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Method for liquid phase catalytic hydrogenation deiodination of iodination X-ray contrast medium

A liquid-phase catalysis and X-ray technology, applied in the direction of protection devices against harmful chemicals, etc., can solve the problems of irreversible leaching, easy agglomeration, catalyst deactivation, etc., and achieve easy degradation, no secondary pollution, and degradation efficiency. high effect

Inactive Publication Date: 2018-08-31
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the inertness of the surface of carbon-based materials and the weak metal-support interaction, noble metal catalysts supported by carbon-based materials are prone to agglomeration and irreversible leaching during the reaction process, resulting in catalyst deactivation.

Method used

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  • Method for liquid phase catalytic hydrogenation deiodination of iodination X-ray contrast medium
  • Method for liquid phase catalytic hydrogenation deiodination of iodination X-ray contrast medium
  • Method for liquid phase catalytic hydrogenation deiodination of iodination X-ray contrast medium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A mesoporous carbon nitride-supported noble metal catalyst was prepared, which included Pd-supported mesoporous carbon nitride Pd / MCN. As a comparison, a mesoporous carbon-supported catalyst Pd / CMK-3 was also prepared. The specific method includes the following steps:

[0038] (1) Synthesis of SBA-15: SBA-15 was synthesized using triblock copolymer P123 as surfactant and tetraethyl orthosilicate (TEOS) as silicon source. Dissolve 4g P123 in 126ml 2mol / l hydrochloric acid, dissolve in a water bath at 40°C, add 20.8gTEOS completely, stir for 24h, then transfer the solution to an autoclave for aging at 80°C for 48h, filter, wash and dry, place in a muffle furnace at 1°C / min to 550°C for 6 hours to remove the P123 organic template.

[0039](2) Synthesis of CMK-3: CMK-3 was synthesized using SBA-15 as a template and sucrose as a carbon source. Dissolve 5g of sucrose in 20ml of deionized water, add 0.56g of concentrated sulfuric acid and 4g of SBA-15, mix well, heat in an ...

Embodiment 2

[0043] The mesoporous carbon nitride supported noble metal catalyst was prepared and characterized according to the method of Example 1.

[0044] Mesoporous carbon nitride (MCN-500) or CMK-3 with a carbonization temperature of 500 °C and Pd salt precursor PdCl 2 Mixing and stirring, and loading by precipitation deposition method to obtain supported Pd / MCN-500 or Pd / CMK-3, wherein the loaded amount of Pd is 2%wt.

[0045] (1) Wide-angle XRD of Pd / CMK-3 and Pd / MCN-500 such as figure 1 As shown, in the wide-angle XRD pattern of Pd / CMK-3, weak diffraction peaks representing the (111) plane and (200) plane of Pd appear at 39.4° and 45.8° respectively, indicating that the noble metal Pd was successfully loaded on the CMK-3 carrier superior. Compared with the XRD pattern of Pd / CMK-3, the corresponding Pd diffraction peaks in the XRD pattern of Pd / MCN-500 are weaker, indicating that the distribution of noble metal Pd on the MCN-500 carrier is more uniform than that of CMK-3.

[004...

Embodiment 3

[0049] The above-prepared Pd / MCN was used as a catalyst to carry out liquid-phase catalytic hydrodeiodination reaction of DTZ and IOP in water. The specific reaction process is as follows: Add an appropriate amount of sodium diatrizoate or iopamidol in a four-necked flask, mix well, add an appropriate amount of the catalyst prepared in Example 1, feed nitrogen and stir vigorously, after a period of equilibrium, nitrogen Switching to hydrogen, the ICM performs a liquid-phase catalytic hydrodeiodination reaction.

[0050] (1) The catalyst is Pd / MCN-500 with a concentration of 0.075g / l, the initial pH of the reaction is 7.0, the hydrogen flow rate is 200ml / min, and the reaction is carried out at normal temperature and pressure for 2 hours. The initial reaction concentration was 0.4 mmol / l for ionic DTZ and 0.7 mmol / l for non-ionic IOP. See Figure 4 : It can be seen from the figure that the Pd / MCN-500 catalyst can complete the hydrodeiodination reaction of DTZ within 70 minutes...

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Abstract

The invention discloses a method for the liquid phase catalytic hydrogenation deiodination reaction of an iodination X-ray contrast medium. The method comprises the steps that a catalyst in the methoduses the porous carbon MCN in the mixed nitrogen as a carrier, the noble metal Pd or Pt is loaded through a precipitation deposition method, and a noble metal catalyst with the MCN loaded is obtained; and the noble metal catalyst with the MCN loaded is added into an aqueous solution containing the iodination X-ray contrast medium, and after nitrogen balancing is carried out, the hydrogen is introduced into the solution for the liquid phase catalytic hydrogenation deiodination reaction. According to the method, the catalyst is used for liquid phase catalytic hydrogenation deiodination of the iodination X-ray contrast medium so that relatively high reaction activity can be realized, the toxicity of the ICM can be effectively removed or reduced, the degradation efficiency is high, and the reaction speed is high.

Description

technical field [0001] The invention relates to a method for treating iodine pollutants, in particular to a method for catalytic hydrodeiodination of iodine X-ray contrast agents. Background technique [0002] Iodine X-ray contrast agent (ICM) is a medical product, which is used for imaging of soft tissues, organs and blood vessels during diagnostic testing through intravenous injection, and is generally excreted with human urine within 24 hours. Compared with other drugs, ICM has higher chemical and biological tolerance and higher water solubility. ICM is very stable in the natural water environment, and it is difficult to remove it in most biological and chemical wastewater treatment processes. Combined with the larger usage, the annual usage is about 3.5×10 6 kg, ICM is often detected in the water environment, and the concentration is increasing year by year. Existing studies have shown that ICM is the source of 90% organic iodine in wastewater and surface water. ICM w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A62D3/34B01J27/24
CPCA62D3/34B01J27/24
Inventor 许昭怡刘慧孙敬雅庄伟毕霁麟郑寿荣李红段倩囡胡媛翁昕
Owner NANJING UNIV
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