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Long-chain triazine macromolecular flame retardant with bicyclic phosphate structure and preparation method thereof

A bicyclic phosphate, triazine-based technology, used in fire-resistant coatings and other directions, can solve the problems of material mechanical and mechanical properties, uneven distribution of components, moisture absorption of flame retardants, etc., to improve the mechanical behavior of materials. Simple preparation process and high carbon formation rate

Active Publication Date: 2014-06-04
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional composite intumescent flame retardant system is made by mixing components such as carbon source, acid source, and foaming source. These components are mostly small molecular compounds. This mixture will inevitably lead to uneven distribution of components in the material. Average, the mechanical and mechanical properties of the material are significantly reduced, and the flame retardants have problems such as moisture absorption, easy migration and seepage

Method used

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  • Long-chain triazine macromolecular flame retardant with bicyclic phosphate structure and preparation method thereof
  • Long-chain triazine macromolecular flame retardant with bicyclic phosphate structure and preparation method thereof
  • Long-chain triazine macromolecular flame retardant with bicyclic phosphate structure and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0036] Embodiment 1: Under the protection of high-purity nitrogen, put 1.84g (10mmol) cyanuric chloride in the reactor, add 50mL N,N-dimethylacetamide in the reaction vessel, stir for 10-30 minutes to make The cyanuric chloride is evenly dispersed, after adding 2.09mL (12mmol) N, N-diisopropylethylamine and 1.80g (10mmol) PEPA, continue stirring for a period of time to make the reactants evenly disperse, react at 50°C for 24 hours, then 4.35 mL (25 mmol) of N,N-diisopropylethylamine and 1.08 g (10 mmol) of p-phenylenediamine were sequentially added to the reaction vessel. Raise the reaction temperature to 80°C, stir and react for 8 hours, then raise the reaction temperature to 120°C, stir and react for 10 hours, stop the reaction, cool, precipitate the product with acetone, filter with acetone, wash with a large amount of acetone, 80°C Dry under vacuum for 32 hours to obtain a long-chain triazine macromolecular flame retardant with a bicyclic phosphate structure.

Embodiment 2

[0037] Embodiment 2: under the protection of high-purity nitrogen, put 1.84g (10mmol) cyanuric chloride in the reactor, add 50mLN in the reaction vessel, N-dimethylacetamide, stir for 10-30 minutes to make three Polycyanogen chloride is dispersed evenly, after adding 2.09mL (12mmol) N, N-diisopropylethylamine and 1.80g (10mmol) PEPA, continue to stir for a period of time to make the reactants evenly dispersed, react at 50°C for 24 hours, and then add 4.35 mL (25 mmol) of N,N-diisopropylethylamine and 1.98 g (10 mmol) of diaminodiphenylmethane were sequentially added to the reaction vessel. Raise the reaction temperature to 80°C, stir and react for 10 hours, then raise the reaction temperature to 110°C, stir and react for 10 hours, stop the reaction, cool, precipitate the product with ethanol, filter with suction, wash with a large amount of ethanol, and put it under 80°C Vacuum drying for 48 hours to obtain a long-chain triazine macromolecular flame retardant with a bicyclic p...

Embodiment 3

[0038] Embodiment 3: under the protection of high-purity nitrogen, put 1.84g (10mmol) cyanuric chloride into the reactor, add 50mLN in the reaction vessel, N-dimethylacetamide, stir for 10-30 minutes to make three Polycyanogen chloride is dispersed evenly. After adding 1.66g of anhydrous potassium carbonate (12mmol) and 1.80g (10mmol) of PEPA, continue to stir for a period of time to make the reactants evenly dispersed. After 24 hours of reaction at 50°C, add 3.45g (25mmol) of anhydrous potassium carbonate and 2.00g (10mmol) of diaminodiphenyl ether. Raise the reaction temperature to 70°C, and stir the reaction for 6 hours. Raise the reaction temperature to 120°C, stir and react for 12 hours, stop the reaction, cool, precipitate the product with water, filter with suction, wash with a large amount of acetone, and dry in vacuum at 80°C for 48 hours to obtain a long-chain bicyclic phosphate ester structure Triazine macromolecular flame retardant.

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Abstract

The invention relates to a long-chain triazine macromolecular flame retardant with a bicyclic phosphate structure and a preparation method thereof. The structure of the flame retardant is shown the specification, and the flame retardant is prepared by carrying out condensation polymerization on cyanuric chloride, 1-O-4-hydroxymethyl-2,6,7-trioxa-1-phosphabicyclo[2,2,2] octane (PEPA) and diamine, binary alcohol / phenol or binary thiol / thiophenol with a structural general formula of ZH-R-ZH in the presence of an acid-binding agent. The preparation method provided by the invention has the advantages that raw materials are readily available and the process is simple. The obtained intumescent flame retardant has the advantages of good thermal stability, high char yield at high temperature and significant expansion properties and can be used in the flame retardant modification of the materials singly or together with other materials; and the carbon source, acid source and foam source components of the flame retardant are in the same macromolecule, thus effectively solving the problems that the components of the flame retardant system are not uniformly distributed in the materials, overcoming the problems of volatilization, migration, exudation and the like of inorganic flame retardants and low-molecular-weight organic flame retardant systems and simultaneously alleviating the defects that the mechanical behavior of the materials deteriorates because of the addition of the flame retardant.

Description

technical field [0001] The invention relates to the technical field of flame retardant development, in particular to the structure and preparation method of a class of long-chain triazine macromolecular flame retardants with a bicyclic phosphate structure. Background technique [0002] With the rapid development of polymer materials, people have higher requirements for the flame retardant properties of materials. The halogenated flame retardants used more in the early days have the advantages of less addition, obvious flame retardant effect, many varieties, and high cost performance. However, when it burns, it releases toxic and corrosive gases and produces large smoke, which causes "secondary disasters" while being flame retardant, so it is gradually eliminated. The intumescent flame retardant has the advantages of low toxicity, smoke suppression, non-corrosion, heat and ultraviolet stability, and good flame retardant effect. The polymer treated with the intumescent flame r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K21/14C09K21/12
Inventor 陶慷李娟薛立新严庆柯晨皓方科益
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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