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Green synthetic phosphate preparation method

A green synthesis, phosphate ester technology, applied in chemical instruments and methods, phosphorus organic compounds, compounds of Group 5/15 elements of the periodic table, etc., can solve problems that have not yet been reported on the application of polymer Lewis acid catalysts, Achieve the effect of reducing production labor cost, high purity and high yield

Active Publication Date: 2019-07-26
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] There have been no reports on the application of polymer Lewis acid catalysts in the ring-opening esterification of phosphate esters

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0048] Examples 1-3 relate to the preparation of polymer Lewis acid catalysts:

Embodiment 1

[0050] 1. Weigh 1000g of macroporous spherical cation exchange resin (hereinafter referred to as macromolecular resin) produced by copolymerization of styrene and divinylbenzene, wash it with distilled water, and dry it in vacuum at 100-105°C for 15 hours before use;

[0051] 2. Weigh 8g of dried macromolecular resin, 50ml of carbon disulfide, 24g of tin tetrachloride and put it into a four-necked flask and heat to reflux for 4-5 hours, cool to room temperature, slowly add 50ml of water dropwise and stir for 30 minutes , Filtered and washed with acetone to obtain a polymer Lewis acid catalyst, dried in vacuum at 100-105°C for 5 hours, measured by atomic absorption spectrometer, and the tin content was 8.5%.

Embodiment 2

[0053] Weigh 8g of dried macromolecular resin, 50ml of carbon disulfide, and 20g of titanium tetrachloride into a four-necked flask and heat to reflux for 4-5 hours, cool to room temperature, slowly add 50ml of water, stir for 30 minutes, and filter , Washed with acetone to obtain a polymer Lewis acid catalyst, dried in vacuum at 100-105°C for 5 hours, measured by atomic absorption spectrometer, and the titanium content was 8.2%.

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Abstract

The invention relates to a green synthetic phosphate preparation method which includes the steps: taking a macromolecular lewis acid catalyst as a catalyst; performing esterification reaction on phosphorus oxychloride and an epoxy compound; recycling the epoxy compound in a decompressed manner after complete reaction; filtering reactants to obtain phosphate. Alkali washing and water scrubbing areomitted, production cost is greatly saved, social environments are not polluted, and the preparation method conforms to green chemical synthesis and suitable for industrial popularization and application.

Description

Technical field [0001] The invention relates to the technical field of fine chemical production, in particular to a preparation method of green synthetic phosphate ester. Background technique [0002] Phosphate is an ester derivative of phosphoric acid. Mainly used for flame retardant of polystyrene, polyurethane foam, polyester, polycarbonate and liquid crystal polymer materials, its production cost is low, the price is cheap, and the advantages of high flame retardancy are broad in the above fields, although it is used in toys by the European Union The field is restricted, but in some fields it has an irreplaceable flame retardant effect. [0003] Common phosphate esters are TDCP, TCPP, TECP. In the preparation methods, most of them use Lewis acid as catalyst, and phosphorus oxychloride reacts with epoxy compound, and the post-treatment is alkali washing and water washing. During the above reaction: [0004] 1) The necessity of the catalyst: the ring-opening reaction of phosphor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
CPCC07F9/091Y02P20/584
Inventor 牛丽丹冯舜金译平
Owner ZHEJIANG WANSHENG
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