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Method for recycling fluorine-containing and iodine-containing waste resources

A waste and resource technology, applied in the field of resource recycling of iodine-containing by-products of perfluoroalkylethyl acrylate, can solve the problems of low product content, affecting product quality, and inability to effectively remove organic impurities, so as to save costs and improve utilization rate effect

Active Publication Date: 2020-12-15
山东博苑医药化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method cannot effectively remove organic impurities, and cannot completely remove fluoride ions, resulting in low product content. The fluoride ions in the product reach 0.5%, which seriously affects product quality, especially in the form of fluoride ions (as potassium fluoride). For food, feed additives, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Add an appropriate amount of water to the reaction kettle, add an appropriate amount of potassium iodide by-product of perfluoroalkylethyl (meth)acrylate under stirring, add an appropriate amount of potassium hydroxide solution, and adjust the pH to 12;

[0041] (2) slowly warming up to reflux, keep reflux for 2 hours;

[0042] (3) concentrated into paste;

[0043] (4) cooling down to 70°C;

[0044] (5) use a converter; incinerate with oxygen at 800 ° C, the organic matter is thoroughly burned or completely carbonized, and the obtained potassium iodide melt is cooled and agglomerated to obtain potassium iodide salt block;

[0045] (6) Potassium iodide salt block is dissolved in water;

[0046] (7) Remove insolubles by filtration to obtain a colorless to pale yellow solution;

[0047] (8) Measure the fluoride ion content, and remove the fluoride ion with 2 to 5 times the theoretical amount of calcium hydroxide;

[0048](9) Remove the generated calcium fluoride by...

Embodiment 2

[0057] (1) Add an appropriate amount of water to the reactor, and add potassium iodide (meth)acrylic acid by-product potassium iodide under stirring; add an appropriate amount of potassium hydroxide solution, and adjust the pH to 12;

[0058] (2) slowly warming up to reflux, keep reflux for 4 hours;

[0059] (3) concentrated into paste;

[0060] (4) cooling down to 60°C;

[0061] (5) use a converter; incinerate with oxygen at 800 ° C, the organic matter is thoroughly burned or completely carbonized, and the obtained potassium iodide melt is cooled and agglomerated to obtain potassium iodide salt block;

[0062] (6) Potassium iodide salt block is dissolved in water;

[0063] (7) Remove insolubles by filtration to obtain a colorless to pale yellow solution;

[0064] (8) Measure the fluoride ion content, and remove the fluoride ion with 2 to 5 times the theoretical amount of calcium hydroxide;

[0065] (9) Remove the generated calcium fluoride by filtration to obtain a potass...

Embodiment 3

[0074] (1) Add an appropriate amount of water to the reaction kettle, add potassium iodide by-product of perfluoroalkylethyl (meth)acrylate under stirring, add an appropriate amount of potassium hydroxide solution, and adjust the pH to 11;

[0075] (2) slowly warming up to reflux, keep reflux for 3 hours;

[0076] (3) concentrated into paste;

[0077] (4) cooling down to 65°C;

[0078] (5) use a converter; incinerate with oxygen at 600 ° C, the organic matter is thoroughly burned or completely carbonized, and the obtained potassium iodide melt is cooled and agglomerated to obtain potassium iodide salt block;

[0079] (6) Potassium iodide salt block is dissolved in water;

[0080] (7) Remove insolubles by filtration to obtain a colorless to pale yellow solution;

[0081] (8) Measure the fluoride ion content, and remove the fluoride ion with 2 to 5 times the theoretical amount of calcium hydroxide;

[0082] (9) Remove the generated calcium fluoride by filtration to obtain a ...

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PUM

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Abstract

The invention relates to a method for recycling fluorine-containing and iodine-containing waste resources. The method comprises the following steps: converting organic fluorine into potassium fluorideby using potassium hydroxide, and performing aerobic incineration at a temperature of 600-800 DEG C by using a converter to completely burn out or carbonize organic matters without generating fluorine-containing toxic substances such as hydrofluoric acid, perfluoroisobutylene and the like; removing fluorine ions by using calcium hydroxide, removing excessive calcium hydroxide by using potassium carbonate, adjusting the pH value by using formic acid, and converting potassium formate into potassium iodide by using iodine. Therefore, elemental iodine does not need to be recovered to reproduce potassium iodide, the cost is saved, and the utilization rate of iodine is increased. According to the potassium iodide finished product, the content of potassium iodide is 99% or above, and fluorine ions are smaller than 1 ppm.

Description

technical field [0001] The present invention relates to a method for recycling waste resources containing fluorine and iodine, especially a method for recycling resources of iodine-containing by-products of perfluoroalkylethyl (meth)acrylate, which can directly carry out a series of treatments to obtain quality qualified The potassium iodide product belongs to the field of waste recycling. Background technique [0002] (Meth)perfluoroalkylethyl acrylate is a surfactant with excellent water and oil repellency, air permeability and washability, antifouling and easy decontamination, and can be used in strong acid, strong alkali, high temperature and high radiation The most important and most critical intermediate of the fluorine-containing hydrophobic and oleophobic fabric finishing agent with high stability in various environments. During the synthesis process, the crude product potassium iodide with a content of 70-85% will be produced by-product. Potassium iodide contains 1...

Claims

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Application Information

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IPC IPC(8): C01D3/12C01D3/14
CPCC01D3/12C01D3/14
Inventor 刘会军刘亚琪邢晓宇周丽娜于国清
Owner 山东博苑医药化学股份有限公司
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