CN112266575B - High-temperature-resistant epoxy resin encapsulating material and preparation method thereof - Google Patents

High-temperature-resistant epoxy resin encapsulating material and preparation method thereof Download PDF

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CN112266575B
CN112266575B CN202011186385.7A CN202011186385A CN112266575B CN 112266575 B CN112266575 B CN 112266575B CN 202011186385 A CN202011186385 A CN 202011186385A CN 112266575 B CN112266575 B CN 112266575B
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epoxy resin
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encapsulating material
temperature
temperature resistant
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CN112266575A (en
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刘念杰
吴先锋
徐文辉
苏小军
林永利
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Xianyang Xinweihua Insulating Material Co ltd
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Xianyang Xinweihua Insulating Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Epoxy Resins (AREA)

Abstract

The application relates to the field of insulating materials, and particularly discloses a high-temperature-resistant epoxy resin encapsulating material and a preparation method thereof, wherein the epoxy resin encapsulating material is prepared from the following raw materials in parts by weight: 35-40 parts of bisphenol A epoxy resin; 3-7 parts of o-cresol formaldehyde epoxy resin; 8-10 parts of glycidyl amine type epoxy resin; 3-5 parts of a curing agent; 0.05-0.1 part of curing accelerator; 2.5-3.5 parts of halogen-free flame retardant; 28-30 parts of silicon dioxide; 8-10 parts of aluminum hydroxide; 2-3 parts of titanium dioxide; 0.5-1 part of pigment; 2-3 parts of a toughening agent; 4-5 parts of a laser marking agent; 0.5-1 part of leveling agent. The high-temperature-resistant epoxy resin encapsulating material has the advantage of good heat-resistant stability.

Description

High-temperature-resistant epoxy resin encapsulating material and preparation method thereof
Technical Field
The application relates to the field of insulating materials, in particular to a high-temperature-resistant epoxy resin encapsulating material and a preparation method thereof.
Background
Along with the development of society and the continuous improvement of people's living standard, the usage and the demand of electronic components are increasing more and more. The packaging material is also a protective garment for electronic components, and plays an important role in the reliability and stability of the electronic components. The encapsulating material for electronic components is phenolic resin-based, epoxy resin-based, polyester resin-based, polyamide resin-based, and the like.
The related technology mainly adopts bisphenol A type epoxy resin or bisphenol F epoxy resin, and then filler, pigment and curing agent are added to prepare the epoxy resin.
In view of the above-mentioned related art, the inventors believe that bisphenol a type epoxy resins and bisphenol F type epoxy resins have relatively low viscosity and are convenient to apply, but have poor heat resistance.
Disclosure of Invention
In order to improve the heat-resistant stability of the epoxy resin, the application provides a high-temperature-resistant epoxy resin encapsulating material and a preparation method thereof.
In a first aspect, the present application provides a high temperature resistant epoxy encapsulating material, which adopts the following technical scheme:
a high-temperature-resistant epoxy resin encapsulating material is prepared from the following raw materials in parts by weight:
35-40 parts of bisphenol A type epoxy resin;
3-7 parts of o-cresol formaldehyde epoxy resin;
8-10 parts of glycidyl amine type epoxy resin;
3-5 parts of a curing agent;
0.05-0.1 part of curing accelerator;
2.5-3.5 parts of halogen-free flame retardant;
28-30 parts of silicon dioxide;
8-10 parts of aluminum hydroxide;
2-3 parts of titanium dioxide;
0.5-1 part of pigment;
2-3 parts of a toughening agent;
4-5 parts of a laser marking agent;
0.5-1 part of leveling agent.
By adopting the technical scheme, as the bisphenol A type epoxy resin, the o-cresol formaldehyde epoxy resin and the glycidylamine type epoxy resin are compounded for use, the o-cresol formaldehyde epoxy resin has higher epoxy value, can provide more crosslinking points during curing, is easy to form a three-dimensional structure with high crosslinking density, and is rich in phenolic aldehyde skeleton after curing, so that the thermal stability of the encapsulating material is improved. And bisphenol A type epoxy resin, o-cresol formaldehyde epoxy resin and glycidylamine type epoxy resin are compounded for use, so that the synergistic effect can be realized, and the thermal stability of the encapsulating material is improved.
