Preparation method of epoxy resin curing agent

Abstract

The invention discloses a preparation method of an epoxy resin curing agent. The epoxy resin curing agent is prepared by carrying out a reaction on a biphenyl-type phenol liquid crystal element and abifunctional epoxy compound, and in the preparation process, the liquid crystal element is introduced into the epoxy resin curing agent. When the epoxy resin curing agent provided by the invention isused for curing epoxy resin, heat conductivity of a cured product can be improved, and meanwhile, the problem of poor compatibility of the biphenyl-type phenol liquid crystal element and an epoxy resin matrix is solved. In addition, the preparation method of the epoxy resin curing agent is simple and is easy to operate, and production is convenient. The raw materials used in the preparation process are wide, cost is low, and the preparation method is easy for wide popularization and use.

Description

technical field

[0001] The present application relates to the technical field of epoxy resin, in particular to a method for preparing an epoxy resin curing agent. Background technique

[0002] The epoxy resin composition with epoxy resin and its curing agent as essential components has excellent properties such as heat resistance and moisture resistance, so it is widely used in coatings, adhesives, composite resin matrix, electronic packaging materials, etc., especially It plays a great role in the packaging of electronic components and integrated circuits. More than 95% of the packaging substrates of electronic components and integrated circuits on the market are prepared from epoxy resin compositions. In today's electronic market, there are more and more high-power components in electronic products, and at the same time, the integration density of components is also getting higher and higher. In order to meet the heat dissipation requirements of electronic products, it is ...

Examples

preparation example Construction

[0021] The application provides a kind of preparation method of epoxy resin curing agent, and its preparation step comprises:

[0022] In step S10, 2 mol of compound A is dissolved in a solvent, wherein compound A is a compound represented by the following general formula (1),

[0023]

[0024] R in general formula (1) 1 , R 2 , R 3 and R 4 independently of each other -H or -CH 3 .

[0025] Step S20, adding 1-1.6 mol of bifunctional epoxy compound into the solvent in which compound A is dissolved.

[0026] In the present application, the difunctional epoxy compound includes one or more of the following five epoxy compounds of I-V,

[0027]

[0028]

[0029] Step S30, uniformly mix the dissolved compound A and the difunctional epoxy compound, raise the temperature to 70-160°C, and react for 1-6h to prepare an epoxy resin curing agent, which includes the following general formula Compounds represented by (2):

[0030]

[0031] In general formula (2), n repres...

Embodiment 1

[0036] The preparation process of epoxy resin curing agent comprises:

[0037] Take 90g of bisphenol A type epoxy with an epoxy equivalent of 175-185g / eq and 93g of 4,4-biphenyldiol and dissolve them in DMF, and react at 120-125°C for 2 hours to obtain it. The actual phenolic hydroxyl equivalent is 388g / eq mol.

[0038] In the present embodiment, the structural formula of bisphenol A type epoxy is:

[0039]

[0040] In the present embodiment, the epoxy resin curing agent that makes comprises following compound:

[0041] Among them, R is

[0042]

Embodiment 2

[0044] The preparation process of epoxy resin curing agent comprises:

[0045] Take 85g of bisphenol F-type epoxy with an epoxy equivalent of 160-180g / eq and 93g of 4,4-biphenyldiol and dissolve them in ethylene glycol methyl ether, then add 0.05g of 2-methylimidazole, 120- It can be obtained by reacting at 125°C for 2 hours, and its phenolic hydroxyl equivalent is measured to be 376g / mol.

[0046] In the present embodiment, the structural formula of bisphenol F type epoxy is:

[0047]

[0048] In the present embodiment, the epoxy resin curing agent that makes comprises following compound:

[0049] Among them, R is

[0050]

technical field

[0001] The present application relates to the technical field of epoxy resin, in particular to a method for preparing an epoxy resin curing agent. Background technique

[0002] The epoxy resin composition with epoxy resin and its curing agent as essential components has excellent properties such as heat resistance and moisture resistance, so it is widely used in coatings, adhesives, composite resin matrix, electronic packaging materials, etc., especially It plays a great role in the packaging of electronic components and integrated circuits. More than 95% of the packaging substrates of electronic components and integrated circuits on the market are prepared from epoxy resin compositions. In today's electronic market, there are more and more high-power components in electronic products, and at the same time, the integration density of components is also getting higher and higher. In order to meet the heat dissipation requirements of electronic products, it is ...

Examples

preparation example Construction

[0021] The application provides a kind of preparation method of epoxy resin curing agent, and its preparation step comprises:

[0022] In step S10, 2 mol of compound A is dissolved in a solvent, wherein compound A is a compound represented by the following general formula (1),

[0023]

[0024] R in general formula (1) 1 , R 2 , R 3 and R 4 independently of each other -H or -CH 3 .

[0025] Step S20, adding 1-1.6 mol of bifunctional epoxy compound into the solvent in which compound A is dissolved.

[0026] In the present application, the difunctional epoxy compound includes one or more of the following five epoxy compounds of I-V,

[0027]

[0028]

[0029] Step S30, uniformly mix the dissolved compound A and the difunctional epoxy compound, raise the temperature to 70-160°C, and react for 1-6h to prepare an epoxy resin curing agent, which includes the following general formula Compounds represented by (2):

[0030]

[0031] In general formula (2), n repres...

Embodiment 1

[0036] The preparation process of epoxy resin curing agent comprises:

[0037] Take 90g of bisphenol A type epoxy with an epoxy equivalent of 175-185g / eq and 93g of 4,4-biphenyldiol and dissolve them in DMF, and react at 120-125°C for 2 hours to obtain it. The actual phenolic hydroxyl equivalent is 388g / eq mol.

[0038] In the present embodiment, the structural formula of bisphenol A type epoxy is:

[0039]

[0040] In the present embodiment, the epoxy resin curing agent that makes comprises following compound:

[0041] Among them, R is

[0042]

Embodiment 2

[0044] The preparation process of epoxy resin curing agent comprises:

[0045] Take 85g of bisphenol F-type epoxy with an epoxy equivalent of 160-180g / eq and 93g of 4,4-biphenyldiol and dissolve them in ethylene glycol methyl ether, then add 0.05g of 2-methylimidazole, 120- It can be obtained by reacting at 125°C for 2 hours, and its phenolic hydroxyl equivalent is measured to be 376g / mol.

[0046] In the present embodiment, the structural formula of bisphenol F type epoxy is:

[0047]

[0048] In the present embodiment, the epoxy resin curing agent that makes comprises following compound:

[0049] Among them, R is

[0050]

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