Phosphate flame retardant containing styrene structure and synthesis method of phosphate flame retardant

A phosphate ester and styrene technology, which is applied in the field of phosphate ester flame retardants and their synthesis, can solve the problems of low reaction yield, difficult product separation, waste of raw materials, etc., and achieve high reaction yield, easy industrialization, and convenient reaction operation Effect

Inactive Publication Date: 2012-10-03
JIANGSU YOKE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that because the flame retardant is added in the form of physical blending, it deteriorates the physical properties of the material such as mechanics and impact resistance.
When prepared by this method, a large amount of hydrog

Method used

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  • Phosphate flame retardant containing styrene structure and synthesis method of phosphate flame retardant
  • Phosphate flame retardant containing styrene structure and synthesis method of phosphate flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1, in the flask equipped with stirring, condensation, drying device, add catalyst sodium hydroxide 0.13g and pyridine 0.49g successively, carbon tetrachloride 6.03g, 4-hydroxystyrene 0.36g, open stirring device, ice Cool in a water bath to 0°C, slowly add a mixture of 0.62g of dibutyl phosphite and 3.52g of carbon tetrachloride dropwise from the dropping funnel, and drop it over in about 2 hours; keep the reaction at 0°C for 42 hours to end the reaction, and filter to form The solid was removed by spinning off the reaction solvent, and the product was separated by column chromatography (ethyl acetate:petroleum ether=2:1) ​​to obtain a sample of 0.90g. The yield is 95.8% (based on 4-hydroxystyrene, the same for the following examples).

Embodiment 2

[0017] Embodiment 2, in the flask equipped with stirring, condensation, drying device, add sodium bicarbonate 0.26g, triethylamine 0.89g, carbon tetrachloride 5.32g, 4-hydroxystyrene 0.36g successively, open stirring device, Cool in an ice-water bath to 5°C, slowly add a mixture of 0.69g of dibutyl phosphite and 4.05g of carbon tetrachloride dropwise from the dropping funnel, and drop it over in 2 hours; keep the reaction at 5-8°C for 36 hours to complete the reaction, and filter to form The solid was spinned off to remove the reaction solvent, and the product was separated by column chromatography (ethyl acetate:petroleum ether=2:1) ​​to obtain sample 0.91. Yield 96.9%.

Embodiment 3

[0018] Embodiment 3, in the four-necked flask that stirring, condensation and drying device are housed, add catalyst sodium carbonate 1.05g and tetrabutylammonium hydroxide 1.25g successively, carbon tetrachloride 6.35g, 4-hydroxystyrene 0.60g, Turn on the stirring device, cool to 3°C in an ice-salt bath, and slowly add a mixture of 0.69 g of diethyl phosphite and 4.37 g of carbon tetrachloride dropwise from the dropping funnel, and the drop will be completed in about 2.5 hours. Keep the reaction at 3-10°C for 40 hours to complete the reaction, filter off the generated solid, spin off the reaction solvent, and separate the product by column chromatography (ethyl acetate:petroleum ether=1:1) to obtain a sample of 1.23g. Yield 96.3%.

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Abstract

The invention discloses a phosphate flame retardant containing a styrene structure, which is prepared from phosphorous acid dialkyl ester, 4-hydroxy styrenes and carbon tetrachloride reacting under the existence of a catalyst. The catalyst is compound of organic alkali and inorganic alkali. The organic alkali catalyst is pyridine or triethylamine or diethylamine or phenylamine or triethanolamine or diethanol amine or alkyl benzene amine or tetrabutylammonium hydroxide or tetraethylammonium hydroxide; the inorganic alkali catalyst is sodium bicarbonate or potassium bicarbonate or sodium hydroxide or potassium hydroxide or sodium carbonate or potassium carbonate or sodium benzoate or potassium benzoate; the molar ratio of the organic alkali to the 4-hydroxy styrenes is 3-1 to 1, and the molar ratio of the inorganic alkali to the 4-hydroxy styrenes is 1.1-1 to 1. A phosphate molecule contains active double bonds and is easily subjected to polymerization reaction together with the active double bonds such as styrene and the like. The carbon tetrachloride is adopted as a solvent to react at the low temperature in a synthesis process. The synthesis method has the advantages of high reaction yield, convenience for reaction operation, easiness of industrialization and the like compared with the traditional phosphoryl chloride method.

Description

technical field [0001] The invention relates to a phosphate ester flame retardant containing styrene structure and a synthesis method thereof. technical background [0002] Phosphate ester flame retardants have been widely used in various plastics such as polyvinyl chloride, polyester, and polyurethane due to their excellent processing and flame retardant properties. Most of the traditional flame retardants are added to the substrate in the form of blending during processing, so as to endow the material with certain flame retardant properties. This method is easy to operate and easy to produce. Its shortcoming is that because the flame retardant is added in the form of physical blending, it deteriorates the mechanical and impact resistance of the material and other physical properties. [0003] The traditional synthetic method of phosphoric acid ester is generally prepared by reacting phosphorus oxychloride and corresponding alcohol at a certain temperature. When prepared ...

Claims

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Application Information

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IPC IPC(8): C08F212/14C07F9/12
Inventor 沈琦杨建伟
Owner JIANGSU YOKE TECH
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