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Method of recovering and purifying iodine

A technology of pure water and potential value, applied in the field of iodine recovery, to achieve the effect of high purity, high refining efficiency and accurate control

Inactive Publication Date: 2014-07-30
山东中氟化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of complex process and high equipment requirements in the above prior art, the present invention provides a simpler method for recovering iodine with higher purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Mix 1000g of crude potassium iodide, a by-product of the production of perfluoroalkyl ethyl acrylate, with 1000g of pure water, stir vigorously, heat up to 95°C and keep it for a certain period of time, then cool down to 70°C, add hydrochloric acid dropwise to adjust the pH value to 3 ~4, the residual polymer in the crude product is precipitated, the above-mentioned material is fully filtered, the filter cake is washed with pure water, and the filtrate is collected for later use;

[0033] 2. Put the filtrate collected above into a container equipped with an ice-water bath for cooling, record the initial temperature and initial solution potential value, then slowly introduce chlorine gas, the solution potential value gradually increases, and when the control potential value rises to 495-515 mv, stop Pass chlorine gas, keep stirring for 30 minutes, the potential value is stable at 495-515mv, the reaction is completed, and the temperature of the reaction process does not...

Embodiment 2

[0047] 1. Mix 1000g of crude potassium iodide, a by-product of perfluoroalkyl alcohol production by solvent method, with 1000g of pure water, stir vigorously, heat up to 95°C and keep it for a certain period of time, then cool down to 70°C, add hydrochloric acid dropwise to adjust the pH value to 3~ 4. The residual polymer in the crude product is precipitated, and the above materials are fully filtered, the filter cake is washed with pure water, and the filtrate is collected for later use;

[0048] 2. Put the liquid collected above into a container equipped with ice-water bath cooling, record the initial temperature and initial solution potential value, then slowly introduce chlorine gas, the solution potential value gradually increases, and when the control potential value rises to 495-515 mv, stop Chlorine gas is passed, and the stirring is continued for 30 minutes, the potential value is stable at 495-515 mv, the reaction is completed, and the temperature of the reaction proce...

Embodiment 3

[0052] 1. Take 2 kg of iodine-containing by-product crude iodine from the oleum synthesis of perfluoroalkyl alcohol and add it to a container cooled by an ice-water bath. Record the initial temperature and initial solution potential value, then slowly feed chlorine gas, and the solution potential value gradually increases. Increase, when the control potential value rises to 495-515 mv, stop the chlorine gas flow, continue to keep stirring for 30 minutes, the potential value is stable at 495-515 mv, the reaction is over, and the reaction process temperature does not exceed 50 °C;

[0053] 2. Filter the reaction product, wash it four times with pure water, filter it with suction, and drain it as much as possible to get 500g of crude iodine;

[0054] 3. Add 500g of crude iodine and 1500g of tetrafluoroethyl ethyl ether into a 2L four-neck flask with mechanical stirring, respectively, and start heating after stirring evenly. Keep the reflux temperature and use a water separator to ...

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PUM

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Abstract

The invention relates to a method of recovering and purifying iodine. The method comprises the following steps: introducing chlorine to a liquid containing iodide ions, wherein the potential value of the solution is gradually increased; controlling the potential value to 495-515mv, and stopping introducing chlorine; continuously maintaining and stirring for 30 minutes; stabilizing the potential value at 495-515mv; finishing reaction, wherein the temperature in the reaction process does not exceed 50 DEG C; washing a filter cake to remove inorganic salts so as to obtain crude iodine; refining the crude iodine to obtain refined iodine. In the method provided by the invention, the reduction end point is judged by the potential value, and the reaction progress is accurately and strictly controlled, so that the method is simpler and more effective, and simple in equipment requirement. The iodine obtained is high in yield, and higher in purity. A fluorine-containing ether solvent is used as a water-carrying agent in the method provided by the invention to refine the crude iodine to effectively remove water in iodine. The method is simple and high in refining efficiency.

Description

technical field [0001] The invention relates to the technical field of iodine recovery, in particular to a method for recovering and purifying iodine. Background technique [0002] Both perfluoroalkyl alcohol and perfluoroalkyl ethyl acrylate are important organic fluorine intermediates, which can be used to synthesize various fluorine-containing surfactants, fabric finishing agents, hydrophobic and oleophobic agents, etc., and play a very important role . [0003] The specific production route is as follows: first, tetrafluoroethylene, iodine, and iodine pentafluoride are used as raw materials to prepare perfluoroalkyl iodide, and then add ethylene to prepare perfluoroalkyl ethyl iodide. Perfluoroalkylethyl iodide is prepared by fuming sulfuric acid method to prepare perfluoroalkylethanol, and the by-product is a mixed solution containing iodide ions and inorganic salts; perfluoroalkylethyl iodide can also be reacted with water and potassium hydroxide by solvent method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/14
Inventor 何日兴张立亭魏菁晶柳飞
Owner 山东中氟化工科技有限公司