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Preparation process for high-purity low-arsenic hydroxyethylidene diphosphonic acid

A technology of hydroxyethylene diphosphonic acid and preparation process, applied in the field of preparation of hydroxyethylene diphosphonic acid, can solve the problems of increasing impurities, increasing production cost, poor quality stability of amino trimethylene phosphonic acid and the like, and achieving The effect of reducing equipment investment, good stability and mild process control conditions

Active Publication Date: 2014-01-15
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] The first step: first put 5500kg of acetic acid and 6kg of ammonium thioacetate into the reactor, under the condition of stirring, the temperature is controlled at 50~60°C and the pressure is below 200mmHg, and 2000 kg of phosphorus trichloride is added dropwise into the reactor, and then 8kg of sulfur Substitute 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 dropwise addition, stir at a speed of 60 r / min for 1 Hours, and 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 p...

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 reaction kettle, control the temperature at 50~60℃ and the pressure below 200mmHg under stirring conditions, add 2500 kg of phosphorus trichloride dropwise into the reaction kettle, and then add 6kg of sulfur Substitute ammonium acetate into the reactor, 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 reactor dropwise, after the addition is complete, stir at a speed of 50 r / min for 2 Hours, and 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 hy...

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] The first step: first put 5800kg of acetic acid and 8kg of ammonium thioacetate into the reactor, under the condition of stirring, the temperature is controlled at 50~60°C and the pressure is below 200mmHg, and 2300 kg of phosphorus trichloride is added dropwise into the reactor, and then 10kg of sulfur Substitute ammonium acetate into the reactor, 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 reactor dropwise, after the addition is completed, stir at a speed of 55 r / min for 3 Hours, and finally the temperature is slowly raised to 100°C. The hydrogen chloride gas produced in this process is absorbed by the hydrogen chloride absorber...

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PUM

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Abstract

The invention relates to a preparation process for high-purity low-arsenic hydroxyethylidene diphosphonic acid. The preparation process comprises the following steps: with phosphorus trichloride, acetic acid and ammonium thioacetate as raw materials, controlling process conditions at first, reacting acetic acid with phosphorus trichloride in a reaction vessel to produce hydroxyethylidene diphosphonic acid and adding ammonium thioacetate in the process of the reaction; and then subjecting an obtained material to concentration and air flushing to remove impurities, adding ammonium thioacetate and carrying out arsenic removal and centrifugation so as to obtain the high-purity low-arsenic hydroxyethylidene diphosphonic acid. According to the invention, scientific technology is employed for product purification, no other substance like a crystal nucleus and a crystallization promoter is added, so no new impurity is introduced. Hydroxyethylidene diphosphonic acid in the high-purity low-arsenic hydroxyethylidene diphosphonic acid prepared in the invention is more than 95%, and arsenic content in the high-purity low-arsenic hydroxyethylidene diphosphonic acid is less than 2 ppm; the preparation process overcomes problems in packaging, transporting and on-site application of liquid hydroxyethylidene diphosphonic acid and broadens the application fields of the high-purity low-arsenic hydroxyethylidene diphosphonic acid.

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 Applications(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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