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Phosphorus-containing flame retardant and preparation method thereof

A phosphorus flame retardant and flame retardant technology are applied in the field of phosphorus-containing flame retardants and their preparation, which can solve the problems of easy formation of cyclic by-products and easy self-polymerization, etc. The effect of reducing the reaction cost

Active Publication Date: 2016-01-20
SHOUGUANG WEIDONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is: to provide a phosphorus-containing flame retardant and its preparation method, so that the formation of ester bonds can be reacted at normal temperature, so as to solve the problem that carboxylic acid and alcohol are easily formed when they are directly esterified with alcohol at high temperature. The problem of cyclic by-products, and the problem that alcohol is prone to self-polymerization at high temperature, improve product purity and yield

Method used

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  • Phosphorus-containing flame retardant and preparation method thereof
  • Phosphorus-containing flame retardant and preparation method thereof
  • Phosphorus-containing flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 21.6g (0.1mol) DOPO, 15.6g (0.12mol) methylene succinic acid, and 100ml toluene to react at 110°C for 5 hours in a 200ml four-neck flask to generate a dicarboxylic acid derivative of DOPO, filter with suction, A white solid was obtained and dried. Add the obtained solid into a 200ml four-necked flask at 40°C, dissolve 11.2g (0.2mol) KOH in 100ml water, add it to the four-necked flask, stir for 2 hours, add 0.4g dodecyl trimethyl chloride Ammonium and 34.4g (0.2mol) 2-iodoethanol, after reacting for 5 hours, the product of the four-neck bottle is poured into the separatory funnel, and the layers are left to stand. The lower layer is a colorless and transparent product, and the upper layer is an aqueous layer. Alkyltrimethylammonium chloride and the resulting KI are in the aqueous phase. The purity of the product is 94.5%, and the viscosity is 519.5mPa.s.

[0024] Present embodiment reaction equation is as follows:

[0025]

[0026]

[0027] The catalytic mec...

Embodiment 2

[0030] Add 21.6g (0.1mol) DOPO, 11.6g (0.1mol) maleic acid, and 100ml toluene to react at 110°C for 6 hours in a 200ml four-neck flask to generate a dicarboxylic acid derivative of DOPO, and filter it with suction to obtain White solid, dry. Add the obtained solid into a 200ml four-necked flask at 30°C, dissolve 11.2g (0.2mol) KOH in 100ml of water, add it to the four-necked flask, stir for 2 hours, add 0.4g benzyltriethylammonium chloride and 16.1g (0.2mol) 2-chloroethanol, after reacting for 8 hours, pour the product in the four-neck bottle into the separatory funnel, let it stand for stratification, the lower layer is a colorless and transparent product, the upper layer is a water layer, benzyl triethyl ammonium chloride and the resulting KCl in the aqueous phase. The purity of the product is 92.6%, and the viscosity is 537.0mPa.s.

Embodiment 3

[0032] Add 21.6g (0.1mol) DOPO, 12.8g (0.11mol) fumaric acid, and 100ml toluene to react at 110°C for 3 hours in a 200ml four-neck flask to generate a dicarboxylic acid derivative of DOPO, and filter it with suction to obtain White solid, dry. Add the obtained solid into a 200ml four-necked flask at 10°C, dissolve 11.2g (0.2mol) KOH in 100ml of water, add it to the four-necked flask, stir for 2 hours, add 0.4g tetrabutylammonium chloride and 25.0g (0.2mol) 2-bromoethanol, after reacting for 6 hours, pour the product of the four-necked bottle into the separatory funnel, let it stand for stratification, the lower layer is a colorless and transparent product, the upper layer is a water layer, tetrabutylammonium chloride and the generated KBr in the aqueous phase. The purity of the product is 93.4%, and the viscosity is 526.0mPa.s.

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Abstract

The present invention relates to the field of organic synthesis, and provides a phosphorus-containing flame retardant and a preparation method thereof. The phosphorus-containing flame retardant has a chemical formula such as formula (i), and the preparation method includes the following steps: (1) combining DOPO and Dibasic carboxylic acid was added to toluene, stirred and heated to 110±2°C, reacted for 2 to 6 hours, stopped heating, and filtered the reacted solution to obtain a white solid, dried to obtain DOPO dibasic carboxylic acid derivative (2) Dissolve DOPO dibasic carboxylic acid derivatives in 2±0.2mol / L potassium hydroxide solution at a temperature of 0-40°C and stir for 1.5-2.5 hours to generate DOPO dibasic carboxylic acid derivatives Potassium salt; (3) Add a phase transfer catalyst and a halogenated alcohol to the solution prepared in step (2), react for 4 to 8 hours, pour into a separating funnel to separate layers, and remove the lower layer to obtain the phosphorus-containing flame-retardant agent. (i).

Description

Technical field [0001] The present invention is an organic synthesis field, which involves a phosphorus -containing flame retardant and its preparation methods. Background technique [0002] 9,10-dihydrogen-9-oxygen-10-phosphorus-10-oxides (referred to as dopo), which is a new type of flame retardant intermediate.Its structure contains P-H bonds, which is very active to olefins, epoxy bonds, and cymbals, and can reflect many derivatives.DOPO and its derivatives are introduced in the form of phenyl ring and the Philippines because the molecular structure contains the phenyl ring and the Philippines.High stability and better flame retardant performance.DOPO and its derivatives can be used as response and added flame retardants. The synthetic flame retardant is halogentian, smoke -free, non -toxic, non -migration, and lasting flame retardant performance.Can be used for flame retardant treatment of linear polyester, polyamide, epoxy resin, polyurethane and other polymer materials.For...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5313C07F9/6574
Inventor 陈如林刘瑞祥朱之军谢忠财李法庭张腾腾
Owner SHOUGUANG WEIDONG CHEM
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