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Hydroxyethylenediphosphonic acid production equipment and method

A hydroxyethylene diphosphonic acid, a technology for producing hydroxyethylene diphosphonic acid, applied in separation methods, chemical instruments and methods, organic chemistry, etc., can solve the volatilization loss of acetyl chloride, prolong the reaction time, and the reaction is not stable and other problems, to achieve the effect of speeding up the reaction, improving the quality of by-product hydrochloric acid, and shortening the reaction time

Active Publication Date: 2015-12-09
SHANDONG HUAYOU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, glacial acetic acid and phosphorus trichloride are used as raw materials. There is an excessive amount of glacial acetic acid in the production process, and the glacial acetic acid needs to be recovered later, resulting in an excessive volume-to-output ratio and a waste of production capacity.
Using glacial acetic acid, water, and phosphorus trichloride as raw materials, there are severe hydrolysis in the initial stage of the reaction, the reaction is not stable, and it is difficult to control the phenomenon
No matter which method, in the reaction process, in order to reduce the content of phosphorous acid, the method of prolonging the reaction time and allowing acetyl chloride to fully reflux is usually adopted. Due to the low boiling point of acetyl chloride, it is difficult to stay in the reactor for a long time in the later stage, so Make the reaction time too long, acetyl chloride volatilization loss and other disadvantages

Method used

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  • Hydroxyethylenediphosphonic acid production equipment and method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Hydroxyethylene diphosphonic acid production equipment is characterized by: a phosphorus trichloride feed tank 1 connected in parallel, a mixed acid feed tank 2 of hydrochloric acid and acetic acid, a glacial acetic acid or acetyl chloride feed tank 3 is connected with the feed port of the reactor 4 The outlet at the top of the reactor 4 is connected to the fractionation tower 10 one way, and the other way is connected to the receiving tank 6 of acetic acid in the hydrolysis stage through the acetic acid condenser 15. The upper outlet of the fractionating tower 10 is connected to the receiving tank 5 of acetyl chloride, and the top gas outlet is The acid chloride condenser 14 is connected, the acetyl chloride condensed in the condenser is led to the receiving tank 5 of acetyl chloride, the uncondensed gas enters the lower inlet of the hydrogen chloride gas scrubber 11, and the bottom of the hydrogen chloride gas scrubber 11 is connected to the acetic acid-hydrochloric acid...

Embodiment 2

[0040] Add 40Kg of industrial glacial acetic acid, 100Kg of recovered washing liquid containing 35.7% of acetic acid and 21.4% of hydrogen chloride into the reactor 4, start stirring, and slowly add 165Kg of phosphorus trichloride. Other operations are the same as in Example 1. In the reaction, 32Kg of acetyl chloride is recovered, and after hydrolysis, a 50% product of 230Kg, 85% acetic acid 27.6Kg, and a dilute acetic acid-hydrochloric acid mixture: 77Kg, 30% hydrochloric acid 391Kg.

Embodiment 3

[0042] Add 48Kg of recovered 91% acetic acid, 91Kg of recovered washing liquid containing 35.7% of acetic acid and 21.4% of hydrogen chloride into the reactor 4, start stirring, and slowly add 165Kg of phosphorus trichloride. Other operations were the same as in Example 1. 31 Kg of acetyl chloride was collected and hydrolyzed with water to obtain 228 Kg of 50% HEDP product, 28 Kg of 85% acetic acid solution, and 82 Kg of acetic acid-hydrochloric acid mixture.

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Abstract

The invention discloses a method for producing etidronic acid, relating to an improved technology of the production process of a water treatment agent, namely, etidronic acid and belonging to the technical field of chemical engineering. According to the method, hydrogen chloride is introduced into the raw materials for reaction, so that water dissolution heat for hydrogen chloride is reduced in the hydrolysis process of phosphorus trichloride, furthermore, the hydrolysis intensity of the phosphorus trichloride is inhibited, the reaction can be carried out stably, and side reactions of hydrolysis of acetylchloride also can be reduced. The method has the beneficial effects that the reaction can be carried out smoothly at the beginning, side reactions are reduced, and the production is relatively high; in middle stage, the reaction of phosphorous acid can be accelerated, so that the reaction time can be shortened obviously, the recycled acetylchloride and acetic acid and a cleaning solution can be reused, and the quality of byproduct hydrochloric acid is improved.

Description

Technical field [0001] The invention relates to equipment and a method used in the production process of a water treatment agent-hydroxyethylene diphosphonic acid, belonging to chemical equipment and a method. Background technique [0002] Hydroxyethylene diphosphonic acid (HEDP) is currently widely used water treatment agent, mainly used in industrial circulating water as scale and corrosion inhibitor, electroplating metal complexing agent, detergent auxiliaries and photographic printing and dyeing auxiliaries. [0003] At present, industrial production methods generally use glacial acetic acid and phosphorus trichloride as raw materials, or take glacial acetic acid, phosphorus trichloride and water as raw materials, and use stepwise heating and hydrolysis to produce hydroxyethylene diphosphonic acid. Among them, glacial acetic acid and phosphorus trichloride are used as raw materials, and there is an excessive amount of glacial acetic acid during the production process, and the g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38B01D53/18
Inventor 段丽菊高乾善苑爱梅纪文华要晓丽
Owner SHANDONG HUAYOU CHEM
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