Phosphorus and nitrogen heterocycle-containing organic halogen-free flame retardant and its preparation method

A nitrogen heterocycle and flame retardant technology is applied in the field of organic halogen-free flame retardants and their preparation, which can solve the problems of material heat resistance and other performance degradation, and achieve mild preparation reaction conditions, high yield and controllable reaction process. adjustable effects

Inactive Publication Date: 2012-11-21
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present, in order to obtain a certain flame retardant effect, it mainly depends on increasing the amount of a single flame retardant element, which leads to the introduction of too many chemical weak bonds, resulting in a significant decline in heat resistance and other properties of the material.

Method used

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  • Phosphorus and nitrogen heterocycle-containing organic halogen-free flame retardant and its preparation method
  • Phosphorus and nitrogen heterocycle-containing organic halogen-free flame retardant and its preparation method
  • Phosphorus and nitrogen heterocycle-containing organic halogen-free flame retardant and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0029] Preparation steps of organic halogen-free flame retardant: Add 21.5g DPPA and 100ml xylene into a 500ml flask equipped with a condenser, mechanical stirring, constant pressure dropping funnel and nitrogen protection, raise the temperature to 90°C, and wait until DPPA is completely dissolved in 1 Add 16.5ml of 37% formaldehyde solution and 10ml of xylene solution containing 0.15g of triethanolamine dropwise within 1 hour, continue to react for 0.5 hour, then filter the reaction mixture, wash with ethanol, and vacuum dry at 60°C for 12 hours to finally obtain phosphorus-containing nitrogen Heterocyclic organic halogen-free flame retardant HO-CH 2 -DPPA-CH 2 -OH 36.1 g, yield 91.8%. Organic Halogen Free Flame Retardant HO-CH 2 -DPPA-CH 2 The mass percentage content of each element in -OH is: C69.14%, H5.76%, O6.58%, P12.76%, N5.76%; the nuclear magnetic spectrum data are: 1 H NMR (DMSO-d6): 7.00-7.88ppm (8H, Ph-H), 4.00-4.30ppm (4H, P-CH 2 -, N-CH 2 -), 5.58-5.64ppm ...

Embodiment 2

[0031] Add 21.5g DAPO and 120ml ethyl acetate / isopropanol (volume ratio 1 / 1) into a 500ml flask equipped with a condenser, mechanical stirring, constant pressure dropping funnel and nitrogen protection, raise the temperature to 75°C, and wait until DAPO is completely dissolved After that, 60ml of acetone solution containing 33g of 2-naphthaldehyde and 10ml of chloroform solution containing 0.2g of hexamethylenetetramine were added dropwise within 2 hours, and the reaction was continued for 1 hour, then the reaction mixture was subjected to rotary evaporation, filtration, ethanol washing, and 60 After vacuum drying at ℃ for 12 hours, 50.6 g of an organic halogen-free flame retardant containing phosphorus and nitrogen heterocycles was finally obtained, with a yield of 92.8%. The effect of flame retardant FRH-2 on the thermal stability of polymer materials and the flame retardant effect are shown in Table 1.

Embodiment 3

[0033]Add 21.5g DPPA and 250ml methanol / toluene (volume ratio 1 / 2) into a 500ml flask equipped with a condenser, mechanical stirring, constant pressure dropping funnel and nitrogen protection, raise the temperature to 65°C, and wait for 0.5 hours after DPPA is completely dissolved Add 50ml of ethanol solution containing 12.2g p-hydroxybenzaldehyde and 11.2g cyclohexyl formaldehyde and 10ml of ethanol solution containing 0.6g benzyldimethylamine dropwise, continue to react for 16 hours, then the reaction mixture is filtered, washed with ethanol, 60 After vacuum drying at ℃ for 12 hours, 40.9 g of an organic halogen-free flame retardant containing phosphorus and nitrogen heterocycles was finally obtained, with a yield of 91.1%. The effect of flame retardant FRH-3 on the thermal stability of polymer materials and the flame retardant effect are shown in Table 1.

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Abstract

The invention discloses a phosphorus and nitrogen heterocycle-containing organic halogen-free flame retardant and its preparation method. The flame retardant has one or more of the following structures: HO-R1-DPPA-R2-OH and HO-R3-DAPO-R4-OH. The preparation method consists of: 1) under the protection of an inert gas, dissolving a phosphorus and nitrogen heterocycle-containing reactant in an organic solvent, then adding an aldehyde and a tertiary amine catalyst, and conducting stirring reaction at 25-150DEG C for 0.5-24 hours so as to obtain a reaction solution; and 2) first subjecting the reaction solution to filtration or rotary evaporation, and then carrying out washing and drying, thus obtaining a target product. The flame retardant provided in the invention can participate in crosslinking, polycondensation and other reactions through a contained hydroxyl active group and form one part of a polymer molecular structure, thus endowing the polymer with an intrinsic flame retardant function or improving its flame retardation. The method has the advantages of mild reaction conditions, controllable and adjustable reaction process, and high yield, etc.

Description

technical field [0001] The invention relates to the field of flame retardant processing aids, in particular to an organic halogen-free flame retardant containing phosphorus and nitrogen heterocycles and a preparation method thereof. Background technique [0002] Polymer materials have the characteristics of light weight, high strength, corrosion resistance, insulation, heat resistance, good elasticity, radiation resistance, transparency, and easy processing. Important materials essential to everyday life. However, most polymer materials are flammable and continue to burn after leaving the fire, which is easy to cause fire. This shortcoming makes it a great safety hazard in the application process, which seriously threatens the lives and property safety of the people. Therefore, improving the flame retardancy of polymer materials is one of the strategic measures to prevent and reduce fire accidents, which has important theoretical and practical significance. [0003] The us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399C08K5/51C08L63/00C08L67/06C08L75/04C08L23/06C07F9/6584
CPCY02P20/52
Inventor 袁彦超赵建青刘述梅袁俊轩王永珍黄皓浩
Owner SOUTH CHINA UNIV OF TECH
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