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Bio-based macromolecular flame retardant as well as preparation method and application thereof

A technology of bio-based macromolecules and flame retardants, applied in the field of flame retardants, can solve the problems of poor thermal stability of tannic acid, etc., to solve poor thermal stability, improve flame retardant effect, good thermal stability and flame retardancy Effect

Active Publication Date: 2020-11-03
江苏艾泰柯新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention proposes a bio-based macromolecular flame retardant and its preparation method and application. As a macromolecular intumescent flame retardant, it has good thermal stability and flame retardancy, and solves the problem of poor thermal stability of tannic acid. As a flame retardant curing agent for epoxy resin, it has little effect on the mechanical properties of epoxy resin

Method used

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  • Bio-based macromolecular flame retardant as well as preparation method and application thereof
  • Bio-based macromolecular flame retardant as well as preparation method and application thereof
  • Bio-based macromolecular flame retardant as well as preparation method and application thereof

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Embodiment 1

[0029] A preparation method of a bio-based macromolecular flame retardant, comprising the following steps:

[0030] (1) Preparation of tannin chlorinated phosphazene by grafting method: add 20g of tannic acid and 10mL of triethylamine to 100ml of acetonitrile to obtain a mixture, heat the mixture to 40°C, and add hexachlorotripolyphosphorus dropwise Add 20ml of nitrile to the mixture, then heat the mixture at 50°C for 2h to obtain a mixed solution containing tannin chlorinated phosphazene ester;

[0031] (2) Reaction of tannin chlorinated phosphazene ester with m-phenylenediamine: add 20 g of m-phenylenediamine to the mixed solution in step (1), heat to 70°C for 3 hours, filter and wash with acetonitrile to remove three Ethylamine salt and unreacted raw materials are dried to obtain a bio-based macromolecular flame retardant (TAFR), and the conversion rate of TAFR is 80-90%.

[0032] The bio-based macromolecule flame retardant is used for the preparation of flame-retardant ep...

Embodiment 2

[0064] A preparation method of a bio-based macromolecular flame retardant, comprising the following steps:

[0065] (1) Preparation of tannin chlorinated phosphazene by grafting method: 10 g of tannic acid and 5 mL of triethylamine were added to 50 mL of acetonitrile to obtain a mixture, the mixture was heated to 30 ° C, and hexachlorotripolyphosphorus was added dropwise Nitrile 10ml was added to the mixture, and then the mixture was heated at 50° C. for 1 h to obtain a mixed solution containing tannin chlorinated phosphazene ester;

[0066] (2) Reaction of tannin phosphazene chloride with m-phenylenediamine: add 10 g of m-phenylenediamine to the mixed solution in step (1), heat to 60°C for 2 hours, filter and wash with acetonitrile to remove three Ethylamine salt and unreacted raw materials are dried to obtain a bio-based macromolecular flame retardant (TAFR).

[0067] The bio-based macromolecule flame retardant is used for the preparation of flame-retardant epoxy resin, and...

Embodiment 3

[0072] A preparation method of a bio-based macromolecular flame retardant, comprising the following steps:

[0073] (1) Preparation of tannin chlorinated phosphazene by grafting method: 30g of tannic acid and 20mL of triethylamine were added to 200ml of acetonitrile to obtain a mixture, the mixture was heated to 45°C, and hexachlorotripolyphosphorus was added dropwise Add 40ml of nitrile to the mixture, and then heat the mixture at 50°C for 3h to obtain a mixed solution containing tannin chlorinated phosphazene ester;

[0074] (2) Reaction of chlorinated phosphonitrile tannin with m-phenylenediamine: add 30 g of m-phenylenediamine to the mixed solution in step (1), heat to 80°C for 4 hours, filter and wash with acetonitrile to remove three Ethylamine salt and unreacted raw materials are dried to obtain a bio-based macromolecular flame retardant (TAFR).

[0075] The bio-based macromolecule flame retardant is used for the preparation of flame-retardant epoxy resin, and the flam...

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Abstract

The invention provides a bio-based macromolecular flame retardant as well as a preparation method and application thereof. The preparation method comprises the following steps of (1) preparing tanninphosphonitrile chloride ester by a grafting method: adding 10-30g of tannin and 5-20mL of triethylamine into 50-200ml of acetonitrile to obtain a mixture, heating the mixture to 30-45 DEG C, dropwiseadding 10-40ml of phosphonitrilic chloride trimer into the mixture, and then heating the mixture at 50 DEG C for 1-3h to obtain a mixed solution containing tannin phosphonitrile chloride ester; and (2) enabling the tannin phosphonitrile chloride to react with metaphenylenediamine: adding 10-30g of the metaphenylenediamine into the mixed solution obtained in the step (1), performing heating to 60-80 DEG C, performing reacting for 2-4 hours, performing filtering, performing cleaning with the acetonitrile, and performing drying to obtain the bio-based macromolecular flame retardant. The flame retardant provided by the invention has good thermal stability and flame retardance, and solves the problem of poor thermal stability of the tannin, and besides, as a flame retardant curing agent, the reticular macromolecular structure has less influence on the mechanical properties of epoxy resins.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a bio-based macromolecular flame retardant and its preparation method and application. Background technique [0002] Epoxy resin (EP) is an important class of thermosetting resins and one of the most widely used matrix resins in polymer composites. The oxygen index of general-purpose epoxy resin is less than 20, which is a flammable material. As the electronics, electrical appliances, coatings and other industries put forward higher requirements for its flame retardancy, improving the flame retardancy of EP has attracted extensive attention of researchers at home and abroad. The most commonly used methods to improve the flame retardant properties of EP are divided into additive flame retardant technology and reactive flame retardant technology. At present, additive flame retardant technology is mostly used at home and abroad. The so-called additive flame retardant tec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/08C07H1/00C08G79/02C08G59/50C08G59/62
CPCC07H1/00C07H13/08C08G59/504C08G59/621C08G79/02
Inventor 高明李永鹏岳丽娜
Owner 江苏艾泰柯新材料科技有限公司
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