Method for recycling iodine from production waste liquid of X-CT series contrast agents

A technology of X-CT and recovery method, applied in the direction of iodine, iodine/hydrogen iodide, etc., can solve the problems of large consumption of oxidant, affecting normal production, and high production cost, achieving low production cost, wide range of use, and low equipment requirements. Effect

Inactive Publication Date: 2014-01-15
SICHUAN UNIV
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  • Description
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  • Application Information

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Problems solved by technology

Therefore, the oxidant consumption is large, and in addition, the use of sodium hypochlorite as the oxidant has high production costs, and hypochlorous acid will cause corrosion to equipment and affect normal production.

Method used

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  • Method for recycling iodine from production waste liquid of X-CT series contrast agents

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Experimental program
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Effect test

Embodiment 1

[0031] Take 500 ml of iohexol production waste liquid in the X-CT series of contrast media (with I + Calculate, containing iodine 15.2 g / L) In the normal pressure reflux device, add NaOH to adjust the pH to 12, and add 0.3 g of zinc powder, heat to boil and reflux for 0.5 hours, and then concentrate to 2 / 3 of the original volume. Cool to room temperature, by adding H 2 SO 4 Adjust the pH to 1.0-3.0, slowly add 10 ml 30% H 2 O 2 , And keep stirring. Allow the reaction for 20 minutes, cool and stand for 20 minutes, filter, and collect 4.8 g of crude iodine. Return the filtrate to the reactor, and slowly add 2 mL saturated FeCl under stirring 3 For the solution, determine the end point of the oxidation reaction by the potential monitoring method, stand for 20 minutes, filter, and collect 2.4 g crude iodine. Then, dichloroethane is used as the extractant to continuously extract the remaining elemental iodine in the waste liquid in multiple stages until the color of the extract liqu...

Embodiment 2

[0033] Take 3 L of iohexol production waste liquid in the X-CT series of contrast media (with I + Calculate, containing 14.6 g / L of iodine) In an atmospheric reactor with reflux device, add NaOH to adjust the pH to 14, and add 3.0 g of zinc powder, heat to boil and reflux for 0.5 hours, and then concentrate to 2 / 3 of the original volume. Cool to room temperature, by adding H 2 SO 4 Adjust the pH to 1.0-3.0, slowly add 25 ml 30% H 2 O 2 , And keep stirring. Allow to react for 30 minutes, cool and stand for 40 minutes, filter, and collect 31.7 g of crude iodine. Return the filtrate to the reactor, and slowly add 10 mL saturated FeCl under stirring 3 Determine the end point of the oxidation reaction of the solution by potential monitoring, let it stand for 20 minutes, filter, and collect 13.9 g of crude iodine. Then, dichloroethane is used as the extractant to continuously extract the remaining elemental iodine in the waste liquid in multiple stages until the color of the extract ...

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Abstract

A method for recycling iodine from production waste liquid of X-CT series contrast agents comprises the following steps: firstly, converting iodine in iodinated organic compounds in organic waste liquid into inorganic iodide; secondly, concentrating, oxidizing the concentrated liquid by using a complex oxidizing agent, oxidizing the iodide anions into elementary iodine, and separating out elementary iodine by filtering; finally, extracting the residual elementary iodine from the filtrate by using an organic solvent so as to completely recycle the low-concentration elementary iodine. The iodine recycling method is applicable to treatment of iodine-containing waste liquid with diverse existing forms of iodine and high iodine content, thus solving the environment pollution problem caused by discharge of the iodine-containing waste liquid in the production process of the X-CT series iodine contrast agents and achieving the recycling of the iodine.

Description

Technical field [0001] The invention relates to a method for recovering iodine-containing organic waste liquid, in particular to a method for recovering iodine in waste liquid from the production of iodine-containing X-CT series contrast media. Background technique [0002] X-CT series of contrast agents, such as iohexol, iopamidol, iodoflurol, iodixanol, iopromide, etc., are a new type of contrast agent with high efficiency and the most widely used. Its structural formula is as follows. Among them, R1, R2, and R3 are different available contrast agents. [0003] [0004] In the production process of X-CT series contrast media, the iodination reaction is the main decision step that affects the production cost of the contrast media and produces polluting waste liquid. Therefore, the iodine in the waste liquid produced by the iodination reaction of X-CT series contrast media must be Recycling. The form of iodine in polluted waste liquid includes inorganic iodine and organic iodine,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/14
Inventor 张坡罗仕忠储伟胡像锋鲁灵江黄亚军倪宏志
Owner SICHUAN UNIV
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