CN115676778A - Method for preparing iodine chloride by using iodine waste liquid - Google Patents
Method for preparing iodine chloride by using iodine waste liquid Download PDFInfo
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- CN115676778A CN115676778A CN202211484900.9A CN202211484900A CN115676778A CN 115676778 A CN115676778 A CN 115676778A CN 202211484900 A CN202211484900 A CN 202211484900A CN 115676778 A CN115676778 A CN 115676778A
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Abstract
The invention provides a method for preparing iodine chloride by using iodine waste liquid, which comprises the following steps: s1, adding an acidic substance into the iodine waste liquid to adjust the pH value of the solution; s2, adding an extracting agent into the solution, adding an oxidizing agent into the iodine waste liquid under stirring, and extracting the generated iodine into an organic phase; s3, separating the organic item containing iodine from the aqueous solution; s4, introducing chlorine into the iodine-containing organic item to generate iodine chloride; and S5, distilling the organic extractant in the iodine chloride to obtain a qualified product. The preparation method of the iodine chloride provided by the invention has the advantages of high iodine recovery rate and iodine chloride purity, simple and convenient operation, low cost and suitability for large-scale application.
Description
Technical Field
The invention relates to a treatment method of iodine waste liquid, in particular to a method for preparing iodine chloride by using the iodine waste liquid.
Background
Iodine is a purple-black glossy lamellar crystal, and is easily soluble in organic solvents. Iodine has a low solubility in water. Iodine and compounds are mainly used in medicine, photography and fuel. Iodine chloride is an important chemical raw material, and the preparation of the iodine chloride is generally prepared by reacting an iodine simple substance with chlorine. However, the iodine particles prepared by oxidation from the iodine waste liquid contain moisture and metal impurities, the moisture in the iodine particles can be lost due to iodine sublimation in the drying process, and the metal impurities in the iodine particles are difficult to remove, so that the purity of iodine chloride can be influenced by direct reaction with chlorine. Meanwhile, iodine in the iodine waste liquid is required to be fully utilized for preparing iodine chloride, and the resource utilization efficiency is improved.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing iodine chloride by using iodine waste liquid, aiming at the defects of the prior art, the method is scientific and reasonable, has high practical value, can fully use the iodine waste liquid to obtain valuable iodine chloride, improves economic benefit and reduces resource waste.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a method for preparing iodine chloride by using iodine waste liquid is characterized by comprising the following operation steps:
s1, quantitatively analyzing iodine in the iodine waste liquid, and adding an acidic substance into the iodine waste liquid to adjust the pH value of the iodine waste liquid;
s2, adding an extracting agent and stirring, adding an oxidant during stirring, and further extracting iodine into an organic phase;
s3, separating the organic phase containing iodine from the aqueous solution;
s4, introducing chlorine into the organic phase containing iodine to generate iodine chloride;
s5, distilling the organic extractant in the iodine chloride to obtain a qualified iodine chloride product.
Preferably, the PH of the iodine waste liquid in S1 is adjusted to range from 1 to 5, and the acidic substances used include, but are not limited to, sulfuric acid, nitric acid, and hydrochloric acid.
Preferably, the amount of the oxidant added into the S2 is 1 to 1.5 times of the amount required by oxidation of iodide ions in the iodine waste liquid, and the oxidant used includes, but is not limited to, hydrogen peroxide, oxygen, ozone, chlorine, sodium iodate and potassium iodate.
Preferably, the extractant used in S2 is carbon tetrachloride or hexachloroethane or perfluorohexane or perfluoroheptane, and the mass of the added extractant is 2 to 10 times of the mass of iodine.
Preferably, the amount of chlorine introduced into S4 is 1-1.1 times of that of iodine.
Preferably, iodide ions are oxidized into iodine simple substances in an acidic environment and deposited at the bottom of the solution, the solution is added with an organic extractant, oxidation and extraction are integrated, oxidized iodine can be directly extracted into organic matters, the organic matters and the aqueous solution are immiscible, an organic phase and a water phase can be separated by simple layering, and chlorine is introduced into the organic phase to react with iodine to generate iodine chloride. The iodine chloride and the organic phase can be separated by rectification, and an iodine chloride product with higher purity is obtained.
Compared with the prior art, the invention has the following advantages:
1. the method is simple and reasonable, has high practical value, can reasonably treat the iodine waste liquid and generate valuable iodine chloride, improves the utilization efficiency of raw materials and improves the economic benefit.
