CN109762436B - Low-temperature-resistant heat-conducting insulating resin paint suitable for superconducting insulating material and preparation method and application thereof - Google Patents
Low-temperature-resistant heat-conducting insulating resin paint suitable for superconducting insulating material and preparation method and application thereof Download PDFInfo
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- CN109762436B CN109762436B CN201811516339.1A CN201811516339A CN109762436B CN 109762436 B CN109762436 B CN 109762436B CN 201811516339 A CN201811516339 A CN 201811516339A CN 109762436 B CN109762436 B CN 109762436B
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Abstract
The invention discloses a low-temperature-resistant heat-conducting insulating resin paint suitable for superconducting insulating materials, and a preparation method and application thereof, wherein the raw materials comprise epoxy resin, polyether epoxy resin, an epoxy curing agent, polyurethane resin, acrylic resin, carboxyl-terminated butadiene-acrylonitrile rubber and nanoscale modified boron nitride accounting for 2-6.5% of the raw materials by mass, and the feeding mass ratio of the epoxy resin, the polyurethane resin, the acrylic resin, the carboxyl-terminated butadiene-acrylonitrile rubber and the nanoscale modified boron nitride is 5.5-17: 2-7: 0.8-2.5: 0.2-2.5: 1; preparation: firstly, mixing epoxy resin with nanoscale modified boron nitride, adding polyurethane resin for reaction, and adding polyether epoxy resin, carboxyl-terminated butadiene-acrylonitrile rubber, an epoxy curing agent and acrylic resin to prepare the polyurethane modified boron nitride; and its application in superconducting insulating materials; the insulating resin paint disclosed by the invention has excellent electrical properties, processability, high heat conductivity and better mechanical properties at low temperature.
Description
Technical Field
The invention belongs to the field of superconducting insulation, particularly relates to a superconducting insulating material, and particularly relates to low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material, and a preparation method and application thereof.
Background
Epoxy resin has been widely used in superconducting insulation systems due to its excellent electrical insulation properties, excellent mechanical properties and good processing properties. However, as a high-temperature superconducting insulating material, it is required to operate at a liquid nitrogen temperature for a long period of time, and therefore, it is required that the epoxy resin has excellent low-temperature mechanical properties. In addition, in order to prevent the damage to the whole superconducting equipment caused by the loss of superconducting effect due to the hindered heat transfer, the epoxy resin is required to have good heat-conducting property, but the traditional epoxy resin has the characteristic of brittleness at low temperature and low heat conductivity at room temperature, which is only about 0.2W/mK, so that the requirements of the superconducting device on the low-temperature mechanical property and the insulating heat-conducting property of the insulating resin cannot be met.
Aiming at the defects of high brittleness, low temperature resistance and the like of the existing epoxy resin, some improvements have been made in the prior art, for example, Chinese invention patent CN 103740059B discloses a low temperature resistant insulating impregnating resin, and the formula of the raw materials of the low temperature resistant insulating impregnating resin is as follows by weight: 100 parts of epoxy resin, 40-90 parts of polyurethane epoxy resin, 20-50 parts of phenolic hydroxyl terminated low molecular weight polyphenylene ether resin with the number average molecular weight of 1500-2500, 100-200 parts of low viscosity polyether epoxy resin with the viscosity of 50-100 mPa.s at 25 ℃, 10-30 parts of epoxy curing agent, wherein the curing and forming temperature of the low temperature resistant insulating impregnating resin is 120-160 ℃; the polyurethane epoxy resin is prepared from the following raw materials in parts by weight: 100 parts of hydantoin epoxy resin, 15-30 parts of poly (tetramethylene-co-ethyleneether) glycol with the number average molecular weight of 1000-2000, 1-3 parts of 1, 4-butanediol and 5-10 parts of hexamethylene isocyanate; although the epoxy resin-based impregnating varnish has good low-temperature resistance and good electrical insulation performance, the epoxy resin-based impregnating varnish can not realize good heat conduction and can not meet the requirement of a superconducting device on the insulation and heat conduction performance of insulation resin.
