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Method for preparing phosphorous acid and hydrogen chloride

A technology of hydrogen chloride and phosphorous acid, applied in the direction of phosphorous acid, chlorine/hydrogen chloride, phosphorus oxyacid, etc., can solve the problems of reaction exotherm, gas entrainment, etc.

Active Publication Date: 2011-03-30
BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can solve the problems of exothermic reaction and phosphorus trichloride entrainment under normal conditions.

Method used

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  • Method for preparing phosphorous acid and hydrogen chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] according to figure 1 Shown is a central airlift internal loop reactor. The volume of the reactor is 5L. First, 2.5L of aqueous solution containing 30% hydrogen chloride is injected into the reactor. 10mol of 98% phosphorus trichloride enters the axial center of the system through the pump at a flow rate of 10mol / h from the bottom 7 of the reactor, and the reactor is controlled. The temperature is 50-80°C, the system pressure is -0.02-0.10MPa, the reaction feed liquid circulates from the outside of the inner sleeve of the reactor, and the hydrogen chloride gas overflows from the top 8 of the reactor and then enters the water system for absorption. After phosphorus trichloride added, continue to insulate for 0.5 hour, final hydrogen chloride yield 99.4% (calculated in phosphorus trichloride), phosphorous acid concentration is 26.51%, phosphorous acid total yield>99% (calculated in phosphorus trichloride ).

Embodiment 2

[0049] Using the same reactor as in Example 1, the volume of the reactor is 5L, first inject 2.0L of 30% hydrogen chloride aqueous solution into the reactor, and heat the aqueous solution to 70-75°C. 98% phosphorus trichloride enters the axial center of the system through a pump at a flow rate of 10 mol / h from the bottom of the reactor, and at the same time, 6.5 mol / h aqueous solution containing 30% hydrogen chloride enters from the top 5 of the reactor through a pump in the form of spraying system, the temperature inside the reactor is controlled at 50-80°C, the system pressure is -0.02-0.15MPa, the reaction feed liquid circulates from the outside of the inner sleeve of the reactor, and flows out continuously at the lower part 6 of the reactor; after the hydrogen chloride gas overflows from the top 8 of the reactor Enter the water system to absorb. The final yield of hydrogen chloride is 99.7% (calculated by phosphorus trichloride), the concentration of phosphorous acid in th...

Embodiment 3

[0051] according to figure 1 Shown is a central airlift internal loop reactor. The volume of the reactor is 5L. Firstly, 2.5L of bisglyphosate condensation mother liquor containing 10% hydrogen chloride is injected into the reactor, and then 10mol of 98% phosphorus trichloride enters the system axial direction through the pump at a flow rate of 2mol / h from the bottom 7 of the reactor. In the center, the feed liquid enters and exits the heat exchanger through 3 and 5 to cool the reaction liquid, and the temperature in the reactor is controlled at 30-50°C, and the system pressure is -0.05-0.1MPa. The reaction feed liquid circulates from the outside of the inner sleeve of the reactor, and the hydrogen chloride gas overflows from the top 8 of the reactor and then enters the water system for absorption. After the reaction temperature begins to drop, turn off the cooling water, adjust the flow rate of phosphorus trichloride to be 10mol / h, and enter the axial center of the system th...

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Abstract

The invention provides a method for preparing phosphorous acid and hydrogen chloride in an inner circulation tower by using phosphorus trichloride. The method comprises the following steps of: intermittently or continuously adding the phosphorus trichloride to the inner circulation tower, and then making the phosphorus trichloride react with a water solution in the tower to prepare a phosphorous acid water solution and a hydrogen chloride gas with large scale and high efficiency and yield and smoothly export the hydrogen chloride gas and heat. The method has the advantages of high reaction conversion rate and yield, steady reaction, high safety and the like and can be used for continuous production.

Description

field of invention [0001] The invention relates to a method for preparing phosphorous acid and hydrogen chloride. Background technique [0002] There are many methods for preparing phosphorous acid, such as: phosphorus trichloride hydrolysis method: direct hydrolysis with phosphorus trichloride and water, by-product hydrogen chloride gas; dimethyl phosphite raffinate hydrolysis method (CN1187459): use The raffinate of methyl ester is hydrolyzed at high temperature to prepare phosphorous acid, and methanol is recovered at the same time. Wang Zhengyan reported "Synthesis of phosphorous acid by hydrolysis of phosphorus trichloride" in the 11th issue of China's "Chlor-Alkali Industry" in 1989. However, the batch reaction was used in the article, and the hydrolysis reaction between phosphorus trichloride and water was violent, and the temperature was difficult to control. It takes a long time to slowly control phosphorus trichloride. Even so, the production safety is low and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/163C01B7/03
Inventor 郭钰来李建虹尹政清陈斌尹应武
Owner BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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