CN109626331A - The recycling separation method of iodine in a kind of Cefepime waste liquid - Google Patents
The recycling separation method of iodine in a kind of Cefepime waste liquid Download PDFInfo
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- CN109626331A CN109626331A CN201811395550.2A CN201811395550A CN109626331A CN 109626331 A CN109626331 A CN 109626331A CN 201811395550 A CN201811395550 A CN 201811395550A CN 109626331 A CN109626331 A CN 109626331A
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- C01B7/00—Halogens; Halogen acids
- C01B7/13—Iodine; Hydrogen iodide
- C01B7/14—Iodine
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Abstract
The present invention settles sth. according to policy or law the recovery method of iodine in cephalosporins medicine waste liquid a kind of, include the following steps: to add alkali extraction and separation to go out methanol, acetone and lye cephalosporins medicine waste liquid, the hydrolysis of lye circulating-heating, acidification slot acidification is transferred to after filtering, stratification removes organic matter not soluble in water, and aqueous phase oxidation reaction tower is by I later‑It is oxidized to IO3 ‑, then be passed through IO in reduction kettle3 ‑It is reduced to I2, elemental iodine is precipitated, thick iodine is recovered by filtration to obtain, continues to heat, distil, elemental iodine of sublimating to obtain.This method recycles noble metal iodine in waste liquid, iodine is set to exist in solution with free state by alkaline hydrolysis, acidification, and decomposite organic matter not soluble in water, this method is not necessarily to strict control oxidizer, safety easy to operate, the rate of recovery of iodine is set to reach 98.5% or more, suitable process amplification production.
Description
Technical field
The present invention relates to a kind of recycling separation methods of iodine in Cefepime waste liquid.
Background technique
The spore rhzomorph drug-Cefepime of a new generation is mainly used for urethral infection, skin sense caused by sensitive bacteria infection
Dye, abdominal infection, gynecological infection and septicemia etc., Cefepime as forth generation cephalosporin compared with the third generation,
Antibacterial action has a deeper development, the antibiotic property of balance and has good antibacterial activity to negative bacillus, these are special
Point makes it the drug for the antibacterial properties that clinical medicine in the future is more widely accepted.
At present most of China production cephalosporins medicine waste liquid does not recycle iodine, in Cefepime waste liquid iodine from
Son derives from trimethyl silicane iodine alkane, and 3 substitution intermediates of production Cefepime need excessive Iodotrimethylsilane just in industry
Iodide reaction can be made complete, with anion ion-exchange reactions occurs for iodide ion again in compound later, so that used in reaction
Iodine in whole trimethyl silicane iodine alkane is all present in cephalosporins medicine waste liquid in the form of iodide ion, but generated due to reaction
Hydroiodic acid is deposited in the solution, and hydriodate is formed in conjunction with cephalosporin compound, and the recycling for causing iodine is difficult.Due to iodine
Simple substance is precious metal, and this phenomenon causes the waste of iodine, therefore the recycling of iodine is extremely urgent.The iodine of devil liquor recovery containing iodine is mainly
Using oxidizing process, reduction method, ion-exchange, air blowout method, floatation, active carbon adsorption, extractive distillation method and liquid film
The methods of method is recycled the iodine in waste liquid containing iodine in the form of thick iodine.
Summary of the invention
The present invention provides a kind of recycling separation method of iodine in Cefepime waste liquid, which uses oxidation-extraction
Combination is taken-distilled, so that the iodide ion rate of recovery in waste liquid is high, purity is good, and has process route simple, is suitble to extensive
Commercial cultivation.
The recycling separation method of iodine in a kind of Cefepime waste liquid, it is characterised in that: pass through Cefepime waste liquid respectively
It after alkalization hydrolysis and acidification hydrolization, is separated with organic phase, water phase is through peroxidating, extraction, and elemental iodine is dissolved in organic phase, through depressurizing
Cooling sublimate of distillation recycles elemental iodine comprising the steps of:
(1) waste liquid that Cefepime generates will be produced and is passed through stirred autoclave, added alkali stirring extraction, isolate methanol and third
The mixed solvent layer and lye layer of ketone, lye circulation enter back into reaction kettle, and heating hydrolysis, stratification removes not soluble in water
Organic matter is acidified with acid later, continues heating stirring hydrolysis, then isolate the organic matter of generation.