2. The invention can remove metal ions in the iodine simple substance by extracting the iodine simple substance through an organic phase, and avoids the metal ions in the iodine simple substance from entering iodine chloride to influence the quality of the iodine chloride because the metal and the ions are almost insoluble in the organic extractant.
3. The invention can easily remove water in the iodine simple substance by extracting the iodine simple substance by an organic phase, otherwise, the iodine loss is generated when the iodine simple substance is dried, and the drying time is longer.
The present invention will be described in further detail with reference to examples.
Detailed Description
Example 1
The embodiment comprises the following operation steps:
s1, quantitatively analyzing the amount of iodide ions in the iodine waste liquid through titration, and adding sulfuric acid into the iodine waste liquid to adjust the pH value of the solution to be 1;
s2, adding carbon tetrachloride into the solution, introducing oxygen into the iodine waste liquid under stirring, wherein the molar weight of the oxygen is 1 time of that of iodide ions, and extracting the generated iodine into the carbon tetrachloride, wherein the mass of the carbon tetrachloride is 10 times of that of the iodine;
s3, separating the carbon tetrachloride containing iodine from the aqueous solution;
s4, introducing chlorine into the iodine-containing carbon tetrachloride, wherein the molar weight of the chlorine is 1.1 times that of the iodine, and generating iodine chloride;
s5, rectifying the organic extractant in the iodine chloride to obtain an iodine chloride product with the purity of 99.92% and metal ion impurities of 3ppm.
Example 2
The embodiment comprises the following operation steps:
s1, quantitatively analyzing the amount of iodide ions in the iodine waste liquid through titration, and adding hydrochloric acid into the iodine waste liquid to adjust the pH value of the solution to be 5;
s2, adding hexachloroethane into the solution, introducing chlorine (with the amount of the introduced chlorine) into the iodine waste liquid under stirring, wherein the molar weight of the chlorine is 1.5 times of the required amount of iodide ions, and extracting the generated iodine into hexachloroethane, wherein the mass of the hexachloroethane is 2 times of that of the iodine;
s3, separating the hexachloroethane containing iodine from the aqueous solution;
s4, introducing chlorine into the iodine-containing hexachloroethane, wherein the molar weight of the chlorine is 1 time of that of the iodine, and generating iodine chloride;
s5, rectifying the organic extractant in the iodine chloride to obtain an iodine chloride product with the purity of 99.95% and metal ion impurities of 2ppm.
Example 3
The embodiment comprises the following operation steps:
s1, quantitatively analyzing the amount of iodide ions in the iodine waste liquid through titration, and adding hydrochloric acid into the iodine waste liquid to adjust the pH value of the solution to be 3;
s2, adding perfluorohexane into the solution, adding sodium iodate into the iodine waste liquid under stirring, wherein the amount of the sodium iodate is 1.3 times of the amount required by iodide ions, and extracting the generated iodine into the perfluorohexane, wherein the mass of the perfluorohexane is 5 times of that of the iodine;
s3, separating the iodine-containing perfluorohexane from the aqueous solution;
s4, introducing chlorine into the iodine-containing perfluorohexane, wherein the molar weight of the chlorine is 1.05 times that of the iodine, and generating iodine chloride;
s5, rectifying the organic extracting agent in the iodine chloride to obtain an iodine chloride product with the purity of 99.97 percent and metal ion impurities of 1ppm.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (5)
1. A method for preparing iodine chloride by using iodine waste liquid is characterized by comprising the following operation steps:
s1, adding an acidic substance into the iodine waste liquid to adjust the pH value of the iodine waste liquid;
s2, adding an extracting agent and stirring, adding an oxidant during stirring, and further extracting iodine into an organic phase;
s3, separating the organic phase containing iodine from the aqueous solution;
s4, introducing chlorine into the iodine-containing organic phase to generate iodine chloride;
s5, distilling the organic extractant in the iodine chloride to obtain a qualified iodine chloride product.
2. The method for preparing iodine chloride from iodine waste liquid according to claim 1, wherein the pH value of the iodine waste liquid in S1 is adjusted to be in a range of 1-5.
3. The method for preparing iodine chloride from the iodine waste liquid as claimed in claim 1, wherein the amount of the oxidant added in S2 is 1-1.5 times of the amount required for oxidizing the iodide ions in the iodine waste liquid.
4. The method for preparing iodine chloride from the iodine waste liquid according to claim 1, wherein the extracting agent used in S2 is carbon tetrachloride or hexachloroethane or perfluorohexane or perfluoroheptane, and the mass of the added extracting agent is 2 to 10 times of the mass of iodine.
