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Reactive epoxy resin flame-retardant curing agent containing phosphorus and nitrogen and preparation method thereof

A technology of epoxy resin and intumescent flame retardant, which is applied in the field of chemical synthesis and its preparation, can solve the problems of few varieties of excellent flame retardants, poor compatibility of flame retardants, and few halogen-free flame retardants, etc., and achieve The preparation method is simple, the post-treatment is convenient, and the effect of mild conditions

Inactive Publication Date: 2015-08-05
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are very few varieties of halogen-free flame retardants that can be applied to the market at present, and it is urgent to develop new products suitable for industrialization
[0006] At present, the halogen-free flame retardants researched more at home and abroad mainly include phosphorus-based, nitrogen-based, boron-based, silicon-based inorganic hydroxides and composite intumescent flame retardants, but these flame retardants have problems such as compatibility Due to the problems of poor performance, easy leakage, poor thermal stability, and high price, there are still few excellent flame retardants that can be widely used, and they need to be further studied by scientific researchers.

Method used

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  • Reactive epoxy resin flame-retardant curing agent containing phosphorus and nitrogen and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0029] The first step: to the equipped with reflux condenser, thermometer N 2 Add 13.62g of pentaerythritol and 23.8ml of phosphorus oxychloride into the 250ml three-necked bottle of the introduction tube and magnet, then add 80ml of chlorobenzene as solvent, 0.3g of AlCl 3 as a catalyst. Pass N 2 Protected, the temperature was raised to 60°C to start the reaction, after 1 hour, the temperature was raised to 80°C for 3 hours, and then the temperature was raised to 100°C for 8 hours. Pass N after the reaction 2 Protected and cooled to room temperature, a white liquid was obtained. After the liquid was filtered, washed and dried, a white powdery solid was obtained.

[0030] Step 2: Add 8.91g of SPDPC and 40ml of acetonitrile to a 250ml three-neck flask equipped with magnetic stirring, dropping funnel and thermometer, add 8.93g of DDS to the dropping funnel and dissolve it with 20ml of acetonitrile, and wait for the temperature to rise to 65°C to start dropping Add, keep ...

Embodiment 2

[0032] The first step: the synthetic method of phosphorus-containing intermediate is the same as embodiment 1.

[0033] Step two:

[0034] Step 2: Add 17.82g of SPDPC and 60ml of acetonitrile to a 250ml three-necked flask equipped with magnetic stirring, dropping funnel and thermometer, add 17.86g of DDS to the dropping funnel and dissolve it with 40ml of acetonitrile, and wait for the temperature to rise to 65°C to start dropping Add, keep the temperature at 90°C for 2 hours to react until no HCl gas is released, then slowly cool down to room temperature, filter, wash with 100ml of dichloromethane and 300ml of cold water, and dry at 50°C to obtain a white powdery solid .

Embodiment 3

[0036] The first step: the synthetic method of phosphorus-containing intermediate is the same as embodiment 1.

[0037] Step 2: Add 26.73g of SPDPC and 80ml of acetonitrile in a 250ml three-necked flask equipped with magnetic stirring, dropping funnel and thermometer, add 26.8g of DDS in the dropping funnel and dilute with 50ml of acetonitrile, wait until the temperature rises to 65°C and start dropping Add, keep the temperature at 90°C for 2 hours to react until no HCl gas is released, then slowly cool down to room temperature, filter, wash with 150ml of dichloromethane and 400ml of cold water, and dry at 50°C to obtain a white powdery solid .

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Abstract

The invention relates to a chemical synthesis agent and a preparation method thereof and provides a reactive epoxy resin flame-retardant curing agent containing phosphorus and nitrogen and a preparation method thereof. Raw materials for preparation of the curing agent comprise pentaerythritol, phosphorus oxychloride and 4,4-diamino diphenyl sulfone (DDS). The preparation method for the curing agent comprises the following two steps: step 1, reacting pentaerythritol (PER) with phosphorus oxychloride (POCl3) under certain conditions so as to produce a phosphorus-containing intermediate, i.e., pentaerythritol bisphosphorate diphosphoryl choloride (SPDPC); and step 2, subjecting SPDPC and DDS to a stirring reaction for a certain period of time under the condition of introduction of inert gas and subjecting a product to filtration, washing, drying and the like so as to obtain a white powder which is a phosphorus-nitrogen intumescent flame retardant. The reactive epoxy resin flame-retardant curing agent has high heat stability, expansibility and char yield and can be used as a flame retardation additive to a plurality of polymer materials so as to improve the flame retardant property of the polymer materials. The preparation method provided by the invention has the advantages of simple production conditions, high product purity, high yield and simple and convenient post treatment.

Description

technical field [0001] The invention relates to a chemical synthesis agent and a preparation method thereof, in particular to a phosphorous and nitrogen reactive epoxy resin flame retardant 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 retard...

Claims

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Application Information

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IPC IPC(8): C08G59/50C08G79/04
Inventor 梁兵王刚宁志高王长松
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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