Preferably, the raw materials of the epoxy resin encapsulating material also comprise 4-8 parts of high-temperature resistant fibers, and the high-temperature resistant fibers are prepared by esterification reaction of plant fibers and aromatic acid.
By adopting the technical scheme, the high-temperature resistant fiber not only can further overcome the defect of brittleness of the o-cresol formaldehyde epoxy resin, but also can further enhance the heat-resistant stability of the encapsulating material.
Preferably, the preparation method of the high temperature resistant fiber comprises the following steps: drying 10 parts of bamboo fiber, adding into a reaction vessel, adding 1-1.2 parts of aromatic acid, 0.1-0.3 part of thionyl chloride and 90-100 parts of ethanol into the reaction vessel, heating to 40-50 ℃, reacting for 1-2h, performing suction filtration, washing with water, and drying to obtain the high-temperature resistant fiber.
By adopting the technical scheme, the bamboo fiber and the aromatic acid are subjected to esterification reaction in an ethanol solvent under the catalytic action of thionyl chloride, so that a benzene ring structure is grafted on the surface of the bamboo fiber, the heat resistance of the bamboo fiber is enhanced, and the heat resistance stability of the encapsulating material is improved; the compatibility of the grafted bamboo fiber and the encapsulating material is greatly improved, and the toughness of the encapsulating material can be enhanced.
Preferably, the length of the bamboo fiber is 0.8-2mm, and the diameter is 15-25 μm.
By adopting the technical scheme, the bamboo fiber with the size can improve the toughness of the packaging material and the heat-resistant stability of the packaging material.
Preferably, the aromatic acid is any one selected from benzoic acid, phenylacetic acid and 3-phenylpropionic acid.
By adopting the technical scheme, the aromatic acid has certain reaction activity, is easy to perform esterification reaction with the bamboo fiber under the catalysis of thionyl chloride, and improves the heat resistance of the bamboo fiber.
Preferably, the curing agent consists of toluenediamine, 2-ethyl-4-methylimidazole and isophorone diamine, and the weight ratio of the toluenediamine, the 2-ethyl-4-methylimidazole and the isophorone diamine is 1: (0.4-0.6): (1-1.5).
By adopting the technical scheme, the molecular structure of the curing agent contains functional groups with higher heat resistance, such as amino groups, benzene rings and the like, so that the curing reaction of the epoxy resin can be catalyzed, and the epoxy resin can also react with the functional groups on the epoxy resin, so that the epoxy resin molecules have a rigid molecular structure, and the heat resistance stability of the encapsulating material is further improved.
Preferably, the curing accelerator is any one selected from the group consisting of 2-methylimidazole, 1-benzyl 2-methylimidazole, and 1-aminoethyl-2-methylimidazole.
By adopting the technical scheme, the curing accelerator can promote the curing of the epoxy resin, shorten the curing time and enhance the mechanical property of the cured epoxy resin, and the curing accelerator also contains a benzene ring structure, so that the heat-resistant stability of the encapsulating material can be improved.
In a second aspect, the application provides a preparation method of a high temperature resistant epoxy resin encapsulating material, which adopts the following technical scheme:
a preparation method of a high-temperature-resistant epoxy resin encapsulating material comprises the following steps: uniformly mixing bisphenol A epoxy resin, o-cresol formaldehyde epoxy resin, glycidol amine epoxy resin, a curing agent, a curing accelerator, a halogen-free flame retardant, silicon dioxide, aluminum hydroxide, titanium dioxide, pigment, a toughening agent, a laser marking agent and a flatting agent for 5-15min, then carrying out melt extrusion mixing, wherein the temperature of an extruder is 80-160 ℃, and crushing, crushing and screening after tabletting and cooling to obtain the high-temperature-resistant epoxy resin encapsulating material.
