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Synthetic method of phosphorus and nitrogen type fire retardant

A synthesis method and flame retardant technology, applied in the field of flame retardant material preparation, can solve the problems of low yield and high energy consumption, and achieve the effects of shortened esterification reaction time, low energy consumption, and low production cost

Inactive Publication Date: 2012-11-28
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] In order to solve the above-mentioned technical problems, the purpose of the present invention is to provide a synthetic method of an efficient environment-friendly phosphorus-nitrogen flame retardant, to solve the problems of low yield and high energy consumption in the synthetic process of the phosphorus-nitrogen flame retardant. Big problem, and the synthesis process is safe and reliable, the process is stable, and the synthesis cost is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] This embodiment provides a phosphorus nitrogen type flame retardant, which is prepared according to the following steps:

[0040] In a four-necked flask equipped with a stirrer, a thermometer, a condenser, and a water separator, add 4.25ml of phosphoric acid (concentration: 85wt%), slowly heat up to 120°C, add 6.8g of pentaerythritol, and react for 4h;

[0041] Add 18ml of solvent water and 12.6g of melamine, react at 80°C for 2 hours, then cool, wash with distilled water until pH = 7, filter with suction, and dry to obtain 13.72g of a white solid product, which is a phosphorus nitrogen type flame retardant.

[0042] In the salt-forming reaction of the phosphorus-nitrogen flame retardant provided in this example, water is added as a solvent, and the product yield increases to 44.3%.

Embodiment 2

[0044] This embodiment provides a phosphorus nitrogen type flame retardant, which is prepared according to the following steps:

[0045] In a four-necked flask equipped with a stirrer, a thermometer, a condenser, and a water separator, add 5.10ml of phosphoric acid (concentration: 85wt%), slowly heat up to 120°C, add 6.8g of pentaerythritol, react for 4h, and then add 18ml of solvent Water and 12.6g of melamine were reacted at 80°C for 2 hours, then cooled, washed with distilled water until pH = 7, filtered with suction, and dried to obtain 13.72g of a white solid product, namely a phosphorus-nitrogen type flame retardant.

[0046] In this embodiment, the product yield is increased to 48.4% by changing the ratio of raw materials.

Embodiment 3

[0048] This embodiment provides a phosphorus nitrogen type flame retardant, which is prepared according to the following steps:

[0049] In a four-necked flask equipped with a stirrer, a thermometer, a condenser, and a water separator, add 6.8ml of phosphoric acid (concentration: 85wt%), slowly raise the temperature to 120°C, add 3.1g of ethylene glycol, and react for 2h;

[0050] Then add 18ml of solvent water and 12.6g of melamine, react at 80°C for 2 hours, then cool, wash with distilled water until pH = 7, filter with suction, and dry to obtain 13.72g of white solid product, namely phosphorus nitrogen type flame retardant.

[0051] In this embodiment, pentaerythritol is replaced with ethylene glycol, and the product yield is 53.6%. The phosphorus-nitrogen type flame retardant can be used for flame retardant of polypropylene plastic: the mass ratio of flame retardant to polypropylene plastic is 30:100, adopt "GBT17037.1-1997" twin-screw extrusion injection molding sample pr...

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Abstract

The invention relates to a synthetic method of a phosphorus and nitrogen type fire retardant, which comprises the following steps of: reacting an assistant with phosphate materials to remove water out of the phosphate materials; reacting polyhydric alcohols with the phosphate materials with water removed to obtain an intermediate; and reacting the intermediate with melamine in a solvent to obtain the phosphorus and nitrogen type fire retardant, wherein the phosphate materials can be one or more than one of phosphoric acid, pyrophosphoric acid and polyphosphoric acid. Compared with the prior art, the synthetic method provided by the invention has the advantages of shortening the esterification reaction time and increasing yield of the phosphorus and nitrogen type fire retardant, improving the purity of the phosphorus and nitrogen type fire retardant and the production process is simple in process and clean and safe.

Description

technical field [0001] The invention relates to a method for synthesizing a novel high-efficiency flame retardant, in particular to a method for synthesizing a phosphorus-nitrogen type flame retardant, and belongs to the technical field of preparation of flame retardant materials. Background technique [0002] A flame retardant is an additive that increases a material's resistance to burning, prevents the material from igniting, or inhibits the spread of flame. There are many classification methods of flame retardants, which can be divided into two categories according to their chemical composition: organic flame retardants and inorganic flame retardants. Among them, the representative flame retardants are phosphorus-based, magnesium hydroxide, antimony oxide, halogen-based, phosphorus-nitrogen-based flame retardants, etc. [0003] Phosphorus-nitrogen flame retardants are also known as intumescent flame retardants. They have the characteristics of halogen-free, strong flame...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L23/12C08L23/06C08L25/06C08L59/00C08K5/521
Inventor 郭巧霞陈庆玺刘晓婷申宝剑
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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