CN112079364B - Method for recycling fluorine-and iodine-containing waste material resources - Google Patents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/12—Iodides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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Abstract
The invention relates to a method for recycling fluorine-and iodine-containing waste materials, which comprises the steps of converting organic fluorine into potassium fluoride by using potassium hydroxide, carrying out aerobic incineration at 600-800 ℃ by using a converter, completely burning or completely carbonizing organic matters, and avoiding generating fluorine-containing toxic substances such as hydrofluoric acid, perfluoroisobutylene and the like; the method has the advantages that fluoride ions are removed by using calcium hydroxide, excessive calcium hydroxide is removed by using potassium carbonate, the pH value is adjusted by using formic acid, and potassium formate is converted into potassium iodide by using iodine, so that the potassium iodide is produced without recovering iodine simple substances, the cost is saved, and the utilization rate of iodine is improved. The potassium iodide finished product obtained by the invention has the potassium iodide content of more than 99 percent and the fluorine ion content of less than 1 ppm.
Description
Technical Field
The invention relates to a method for recycling fluorine-and iodine-containing waste materials, in particular to a method for recycling iodine-containing byproduct resources of perfluoroalkyl ethyl (meth) acrylate, which can be directly subjected to a series of treatments to obtain a potassium iodide product with qualified quality, and belongs to the field of waste recycling.
Background
The perfluoroalkyl ethyl (meth) acrylate is the most important and key intermediate for preparing a surfactant with excellent hydrophobic and oleophobic properties, air permeability, washing resistance, stain resistance and easy stain removal, and a fluorine-containing hydrophobic and oleophobic fabric finishing agent with high stability in various environments such as strong acid, strong alkali, high temperature, high radiation and the like, and can be used for industrially recovering iodine by producing a crude potassium iodide product with the byproduct content of 70-85% in the synthesis process, wherein the potassium iodide product contains 15-20% of organic matters and 1-3% of fluorine, the obtained iodine has poor quality, the content of the organic matters in the iodine is high, the iodine contains fluorine ions, the iodide cannot be directly prepared and can be used after being refined, and the residual organic matters are difficult to treat, thereby causing environmental pollution.
The existing potassium iodide purification method is a calcination method, namely, crude potassium iodide is directly added into a rotary kiln or an incinerator for high-temperature incineration, high-boiling-point organic matters in the potassium iodide are decomposed, and then the potassium iodide is dissolved, filtered and recrystallized. The process can generate a large amount of strong corrosive hydrofluoric acid to severely corrode equipment, and meanwhile, because the C-F bond energy is large, fluorine-containing organic matters can be remained in the system, and even highly toxic perfluoroisobutylene can be generated. Resulting in poor safety, high environmental protection pressure and poor product quality.
Patent CN103241747A discloses a method for purifying KI in perfluoroalkyl ethyl acrylate synthesis byproducts, which comprises the steps of adsorbing with an adsorbent, filtering with an ultrafiltration membrane to remove colloid and macromolecular organic matters in the solution, sending the filtrate to a reverse osmosis membrane for filtering, and enriching the micromolecular organic matters and water in the filtrate together, thereby realizing the enrichment of KI. But the ultrafiltration membrane can not remove low molecular weight fluorine-containing organic matters and finally remains in the product, the ultrafiltrate is treated by a reverse osmosis membrane, and fluorine ions in the solution can not be effectively removed, so that the fluorine ions in the product can reach 0.5 percent, the product quality is seriously influenced, the treatment cost is high, impurity ions such as F and the like are difficult to completely remove, and the purity of KI is still difficult to meet the requirement. Especially fluoride ions (in the form of potassium fluoride) are present in the product and cannot be used in food, feed additives and the like.
The patent CN110002470A discloses a method for purifying potassium iodide from a perfluoroalkyl ethyl acrylate byproduct, which comprises the steps of adding the perfluoroalkyl ethyl acrylate byproduct into a stirring kettle, and adding 1-2 times of anhydrous ethanol by weight to obtain a crude potassium iodide mixed solution; and cooling the mixed solution, and carrying out centrifugal filtration to obtain the refined potassium iodide. The method can not effectively remove organic impurities and completely remove fluorine ions, so that the product content is low, the fluorine ions in the product reach 0.5 percent, the product quality is seriously influenced, and particularly, the fluorine ions (in the form of potassium fluoride) exist in the product and can not be used for food, feed additives and the like.
