A kind of method for preparing trialkyl phosphate

A technology of trialkyl phosphate and phosphorus oxyhalide, which is applied in the chemical industry, can solve the problems of product yield and purity decline, and achieve the effects of improving yield and purity, mild reaction, and shortening reaction time

Active Publication Date: 2020-06-16
江苏中丽新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of doing this is that the catalyst is easily complexed with the product trialkyl phosphate, resulting in a decrease in product yield and purity. It is difficult to remove the acid and excess alcohol generated by vacuum distillation, which will also lead to product yield and purity. Purity drops

Method used

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Examples

Experimental program
Comparison scheme
Effect test

no. 1 example

[0017] Under the protection of nitrogen, under the condition of ice-water bath, 15.3g (0.1mol) phosphorus oxychloride and 9.4g (0.3mol) methanol were slowly added to the reaction vessel, stirred slowly for 10min, and then gradually heated to 20°C, Control the temperature for 10 minutes, add 1.2 g of D113 type resin, then slowly raise the temperature of the system to reflux for 20 minutes, stop the reaction, keep the temperature for another 10 minutes, slowly cool the system to room temperature, and distill under reduced pressure to remove excess alcohol and produced acid, the reduced pressure is -0.1MPa, the distillation time is 1h, and the bubbling method is used to further remove impurities for 1h, and the pH value of the crude product of trimethyl phosphate is measured to be 6.8, which meets the pH conditions. The product is rectified to obtain the product 13.5 g, the yield is 96.4%, as determined by HPLC, the purity is greater than 99.8%.

no. 2 example

[0019] Under the protection of helium, under the condition of ice-water bath, slowly add 15.3g (0.1mol) phosphorus oxychloride and 12.8g (0.4mol) methanol into the reaction vessel, stir slowly for 15min, and then gradually raise the temperature to 20°C , control the temperature for 15 minutes, add 1.4 g of D113 resin, then slowly raise the temperature of the system to reflux for 30 minutes, stop the reaction, keep the temperature for 10 minutes, slowly cool the system to room temperature, and distill under reduced pressure to remove excess alcohol and produced acid, the decompression pressure is -0.5MPa, the distillation time is 1.5h, and the bubbling method is used to continue to remove impurities for 1.5h, and the pH value of the crude product of trimethyl phosphate is measured to be 6, and the crude product is put into hydrogen with a mass concentration of 5%. Wash with alkali in sodium oxide solution, the measured pH is 7, extract, collect the organic phase, and rectify the...

no. 3 example

[0021] Under the protection of nitrogen, under the condition of ice-water bath, 30.7g (0.2mol) of phosphorus oxychloride and 55.2g (1.2mol) of ethanol were slowly added to the reaction vessel, stirred slowly for 15min, and then gradually heated to 30°C, Control the temperature for 20 minutes, add 8g of 732 type resin, then slowly raise the temperature of the system to reflux for 30 minutes, stop the reaction, keep the temperature for another 30 minutes, slowly cool the system to room temperature, and distill under reduced pressure to remove excess alcohol and acid produced in the system , the decompression pressure is -1MPa, the distillation time is 3h, and the bubbling method is used to further remove impurities for 2h. The pH value of the crude triethyl phosphate product is 6.9, which meets the pH condition. The product is rectified to obtain 35.3g of the product. The yield was 97%, and the purity was greater than 99.8% as determined by HPLC.

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PUM

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Abstract

The invention provides a method for preparing trialkyl phosphate, belonging to the chemical engineering field. The method comprises the steps of reacting by virtue of phosphorus oxyhalide and alcoholin an ice-water bath under the protection of inert gas, cooling a system to room temperature by taking ion exchange resin as a catalyst after the reaction, carrying out reduced pressure distillation to remove redundant alcohol and hydrochloric acid, further removing alcohol and acid in the system in one step by virtue of a bubbling method so as to obtain a trialkyl phosphate rough product, and carrying out reduced pressure rectification, so as to obtain a trialkyl phosphate purified product. By utilizing the catalyst, the compexing with trialkyl phosphate is avoided, so that the adverse effects caused by the complexing between a traditional catalyst and a product are effectively avoided, and the yield and purity of the product are increased; by further removing impurities in a bubbling manner, the impurities remained in the reduced pressure distillation process are effectively removed, so that the yield and purity of trialkyl phosphate are further increased; and the total yield of theproduct is more than 95.9%, and the purity of the product is more than 99.8%.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for preparing trialkyl phosphate. Background technique [0002] Trialkyl phosphate has a wide range of uses, such as plasticizers, flame retardants, and hardeners in plastics and coatings, as well as wetting agents, flotation agents, defoamers, emulsifiers, stabilizers, etc. . [0003] At present, the preparation method of trialkyl phosphate mainly adopts the reaction of phosphorus oxychloride and alcohol, and a catalyst can be added in the preparation process to facilitate the reaction. In the prior art, Lewis acid or titanate is usually used as a catalyst , in order to remove excess alcohol and generated acid, vacuum distillation is often used. The disadvantage of doing this is that the catalyst is easily complexed with the product trialkyl phosphate, resulting in a decrease in product yield and purity. It is difficult to remove the acid and excess alcoho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/11
CPCC07F9/11
Inventor 邹伟
Owner 江苏中丽新材料有限公司
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