(2) water phase is passed through in oxidation-extraction tower, being first added oxidizing is elemental iodine, and extractant extraction is added later
It takes to the purplish red decoloration of aqueous solution, stratification merges organic phase;The exhaust gas that oxidation reaction generates is passed through sodium hydroxide solution and returns
Receipts processing;
(3) organic phase is passed through in distillation still, and vacuum distillation removes 70%~80% extractant, the recyclable circulation benefit of extractant
With;
(4) slow heating makes iodine distillation be iodine vapor under the conditions of distillation still vacuum tightness, and the iodine that cools is sublimated crystallization, time
Receive iodine.
In further preferred step (1), alkali is 20%~30% sodium hydroxide or potassium hydroxide solution, adjust pH value 12~
13,90~120 DEG C of hydrolysis temperature are heated, acidification pH value is 0.5~2, is stirred to react 1~3h.
In further preferred step (2), oxidant is sodium nitrite, and Cefepime waste liquid is with oxidant volume mass ratio
1L:8.6~22.5g, 10~30min of oxidation time;Extractant is methylene chloride or ether;Extractant is sprayed using tower top
Mode is injected in tower, and each dosage of extractant is 1~2 times of waste liquid dosage;The naoh concentration for handling tail gas is 20%
~30%.
In further preferred step (3), 12~18 DEG C of vacuum distillation temperature, pressure is controlled in 0.08-0.15MPa.
In further preferred step (4), temperature programming to 30 DEG C, 10~15 minutes heat up 1 DEG C under vacuum condition.
20%~30% sodium hydroxide or potassium hydroxide solution is added in step (1) Cefepime waste liquid, by destroying drug
Component separates methanol and acetone from waste liquid, and remaining lye heating hydrolysis separates the organic matter generated from lye, it
Acidification heating afterwards is further separated out organic matter, separates by stratification water phase with organic phase, the iodine generated in reaction in this way
It is all enriched with and is in water phase in the form of iodine anion.
Step (2) iodide ion selects sodium nitrite by being oxidized to elemental iodine, oxidant, with recycling iodine in the prior art
Method is compared, and sodium nitrite does not have peroxidization, and other techniques are using hydrogen peroxide, sodium hypochlorite, postassium hypochlorite, five oxidations
The oxidants such as two vanadium are easy I-It is oxidized to IO3 -, reduce the rate of recovery of iodine, so needing strict control oxidant in reaction
Dosage, and sodium nitrite does not have peroxidization, be easy to use, while emission-control equipment is additionally added in process device figure,
The nitric oxide generated in reaction is avoided to pollute the environment.Since elemental iodine easily distils, in order to avoid the distillation of iodine wastes,
In technique by oxidation process in conjunction with extraction process, since elemental iodine slightly soluble enters water, extractant is sprayed by oxidation-extraction top of tower
Into coming into full contact with dissolution with iodine, avoid causing for loss, and the solvent selection good dichloro of low boiling point, dissolubility
Methane and ether, vacuum distillation temperature is low, avoids the distillation of iodine, while facilitating the separation and recycling of extractant.
Step (3) will be passed through in vacuum distillation kettle dissolved with the organic solvent of iodine and steam most of extractant, and vacuum heating is adopted
With the slow temperature control of program, guarantee that elemental iodine all becomes iodine vapor, sublimate ensures to obtain high-purity elemental iodine later.Device process
Neutral and alkali hydrolysis and the public reactor tank of acidic hydrolysis, distillation-distillation-condensation process share a vacuum distillation tank, device
Simply, cost is saved.
The present invention has the beneficial effect that:
(1) the technical issues of the invention patent is solved recycles iodide ion in Cefepime waste liquid, passes through knot
Closing alkalization hydrolysis and acidification hydrolization processing separates iodide ion with organic matter, and iodide ion is enriched in water phase, facilitates point of elemental iodine
A reactor tank is shared from recycling, and in the hydrolysis of device process neutral and alkali and acidic hydrolysis.
