阅读说明：本技术 一种用于铝板材生产用环氧树脂固化剂配置方法 (Preparation method of epoxy resin curing agent for aluminum plate production ) 是由 俞金发 朱良科 林士兵 于 2021-08-18 设计创作，主要内容包括：本发明涉及一种用于铝板材生产用环氧树脂固化剂配置方法,本发明中的固化剂由多种固化组分混合组成,其中包含N,N-二甲基甲酰胺(DMF)、氨苯砜(DDS)、2-甲基唑咪(2MI)、双氰胺(DICY),在常温下呈现液态,使用方便,加入树脂后分散效果好,无需添加固化促进剂也可以获得良好的固化效率,且其中的双氰胺(DICY)具有良好的金属相容性,适用于各类金属型材及PCB板的加工,可以提高固化后的环氧树脂的物理性能。(The invention relates to a method for preparing an epoxy resin curing agent for aluminum plate production, wherein the curing agent is prepared by mixing a plurality of curing components, wherein the curing components comprise N, N-Dimethylformamide (DMF), dapsone (DDS), 2-methyl imidazole (2MI) and Dicyandiamide (DICY), the curing agent is liquid at normal temperature, the use is convenient, the dispersion effect is good after the resin is added, the good curing efficiency can be obtained without adding a curing accelerator, and the Dicyandiamide (DICY) has good metal compatibility, is suitable for processing various metal profiles and PCB plates, and can improve the physical properties of the cured epoxy resin.)

1. A preparation method of an epoxy resin curing agent for aluminum plate production is characterized by comprising the following steps: comprises the following steps;

pretreatment of raw materials: weighing N, N-Dimethylformamide (DMF), dapsone (DDS), 2-mezzanine (2MI) and Dicyandiamide (DICY), heating the N, N-Dimethylformamide (DMF) to 50-70 deg.C, and determining the granularity of Dicyandiamide (DICY);

mixing raw materials: pouring dapsone (DDS), 2-mezzanine (2MI) and Dicyandiamide (DICY) into N, N-Dimethylformamide (DMF) to obtain a mixed solution;

stirring at constant temperature: keeping the temperature of the mixed solution at 50-70 deg.C, slowly stirring until the powder is dissolved, and no visible precipitate is formed to obtain liquid solidifying agent;

and (4) sealing and storing: and sealing the liquid curing agent in an air-tight manner, preserving heat and preserving for later use.

2. The preparation method of the epoxy resin curing agent for aluminum plate production as claimed in claim 1, wherein the curing agent comprises the following steps: in the raw material pretreatment step, the N, N-Dimethylformamide (DMF), the dapsone (DDS), the 2-methylimidazole (2MI) and the Dicyandiamide (DICY) are mixed according to the mass part ratio as follows: 30-50 parts of N, N-Dimethylformamide (DMF), 2-5 parts of dapsone (DDS), 8-13 parts of 2-methylzolmitanide (2MI) and 10-18 parts of Dicyandiamide (DICY).

3. The method for preparing the epoxy resin curing agent for aluminum plate production according to claim 2, wherein the method comprises the following steps: the purity of the 2-mezzolamide (2MI) is more than 99 percent.

4. The method for preparing the epoxy resin curing agent for aluminum plate production according to claim 2, wherein the method comprises the following steps: the Dicyandiamide (DICY) is electronic grade Dicyandiamide (DICY).

5. The method for preparing the epoxy resin curing agent for aluminum plate production according to claim 1, wherein the method comprises the following steps: in the raw material mixing step, the next raw material is added after the previous raw material is completely infiltrated by the DFM.

6. The method for preparing the epoxy resin curing agent for producing the aluminum plate as claimed in claim 5, wherein the method comprises the following steps: DFM is continuously added in the raw material mixing step, so that the dissolving efficiency is prevented from being influenced by temperature reduction.

7. The preparation method of the epoxy resin curing agent for aluminum plate production as claimed in claim 1, wherein the curing agent comprises the following steps: in the constant-temperature stirring step, the raw materials are poured into a stirrer to be stirred at the speed of 15-20 r/min.

8. The method for preparing the epoxy resin curing agent for aluminum plate production according to claim 7, wherein the method comprises the following steps: the temperature of the liquid curing agent is kept above 45 ℃ during the sealing and storage.

Technical Field

The invention belongs to the technical field of curing agents, and particularly relates to a preparation method of an epoxy resin curing agent for aluminum plate production.

