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Clean technique for producing nitrilotriacetic acid

A technology of nitrilotriacetic acid and trisodium nitrilotriacetate, which is applied in the field of organic chemical synthesis, can solve the problems of rare HCN raw materials, high safety protection requirements, easy condensation, etc., achieve high theoretical and use value, and the raw materials are cheap and non-toxic , The effect of cheap and easy-to-obtain raw materials

Active Publication Date: 2012-08-15
石家庄杰克化工有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

In this method, highly toxic sodium cyanide is used, which is unfavorable for industrial production, and the raw material price of iminodiacetonitrile is relatively high, resulting in high cost
[0007] Hydrocyanic acid method: Mix hydrocyanic acid, formaldehyde, and ammonia water to synthesize NTA in one step. This method involves the highly toxic substance HCN, which requires high safety protection for production equipment sealing and operation. HCN raw materials are rare and easy to condense. It is ready-to-use, high cost, not conducive to industrial production
[0008] Triethanolamine method: In the presence of a catalyst, triethanolamine and alkali are mixed and reacted, and acidified to obtain NTA. This method is carried out at high temperature and high pressure. The safety protection requirements for equipment and operation are high, and the catalyst and raw materials used are more expensive.

Method used

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  • Clean technique for producing nitrilotriacetic acid
  • Clean technique for producing nitrilotriacetic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 637Kg of 15% ammonia water to the reaction tank, inject 2560Kg of 30% sodium hydroxide solution with a pump, turn on the cooling system to cool down to 50°C, then gradually add 2115Kg of 50% hydroxyacetonitrile, and control the temperature of the reaction system at 90°C After that, add ammonia and keep it warm for 6 hours to obtain NTA-3Na feed liquid; cool down to about 60°C and neutralize with sulfuric acid to a pH of about 2.5, cool down to about 50°C, and centrifuge to obtain a product of 1052Kg, with a yield of 97.46% and a content of 99.5 %; the recovery rate of by-product ammonia water in the heat preservation process reaches 80%, which can be used as the raw material of the next batch.

Embodiment 2

[0028] Add 600Kg of 15% ammonia water to the reaction tank, inject 2120Kg of 30% sodium hydroxide solution with a pump, turn on the cooling system to cool down to 10°C after the addition, and then gradually add 1869Kg of 50% hydroxyacetonitrile to control the temperature of the reaction system at 90°C After that, add ammonia and keep it warm for 4 hours to obtain NTA-3Na feed liquid; cool down to about 60°C and neutralize with sulfuric acid to a pH of about 1.0, cool down to about 50°C, and centrifuge to obtain a product of 961Kg with a yield of 94.29% and a content of 99.2 %; The recovery rate of ammonia water by-product in the heat preservation process reaches 92% and can be used as the raw material of the next batch.

Embodiment 3

[0030] Add 800Kg of 10% ammonia water to the reaction tank, inject 2060Kg of 32% sodium hydroxide solution with a pump, turn on the cooling system to cool down to 40°C, and then gradually add 1826Kg of 50% hydroxyacetonitrile to control the temperature of the reaction system at 90°C After that, add ammonia and keep it warm for 1 hour to obtain NTA-3Na feed liquid; cool down to about 60°C and neutralize it with hydrochloric acid to a pH of about 1.5, cool down to about 50°C, and centrifuge to obtain a product of 864Kg, with a yield of 95.8% and a content of 99.8%. ; The recovery rate of the by-product ammonia water in the heat preservation process reaches 94.3%, which can be used as the raw material of the next batch.

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Abstract

The invention relates to a method for producing a chelator nitrilotriacetic acid from conveniently and readily accessible raw materials, belonging to the technical field of organic chemistry synthesis. Ammonia water, sodium hydroxide and hydroxyacetonitrile are utilized as raw materials to synthesize the nitrilotriacetic acid. The method specifically comprises the following steps: gradually and dropwisely adding the hydroxyacetonitrile into the mixed solution of ammonia water and sodium hydroxide; and hydrolyzing under heating conditions to obtain an aqueous solution of sodium nitrilotriacetate. The byproduct ammonia gas is absorbed by a falling film absorption column to prepare ammonia water for cyclic use. The invention has the advantages of accessible raw materials and simple technological process, and the byproduct can be effectively recycled and reutilized.

Description

technical field [0001] The invention relates to a production method of a chelating agent nitrilotriacetic acid using convenient and easily available raw materials, which belongs to the technical field of organic chemical synthesis. The technology has the advantages of readily available raw materials, simple process flow, and effective recycling of by-products. Background technique [0002] Nitrilotriacetic acid (NTA) is a widely used chelating agent product, mainly used in synthetic detergents, chemical plating, and cyanide-free electroplating, scale removers and scale inhibitors, printing and dyeing auxiliaries, plastic additives, industrial desulfurization, chemical Analysis, photographic industry, crop production inhibition and printing ink, rare earth extraction and other industries have a wide range of applications. The research on its synthesis has profound significance. [0003] There are several ways to synthesize NTA, such as: [0004] Chloroacetic acid method: Ch...

Claims

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Application Information

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IPC IPC(8): C07C229/16C07C227/12
Inventor 张辰亮彭艳丽卢冬梅杨扬张朝纯张德路
Owner 石家庄杰克化工有限公司
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