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Method for recovering iodine from perfluoroalkylethyl acrylate synthesis byproduct

A technology of perfluoroalkyl ethyl acrylate and by-products, applied in the field of KI purification, can solve the problems of long production cycle, legacy and high production cost, and achieve the effect of cost reduction

Active Publication Date: 2014-12-03
SICHUAN XIAIFU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] The above method adds other chemical substances, such as phosphoric acid, etc., which inevitably has the disadvantage that it will be left in the elemental iodine. At the same time, there are many chemical reactions in this method, resulting in long production cycles and high production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] According to the requirements of the synthesis process, 100Kg of iodine pentafluoride, 280Kg of tetrafluoroethylene, and 150Kg of elemental iodine were added to the pentafluoroiodoethane reaction kettle. After the reaction is over, the reactant is recovered through the gas phase, and washed through an alkali washing tower to recover elemental iodine and a small amount of iodine pentafluoride that did not participate in the reaction. The gas recovery time is 60 minutes, and the alkali flow rate of the alkali washing tower is 15m 3 / h, the lye is recycled.

[0062] Take the perfluoroalkyl ethyl acrylate synthesis reaction by-product KI crude product, dissolve it in hot deionized water equivalent to 2.5 times the weight of the KI crude product, and add an adsorbent equivalent to 0.10 times the weight of the KI crude product at 65 ° C, The adsorbent is a mixture of activated carbon and activated clay mixed in a weight ratio of 1:5. After 70 minutes of adsorption, filter a...

Embodiment 2

[0067] According to the requirements of the synthesis process, 100Kg of iodine pentafluoride, 280Kg of tetrafluoroethylene, and 150Kg of elemental iodine were added to the pentafluoroiodoethane reaction kettle. After the reaction is over, the reactant is recovered through the gas phase, and washed through an alkali washing tower to recover elemental iodine and a small amount of iodine pentafluoride that did not participate in the reaction. The gas recovery time is 40 minutes, and the alkali flow rate of the alkali washing tower is 20m 3 / h, the lye is recycled.

[0068] Take the perfluoroalkyl ethyl acrylate synthesis reaction by-product KI crude product, dissolve it in hot deionized water equivalent to 5 times the weight of the KI crude product, and add an adsorbent equivalent to 0.16 times the weight of the KI crude product at 80°C, The adsorbent is a mixture of activated carbon and activated clay mixed in a weight ratio of 3:20. After 120 minutes of adsorption, filter and...

Embodiment 3

[0073] According to the requirements of the synthesis process, 100Kg of iodine pentafluoride, 280Kg of tetrafluoroethylene, and 150Kg of elemental iodine were added to the pentafluoroiodoethane reaction kettle. After the reaction is over, the reactant is recovered through the gas phase, and washed through an alkali washing tower to recover elemental iodine and a small amount of iodine pentafluoride that did not participate in the reaction. The gas recovery time is 40 minutes, and the alkali flow rate of the alkali washing tower is 5m 3 / h, the lye is recycled.

[0074] Take the perfluoroalkyl ethyl acrylate synthesis reaction by-product KI crude product, dissolve it in hot deionized water equivalent to 1.4 times the weight of the KI crude product, and add an adsorbent equivalent to 0.01 times the weight of the KI crude product at 50°C, The adsorbent is a mixture of activated carbon and activated clay in a weight ratio of 1:8. After 20 minutes of adsorption, filter and collec...

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Abstract

The invention provides a method for recovering iodine from a perfluoroalkylethyl acrylate synthesis byproduct. The method comprises the following steps: dissolving crude KI which is the perfluoroalkylethyl acrylate synthesis byproduct in 1.4-5 parts of hot deionized water, adsorbing by using an adsorbent, and filtering through using an ultrafilter membrane to remove colloids and macromolecular organic matters in the obtained solution; sending the obtained filtrate to a reverse osmosis membrane, and filtering to enrich micro-molecular organic matters in the filtrate and water together in order to realize KI enrichment; sending the obtained KI-rich solution to a vacuum concentration kettle, carrying out distillation concentration, letting in chlorine, and reacting at a certain temperature under a certain pressure to directly obtain solid iodine; and fusing the solid iodine, sending to a fusion granulator, and granulating to obtain high-purity iodine. In the invention, the recovery rate and the purity of iodine reach about 95% and above 99% respectively, and the synthetic cost of perfluoroalkylethyl acrylate can be reduced by 60%.

Description

technical field [0001] The invention relates to a method for purifying KI, in particular to a method for recovering iodine from by-products of perfluoroalkyl ethyl acrylate synthesis. Background technique [0002] As an important fluorine-containing surfactant and fabric finishing agent, perfluoroalkyl ethyl acrylate has a wide range of applications. The industrialized device uses iodine, iodine pentafluoride and tetrafluoroethylene as raw materials to synthesize polyfluoroalkyl iodide, and then reacts with ethylene to generate perfluoroalkyl ethyl iodide, and then reacts with potassium acrylate to generate perfluoroalkyl ethyl iodide. Acrylates and KI by-products. [0003] Iodine itself does not make it into the final product, but without iodine the entire reaction cannot proceed. Among all raw materials for the synthesis of perfluoroalkyl ethyl acrylate, the price of iodine is the most expensive. If the circulation of iodine can be realized, the production cost can be re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B7/14
Inventor 胡有荣张金刚李瑞涛陈千友
Owner SICHUAN XIAIFU TECH
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