The invention is mainly concerned with how to treat the fluorine and iodine-containing waste material, especially the perfluoroalkyl ethyl (meth) acrylate iodine-containing byproduct into qualified potassium iodide, and the harmless treatment of the residual waste material.
Disclosure of Invention
In view of the above problems, the present invention is directed to: (1) extracting potassium iodide from the waste material, and processing the potassium iodide into qualified potassium iodide; (2) and (4) performing harmless treatment on the residual waste. The invention provides a method for recycling fluorine-and iodine-containing waste materials, which comprises the steps of adding a proper amount of water into a reaction kettle, adding crude potassium iodide, adding a proper amount of potassium hydroxide, slowly heating to reflux, keeping the reflux for 2-4 hours to form paste, burning the paste in a converter at 600-800 ℃ with oxygen, completely burning or completely carbonizing organic matters, cooling the obtained potassium iodide melt to form blocks, dissolving the blocks in water, filtering to remove insoluble substances to obtain a colorless to light yellow solution, measuring the content of fluoride ions, removing the fluoride ions by using 2-5 times of theoretical amount of calcium hydroxide, filtering to remove the generated calcium fluoride to obtain a potassium iodide solution without the fluoride ions, and removing excessive calcium hydroxide by using potassium carbonate with the same mole as the calcium hydroxide. Adjusting the pH of the solution to 6-8 by using formic acid, controlling the temperature to 80-90 ℃, adding iodine for reaction, after the reaction is finished, adjusting the pH to about 8 by using potassium hydroxide solution, decoloring by using proper amount of activated carbon, filtering to obtain filtrate, distilling and concentrating the filtrate, cooling and crystallizing, centrifuging and filtering to obtain a potassium iodide wet product, and drying to obtain a potassium iodide finished product, wherein the content of the potassium iodide finished product is more than 99%, and the content of fluorine ions is less than 1 ppm.
The technical scheme of the invention is as follows:
the invention relates to a method for recycling fluorine-and iodine-containing waste materials, in particular to potassium iodide as a byproduct of perfluoroalkyl ethyl (meth) acrylate, wherein the potassium iodide content is 70-80%, 15-20% of organic matters contain 1-3% of fluorine, and the potassium iodide is subjected to alkali boiling, concentration, high-temperature incineration in a converter to form salt, dissolution, filtration, fluoride ion removal by calcium hydroxide, and removal of excessive calcium hydroxide by potassium carbonate with the same mol as that of the calcium hydroxide. And (3) obtaining a potassium iodide solution without fluoride ions, adjusting the pH of the solution by using formic acid, adding iodine for reaction, adjusting the pH by using a potassium hydroxide solution, decoloring by using proper amount of activated carbon, filtering to obtain a filtrate, distilling and concentrating the filtrate, cooling for crystallization, centrifuging and filtering to obtain a wet potassium iodide product, and drying to obtain a finished potassium iodide product with the content of more than 99% and the fluoride ions of less than 1 ppm.
The more specific technical scheme is as follows:
a method for recycling fluorine-and iodine-containing waste materials comprises the following steps:
(1) adding a proper amount of water into a reaction kettle, adding potassium iodide which is a byproduct of perfluoroalkyl ethyl (meth) acrylate while stirring, and adding a proper amount of potassium hydroxide solution, wherein the solution is strongly alkaline;
(2) slowly heating to reflux, and keeping the reflux for 2-4 hours;
(3) forming into paste;
(4) cooling to below 70 ℃;
(5) using a converter; carrying out aerobic incineration at 600-800 ℃, completely burning out or completely carbonizing organic matters, and cooling and agglomerating the obtained potassium iodide melt to obtain potassium iodide salt blocks;
(6) dissolving potassium iodide salt blocks with water;
(7) filtering to remove insoluble substances to obtain colorless to light yellow solution;
(8) measuring the content of fluoride ions, and removing the fluoride ions by using 2-5 times of theoretical amount of calcium hydroxide;
(9) filtering and removing the generated calcium fluoride to obtain a potassium iodide solution without fluoride ions, adding potassium carbonate with the same mole as that of calcium hydroxide into the solution, stirring for 30-60 minutes, and filtering to obtain a potassium iodide solution without fluoride ions and calcium ions;
(10) adjusting the pH value of the potassium iodide solution obtained in the step (9) to 6-8 by using formic acid;
(11) controlling the temperature to be 80-90 ℃ and adding iodine for reaction;
(12) after the reaction is finished, regulating the pH value to about 8 by using a potassium hydroxide solution, decoloring by using a proper amount of activated carbon, and filtering to obtain a filtrate; adjusting the pH value to 8, wherein potassium hydroxide is slightly excessive, potassium iodide is filtered out by distillation, concentration, temperature reduction and condensation, and a trace amount of potassium hydroxide is left in the mother liquor, so that the separation is realized; HI can be completely removed by adjusting the pH to 7.0, and the pH value of the product can be qualified by adjusting the pH to 8.0.
