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Pentaerythritol derivative based intumescent flame retardant and preparation method thereof

The technology of intumescent flame retardant and pentaerythritol is applied in the field of flame retardant of organic polymer materials, which can solve the problems of insufficient environmental protection of organic flame retardants, and achieve the effects of excellent smoke suppression performance, combustion prevention and flame retardant performance.

Active Publication Date: 2017-01-25
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the defect of insufficient environmental protection of existing organic flame retardants, the present invention provides an intumescent flame retardant of pentaerythritol derivatives and a preparation method thereof. The obtained flame retardant has good compatibility with polymer resins and does not affect Mechanical properties of polymer materials, while obtaining good flame retardant effect

Method used

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  • Pentaerythritol derivative based intumescent flame retardant and preparation method thereof
  • Pentaerythritol derivative based intumescent flame retardant and preparation method thereof
  • Pentaerythritol derivative based intumescent flame retardant and preparation method thereof

Examples

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Effect test

Embodiment 1

[0031] 3,9-bis-(4,6-di-phenoxy-[1,3,5]triazine-2-oxo)-2,4,8,10-tetraoxa-3,9-di Preparation of boron-spiro[5.5]undecane (PTBO)

[0032] Step 1: Add 3.2g of boric acid and 6.8g of pentaerythritol into a three-necked flask, add 40ml of toluene as a water-carrying agent, stir and reflux until the water in the water separator no longer increases, keep the temperature and continue the reaction for 2 hours, evaporate to dryness and carry water agent, a whitish solid;

[0033] The second step: the white solid obtained in the first step is recrystallized with acetone, filtered, and dried to obtain intermediate product 1;

[0034] The third step: take by weighing 7.5g intermediate product 1 and 2.4g sodium hydroxide and be dissolved in distilled water, reflux 1 hour, be cooled to room temperature, add the acetone solution of cyanuric chloride in proportion (15.5g of cyanuric chloride, Acetone 30ml), specifically add in three times, add one-third every 15min; react for 4 hours, carry o...

Embodiment 2

[0041] 3,9-bis-(4,6-di-phenoxy-[1,3,5]triazine-2-oxo)-2,4,8,10-tetraoxa-3,9-di Preparation of boron-spiro[5.5]undecane (PTBO)

[0042]Step 1: Add 6.5g of boric acid and 14g of pentaerythritol into a three-necked flask, add 80ml of toluene as a water-carrying agent, stir and reflux until the water in the water separator does not increase, keep the temperature and continue to react for 2 hours, then evaporate to dry the water-carrying agent , with a white solid;

[0043] The second step: the white solid obtained in the first step is recrystallized with acetone, filtered, and dried to obtain intermediate product 1;

[0044] The third step: take 15g intermediate product 1 and 5g sodium hydroxide and dissolve in distilled water, reflux for 1 hour, cool to room temperature, add the acetone solution of cyanuric chloride (31g of cyanuric chloride, 60ml of acetone) in batches in proportion , add in three times, add one-third every 15min, react for 4 hours, and filter the crude produc...

Embodiment 3

[0048] 3,9-bis-(4,6-di-phenoxy-[1,3,5]triazine-2-oxo)-2,4,8,10-tetraoxa-3,9-di Preparation of boron-spiro[5.5]undecane (PTBO)

[0049] Step 1: Add 9.8g of boric acid and 20.7g of pentaerythritol into a three-necked flask, add 120ml of toluene as a water-carrying agent, stir and reflux until the water in the water separator does not increase, keep the temperature and continue to react for 3 hours, evaporate to dryness and carry water agent, a whitish solid;

[0050] The second step: the white solid obtained in the first step is recrystallized with acetone, filtered, and dried to obtain intermediate product 1;

[0051] The third step: take by weighing 22.5g intermediate product 1 and 7.2g sodium hydroxide and dissolve in distilled water, reflux for 3 hours, cool to room temperature, add the acetone solution of cyanuric chloride in batches in proportion (46.3g of cyanuric chloride, Acetone 100ml), add in three times, add one-third every 15min, react for 5 hours, carry out sucti...

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Abstract

The invention discloses a pentaerythritol derivative based intumescent flame retardant and a preparation method thereof. In the preparation process, the method comprises the steps of mixing pentaerythritol and boric acid, taking methylbenzene as a water carrying agent, stirring and backflowing until moisture in a water knockout vessel is no more increased, obtaining a product, recrystallizing, filtering and drying to obtain an intermediate product 1; dissolving the intermediate product 1 and sodium hydroxide in distilled water, backflowing, cooling to the room temperature, adding a cyanuric chloride acetone solution in batches, reacting, and suction-filtering; purifying to obtain an intermediate product 2; dissolving phenol and N,N-diisopropylethylamine in methylbenzene under the protection nitrogen, slowly adding into a methylbenzene solution of the intermediate product 2, stirring for 1-3 hours, gradually raising the temperature to 80 DEG C, stirring for reaction for 2-5 hours, filtering, and removing a solvent in a filtrate to obtain a solid product; repeatedly washing with water and acetone, and drying in vacuum to obtain the pentaerythritol derivative based intumescent flame retardant. The product PTBO can serve as an excellent environment-friendly flame retardant.

Description

technical field [0001] The invention relates to an intumescent flame retardant, in particular to an intumescent flame retardant based on pentaerythritol derivatives and a preparation method thereof, belonging to the technical field of flame retardant of organic polymer materials. Background technique [0002] Although polymer materials play an important role in various fields, most polymer materials are flammable. Therefore, it is very important to develop flame-retardant polymer materials. The flame retardancy of polymer materials is closely related to flame retardants. Organic flame retardants are a class of commonly used flame retardants, including halogenated flame retardants, organophosphorus flame retardants, etc., but halogenated flame retardants and organophosphorus flame Disadvantages such as dripping and poor thermal stability. Therefore, the development of halogen-free, low toxicity, smoke suppression, and high-efficiency organic flame retardants has become the...

Claims

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Application Information

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IPC IPC(8): C08K7/22C08K5/55C07F5/04C08L63/00
CPCC07F5/04C08K5/55C08K7/22C08L2201/02C08L63/00
Inventor 张晓远李艳刘平陈珊珊张铁刘伟时潘永红刘东发徐添贵
Owner SOUTH CHINA UNIV OF TECH
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