CN113501917B - Environment-friendly impregnating resin with high heat conductivity coefficient and preparation method and application thereof - Google Patents
Environment-friendly impregnating resin with high heat conductivity coefficient and preparation method and application thereof Download PDFInfo
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- CN113501917B CN113501917B CN202110872341.8A CN202110872341A CN113501917B CN 113501917 B CN113501917 B CN 113501917B CN 202110872341 A CN202110872341 A CN 202110872341A CN 113501917 B CN113501917 B CN 113501917B
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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 application discloses an environment-friendly impregnating resin with high heat conductivity coefficient, and 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; environment-friendly reactive diluent: 20-50 parts; zirconium phosphate: 5-60 parts; and (3) an initiator: 1-2 parts; auxiliary agent: 0.01 to 2 parts. The preparation method of the environment-friendly impregnating resin comprises the following steps: step S1: premixing unsaturated polyester resin, zirconium phosphate and environment-friendly reactive diluent for 10-40 minutes at low speed to obtain a premixed intermediate; step S2: and (3) after the premixed intermediate is dispersed for 10 to 40 minutes at high speed, adding an initiator and other auxiliary agents, uniformly stirring and defoaming to obtain the final impregnating resin. The environment-friendly impregnating resin with high heat conductivity not only enhances the heat conductivity of the environment-friendly impregnating resin by improving the filler, but also has the advantages of low viscosity and high heat conductivity on the basis of ensuring environment friendliness.
Description
Technical Field
The application belongs to the field of synthetic resin, and particularly relates to an environment-friendly impregnating resin with high heat conductivity, a preparation method and application thereof.
Background
Currently, the main direction of development of impregnating resins is the environmentally friendly high performance products. In the face of increasingly higher performance requirements, particularly heat resistance, a very effective approach is to increase the thermal conductivity of the impregnating varnish product, thereby achieving the objective of reducing the temperature rise of the electrical components. In order to increase the thermal conductivity of the impregnating resin, it is common practice to add fillers 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 diluents are mainly acrylic esters, methacrylic esters, diallyl phthalate and the like; (3) The filler mainly comprises aluminum oxide, silicon oxide, boron nitride and the like; (4) Adjuvants, including, but not limited to, curing agents, inhibitors, wetting and dispersing agents, leveling agents, and defoamers, and the like.
The high-energy density motor represented by the new energy automobile motor has higher requirement 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 quick, the temperature rise of the system is low, and the service life of the motor can be further prolonged.
Manufacturing difficulty of environment-friendly high-heat-conductivity impregnating resin:
1. the environment-friendly impregnating resin has high viscosity, the viscosity is further increased after the filler is added, the conventional process of the client cannot be met in the later period, and the use is difficult.
2. Storage stability, the filler added is liable to precipitate and precipitate at a later stage, becoming heterogeneous, i.e. its shelf life is very short.
The common heat-conducting impregnating resins in domestic markets are of two types, and styrene is used as a diluent for low-viscosity finished products, so that the styrene has heavy taste and large volatilization, and cannot meet the environmental protection requirement. Another class of products has too high a viscosity but poor stability. The main reason is that the amount of filler (weight percentage) to be used needs to be increased in order to achieve the heat conduction effect, but the viscosity of the finished product increases rapidly with the increase of the amount, and the storage stability further decreases.
The inventor finds that the conventional filler can not 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 qualified finished product is difficult to manufacture.
Secondly, the heat conducting filler in the current products is commonly alumina and silicon oxide, and in addition, boron nitride, montmorillonite, aluminum nitride and the like, and various fillers generally have various shapes, particle sizes and distributions and surface treatments.
Third, other materials, due to their high price or poor performance, cannot be used to make up the use of thermally insulating impregnating resins.
In the prior art, for example: chinese patent publication No. CN102617886a, publication No. 2012, month 8 and day 1, entitled "application of heat conductive filler in VPI vacuum pressure impregnation resin" discloses an application of heat conductive filler in VPI vacuum pressure impregnation resin. In the technical solution disclosed in this patent document, the thermally conductive filler is boron nitride having a hexagonal structure.