(13) Distilling and concentrating the filtrate;
(14) cooling and crystallizing;
(15) centrifuging and filtering to obtain a wet potassium iodide product;
(16) drying to obtain potassium iodide product with content over 99% and fluorion less than 1 ppm.
The step 2 comprises the main reaction: R-F + KOH ═ KF + R-OH
Step 8, the main reaction F-+Ca2+＝CaF2↓Ca2++CO3 2-＝CaCO3↓
The 10 th step mainly comprises the following reaction: KOH + HCOOH ═ HCOOK + H2O
The main reaction in the 11 th step: HCOOK + I2＝KI+HI+CO2↑
The main reaction in the 12 th step: HI + KOH ═ KI + H2O
The invention has the beneficial effects that:
(1) converting organic fluorine into potassium fluoride by adding potassium hydroxide, and carrying out aerobic incineration at 600-800 ℃ by using a converter to thoroughly burn out or thoroughly carbonize organic matters without generating fluorine-containing toxic substances such as hydrofluoric acid, perfluoroisobutylene and the like;
(2) removing various impurity ions step by step, firstly removing fluoride ions by using calcium hydroxide, and then removing excessive calcium hydroxide by using potassium carbonate; regulating the pH value with formic acid; converting the potassium formate into potassium iodide by using iodine, thereby realizing the purification of the potassium iodide and obtaining qualified potassium iodide;
(3) through the impurity removal design utilizing various impurity ions, qualified potassium iodide can be directly extracted from the waste, the recovery of iodine simple substances is not needed to reproduce the potassium iodide, the cost is saved, and the utilization rate of iodine is improved.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. Further, it should be understood that various changes and modifications can be made by those skilled in the art after reading the teaching of the present invention, and those equivalents also fall within the scope of the appended claims of the present application.
The fluorine-containing and iodine-containing waste materials used in the embodiment of the invention are all prepared from perfluoroalkyl ethyl (meth) acrylate iodine-containing byproducts, wherein the content of potassium iodide is 70-80%, 15-20% of organic matters are contained, and 1-3% of fluorine is contained.
Example 1:
(1) adding a proper amount of water into a reaction kettle, adding a proper amount of potassium iodide which is a byproduct of perfluoroalkyl ethyl (meth) acrylate under stirring, adding a proper amount of potassium hydroxide solution, and adjusting the pH to 12;
(2) slowly heating to reflux, and keeping reflux for 2 hours;
(3) concentrating into paste;
(4) cooling to 70 ℃;
(5) using a converter; carrying out aerobic incineration at 800 ℃, completely burning out or completely carbonizing organic matters, and cooling and agglomerating the obtained potassium iodide melt to obtain potassium iodide salt blocks;
(6) dissolving potassium iodide salt blocks with water;
(7) filtering to remove insoluble substances to obtain colorless to light yellow solution;
(8) measuring the content of fluoride ions, and removing the fluoride ions by using 2-5 times of theoretical amount of calcium hydroxide;
(9) filtering and removing the generated calcium fluoride to obtain a potassium iodide solution without fluoride ions, adding potassium carbonate with the same mole as that of calcium hydroxide into the solution, stirring for 30-60 minutes, and filtering to obtain a potassium iodide solution without fluoride ions and calcium ions; (ii) a
(10) Adjusting the pH value of the potassium iodide solution obtained in the step (9) with formic acid to 8;
(11) controlling the temperature to be 90 ℃ and adding iodine for reaction;
(12) after the reaction is finished, regulating the pH value to about 8 by using a potassium hydroxide solution, decoloring by using a proper amount of activated carbon, and filtering to obtain a filtrate;
(13) distilling and concentrating the filtrate;
(14) cooling and crystallizing;
(15) centrifuging and filtering to obtain a wet potassium iodide product;
(16) drying to obtain potassium iodide product with potassium iodide content of 99.1% and fluorion content of 0.9 ppm.