In order to improve the heat-conducting performance, one of the current common methods is to add a heat-conducting filler into the resin, however, the direct incorporation or filling of the heat-conducting filler into the resin matrix has some technical difficulties: (1) the better compatibility of the heat-conducting filler and the polymer matrix is not easy to realize while the interface thermal resistance is not increased; (2) the method is to realize the improvement of the thermal conductivity of the polymer matrix composite material by adding a small amount of the heat-conducting filler without losing the good processability and the low cost of the polymer; (3) how to improve the thermal conductivity of the polymer on the premise of keeping the insulating property of the polymer. However, no insulating resin paint which can use epoxy resin as matrix resin and has high heat conductivity and good mechanical property at low temperature exists in the prior art.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art, and provide the low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material, which has excellent electrical property, processability, high heat conductivity and better mechanical property at low temperature.
The invention also provides a preparation method of the low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material.
The invention also provides application of the low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material in the superconducting insulating material.
In order to solve the technical problems, the invention adopts a technical scheme as follows:
the low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material comprises raw materials of epoxy resin, polyether epoxy resin and an epoxy curing agent, and also comprises polyurethane resin, acrylic resin, carboxyl-terminated butadiene-acrylonitrile rubber and nanoscale modified boron nitride, wherein the feeding mass ratio of the epoxy resin, the polyurethane resin, the acrylic resin, the carboxyl-terminated butadiene-acrylonitrile rubber and the nanoscale modified boron nitride is 5.5-17: 2-7: 0.8-2.5: 0.2-2.5: 1, and the nanoscale modified boron nitride accounts for 2-6.5% of the raw materials by mass percentage.
According to some preferred aspects of the present invention, the mass ratio of the epoxy resin, the polyurethane resin, the acrylic resin, the carboxyl-terminated nitrile rubber and the nanoscale modified boron nitride is 5.5-13: 2-5: 0.8-2: 0.5-2: 1. More preferably, the mass ratio of the epoxy resin, the polyurethane resin, the acrylic resin, the carboxyl-terminated butadiene-acrylonitrile rubber and the nanoscale modified boron nitride is 5.5-12.5: 2.1-5: 0.8-1.9: 0.5-1.5: 1.
According to some specific and preferred aspects of the present invention, the nanoscale modified boron nitride is prepared by: the method comprises the steps of mixing and reacting alkaline hydroxide with hexagonal boron nitride to prepare modified boron nitride, and then carrying out ultrasonic dispersion on the modified boron nitride to generate nanoscale modified boron nitride.
According to some specific aspects of the present invention, the nanoscale modified boron nitride is in the shape of a plate.
According to some specific and preferred aspects of the present invention, the alkaline hydroxide is sodium hydroxide and/or potassium hydroxide.
According to some preferred aspects of the invention, the boron nitride is hexagonal boron nitride.
According to some preferred aspects of the present invention, the insulating resin varnish is prepared by: and mixing the epoxy resin and the nanoscale modified boron nitride at 90-110 ℃, then adding the polyurethane resin, keeping the temperature for reaction, cooling to 40-60 ℃, adding the polyether epoxy resin for mixing, adding the carboxyl-terminated butadiene-acrylonitrile rubber for mixing, adding an epoxy curing agent and acrylic resin for mixing, and preparing the insulating resin paint.
According to some preferred aspects of the present invention, the epoxy resin is a combination of one or more selected from the group consisting of bisphenol a type epoxy resins, bisphenol F type epoxy resins, and hyperbranched epoxy resins. According to a specific and preferred aspect of the present invention, the epoxy resin is composed of a bisphenol a type epoxy resin, a bisphenol F type epoxy resin, and a hyperbranched epoxy resin. Further preferably, the epoxy resin is composed of bisphenol A type epoxy resin, bisphenol F type epoxy resin and hyperbranched epoxy resin which are fed in a mass ratio of 0.6-0.8: 1.
According to some preferred aspects of the present invention, the epoxy curing agent is a combination of one or more selected from the group consisting of polyamide 650, diethyltoluenediamine, and methylnadic anhydride.
According to some preferred aspects of the present invention, the epoxy curing agent is composed of polyamide 650, diethyltoluenediamine, and methylnadic anhydride, and the polyamide 650, the diethyltoluenediamine, and the methylnadic anhydride are fed in a mass ratio of 0.8-1.2: 1.
