Preparation of diethyl phosphoric acid

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

Inactive Publication Date: 2003-06-04
BAYER AG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This results in an undesired loss

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0041]The first stirred tank was maintained at an internal temperature (reaction temperature) of 3-6 °C, the second at 13-15 °C and the third 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 stirred tank group and the storage tank are connected through a valve, and connected to a vacuum pump through a scrubber, which is used to maintain the pressure of the stirred tank group at 50 m...

Embodiment 2

[0048] Example 2 was carried out analogously to example 1, except that 598 g / h of ethanol (13 mol / h) and 307 g / h of phosphorus oxychloride (2 mol / h) were continuously metered into the first stirred tank.

[0049] The reaction product obtained in the storage tank consisted of 57.4% by weight of triethylphosphate, 35.5% by weight of ethanol and 7.1% by weight of hydrogen chloride when the equilibrium of the reaction tank set was reached. Separation in the degassing column yielded 367 g / h of crude product containing 96.8% by weight of triethylphosphate. The product obtained was removed by distillation and contained more than 99% by weight of triethyl phosphate in a yield of 96.3%, based on the phosphorus 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 o...

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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 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, it is used as a plasticizer, non-reactive flame retardant, hardener and accelerator in plastics and coatings, and as an auxiliary agent 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 trialkylphosphates from phosphorus oxychloride and the corresponding alcohols. In the past, attempts were made to improve the preparation method from the aspects of reaction temperature, ratio of ingredients used and transfer of heat of reaction. A problem in the reaction of these two components is the formation of hydrogen chloride, which must be removed very quickly and completely from the reactio...

Claims

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Application Information

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