By adopting the technical scheme, the organic raw materials and the inorganic raw materials are mechanically mixed and then are melted, extruded and mixed, so that the components are fully and uniformly mixed, the mechanical property of the encapsulated electronic component is enhanced, and the electronic component is conveniently encapsulated after the powder is prepared.
In summary, the present application has the following beneficial effects:
1. because the bisphenol A type epoxy resin, the o-cresol formaldehyde epoxy resin and the glycidylamine type epoxy resin are compounded for use, the o-cresol formaldehyde epoxy resin has a higher epoxy value, can provide more crosslinking points during curing, is easy to form a three-dimensional structure with high crosslinking density, and is rich in phenolic aldehyde frameworks after curing, so that the thermal stability of the encapsulating material is improved. And bisphenol A type epoxy resin, o-cresol formaldehyde epoxy resin and glycidylamine type epoxy resin are compounded for use, so that the synergistic effect can be realized, and the thermal stability of the encapsulating material is improved.
2. In the application, the high-temperature resistant fiber is preferably added, and the bamboo fiber and the aromatic acid are subjected to esterification reaction in an ethanol solvent under the catalytic action of thionyl chloride, so that a benzene ring structure is grafted on the surface of the bamboo fiber, the heat resistance of the bamboo fiber is enhanced, and the heat-resistant stability of the encapsulating material is improved; the compatibility of the grafted bamboo fiber and the encapsulating material is greatly improved, and the toughness of the encapsulating material can be enhanced.
3. In the application, toluenediamine, 2-ethyl-4-methylimidazole and isophorone diamine are preferably compounded to serve as a curing agent, and the molecular structure of the curing agent contains functional groups with high heat resistance, such as amino groups and benzene rings, so that the curing reaction of epoxy resin can be catalyzed, and the reaction with the functional groups on the epoxy resin can be realized, so that the epoxy resin has a rigid molecular structure on the molecules, and the heat resistance stability of the encapsulating material is further improved.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation examples of raw materials
Preparation example 1
The high-temperature resistant fiber is prepared by the following steps: drying 10kg of bamboo fiber, adding into a reaction vessel, adding 1kg of benzoic acid, 0.1kg of thionyl chloride and 90kg of ethanol into the reaction vessel, heating to 40 ℃, reacting for 2 hours, filtering, washing with water, and drying to obtain the high-temperature resistant fiber. The length of the bamboo fiber is 0.8mm, and the diameter is 15 μm.
Preparation example 2
The high-temperature resistant fiber is prepared by the following steps: drying 10kg of bamboo fiber, adding into a reaction vessel, adding 1.2kg of benzoic acid, 0.1kg of thionyl chloride and 90kg of ethanol into the reaction vessel, heating to 40 ℃, reacting for 2 hours, filtering, washing with water, and drying to obtain the high-temperature resistant fiber. The length of the bamboo fiber is 0.8mm, and the diameter is 15 μm.
Preparation example 3
The high-temperature resistant fiber is prepared by the following steps: drying 10kg of bamboo fiber, adding into a reaction vessel, adding 1kg of benzoic acid, 0.3kg of thionyl chloride and 100kg of ethanol into the reaction vessel, heating to 40 ℃, reacting for 2 hours, filtering, washing with water, and drying to obtain the high-temperature resistant fiber. The length of the bamboo fiber is 0.8mm, and the diameter is 15 μm.
Preparation example 4
The high-temperature resistant fiber is different from the preparation example 1 in that the temperature is increased to 45 ℃ in the preparation step, and the reaction is carried out for 1.5h.
Preparation example 5
The high-temperature resistant fiber is different from the preparation example 1 in that the temperature is increased to 50 ℃ in the preparation step, and the reaction is carried out for 1h.
Preparation example 6
The refractory fiber is different from the fiber prepared in preparation example 1 in that the length of the bamboo fiber is 2mm and the diameter is 15 μm.
Preparation example 7
The refractory fiber is different from the refractory fiber of preparation example 1 in that the length of the bamboo fiber is 2mm and the diameter is 25 μm.
Preparation example 8
A high temperature resistant fiber, which is different from preparation example 1 in that benzoic acid was replaced with phenylacetic acid of equal weight.
