Preparation method of phosphate ester compound

一种磷酸酯类、化合物的技术,应用在磷酸酯类化合物领域,能够解决副产物多、后处理复杂、成本高等问题,达到减少三废的产生、后处理简单、反应步骤少的效果

Active Publication Date: 2021-08-24
ZHEJIANG HONGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016]This method has many by-products, complex post-processing, high cost, and environmental protection
And diethyl sulfate price is more expensive, so the method cost is higher
[0017] In summary, there are many shortcomings in the prior art, for example, the raw materials used in method 1 and method 2 have potential safety hazards, method 3 has advantages in terms of safety, and phosphoric acid Sodium diethyl acetate is a common by-product in the production process. For example, sodium diethyl phosphate will be produced in the production process of whitening agent, so it can be used as a resource to produce valuable triethyl phosphate
However, the by-products generated in the reaction of the current method cannot be directly used and need subsequent treatment, so there are some defects in cost and environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1: the synthesis of triethyl phosphate

[0043] Experimental operation: Add 97g of sodium diethyl phosphate obtained from wastewater treatment into a 1000mL autoclave. Add 112g of cold ethyl chloride to 350mL of cold toluene to form a mixture of toluene and ethyl chloride. Add 6.2 g of benzyltriethylammonium bromide and toluene ethyl chloride mixture to the autoclave in turn. Seal the autoclave, heat up to 110°C with stirring, and keep it warm for 20 hours. After the reaction was completed, the autoclave was turned off and heated, and the temperature was naturally lowered to 50° C. under stirring. The reaction system was filtered and separated, and the filter cake was washed 3 times with 70 mL of toluene. All the toluene solutions obtained in the above process were combined and added to a 500mL single-necked round bottom flask, concentrated under reduced pressure to obtain the crude product of triethyl phosphate, and the crude product was distilled under re...

Embodiment 2

[0044] Embodiment 2: the synthesis of triethyl phosphate

[0045] Experimental operation: Add 97g of sodium diethyl phosphate obtained from wastewater treatment into a 1000mL autoclave. Add 112g of cold ethyl chloride to 350mL of cold xylene to form a mixture of xylene chloride and ethyl chloride. Add 6.2 g of benzyltriethylammonium chloride and xylene chloride into the autoclave in turn. Seal the autoclave, heat up to 130°C with stirring, and keep the temperature for 20 hours. After the reaction was completed, the autoclave was turned off and heated, and the temperature was naturally lowered to 50° C. under stirring. The reaction system was filtered and separated, and the filter cake was washed 3 times with 70 mL of xylene. All the xylene solutions obtained in the above process were combined and added into a 500mL single-necked round-bottomed flask, concentrated under reduced pressure to obtain the crude product of triethyl phosphate, and the crude product was distilled und...

Embodiment 3

[0046] Embodiment 3: the synthesis of triethyl phosphate

[0047] Experimental operation: Add 97g of sodium diethyl phosphate obtained from wastewater treatment into a 1000mL autoclave. Add 112g of cold ethyl chloride to 350mL of cold xylene to form a mixture of xylene chloride and ethyl chloride. Add 9.3g of tetrabutylammonium bromide and xylene chloride ethyl ethane mixture to the autoclave in turn. Seal the autoclave, heat up to 130°C with stirring, and keep the temperature for 5h. After the reaction was completed, the autoclave was turned off and heated, and the temperature was naturally lowered to 50° C. under stirring. The reaction system was filtered and separated, and the filter cake was washed 3 times with 70 mL of xylene. All the xylene solutions obtained in the above process were combined and added in a 500mL single-necked round-bottomed flask, concentrated under reduced pressure to obtain the crude product of triethyl phosphate, and the crude product was distille...

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Abstract

The invention discloses a preparation method of a phosphate ester compound, belonging to the field of phosphate ester compounds. The preparation method of the phosphate ester compound comprises the following steps: putting sodium diethyl phosphate into a reactor as a raw material, then putting a catalyst, a reaction solvent and an alkylating reagent into the reactor, conducting stirring, heating and reacting for a period of time, and finally, carrying out post-treatment on reaction liquid to obtain triethyl phosphate. According to the method, sodium diethyl phosphate is taken as the raw material, so the waste is treated by the waste, resources are recycled, and pollution is reduced; chloroethane is taken as the alkylating reagent; and thus, a novel, efficient, environment-friendly and economical method for synthesizing a triethyl phosphate compound is provided.

Description

technical field [0001] The invention relates to the field of phosphoric acid ester compounds, more specifically, relates to a new method for using ethyl chloride (CH3CH2Cl) as an alkylating agent to promote the reaction to generate triethyl phosphate. Background technique [0002] Due to its special physical properties and chemical stability, triethyl phosphate is widely used as a plasticizer for rubber and plastics, as well as a catalyst for organic synthesis reactions and a raw material for pesticides. Its molecular formula is C6H15O4P, and its relative molecular mass is 182.15. The structural formula of triethyl phosphate is: [0003] [0004] The existing method for preparing triethyl phosphate mainly comprises following three kinds: [0005] Method 1 is to mix phosphorus trichloride and toluene, add absolute ethanol under stirring, and control the temperature at 30-40°C. Continue to stir for 0.5h after the addition, and the reaction generates diethyl phosphite. T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11
CPCC07F9/11Y02P20/584
Inventor 王国森叶根灿刘肖晖袁银浩
Owner ZHEJIANG HONGDA CHEM
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