(2) the elemental iodine high income for recycling iodine, obtaining is distilled-sublimates by oxidation-extraction-, purity is good, distillation-distillation-
Condensation process shares a vacuum distillation kettle, and device is simple, saves cost;Oxidation-extraction combines so that technique improves iodine
Extraction yield, entrainment impurity it is few.
(3) oxidant uses sodium nitrite, without the dosage of strict control oxidant, avoids I in reaction-Peroxidating occurs
Phenomenon generates IO3 -, this process is easy to operate, and the rate of recovery of iodine is high, purity is good, is suitble to large-scale production.
Detailed description of the invention
Fig. 1 is process equipment flow chart of the invention;
In Fig. 1: 1- stirred autoclave;2- alkali liquid tank;3- acid solution tank;4- solvent tank;5- lye fluid reservoir;6- fluid reservoir;
7- heat exchanger;8- transfering material pump;9- oxidation-extraction tower;10- extractant holding vessel;11- water phase recycling can;12- condenser pipe;13- extraction
Take agent recycling can;14- iodine recycles storage tank;15- is evaporated under reduced pressure kettle;16- waste residue reserve tank;17- waste gas treating tank;18- air blower.
Specific embodiment
In order to deepen the understanding of the present invention, the invention will be further described with reference to the accompanying drawings and examples, but not
Constitute limiting the scope of the present invention.
Fig. 1 is process equipment flow chart of the invention, as described in Figure 1, iodine in a kind of Cefepime waste liquid of the present invention
Recycling separation method, Cefepime waste liquid initially enter pretreatment 1- stirred autoclave be added lye after, stirring, stand point
Layer, isolates methanol, acetone and lye, recycles lye later, is recycled into the heating hydrolysis of 1- stirred autoclave, separates insoluble
Object, acidification hydrolization destroys drug component and isolates water phase and organic phase again later, and water phase continues to be passed through 9- oxidation-extraction tower, generates
Exhaust gas enter the recovery processing of 17- waste gas treating tank through tower top, air blower is passed through air, water phase oxygen into 17- waste gas treating tank
Extractant extraction is added after change, separates organic phase, organic phase enters 15- and is evaporated under reduced pressure kettle after merging, heating uses water-bath
Heating, decompression steam 70%~80% extractant, and extractant is by cooling recycling, remaining a small amount of extractant and iodine
Simple substance makes iodine distil in the case where being evaporated under reduced pressure kettle vacuum tightness state, and being passed through condensed water cooling later makes iodine vapor sublimate, and recycles iodine
Simple substance.
Embodiment 1
3L Cefepime waste liquid is added in stirred autoclave, lye is 20% sodium hydroxide, adjusts pH=12 and separates alkali
Agitating and heating hydrolyzes after liquid, 90 DEG C of heating temperature, after separating organic phase, adds 36% hydrochloric acid and adjusts pH=0.5, continue to heat
3h is hydrolyzed, water phase is recycled, it is cooling, it is passed through oxidation-extraction tower, sodium nitrite 25.8g carries out oxidation reaction 10min, and tower top sprays later
Entering methylene chloride, is extracted to purplish red decoloration in water phase, organic phase, which flows into, is evaporated under reduced pressure kettle, pressure 0.15MPa, and 12 DEG C of temperature,
Most of extractant methylene chloride is steamed to recycle, remaining ingredient continue under vacuum conditions heated sealed to 30 DEG C, every 10
Minute rises 1 DEG C, and elemental iodine distillation, distillation still cools later, and iodine is sublimated to obtain sterling, the rate of recovery 98.9%, the content of iodine
99%.
Embodiment 2
4L Cefepime waste liquid is added in stirred autoclave, lye is 20% potassium hydroxide, adjusts pH=13 and separates alkali
Agitating and heating hydrolyzes after liquid, 120 DEG C of heating temperature, after separating organic phase, adds 36% hydrochloric acid and adjusts pH=2, continue to heat
3h is hydrolyzed, water phase is recycled, it is cooling, it is passed through oxidation-extraction tower, sodium nitrite 90g carries out oxidation reaction 20min, and tower top sprays into later
Ether is extracted to purplish red decoloration in water phase, and organic phase flows into vacuum distillation kettle, and pressure 0.08MPa, is steamed big by 18 DEG C of temperature
Partial extraction agent ether recycles, and remaining ingredient continues heated sealed under vacuum conditions and rises 1 DEG C within every 15 minutes to 30 DEG C,
Elemental iodine distillation, distillation still cools later, and iodine is sublimated to obtain sterling, the rate of recovery 98.7%, the content 98% of iodine.
