Halogen-free epoxy resin flame retardant and preparation method thereof
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A halogenated epoxy resin and flame retardant technology, applied in the field of chemical synthesis agent and its preparation, to achieve the effects of high purity, easy control and convenient post-processing
Active Publication Date: 2015-12-02
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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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
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Embodiment 1
[0025] 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 Protection, 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.
[0026] Step 2: Add 5.94g of SPDPC to a 100ml three-necked flask equipped with magnetic stirring, dropping funnel and thermometer, then add 30ml of DMF as a solvent, add 3.4ml of glycidol and 10ml of DMF solvent in the dropping funnel to dilute, start under ice bath Add dropwise, after 1.5h dropwise addition, na...
Embodiment 2
[0028] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.
[0029] Step 2: Add SPDPC11.88g into a 100ml three-necked flask equipped with magnetic stirring, dropping funnel and thermometer, then add 40ml of DMF as a solvent, add 6.8ml of glycidol and 15ml of DMF solvent in the dropping funnel to dilute, start under ice bath Add dropwise, after 2 hours of dropwise addition, naturally warm up to room temperature, react until no HCl gas is released, and end the reaction, after treatment, a milky white liquid can be obtained.
Embodiment 3
[0031] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.
[0032] Step 2: Add SPDPC23.76g into a 250ml three-necked bottle equipped with magnetic stirring, dropping funnel and thermometer, then add 100ml of DMF as solvent, add 17ml of glycidol and 25ml of DMF solvent in the dropping funnel to dilute, and start dripping under ice bath Add, after 2 hours of dropwise addition, naturally warm up to room temperature, react until no HCl gas is released, and end the reaction, after treatment, a milky white liquid can be obtained.
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Abstract
The invention provides a halogen-free epoxy resin flame retardant and a preparation method thereof, relating to a chemical synthesis agent and a preparation method thereof. Preparation raw materials include pentaerythritol (PER), phosphorus oxychloride and glycidol. The method for preparing the flame retardant comprises the following two steps: I. reacting PER and phosphorus oxychloride (POCl3) under certain conditions to generate an intermediate PER diphosphonic chloride diphosphate (SPDPC); and II. stirring SPDPC 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 milk white liquid. The halogen-free epoxy resin flame retardant and the preparation method have the beneficial effects that the obtained compound has a halogen-free structure and has good compatibility with epoxy resin; epoxy groups at the two ends of the compound have smaller effects on the mechanical properties of cured products; the compound can conduce to effectively improving the mechanical properties of epoxy resin, is also environment-friendly and is an environment-friendly flame retardant; and 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 halogen-free epoxy resin flame retardant and a preparation method thereof. Background technique [0002] Epoxy resin (EP) is the most widely used matrix resin for polymer matrix composites. EP is a kind of thermosetting resin, which came out in 1930 and has a history of more than 50 years since the United States realized industrial production in 1947. Epoxy resin is widely used because of its excellent bonding performance, abrasion resistance, mechanical properties, chemical stability, electrical insulation, low shrinkage, easy processing, good stress transmission and low cost. Coatings, adhesives, light industry, construction, machinery, aerospace, electrical and electronic insulation materials, advanced composite materials and other fields. However, the application of epoxy resin has one of the biggest disadvantages, that is, it is easy to burn,...
Claims
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