Preparation example 9
The high-temperature resistant fiber is different from the preparation example 1 in that benzoic acid is replaced by 3-phenylpropionic acid with the same weight.
Examples
Example 1
A high-temperature-resistant epoxy resin encapsulating material is prepared from the raw materials in parts by weight shown in Table 1. The preparation method of the high-temperature-resistant epoxy resin encapsulating material comprises the following steps: uniformly mixing bisphenol A type epoxy resin, o-cresol formaldehyde epoxy resin, glycidol amine type epoxy resin, a curing agent, a curing accelerator, a halogen-free flame retardant, silicon dioxide, aluminum hydroxide, titanium dioxide, pigment, a toughening agent, a laser marking agent and a leveling agent for 15min at a rotation speed of 800r/min, then performing melt extrusion mixing by using a screw extruder at a temperature of 160 ℃ at a rotation speed of 1000r/min, performing tabletting and cooling by using a tabletting machine, crushing to 80 meshes, crushing and screening to obtain the high-temperature-resistant epoxy resin encapsulating material.
Wherein the bisphenol A type epoxy resin is E-20, the o-cresol novolac epoxy resin is SQCN700 from Jinan Shengquan group, inc., and the glycidyl amine type epoxy resin is 4,4' -diaminodiphenylmethane tetraglycidyl amine from Hubeide super chemical, inc. The curing agent is toluenediamine, the curing accelerator is 2-methylimidazole, the halogen-free flame retardant is ammonium polyphosphate, the pigment is phthalocyanine blue, the toughening agent is polypropylene alcohol, the laser marking agent is copper oxalate, the flatting agent is polyethylacrylate, and the molecular weight of the flatting agent is 2000.
Examples 2 to 3
The difference between the high-temperature-resistant epoxy resin encapsulating material and the embodiment 1 is that the raw materials and the parts by weight thereof are shown in Table 1.
TABLE 1 materials of examples 1-3 and parts by weight (kg) thereof
Components Example 1 Example 2 Example 3
Bisphenol A epoxy resin 35 38 40
O-cresol formaldehyde epoxy resin 3 5 7
Glycidylamine type epoxy resin 10 9 8
Curing agent 3 4 5
Curing accelerator 0.1 0.08 0.05
Halogen-free flame retardant 2.5 3 3.5
Silicon dioxide 28 29 30
Aluminum hydroxide 8 9 10
Titanium white powder 3 2.5 2
Pigment (I) 0.5 0.8 1
Toughening agent 2 2.5 3
Laser marking agent 4 4.5 5
Leveling agent 0.5 0.7 1
Example 4
The high-temperature-resistant epoxy resin encapsulating material is different from the material in the embodiment 1 in that the material also contains 4kg of high-temperature-resistant fibers, and the high-temperature-resistant fibers are prepared by the preparation example 1.
Examples 5 to 12
A high temperature resistant epoxy resin encapsulating material is different from the embodiment 4 in that the high temperature resistant fiber is respectively prepared by the preparation examples 2-9.
Example 13
The difference between the high-temperature-resistant epoxy resin encapsulating material and the embodiment 4 is that the raw material also contains 1kg of high-temperature-resistant fibers.
Example 14
The difference between the high-temperature-resistant epoxy resin encapsulating material and the embodiment 4 is that the raw material also contains 6kg of high-temperature-resistant fibers.
Example 15
The difference between the high-temperature resistant epoxy resin encapsulating material and the material in the embodiment 4 is that the raw material also contains 8kg of high-temperature resistant fiber.
Example 16
The difference between the high-temperature resistant epoxy resin encapsulating material and the material in the embodiment 4 is that the raw material also contains 12kg of high-temperature resistant fiber.
Example 17
The difference between the high-temperature-resistant epoxy resin encapsulating material and the example 1 is that the curing agent is 2-ethyl-4-methylimidazole.
Example 18
A high temperature resistant epoxy resin encapsulant differs from example 1 in that the curing agent is isophorone diamine.
