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Method for producing ethyl phosphate with high purity

A technology for the production of triethyl phosphate, applied in the direction of phosphorus organic compounds, can solve the problems of increased alcohol consumption, increased production cost, incomplete reaction, etc., and achieve the effect of reducing consumption, reducing equipment investment, and complete reaction

Inactive Publication Date: 2003-05-07
无锡市红星化工厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The defect of this technique is that because the reaction temperature is relatively low, usually below 15°C, it needs to be cooled in most seasons, which increases the production cost; secondly, in this technique, the combination of phosphorus oxychloride and absolute ethanol Ratio is usually 1: 6 or more than 1: 8, when adopting the proportioning ratio of 1: 6, reaction is not complete, when adopting the proportioning ratio of 1: 8 or more, increased alcohol consumption again; In addition, in the prior art Among them, rectification is usually used to obtain high-purity triethyl phosphate, so the equipment investment is relatively large, the output rate is relatively low, and the product is also easy to decompose during the rectification process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] a. Esterification reaction, put 30 kg of absolute ethanol into a 1000 liter reactor, start stirring, and inject cooling liquid ice salt water into the jacket of the reactor, and when the temperature in the reactor drops to 15°C, start Phosphorus oxychloride is added dropwise, and the reaction temperature is controlled by the rate of addition during the whole dropping process. The reaction temperature is maintained at 25°C. The time for dropping phosphorus oxychloride is greater than or equal to 1.5 hours until the ratio of phosphorus oxychloride to absolute ethanol reaches Up to 1:7, the unit is molar concentration. After dropping phosphorus oxychloride into the reactor, continue to keep the temperature at 25°C to carry out the deepening reaction for 2 hours. The vacuum degree in the reaction kettle is limited to the dropwise addition of phosphorus oxychloride, generally 0.06 MPa.

[0015] b, dealcoholization, the deepening reaction is completed, the material is transfe...

Embodiment 2

[0020] The difference between embodiment two and embodiment one is that the temperature that begins to drop phosphorus oxychloride in esterification reaction a is 13 ℃, and the reaction temperature used is 20 ℃, and the time of deepening reaction is 2.5 hours; The dealcoholization time is 1 hour; when neutralizing, the PH value is 6, and after stopping adding soda ash, continue to stir for 8 minutes; when distilling, the initial distillation time is 2 hours, and during the second distillation, remove the low boiler for the first time The temperature is 85°C.

Embodiment 3

[0022] The difference between embodiment three and embodiment one is that the temperature that begins to drop phosphorus oxychloride in esterification reaction a is 17 ℃, and the reaction temperature used is 30 ℃, and the time of deepening reaction is 1.5 hours; The dealcoholization time is 1.5 hours; when neutralizing, the pH value is 7, after stopping adding soda ash, continue to stir for 12 minutes; when distilling, the initial distillation time is 3 hours

[0023] During the second distillation, the temperature for removing the low boilers for the first time is 95°C.

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PUM

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Abstract

A process for preparing high-purity triethyl phosphate includes such steps as esterifying reaction between absolute alcohol and phosphorus trioxychloride at 20-30 deg.C, removing alcohol under 0.098 MPa for 1-1.5 hr, neutralizing by adding sodium carbonate while stirring to pH 6-7, and distilling. Its advantages are high purity and output rate and low cost.

Description

technical field [0001] The invention relates to a chemical product, in particular to a method for producing high-purity triethyl phosphate. Background technique [0002] Triethyl phosphate (TEP) is generally used as a catalyst for the production of ketene, an ethylating agent, a high boiling point solvent, a stabilizer for chlorine-based pesticides, a plasticizer for synthetic resins, a flame retardant for polyester resins, and lubricating oils additives, etc. In the prior art, triethyl phosphate is mainly prepared by adding phosphorus oxychloride into a container of absolute ethanol in a certain ratio, performing a chemical reaction at a lower temperature, and then undergoing rectification and other processes. . The defect of this technique is that because the reaction temperature is relatively low, usually below 15°C, it needs to be cooled in most seasons, which increases the production cost; secondly, in this technique, the combination of phosphorus oxychloride and abso...

Claims

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Application Information

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IPC IPC(8): C07F9/09
Inventor 陈静忠姚国良
Owner 无锡市红星化工厂
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