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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 self-polymerization and easy formation of cyclic by-products, etc. The effect of increasing productivity

Active Publication Date: 2014-05-07
SHOUGUANG WEIDONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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
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Embodiment 1

[0023] In a 200ml four-neck flask, add 21.6g (0.1mol) DOPO, 15.6g (0.12mol) methylenesuccinic acid, and 100ml toluene to react at 110°C for 5 hours to generate a dicarboxylic acid derivative of DOPO, suction filtration, A white solid was obtained, which was dried. The obtained solid was added to a 200ml four-necked flask at 40°C, 11.2g (0.2mol) of KOH was dissolved in 100ml of water, added to the four-necked flask, stirred for 2 hours, and 0.4g of dodecyltrimethyl chloride was added. Ammonium and 34.4g (0.2mol) 2-iodoethanol, after the reaction for 5 hours, pour the product of the four-necked bottle into a separatory funnel, let stand for stratification, the lower layer is a colorless and transparent product, the upper layer is a water layer, twelve The alkyl trimethyl ammonium chloride and the resulting KI are in the aqueous phase. The product has a purity of 94.5% and a viscosity of 519.5 mPa.s.

[0024] The reaction equation of the present embodiment is as follows:

[00...

Embodiment 2

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

Embodiment 3

[0032] In a 200ml four-necked flask, add 21.6g (0.1mol) DOPO, 12.8g (0.11mol) fumaric acid, and 100ml toluene to react at 110°C for 3 hours to generate a dicarboxylic acid derivative of DOPO, and suction filtration to obtain White solid, dried. The obtained solid was added to a 200ml four-necked flask at 10°C, 11.2g (0.2mol) of KOH was dissolved in 100ml of water, added to the four-necked flask, stirred for 2 hours, 0.4g of tetrabutylammonium chloride and 25.0g of tetrabutylammonium chloride were added. (0.2mol) 2-bromoethanol, pour the product of the four-necked bottle into a separatory funnel after 6 hours of reaction, let stand for stratification, the lower layer is a colorless and transparent product, the upper layer is an aqueous layer, tetrabutylammonium chloride and the resulting KBr in the aqueous phase. The product has a purity of 93.4% and a viscosity of 526.0 mPa.s.

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Abstract

The 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 shown as a formula (i). The preparation method comprises the following steps: (1) adding DOPO and dicarboxylic acid into toluene, stirring and heating to 110+ / -2 DEG C, reacting for 2-6 hours, stopping heating, performing suction filtration on the reacted solution, obtaining white solids, drying, and preparing a DOPO dicarboxylic acid derivative; (2) dissolving the DOPO dicarboxylic acid derivative in a 2+ / -0.2 mol / L of potassium hydroxide solution at the temperature of 0-40 DEG C, stirring for 1.5-2.5 hours, and generating sylvite of the DOPO dicarboxylic acid derivative; (3) adding a phase transfer catalyst and halohydrin into the solution prepared in the step (2), reacting for 4-8 hours, layering the solution in a separating funnel, taking the lower layer, and obtaining the phosphorus-containing flame retardant. (img file='2014100188078100004dest-path-image001.TIF' wi='366' he='207' / ) (i).

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a phosphorus-containing flame retardant and a preparation method thereof. Background technique [0002] 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO for short) is a new type of flame retardant intermediate. Its structure contains P-H bonds, and it is very active to olefins, epoxy bonds and carbonyl groups, and can react to generate many derivatives. Because DOPO and its derivatives contain biphenyl ring and phenanthrene ring structure in their molecular structure, especially the introduction of side phosphorus groups in the form of cyclic O=P-O bonds, they are more thermally stable and chemically stable than ordinary, non-cyclic organic phosphates. High stability, better flame retardant performance. DOPO and its derivatives can be used as reactive and additive flame retardants. The synthesized flame retardants are halogen-free, smoke-free, non-toxic, non...

Claims

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Application Information

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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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