CN113501917A - Environment-friendly impregnating resin with high thermal conductivity coefficient and preparation method and application thereof - Google Patents
Environment-friendly impregnating resin with high thermal conductivity coefficient and preparation method and application thereof Download PDFInfo
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- CN113501917A CN113501917A CN202110872341.8A CN202110872341A CN113501917A CN 113501917 A CN113501917 A CN 113501917A CN 202110872341 A CN202110872341 A CN 202110872341A CN 113501917 A CN113501917 A CN 113501917A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/01—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to unsaturated polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/328—Phosphates of heavy metals
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Abstract
The invention discloses an environment-friendly impregnating resin with high heat conductivity coefficient, a preparation method and application thereof. The environment-friendly impregnating resin comprises the following components in parts by weight: unsaturated polyester resin: 20-50 parts of a solvent; environmentally friendly reactive diluents: 20-50 parts of a solvent; zirconium phosphate: 5-60 parts; initiator: 1-2 parts; auxiliary agent: 0.01-2 parts. The preparation method of the environment-friendly impregnating resin comprises the following steps: step S1: premixing unsaturated polyester resin, zirconium phosphate and an environment-friendly reactive diluent at a low speed for 10-40 minutes to obtain a premixed intermediate; step S2: and dispersing the premixed intermediate at a high speed for 10-40 minutes, adding an initiator and other auxiliaries, uniformly stirring and defoaming to obtain the final impregnating resin. The environment-friendly impregnating resin with high thermal conductivity coefficient not only enhances the thermal conductivity coefficient of the environment-friendly impregnating resin by improving the filler, but also has low cost, and has the advantages of low viscosity and high thermal conductivity on the basis of ensuring environment protection.
Description
Technical Field
The invention belongs to the field of synthetic resin, and particularly relates to environment-friendly impregnating resin with high heat conductivity coefficient, and a preparation method and application thereof.
Background
Currently, the main development direction of impregnating resins is the environmentally friendly high performance products. In the face of ever-increasing performance requirements, particularly heat resistance, a very effective approach has been to increase the thermal conductivity of the impregnated enamel product in order to reduce the temperature rise of the electrical components. In order to increase the thermal conductivity of the impregnating resin, it is common practice to add a filler to the impregnating resin. Generally, the main components of the environment-friendly heat-conducting impregnating resin comprise (1) unsaturated polyester (including unsaturated polyester imide) resin; (2) the environment-friendly reactive diluent mainly comprises acrylate, methacrylate, diallyl phthalate and the like; (3) fillers, mainly alumina, silica, boron nitride and the like; (4) and the auxiliary agents comprise but are not limited to curing agents, polymerization inhibitors, wetting and dispersing agents, flatting agents, defoaming agents and the like.
The high-energy-density motor represented by the new energy automobile motor has higher requirements on the heat conductivity coefficient of the impregnating resin, the heat conductivity coefficient of the impregnating resin is high, the heat transfer of the motor is fast, the temperature rise of a system is low, and the service life of the motor can be further prolonged.
The difficulty in manufacturing the environment-friendly high-thermal-conductivity impregnating resin is as follows:
1. the viscosity of the environment-friendly impregnating resin is high, the viscosity is further increased after the filler is added, the conventional process of a client cannot be met in the later stage, and the use is difficult.
2. The storage stability, the added filler is easy to separate out and precipitate in the later period, and becomes heterogeneous, that is to say the shelf life is very short.
The heat-conducting impregnating resins commonly used in domestic markets are of two types, styrene is used as a diluent in one type of low-viscosity finished products, the styrene is heavy in taste and large in volatilization, and the environmental protection requirement cannot be met. The other type of product has too high a viscosity but poor stability. The reason is mainly because the amount (weight percentage) of the filler used needs to be increased in order to pursue the heat conduction effect, but the viscosity of the finished product rapidly increases with the increase of the amount used, and the storage stability further decreases.