According to some preferred aspects of the invention, the raw materials comprise, by mass, 100 parts of epoxy resin, 30-50 parts of polyurethane resin, 90-110 parts of polyether epoxy resin, 10-20 parts of acrylic resin, 5-15 parts of carboxyl-terminated nitrile butadiene rubber, 6-18 parts of nanoscale modified boron nitride and 10-20 parts of epoxy curing agent.
According to the present invention, the polyurethane resin is a conventional polyurethane resin commercially available, including but not limited to FR-C609 from resins of choice, Inc. of Dongguan.
According to the present invention, the polyether epoxy resin is a conventional polyether epoxy resin commercially available, including but not limited to E208 available from Shenzhen flying Jun research New materials GmbH.
According to the present invention, the acrylic resin is a conventional acrylic resin commercially available, including but not limited to AC10331 from alder resins.
The invention provides another technical scheme that: the preparation method of the low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material comprises the following steps:
(1) weighing the raw materials according to the formula, adding epoxy resin into a reaction container, heating to 90-110 ℃, and vacuumizing;
(2) adding nano-grade modified boron nitride, and mixing;
(3) adding polyurethane resin, and keeping the temperature at 90-110 ℃ for reaction;
(4) cooling to 40-60 deg.C, adding polyether epoxy resin, and mixing;
(5) adding carboxyl-terminated butadiene-acrylonitrile rubber at 40-60 ℃, and mixing;
(6) and adding an epoxy curing agent and acrylic resin, and mixing to prepare the low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material.
The invention provides another technical scheme that: the application of the low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material in the superconducting insulating material is disclosed.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
the modified epoxy resin-based insulating resin paint is formed by compounding the polyurethane resin, the acrylic resin, the carboxyl-terminated butyl rubber, the epoxy resin and the polyether epoxy resin, so that the insulating resin paint has excellent low-temperature resistance, and meanwhile, the adverse effects on the electrical performance, the mechanical performance and the processing performance caused by the addition of the heat-conducting filler are overcome by selecting the specific heat-conducting filler, namely the nanoscale modified boron nitride and controlling the addition amount of the controller on the basis of endowing the insulating resin paint with excellent heat-conducting performance, so that the insulating resin paint disclosed by the invention has excellent high heat-conducting performance, low-temperature resistance, excellent electrical performance and processing performance, and is particularly suitable for superconducting insulating materials.
Detailed Description
The above-described scheme is further illustrated below with reference to specific examples; it is to be understood that these embodiments are provided to illustrate the general principles, essential features and advantages of the present invention, and the present invention is not limited in scope by the following embodiments; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments.
In the following, all starting materials are either commercially available or prepared by conventional methods in the art, unless otherwise specified. Bisphenol a type epoxy resin (available from ba ling petrochemical E-44); bisphenol F type epoxy resin (available from south Taiwan Asia NPEF-170); hyperbranched epoxy resin (available from Wuhan hyperbranched resin technology Ltd. HyPer E102); polyurethane resin (available from competitive resins Co., Ltd., Dongguan city FR-C609); polyether epoxy resin (purchased from Shenzhen flying Jun research New Material Co., Ltd., E208); acrylic resin (from the same german resin AC 10331); carboxyl-terminated nitrile rubber (available from Jingjiang, Tokyo, high chemical industry Co., Ltd., TL 910).
Example 1
The embodiment provides a nanoscale modified boron nitride, and the preparation method comprises the following steps:
step 1) weighing 3 parts of hexagonal boron nitride, adding the hexagonal boron nitride into 50 parts of ethanol solution, and dispersing to obtain milky white liquid for later use. And then 100 parts of 5mol/L (0.2g/ml) NaOH aqueous solution (mass fraction is 16.7%) are prepared for standby application, the two solutions are added into a three-neck flask, magnetic stirring is carried out under 100 ℃ oil bath, condensation reflux is carried out for 18 hours, then the obtained solution is filtered, washed to be neutral, and dried, thus obtaining the modified h-BN (namely modified boron nitride).
Step 2) 50 parts of deionized water was blended with 50 parts of isopropyl alcohol, (deionized water: isopropanol 1:1), 2 parts of modified boron nitride was added to the blended solution to form a milky white solution. And (3) carrying out ultrasonic dispersion treatment on the milky white solution for 4h (JY92-2D ultrasonic cell crusher) to obtain a dispersion solution of modified boron nitride, then carrying out centrifugal treatment (4000r, 10min) on the dispersion solution to remove the non-stripped modified boron nitride, collecting supernatant, and continuing the centrifugal treatment (10000r, 10min) to finally obtain stripped flaky nanoscale modified boron nitride (BNNS-OH).
