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Preparation method of phosphorus-containing flame retardant

A flame retardant and organic solvent technology, which is applied in the field of preparation of DOPO derivative flame retardants, can solve the problems of limited use, containing low melting point isomers, and the yield needs to be further improved, so as to achieve high purity and increase yield Effect

Inactive Publication Date: 2019-01-11
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Patent WO2011123389A1 reports a very potential DOPO derivative compound I, which uses DOPO and ethylene glycol (EG) as raw materials to synthesize the DOPO derivative, but the product contains isomers with low melting points, which limits its use
[0004] Chinese patent 201310281306.4 reports a method that uses CDOP, an intermediate for synthesizing DOPO, as a raw material to react with ethylene glycol to directly prepare a single product with high purity and no enantiomers. This method has certain advantages in product configuration. , but the yield still needs to be further improved

Method used

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  • Preparation method of phosphorus-containing flame retardant
  • Preparation method of phosphorus-containing flame retardant
  • Preparation method of phosphorus-containing flame retardant

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Add 3.12g of raw material ethylene glycol into 20ml of diphenylmethane, add 15g of triethylamine, control the temperature between -10°C and 10°C, add dropwise the diphenylmethane solution of CDOP (23.68g dissolved in 50ml of diphenylmethane ), dropwise, and react at room temperature for 2 hours; then add 3.75 g of methyl p-toluenesulfonate and 10 g of formic acid, heat up to 180 ° C for 3 h, cool to 50 ° C, add 100 ml of methanol, stir, filter, and wash to obtain 20.93 g of formula I The indicated DOPO analogue, the yield is 90%, 31 P-NMR showed that the proportion of the high melting point isomer was 98.7%, and the melting point was 297-298°C.

Embodiment 2

[0031] Add 6.21g of raw material ethylene glycol into 45ml of diphenylmethane, add 32g of triethylamine, control the temperature between -10°C and 10°C, and dropwise add CDOP diphenylmethane solution (47.50g dissolved in 100ml of diphenylmethane ), dropwise, and react at room temperature for 0.5h; then add 6.42g of methyl benzenesulfonate and 25.46g of formic acid, heat up to 170°C for 3h, cool to 50°C, add 180ml of ethanol, stir, filter, and wash to obtain 43.24g of formula The DOPO analog shown in I, yield is 94%, 31 P-NMR showed that the proportion of the high melting point isomer was 99.8%, and the melting point was 300-301°C.

Embodiment 3

[0033] Add 3.12g of raw material ethylene glycol into 25ml of diphenylmethane, add 16g of triethylamine, control the temperature between -10°C and 10°C, add dropwise the diphenylmethane solution of CDOP (23.85g dissolved in 50ml of diphenylmethane ), dropwise, and react at room temperature for 1 h; then add 3.92 g of methyl p-toluenesulfonate and 15.6 g of acetic acid, heat up to 200 ° C for 5 h, cool to 50 ° C, add 100 ml of acetone, stir, filter, and wash to obtain 20.81 g of formula DOPO analog shown in I, 31 P-NMR showed that the high melting point isomer ratio was 99.2%.

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Abstract

The invention provides a preparation method of a phosphorus-containing flame retardant. The compound of formula I is prepared from CDOP and ethylene glycol under the catalysis of a sulfonate compoundand an acid. The method has the advantages of simplicity in operation, high yield, and high content of a high melting point isomer in the product.

Description

technical field [0001] The invention belongs to the field of flame retardants, and in particular relates to a preparation method of a DOPO derivative flame retardant. Background technique [0002] Phosphorus-containing flame retardants have important application value, especially high melting point phosphorus-containing flame retardants have a broad market. [0003] Patent WO2011123389A1 reports a very potential DOPO derivative compound I, which uses DOPO and ethylene glycol (EG) as raw materials to synthesize the DOPO derivative, but the product contains isomers with low melting points, which limits its use . [0004] Chinese patent 201310281306.4 reports a method that uses CDOP, an intermediate for synthesizing DOPO, as a raw material to react with ethylene glycol to directly prepare a single product with high purity and no enantiomers. This method has certain advantages in product configuration. , but the yield still needs to be further improved. [0005] [0006] P...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
CPCC07F9/657172
Inventor 袁寒梦郭鑫王元兰张贵王文磊谢练武马强肖滕
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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