CN107652933B - Nanoscale single-component tough epoxy compound for bonding magnetic cores and preparation method thereof - Google Patents
Nanoscale single-component tough epoxy compound for bonding magnetic cores and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nanoscale single-component tough epoxy compound for bonding a magnetic core, which comprises the following components in parts by mass: 100 parts of epoxy resin; 4-30 parts of a curing agent; 4-20% of an accelerator; 0-5 parts of color paste; 3-60 parts of tetrafunctional organic silicon modified epoxy resin; 1-20 parts of nano rubber core-shell particles; 05-0.2% of defoaming agent; 0-0.2 of a coupling agent; 0-0.2 of a dispersant; 1-30 parts of a thixotropic agent; 10-300 parts of filler. The invention also provides a preparation method of the single-component epoxy resin compound. The nanoscale single-component tough epoxy compound for bonding the magnetic core has low viscosity and small addition amount; the functionality is high, so that the bonding can be improved, and the linear expansion coefficient can be reduced; the brittleness of the Si-O bond during curing is not as great as that of C-C bond multifunctional diluents.
Description
Technical Field
The invention relates to an epoxy compound, in particular to a nanoscale single-component tough epoxy compound for bonding a magnetic core and a preparation method thereof, and belongs to the technical field of epoxy resin compounds.
Background
The single-component epoxy resin compound has the advantages of strong adhesive force, low linear expansion coefficient and the like when being used as an adhesive for electronic components such as magnetic cores, transformers and the like, but the cracking of the magnetic cores is easily caused due to large stress during the curing of the epoxy resin. Therefore, it is important to toughen epoxy composites and reduce their linear expansion coefficients.
The epoxy is typically toughened by the addition of a toughening agent. Common toughening agents such as polyurethane modified epoxy, nitrile rubber modified epoxy, dimer acid modified epoxy and the like can improve the toughness of the cured epoxy resin, but have the defects of lowering the glass transition temperature of the cured epoxy resin and influencing the heat resistance of the cured epoxy resin. It is not suitable for some electronic components which need to be used at higher temperature for a long time. Nowadays, core-shell rubbers such as MX-125, MX-154, and MX-257 from Kaneka corporation of Japan, W35 from Wacker corporation of Germany, and EXL-2314, EXL-2655, and EX-2620 from DOW chemical corporation of America are also widely used, and although these tougheners obtained by blending with ordinary epoxy resins have good heat resistance (Tg is hardly decreased), the viscosity is high, and if the amount of the tougheners added is large, it is difficult to add sufficient filler to lower the linear expansion coefficient of the system.
In order to reduce the viscosity, the conventional method is to add a reactive epoxy diluent, but the addition of the diluent also causes problems of lowering of the glass transition temperature and increase of the linear expansion coefficient; in addition, the polyfunctional epoxy diluent has disadvantages of poor diluting effect and increased brittleness of the system, and thus, it is disadvantageous in use.
Disclosure of Invention
The invention aims to provide a nanoscale single-component tough epoxy compound for bonding a magnetic core, which has strong bonding force, low linear expansion coefficient and excellent high and low temperature resistance.
The invention is realized by the following steps:
a nanoscale single-component tough epoxy compound for bonding a magnetic core comprises the following components in parts by mass:
in the invention, the compound is a single-component epoxy resin system, and the epoxy resin is one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, phenolic aldehyde modified epoxy resin or other epoxy resin prepolymers capable of reacting with latent curing agents such as dicyandiamide, modified amine, imidazole and the like.
The curing agent is one or more of dicyandiamide, modified dicyandiamide derivatives, modified microcapsule-coated latent amine curing agents, imidazole and the like. The dosage of the curing agent is 4-30 parts per 100 parts of resin.
The accelerator may be one or more of urea, imidazole, or modified amine. The amount of the accelerator is 4-20 parts per 100 parts of resin.
The tetrafunctional organic silicon modified epoxy resin is a tetrafunctional organic silicon modified epoxy resin (without solvent) obtained by tetramethylhydrogen cyclotetrasiloxane and excessive allyl glycidyl ether under the condition of platinum complex catalysis, and the tetrafunctional organic silicon modified epoxy resin has the following structure:
the nano rubber core-shell particles are used for modifying the tetrafunctional organic silicon modified epoxy resin in a system, the modified tetrafunctional organic silicon modified epoxy resin is used as a toughening agent, and the rubber adopted by the nano rubber core-shell particles is one or more of polybutadiene rubber, organic silicon rubber and styrene butadiene rubber. The rubber particles and the tetrafunctional modified epoxy resin are subjected to blending modification, the amount of the tetrafunctional organic silicon modified epoxy resin is 3-60 parts per 100 parts of the epoxy resin, and the amount of the nano core-shell rubber particles is 1-20 parts per 100 parts of the epoxy resin.