Through the research of the inventor, the conventional filler cannot overcome the defects of the prior art in the aspect ratio, and the reason is based on the following points:
in the first, grinding or high-speed dispersing process, the pigment ratio is in a certain range, and the dispersed product can be stable, so that the product is difficult to be made into a qualified finished product.
Second, the heat conductive fillers in such products are usually alumina and silica, and in addition, boron nitride, montmorillonite, aluminum nitride, etc. each filler usually has various shapes, particle sizes and distributions, and surface treatment.
Third, other materials cannot be used to achieve the use of the thermal insulating impregnating resin because of their high price and poor performance.
In the prior art, for example: chinese patent publication No. CN102617886A, published as 2012, 8/1/2012, entitled "application of thermally conductive filler in VPI vacuum pressure impregnation resin" discloses an application of thermally conductive filler in VPI vacuum pressure impregnation resin. In the technical solution disclosed in this patent document, hexagonal boron nitride is used as the heat conductive filler.
Another example is: chinese patent publication No. CN101768404A, published as 7.7.2010, entitled "a dipping insulating varnish and a preparation method thereof", discloses a dipping insulating varnish and a preparation method thereof. In the technical scheme disclosed in the patent document, two compound fillers of silicon micropowder and aluminum nitride are used for preparing the impregnating insulating paint with high thermal conductivity.
In the research on nano SiO2/BNNSs modified organosilicon epoxy high-thermal-conductivity insulating impregnating varnish (national research and discussion on heat-conducting and insulating materials and application special topics, 2017-07), the high-thermal-conductivity insulating impregnating varnish of silicon oxide and boron nitride compounded organosilicon epoxy is researched.
Based on the above, it is desirable to obtain an environment-friendly heat-conducting impregnating resin, which has the advantages of low viscosity and high heat conductivity on the basis of ensuring environment friendliness by improving fillers in a component system. In addition, the environment-friendly heat-conducting impregnating resin also has the advantages of taking the performance advantage of the material into consideration and the advantage of convenient use.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an environment-friendly impregnating resin with high heat conductivity coefficient, an application and a preparation method thereof. The environment-friendly impregnating resin with high thermal conductivity coefficient not only enhances the thermal conductivity coefficient of the environment-friendly impregnating resin, but also has low cost by improving the filler. In addition, the environment-friendly heat-conducting impregnating resin has the advantages of low viscosity and high heat conductivity on the basis of ensuring the environment-friendly property. In addition, the environment-friendly heat-conducting impregnating resin also has the advantages of taking the performance advantage of the material into consideration and the advantage of convenient use.
In order to achieve the purpose, the invention is realized by the following technical scheme:
in a first aspect, the invention provides an environment-friendly impregnating resin with a high thermal conductivity, which comprises the following components in parts by weight:
unsaturated polyester resin: 20-50 parts of a solvent;
environmentally friendly reactive diluents: 20-50 parts of a solvent;
zirconium phosphate: 5-60 parts;
initiator: 1-2 parts;
and an auxiliary agent: 0.01-2 parts.
The thermal conductivity of different substances is different, the thermal conductivity of the unsaturated polyester impregnating resin without the filler is 0.23W/(m.K), and the thermal conductivity of the environment-friendly impregnating resin is more than 0.30W/(m.K). In the technical scheme of the invention, the effects of the components are as follows:
unsaturated polyester resin: the unsaturated polyester resin provides the basic mechanical and chemical properties of the material.
Environmentally friendly reactive diluents: the environment-friendly reactive diluent is a solvent and a crosslinking agent. Can dissolve unsaturated polyester resin to make the double bonds of the unsaturated polyester resin generate copolymerization reaction to obtain a body type product.
Zirconium phosphate: zirconium phosphate is used as a filler, when the amount is small, the surface of the zirconium phosphate is wrapped by the polymer, the thermal conductivity of the system is determined by the thermal conductivity of the polymer matrix, and the thermal conductivity is not much different from that of the case that the zirconium phosphate filler is not added. When the amount of the filler is continuously increased to a certain critical value, the fillers are mutually contacted to form a heat conduction network chain structure in the system, and at the moment, heat flow is transmitted along the heat conduction network with the minimum heat resistance, so that the heat conduction performance of the material is greatly improved.
