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A kind of preparation technology of high-purity low-arsenic hydroxyethylidene diphosphonic acid

A hydroxyethylene diphosphonic acid and a preparation process technology, applied in the field of preparation of hydroxyethylene diphosphonic acid, can solve the problems of poor quality stability of aminotrimethylene phosphonic acid, increase of impurities, increase of production cost, etc., and achieve Moderate process control conditions, reduced equipment investment, and good stability

Active Publication Date: 2016-08-03
HENAN QINGSHUIYUAN TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] These processes all divide the production, purification and arsenic removal procedures of hydroxyethylene diphosphonic acid into a single independent production process, which undoubtedly increases the entire production cost, and the quality of aminotrimethylene phosphonic acid produced by the above processes poor stability
In the preparation process, the purpose of concentration and purification has been achieved by adding crystal nuclei and crystal aids. Such operations will undoubtedly increase the impurities of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation process of high-purity and low-arsenic hydroxyethylene diphosphonic acid uses phosphorus trichloride, acetic acid, and ammonium thioacetate as raw materials, and proceeds in accordance with the following steps:

[0021] Step 1: First put 5500kg of acetic acid and 6kg of ammonium thioacetate into the reactor, under stirring conditions, control the temperature at 50~60°C and the pressure below 200mmHg, add 2000kg of phosphorus trichloride dropwise into the reactor, and then add 8kg of thioacetate Put ammonium acetate into the reactor, stop stirring, let it stand for 2 hours, then control the temperature at 40~50°C and the pressure below 200mmHg, add 5500kg of phosphorus trichloride to the reactor dropwise, after the addition is completed, stir at a speed of 60r / min for 1 hour, Finally, the temperature is slowly raised to 100°C. The hydrogen chloride gas produced in this process is absorbed by the hydrogen chloride absorber to produce hydrochloric acid as a by...

Embodiment 2

[0030] A preparation process of high-purity and low-arsenic hydroxyethylene diphosphonic acid uses phosphorus trichloride, acetic acid, and ammonium thioacetate as raw materials, and proceeds in accordance with the following steps:

[0031] Step 1: First, put 6000kg of acetic acid and 10kg of ammonium thioacetate into the reactor, control the temperature at 50~60°C and the pressure below 200mmHg under stirring conditions, add 2500kg of phosphorus trichloride dropwise into the reactor, and then add 6kg of thioacetate Put ammonium acetate into the reaction kettle, stop stirring, let it stand for 3 hours, then control the temperature at 40~50°C and the pressure below 200mmHg, add 5000 g of phosphorus trichloride to the kettle dropwise, after the addition is completed, stir at a speed of 50r / min for 2 hours, Finally, the temperature is slowly raised to 100°C. The hydrogen chloride gas produced in this process is absorbed by the hydrogen chloride absorber to produce hydrochloric aci...

Embodiment 3

[0040] A preparation process of high-purity and low-arsenic hydroxyethylene diphosphonic acid uses phosphorus trichloride, acetic acid, and ammonium thioacetate as raw materials, and proceeds in accordance with the following steps:

[0041] Step 1: First, put 5800kg of acetic acid and 8kg of ammonium thioacetate into the reactor, under stirring conditions, control the temperature at 50~60°C and the pressure below 200mmHg, add 2300kg of phosphorus trichloride dropwise into the reactor, and then add 10kg of thioacetate Put ammonium acetate into the reaction kettle, stop stirring, let it stand for 4 hours, then control the temperature at 40~50°C and the pressure below 200mmHg, add 5200 g of phosphorus trichloride to the kettle dropwise, after the addition is completed, stir at a speed of 55r / min for 3 hours, Finally, the temperature is slowly raised to 100°C. The hydrogen chloride gas produced in this process is absorbed by the hydrogen chloride absorber to produce hydrochloric ac...

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Abstract

The invention relates to a preparation process of high-purity and low-arsenic hydroxyethylidene diphosphonic acid. It uses phosphorus trichloride, acetic acid and ammonium thioacetate as raw materials. Firstly, the process conditions are controlled, and the acetic acid and phosphorus trichloride are React in a reactor to generate hydroxyethylene diphosphonic acid, add ammonium thioacetate during the reaction process; then concentrate the material, aerate, remove impurities, add ammonium thioacetate during the process, remove arsenic, and finally centrifuge to obtain High purity low arsenic hydroxyethylene diphosphonic acid. The present invention adopts a scientific process to purify the product without adding other substances, such as crystal nuclei and crystal aids, and without introducing new impurities. The hydroxyethylene diphosphonic acid in the high-purity and low-arsenic hydroxyethylene diphosphonic acid obtained by the present invention reaches more than 95%, and the arsenic content is lower than 2ppm, which not only solves the problem of liquid hydroxyethylene diphosphonic acid packaging, The problem of circulation and on-site application, and broaden the application field of the product.

Description

technical field [0001] The invention relates to a preparation process of high-purity and low-arsenic hydroxyethylene diphosphonic acid, which belongs to the field of chemical industry. Background technique [0002] Hydroxyethylene diphosphonic acid is mainly used in industrial water treatment as a highly efficient stabilizer. It has good chelation, low limit inhibition, lattice distortion and other effects. It can prevent the formation of scaling salts in water, especially the formation of calcium carbonate scale. It also has a corrosion inhibitory effect and can be used as a chelating agent and a corrosion inhibitor. It is widely used as a scale and corrosion inhibitor in large-scale thermal power plants, circulating cooling water in oil refineries, oilfield water injection systems, and low-pressure boiler water. It is also used as a peroxide stabilizer and in industrial cleaning formulations, and as a flame retardant polyurethane foam. [0003] Generally, the produced ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 王志清杨海星李翠娥李太平
Owner HENAN QINGSHUIYUAN TECH
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