Also for example: chinese patent document with publication number CN101768404a, publication date of 2010, 7 months and 7 days, named "an impregnating varnish and method for preparing same" discloses an impregnating varnish and method for preparing same. In the technical scheme disclosed in the patent document, two compound fillers of silicon micropowder and aluminum nitride are used for preparing the impregnating varnish with high thermal conductivity.
In research of nano SiO 2/BNSs modified organosilicon epoxy high thermal conductivity insulating impregnating varnish (national heat conductivity insulating material and application thematic workshop, 2017-07), a high thermal conductivity insulating impregnating varnish of silicon oxide and boron nitride compounded organosilicon epoxy is researched.
Based on this, it is desired to obtain an environmentally friendly heat conductive impregnating resin which has the advantages of low viscosity and high heat conductivity on the basis of ensuring environmental protection by improving the filler in the component system. In addition, the environment-friendly heat-conducting impregnating resin also has the advantages of taking the performance advantages of the material into consideration and the convenience in use.
Disclosure of Invention
Aiming at the defects of the prior art, the application provides an environment-friendly impregnating resin with high heat conductivity coefficient, application and a preparation method thereof. The environment-friendly impregnating resin with high heat conductivity not only enhances the heat conductivity of the environment-friendly impregnating resin by improving the filler, but also has low cost. In addition, the environment-friendly heat conduction impregnating resin has the advantages of low viscosity and high heat conduction on the basis of ensuring environment friendliness. In addition, the environment-friendly heat-conducting impregnating resin also has the advantages of taking the performance advantages of the material into consideration and the convenience in use.
In order to achieve the above object, the present application is realized by the following technical scheme:
in a first aspect, the application provides an environment-friendly impregnating resin with high thermal conductivity, which comprises the following components in parts by weight:
unsaturated polyester resin: 20-50 parts;
environment-friendly reactive diluent: 20-50 parts;
zirconium phosphate: 5-60 parts;
and (3) an initiator: 1-2 parts;
and (3) auxiliary agents: 0.01 to 2 parts.
The thermal conductivity coefficients of different substances are different, the thermal conductivity coefficient of the unsaturated polyester impregnating resin without the filler is 0.23W/(m.K), and the thermal conductivity coefficient of the environment-friendly impregnating resin is more than 0.30W/(m.K). In the technical scheme of the application, the functions of the components are as follows:
unsaturated polyester resin: the unsaturated polyester resin provides the mechanical and chemical properties of the base of the material.
Environment-friendly reactive diluent: the environment-friendly reactive diluent is a solvent and a cross-linking agent. Can dissolve unsaturated polyester resin to make its double bonds produce copolymerization reaction so as to obtain the invented product.
Zirconium phosphate: zirconium phosphate is used as filler here, when the amount is small, the zirconium phosphate surface is wrapped by a polymer, the system heat conductivity is determined by the heat conductivity of a polymer matrix, and the heat conductivity coefficient is not much different from that when the zirconium phosphate filler is not added. When the amount of the filler is continuously increased to a certain critical value, the fillers are contacted with each other to form a heat conducting network chain structure in the system, and at the moment, heat flow is transferred along a heat conducting network with minimum heat resistance, so that the heat conducting property of the material is greatly improved.
Preferably, the environmentally friendly reactive diluent is selected from: one of acrylic esters, methacrylic esters and diallyl phthalate.
More preferably, the acrylic acid esters are preferably hexanediol diacrylate, dipropylene glycol diacrylate, 1,4 butanediol diacrylate, and the methacrylic acid esters are preferably 1,4 butanediol dimethacrylate, triethylene glycol dimethacrylate.
Preferably, the zirconium phosphate is 20 to 40 parts by weight.
