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
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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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