The filler is spherical silicon micropowder with the maximum particle size of less than 0.5 mu m, and the using amount of the filler is 10-300 parts per 100 parts of epoxy resin.
The thixotropic agent is nano calcium carbonate with the grain diameter of less than 0.2 mu m, fumed silica or modified organic bentonite, and the dosage of the thixotropic agent is 1-30 parts per 100 parts of epoxy resin.
The defoaming agent comprises one or more of organosilicon defoaming agent, non-organosilicon defoaming agent and inorganic mineral salt defoaming agent, such as BYK-A530, BYK-A550, BYK-A555, BYK-1710, BYK-141, Tego Airex 931, Tego Airex962 and the like.
The coupling agent comprises one or more silane coupling agents with epoxy groups, such as 3- (2, 3-glycidoxy) propyltrimethoxysilane, 3- (2, 3-glycidoxy) propyltriethoxysilane, 3- (2, 3-glycidoxy) propylmethyldiethoxysilane, etc.
The dispersing agent is one or more of auxiliary agents which can help the system resin and the filler to be uniformly dispersed, and can be not added. Such as BYK-W9010, BYK-W9011, BYK-W9012 and the like.
The color paste is one or more of mixtures of pigment toner and epoxy resin, and is used for toning the compound or not added. The color paste includes white paste, black paste, red paste, green paste, blue paste, etc.
The invention also provides a preparation method of the single-component epoxy resin compound, which comprises the following specific steps:
(1) preparing a toughening agent: premixing the tetrafunctional organic silicon modified epoxy resin and half of the expected addition amount of the nano core-shell rubber particles, gradually adding the rest half of the nano core-shell rubber particles under high-speed or planetary stirring, and then stirring for 10-120 minutes under high-speed or planetary stirring; and then grinding the mixture for 1-3 times by three rollers, and finally defoaming to obtain the composite material.
(2) Preparing a single-component epoxy resin compound: the epoxy resin, the nano rubber toughening agent, the defoaming agent, the coupling agent, the filler and the thixotropic agent are premixed, stirred for 10-120 minutes at high speed or under planetary stirring, then the latent curing agent and the accelerator are added while stirring, stirred for 10-120 minutes at high speed or under planetary stirring and defoamed in vacuum to obtain the epoxy resin nano rubber composite material.
The epoxy resin compound adopts a nano core-shell rubber toughening mode to improve the toughness of a cured product, and the nano core-shell rubber particles are compounded in a mode of blending with organic silicon modified tetra-functional epoxy resin, so that the obtained toughening agent has the following characteristics:
(1) the viscosity is low, and the addition amount is small; (2) the functionality is high, so that the bonding can be improved, and the linear expansion coefficient can be reduced; (3) the brittleness of the Si-O bond during curing is not as great as that of C-C bond multifunctional diluents.
In addition, in order to control the inductance of the two poles of the magnetic material, the epoxy resin of the invention adopts spherical silicon powder with the grain diameter of less than 0.5 μm to reduce the gap between the magnetic materials. Meanwhile, when the spherical silicon micro powder with the particle size of 0.5 mu m is added into the composite, the viscosity is not obviously increased, more dosage can be added to further reduce the linear expansion coefficient of a cured material, the viscosity and the fluidity of the material are convenient to control, and the single-component tough epoxy composite with excellent technological performance is obtained.
Detailed Description
Example 1:
premixing 100g of tetrafunctional organic silicon modified epoxy resin and 12.5g of EXL-2620 nanometer nuclear shell rubber particles of Dow chemical company, gradually adding the rest 12.5g of EXL-2620 nanometer nuclear shell rubber particles under the planetary stirring, and then stirring for 60 minutes under the planetary stirring; and then grinding the mixture for 1 time by three rollers, and finally defoaming to prepare the nano core-shell rubber toughening agent a, wherein the viscosity of the nano core-shell rubber toughening agent a at 25 ℃ is 1360 mPa.s.
Firstly, premixing 100g of E51 bisphenol A epoxy resin, 60g of nano core-shell rubber toughening agent a, 0.2g of defoaming agent, 0.2g of coupling agent, 150g of spherical silica powder with the average particle size of 0.2 mu m and 10g of thixotropic agent nano calcium carbonate; stirring for 60 minutes under planetary stirring, adding 14g of dicyandiamide curing agent and 10g of accelerator substituted urea under stirring, stirring for 60 minutes under planetary stirring, and defoaming in vacuum to obtain the single-component tough epoxy compound a.