Preferably, the initiator is selected from: one of peroxide initiator, azo initiator and carbon-carbon bond initiator.
The peroxide initiator is preferably dicumyl peroxide or tert-butyl perbenzoate;
the azo initiator is preferably azo-iso Ding Qingji formamide; the carbon-carbon bond initiator is preferably silylated tetraphenyl-1, 2-ethylene glycol.
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 application provides a method for preparing the above-mentioned environmentally friendly impregnating resin, comprising the steps of:
step S1: premixing unsaturated polyester resin, zirconium phosphate and environment-friendly reactive diluent for 10-40 minutes at low speed to obtain a premixed intermediate;
step S2: and (3) after the premixed intermediate is dispersed for 10 to 40 minutes at high speed, adding an initiator and other auxiliary agents, uniformly stirring and defoaming to obtain the final impregnating resin.
Preferably, in the step S1, the low speed is 50 to 1000 rpm;
in the step S2, the high speed is 1000 to 6000 rpm.
In a third aspect, the present application provides a use of the above-described environmentally friendly impregnating resin for impregnating electrical equipment.
Preferably, the motor apparatus includes at least one of a motor stator, a rotor, and a transformer;
the dipping treatment comprises at least one of dipping, drip dipping, roll dipping, vacuum dipping and vacuum pressure dipping.
It should be noted that, in the use process of the environment-friendly impregnating resin, curing treatment can be performed after impregnation.
The curing means includes ultraviolet radiation curing and/or thermal curing means.
Compared with the prior art, the application has the following beneficial effects:
(1) The environment-friendly heat conduction impregnating resin has the advantages of low viscosity and high heat conduction on the basis of ensuring environment friendliness.
(2) The environment-friendly heat-conducting impregnating resin also has the advantages of taking the performance advantages of the material into consideration and the convenience in use.
(3) According to the application, zirconium phosphate is used as a filler in the hot-dipping resin for the first time, so that the heat conduction performance of the environment-friendly hot-dipping resin is greatly improved, and the heat conduction test values are all higher than 0.3W (m.K).
Detailed Description
The present application will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present application, but are not intended to limit the application in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present application.
Examples 1 to 20 and comparative examples 1 to 7 were prepared by the following steps:
step S1: premixing unsaturated polyester resin, zirconium phosphate and environment-friendly reactive diluent for 10-40 minutes at low speed according to the component proportions shown in table 1 to obtain a premixed intermediate;
step S2: and (3) after the premixed intermediate is dispersed for 10 to 40 minutes at high speed, adding an initiator and other auxiliary agents, uniformly stirring and defoaming to obtain the final impregnating resin. The specific process parameters for each example are shown in table 2.
Among these, the polymerization inhibitor used is one of alkylated phenols, hydroquinone and benzoquinone, and 2, 4-di-tert-butylphenol or methyl hydroquinone is commonly used for alkylated phenols.
The auxiliary agent can also comprise other auxiliary agents such as leveling agent, defoamer and the like, and the types and the like are not limited. Those skilled in the art can add the leveling agent EFKA 3777, BYK-370 and BYK-392 of Pick chemical Co., ltd, AFCONA-3773 of Efaku chemical Co., ltd, etc. as required, and the defoaming agent selected from TEG0 900, AFCONA-3773 of Efaku chemical Co., ltd, BYK-057 of Pick chemical Co., ltd, etc.
It is well known to 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 alcoholAfter the addition of the unsaturated dibasic acid (or anhydride) in portions, the mixture is heated to 180-230 ℃ typically stepwise with stirring. After each index reaches the requirement, the reaction mixture is cooled down to obtain the required unsaturated polyester resin.
The structure of the unsaturated polyester resin can be illustrated by the following formula:
wherein x and y represent the polymerization degree of each chain segment; r is R 1 、R 2 、R 3 Respectively the skeleton structures except the active end groups in the dihydric alcohol, the unsaturated dibasic acid (anhydride) and the saturated dibasic acid (anhydride). R is R 1 、R 2 、R 3 The unsaturated polyester resin molecular chain has rich structure and different properties, 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) may be selected from: maleic anhydride, fumaric acid.