Embodiment 3
1L Cefepime waste liquid is added in stirred autoclave, lye is 30% sodium hydroxide, adjusts pH=13 and separates alkali
Agitating and heating hydrolyzes after liquid, 120 DEG C of heating temperature, after separating organic phase, adds 36% hydrochloric acid and adjusts pH=1.5, continue to add
Pyrohydrolysis 2h recycles water phase, cooling, is passed through oxidation-extraction tower, and sodium nitrite 20g carries out oxidation reaction 30min, and tower top sprays later
Enter methylene chloride, be extracted to purplish red decoloration in water phase, organic phase flows into vacuum distillation kettle, and pressure 0.1MPa, steams by 15 DEG C of temperature
Most of extractant methylene chloride recycles out, and heated sealed is to 30 DEG C under vacuum conditions for remaining ingredient continuation, and every 15 points
Clock rises 1 DEG C, and elemental iodine distillation, distillation still cools later, and iodine is sublimated to obtain sterling, the rate of recovery 98.8%, the content 99% of iodine.
Comparative example 1
2L Cefepime waste liquid is added in stirred autoclave, lye is 30% potassium hydroxide, adjusts pH=12 and separates alkali
Agitating and heating hydrolyzes after liquid, 90 DEG C of heating temperature, after separating organic phase, adds 36% hydrochloric acid and adjusts pH=2, continue to heat water
3h is solved, water phase is recycled, it is cooling, it is passed through oxidation-extraction tower, 30% hydrogen peroxide 20g carries out oxidation reaction 10min, and tower top sprays into later
Ether is extracted to purplish red decoloration in water phase, and organic phase flows into vacuum distillation kettle, and pressure 0.12MPa, is steamed big by 14 DEG C of temperature
Partial extraction agent ether recycles, and remaining ingredient continues heated sealed under vacuum conditions and rises 1 DEG C of iodine within every 10 minutes to 30 DEG C
Simple substance distillation, distillation still cools later, and iodine is sublimated to obtain sterling, the rate of recovery 84.6%.
Comparative example 2
3L Cefepime waste liquid is added in stirred autoclave, lye is 20% sodium hydroxide, adjusts pH=13 and separates alkali
Agitating and heating hydrolyzes after liquid, 110 DEG C of heating temperature, after separating organic phase, adds 36% hydrochloric acid and adjusts pH=4, continue to heat
1h is hydrolyzed, water phase is recycled, it is cooling, it is passed through oxidation-extraction tower, 10% sodium hypochlorite 30g carries out oxidation reaction 20min, later tower top
Ether is sprayed into, purplish red decoloration in water phase is extracted to, organic phase flows into vacuum distillation kettle, and pressure 0.09MPa, steams by 16 DEG C of temperature
Most of extractant ether recycles out, and remaining ingredient continues heated sealed under vacuum conditions and rises 1 within every 15 minutes to 30 DEG C
The distillation of DEG C elemental iodine, distillation still cools later, and iodine is sublimated to obtain sterling, the rate of recovery 81.9%.
Comparative example 3
1L Cefepime waste liquid is added in stirred autoclave, lye is 30% sodium hydroxide, adjusts pH=13 and separates alkali
Agitating and heating hydrolyzes after liquid, 120 DEG C of heating temperature, after separating organic phase, adds 36% hydrochloric acid and adjusts pH=1, continue to heat
2h is hydrolyzed, water phase is recycled, it is cooling, it is passed through oxidation-extraction tower, sodium nitrite 20g carries out oxidation reaction 10min, and tower top sprays into later
Methylene chloride is extracted to purplish red decoloration in water phase, and organic phase flows into vacuum distillation kettle, and pressure 0.1MPa, is steamed by 15 DEG C of temperature
Most of extractant methylene chloride recycles, and heated sealed is to 30 DEG C under vacuum conditions for remaining ingredient continuation, and every 15 minutes
5 DEG C are risen, elemental iodine distillation, distillation still cools later, and iodine is sublimated to obtain sterling, the rate of recovery 84.6%.