Example 2
The embodiment provides a low-temperature-resistant heat-conducting insulating resin paint suitable for a superconducting insulating material, which comprises the following raw materials in parts by mass:
wherein the epoxy resin is composed of 30 parts of bisphenol A epoxy resin, 30 parts of bisphenol F epoxy resin and 40 parts of hyperbranched epoxy resin;
the curing agent is composed of 5 parts of polyamide 650, 5 parts of diethyltoluenediamine and 5 parts of methylnadic anhydride.
The preparation method of the low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material comprises the following steps:
(1) weighing the raw materials according to the formula, adding epoxy resin into a reaction container, heating to 100 ℃, and vacuumizing for 30 min;
(2) adding nanoscale modified boron nitride, mixing and stirring for 2 hours;
(3) adding polyurethane resin, and keeping the temperature at 100 ℃ for reaction;
(4) cooling to 50 ℃, adding polyether epoxy resin, mixing and stirring for 1 h;
(5) adding carboxyl-terminated butadiene-acrylonitrile rubber at 40-60 ℃, and mixing and stirring for 1 h;
(6) and adding an epoxy curing agent and acrylic resin, and mixing to obtain the low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material.
Example 3
The embodiment provides a low-temperature-resistant heat-conducting insulating resin paint suitable for a superconducting insulating material, which comprises the following raw materials in parts by mass:
the rest is the same as example 2.
Example 4
The embodiment provides a low-temperature-resistant heat-conducting insulating resin paint suitable for a superconducting insulating material, which comprises the following raw materials in parts by mass:
the rest is the same as example 2.
Example 5
The embodiment provides a low-temperature-resistant heat-conducting insulating resin paint suitable for a superconducting insulating material, which comprises the following raw materials in parts by mass:
the rest is the same as example 2.
Comparative example 1
The process is substantially the same as example 2 except that no acrylic resin is added to the raw materials and the content of the epoxy resin is adjusted accordingly.
Comparative example 2
The procedure is essentially the same as in example 2, except that no carboxyl-terminated nitrile rubber is added to the starting materials and the epoxy resin content is adjusted accordingly.
Comparative example 3
Essentially the same as example 2, except that the carboxyl-terminated nitrile rubber was replaced with an equivalent mass of silicone rubber.
Comparative example 4
The method is basically the same as example 2, and the difference is that: mixing epoxy resin, nanoscale modified boron nitride, polyurethane resin, polyether epoxy resin, acrylic resin and carboxyl-terminated butadiene-acrylonitrile rubber, keeping stirring at 80 ℃ for 2 hours, adding an epoxy curing agent, and uniformly mixing to obtain the epoxy resin modified boron nitride modified polyurethane epoxy resin modified polyurethane resin.
Performance testing
The performance parameters of the cured coating films formed after curing the insulating resin paints obtained in examples 2 to 5 and comparative examples 1 to 4 to form films are shown in Table 1. The liquid nitrogen environment in the following is more than 40 cycles.
