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Phosphorous epoxy resin curing agent and preparation method thereof

An epoxy resin curing and solvent technology, which is applied in the field of phosphorus-containing epoxy resin curing agent and its preparation, can solve the problems of easy fire, application limitation, low oxygen index of epoxy resin, etc., and achieve simple post-treatment process and high production efficiency. Simple conditions, high product purity and high yield

Inactive Publication Date: 2011-05-25
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the oxygen index of epoxy resin is low (about 19.8), and it is a flammable substance. Continuous spontaneous combustion after leaving the fire is easy to cause fire, which greatly restricts its application. Therefore, to improve and improve the flame retardancy of epoxy resin, Has far-reaching implications for reducing fire hazards

Method used

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  • Phosphorous epoxy resin curing agent and preparation method thereof
  • Phosphorous epoxy resin curing agent and preparation method thereof
  • Phosphorous epoxy resin curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add ODOPB (3.243g, 0.01mol) and trimellitic anhydride acid chloride (4.220g, 0.02mol) to a 250ml four-necked flask equipped with a thermometer, nitrogen gas introduction, magnetron, reflux condenser and tail gas absorption device, and then add 100ml Toluene, heated to 110°C with stirring, reacted for 5 hours, and continued to pass N after the reaction 2 Bring to room temperature. Then the mixed solution was stirred and poured into 200ml of petroleum ether, a white precipitate was precipitated, filtered under reduced pressure, and the filter cake was washed with 100ml of petroleum ether, and dried at 120°C for 6 hours to obtain 3.106g of product BPA-ODOPE, the yield 46.2%, purity.

Embodiment 2

[0028] Add ODOPB (3.243g, 0.01mol) and trimellitic anhydride acid chloride (6.320g, 0.03mol) to a 250ml four-necked flask equipped with a thermometer, nitrogen gas introduction, magnetron, reflux condenser and tail gas absorption device, and then add 100ml Xylene, heated to 140°C under stirring, reacted for 5 hours, and continued to pass N after the reaction 2 Bring to room temperature. Then the mixed solution was stirred and poured into 200ml of petroleum ether, a white precipitate was precipitated, filtered under reduced pressure, and the filter cake was washed with 100ml of petroleum ether, and dried at 120°C for 6 hours to obtain 5.359g of product BPA-ODOPE, the yield 79.7%, purity.

Embodiment 3

[0030] Add ODOPB (3.243g, 0.01mol) and trimellitic anhydride acid chloride (6.320g, 0.03mol) to a 250ml four-necked flask equipped with a thermometer, nitrogen gas introduction, magnetron, reflux condenser and tail gas absorption device, and then add 100ml Chlorobenzene, heated to 130°C with stirring, reacted for 5 hours, and continued to pass N after the reaction 2 Bring to room temperature. Then the mixed solution was stirred and poured into 200ml of petroleum ether, a white precipitate was precipitated, filtered under reduced pressure, and the filter cake was washed with 100ml of petroleum ether, and dried at 120°C for 6 hours to obtain 5.554g of product BPA-ODOPE, the yield 82.6%, purity.

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Abstract

The invention provides a phosphorous epoxy resin curing agent and a preparation method thereof, relating to a curing agent and a preparation method thereof. In the preparation method for synthesizing the phosphorous epoxy resin curing agent BPA-ODOPE, the mole ratio of trimellitic anhydride chloride to ODOPB ranges from (2:1) to (10:1), organic solvents are benzene, toluene and the like, inert gases are nitrogen, argon and helium, and the inert solvents for precipitation and washing are petroleum ether, pentane and the like. The preparation method comprises the following steps of: 1, adding the trimellitic anhydride chloride and the ODOPB in a reactor, adding the organic solvents, stirring under the protection of the inert gases, and obtaining the compound BPA-ODOPE; and 2, cooling the reaction mixing liquid, precipitating in the inert solvents to separate out the BPA-ODOPE, vacuum filtering, washing the precipitate with the inert solvents, drying, and obtaining white or yellowish powder-shaped product. The compound can be used as a curing agent applied in epoxy resin and also as halogen-free fire retardant.

Description

technical field [0001] The invention relates to a curing agent and a preparation method thereof, in particular to a phosphorus-containing epoxy resin curing agent and a preparation method thereof. Background technique [0002] Epoxy resin has been widely used in many fields due to its excellent performance, and has become an extremely important type of thermosetting resin. In recent years, with the rapid development of the electrical and electronic industry, epoxy resin has also been widely used in the fields of electronic component bonding, packaging, and printed circuit board (PCBs) production, and has become one of the most important electronic chemical materials. . However, the oxygen index of epoxy resin is low (about 19.8), and it is a flammable substance. Continuous spontaneous combustion after leaving the fire is easy to cause fire, which greatly restricts its application. Therefore, to improve and improve the flame retardancy of epoxy resin, It has far-reaching si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/42C07F9/6574C08L63/02
Inventor 梁兵曹俊王长松宁志高
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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