Process for synthesis of hydroxy ethidene diphosphoric acid

A technology of hydroxyethylene diphosphonic acid and synthesis method, which is applied in the field of organic phosphonic acid synthesis, can solve the problems of increased equipment investment and energy consumption, incomplete recovery of by-products, hindered material viscosity and stirring, etc., and saves equipment investment. , beneficial to environmental protection, the effect of large equipment production capacity

Inactive Publication Date: 2006-09-06
傅明珠
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its shortcoming is that it adds operating procedures, which brings unsafe factors; increases equipment investment and energy consumption, and has a long production cycle and low equipment production capacity.
Its disadvantage is that it is not safe to add phosphorus trichloride dropwise under normal pressure and high temperature, and a large amount of acetyl chloride and acetic acid are entrained in the

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 900 kg of acetic acid and 270 kg of water into the reactor, and continuously add 1373 kg of phosphorus trichloride at a temperature of 20°C-100°C and a pressure of less than 760mmHg (absolute). After the addition, the temperature is raised to 120°C-135°C and the reaction is continued for 1-2 hours to generate acetylated hydroxyethylene diphosphonic acid. By-product hydrogen chloride gas and a small amount of uncondensed acetyl chloride continuously enter the combined recovery system of acetic acid and hydrochloric acid. Acetyl chloride is hydrolyzed by water in the acetic acid recovery tower to generate acetic acid which is collected as a raw material. The hydrogen chloride produced by the hydrolysis of acetyl chloride is absorbed by water in the hydrochloric acid recovery tower along with the hydrogen chloride gas from the acetylation reaction system to produce hydrochloric acid as a by-product.

[0028] The intermediate product acetylated hydroxyethylene diphosph...

Embodiment 2

[0030] At a temperature of 50°C-100°C and a pressure of less than 760mmHg (absolute), add 1,373 kg of phosphorus trichloride to 1,800 kg of acetic acid, and then raise the temperature to 120°C-135°C to continue the reaction for 1-2 hours to complete the acetyl group. Hydrogen chloride gas and a small amount of uncondensed acetyl chloride continuously enter the combined recovery system of acetic acid and hydrochloric acid during the reaction process. Acetyl chloride is absorbed and hydrolyzed into acetic acid and hydrogen chloride in the acetic acid recovery tower, and the acetic acid solution is collected as the raw material of the present invention. The hydrolyzed hydrogen chloride and the hydrogen chloride from the acetylation reaction go to the hydrochloric acid recovery tower together, and are absorbed by water to produce hydrochloric acid as a by-product.

[0031] The acetylation reaction product, acetylated hydroxyethylidene diphosphonic acid, is hydrolyzed by 200-400 kg...

Embodiment 3

[0033] According to the method of embodiment 1, phosphorus trichloride 1373 kilograms, acetic acid 1560 kilograms, water 72 kilograms after acetylation and hydrolysis reaction are completed. Reclaim acetic acid, concentrate and crystallize, dissolve with water then, get 1690 kilograms of 60% hydroxyethylidene diphosphonic acid solution product, detect phosphorous acid content through product purity and be 0.08%; Product is 98.42% with phosphorus trichloride calculation yield, Consumption of 299 kg of acetic acid, the yield of the product calculated in terms of acetic acid is 96.13%; the generation cycle is 18-20 hours.

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Abstract

A method for synthesizing hydroxyl ethylidenediphosphonic acid belongs to synthesis of organo-phosphonic acid and is used in water stabilization. The phsophorus trichloride and acetic acid react at a temperature between 80 DEG C and 150 DEG C with an absolute pressure less than 760 millimeters mercury column, and the byproducts of hydrochloride and a few acetyl chlorides free of condensation are respectively retrieved and reused by combined recovery system of acetic acid and hydrochloric acid. The product of this method is obtained by hydrolyzing the acetylated hydroxyl ethylidenediphosphonic acid at a temperature between 80 DEG C and 150 DEG C with an absolute pressure no more than 760 millimeters mercury column; the collected hydrolysate of acetic acid after the distillation and the condensation is selected as raw material together with the acetic acid solution from the reclamation tower of acetic acid. The autoclave of 1000 litres daily produces products of 2500 kilograms with 60 % of solid content and less than 0.15 % of phosphorous acid; the yield rate of the products is more than 98 % calculated by phsophorus trichloride and is more than 96 % calculated by acetic acid.

Description

technical field [0001] The invention relates to a synthesis method of hydroxyethylene diphosphonic acid, which belongs to the synthesis of organic phosphonic acid. The commonly used method is to obtain phosphorus trichloride and acetic acid as raw materials through acetylation and then hydrolysis. Background technique [0002] Hydroxyethylene diphosphonic acid has a stable structure and strong complexing ability. It is mostly used for water quality stabilization treatment. A kind of production method of hydroxyethylene diphosphonic acid is disclosed in CN-1043044C. Its purpose is to collect the acetyl chloride taken out by the by-product hydrogen chloride. Its measure is to add a secondary Frozen brine condenser. The collected acetyl chloride is added to the acetic acid solution and used as part of the raw material acetic acid. Its shortcoming is that it adds operating procedures, which brings unsafe factors; increases equipment investment and energy consumption, and has...

Claims

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Application Information

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IPC IPC(8): C07F9/38
Inventor 傅明珠
Owner 傅明珠
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