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Preparation of diethyl phosphoric acid

A technology of triethyl phosphate and ethanol, which is applied to organic phosphorus compounds, compounds of group 5/15 elements of the periodic table, chemical instruments and methods, and can solve problems such as loss of products, ethanol and extractants

Inactive Publication Date: 2006-01-18
BAYER AG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This results in an undesired loss of product, ethanol and extractant

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Reactions were carried out in a stirred tube reaction set consisting of three stirred tanks each with a liquid capacity of 1 liter. The three stirring tanks are connected to each other and to the storage tank via a submerged connection so that the reaction product can easily overflow to the storage tank. All three stirred tanks were fitted with reflux condensers, which were connected to each other and to a cooling circuit at -20°C.

[0041]The first stirred tank was kept at internal temperature (reaction temperature) 3-6°C, the second stirred tank was at 13-15°C, and the third stirred tank was at 18-20°C by external cooling (thermostat). 517.5 g / h of ethanol (11.25 mol / h) and 383.8 g / h of phosphorus oxychloride (2.5 mol / h) were metered continuously into the first stirred tank.

[0042] The stirring tank set and the storage tank are connected via a valve and connected to a vacuum pump via a scrubber, which is used to maintain the pressure of the stirring tank set at 50 ...

Embodiment 2

[0048] Example 2 was carried out in a similar manner to Example 1, except that 598 g / h ethanol (13 mol / h) and 307 g / h phosphorous oxychloride (2 mol / h) were metered in continuously into the first stirred tank.

[0049] Upon reaching the equilibrium of the reaction tank set, the reaction product obtained in the storage tank consisted of 57.4 wt % triethyl phosphate, 35.5 wt % ethanol and 7.1 wt % hydrogen chloride. Separation in the degassing column gave 367 g / h of crude product containing 96.8% by weight of triethyl phosphate. The resulting product was extracted by distillation and contained more than 99% by weight of triethyl phosphate in 96.3% yield based on phosphorous oxychloride used.

[0050] 1034g / h of fresh water is added to the washing tower from above, and about 1575g / h of liquid from the washing circuit is sent to the connected distillation tower for azeotropic distillation. At the top of the distillation column, 358 g / h of a mixture of 90% by weight of ethanol and...

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PUM

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Abstract

The invention relates to a process for preparing triethyl phosphate by reacting phosphorus oxychloride with a greater than stoichiometric quantity of ethanol under reduced pressure at temperatures of from 0 to 50 DEG C. in a reaction vessel, whereina) the volatile components resulting from the reaction are predominantly condensed by means of a reflux condenser and the remaining volatile components are passed into a scrubber filled with water,b) after the end of the reaction, the reaction mixture is separated distillatively in an outgassing column into a top product and a bottom product which predominantly comprises triethyl phosphate,c) the top product of the outgassing column is combined with the contents of the scrubber and d) the contents of the scrubber are separated distillatively in an azeotropic distillation to obtain water and ethanol as top product and the ethanol, preferably after dewatering, is preferably returned to the reaction.

Description

Field of Invention [0001] The present invention relates to a method for preparing triethyl phosphate by reacting phosphorus oxychloride with ethanol. technical background [0002] Trialkyl phosphates are very versatile. For example, as plasticizers, non-reactive flame retardants, hardeners and accelerators in plastics and coatings, and as auxiliaries in textiles and paper products. They are also used in the chemical industry as wetting agents, flotation agents, defoamers, emulsifiers, stabilizers or extractants. [0003] Various methods are known for the preparation of trialkyl phosphates from phosphorus oxychloride and the corresponding alcohol. In the past, attempts have been made to improve the preparation method in terms of reaction temperature, proportions of ingredients used and transfer of heat of reaction. The problem in the reaction of these two components is the formation of hydrogen chloride, which must be removed from the reaction mixture very rapidly and comp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/09C07F9/11
CPCC07F9/11
Inventor K·-H·米特施克K·哈伦博格O·施拉克J·考伦
Owner BAYER AG