Example 19
The difference between the high-temperature-resistant epoxy resin encapsulating material and the embodiment 1 is that a curing agent consists of toluenediamine, 2-ethyl-4-methylimidazole and isophorone diamine, and the weight ratio of the toluenediamine to the 2-ethyl-4-methylimidazole to the isophorone diamine is 1:0.4:1.
example 20
The difference between the high-temperature-resistant epoxy resin encapsulating material and the embodiment 1 is that a curing agent consists of toluenediamine, 2-ethyl-4-methylimidazole and isophorone diamine, and the weight ratio of the toluenediamine to the 2-ethyl-4-methylimidazole to the isophorone diamine is 1:0.6:1.5.
example 21
The difference between the high-temperature-resistant epoxy resin encapsulating material and the embodiment 1 is that a curing agent consists of toluenediamine, 2-ethyl-4-methylimidazole and isophorone diamine, and the weight ratio of the toluenediamine to the 2-ethyl-4-methylimidazole to the isophorone diamine is 1:0.6:0.3.
example 22
A high temperature resistant epoxy resin encapsulating material is different from the epoxy resin encapsulating material in the embodiment 1 in that the curing accelerator is 1-benzyl 2-methylimidazole.
Example 23
A high temperature resistant epoxy resin encapsulating material is different from the material in the embodiment 1 in that the curing accelerator is 1-aminoethyl-2-methylimidazole.
Comparative example
Comparative example 1
A high temperature resistant epoxy resin encapsulant differs from example 1 in that no ortho-cresol formaldehyde epoxy resin and no glycidylamine type epoxy resin are added.
Comparative example 2
The difference between the high-temperature-resistant epoxy resin encapsulating material and the embodiment 1 is that the o-cresol formaldehyde epoxy resin is replaced by bisphenol A type epoxy resin with equal weight.
Comparative example 3
A high-temperature resistant epoxy resin encapsulating material is different from the material in the embodiment 1 in that glycidyl amine type epoxy resin is replaced by bisphenol A type epoxy resin with equal weight parts.
Comparative example 4
The difference between the high-temperature resistant epoxy resin encapsulating material and the high-temperature resistant epoxy resin encapsulating material in the embodiment 1 is that o-cresol formaldehyde epoxy resin is not added.
Comparative example 5
A high temperature resistant epoxy resin encapsulant differs from example 1 in that no glycidylamine type epoxy resin is added.
Comparative example 6
A high temperature resistant epoxy resin encapsulating material is different from the material in the embodiment 1 in that bisphenol A type epoxy resin is not added.
Comparative example 7
A high temperature resistant epoxy resin encapsulating material is different from the material in the embodiment 1 in that no curing accelerator is added.
Comparative example 8
A high temperature resistant epoxy resin encapsulating material is different from the material in the embodiment 1 in that the weight of the curing accelerator is 0.02kg.
The performance detection test detection method comprises the following steps: (1) Epoxy resin encapsulants prepared in examples 1 to 23 and comparative examples 1 to 8 were tested for flexural strength and impact strength according to the GB/T2567-2008 resin casting property test method.
(2) Thermogravimetric analysis: the 5% weight loss temperature (T5) of the epoxy resin encapsulants prepared in examples 1 to 23 and comparative examples 1 to 8 was determined according to the TGA curve using a Perkin-Elmer Ppyril thermal analyzer with a gas flow rate of 20mL/min, a temperature rise rate of 10 ℃/min and a temperature range of 30 to 800 ℃.