Saturated dibasic acids (anhydrides) may be selected: 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 resins used were synthesized from neopentyl glycol, maleic anhydride, phthalic anhydride, x and y each ranging from 3 to 8.
It should be noted that the content of the solvent in the auxiliary agent in the whole system is low, the influence on the system is negligible, and the solid content of the auxiliary agent in each manufacturer is not consistent, so the auxiliary agent is measured by the amount of solid solute in table 1.
Table 1 (the mass unit of each component in Table 1 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 criteria: hardness is according to ISO 868; bond strength according to IEC 61033, method a (units, mPas); thermal conductivity is in accordance with ASTM D5470-17; volume resistivity was according to IEC 60093; gel time was in accordance with DIN 46448; the test results are shown in table 3:
table 3, examples 1 to 20 and comparative examples 1 to 7 test data
As can be seen from the data in Table 3, the D hardness after curing was 78 or more, which indicates that the curing was good for each of the examples and comparative examples, and the measured correlation results were of comparative significance, as well as the volume resistivity test results. In examples 1-6, the thermal conductivity increased with increasing zirconium phosphate content, but the viscosity of the finished product in example 6 increased rapidly, with some difficulty in application.
When the unsaturated polyester resin content in examples 7 to 10 is more than 35 parts, the heat conductivity becomes low; below 35 parts, the viscosity of the finished product becomes large.
In examples 11-12, the environment-friendly reactive diluent content was too high and the thermal conductivity was low; too low, the viscosity of the finished product becomes large.
In general, the gel time is within 5-7 minutes at 120 ℃, which is suitable to balance the requirements of rapid curing and stable storage of the resin. Too little or too much initiator in examples 13-14 is liable to cause problems in one aspect thereof.
Examples 15-16 and example 5 optimize the adjuvant content, which has a large impact on the storage stability of the finished product, and can be manifested in terms of gel time.
In examples 17-18, triethylene glycol dimethacrylate was softer after curing, had lower hardness, diallyl phthalate was less reactive and the gel time was relatively longer.
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 heat conduction property is poor.
In comparative examples 3 to 4, when the content of zirconium phosphate is too low, the heat conductive property is poor; excessive filler, high viscosity and poor dispersing effect.
Comparative examples 5, 6, compared to example 5, the same proportions of silica and alumina filler give a finished product having a higher viscosity than zirconium phosphate and a lower thermal conductivity than zirconium phosphate.
Comparative example 7 contained no filler and had the lowest dilution of heat conduction, which was only 0.23W/m.K.
The above embodiments are merely illustrative of the principles of the present application and its effectiveness, and are not intended to limit the application. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the application. Accordingly, it is intended that all equivalent modifications and variations of the application be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure. It should be noted that the prior art part in the protection scope of the present application is not limited to the embodiments given in the present document, and all prior art that does not contradict the scheme of the present application, including but not limited to the prior patent document, the prior publication, the prior disclosure, the use, etc., can be included in the protection scope of the present application.
In addition, the combination of the features described in the present application is not limited to the combination described in the claims 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 contradiction occurs between them.
The foregoing describes specific embodiments of the present application. It is to be understood that the application is not limited to the particular embodiments described above, and that various changes or modifications may be made by those skilled in the art within the scope of the appended claims without affecting the spirit of the application. The embodiments of the application and the features of the embodiments may be combined with each other arbitrarily without conflict.