Comparative example 4
4L Cefepime waste liquid is added in stirred autoclave, lye is 30% sodium hydroxide, adjusts pH=13 and separates alkali
Agitating and heating hydrolyzes after liquid, 120 DEG C of heating temperature, after separating organic phase, adds 36% hydrochloric acid and adjusts pH=1.5, continue to add
Pyrohydrolysis 2h recycles water phase, cooling, is passed through oxidation-extraction tower, and sodium nitrite 80g carries out oxidation reaction 30min, and tower top sprays later
Enter methylene chloride, be extracted to purplish red decoloration in water phase, organic phase flows into vacuum distillation kettle, and pressure 0.3MPa, steams by 30 DEG C of temperature
Most of extractant methylene chloride recycles out, and heated sealed is to 30 DEG C under vacuum conditions for remaining ingredient continuation, and every 15 points
Clock rises 3 DEG C, and elemental iodine distillation, distillation still cools later, and iodine is sublimated to obtain sterling, the rate of recovery 84.2%.
Comparative example 5
5L Cefepime waste liquid is added in stirred autoclave, lye is 30% sodium hydroxide, adjusts pH=8 and separates lye
Agitating and heating hydrolyzes afterwards, 120 DEG C of heating temperature, after separating organic phase, adds 36% hydrochloric acid and adjusts pH=1.5, continue to heat
2h is hydrolyzed, water phase is recycled, it is cooling, it is passed through oxidation-extraction tower, sodium nitrite 100g carries out oxidation reaction 30min, and tower top sprays later
Enter methylene chloride, be extracted to purplish red decoloration in water phase, organic phase flows into vacuum distillation kettle, and pressure 0.1MPa, steams by 15 DEG C of temperature
Most of extractant methylene chloride recycles out, and heated sealed is to 30 DEG C under vacuum conditions for remaining ingredient continuation, and every 15 points
Clock rises 1 DEG C, and elemental iodine distillation, distillation still cools later, and iodine is sublimated to obtain sterling, the rate of recovery 81.3%.
Comparative example 6
3L Cefepime waste liquid is added in stirred autoclave, lye is 20% potassium hydroxide, adjusts pH=14 and separates alkali
Agitating and heating hydrolyzes after liquid, 120 DEG C of heating temperature, after separating organic phase, adds 36% hydrochloric acid and adjusts pH=2, continue to heat
3h is hydrolyzed, water phase is recycled, it is cooling, it is passed through oxidation-extraction tower, sodium nitrite 67.5g carries out oxidation reaction 20min, and tower top sprays later
Enter ether, be extracted to purplish red decoloration in water phase, organic phase flows into vacuum distillation kettle, and pressure 0.08MPa, is steamed by 18 DEG C of temperature
Most of extractant ether recycles, and remaining ingredient continues heated sealed under vacuum conditions and rises 1 within every 15 minutes to 30 DEG C
DEG C, elemental iodine distillation, distillation still cools later, and iodine is sublimated to obtain sterling, the rate of recovery 84.5%.
Claims (6)
1. the recovery method of iodine in a kind of cephalosporins medicine waste liquid, it is characterised in that comprise the steps of:
A, cephalosporins medicine waste liquid is passed through in reaction kettle, alkali extraction and separation is added to go out methanol, acetone and water phase, water phase circulation flows again
It returns in reaction kettle and heats, be filtered to remove insoluble impurity after treatment;
B, after water phase enters the acidification of acidification slot, stir process, stratification removes organic matter not soluble in water.
C, water phase is passed through oxidizing tower to react, liquid enters in tower from tower top sprinkling by water phase I-It is oxidized to IO3 -;
D, water phase is passed through reduction kettle later and reducing agent is added by IO3 -It is reduced to I2Purple red precipitate is generated, by filtering, is added
Heat distils, elemental iodine of sublimating to obtain.
