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Preparation method of hydrogen isotope substituted acid

A hydrogen isotope and acid radical technology, which is applied in the field of hydrogen isotope-substituted acid preparation, can solve the problems of large consumption of hydrogen isotope water raw materials, difficult to completely remove water, difficult separation, etc., and achieves low cost, low consumption and simple operation. Effect

Pending Publication Date: 2022-03-22
SUZHOU SITRI ISOTOPE TECH RES INSITITUTE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hydrogen isotopes (mainly deuterium ( 2 H) and tritium ( 3 H)) Substituted acid is currently mainly prepared by batch method, that is, it is produced in the form of multiple exchanges of heavy water or tritium water. Separation of acid and water, after the separation, add new heavy water or tritium water to the acid for exchange, so it has a long production cycle, and a large amount of heavy water or tritium water with different abundances is produced during the process, resulting in a large consumption of hydrogen isotope water raw materials The problem
And because the separation between acid and water is difficult, it is difficult to completely remove the water in the hydrogen isotope-substituted acid. Therefore, in order to remove the water in the hydrogen-isotope-substituted acid, relatively high energy consumption is required.

Method used

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Examples

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Effect test

preparation example Construction

[0026] A method for preparing a hydrogen isotope-substituted acid, comprising the steps of:

[0027] S1: Fill the H-type sulfonic acid-based cation exchange resin into a cylindrical container to make an ion-exchange column;

[0028] Ion exchange columns are used to prepare hydrogen isotope-substituted acids. If the sulfonic acid-based cation exchange resin is H-type, it can be filled directly. If the sulfonic-acid cation-exchange resin is Na-type or K-type, it needs to be cleaned by acid washing. Na type or K type sulfonic acid group cation exchange resin is converted into H type sulfonic acid group cation exchange resin; In addition in specific preparation, described Na type, K type or H type sulfonic acid group cation exchange resin is aliphatic sulfonic acid group cation exchange resin Acid-based strong acid-type cation exchange resin, or polystyrene sulfonic acid-type ion-exchange resin, and the loading capacity of sulfonic acid groups in Na-type, K-type or H-type sulfonic...

Embodiment 1

[0044] Embodiment one: the acid that needs to be prepared is deuterated hydrochloric acid, and the specific preparation method is as follows:

[0045] S1: Select 500g of Na-type aliphatic sulfonic acid-based strong-acid cation exchange resin, wash it with 5% dilute hydrochloric acid to form a strongly acidic H-type aliphatic sulfonic acid-based strong-acid cation exchange resin, and then pack it into an ion-exchange column, or Firstly, the ion exchange resin is loaded into the exchange column, and then washed with dilute hydrochloric acid to a strongly acidic H-type aliphatic sulfonic acid group strong acid cation exchange resin, in which the Na type aliphatic sulfonic acid group strong acid cation exchange resin The loading capacity is 3mmol / g;

[0046] S2: Take 400g of heavy water, pass it into the ion exchange column three times, and stay for 30min each time to obtain the deuterated sulfonic acid group cation exchange resin;

[0047] S3: Take 58g of high-purity sodium chlo...

Embodiment 2

[0050] Embodiment two: the acid that needs to be prepared is deuterated hydrochloric acid, and the specific preparation method is as follows:

[0051] S1: Choose 800g of Na-type aliphatic sulfonic acid-based strong-acid cation exchange resin, wash it with 5% dilute hydrochloric acid to become strongly acidic H-type aliphatic sulfonic-acid-based strong-acid cation exchange resin, and then pack it into an ion exchange column, or Firstly, the ion exchange resin is loaded into the exchange column, and then washed with dilute hydrochloric acid to a strongly acidic H-type aliphatic sulfonic acid group strong acid cation exchange resin, in which the Na type aliphatic sulfonic acid group strong acid cation exchange resin The loading capacity is 3mmol / g;

[0052] S2: Take 400g of heavy water, pass it into the ion exchange column three times, and stay for 30min each time to obtain the deuterated sulfonic acid group cation exchange resin;

[0053] S3: Dissolve 111g of high-purity calciu...

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Abstract

The invention belongs to the field of preparation of hydrogen isotope substituted acid, and particularly discloses a preparation method of hydrogen isotope substituted acid, which comprises the following steps: filling H-type sulfonic cation exchange resin into a cylindrical container to prepare an ion exchange column; introducing the water containing the hydrogen isotope into an ion exchange column, and carrying out hydrogen isotope and hydrogen exchange on the hydrogen isotope and the H-type sulfonic cation exchange resin in the ion exchange column to obtain the sulfonic cation exchange resin containing the hydrogen isotope; dissolving a metal salt of a corresponding acid radical in water containing hydrogen isotope to prepare a salt solution; and continuously flowing the prepared salt solution through the hydrogen isotope sulfonic cation exchange resin in S2 to obtain a hydrogen isotope substituted acid solution. The solid ion exchange resin is used as a medium, the acid substitution process is mild, the operation is simple, the utilization rate of the hydrogen isotope raw material can be greatly improved, and continuous production can be realized.

Description

technical field [0001] The invention belongs to the technical field of preparation of hydrogen isotope substituted acids, in particular to a preparation method of hydrogen isotope substituted acids. Background technique [0002] Hydrogen isotope substitution acid is an important isotope labeling reagent. Hydrogen and protium in nature ( 1 H), deuterium ( 2 H), tritium ( 3 H) There are three isotope forms, among which deuterated acid reagents are mainly used in nuclear magnetic resonance analysis, which can be used to adjust the pH of the sample solution and prepare deuterium-labeled compounds; while tritiated acid is mainly used to synthesize tritium-labeled substances. Hydrogen isotopes (mainly deuterium ( 2 H) and tritium ( 3 H)) Substituted acid is currently mainly prepared by batch method, that is, it is produced in the form of multiple exchanges of heavy water or tritium water. Separation of acid and water, after the separation, add new heavy water or tritium wate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J47/02B01J47/14B01D59/30
CPCB01J47/02B01J47/14B01D59/30
Inventor 徐志红桂媛陈伟沈佳宇
Owner SUZHOU SITRI ISOTOPE TECH RES INSITITUTE CO LTD
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