TABLE 1
TABLE 1
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (6)
1. The low-temperature-resistant heat-conducting insulating resin paint is suitable for superconducting insulating materials, and raw materials of the insulating resin paint comprise epoxy resin, polyether epoxy resin and an epoxy curing agent, and is characterized by further comprising polyurethane resin, acrylic resin, carboxyl-terminated butadiene-acrylonitrile rubber and nanoscale modified boron nitride;
the material comprises, by mass, 100 parts of epoxy resin, 30-50 parts of polyurethane resin, 90-110 parts of polyether epoxy resin, 10-20 parts of acrylic resin, 5-15 parts of carboxyl-terminated nitrile rubber, 6-18 parts of nano-modified boron nitride and 10-20 parts of epoxy curing agent;
the mass ratio of the epoxy resin, the polyurethane resin, the acrylic resin, the carboxyl-terminated butadiene-acrylonitrile rubber and the nanoscale modified boron nitride is 5.5-17: 2-7: 0.8-2.5: 0.2-2.5: 1, and the nanoscale modified boron nitride accounts for 2-6.5% of the raw materials in mass percentage;
the epoxy resin is composed of bisphenol A type epoxy resin, bisphenol F type epoxy resin and hyperbranched epoxy resin with the feeding mass ratio of 0.6-0.8: 1;
the epoxy curing agent is composed of polyamide 650, diethyl toluene diamine and methyl nadic anhydride, and the feeding mass ratio of the polyamide 650 to the diethyl toluene diamine to the methyl nadic anhydride is 0.8-1.2: 1;
the nanoscale modified boron nitride is prepared by the following method: mixing and reacting alkaline hydroxide and hexagonal boron nitride to prepare modified boron nitride, and then ultrasonically dispersing the modified boron nitride to generate nano-scale modified boron nitride;
the insulating resin paint is prepared by the following method: and mixing the epoxy resin and the nanoscale modified boron nitride at 90-110 ℃, then adding the polyurethane resin, keeping the temperature for reaction, cooling to 40-60 ℃, adding the polyether epoxy resin for mixing, adding the carboxyl-terminated butadiene-acrylonitrile rubber for mixing, adding an epoxy curing agent and acrylic resin for mixing, and preparing the insulating resin paint.
2. The low temperature resistant thermal conductive insulating resin varnish suitable for superconducting insulation material according to claim 1, wherein the nanoscale modified boron nitride is in the shape of a sheet; and/or, the alkaline hydroxide is sodium hydroxide and/or potassium hydroxide.
3. The low temperature resistant heat conductive insulating resin paint suitable for superconducting insulating materials according to claim 1, wherein the mass ratio of the epoxy resin, the polyurethane resin, the acrylic resin, the carboxyl-terminated nitrile rubber and the nanoscale modified boron nitride is 5.5-13: 2-5: 0.8-2: 0.5-2: 1.
4. The low temperature resistant heat conductive insulating resin paint suitable for superconducting insulating materials according to claim 3, wherein the mass ratio of the epoxy resin, the polyurethane resin, the acrylic resin, the carboxyl-terminated nitrile rubber and the nanoscale modified boron nitride is 5.5-12.5: 2.1-5: 0.8-1.9: 0.5-1.5: 1.
5. A preparation method of the low temperature resistant heat conduction insulating resin paint suitable for the superconducting insulating material according to any one of claims 1 to 4, characterized by comprising the following steps:
(1) weighing the raw materials according to the formula, adding epoxy resin into a reaction container, heating to 90-110 ℃, and vacuumizing;
(2) adding nano-grade modified boron nitride, and mixing;
(3) adding polyurethane resin, and keeping the temperature at 90-110 ℃ for reaction;
(4) cooling to 40-60 deg.C, adding polyether epoxy resin, and mixing;
(5) adding carboxyl-terminated butadiene-acrylonitrile rubber at 40-60 ℃, and mixing;
(6) and adding an epoxy curing agent and acrylic resin, and mixing to prepare the low-temperature-resistant heat-conducting insulating resin paint suitable for the superconducting insulating material.
6. Use of the low temperature resistant heat conductive insulating resin varnish for superconducting insulation material according to any one of claims 1 to 4 in superconducting insulation material.
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| CN110305298B (en) * | 2019-06-26 | 2021-06-22 | 苏州太湖电工新材料股份有限公司 | Epoxy curing accelerator suitable for epoxy adhesive and preparation method and application thereof |
| CN110194918B (en) * | 2019-06-26 | 2020-07-03 | 苏州太湖电工新材料股份有限公司 | Modified epoxy organic silicon high-thermal-conductivity insulating impregnating varnish and preparation method thereof |
| CN110452563B (en) * | 2019-08-19 | 2021-12-21 | 苏州新材料研究所有限公司 | Preparation method of superconducting tape insulating coating |
| CN112574643B (en) * | 2020-12-16 | 2022-02-11 | 苏州太湖电工新材料股份有限公司 | Flame-retardant water-based insulating paint and preparation method and application thereof |
| CN112795220A (en) * | 2021-01-05 | 2021-05-14 | 上海交通大学 | Low-temperature coating for insulating materials, use and preparation method thereof |
| CN113845775B (en) * | 2021-11-08 | 2022-06-21 | 江南大学 | Preparation method of hyperbranched polymer modified boron nitride heat-conducting and insulating composite material |
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