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Phosphorus-nitrogen intumescent epoxy resin flame retardant and preparation method thereof

A technology of epoxy resin and flame retardant, applied in the field of chemical synthesis agent and its preparation, to achieve the effect of simple preparation method, good mechanical properties and easy control

Active Publication Date: 2015-12-02
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, relevant studies have shown that advanced brominated epoxy resins will release irritating and corrosive substances such as hydrogen bromide, polybrominated dibenzoxanes (PBDDs) and polybrominated dibenzofurans (PBDFs) during combustion. Toxic gas, and polybrominated substances are strong carcinogens

Method used

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  • Phosphorus-nitrogen intumescent epoxy resin flame retardant and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The first step: to the equipped with reflux condenser, thermometer N 2 Add 27.5ml of phosphorus oxychloride to the 250ml three-necked flask of the introduction tube and magnet, then add 60ml of dichloromethane as solvent, add 62.5ml of DEA and 30ml of dichloromethane to the constant pressure dropping funnel to dilute. Pass N 2 Protected, start dropwise addition of EDA solution under ice bath for reaction, after completion of EDA dropwise, naturally warm up to room temperature for 8h reaction. After the reaction, a light yellow liquid slurry was obtained, and the liquid was filtered, washed, rotary evaporated, and dried to obtain a colorless transparent body.

[0026] The second step: add 8ml of glycidol in a 100ml three-necked flask equipped with magnetic stirring, dropping funnel and thermometer, then add 30ml of dichloromethane as solvent, add DPAD6.2ml and 20ml of dichloromethane in the dropping funnel to dilute, The dropwise addition was started under ice bath, an...

Embodiment 2

[0028] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.

[0029] Step two:

[0030] Step 2: Add 12ml of glycidol to a 100ml three-necked flask equipped with magnetic stirring, dropping funnel and thermometer, then add 40ml of dichloromethane as solvent, add 9.3ml of DPAD and 30ml of dichloromethane in the dropping funnel to dilute, place on ice The dropwise addition started under the bath, and after 1.5 hours of the dropwise addition, the temperature was naturally raised to room temperature, and reacted until no HCl gas was released, and the reaction was terminated, and a light yellow liquid could be obtained after treatment.

Embodiment 3

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

[0033] Step 2: Add 24ml of glycidol to a 250ml three-necked flask equipped with magnetic stirring, dropping funnel and thermometer, then add 60ml of dichloromethane as a solvent, add 18.6ml of DPAD and 80ml of dichloromethane in the dropping funnel to dilute, place on ice The dropwise addition started under the bath, and after 2 hours of the dropwise addition, the temperature was naturally raised to room temperature, and the reaction was continued until no HCl gas was released, and the reaction was terminated, and a light yellow liquid could be obtained after treatment.

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Abstract

The invention provides a phosphorus-nitrogen intumescent epoxy resin flame retardant and a preparation method thereof, relating to a chemical synthesis agent and a preparation method thereof. Preparation raw materials include phosphorus oxychloride, diethylamine and glycidol. The method for preparing the flame retardant comprises the following two steps: I. reacting phosphorus oxychloride (POCl3) and diethylamine (EDA) under certain conditions to generate a phosphorus-nitrogen intermediate diethylphosphoramidic dichloride (DPAD); II. stirring DPAD and glycidol to react for a certain time under the condition of inert gas import and carrying out filtration, washing, rotary evaporation, drying and other treatment on the product, thus obtaining a faint yellow liquid. The compound has good compatibility with epoxy resin, can be cured with epoxy resin into one, has smaller effects on the mechanical properties of cured products, can serve as an epoxy resin reactive diluent and can conduce to effectively improving the flame retardance of epoxy resin. The process is simple in production conditions, higher in product purity and yield and simple and convenient in after-treatment process.

Description

technical field [0001] The invention relates to a chemical synthesis agent and a preparation method thereof, in particular to a phosphorus and nitrogen expansion type epoxy resin flame retardant and a preparation method thereof. Background technique [0002] Epoxy resin is a kind of thermosetting polymer synthetic material with excellent properties such as good adhesion, corrosion resistance, insulation, and high strength. It has been widely used in the bonding of various metals and non-metallic materials, the manufacture of corrosion-resistant coatings, electrical insulation materials, FRP / composite materials, etc. And it plays an important role in electronics, electricity, machinery manufacturing, chemical anticorrosion, aerospace, ship transportation, chemical building materials, water conservancy and electric power and many other industrial fields, and has become an indispensable basic material in various industrial fields. However, the application of epoxy resin has on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08K5/5399C07F9/655
Inventor 梁兵王刚宁志高王长松
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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