Spiro-phosphorus phenone polyesteramide intumescent flame retardant and synthetic method thereof

A technology of spirocyclic phosphorophenyl benzotripolyamide ester and intumescent flame retardant, which is applied in the field of intumescent flame retardant and its synthesis, can solve the problems of poor thermal stability, poor flame retardant effect, complicated process, etc., and achieve Good thermal stability, good flame retardant effect, simple process effect

Inactive Publication Date: 2009-12-30
NORTHEAST FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of poor thermal stability and poor flame retardant effect of the existing intumescent flame retardants, as well as the complex process and high energy consumption of the existing intumescent flame retardant synthesis methods. The present invention provides a spiral ring Phosphoryl benzotripolyamide ester intumescent flame retardant and its synthesis method

Method used

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  • Spiro-phosphorus phenone polyesteramide intumescent flame retardant and synthetic method thereof
  • Spiro-phosphorus phenone polyesteramide intumescent flame retardant and synthetic method thereof
  • Spiro-phosphorus phenone polyesteramide intumescent flame retardant and synthetic method thereof

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specific Embodiment approach 1

[0015] Specific implementation mode 1: The molecular formula of the spirocyclic phosphorophenyl tripolyamide ester intumescent flame retardant in this implementation mode is:

[0016]

[0017] The spirocyclic phosphorophenyl tripolyamide ester intumescent flame retardant in this embodiment is a white powdery solid with a melting point of 256°C to 258°C. In this embodiment, a Carlo Erba 1110 elemental analyzer is used to analyze and test the element content of the spirophosphoryl phenylated tripolyamide ester intumescent flame retardant. The test results are respectively 20.2% phosphorus content and 5.7% nitrogen content in terms of mass percentage. The carbon content is 28.3%, the hydrogen content is 3.0%, and the chlorine content is 11.5%.

[0018] In this embodiment, the spirocyclic phosphorophenyl tripolyamide ester intumescent flame retardant is subjected to thermogravimetric analysis (TG) test, and the test results are as follows figure 1 shown. Depend on figure 1 T...

specific Embodiment approach 2

[0020] Specific embodiment two: the synthetic method of the spirocyclic phosphorobenzoyl tripolyamide ester intumescent flame retardant described in the specific embodiment one is realized by the following steps: one, spirocyclic phosphoryl chloride and benzomelamine Add into the organic solvent, stir for 15~25min, then heat to 50℃~60℃, after the spirophosphoryl chloride and benzomelamine are completely dissolved in the organic solvent, keep stirring and reflux for 1~2h, then add the amine catalyst to continue Insulated and stirred under reflux for 6 to 8 hours to obtain a white suspension, wherein the mass ratio of spirophosphoryl chloride to benzomelamine is 1 to 6:1, the ratio of organic solvent to spirophosphoryl chloride is 40 to 50ml: 1g, and the amine The ratio of the catalyst addition amount to spirophosphoryl chloride is 1 to 3ml: 1g; 2. Suction filtration of the white suspension obtained in step 1 to obtain a filter cake, and then the filter cake is desiccated with -1...

specific Embodiment approach 3

[0025] Specific embodiment three: the difference between this embodiment and specific embodiment two is that in step one, spirocyclic phosphorus oxychloride, benzomelamine and organic solvent are stirred in a four-necked flask equipped with a reflux condenser, a thermometer, and an agitator reaction. Other steps and parameters are the same as in the second embodiment.

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Abstract

The invention provides spiro-phosphorus phenone polyesteramide intumescent flame retardant and a synthetic method thereof, and relates to a intumescent flame retardant and a synthetic method thereof. The invention solves the problems that the existing intumescent flame retardant has poor thermostability and poor effect of flame retardance, and the synthetic method of the existing intumescent flame retardant has complex process and large energy-consumption. The molecular formula of the intumescent flame retardant of the invention is right type. The synthetic method of the intumescent flame retardant of the invention is as follows: 1,adding spiro hosphorus oxychloride and benzoguanamine into organic solvent, and stirring the solution, heating to fully dissolve the mixture, carrying out heat insulation, stirring and refluxing, and then adding amine catalyst to carry out heat insulation, stirring and refluxing to obtain white turbid liquid; 2, filtering the white turbid liquid, then filtering again and drying to prepare the spiro-phosphorus phenone polyesteramide intumescent flame retardant. The intumescent flame retardant of the invention has good thermostability and good effect of flame retardance, the synthetic method has simple process and less energy-consumption.

Description

technical field [0001] The invention relates to an intumescent flame retardant and a synthesis method thereof. Background technique [0002] Intumescent flame retardant (IFR), with phosphorus and nitrogen as the main components, is a new type of environmentally friendly flame retardant that integrates acid source, carbon source and gas source. It can be combined with flammable polymers to prepare new When the material is heated and burned, a uniform carbon foam layer will be formed on the surface. The carbon foam layer has good density and contains non-combustible gas, which has the functions of blocking heat and oxygen transfer and suppressing smoke. Therefore, the research on intumescent flame retardants has become a hot spot in the research and development of flame retardants. [0003] The existing "trinity" intumescent flame retardants are all nitrogen-containing salts of phosphoric acid or polyphosphoric acid, which are ionic flame retardants, and have the problems of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/12C07F9/6574
Inventor 张庆波孙才英邢海涛向海旺姜大伟胡树林董春梅
Owner NORTHEAST FORESTRY UNIVERSITY
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