Example 2:
premixing 100g of tetrafunctional organic silicon modified epoxy resin and 16.5g of EXL-2620 nanometer nuclear shell rubber particles of Dow chemical company, gradually adding the rest 16.5g of EXL-2620 nanometer nuclear shell rubber particles under the planetary stirring, and then stirring for 60 minutes under the planetary stirring; and then grinding the mixture for 1 time by three rollers, and finally defoaming to prepare the nano core-shell rubber toughening agent b, wherein the viscosity of the nano core-shell rubber toughening agent b at 25 ℃ is 5100 mPa.s.
Firstly, premixing 100g of E51 bisphenol A epoxy resin, 45g of nano core-shell rubber toughening agent b, 0.2g of defoaming agent, 0.2g of coupling agent, 150g of spherical silica powder with the average particle size of 0.2 mu m and 10g of thixotropic agent nano calcium carbonate; stirring for 60 minutes under planetary stirring, adding 12g of curing agent dicyandiamide and 8g of accelerant substituted urea while stirring, stirring for 60 minutes under planetary stirring, and defoaming in vacuum to obtain the single-component tough epoxy compound b.
Example 3:
premixing 100g of tetrafunctional organic silicon modified epoxy resin and 12.5g of W35 nano core-shell rubber particles of Wacker company, gradually adding the rest 12.5g of W35 nano core-shell rubber particles under planetary stirring, and then stirring for 60 minutes under planetary stirring; and then grinding the mixture for 1 time by three rollers, and finally defoaming to prepare the nano core-shell rubber toughening agent c, wherein the viscosity of the nano core-shell rubber toughening agent c at 25 ℃ is 1250 mPa.s.
Firstly, premixing 100g of E51 bisphenol A epoxy resin, 60g of nano core-shell rubber toughening agent c, 0.2g of defoaming agent, 0.2g of coupling agent, 150g of spherical silica powder with the average particle size of 0.2 mu m and 10g of thixotropic agent nano calcium carbonate; stirring for 60 minutes under planetary stirring, adding 14g of dicyandiamide curing agent and 8g of imidazole accelerator under stirring, stirring for 60 minutes under planetary stirring, and defoaming in vacuum to obtain the single-component tough epoxy compound.
Example 4:
premixing 100g of tetrafunctional organic silicon modified epoxy resin and 12.5g of EXL-2655 rubber nano core-shell rubber particles, gradually adding the rest 12.5g of EXL-2655 rubber nano core-shell rubber particles under planetary stirring, and then stirring for 60 minutes under planetary stirring; and then grinding the mixture for 1 time by three rollers, and finally defoaming to prepare the nano core-shell rubber toughening agent d, wherein the viscosity of the nano core-shell rubber toughening agent d at 25 ℃ is 1360 mPa.s.
Firstly, premixing 100g of E51 bisphenol A epoxy resin, 45g of nano core-shell rubber toughening agent d, 0.2g of defoaming agent, 0.2g of coupling agent, 300g of spherical silica powder with the average particle size of 0.2 mu m and 10g of thixotropic agent nano calcium carbonate; stirring for 60 minutes under planetary stirring, adding 12g of curing agent dicyandiamide and 8g of modified amine coated by accelerator microcapsules under stirring, stirring for 60 minutes under high speed or planetary stirring, and defoaming in vacuum to obtain the single-component tough epoxy compound d.
Comparative example 1:
premixing 100g E51 bisphenol A epoxy resin and 16.5g of EXL-2620 nanometer core-shell rubber particles of Dow chemical company, gradually adding the rest 16.5g of EXL-2620 nanometer core-shell rubber particles under planetary stirring, and then stirring for 60 minutes under planetary stirring; and then grinding the mixture for 1 time by three rollers, and finally defoaming to prepare the nano core-shell rubber toughening agent e, wherein the viscosity of the nano core-shell rubber toughening agent e is 237000mPa.s at 25 ℃.
Firstly, premixing 100g of E51 bisphenol A epoxy resin, 45g of nano core-shell rubber toughening agent E, 0.2g of defoaming agent, 0.2g of coupling agent, 150g of spherical silica powder with the average particle size of 0.2 mu m and 10g of thixotropic agent nano calcium carbonate; stirring for 60 minutes under planetary stirring, adding 14g of dicyandiamide curing agent and 10g of accelerator substituted urea under stirring, stirring for 60 minutes under planetary stirring, and defoaming in vacuum to obtain the single-component epoxy compound e.