Background

With the continuous development of social productivity, more and more products need to use different metal substrates, and the metal substrates are usually processed with epoxy resin in an auxiliary way in the production process, which puts certain requirements on the curing of the epoxy resin.

The epoxy resin is an oligomer containing two or more epoxy groups, and the epoxy resin has active epoxy groups in a molecular structure, so that the epoxy resin and various curing agents can be crosslinked to form a thermosetting three-dimensional crosslinking structure, so that excellent physical and mechanical properties, electric insulation properties, chemical resistance and adhesive properties are obtained, and the epoxy resin is widely applied to various fields. The alicyclic epoxy resin does not contain chlorine, sodium and other ions in the synthesis process, has good dielectric property, and is very suitable for processing and manufacturing metal sections. And because the alicyclic epoxy resin has low requirement on a curing agent due to excellent thermal stability and weather resistance, different curing agents can be used for curing. Meanwhile, the alicyclic epoxy resin has good processability and low viscosity, is not easy to bond when a product is cast and pressed, and is very convenient. However, like other types of epoxy resins, alicyclic epoxy resins have disadvantages of high brittleness, poor fatigue resistance, heat resistance, and impact resistance due to high crosslinking density and large internal stress, and commonly used solid curing agents have poor dispersibility in resins and are difficult to achieve rapid curing and poor in curing uniformity.

In order to overcome the disadvantages, improvement on the aspect of the curing agent is needed, and the performance of the epoxy resin is improved through the improvement of the formula proportion of the curing agent.

Disclosure of Invention

The invention aims to provide a preparation method of an epoxy resin curing agent for aluminum plate production, which solves the physical property defect of epoxy resin.

The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of an epoxy resin curing agent for aluminum plate production comprises the following steps;

pretreatment of raw materials: weighing N, N-Dimethylformamide (DMF), dapsone (DDS), 2-mezzanine (2MI) and Dicyandiamide (DICY), heating the DMF to 60 deg.C, and determining the particle size of Dicyandiamide (DICY);

mixing raw materials: pouring dapsone (DDS), 2-mezzanine (2MI) and Dicyandiamide (DICY) into N, N-Dimethylformamide (DMF) to obtain a mixed solution;

stirring at constant temperature: keeping the temperature of the mixed solution at 50 ℃, slowly stirring until the powder is dissolved, and obtaining a liquid curing agent without visible precipitation;

and (4) sealing and storing: and sealing the liquid curing agent in an air-tight manner, preserving heat and preserving for later use.

Preferably, in the raw material pretreatment step, the N, N-Dimethylformamide (DMF), dapsone (DDS), 2-mezzanine (2MI) and Dicyandiamide (DICY) are mixed in parts by mass: 30-50 parts of N, N-Dimethylformamide (DMF), 2-5 parts of dapsone (DDS), 8-13 parts of 2-methylzolmitanide (2MI) and 10-18 parts of Dicyandiamide (DICY).

Preferably, the 2-methylimidazoles (2MI) have a purity of more than 99%.

Preferably, the Dicyandiamide (DICY) is electronic grade Dicyandiamide (DICY).

Preferably, in the raw material mixing step, the next raw material is added after the previous raw material is completely infiltrated by the DFM.

Preferably, the DFM is continuously added during the raw material mixing step to avoid temperature drop from affecting dissolution efficiency.

Preferably, in the constant-temperature stirring step, the raw materials are poured into a stirrer to be stirred at the speed of 15-20 r/min.

Preferably, the temperature of the liquid curing agent is kept at 45 ℃ or higher during the sealed storage.

The invention has the following beneficial effects: the curing agent is prepared by mixing N, N-Dimethylformamide (DMF), dapsone (DDS), 2-methylimidazole (2MI) and Dicyandiamide (DICY), the final product is liquid, the dispersion effect in resin is good, the curing efficiency is high, the resin can be uniformly cured, the mechanical property difference among all parts can be reduced, meanwhile, various curing materials are mixed, and the physical property of resin curing is further improved.