Example 2:
(1) adding a proper amount of water into a reaction kettle, and adding potassium iodide which is a byproduct of perfluoroalkyl ethyl (meth) acrylate under stirring; adding a proper amount of potassium hydroxide solution, and adjusting the pH value to 12;
(2) slowly heating to reflux, and keeping reflux for 4 hours;
(3) concentrating into paste;
(4) cooling to 60 ℃;
(5) using a converter; carrying out aerobic incineration at 800 ℃, completely burning out or completely carbonizing organic matters, and cooling and agglomerating the obtained potassium iodide melt to obtain potassium iodide salt blocks;
(6) dissolving potassium iodide salt blocks with water;
(7) filtering to remove insoluble substances to obtain colorless to light yellow solution;
(8) measuring the content of fluoride ions, and removing the fluoride ions by using 2-5 times of theoretical amount of calcium hydroxide;
(9) filtering and removing the generated calcium fluoride to obtain a potassium iodide solution without fluoride ions, adding potassium carbonate with the same mole as that of calcium hydroxide into the solution, stirring for 30-60 minutes, and filtering to obtain a potassium iodide solution without fluoride ions and calcium ions; (ii) a
(10) Adjusting the pH value of the potassium iodide solution obtained in the step (9) with formic acid to 6;
(11) controlling the temperature to be 80 ℃ and adding iodine for reaction;
(12) after the reaction is finished, regulating the pH value to about 8 by using a potassium hydroxide solution, decoloring by using a proper amount of activated carbon, and filtering to obtain a filtrate;
(13) distilling and concentrating the filtrate;
(14) cooling and crystallizing;
(15) centrifuging and filtering to obtain a wet potassium iodide product;
(16) drying to obtain potassium iodide product with potassium iodide content of 99.5% and fluorion content of 0.5 ppm.
Example 3:
(1) adding a proper amount of water into a reaction kettle, adding potassium iodide which is a byproduct of perfluoroalkyl ethyl (meth) acrylate while stirring, adding a proper amount of potassium hydroxide solution, and adjusting the pH to 11;
(2) slowly heating to reflux, and keeping reflux for 3 hours;
(3) concentrating into paste;
(4) cooling to 65 ℃;
(5) using a converter; carrying out aerobic incineration at 600 ℃, completely burning out or completely carbonizing organic matters, and cooling and agglomerating the obtained potassium iodide melt to obtain potassium iodide salt blocks;
(6) dissolving potassium iodide salt blocks with water;
(7) filtering to remove insoluble substances to obtain colorless to light yellow solution;
(8) measuring the content of fluoride ions, and removing the fluoride ions by using 2-5 times of theoretical amount of calcium hydroxide;
(9) filtering and removing the generated calcium fluoride to obtain a potassium iodide solution without fluoride ions, adding potassium carbonate with the same mole as that of calcium hydroxide into the solution, stirring for 30-60 minutes, and filtering to obtain a potassium iodide solution without fluoride ions and calcium ions; (ii) a
(10) Adjusting the pH value of the potassium iodide solution obtained in the step (9) with formic acid to 6;
(11) controlling the temperature to be 85 ℃, and adding iodine for reaction;
(12) after the reaction is finished, regulating the pH value to about 8 by using a potassium hydroxide solution, decoloring by using a proper amount of activated carbon, and filtering to obtain a filtrate;
(13) distilling and concentrating the filtrate;
(14) cooling and crystallizing;
(15) centrifuging and filtering to obtain a wet potassium iodide product;
(16) drying to obtain potassium iodide product with potassium iodide content of 99.3% and fluoric ion content of 0.9 ppm.