Comparative example 2:
firstly, premixing 100g of E51 bisphenol A epoxy resin, 60g of reactive carboxyl-terminated nitrile rubber epoxy resin (25 percent of nitrile rubber active ingredient), 0.2g of defoaming agent, 0.2g of coupling agent, 150g of spherical silicon micropowder with the average particle size of 0.2 mu m and 10g of thixotropic agent nano calcium carbonate; stirring for 120 minutes under planetary stirring, adding 14g of curing agent dicyandiamide and 10g of accelerator substituted urea under stirring, stirring for 120 minutes under planetary stirring, and defoaming in vacuum to obtain the single-component epoxy compound f.
Comparative example 3:
firstly, 145g of E51 bisphenol A epoxy resin, 0.2g of defoaming agent, 0.2g of coupling agent, 150g of spherical silica micropowder with the average particle size of 0.2 mu m and 10g of thixotropic agent nano calcium carbonate are premixed; stirring for 60 minutes under planetary stirring, adding 14g of curing agent dicyandiamide and 10g of accelerator substituted urea under stirring, stirring for 60 minutes under planetary stirring, and defoaming in vacuum to obtain the single-component epoxy compound g.
Curing and testing:
(1) performance comparison of the toughening agent:
in the table, the content of core-shell rubber particles of the toughening agent a and the toughening agent c is 20%, and the content of rubber in the toughening agent b, the toughening agent d, the toughening agent e in comparative example 1, and the reactive carboxyl-terminated nitrile butadiene rubber epoxy resin in comparative example 2 is 25%. As can be seen from the table, the toughener obtained by using the tetrafunctional organic silicon modified epoxy resin as the matrix resin has low viscosity, under the condition of the same effective content of rubber, more filler can be added into the toughener, and under the premise of the same manufacturability, the linear expansion coefficient of a cured product can be reduced to a greater extent, the high and low temperature performance of the cured product is improved, and cracking is prevented.
(2) And (3) comparing the performances of the cured product:
as can be seen in the table:
(1) examples 1-4 the toughener system obtained by using the tetrafunctional organosilicon modified epoxy resin as the matrix resin had a lower viscosity of the composite obtained by adding the same amount of spherical silica powder, and the same viscosity was obtained by adding more spherical silica powder as the filler to lower the linear expansion coefficient.
(2) In examples 1 to 4, the organosilicon modified epoxy resin has high functionality and high crosslinking density in the reaction process, so that the linear expansion coefficient is reduced, the glass transition temperature is basically unchanged, and the linear expansion coefficient can be further reduced by increasing the use amount of the filler due to low viscosity; the linear expansion coefficient of the core-shell resin toughening agent prepared from the bisphenol A epoxy resin in the comparative example 1 is higher, and the reactive carboxyl-terminated butadiene-acrylonitrile rubber toughening agent in the comparative example 2 is mainly characterized in that the glass transition temperature is reduced.
(3) In the embodiments 1-4, the organosilicon modified epoxy resin has four epoxy groups and is matched with the action of the toughening agent, so that the adhesive property of the composite is obviously improved; in comparative examples 1 and 2, the bonding strength of only the common core-shell rubber toughening agent compound or the reactive carboxyl-terminated butadiene-acrylonitrile rubber toughening agent is lower, while in comparative example 3, the bonding strength of the compound without the toughening agent after curing is far lower than that of examples 1-4.
(4) The toughening agents in the examples 1 to 4 have the toughening effect of the Si-O bond, so that the cracking resistance is obviously improved, the toughening agents in the comparative examples 1 to 2 have certain improvement on cracking, but the cracking phenomenon is slight even after the high and low temperature cycle times and temperature are increased, and the composite system without the toughening agent in the comparative example 3 has a serious cracking phenomenon.
The patent compares the results of the examples and the comparative examples as follows:
examples 1-4 are tougheners prepared by adding a tetrafunctional organosilicon modified epoxy compound, in comparative examples 1 and 2, only a common core-shell rubber toughening agent compound or a reactive carboxyl-terminated butadiene-acrylonitrile rubber toughening agent is used, and in comparative example 3, no toughening agent is used. The curing performance shows that the toughening agent prepared by adding the four-functionality organosilicon modified epoxy compound has the advantages of reducing the linear expansion coefficient, improving the bonding strength and not influencing the glass transition temperature; and because the viscosity of the toughening agent is low, the linear expansion coefficient of the cured material can be further reduced by increasing the using amount of the spherical silicon micro powder; in addition, the existence of the organic silicon structure enables a cured product to have certain toughness, so that the high and low temperature cracking resistance of the single-component tough epoxy compound can be improved by matching with the characteristics of the toughening agent and the low linear expansion coefficient.