TABLE 2 results of the Performance test of examples 1 to 23 and comparative examples 1 to 8
Figure BDA0002751424080000071
Figure BDA0002751424080000081
It can be seen by combining examples 1 to 23 and comparative examples 1 to 8 and by combining table 2 that the 5% thermogravimetric temperature is only 185% when the bisphenol a type epoxy resin is used in comparative example 1, is increased to 192% when the o-cresol novolac epoxy resin is used in comparative example 2, and is increased to 190% when the glycidylamine type epoxy resin is used in comparative example 3, indicating that the heat resistance stability of the o-cresol novolac epoxy resin and the glycidylamine type epoxy resin is higher than that of the bisphenol a type epoxy resin, and that the flexural strength and the impact strength are lower than those of comparative example 1 and comparative example 3 when the o-cresol novolac epoxy resin is used in comparative example 2, indicating that the toughness of the o-cresol novolac epoxy resin is poor. Comparative example 4 when bisphenol A type epoxy resin and glycidyl amine type epoxy resin were compounded, the 5% thermogravimetric temperature was 192 ℃ and the bending strength and impact strength were improved to 124MPa and 20KJ/m2Bisphenol A type epoxy resin and glycidylamine type epoxy resin are explainedThe heat resistance stability and toughness of the encapsulating material can be improved by compounding; comparative example 5 compounding bisphenol A epoxy resin and o-cresol novolac epoxy resin, the 5% thermogravimetric temperature was 195 deg.C, and the flexural strength and impact strength were 118MPa and 17KJ/m2The compound use of the bisphenol A type epoxy resin and the o-cresol formaldehyde epoxy resin is proved to improve the heat-resistant stability of the encapsulating material, but the toughness of the encapsulating material is reduced; comparative example 6 when o-cresol formaldehyde epoxy resin and glycidylamine epoxy resin are compounded, the 5% thermal weight loss temperature is greatly increased to 205 ℃, and the bending strength and the impact strength are 125MPa and 20KJ/m2The o-cresol formaldehyde epoxy resin and the glycidylamine epoxy resin are compounded for use, so that the synergistic effect can be realized, and the heat resistance stability and the toughness of the encapsulating material are improved.
In the embodiment 1, bisphenol A type epoxy resin, o-cresol formaldehyde epoxy resin and glycidylamine type epoxy resin are compounded for use, the 5 percent thermal weight loss temperature is greatly improved to 300 ℃, and the bending strength and the impact strength are 131MPa and 22KJ/m2The bisphenol A epoxy resin, the o-cresol formaldehyde epoxy resin and the glycidylamine epoxy resin are compounded for use, so that the synergistic effect can be realized, and the heat-resistant stability and the toughness of the encapsulating material are improved.
Example 4 high temperature resistant fiber is added on the basis of example 1, the 5% thermal weight loss temperature is greatly increased to 325 ℃, the bending strength and the impact strength are increased to 150MPa and 26KJ/m2In examples 5 to 12, when the preparation parameters of the refractory fibers are changed within the range of the present application, the 5% thermal weight loss temperature, the bending strength and the impact strength are all improved compared with example 1, which shows that the refractory fibers can obviously enhance the heat resistance stability and the toughness of the encapsulating material.
Example 13 with the addition of only 1kg of high temperature resistant fiber, the 5% thermogravimetric temperature was increased to 310 ℃ and the flexural and impact strength was increased to 136MPa and 23KJ/m2It is said that the addition amount of the high-temperature resistant fiber is too small to greatly improve the heat resistance stability and toughness of the potting material. Example 16 with the addition of excess refractory fiber, the 5% thermogravimetric temperature was 324 ℃ and the flexural and impact strengths were 135MPa and 22KJ/m, respectively2The resistance was slightly lower than that in example 4, which shows thatThe addition amount of the high-temperature fibers is too much, so that the heat resistance stability and the toughness of the encapsulating material cannot be further improved, and certain negative effects can be caused.
When 2-ethyl-4-methylimidazole alone was used as the curing agent in example 17, the 5% thermogravimetric temperature was 301 ℃ and the flexural strength and impact strength were 132MPa and 22KJ/m, respectively2In the case of using only isophorone diamine as the curing agent in example 18, the 5% thermogravimetric loss temperature was 302 ℃ and the bending strength and impact strength were 131MPa and 22KJ/m, respectively2The difference from the example 1 is not great, but when the toluenediamine, the 2-ethyl-4-methylimidazole and the isophorone diamine are compounded and used according to a specific ratio in the examples 19 to 20, the 5% thermal weight loss temperature, the bending strength and the impact strength are greatly improved, which shows that when the toluenediamine, the 2-ethyl-4-methylimidazole and the isophorone diamine are compounded and used, the synergistic effect can be achieved, and the heat resistance stability and the toughness of the encapsulating material are obviously improved. In example 21, when the mixture ratio of toluenediamine, 2-ethyl-4-methylimidazole and isophoronediamine is out of the range of the application, the 5% thermogravimetric temperature, the bending strength and the impact strength are not substantially improved, which indicates that the toluenediamine, 2-ethyl-4-methylimidazole and isophoronediamine need to be in a specific mixture ratio to be synergistic.
