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Desalination and purification method of pentasodium diethylenetriamine pentaacetic acid (DTPA)

A purification method, pentasodium salt technology, which is applied in the field of desalination and purification of DTPA pentasodium salt, can solve the problems of inconvenient production management, blocked pipelines, high salt content, etc., achieve good social and economic benefits, reduce waste water discharge, and reduce environmental pollution.

Active Publication Date: 2014-02-26
YIXING FENGZE CHEM
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] The DTPA industrial production method has following two kinds at present: the first kind of method is the chloroacetic acid method, CN101607921A a kind of preparation method of diethylenetriaminepentaacetic acid, the research of pentasodium diethylenetriaminepentaacetic acid synthetic technique ("Chemical Industry and Engineering Technology" (2008.29. (1). 18-19)), DTPA chelating agent and its manufacture ("Paper and Paper" (2005.3.63-64)), DTPA synthesis process ("Paper Chemicals" (1997.9 ( 4) .7-10)), the synthesis of papermaking chemical DTPA ("China Paper" (1997.5.68-69)) and other documents have introduced this method, using chloroacetic acid, diethylenetriamine and sodium hydroxide or Synthesis of raw materials such as sodium carbonate, the process is relatively simple, but a large amount of by-product sodium chloride will be produced in the production process, which needs to be desalted and purified; in addition, the raw material chloroacetic acid is easy to hydrolyze during the production process, which seriously affects the yield
[0004] The second method is the sodium cyanide method, the research on the synthesis method of DTPA ("Leather Chemical Industry" (2002.19. (5). 26-28)), the synthesis of diethylenetriaminepentaacetic acid ("Chemical Industry and Engineering Technology" ( 2006.27.(6).24-25)) and other documents have introduced this method, using sodium cyanide, formaldehyde and diethylenetriamine and other raw materials to synthesize, the advantages are simple operation, low cost, good product quality, and No by-product sodium chloride is produced in the production process, but this method uses highly toxic cyanide as a raw material, which is not convenient for production management, which makes this method very limited
[0005] At present, the domestic production of DTPA mostly adopts the chloroacetic acid method, but the products prepared by this method contain a large amount of by-product sodium chloride, which leads to the fact that the quality of domestic products has no competitive advantage compared with similar foreign products
In addition, the salt content of the actual product produced by this method is too high, and the salt crystallization will occur during the use of the product, resulting in the accident of clogging the pipeline
The purification and purification of DTPA mentioned in the current literature basically adopts the method of acidification, crystallization and separation of mother liquor, which has large loss and low yield

Method used

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  • Desalination and purification method of pentasodium diethylenetriamine pentaacetic acid (DTPA)
  • Desalination and purification method of pentasodium diethylenetriamine pentaacetic acid (DTPA)
  • Desalination and purification method of pentasodium diethylenetriamine pentaacetic acid (DTPA)

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Experimental program
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Effect test

Embodiment 1

[0058] DTPA pentasodium salt crude product solution preparation:

[0059] Dissolve 240 kg of chloroacetic acid in 80 kg of deionized water, slowly add 52 kg of diethylenetriamine, turn on the cooling device, and put ice water into the jacket to control the temperature of the reaction system at -10~-5°C; then slowly divide into 2 batches Add 630 kg of 32-33% sodium hydroxide solution. When the first 315 kg of sodium hydroxide solution is slowly added, the jacket is passed into ice water to control the reaction temperature at -10~-5°C; when the last 315 kg of sodium hydroxide solution is slowly added, Water is passed into the jacket to control the temperature of the reaction system to be 55-60°C, and the sodium hydroxide solution is added to keep warm for 3 hours; the pH value of the solution is adjusted to 11.5, and the solution is lowered to room temperature, and the material is filtered out. At this time, the content of DTPA pentasodium salt It was 24.8%, and the yield was 99...

