Modified novel epoxy insulating resin matrix and preparation method thereof

文档序号:1264469 发布日期:2020-08-25 浏览:27次 中文

阅读说明:本技术 改性新型环氧绝缘树脂基体及其制备方法 (Modified novel epoxy insulating resin matrix and preparation method thereof ) 是由 马超强 马宏 马奎 张桂苹 马俊 赵梦洋 孙振 李雨含 于 2020-04-13 设计创作,主要内容包括:本发明公开了改性新型环氧绝缘树脂基体及其制备方法,首先,将双氰胺8.4kg与改性剂乙二胺6.0kg加入300kg 0.8mol/L的盐酸溶液中,加热至180℃,进行反应,每隔1小时进行减压除去反应产生的氨气,反应4小时,反应结束后,冷却、过滤,25℃室温干燥,得到固化剂;然后将5kg固化剂超声溶解于30kg乙醇中;然后,将含有固化剂的乙醇溶液与80kg环氧树脂均匀混合,得到混合体系;最后,将混合体系在25℃、-0.1MPa下进行减压干燥,至无乙醇蒸出,得到环氧绝缘树脂基体,本发明克服了现有技术的不足,制备的环氧绝缘树脂基体的室温贮存稳定性良好,起始固化温度低。(The invention discloses a modified novel epoxy insulating resin matrix and a preparation method thereof, and the preparation method comprises the following steps of firstly, adding 8.4kg of dicyandiamide and 6.0kg of modifier ethylenediamine into 300kg of 0.8mol/L hydrochloric acid solution, heating to 180 ℃, reacting, decompressing every 1 hour to remove ammonia gas generated by the reaction, reacting for 4 hours, cooling and filtering after the reaction is finished, and drying at 25 ℃ room temperature to obtain a curing agent; then 5kg of curing agent is ultrasonically dissolved in 30kg of ethanol; then, uniformly mixing the ethanol solution containing the curing agent with 80kg of epoxy resin to obtain a mixed system; and finally, drying the mixed system at 25 ℃ and under-0.1 MPa under reduced pressure until no ethanol is evaporated to obtain the epoxy insulating resin matrix.)

1. The modified novel epoxy insulating resin matrix and the preparation method thereof are characterized in that the raw materials comprise a curing agent and epoxy resin.

2. The modified novel epoxy insulating resin matrix and the preparation method thereof as claimed in claim 1, wherein the raw materials comprise 3-8 parts of curing agent and 70-80 parts of epoxy resin.

3. The modified novel epoxy insulating resin matrix and the preparation method thereof according to claim 1 or 2, characterized in that: the curing agent is dicyandiamide.

4. The modified novel epoxy insulating resin matrix and the preparation method thereof according to claim 1 or 2, characterized in that the curing agent is modified dicyandiamide, and the modification method of the modified dicyandiamide is as follows: adding 84 parts by weight of dicyandiamide and 60 parts by weight of modifier ethylenediamine into 300 parts of 0.8mol/L hydrochloric acid solution, heating to 180 ℃, reacting, decompressing every 1 hour to remove ammonia gas generated by the reaction, reacting for 4-12 hours, cooling, filtering and drying at room temperature after the reaction is finished to obtain the curing agent.

5. The method for preparing any of the modified novel epoxy insulating resin matrices and the methods for preparing the same according to claims 1-4, characterized by comprising the following steps: firstly, dissolving 3-8 parts of curing agent in 20-30 parts of ethanol by ultrasonic waves; then, uniformly mixing the ethanol solution containing the curing agent with 70-80 parts of epoxy resin to obtain a mixed system; and finally, drying the mixed system at 20-35 ℃ and under the pressure of-0.1 MPa under reduced pressure until no ethanol is evaporated out to obtain the epoxy insulating resin matrix.

Technical Field

The invention relates to the technical field of epoxy insulating resin matrixes, and particularly belongs to a modified novel epoxy insulating resin matrix and a preparation method thereof.