2. the recovery method of iodine in cephalosporins medicine waste liquid according to claim 1, it is characterised in that in step a, alkali is
20%~30% sodium hydroxide or potassium hydroxide solution adjust pH value 12~13, heat 90~120 DEG C of hydrolysis temperature.
3. the recovery method of iodine in cephalosporins medicine waste liquid according to claim 1, it is characterised in that in step b, acidification
PH value is 1~5, is stirred to react 1~3h.
4. the recovery method of iodine in cephalosporins medicine waste liquid according to claim 1, it is characterised in that in step c, oxidation
Agent is potassium chlorate or sodium chlorate, and oxidant and cephalosporins medicine waste liquid mass volume ratio are 20~30g:1L.
5. the recovery method of iodine in cephalosporins medicine waste liquid according to claim 1, it is characterised in that in step d, reduction
Agent is sulfur dioxide or sodium hydrogensulfite, and sodium hydrogensulfite and cephalosporins medicine waste liquid mass volume ratio are 50~100g:1L, two
Sulfur oxide and cephalosporins medicine waste liquid mass volume ratio are 25~50g:1L.
6. the recovery method of iodine in cephalosporins medicine waste liquid according to claim 1, it is characterised in that in step d, filtering,
It heats, distil, sublimating and completed in same device, obtaining thick iodine after filtering removal waste liquid, continuing to heat iodine distillation later to be iodine vapor,
It is cooling that it is passed through condensed water again, so that iodine vapor is sublimated to obtain elemental iodine, heating temperature is 50~100 DEG C.
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Cited By (5)
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CN108862199A (en) * | 2018-06-28 | 2018-11-23 | 广东先导稀材股份有限公司 | The method of iodine is recycled in the waste liquid of trimethyl gallium containing iodine |
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 |
CN112194204A (en) * | 2020-09-10 | 2021-01-08 | 昆明铂锐金属材料有限公司 | Preparation method of high-purity rhodium triiodide |
CN114715848A (en) * | 2021-01-04 | 2022-07-08 | 中国科学院江西稀土研究院 | Method for recovering iodine from iodine-containing solution |
CN117654423A (en) * | 2024-02-01 | 2024-03-08 | 中国科学院地球环境研究所 | System and method for extracting iodine in different occurrence forms in sediment |
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CN103508421A (en) * | 2013-10-15 | 2014-01-15 | 四川大学 | Method for recycling iodine from production waste liquid of X-CT series contrast agents |
CN106430105A (en) * | 2016-10-10 | 2017-02-22 | 云南民族大学 | Method for recycling iodine from acetic acid factory iodine-containing waste liquor |
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CN103508421A (en) * | 2013-10-15 | 2014-01-15 | 四川大学 | Method for recycling iodine from production waste liquid of X-CT series contrast agents |
CN106430105A (en) * | 2016-10-10 | 2017-02-22 | 云南民族大学 | Method for recycling iodine from acetic acid factory iodine-containing waste liquor |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108862199A (en) * | 2018-06-28 | 2018-11-23 | 广东先导稀材股份有限公司 | The method of iodine is recycled in the waste liquid of trimethyl gallium containing iodine |
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 |
CN112028020B (en) * | 2020-09-02 | 2021-06-22 | 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 |
CN112194204A (en) * | 2020-09-10 | 2021-01-08 | 昆明铂锐金属材料有限公司 | Preparation method of high-purity rhodium triiodide |
CN114715848A (en) * | 2021-01-04 | 2022-07-08 | 中国科学院江西稀土研究院 | Method for recovering iodine from iodine-containing solution |
CN114715848B (en) * | 2021-01-04 | 2023-09-12 | 中国科学院江西稀土研究院 | Method for recovering iodine from iodine-containing solution |
CN117654423A (en) * | 2024-02-01 | 2024-03-08 | 中国科学院地球环境研究所 | System and method for extracting iodine in different occurrence forms in sediment |
CN117654423B (en) * | 2024-02-01 | 2024-04-26 | 中国科学院地球环境研究所 | System and method for extracting iodine in different occurrence forms in sediment |
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