In addition, in order to control the inductance of two poles of the magnetic material conveniently, the spherical silicon micro powder with the particle size of less than 0.5 mu m is adopted by the single-component tough epoxy resin compound to reduce the gap between the magnetic materials, so that a client can control the inductance conveniently, and the usability of the client is met.
Although the present invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be preferred embodiments of the present invention, it is to be understood that the invention is not limited thereto, and that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (8)
1. The nanoscale single-component tough epoxy compound for bonding the magnetic core is characterized by comprising the following components in parts by mass:
the filler is spherical silicon micro powder with the maximum grain diameter of less than 0.5 mu m;
the nano rubber core-shell particles are used for modifying the tetrafunctional organic silicon modified epoxy resin in a system, the nano rubber core-shell particles and the tetrafunctional organic silicon modified epoxy resin are subjected to blending modification, and the modified tetrafunctional organic silicon modified epoxy resin is used as a toughening agent.
2. The nanoscale one-component tough epoxy compound for magnetic core bonding according to claim 1, wherein:
the epoxy resin is one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, phenolic aldehyde modified epoxy resin or other epoxy resin prepolymers capable of reacting with dicyandiamide, modified amine and imidazole latent curing agent.
3. The nanoscale one-component tough epoxy compound for magnetic core bonding according to claim 1, wherein:
the curing agent is one or more of dicyandiamide, a modified dicyandiamide derivative, a modified microcapsule-coated latent amine curing agent and imidazole.
4. The nanoscale one-component tough epoxy compound for magnetic core bonding according to claim 1, wherein:
the accelerator is one or more of urea, imidazole or modified amine.
5. The nanoscale one-component tough epoxy compound for magnetic core bonding according to claim 1, wherein:
the tetrafunctional organic silicon modified epoxy resin is obtained by tetramethylhydrogen cyclotetrasiloxane and excessive allyl glycidyl ether under the condition of platinum complex catalysis, and has the following structure:
6. the nanoscale one-component tough epoxy compound for magnetic core bonding according to claim 5, wherein:
the rubber adopted by the nano rubber core-shell particles is one or more of polybutadiene rubber, organic silicon rubber and styrene butadiene rubber.
7. The nanoscale one-component tough epoxy compound for magnetic core bonding according to claim 1, wherein:
the thixotropic agent is nano calcium carbonate with the grain diameter less than 0.2 mu m, fumed silica or modified organic bentonite.
8. The preparation method of the nanoscale one-component tough epoxy compound for bonding the magnetic core as claimed in any one of claims 1 to 7 is characterized by comprising the following steps:
(1) preparing a toughening agent: premixing the tetrafunctional organic silicon modified epoxy resin and half of the expected addition amount of the nano core-shell rubber particles, gradually adding the rest half of the nano core-shell rubber particles under high-speed or planetary stirring, and then stirring for 10-120 minutes under high-speed or planetary stirring; then grinding the mixture for 1-3 times by three rollers, and finally defoaming to obtain the product;
(2) preparing a single-component epoxy resin compound: the epoxy resin toughening agent is prepared by premixing epoxy resin, the toughening agent, the defoaming agent, the coupling agent, the filler and the thixotropic agent, stirring for 10-120 minutes at high speed or under planetary stirring, adding the latent curing agent and the accelerator while stirring, stirring for 10-120 minutes at high speed or under planetary stirring, and defoaming in vacuum.
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| CN113999486A (en) * | 2020-12-29 | 2022-02-01 | 深材科技（深圳）有限公司 | Nano modified high-strength high-elasticity modulus polyurethane epoxy resin for reinforced carbon fiber composite material transmission tower and preparation method thereof |
| CN113004846A (en) * | 2021-04-13 | 2021-06-22 | 东莞市恒尔朗实业有限公司 | Low-temperature fast-curing epoxy adhesive for flat transformer |
| CN114058034A (en) * | 2021-12-20 | 2022-02-18 | 洛阳赛图新材料科技有限公司 | Nano rubber dispersing method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105176005A (en) * | 2015-10-23 | 2015-12-23 | 绵阳惠利电子材料有限公司 | Low-water-absorptivity dicyandiamide-curing epoxy composite |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105176005A (en) * | 2015-10-23 | 2015-12-23 | 绵阳惠利电子材料有限公司 | Low-water-absorptivity dicyandiamide-curing epoxy composite |
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