Method for recovering iodine in production waste liquid of X-CT series contrast media

A recovery method and contrast agent technology, applied to chemical instruments and methods, iodine, iodine/hydrogen iodide, etc., to achieve the effects of simple operation, low cost, and avoiding waste

Active Publication Date: 2009-10-14
山西新天源药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] This shows that above-mentioned various iodine recovery techniques are all only suitable for processing the iodine-containing waste liquid that exists in a single form, and are not suitable for processing strong acidity (pH=0.3~1

Method used

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  • Method for recovering iodine in production waste liquid of X-CT series contrast media

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Experimental program
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Effect test

Embodiment 1

[0033] Get the black production waste liquid 300mL (with I + Calculated, containing iodine 3.5%) in the normal pressure reflux device, directly heated and digested and refluxed for 1.0h, cooled to room temperature in a water bath, collected the iodine element attached to the wall of the condensation tube, and the yield was about 31.3%. Control the temperature of the solution in the reactor at 0°C, and add 3.5g Na in batches under stirring. 2 SO 3 , determined the end point of the reduction reaction by the potentiometric monitoring method, allowed to stand for 20 minutes, filtered, and collected the solid iodine element, and the yield was about 40.4%. Put the filtrate back into the reactor, slowly add 6 mL of 30% H 2 o 2 , the end point of the oxidation reaction was determined by the potentiometric monitoring method, and granular solids were precipitated, and filtered after standing for 20 minutes to collect solid iodine, with a yield of about 12.1%. Put the filtrate back i...

Embodiment 2

[0035] Get the production waste liquid of 300mLX-CT series contrast agent iodination reaction (black, with I + Calculated, containing iodine 3.2%) in the normal pressure reflux device, direct heating, cooking and reflux treatment for 1.0h, cooling to room temperature in a water bath, collecting iodine simple substance attached to the wall of the condensation tube, the yield is about 30.2%. Use the waste liquid after the above treatment as catholyte, lead plate as cathode, externally connect salt bridge, water as anolyte, lead dioxide as anode, control cathode current density 5mA / cm 2 , electroreduction treatment under stirring for 1 h, standing and filtering, and collecting solid iodine simple substance, the yield is about 39.7%. Then use the filtrate as the anolyte, lead dioxide as the anode, externally connect the salt bridge, water as the catholyte, lead plate as the cathode, and control the anode current density to 10mA / cm 2 , electrooxidized for 30 minutes under stirring...

Embodiment 3

[0037] Get the production waste liquid of 400mLX-CT series contrast agent iodination reaction (black, with I + Calculated, containing iodine 3.9%) in the normal pressure reflux device, directly heated and digested and refluxed for 1.5h, cooled to room temperature in a water bath, collected the iodine element attached to the wall of the condensation tube, and the yield was about 32.7%. Control the temperature of the solution in the reactor at -10°C, add 3.3g NaHSO in batches under stirring 3 , determined the end point of the reduction reaction by the potentiometric monitoring method, allowed to stand for 30 minutes, filtered, and collected the solid iodine element, and the yield was about 38.4%. The filtrate was put back into the reactor, and 8 mL of 30% H was slowly added dropwise under stirring. 2 o 2 , determined the end point of the oxidation reaction by the potentiometric monitoring method, precipitated granular solids, filtered after standing for 30 minutes, and collect...

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Abstract

The invention relates to a method for recovering iodine in production waste liquid of X-CT series contrast media. The method comprises the following steps: stewing and refluxing the waste liquid first to recover most of dissociated elementary substance iodine, reducing most of high hypervalent iodine into elementary substance iodine for precipitation; conducting filtration and separation, oxidizing the filtrate to oxidize most of iodine negative ions into elementary substance iodine for precipitation, conducting filtration and separation; and finally conducting active carbon absorption and sublimation and crystallization on filtrate to recover the low-concentration dissociated elementary substance iodine completely. The method for recovering iodine is suitable for treating the iodine-containing waste liquid that has strong acidity, high iodine content and multiple existing forms of iodine, and not only solves the problem that the discharge of iodine-containing waste liquid pollutes environment in the production process of X-CT series contrast media, but also realizes the recovery of iodine as well as the cyclic utilization of production waste liquid.

Description

technical field [0001] The invention relates to a method for recovering iodine, in particular to a method for recovering iodine in waste liquid from production of iodine-containing X-CT series contrast agents. Background technique [0002] X-CT series of contrast agents such as iohexol, iopamidol, ioversol, iodixanol, etc. are a new type of contrast agent with high efficiency and the most widely used. Its structure is as follows: [0003] [0004] In the production process of X-CT series contrast media, iodination reaction is the main decision step that affects the production cost of contrast media and produces polluting waste liquid. (mainly I - , I 2 , I + and other forms) for recycling. [0005] At present, the recovery methods about iodine mainly include: [0006] 1) Oxidation method: iodine ion is oxidized into free iodine by oxidant or electro-oxidation method, and then separated. Commonly used oxidants include hypochlorite, chlorate, ferric salt, nitrite, and...

Claims

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Application Information

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IPC IPC(8): C01B7/14C02F9/10C02F1/04C02F1/28C02F1/70C02F1/72
Inventor 苏斌林陈万成高志伟褚丕明苏蔚康福堂
Owner 山西新天源药业有限公司
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