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Method for producing dibutyl phosphate by comprehensively using three wastes in production process

A technology of dibutyl phosphate and production process, which is applied in the field of directly producing dibutyl phosphate with alcohol and phosphorus oxychloride, can solve the problems of repetition, waste of water, large energy consumption, etc., so as to save processes and equipment, reduce Water consumption and effect of reducing equipment investment

Inactive Publication Date: 2012-02-15
周滢
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The method for existing production dibutyl phosphate has following shortcoming: 1, waste raw material, yield is low, cost is high; 2, have a large amount of three wastes that can't handle and cause environmental pollution; Phosphate dibutyl ester or tributyl phosphate, reproducing dibutyl phosphate, the process design is unreasonable, there are repetitions, the whole production process has not only wasted equipment, but also wasted manpower, material resources and financial resources; 5, in the production process, a large amount of Washing with water, not only wastes water, but also pollutes water

Method used

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  • Method for producing dibutyl phosphate by comprehensively using three wastes in production process
  • Method for producing dibutyl phosphate by comprehensively using three wastes in production process
  • Method for producing dibutyl phosphate by comprehensively using three wastes in production process

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Effect test

Embodiment 1

[0024] (1) Synthesis: Take 0.90mol of phosphorus oxychloride and place it in a jacketed enamel reaction kettle, pass supercooled water below 0°C in the enamel reaction kettle jacket, and install a 10m 2 Cooling water is passed through the condenser; slowly add 2.20mol n-butanol and stir to keep the temperature of the whole reaction process at 0-10°C; continue stirring for 1 hour after the addition of n-butanol is completed, and keep the temperature at 10°C under normal pressure ;

[0025] (2) Ripening: heat up to raise the temperature of the reaction solution to 30°C, keep stirring at normal pressure for 3 hours, and the HCl gas generated during the ripening process is absorbed by n-butanol through the condenser;

[0026] (3) Acid discharge: heat up to 40°C, pressurize to 80kPa, continue stirring for 3 hours; then heat up to 50°C, vacuumize, the vacuum degree is greater than 18mmHg column, and continue stirring for 3 hours; the HCl gas generated during the acid discharge proce...

Embodiment 2

[0042] (1) Synthesis: Take 1.10mol of phosphorus oxychloride and place it in a jacketed enamel reaction kettle, pass supercooled water below 0°C in the enamel reaction kettle jacket, and install a 10m 2 Cooling water is passed through the condenser; slowly add 2.30mol n-butanol and stir to keep the temperature of the whole reaction process at 0-10°C; continue to stir for 2 hours after the addition of n-butanol is completed, and keep the temperature at 10°C under normal pressure ;

[0043] (2) Ripening: heat up, make the temperature of the reaction solution rise to 25°C, keep the normal pressure and continue to stir for 2h, the HCl gas generated during the ripening process is absorbed by n-butanol through the condenser;

[0044] (3) Acid discharge: raise the temperature to 35°C, pressurize to 75kPa, continue to stir for 2 hours; then raise the temperature to 45°C, evacuate, the vacuum degree is greater than 18mmHg column, and continue to stir for 2 hours; the HCl gas generated ...

Embodiment 3

[0052] (1) Synthesis: Take 1mol of phosphorus oxychloride and place it in a jacketed enamel reaction kettle, pass supercooled water below 0°C in the enamel reaction kettle jacket, and install a 10m 2 Cooling water in the condenser; slowly add 2.3mol n-butanol and stir, keep the temperature of the whole reaction process at 0-10°C; continue stirring for 1 hour after the addition of n-butanol, and keep the temperature at 12°C under normal pressure ;

[0053] (2) Ripening: heat up to raise the temperature of the reaction solution to 30°C, keep stirring at normal pressure for 3 hours, and the HCl gas generated during the ripening process is absorbed by n-butanol through the condenser;

[0054] (3) Acid discharge: heat up to 45°C, pressurize to 85kPa, continue stirring for 3 hours; then heat up to 55°C, vacuumize, the vacuum degree is greater than 18mmHg column, and continue stirring for 3 hours; the HCl gas generated during the acid discharge process is condensed The device is abs...

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Abstract

The invention relates to a method for producing dibutyl phosphate by comprehensively using three wastes in a production process, and belongs to the technical field of organic synthesis. The dibutyl phosphate product is obtained by reacting butanol and phosphorus oxychloride, synthesizing, curing, discharging acid, alkali washing, acid washing, washing and refining. By the method, the equipment investment is reduced, and processes and equipment for producing dibutyl phosphite or tributyl phosphate are saved; manpower is reduced, energy is saved, and pollution is reduced; and the three wastes generated in the production process are totally utilized and treated, so that the consumption of water is greatly reduced, water pollution is prevented, the yield is improved, and the cost is reduced. After the three wastes are treated, the butanol serving as a secondary product can be obtained; and after HCl is reclaimed by using alcohol, the HCl is easily separated from the alcohol, and the separated HCl can be used for producing methyl chloromethyl ether, triethyl orthoacetate, ethanamidine hydrochloride and the like.

Description

technical field [0001] The invention relates to a production method of dibutyl phosphate in which three wastes are comprehensively utilized in the production process, in particular to a method for directly using alcohol and phosphorus oxychloride to produce dibutyl phosphate, and the three wastes are effectively eliminated in the whole production process The comprehensive utilization and treatment belongs to the technical field of organic synthesis. Background technique [0002] According to "Xinhua Dictionary", the three wastes refer to the waste water, waste gas and waste residue of factories. For the "three wastes" according to different situations, measures such as multi-stage purification, decontamination, compression and volume reduction, incineration, and solidification are adopted for treatment and disposal. This process is called "three wastes" treatment and disposal. [0003] The existing production of dibutyl phosphate is mainly made by adding a strong oxidant p...

Claims

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Application Information

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IPC IPC(8): C07F9/11C07C31/12C07C29/74B01D53/14
Inventor 周滢
Owner 周滢
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