Embodiment 2

[0066] DTPA pentasodium salt crude product solution preparation:

[0067] Dissolve 240 kg of chloroacetic acid in 80 kg of deionized water, slowly add 52 kg of diethylenetriamine, turn on the cooling device, put ice water into the jacket to control the temperature of the reaction system at -5 ~ 0 °C; then slowly add in 2 batches 630 kg of 32-33% sodium hydroxide solution. When the first 315 kg of sodium hydroxide solution is slowly added, the jacket is fed with ice water to control the reaction temperature at -5~0°C; when the last 315 kg of sodium hydroxide solution is slowly added, the jacket Feed water to control the temperature of the reaction system to be 45-50°C, and keep warm for 4 hours after adding the sodium hydroxide solution; adjust the pH value of the solution to 11.5, drop to room temperature, and filter the material. At this time, the content of DTPA pentasodium salt is 24.5 %, the yield is 98%.

[0068] Purification of crude product of DTPA pentasodium salt:

...

Embodiment 3

[0074] DTPA pentasodium salt crude product solution preparation:

[0075] Dissolve 240 kg of chloroacetic acid in 80 kg of deionized water, slowly add 52 kg of diethylenetriamine, turn on the cooling device, put ice water into the jacket to control the temperature of the reaction system at 0-5°C; then slowly add 630 Kg of 32-33% sodium hydroxide solution. When the first 315 kg of sodium hydroxide solution is slowly added, the jacket is passed into ice water to control the reaction temperature at 0-5°C; when the last 315 kg of sodium hydroxide solution is slowly added, the jacket is passed into water The temperature of the control reaction system is 50~55 ℃, and the sodium hydroxide solution is added and incubated for 5 hours after the end; the pH value of the solution is adjusted to 11.5, down to room temperature, and filtered to discharge the material. At this time, the content of DTPA pentasodium salt is 24%. The yield was 96%.

[0076] Purification of crude product of DTPA...

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Abstract

The invention discloses a desalination and purification method of pentasodium diethylenetriamine pentaacetic acid (DTPA) and belongs to the field of chemical purification. The purification method comprises the steps of adding deionized water in a crude product pentasodium DTPA solution to obtain a diluent and regulating the pH (potential of Hydrogen) of the diluent to 11-11.5; carrying out desalination separation on the obtained diluent under the pressure of 1-3MPa by adopting a nanofiltration membrane with the molecular weight cut-off of 100-300, thus respectively obtaining a pentasodium DTPA desalination liquid and saline water; and continuously adding the deionized water in the pentasodium DTPA desalination liquid obtained through the separation and carrying out circular desalination separation under the pressure of 1-3MPa by adopting the nanofiltration membrane with the molecular weight cut-off of 100-300 till the salinity of the obtained pentasodium DTPA desalination liquid is below 0.5%. The method for removing the sodium chloride of the pentasodium DTPA has the advantages of high efficiency, rapidness, easiness in control and the like; in addition, by adopting the method, the pentasodium DTPA purifying yield can be up to more than 98%.

Description

technical field [0001] The invention relates to the field of chemical purification, in particular to a method for desalination and purification of DTPA pentasodium salt. Background technique [0002] Diethylenetriaminepentaacetic acid (DTPA) is an important aminocarboxyl complexing agent, and its pentasodium salt is often used in practical applications. It has a particularly strong complexing ability for metal ions, especially high-valence metal ions. The stability and antioxidant capacity of metal ions forming chelates are stronger than those of ethylenediaminetetraacetic acid (EDTA). , Textile, leather and other industries have important applications, and in recent years its application in medical research is also deepening. [0003] The DTPA industrial production method has following two kinds at present: the first kind of method is the chloroacetic acid method, CN101607921A a kind of preparation method of diethylenetriaminepentaacetic acid, the research of pentasodium d...

Claims

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Application Information

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IPC IPC(8): C07C229/16C07C227/40
Inventor 艾飞艾强陈强黄建平
Owner YIXING FENGZE CHEM
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