Preferably, the environmentally friendly reactive diluent is selected from: one of acrylates, methacrylates, and diallyl phthalate.
More preferably, the acrylate is preferably hexanediol diacrylate, dipropylene glycol diacrylate, 1, 4-butanediol diacrylate, and the methacrylate is preferably 1, 4-butanediol dimethacrylate, triethylene glycol dimethacrylate.
Preferably, the weight part of the zirconium phosphate is 20-40 parts.
Preferably, the initiator is selected from: one of a peroxide initiator, an azo initiator and a carbon-carbon bond initiator.
The peroxide initiator is preferably dicumyl peroxide or tert-butyl perbenzoate;
the azo initiator is preferably azoisobutyryl cyano formamide; the carbon-carbon bond initiator is preferably silylated tetraphenyl-1, 2-ethanediol.
Preferably, the auxiliary agent includes at least one of a polymerization inhibitor, a leveling agent, and a defoaming agent.
In a second aspect, the present invention provides a method for preparing the above-mentioned environment-friendly impregnating resin, which comprises the following steps:
step S1: premixing unsaturated polyester resin, zirconium phosphate and an environment-friendly reactive diluent at a low speed for 10-40 minutes to obtain a premixed intermediate;
step S2: and dispersing the premixed intermediate at a high speed for 10-40 minutes, adding an initiator and other auxiliaries, uniformly stirring and defoaming to obtain the final impregnating resin.
Preferably, in the step S1, the low speed is 50-1000 r/S;
in the step S2, the high speed is 1000-6000 rpm.
In a third aspect, the invention provides a use of the above-mentioned environment-friendly impregnating resin for impregnating motor equipment.
Preferably, the motor apparatus includes at least one of a motor stator, a rotor, and a transformer;
the impregnation treatment includes at least one of immersion, drip immersion, roll immersion, vacuum immersion, and vacuum pressure immersion.
The environment-friendly impregnating resin can be cured after impregnation in the using process.
The curing means includes ultraviolet radiation curing and/or thermal curing means.
Compared with the prior art, the invention has the following beneficial effects:
(1) the environment-friendly heat-conducting impregnating resin disclosed by the invention has the advantages of low viscosity and high heat conductivity on the basis of ensuring environment friendliness.
(2) The environment-friendly heat-conducting impregnating resin also has the advantages of taking the performance advantage of the material into consideration and being convenient to use.
(3) According to the invention, the zirconium phosphate is used as the filler in the hot dipping resin for the first time, so that the heat conductivity of the environment-friendly hot dipping resin is greatly improved, and the heat conductivity test values are all higher than 0.3W (m.K).
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The examples 1 to 20 and the comparative examples 1 to 7 were prepared by the following steps:
step S1: premixing unsaturated polyester resin, zirconium phosphate and an environment-friendly reactive diluent at a low speed for 10-40 minutes according to the component ratio shown in Table 1 to obtain a premixed intermediate;
step S2: and dispersing the premixed intermediate at a high speed for 10-40 minutes, adding an initiator and other auxiliaries, uniformly stirring and defoaming to obtain the final impregnating resin. The specific process parameters of each example are shown in table 2.
Wherein the polymerization inhibitor is one of alkylated phenol, hydroquinone and benzoquinone, and the alkylated phenol is usually 2, 4-di-tert-butyl phenol or methyl hydroquinone.
The auxiliary agent may also include leveling agent, defoaming agent and other auxiliary agents, and the kind and the like are not limited. The leveling agent EFKA 3777, BYK-370 and BYK-392 from Bick chemical Co., Ltd, AFCONA-3773 from Effolcon chemical Co., Ltd, etc., the antifoaming agent selected from Didi high TEG 0900, AFCONA-3773 from Effolcon chemical Co., Ltd, BYK-057 from Bick chemical Co., Ltd, etc. can be added by those skilled in the art according to production requirements.
