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Recovery method of iodine in x-ct series contrast agent production wastewater

A technology for producing wastewater and a recovery method, which is applied in the directions of iodine, iodine/hydrogen iodide, etc., can solve the problems of many equipments, high production cost, high energy consumption and production cost, and achieves wide application range, easy operation, and recovery rate. high effect

Active Publication Date: 2018-02-06
ZHEJIANG HAIZHOU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The method currently disclosed in the patent CN103508421 is the method of recovering iodine from X-CT contrast agent production waste liquid, which converts organic iodine into inorganic iodine, and then concentrates it. The concentrated solution is oxidized by a composite oxidant to separate out the elemental iodine, and then extracts the residual elemental substance with organic matter. Iodine has high production cost, is not easy to operate, and a large amount of organic iodine cannot be recovered
[0016] In the method disclosed in the patent CN101554994 at present, the X-CT series contrast agent production waste liquid is subjected to cooking and reflux treatment to recover most of the free elemental iodine (I) in the waste liquid. 2 ); followed by reduction treatment, most of the hypervalent iodine (I + etc.) to be reduced to the form of elemental iodine and separate out by filtration; the filtrate is oxidized again to remove most of the iodide anion (I - ) is oxidized into the form of elemental iodine and separated by filtration again; finally, the filtrate is treated with activated carbon adsorption and sublimation crystallization to completely remove the low-concentration free elemental iodine in the filtrate. Although this method can completely recover the iodine in the waste water, the operation Many steps require more equipment and higher energy consumption, which is not conducive to industrial recycling
[0017] It can be seen that the above-mentioned various iodine recovery technologies are either suitable for treating iodine-containing waste liquid in a single form, or the process is complicated, and the energy consumption and production cost are high. Therefore, it is economical, easy to operate, high in yield and low in cost. It is necessary to effectively recover the iodine in the X-CT series contrast agent production wastewater and reduce the COD in the wastewater

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  • Recovery method of iodine in x-ct series contrast agent production wastewater

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Effect test

Embodiment 1

[0036] Take 3 tons of production waste liquid from the iodination reaction of X-CT series contrast agents, containing 0.6% iodine (mass percentage content, the same as other examples), COD content 40000mg / L, adjust pH=2 with sulfuric acid discarded in the production process , adding composite oxidant C / Fe 2+ 9kg (obtained by mixing 2kg of activated carbon and 7kg of ferrous sulfate), stir, and heat to 50°C, keep stirring for 1 hour, pump it into the separation tower, adjust the flow rate of the feed pump to 10L / h and slowly add hydrogen peroxide. Start the ultrasonic generating device, the purple smoke formed by the iodine element is collected and introduced into the bottom of the absorption tower through the pipeline, start the reductant absorption liquid circulation pump, and circulate the convective absorption of the iodine element, observe that the separation tower and the absorption tower change from purple to colorless, then stop Ultrasonic generating device and reductan...

Embodiment 2

[0039] Take 5 tons of production waste liquid from iodination reaction of X-CT series contrast agent, containing 1.5% iodine, COD content 60000mg / L, adjust pH=2 with hydrochloric acid discarded in the production process, add composite oxidant C / Fe 2+ 15kg (obtained by mixing 3kg of activated carbon and 12kg of ferrous chloride), stir, heat to 80°C, heat and stir for 20 minutes, pump it into the separation tower, adjust the flow rate of the feed pump to 15L / h and slowly add hydrogen peroxide. Start the ultrasonic generating device, the purple smoke formed by the iodine element is collected and introduced into the bottom of the absorption tower through the pipeline, start the reductant absorption liquid circulation pump, and circulate the convective absorption of the iodine element, observe that the separation tower and the absorption tower change from purple to colorless, then stop Ultrasonic generating device and reductant absorption liquid circulation pump pump the reductant a...

Embodiment 3

[0042] Take 5 tons of production waste liquid from iodination reaction of X-CT series contrast agent, containing 1.2% iodine, COD content 54000mg / L, adjust pH=2 with nitric acid discarded in the production process, add composite oxidant Fe / Fe 3+ 15kg (obtained by mixing 3kg of iron powder and 12kg of ferric chloride), heated to 70°C, kept warm and stirred for 50 minutes, pumped into the separation tower, adjusted the flow rate of the feed pump to 20L / h, slowly added hydrogen peroxide, and started at the same time Ultrasonic generating device, the purple smoke formed by simple iodine is collected and introduced into the bottom of the absorption tower through the pipeline, and the reductant absorption liquid circulation pump is started to circulate and convectively absorb simple iodine. After observing the separation tower and absorption tower from purple to colorless, stop the ultrasonic wave The generating device and the reductant absorption liquid circulation pump pump the red...

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Abstract

The invention discloses a recovery method for iodine in X-CT series contrast medium production wastewater. The method comprises the steps that the X-CT series contrast medium production wastewater is acidified with acid first, then a composite oxidant is used for oxidizing organic iodine on an X-CT contrast medium benzene ring into simple iodine substances or negative iodine ions, hydrogen peroxide is continuously dripped into a separation device to oxidize the negative iodine ions into simple iodine substances, ultrasonic waves are used for separating out the simple iodine substances, reducing agent absorption liquid is used for cyclic absorption to reduce the simple iodine substances into negative iodine ions, the reducing agent absorption liquid after cyclic absorption is oxidized with hydrogen peroxide, and filtration and separation are performed to obtain coarse iodine; the acid for acidification is sulfuric acid or hydrochloric acid or nitric acid; the composite oxidant is C / Fe2+ or a Fe / Fe3+ mixture; the reducing agent absorption liquid is a sulfurous acid solution or a sodium bisulfite solution or a sodium sulfite solution. The recovery method has the advantages of environmental friendliness, economy, feasibility, easy and convenient operation, low cost, a high recovery rate, a wide application range and the like.

Description

technical field [0001] The invention relates to a method for recovering iodine, in particular to a method for recovering iodine in waste water produced by X-CT series contrast agents. Background technique [0002] X-CT series contrast agents such as iohexol, iopamidol, ioversol, iodixanol, etc. are a new type of contrast agent with high efficiency and the most widely used, and its structure is shown in formula (I), where R 1 , R 2 , R 3 Different substituents correspond to different intermediates. [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 and organic iodine form) for recovery. [0005] At present, the recovery methods about iodine mainly contain: [0006] 1) Oxidation method: iodide ion is oxidized to free iodine by oxidant or electro-oxidation method, and then separated. Commonly ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B7/14
CPCC01B7/14C01P2006/80
Inventor 石国兴王必伟周晶晶
Owner ZHEJIANG HAIZHOU PHARMA CO LTD