.
10. suitable for the low temperature resistant thermally conductive exhausted of superconducting insulation material described in a kind of any one of claim 1-8 claim
Application of the edge lacquer type organic coating in superconducting insulation material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811516339.1A CN109762436B (en) | 2018-12-12 | 2018-12-12 | Low-temperature-resistant heat-conducting insulating resin paint suitable for superconducting insulating material and preparation method and application thereof |
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| CN201811516339.1A CN109762436B (en) | 2018-12-12 | 2018-12-12 | Low-temperature-resistant heat-conducting insulating resin paint suitable for superconducting insulating material and preparation method and application thereof |
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