It is a general knowledge of those skilled in the art how to synthesize unsaturated polyester resins. During the synthesis, the progress of the reaction can be followed by measuring the acid number of the mixture and the viscosity of the test resin. During the reaction, dihydric alcohol is added
After batchwise addition with the unsaturated dibasic acid (or anhydride) and the saturated dibasic acid (or anhydride), the mixture is generally heated gradually to a temperature of 180 ℃ and 230 ℃ with stirring. After each index meets the requirement, the reaction mixture is cooled down to obtain the required unsaturated polyester resin.
The structure of the unsaturated polyester resin can be represented by the following formula:
wherein x and y represent eachThe degree of polymerization of the mer; r1、R2、R3Respectively are skeleton structures except active end groups in dihydric alcohol, unsaturated dibasic acid (anhydride) and saturated dibasic acid (anhydride). R1、R2、R3The unsaturated polyester resin has rich molecular chains and different performances, and can meet various use requirements.
The dihydric alcohol can be selected from: propylene glycol, ethylene glycol, diethylene glycol, dipropylene glycol, neopentyl glycol, hydrogenated bisphenol a, bisphenol a derivatives, dibromoneopentyl glycol, and the like.
The unsaturated dibasic acid (anhydride) can be selected from: maleic anhydride, fumaric acid.
Saturated dibasic acids (anhydrides) can be selected from: phthalic anhydride, isophthalic acid, oxalic acid, tetrachlorophthalic anhydride, tetrabromophthalic anhydride, tetrahydrophthalic anhydride, and the like.
In examples 1 to 20 and comparative examples 1 to 7, the unsaturated polyester resin was synthesized from neopentyl glycol, maleic anhydride, and phthalic anhydride, and x and y were in the range of 3 to 8.
It should be noted that the solvent content of the adjuvant is very low in the whole system, the influence on the system is negligible, and the solid contents of the adjuvant are not consistent from manufacturer to manufacturer, so the adjuvant is measured by the solid solute amount in table 1.
Table 1, (in Table 1, the unit of mass of each component is g)
Table 2, examples 1 to 20 and comparative examples 1 to 7 relate to specific process parameters
Performance effect verification：
Examples 1 to 20 and comparative examples 1 to 7 were tested according to the relevant test standards: hardness according to ISO 868; bond strength according to IEC 61033, method a (units, mPas); thermal conductivity according to ASTM D5470-17; volume resistivity in accordance with IEC 60093; gel time to DIN 46448; the test results are shown in table 3:
table 3, examples 1-20 and comparative examples 1-7 test data
As can be seen from the data in Table 3, the cured D hardness was 78 or higher, indicating that the curing was good for each of the examples and comparative examples, the results obtained were comparative and confirmed by the volume resistivity test. In examples 1 to 6, the thermal conductivity increased with the increase in the content of zirconium phosphate, but the viscosity of the final product in example 6 increased rapidly and was difficult to apply.
When the content of the unsaturated polyester resin is more than 35 parts in examples 7 to 10, the thermal conductivity becomes low; when the amount is less than 35 parts, the viscosity of the final product becomes high.
In examples 11-12, the environmentally friendly reactive diluent was too high and the thermal conductivity was low; too low, the viscosity of the finished product becomes high.
Generally, the gel time is within 5-7 minutes at 120 ℃, which is suitable for balancing the requirements of quick curing and stable storage of the resin. Too little or too much initiator in examples 13-14 is likely to cause problems in one aspect.
Examples 15-16 and example 5 optimization of the adjuvant content has a major impact on the storage stability of the finished product, as can be seen in gel time.
In examples 17-18, the triethylene glycol dimethacrylate cured was soft, had low hardness, had low reactivity with diallyl phthalate, and had a relatively long gel time.