Example 4:
(1) adding a proper amount of water into a reaction kettle, adding potassium iodide which is a byproduct of perfluoroalkyl ethyl (meth) acrylate while stirring, adding a proper amount of potassium hydroxide solution, and adjusting the pH to 9;
(2) slowly heating to reflux, and keeping reflux for 4 hours;
(3) concentrating into paste;
(4) cooling to 70 ℃;
(5) using a converter; carrying out aerobic incineration at 800 ℃, completely burning out or completely carbonizing organic matters, and cooling and agglomerating the obtained potassium iodide melt to obtain potassium iodide salt blocks;
(6) dissolving potassium iodide salt blocks with water;
(7) filtering to remove insoluble substances to obtain colorless to light yellow solution;
(8) measuring the content of fluoride ions, and removing the fluoride ions by using 2-5 times of theoretical amount of calcium hydroxide;
(9) filtering and removing the generated calcium fluoride to obtain a potassium iodide solution without fluoride ions, adding potassium carbonate with the same mole as that of calcium hydroxide into the solution, stirring for 30-60 minutes, and filtering to obtain a potassium iodide solution without fluoride ions and calcium ions; (ii) a
(10) Adjusting the pH value of the potassium iodide solution obtained in the step (9) to 7.5 by using formic acid;
(11) controlling the temperature to be 90 ℃ and adding iodine for reaction;
(12) after the reaction is finished, regulating the pH value to about 8 by using a potassium hydroxide solution, decoloring by using a proper amount of activated carbon, and filtering to obtain a filtrate;
(13) distilling and concentrating the filtrate;
(14) cooling and crystallizing;
(15) centrifuging and filtering to obtain a wet potassium iodide product;
(16) drying to obtain potassium iodide product with content over 99.2% and fluoride ion content of 1 ppm.
The materials treated by the method are not only limited to the byproduct potassium iodide of perfluoroalkyl ethyl (meth) acrylate, but also comprise iodine-containing materials with similar components, and belong to the protection scope of the patent.
Claims (6)
1. A method for recycling fluorine-and iodine-containing waste materials comprises the following steps:
(1) adding a proper amount of water into a reaction kettle, adding potassium iodide which is a byproduct of perfluoroalkyl ethyl (meth) acrylate while stirring, and adding a proper amount of potassium hydroxide solution, wherein the solution is strongly alkaline;
(2) slowly heating to reflux, and keeping the reflux for 2-4 hours;
(3) forming into paste;
(4) cooling to below 70 ℃;
(5) carrying out aerobic incineration at 600-800 ℃ by using a converter, completely burning out or completely carbonizing organic matters, and cooling and agglomerating the obtained potassium iodide melt to obtain potassium iodide salt blocks;
(6) dissolving potassium iodide salt blocks with water;
(7) filtering;
(8) adding calcium hydroxide to remove fluoride ions;
(9) filtering and removing the generated calcium fluoride to obtain a potassium iodide solution without fluoride ions, adding potassium carbonate with the same mole as that of calcium hydroxide into the solution, stirring for 30-60 minutes, and filtering to obtain a potassium iodide solution without fluoride ions and calcium ions;
(10) adjusting the pH value of the potassium iodide solution obtained in the step (9) to 6-8 by using formic acid;
(11) controlling the temperature to be 80-90 ℃ and adding iodine for reaction;
(12) after the reaction is finished, adjusting the pH value to 8 by using a potassium hydroxide solution, and filtering to obtain a filtrate;
(13) distilling and concentrating the filtrate;
(14) cooling and crystallizing;
(15) centrifuging and filtering to obtain a wet potassium iodide product;
(16) drying to obtain the potassium iodide finished product.
2. The method of claim 1, wherein: insoluble matter is removed by filtration in step (7), and a colorless to pale yellow solution is obtained.
3. The method of claim 1, wherein: in the step (8), the content of fluoride ions is measured, 2-5 times of theoretical amount of calcium hydroxide is used for removing fluoride ions, and excessive calcium hydroxide is removed by using potassium carbonate which is equimolar with calcium hydroxide.
4. The method of claim 1, wherein: in the step (12), a proper amount of activated carbon is used for decoloring.
5. The method of claim 1, wherein: and (3) the potassium iodide finished product obtained in the step (16) has the potassium iodide content of over 99 percent and the fluorine ion content of less than 1 ppm.
6. The method of claim 1, wherein: the byproduct potassium iodide of the perfluoroalkyl ethyl (meth) acrylate contains 70-80% of potassium iodide, 15-20% of organic matters and 1-3% of fluorine.
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| US12275661B2 (en) | 2024-07-12 | 2025-04-15 | Claros Technologies Inc. | Methods and systems of iodine capture from aqueous solutions |
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| CN112557142B (en) * | 2020-12-24 | 2024-05-31 | 广州博诺通技术股份有限公司 | Sample pretreatment method, halogen content detection method and application |
| CN113526528A (en) * | 2021-07-16 | 2021-10-22 | 自贡鸿鹤制药有限责任公司 | Preparation method of medicinal potassium iodide |
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