5. The method for preparing iodine chloride from iodine waste liquid according to claim 1, wherein the amount of chlorine gas introduced into S4 is 1-1.1 times of that of iodine.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211484900.9A CN115676778A (en) | 2022-11-24 | 2022-11-24 | Method for preparing iodine chloride by using iodine waste liquid |
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| CN202211484900.9A CN115676778A (en) | 2022-11-24 | 2022-11-24 | Method for preparing iodine chloride by using iodine waste liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116924339A (en) * | 2023-07-24 | 2023-10-24 | 山东华氟化工有限责任公司 | Method for recovering iodine from tail liquid of perfluoroalkyl iodide downstream product production |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010215469A (en) * | 2009-03-18 | 2010-09-30 | Daikin Ind Ltd | Method of refining iodine, and method for producing iodine |
| CN103754823A (en) * | 2014-01-08 | 2014-04-30 | 清华大学 | Reaction-extraction coupling method for extracting molecular bromine or iodine |
| CN104961100A (en) * | 2015-07-06 | 2015-10-07 | 哈尔滨工业大学（威海） | Method for extracting iodine from iodine-containing solution |
| JP2016124774A (en) * | 2015-01-07 | 2016-07-11 | 日宝化学株式会社 | Iodine recovery method |
| CN106336342A (en) * | 2016-07-19 | 2017-01-18 | 浙江博瑞电子科技有限公司 | Method for preparing hexafluorobutadiene from iodine and chlorine |
| CN110577191A (en) * | 2019-08-20 | 2019-12-17 | 中船重工（邯郸）派瑞特种气体有限公司 | Method for directly preparing iodine monochloride from iodine-containing salt |
| CN112028020A (en) * | 2020-09-02 | 2020-12-04 | 山东博苑医药化学股份有限公司 | Process for recovering iodine from iodine bromide-containing medical organic waste liquid |
| CN112938901A (en) * | 2021-02-08 | 2021-06-11 | 中船重工（邯郸）派瑞特种气体有限公司 | Method for recovering iodine simple substance from zinc iodide waste salt |
| CN113387329A (en) * | 2021-07-16 | 2021-09-14 | 成都市科隆化学品有限公司 | Low-cost high-efficiency preparation method of iodine monochloride and obtained iodine monochloride |
-
2022
- 2022-11-24 CN CN202211484900.9A patent/CN115676778A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010215469A (en) * | 2009-03-18 | 2010-09-30 | Daikin Ind Ltd | Method of refining iodine, and method for producing iodine |
| CN103754823A (en) * | 2014-01-08 | 2014-04-30 | 清华大学 | Reaction-extraction coupling method for extracting molecular bromine or iodine |
| JP2016124774A (en) * | 2015-01-07 | 2016-07-11 | 日宝化学株式会社 | Iodine recovery method |
| CN104961100A (en) * | 2015-07-06 | 2015-10-07 | 哈尔滨工业大学（威海） | Method for extracting iodine from iodine-containing solution |
| CN106336342A (en) * | 2016-07-19 | 2017-01-18 | 浙江博瑞电子科技有限公司 | Method for preparing hexafluorobutadiene from iodine and chlorine |
| CN110577191A (en) * | 2019-08-20 | 2019-12-17 | 中船重工（邯郸）派瑞特种气体有限公司 | Method for directly preparing iodine monochloride from iodine-containing salt |
| CN112028020A (en) * | 2020-09-02 | 2020-12-04 | 山东博苑医药化学股份有限公司 | Process for recovering iodine from iodine bromide-containing medical organic waste liquid |
| CN112938901A (en) * | 2021-02-08 | 2021-06-11 | 中船重工（邯郸）派瑞特种气体有限公司 | Method for recovering iodine simple substance from zinc iodide waste salt |
| CN113387329A (en) * | 2021-07-16 | 2021-09-14 | 成都市科隆化学品有限公司 | Low-cost high-efficiency preparation method of iodine monochloride and obtained iodine monochloride |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116924339A (en) * | 2023-07-24 | 2023-10-24 | 山东华氟化工有限责任公司 | Method for recovering iodine from tail liquid of perfluoroalkyl iodide downstream product production |
| CN116924339B (en) * | 2023-07-24 | 2024-01-23 | 山东华氟化工有限责任公司 | Method for recovering iodine from tail liquid of perfluoroalkyl iodide downstream product production |
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