The initiators selected in examples 19-20 have low decomposition temperatures and short gel times, which are detrimental to the storage and stability of the finished product.
In comparative example 1, the resin content was too low, and the filler could not be uniformly dispersed in the resin.
In comparative example 2, when the resin content is too high, the proportion of the filler in the finished product is too low, and the thermal conductivity is not good.
In comparative examples 3 to 4, when the content of zirconium phosphate was too low, the heat conductivity was not good; too much filler, high viscosity and poor dispersion effect.
Comparative examples 5 and 6 compare example 5, with the same proportions of silica and alumina filler, the final product has a higher viscosity and poorer thermal conductivity than zirconium phosphate.
Comparative example 7, which contained no filler, had the lowest thermally conductive dilution of 0.23W/m.k.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention. It should be noted that the prior art in the protection scope of the present invention is not limited to the examples given in the present application, and all the prior art which is not inconsistent with the technical scheme of the present invention, including but not limited to the prior patent documents, the prior publications and the like, can be included in the protection scope of the present invention.
In addition, the combination of the features in the present application is not limited to the combination described in the claims of the present application or the combination described in the embodiments, and all the features described in the present application may be freely combined or combined in any manner unless contradictory to each other.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (10)
1. The environment-friendly impregnating resin with high thermal conductivity is characterized by comprising the following components in parts by weight:
unsaturated polyester resin: 20-50 parts of a solvent;
environmentally friendly reactive diluents: 20-50 parts of a solvent;
zirconium phosphate: 5-60 parts;
initiator: 1-2 parts;
and an auxiliary agent: 0.01-2 parts.
2. The high thermal conductivity, environmentally friendly infusion resin of claim 1, wherein the unsaturated polyester resin comprises an unsaturated polyester imide.
3. The high thermal conductivity eco-friendly impregnating resin according to claim 1, wherein said eco-friendly reactive diluent is selected from the group consisting of: one of acrylates, methacrylates, and diallyl phthalate.
4. The environmentally friendly impregnating resin with high thermal conductivity as claimed in claim 1, wherein the amount of zirconium phosphate is 20-40 parts by weight.
5. The high thermal conductivity eco-friendly impregnating resin according to claim 1, wherein said initiator is selected from the group consisting of: peroxide initiator, azo initiator and carbon-carbon bond initiator.
6. The high thermal conductivity environment-friendly impregnating resin according to claim 1, wherein said auxiliary agent comprises at least one of polymerization inhibitor, leveling agent and defoaming agent.
7. The preparation method of the environment-friendly impregnating resin with high thermal conductivity according to any one of claims 1-6, characterized by comprising the following steps:
step S1: premixing unsaturated polyester resin, zirconium phosphate and an environment-friendly reactive diluent at a low speed for 10-40 minutes to obtain a premixed intermediate;
step S2: and dispersing the premixed intermediate at a high speed for 10-40 minutes, adding an initiator and an auxiliary agent, uniformly stirring and defoaming to obtain the final impregnating resin.
8. The method for preparing the environmentally friendly impregnating resin with high thermal conductivity as claimed in claim 7, wherein in the step S1, the low speed is 50-1000 rpm; in the step S2, the high speed is 1000-6000 rpm.
9. Use of the environmentally friendly impregnating resin with high thermal conductivity according to any one of claims 1 to 6, wherein the environmentally friendly impregnating resin is used in the impregnating treatment of motor equipment.
10. Use of the environmentally friendly impregnating resin with high thermal conductivity according to claim 9, wherein said electrical machine equipment comprises at least one of a stator, a rotor and a transformer of an electrical machine;
the impregnation treatment includes at least one of immersion, drip immersion, roll immersion, vacuum immersion, and vacuum pressure immersion.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4175126A3 (en) * | 2021-10-26 | 2023-06-28 | Huawei Digital Power Technologies Co., Ltd. | Method for improving heat dissipation capability of oil-cooled motor, insulation paint, and method for manufacturing insulation paint |
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