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Triazine ring combustion inhibitor containing phosphorus and its preparing process

A technology of triazine ring and flame retardant, which is applied in the field of flame retardants, can solve the problems of easy decomposition, limited application, and low thermal stability of compounds, and achieves the effect of increasing the decomposition temperature and improving thermal stability.

Inactive Publication Date: 2007-08-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the thermal stability of this compound is not very high, and it is easy to decompose in the process of polymer flame retardant processing, which limits its application in the field of polymer materials

Method used

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  • Triazine ring combustion inhibitor containing phosphorus and its preparing process
  • Triazine ring combustion inhibitor containing phosphorus and its preparing process
  • Triazine ring combustion inhibitor containing phosphorus and its preparing process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Preparation of 1,3,5-triazine cycloneopentyl glycol phosphate: 36.9g (0.2mol) cyanuric chloride and 600g toluene are added to a 1000mL device equipped with magnetic stirring, condenser, constant pressure dropwise Four-neck flask with funnel and thermometer. The reaction system was kept at room temperature with a water bath, and 103.3 g (0.63 mol) of neopentyl glycol ethyl phosphite was added dropwise to the system in about 2 hours. When the dropwise addition was completed, the reaction system was heated to reflux for 4h. During this process, crude product solids were produced when refluxed for about 10 minutes. After the reaction was complete, the mixture was cooled to room temperature. The resulting crude product was filtered, washed with toluene and n-hexane, and dried under vacuum at 40-50°C. The obtained crude product was recrystallized from absolute ethanol to obtain 96.7 g of white crystals of tris(neopentyl glycol cyclic phosphate)-1,3,5-triazine ring with...

Embodiment 2

[0040] (1) Preparation of 1,3,5-triazine cycloneopentyl glycol phosphate: a mixed solution of 36.9g (0.2mol) cyanuric chloride and 300g xylene and ethylbenzene was added to a 1000mL magnetic stirrer , a condenser, a constant pressure dropping funnel and a four-neck flask with a thermometer. The reaction system was kept at room temperature with a water bath, and 94.8 g (0.63 mol) of neopentyl glycol methyl phosphite was added dropwise into the system in about 3 hours. After the dropwise addition was completed, the reaction system was heated to 140° C. for 2 h. During this process, crude product solids were produced when refluxing for about 5 minutes. After the reaction was complete, the mixture was cooled to room temperature. The resulting crude product was filtered, washed with xylene and n-hexane, and dried under vacuum at 40-50°C. The obtained crude product was recrystallized with absolute ethanol to obtain 88.7 g of light yellow crystal tris(neopentyl glycol cyclic phosp...

Embodiment 3

[0043] (1) Preparation of 1,3,5-triazine cycloneopentyl glycol phosphate: 36.9g (0.2mol) cyanuric chloride and 900g N, N-dimethylformamide were added to a 1000mL magnetic stirrer , constant pressure dropping funnel and a four-necked flask with a thermometer. The reaction system was kept at room temperature with a water bath, and 112.1 g (0.63 mol) of neopentyl glycol isopropyl phosphite was added dropwise to the system in about 3 hours. After the dropwise addition was completed, the reaction system was reacted at 40° C. for 10 h. After the reaction was complete, the mixture was cooled to room temperature. The solvent was distilled from the product mixture under reduced pressure, and the obtained crude product was recrystallized from absolute ethanol to obtain 55.8 g of light yellow crystal tris(neopentyl glycol cyclic phosphate)-1,3,5-triazine ring, with a yield of 53.2%.

[0044] (2) Preparation of phosphorus-containing triazine ring flame retardant: install magnetic stirri...

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Abstract

The invention discloses a phosphoric triazine radical containing fire retarding agent and the preparing method. The method comprises following steps: putting neopentyl glycol phosphite ester and cyanuric acid of same equivalent weight in organic solvent, reacting for 2- 10 hours at normal temperature to 140 Deg. C, getting 1, 3, 5- triazine neopentyl glycol phosphate; then putting got 1, 3, 5- triazine neopentyl glycol phosphate and diamine of same equivalent weight in inert liquid for replace reaction and getting phosphoric triazine radical containing fire retarding agent, the reacting temperature is from normal temperatur to 160 Deg. C, reacting time is 6- 72 hours. The number average molecular weight of product is 2000- 20000, and the decompostion temperature is 240- 400 Deg. C. The invention increases the fire retarding agent's decompostion temperature, which enables it not to decompose during macromolecular material processing; and the expanded fire retarding agent ploymer prepared in this invention contains P, N and C element, which is multifunctional.

Description

technical field [0001] The invention relates to a flame retardant, in particular to a phosphorus-containing triazine ring flame retardant and a preparation method thereof. Background technique [0002] The flame retardant mechanism of the currently used intumescent phosphorus-nitrogen flame retardant is to release phosphoric acid and non-combustible gas through thermal decomposition, and the latter dilutes the oxygen in the air. Nitrogen-containing compounds act as foaming agents and coke enhancers, while phosphoric acid is a catalyst for coking, which promotes the formation of a porous coking protective film on the combustion surface, which plays the role of heat insulation and oxygen insulation, and can interrupt the chain of combustion reaction. [0003] Based on the requirements of low smoke, low corrosion and low toxicity of flame retardant materials, the development of intumescent flame retardants has become an important substitute for traditional halogen flame retard...

Claims

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Application Information

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IPC IPC(8): C09K21/14C07F9/547C08K5/5373
Inventor 赵建青刘刚生启刘述梅章永化朱亚明叶华
Owner SOUTH CHINA UNIV OF TECH
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