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Method for producing etidronic acid

A technology of hydroxyethylene diphosphonic acid and production method is applied in the field of process improvement of the production process of water treatment agent-hydroxyethylene diphosphonic acid, and can solve the problems of severe hydrolysis, unstable reaction, difficult control and the like, Achieve stable reaction, reduce side reactions, and reduce production costs

Active Publication Date: 2014-02-12
SHANDONG HUAYOU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the phenomenon that glacial acetic acid, water, and phosphorus trichloride are used as raw materials in the prior art, there are severe hydrolysis in the initial stage of the reaction, unsteady reaction, and difficult control

Method used

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  • Method for producing etidronic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0030] 1): Add 75Kg of industrial glacial acetic acid and 62Kg of 31% industrial hydrochloric acid into the reaction kettle. The configuration of the reaction kettle is shown in the figure, start stirring, pass cooling water through the interlayer of the reaction kettle, slowly add 165Kg of phosphorus trichloride, control the addition speed, and maintain the internal temperature Not higher than 45°C. The hydrogen chloride gas produced by the reaction enters the multi-stage absorption tank for absorption after being cooled in series and washing towers.

[0031] 2): After adding phosphorus trichloride, stir and heat up to 45-60°C.

[0032] 3): Keep the acetyl chloride in a state of total reflux, and stir and react at 60-75°C for 3 hours.

[0033] 4): Raise the temperature to 70°C and then add 36Kg of excess acetyl chloride through the feeding tank to maintain a high reflux ratio state.

[0034] 5): Stir and react at 65-80°C for 3 hours, and distill off excess acetyl chloride t...

Embodiment 2

[0041] Add 40Kg of industrial glacial acetic acid, 100Kg of recovered washing solution containing 35.7% acetic acid and 21.4% hydrogen chloride into the reaction kettle, start stirring, and slowly add 165Kg of phosphorus trichloride. Other operation is the same as embodiment 1, reclaims acetyl chloride 32Kg in the reaction, obtains 50% product 230Kg after hydrolysis, 85% acetic acid 27.6Kg, dilute acetic acid-hydrochloric acid mixture: 77Kg, 30% hydrochloric acid 391Kg. Example 3

Embodiment 3

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

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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 a water treatment agent-the process improvement of the production process of hydroxyethylene diphosphonic acid, which belongs to the technical field of chemical industry. Background technique [0002] Hydroxyethylidene diphosphonic acid (HEDP) is a widely used water treatment agent, mainly used in scale and corrosion inhibitors for industrial circulating water, metal complexing agents for electroplating, detergent aids, and photographic printing and dyeing aids. [0003] The current industrial production method generally adopts glacial acetic acid and phosphorus trichloride as raw materials, or adopts glacial acetic acid, phosphorus trichloride and water as raw materials, and adopts step-by-step heating method and hydrolysis method to produce hydroxyethylene diphosphonic acid. Among them, glacial acetic acid and phosphorus trichloride are used as raw materials. There is an excess of glacial acetic acid in the production process...

Claims

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Application Information

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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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