Detailed Description

Example 1

Pretreatment of raw materials: weighing 40 parts of N, N-Dimethylformamide (DMF), 3 parts of dapsone (DDS), 12 parts of 2-methylimidazole (2MI) and 15 parts of electronic grade Dicyandiamide (DICY), and heating the N, N-Dimethylformamide (DMF) to 60 ℃;

mixing raw materials: pouring dapsone (DDS), 2-mezzanine (2MI) and Dicyandiamide (DICY) into N, N-Dimethylformamide (DMF) to obtain a mixed solution, and adding the next component after the former component is completely soaked;

stirring at constant temperature: keeping the temperature of the mixture at 50 ℃, placing the mixture into a stirrer, slowly stirring the mixture until the powder is dissolved, wherein the stirring speed is 18r/min, and stirring the mixture until no visible precipitate exists, thus obtaining a liquid curing agent;

and (4) sealing and storing: sealing and preserving the liquid curing agent in an air-isolated manner for later use, wherein the temperature is kept above 45 ℃.

Pouring a liquid curing agent into the epoxy resin raw material, uniformly stirring, curing for 60min at the temperature of 60 ℃, then heating to 100 ℃ for curing for 120min to obtain a cured epoxy resin sample 1

Example 2

Pretreatment of raw materials: weighing 45 parts of N, N-Dimethylformamide (DMF), 4 parts of dapsone (DDS), 12 parts of 2-methylimidazole (2MI) and 16 parts of electronic grade Dicyandiamide (DICY), and heating the N, N-Dimethylformamide (DMF) to 60 ℃;

mixing raw materials: pouring dapsone (DDS), 2-mezzanine (2MI) and Dicyandiamide (DICY) into N, N-Dimethylformamide (DMF) to obtain a mixed solution, and adding the next component after the former component is completely soaked;

stirring at constant temperature: keeping the temperature of the mixture at 50 ℃, placing the mixture into a stirrer, slowly stirring the mixture until the powder is dissolved, wherein the stirring speed is 18r/min, and stirring the mixture until no visible precipitate exists, thus obtaining a liquid curing agent;

and (4) sealing and storing: sealing and preserving the liquid curing agent in an air-isolated manner for later use, wherein the temperature is kept above 45 ℃.

And pouring the liquid curing agent into the epoxy resin raw material, uniformly stirring, curing for 60min at the temperature of 60 ℃, then heating to 100 ℃ and curing for 120min to obtain a cured epoxy resin sample 2.

Example 3

Pretreatment of raw materials: weighing 50 parts of N, N-Dimethylformamide (DMF), 5 parts of dapsone (DDS), 13 parts of 2-methylimidazole (2MI) and 18 parts of electronic grade Dicyandiamide (DICY), and heating the N, N-Dimethylformamide (DMF) to 60 ℃;

mixing raw materials: pouring dapsone (DDS), 2-mezzanine (2MI) and Dicyandiamide (DICY) into N, N-Dimethylformamide (DMF) to obtain a mixed solution, and adding the next component after the former component is completely soaked;

stirring at constant temperature: keeping the temperature of the mixture at 50 ℃, placing the mixture into a stirrer, slowly stirring the mixture until the powder is dissolved, wherein the stirring speed is 18r/min, and stirring the mixture until no visible precipitate exists, thus obtaining a liquid curing agent;

and (4) sealing and storing: sealing and preserving the liquid curing agent in an air-isolated manner for later use, wherein the temperature is kept above 45 ℃.

And pouring the liquid curing agent into the epoxy resin raw material, uniformly stirring, curing for 60min at the temperature of 60 ℃, then heating to 100 ℃ and curing for 120min to obtain a cured epoxy resin sample 3.

Comparative example 1

The difference from the examples is that the epoxy resin is cured by using a common amine curing agent to obtain epoxy resin sample 4.

The mechanical properties of each resin sample are measured by adopting a performance test method of an international standard method GB/T2567-

TABLE 1

Sample (I)	Sample 1	Sample 2	Sample 3	Sample No. 4
					Impact Strength (MPa)	50	54	57	36
Flexural Strength (kJ/m)2)	154	159	163	98

As can be seen from the final performance detection indexes, the improved liquid curing agent formula has good dispersion effect, so that all parts of the epoxy resin are uniformly cured in the curing process, and the mechanical property difference is small, so that the impact strength and the bending strength of the epoxy resin are obviously improved compared with the traditional curing agent, the mechanical property of the epoxy resin is effectively improved, and the epoxy resin is more suitable for manufacturing metal sections.

In summary, although the present invention has been described with reference to the preferred embodiments, the above-described preferred embodiments are not intended to limit the present invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention, therefore, the scope of the present invention shall be determined by the appended claims.