A kind of preparation method of synthetic phosphoric acid ester

A phosphate ester and Lewis acid 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 costs, reducing environmental pollution, and high purity

Active Publication Date: 2021-07-23
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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  • A kind of preparation method of synthetic phosphoric acid ester
  • A kind of preparation method of synthetic phosphoric acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0048] Embodiment 1-3 relates to the preparation of polymer Lewis acid catalyst:

Embodiment 1

[0050] 1. Weigh 1000 g of macroporous spherical cation exchange resin (hereinafter referred to as macromolecular resin) generated by the copolymerization of styrene and divinylbenzene, wash with distilled water, and vacuum-dry at 100-105° C. for 15 hours after washing, and set aside;

[0051]2. Weigh 8g of dried macromolecular resin, 50ml of carbon disulfide, and 24g of tin tetrachloride into a four-necked flask, heat and 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, which was vacuum-dried at 100-105° C. for 5 hours, and determined by an 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-neck flask, heat and reflux for 4-5 hours, cool to room temperature, slowly add 50ml of water dropwise, stir for 30 minutes, and filter , washed with acetone to obtain a polymer Lewis acid catalyst, vacuum-dried at 100-105° C. for 5 hours, and determined by an atomic absorption spectrometer, the titanium content was 8.2%.

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Abstract

The invention relates to a preparation method for synthesizing phosphoric acid ester. The method comprises the following steps: using a polymer Lewis acid catalyst as a catalyst, carrying out esterification reaction between phosphorus oxychloride and an epoxy compound, and recovering the epoxy compound under reduced pressure after the reaction is complete. Filter to obtain phosphate ester. The preparation method provided by the invention does not need alkali washing or water washing, greatly saves production cost, has no pollution to the social environment, conforms to the synthesis of green chemistry, and is suitable for industrial promotion and application.

Description

technical field [0001] The invention relates to the technical field of fine chemical production, in particular to a preparation method for synthesizing phosphoric acid ester. Background technique [0002] Phosphates are ester derivatives of phosphoric acid. It is mainly used for the flame retardancy of polystyrene, polyurethane foam, polyester, polycarbonate and liquid crystal polymer materials. Its production cost is low, the price is cheap, and its advantages such as high flame retardancy are widely used in the above fields. Although it is used by the European Union in toys The field is limited, but it has an irreplaceable flame retardant effect in some fields. [0003] Common phosphoric acid esters include TDCP, TCPP, and TECP. Most of the preparation methods use Lewis acid as a catalyst, react phosphorus oxychloride with epoxy compounds, and perform alkali washing and water washing in post-treatment. During the above reaction process: [0004] 1) Necessity of catalyst...

Claims

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Application Information

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Patent Type & Authority Patents(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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