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Synthesis method of aromatic amide phosphate compound and flame retardant containing compound

A phosphate ester amide and synthesis method technology, which is applied to the "one-pot" synthesis of aromatic phosphate amide compounds and the field of flame retardants, which can solve the limitations of popularization and application, high energy consumption, and the production cost of aryl phosphate amide compounds Problems such as staying high

Inactive Publication Date: 2016-07-13
YWK CHEM TAICANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It also has the difficulty of obtaining and storing halogenated phosphate esters, and the recovery and treatment of high boiling point solvents is troublesome, and also requires high temperature and high vacuum. Set of high temperature distillation equipment
[0006] In view of the various shortcomings of the aforementioned production technology, especially because the production equipment is too complicated and the energy consumption is too high, the production cost of the aryl phosphate ester amide compound is finally high, making it difficult to reduce the cost of using it as a flame retardant. Widespread application is severely limited

Method used

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  • Synthesis method of aromatic amide phosphate compound and flame retardant containing compound
  • Synthesis method of aromatic amide phosphate compound and flame retardant containing compound
  • Synthesis method of aromatic amide phosphate compound and flame retardant containing compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～3

[0064] A 100ml four-necked bottle is equipped with stirring, thermometer, condenser, drying tube and acid tail gas absorption device, add 30.67g of phosphorus oxychloride, 0.80g of anhydrous magnesium chloride, raise the temperature to an internal temperature above 70°C, add 36.71g / l of phenol dropwise, 36.71 g of 2-dichloroethane solution, added dropwise over 2 hours. After the dropwise addition, keep warm at 90-100°C and react for 2 hours or more. The HPLC central control detects that the phenol residue is ≤0.1% (Area%) and then cools down to room temperature to obtain a DCM / DPCP solution for use.

[0065] A 250ml four-necked bottle is equipped with stirring, thermometer, condenser and drying tube, add 20.00g of aniline, 100.00g of 1,2-dichloroethane, add the aforementioned DCM / DPCP solution dropwise under stirring, and keep the internal temperature at ≤20 ℃. After the dropwise addition, raise the temperature to an internal temperature above 30°C, add a solution of 20.00g t...

Embodiment 4

[0068] 100ml four-necked bottle equipped with stirring, thermometer, condenser, drying tube and acid tail gas absorption device, add 30.67g of phosphorus oxychloride, 0.80g of anhydrous magnesium chloride, raise the temperature to above 85°C, add 37.27g / l of phenol dropwise, 40.00g solution of 2-dichloroethane, added dropwise for more than 2 hours. After the dropwise addition, keep warm at 90-100°C and react for 2 hours or more. The HPLC central control detects that the phenol residue is ≤0.1% (Area%) and then cools down to room temperature to obtain a DCM / DPCP solution for use.

[0069] A 250ml four-necked bottle is equipped with stirring, thermometer, condenser and drying tube, add 9.26g of anhydrous piperazine, 200.00g of 1,2-dichloroethane, add the aforementioned DCM / DPCP solution dropwise under stirring, and keep the internal temperature during the dropwise addition At ≤20°C. After the dropwise addition, the temperature was raised to above 30°C, and a solution of 10.00g ...

Embodiment 5

[0071] Use p-phenylenediamine 11.63g instead of anhydrous piperazine, and all the other operations are the same as in Example 4, to obtain 71.75g ​​of bis(diphenyl phosphate)-1,4-p-phenylenediphosphoramide, with a yield of 63.29% (based on phenol base calculation yield).

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PUM

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Abstract

The invention discloses a one-pot synthesis method of an aromatic amide phosphate compound. Firstly, phosphorus trioxyhalogen and a monophenol compound or a bisphenol compound react in the presence of a lewis acid catalyst to produce a mono- and / or poly-halogenated phosphate ester compound; secondarily, the mono- and / or poly-halogenated phosphate ester compound and at least one amine compound of a monoamine compound with one primary amino group and / or secondary amino group in molecules and a diamine compound with two primary amino groups and / or secondary amino groups in molecules are subjected to a dehydrohalogenation reaction in the presence of lewis base, and the aromatic amide phosphate compound is produced; finally, the aromatic amide phosphate compound is purified, and a target product is obtained. The one-pot synthesis method has the advantages that with the adoption of one-pot, an intermediate, namely, the mono- and / or poly-halogenated phosphate ester compound, obtained through the reaction is not required to be distilled and / or rectified and purified, required energy consumption is greatly reduced, required production equipment is greatly simplified, corrosive damage of equipment is greatly reduced, the whole process is simple and practical, the production cost is low, the environmental pressure is small, and the product quality is high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a "one-pot" synthesis method of an aromatic phosphate ester amide compound and a flame retardant containing the compound. Background technique [0002] At present, phosphorus-nitrogen (P-N) series intumescent flame retardants can not only reduce the heat release rate of materials and improve the flame retardant effect, It also overcomes the shortcomings of halogen-based flame retardants that easily release irritating and corrosive gases and a large amount of toxic smoke when they burn. It has been used in textiles, leather, polyester fibers, coatings, cables, engineering plastics and other industries. Products are being used more and more widely, among which aromatic phosphate ester amide is one of the representative compounds of phosphorus-nitrogen (P-N) intumescent flame retardants. [0003] According to the literature, the current manufacturing methods a...

Claims

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Application Information

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IPC IPC(8): C07F9/24C09K21/12
CPCC07F9/247C07F9/2454C09K21/12
Inventor 浜田申一浜田智子唐成见
Owner YWK CHEM TAICANG
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