Claims (9)
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;
environment-friendly reactive diluent: 20-50 parts;
zirconium phosphate: 5-60 parts;
and (3) an initiator: 1-2 parts;
and (3) auxiliary agents: 0.01 to 2 parts;
the structure of the unsaturated polyester resin is illustrated below:
wherein x isY represents the degree of polymerization of each segment; r is R 1 、R 2 、R 3 Respectively a framework structure except for an active end group in dihydric alcohol, unsaturated dibasic acid (anhydride) and saturated dibasic acid (anhydride);
the dihydric alcohol can be selected from: propylene glycol, ethylene glycol, diethylene glycol, dipropylene glycol, neopentyl glycol;
the unsaturated dibasic acid (anhydride) may be selected from: maleic anhydride, fumaric acid;
saturated dibasic acids (anhydrides) may be selected: phthalic anhydride, isophthalic acid, oxalic acid.
2. The environmentally friendly impregnating resin of claim 1 wherein said environmentally friendly reactive diluent is selected from the group consisting of: one of acrylic esters, methacrylic esters and diallyl phthalate.
3. The high thermal conductivity environmental protection impregnating resin according to claim 1, wherein the weight portion of zirconium phosphate is 20-40.
4. The high thermal conductivity environmentally friendly impregnating resin of claim 1 wherein said initiator is selected from the group consisting of: a peroxide initiator, an azo initiator and a carbon-carbon bond initiator.
5. The high thermal conductivity environmentally friendly impregnating resin of claim 1, wherein said adjuvants comprise at least one of polymerization inhibitors, leveling agents and defoamers.
6. A method for preparing the environmentally friendly impregnating resin with high thermal conductivity according to any one of claims 1 to 5, comprising the steps of:
step S1: premixing unsaturated polyester resin, zirconium phosphate and environment-friendly reactive diluent for 10-40 minutes at low speed to obtain a premixed intermediate;
step S2: and (3) after the premixed intermediate is dispersed for 10 to 40 minutes at high speed, adding an initiator and an auxiliary agent, uniformly stirring and defoaming to obtain the final impregnating resin.
7. The method for preparing an environmentally friendly impregnating resin with high thermal conductivity according to claim 6, wherein in the step S1, the low speed is 50 to 1000 rpm; in the step S2, the high speed is 1000 to 6000 rpm.
8. Use of the environmentally friendly impregnating resin with high thermal conductivity according to any one of claims 1 to 5, wherein the environmentally friendly impregnating resin is used in impregnating treatment of electrical machinery.
9. The use of the high thermal conductivity environmentally friendly impregnating resin according to claim 8, wherein said motor apparatus comprises at least one of a motor stator, a rotor and a transformer;
the dipping treatment includes at least one of dipping, drip dipping, roll dipping, vacuum dipping, and vacuum pressure dipping.
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| CN116032048A (en) * | 2021-10-26 | 2023-04-28 | 华为数字能源技术有限公司 | Method for improving heat dissipation capacity of oil-cooled motor, insulating paint and preparation method thereof |
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| JP2012224518A (en) * | 2011-04-20 | 2012-11-15 | Toagosei Co Ltd | Method for producing layered zirconium phosphate |
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| JP2008137849A (en) * | 2006-12-01 | 2008-06-19 | Akebono Brake Ind Co Ltd | Resin impregnated porous filler |
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| JP2012224518A (en) * | 2011-04-20 | 2012-11-15 | Toagosei Co Ltd | Method for producing layered zirconium phosphate |
| CN102225986A (en) * | 2011-04-21 | 2011-10-26 | 苏州巨峰电气绝缘系统股份有限公司 | Environmentally-friendly type solvent-free impregnating resin and preparation method thereof |
| CN103524875A (en) * | 2013-09-25 | 2014-01-22 | 吴江市天源塑胶有限公司 | Anti-aging thermal conductive plastic |
| CN109912749A (en) * | 2019-03-01 | 2019-06-21 | 江门市德山复合材料科技有限公司 | A kind of selfreparing unsaturated polyester composite and preparation method thereof for 3D printing |
| CN111574934A (en) * | 2020-05-19 | 2020-08-25 | 常州百佳年代薄膜科技股份有限公司 | Nano heat-conducting adhesive film, microcapsule, preparation method of microcapsule, photovoltaic module and detection method |
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