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Epoxy resin curing agent and preparation method thereof

An epoxy resin curing and solvent technology, applied in the field of epoxy resin curing agent and its preparation, can solve the problems of poor dispersion and compatibility of additives, reduce the mechanical properties of epoxy resin, etc., achieve high synergistic flame retardancy, avoid The effect of poor matrix compatibility and simple preparation process

Inactive Publication Date: 2014-03-19
IND RES INST ZHIJIANG COLLEGE OF ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The epoxy resin curing agent sold in the existing market can only play the role of curing and crosslinking. If it is necessary to improve the heat resistance and flame retardancy of the epoxy resin, it needs to be filled with other functional additives to meet the relevant technical requirements. To a certain extent, there are problems of poor dispersion and compatibility of additives in the matrix, thereby reducing the defects in the mechanical properties of epoxy resins

Method used

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  • Epoxy resin curing agent and preparation method thereof
  • Epoxy resin curing agent and preparation method thereof
  • Epoxy resin curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The synthesis of epoxy resin curing agent is realized through the following steps:

[0031] (1) In a 100mL three-neck flask equipped with a magnetic rotor stirring, a condenser, and a thermometer, dissolve hexachlorocyclotriphosphazene (6.94g, 0.02mol) prepared by multiple sublimation in 50mL of tetrahydrofuran (THF) solvent, drop Add the prepared (9.28g, 0.08mol) THF solution of sodium phenate, and react at 40°C for 12 hours under nitrogen protection; remove THF by rotary distillation, wash with deionized water several times, and vacuum dry at 50°C for 24 hours. A milky white colloid is obtained. Among them, the preparation method of sodium phenate is: under the protection of nitrogen, (1.84g, 0.08mol) metal sodium and (7.52g, 0.08mol) phenol are reacted in 50mL THF solution at 25°C for 2 hours.

[0032] (2) Dissolve (4.36g, 0.04mol) p-aminophenol in 50mL tetrahydrofuran (THF) solvent in a 100mL three-neck flask equipped with magnetic rotor stirring, condenser and the...

Embodiment 2

[0035] The synthesis of epoxy resin curing agent is realized through the following steps:

[0036] (1) In a 100mL three-neck flask equipped with a magnetic rotor stirring, a condenser, and a thermometer, dissolve hexachlorocyclotriphosphazene (3.47g, 0.01mol) prepared by multiple sublimation in 50mL of tetrahydrofuran (THF) solvent, drop Add the prepared (4.64g, 0.04mol) sodium phenoxide THF solution, and react at 40°C for 12 hours under nitrogen protection; remove THF by rotary distillation, wash with deionized water several times, and vacuum dry at 50°C for 24 hours to obtain Milky white colloid. Among them, the preparation method of sodium phenate is: under the protection of nitrogen, (0.92g0.04mol) metal sodium and (3.76g0.04mol) phenol are reacted in 50mL THF solution at 25°C for 2 hours.

[0037] (2) Dissolve (2.18g, 0.02mol) p-aminophenol in 50mL tetrahydrofuran (THF) solvent in a 100mL three-necked flask equipped with magnetic rotor stirring, condenser and thermometer...

Embodiment 3

[0040] The synthesis of epoxy resin curing agent is realized through the following steps:

[0041] (1) In a 100mL three-neck flask equipped with a magnetic rotor stirring, a condenser, and a thermometer, dissolve hexachlorocyclotriphosphazene (34.70g, 0.10mol) prepared by multiple sublimation in 50mL of tetrahydrofuran (THF) solvent, drop Add the prepared (46.40g, 0.40mol) sodium phenoxide THF solution, and react at 40°C for 12 hours under nitrogen protection; remove THF by rotary distillation, wash with deionized water several times, and vacuum dry at 50°C for 24 hours to obtain Milky white colloid. Among them, the preparation method of sodium phenate is: under the protection of nitrogen, (9.20g0.40mol) metallic sodium and (37.60g0.40mol) are reacted in 50mL THF solution at 25°C for 2 hours.

[0042] (2) Dissolve (21.80g, 0.20mol) p-aminophenol in 50mL tetrahydrofuran (THF) solvent in a 100mL three-necked flask equipped with magnetic rotor stirring, condenser and thermometer...

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Abstract

The invention relates an epoxy resin curing agent and a preparation method thereof, belonging to the technical field of auxiliary synthesis. A preparation process of the epoxy resin curing agent comprises synthesis of a first intermediate, synthesis of a second intermediate and synthesis of an end product. The preparation method specifically comprises the following steps: under protection of an inert atmosphere, dissolving phosphonitrilic chloride trimer in a solvent tetrahydrofuran, dropwise adding tetrahydrofuran liquor of sodium phenoxide, and reacting to obtain the first intermediate; dissolving aminophenol into the solvent tetrahydrofuran, dropwise adding tetrahydrofuran liquor of sodium hydride, and curing to obtain the second intermediate; and obtaining the product by reacting the first intermediate with the second intermediate. The curing agent obtained by adopting the technical scheme disclosed by the invention has characteristics of being simple to synthesize and prepare, high in thermal stability and high in high-temperature solid residual rate, contains a large number of nitrogen-phosphor elements, and has excellent halogen-free flame-retardant performance.

Description

technical field [0001] The invention relates to an epoxy resin curing agent and a preparation method thereof, belonging to the technical field of auxiliary agent synthesis. Background technique [0002] Epoxy resin is currently the most widely used thermosetting resin material in industry. Due to its poor performance, it can only show good physical and chemical properties after curing with a curing agent to form a three-dimensional cross-linked network structure. The surface of metal and non-metal materials has the advantages of excellent bonding strength, high and low temperature resistance, good dielectric properties, small shrinkage, easy processing and molding, stable to alkali and most solvents, so it is widely used in aerospace, electronic packaging , light industry, construction, machinery and other fields. [0003] The main research of epoxy resin chemistry is curing agent. Generally, epoxy resin curing agent can be used alone in its original state, or it can be use...

Claims

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Application Information

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IPC IPC(8): C08G59/50C07F9/6593
Inventor 赵正平计建炳
Owner IND RES INST ZHIJIANG COLLEGE OF ZHEJIANG UNIV OF TECH
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