Background

Currently, in the production of fishing rods, the most used resin matrix is high-temperature cured phenolic resin and medium-temperature cured epoxy resin. The phenolic resin has the advantages of low price and the like, but can only be used for producing lower-grade fishing rods because water and other low molecular products are discharged in the curing process, so that a plurality of micropores and bubbles are generated in the blank and on the surface, and the mechanical property and the appearance of the product are influenced. Epoxy resin does not discharge low molecular products in the curing process, the surface of the product is smooth and compact, and the product has excellent mechanical properties, so that the epoxy resin is generally adopted as matrix resin of a fishing rod in the production of high-grade fishing rods such as carbon fiber fishing rods and mixed fiber fishing rods. However, the existing epoxy resin has the following disadvantages: firstly, epoxy resin is easy to cure at low temperature, so that production raw materials cannot be stored for a long time; second, the initial curing temperature of the epoxy resin is high, which increases the production cost.

Disclosure of Invention

The invention aims to provide a novel modified epoxy insulating resin matrix for fishing gear products and a preparation method thereof, and solves the problems that epoxy resin in the prior art is easy to cure at low temperature and has high initial curing temperature.

In order to solve the problems, the technical scheme adopted by the invention is as follows:

the novel modified epoxy insulating resin matrix comprises a curing agent and epoxy resin.

Preferably, the raw materials comprise 3-8 parts of curing agent and 70-80 parts of epoxy resin.

Preferably, the curing agent is dicyandiamide.

Preferably, the curing agent is modified dicyandiamide, and the modification method of the modified dicyandiamide is as follows: adding 84 parts by weight of dicyandiamide and 60 parts by weight of modifier ethylenediamine into 300 parts by weight of 0.8mol/L hydrochloric acid solution, heating to 180 ℃, and reacting, wherein the reaction equation is as follows:

and (3) reducing the pressure every 1 hour to remove ammonia gas generated by the reaction, reacting for 4-12 hours, cooling, filtering and drying at room temperature after the reaction is finished to obtain the curing agent.

The preparation method of the modified novel epoxy insulating resin matrix for the fishing gear product comprises the following steps: firstly, dissolving 3-8 parts of curing agent in 20-30 parts of ethanol by ultrasonic waves; then, uniformly mixing the ethanol solution containing the curing agent with 70-80 parts of epoxy resin to obtain a mixed system; and finally, drying the mixed system at 20-35 ℃ and under the pressure of-0.1 MPa under reduced pressure until no ethanol is evaporated out to obtain the epoxy insulating resin matrix.

Compared with the prior art, the invention has the following implementation effects: the invention adopts hexanediamine to modify dicyandiamide to prepare the curing agent, the terminal amino group is also subjected to deamination polycondensation while the cyano group is subjected to addition reaction, and the molecular weight is gradually increased along with the extension of the reaction time; but the molecular weight is increased, the average polymerization degree is increased, the lattice spacing is increased, and doping and lattice distortion occur; when the polymerization degree is larger, a large number of incomplete crystals exist in the structure, the molecules of the curing agent break the diffusion of crystal lattices into an epoxy resin system, the curing reaction is accelerated, and the curing peak temperature is reduced by 30 ℃; but the curing agent with smaller polymerization degree has more complete crystal lattices, only amino, biguanidino, hexyl and epoxy resin in the curing agent have poorer compatibility, and only when the curing reaction is started and the molecular chain of the curing agent is connected with the epoxy resin chain segment, the amino, biguanidino, hexyl and epoxy resin can start to be compatible and mutually diffuse to further perform the curing reaction, and simultaneously, the initial curing temperature is reduced by 80 ℃ due to the introduction of a strong electron-donating group, but the storage performance at low temperature is improved; the epoxy insulating resin matrix prepared by the invention has good room temperature storage stability and low initial curing temperature.

Drawings

FIG. 1 is an infrared spectrum of hexamethylenediamine, dicyandiamide and the curing agent of examples 2-4.

FIG. 2 is a 1H-NMR spectrum of the curing agent in examples 2 to 4.

FIG. 3 is an XRD diffraction pattern of the curing agents of examples 2-4.

FIG. 4 is a DSC chart of the epoxy insulating resin matrix in examples 1 to 4.

FIG. 5 is a graph showing the relationship between the storage time and the transition rate at room temperature of the epoxy insulating resin matrix in examples 2 to 4.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The epoxy resin used in the invention adopts a product produced by the North Hebei jumping anticorrosive material company Limited, and other raw materials are all industrial pure raw materials.

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