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Preparation method of triethyl phosphate

A technology of triethyl phosphate and phosphorus trichloride, which is applied in the chemical industry, can solve problems such as insufficient reaction, many organic salt waste residues, and large loss of ethanol, and achieves low-cost raw materials, simple production process, and low unit consumption of ethanol Effect

Inactive Publication Date: 2013-10-30
JIANGSU DAMING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the reaction process of this process, a large amount of hydrogen chloride gas and a small amount of ethyl chloride will be generated, the loss of ethanol is also large, there are many side reactions, and the reaction is not sufficient. The generated triethyl phosphate will decompose under acidic conditions. Also can produce more organic salt waste residue, product yield only has 85~90%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 150g of absolute ethanol into a stirred 500ml four-necked flask equipped with reflux condenser, add 3 drops of methyl red as indicator, turn on the stirring, slowly pass in ammonia gas, and add 137.5g of phosphorus trichloride dropwise at the same time , Adjust the adding rate of ammonia and phosphorus trichloride, make the reaction liquid always orange, and cool with ice water, control the reaction temperature to 0~10℃, after the addition of phosphorus trichloride is completed, stop the ammonia gas and The reaction was kept at 10°C for 2 hours, and then the by-product ammonium chloride was removed by filtration (about 160 g of ammonium chloride was obtained after drying). Transfer the filtrate to another 500ml four-necked flask, continuously pour high-purity oxygen into the solution, cool and control the reaction temperature to 80℃, after the solution no longer exotherms significantly, continue to pour in oxygen and keep at 80℃ for 2h After the reaction is completed...

Embodiment 2

[0017] Put 300g of absolute ethanol in a stirred 500ml four-necked flask equipped with reflux condenser, drop 3 drops of methyl red as indicator, turn on the stirring, slowly pass in ammonia gas, while adding 137.5g of phosphorus trichloride dropwise , Adjust the adding rate of ammonia and phosphorus trichloride, make the reaction liquid always orange, and cool with ice water, control the reaction temperature to 0~10℃, after the addition of phosphorus trichloride is completed, stop the ammonia gas and The reaction was kept at 10°C for 2 hours, and then the by-product ammonium chloride was removed by filtration (about 160 g of ammonium chloride was obtained after drying). Transfer the filtrate to another 500ml four-necked flask, continuously pour high-purity oxygen into the solution, cool and control the reaction temperature to 80℃, after the solution no longer exotherms significantly, continue to pour in oxygen and keep at 80℃ for 2h After the reaction is completed, the materia...

Embodiment 3

[0019] Put 150g of absolute ethanol into a stirred 500ml four-necked flask equipped with reflux condenser, add 3 drops of methyl red as indicator, turn on the stirring, slowly pass in ammonia gas, and add 137.5g of phosphorus trichloride dropwise at the same time , Adjust the adding rate of ammonia and phosphorus trichloride, make the reaction liquid always orange, and cool with ice water, control the reaction temperature to 10-20 ℃, after the dropwise addition of phosphorus trichloride, stop the ammonia gas and The reaction was kept at 10°C for 2 hours, and then the by-product ammonium chloride was removed by filtration (about 160 g of ammonium chloride was obtained after drying). Transfer the filtrate to another 500ml four-necked flask, continuously pour high-purity oxygen into the solution, cool and control the reaction temperature to 80℃, after the solution no longer exotherms significantly, continue to pour in oxygen and keep at 80℃ for 2h After the reaction is completed, ...

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Abstract

The invention relates to a preparation method of triethyl phosphate. The method specifically comprises the following steps of: first, with ammonia gas as an acid-binding agent and methyl red as an indicator, reacting phosphorus trichloride with absolute ethyl alcohol to generate triethyl phosphite; filtering out the byproduct ammonium chloride and then, introducing a certain amount of oxygen for oxidization; and finally, distilling and purifying at reduced pressure to obtain the target product triethyl phosphate. The method provided by the invention has the advantages that the yield is high, the unit consumption is low, and the byproduct ammonium chloride can be used as a fertilizer; and the method is simple in production process, the raw materials are easily available and the production safety is high.

Description

Technical field [0001] The invention belongs to the field of chemical engineering, and specifically relates to a preparation method of triethyl phosphate. Background technique [0002] Triethyl phosphate, molecular formula C 6 H 15 O 4 P, whose English name is abbreviated as TEP, is a colorless transparent liquid, soluble in water, and also soluble in organic solvents such as ethanol, benzene, aromatic hydrocarbons, esters, and chloroform. It is mainly used as high boiling point solvents, rubber and plastic enhancement Plasticizers can also be used as halogen-free flame retardants, raw materials for the preparation of pesticides and pesticides, ethylating reagents, etc. [0003] The existing preparation processes all use phosphorus oxychloride and excess absolute ethanol to undergo an esterification reaction, and then undergo dealcoholization, neutralization, rectification and other processes to obtain a finished product of triethyl phosphate. During the process of this process, a...

Claims

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Application Information

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IPC IPC(8): C07F9/11
Inventor 潘小明仇国才史广平
Owner JIANGSU DAMING TECH
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