Examples 22 to 23, in which 1-benzyl 2-methylimidazole and 1-aminoethyl-2-methylimidazole were used as the curing accelerators, respectively, the 5% thermogravimetric temperature, the flexural strength and the impact strength were substantially unchanged from example 1; the comparative example 7 has slightly reduced 5% thermal weight loss temperature, bending strength and impact strength when no curing accelerator is added, and the comparative example 8 has slightly reduced 5% thermal weight loss temperature, bending strength and impact strength when a small amount of curing accelerator is added, which shows that the curing accelerator of the application has certain improvement effect on the 5% thermal weight loss temperature, bending strength and impact strength.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (5)

1. The high-temperature-resistant epoxy resin encapsulating material is characterized by being prepared from the following raw materials in parts by weight:
35-40 parts of bisphenol A epoxy resin;
3-7 parts of o-cresol formaldehyde epoxy resin;
8-10 parts of glycidyl amine type epoxy resin;
3-5 parts of a curing agent;
0.05-0.1 part of curing accelerator;
2.5-3.5 parts of halogen-free flame retardant;
28-30 parts of silicon dioxide;
8-10 parts of aluminum hydroxide;
2-3 parts of titanium dioxide;
0.5-1 part of pigment;
2-3 parts of a toughening agent;
4-5 parts of a laser marking agent;
0.5-1 part of a leveling agent;
the raw materials of the epoxy resin encapsulating material also comprise 4-8 parts of high-temperature resistant fiber, and the high-temperature resistant fiber is prepared by esterification reaction of plant fiber and aromatic acid;
the preparation method of the high-temperature resistant fiber comprises the following steps: drying 10 parts of bamboo fiber, adding into a reaction vessel, adding 1-1.2 parts of aromatic acid, 0.1-0.3 part of thionyl chloride and 90-100 parts of ethanol into the reaction vessel, heating to 40-50 ℃, reacting for 1-2 hours, performing suction filtration, washing with water, and drying to obtain high-temperature resistant fiber;
the curing agent consists of toluenediamine, 2-ethyl-4-methylimidazole and isophorone diamine, and the weight ratio of the toluenediamine to the 2-ethyl-4-methylimidazole to the isophorone diamine is 1: (0.4-0.6): (1-1.5).
2. The high temperature resistant epoxy resin encapsulating material as claimed in claim 1, wherein: the length of the bamboo fiber is 0.8-2mm, and the diameter is 15-25 μm.
3. The high temperature resistant epoxy resin encapsulating material as claimed in claim 1, wherein: the aromatic acid is selected from any one of benzoic acid, phenylacetic acid and 3-phenylpropionic acid.
4. The high temperature resistant epoxy resin encapsulating material as claimed in claim 1, wherein: the curing accelerator is any one of 2-methylimidazole, 1-benzyl 2-methylimidazole and 1-aminoethyl-2-methylimidazole.
5. The method for preparing the high temperature resistant epoxy resin encapsulating material according to any one of claims 1 to 4, which is characterized in that: the method comprises the following steps: uniformly mixing bisphenol A epoxy resin, o-cresol formaldehyde epoxy resin, glycidol amine epoxy resin, a curing agent, a curing accelerator, a halogen-free flame retardant, silicon dioxide, aluminum hydroxide, titanium dioxide, pigment, a toughening agent, a laser marking agent and a leveling agent for 5-15min, then carrying out melt extrusion mixing, extruding at the temperature of 80-160 ℃, tabletting, cooling, crushing and screening to obtain the high-temperature-resistant epoxy resin encapsulating material.
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