CN116555568A - Method for extracting metal ions in strong acid system - Google Patents
Method for extracting metal ions in strong acid system Download PDFInfo
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- CN116555568A CN116555568A CN202310553233.3A CN202310553233A CN116555568A CN 116555568 A CN116555568 A CN 116555568A CN 202310553233 A CN202310553233 A CN 202310553233A CN 116555568 A CN116555568 A CN 116555568A
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- 229910021645 metal ion Inorganic materials 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000002253 acid Substances 0.000 title abstract description 14
- 238000000605 extraction Methods 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 239000013522 chelant Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002927 high level radioactive waste Substances 0.000 claims abstract description 17
- 239000012074 organic phase Substances 0.000 claims abstract description 12
- FTQWRYSLUYAIRQ-UHFFFAOYSA-N n-[(octadecanoylamino)methyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCNC(=O)CCCCCCCCCCCCCCCCC FTQWRYSLUYAIRQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 239000003381 stabilizer Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 22
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 16
- 150000002602 lanthanoids Chemical class 0.000 claims description 16
- 230000002378 acidificating effect Effects 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 230000000274 adsorptive effect Effects 0.000 claims description 8
- 159000000011 group IA salts Chemical group 0.000 claims description 7
- 239000012266 salt solution Substances 0.000 claims description 7
- 229920001817 Agar Polymers 0.000 claims description 5
- 239000008272 agar Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 229920001661 Chitosan Polymers 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- 150000001447 alkali salts Chemical class 0.000 claims 1
- 239000003758 nuclear fuel Substances 0.000 description 10
- VRZYWIAVUGQHKB-UHFFFAOYSA-N 2-[2-(dioctylamino)-2-oxoethoxy]-n,n-dioctylacetamide Chemical compound CCCCCCCCN(CCCCCCCC)C(=O)COCC(=O)N(CCCCCCCC)CCCCCCCC VRZYWIAVUGQHKB-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 4
- 229910052768 actinide Inorganic materials 0.000 description 3
- 150000001255 actinides Chemical class 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- 150000004697 chelate complex Chemical class 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- WHTMDGKHKZCZDV-UHFFFAOYSA-N 2-[2-(dioctylamino)-2-oxoethoxy]-N,N-dioctylpropanamide Chemical compound C(CCCCCCC)N(C(COC(C(=O)N(CCCCCCCC)CCCCCCCC)C)=O)CCCCCCCC WHTMDGKHKZCZDV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/302—Ethers or epoxides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
- G21F9/125—Processing by absorption; by adsorption; by ion-exchange by solvent extraction
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for extracting metal ions in a strong acid system, and belongs to the technical field of metal ion extraction. The method comprises the following steps: s1, mixing high-level radioactive waste liquid and a metal ion chelate stabilizer to obtain a liquid to be extracted; s2, mixing the obtained to-be-extracted liquid with a bisamide pod ether extractant, performing extraction reaction, and performing liquid-liquid separation after the reaction is finished to obtain an organic phase rich in metal ions. The invention can realize the extraction of metal ions, and the metal ion chelate is kept stable in the environment with over-strong acidity in the extraction process, so that the extraction efficiency of the metal ions is high.
Description
Technical Field
The invention belongs to the technical field of metal ion extraction, and particularly relates to a method for extracting metal ions in a strong acid system.
Background
Rare earth is an important nonferrous metal, and has great application value in the fields of new material development, ultrapure material preparation and the like. The solvent extraction has the characteristics of high separation efficiency and low energy consumption, and becomes an important means for separating and purifying rare earth. In addition, during nuclear fuel post-treatment, actinides with long half-life are converted into isotopes with short half-life by neutrons, but lanthanoids can effectively capture neutrons, so that the lanthanoids and the actinoids in the high-level radioactive waste liquid must be separated by a solvent extraction method. Development of novel extractant and scientific design of process flow are two important aspects of solvent extraction all the time, so that exploration of efficient and low-cost extractant has great significance for development of extraction chemistry.
N, N, N ', N' -tetraoctyl-3-oxaglutaramide (TODGA) extractants are widely used for extracting part of heavy metals, lanthanoids and noble metals. However, the extractant has the defect that the phase separation phenomenon is easy to occur in a system with high concentration of strong acid or metal ions, and the reason is that the metal ion chelate is unstable in a strong acid environment in the extraction process, so that the extraction efficiency of the metal ions is low.
Disclosure of Invention
In view of the above, the present invention aims to solve the problems in the prior art, and provides a method for extracting metal ions in a strongly acidic system, by which the metal ions are extracted, and the metal ion chelate remains stable in the environment of the strong acid during the extraction process, so that the extraction efficiency of the metal ions is high.
In order to achieve the above object, the technical scheme of the present invention is as follows:
in a first aspect, the present invention provides a method for extracting metal ions in a strongly acidic system, comprising the steps of:
s1, mixing high-level radioactive waste liquid and a metal ion chelate stabilizer to obtain a liquid to be extracted;
s2, mixing the obtained liquid to be extracted with a bisamide pod ether extractant, performing extraction reaction, and performing liquid-liquid separation after the reaction is finished to obtain an organic phase rich in metal ions.
Wherein the pH value of the strong acid system is 1-2.
Preferably, the bisamide-pod ether extractant is N, N, N ', N' -tetraoctyl-3-oxaglutaramide, me-TODGA, DODDDGA, DMDODGA or DMDDDGA.
Preferably, the metal ion chelate stabilizer is an alkaline salt solution or an adsorptive carrier for the metal ion chelate.
Preferably, the alkaline salt solution comprises one or more of sodium carbonate solution, sodium acetate solution, sodium silicate solution, sodium phosphate solution.
Preferably, the adsorptive carrier of the metal ion chelate is one of chitosan and agar.
Preferably, in the step S2, the extraction reaction condition is that the extraction time is 10-30 min and the extraction temperature is 30-45 ℃.
In a second aspect, the present invention provides the use of a method for extracting metal ions in a strongly acidic system for extracting lanthanide metal ions.
Compared with the prior art, the invention has the following beneficial effects:
1) According to the method for extracting the metal ions in the strong acid system, disclosed by the invention, the metal chelate generated by the extraction reaction is stabilized by the metal ion chelate stabilizer, so that the dissociation of the metal ion chelate in an environment with excessive acidity is avoided, and the phenomenon of phase separation is not easy to occur, thereby improving the extraction rate of the metal ions.
2) The invention provides a method for extracting metal ions in a strong acid system, wherein a metal ion chelate stabilizer is an alkaline salt solution or an adsorptive carrier of the metal ion chelate, wherein the alkaline salt solution can improve the pH value of the solution in the extraction reaction process, and the ion concentration of the metal ions in the solution is regulated, so that the metal ion chelate generated by the reaction is maintained within the range of the acidity of the proper solution and the ion concentration of the metal ions, the metal ion chelate is kept stable, and the adsorptive carrier is used for blocking the diffusion of the metal ions after the dissociation of the metal ion chelate in an organic phase to another phase after the extraction reaction by absorbing the metal ion chelate and improving the stability of the metal ion chelate.
3) The invention provides an application of a method for extracting metal ions in a strong acid system in extracting lanthanoid elements, which is used for separating lanthanoid elements and actinoid elements in high-level radioactive waste liquid and is convenient for the post-treatment process of nuclear fuel.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a method for extracting metal ions in a strong acid system, which comprises the following steps:
s1, mixing high-level waste liquid obtained by nuclear fuel post-treatment with 0.5mol/L sodium carbonate solution, wherein the acidity of the high-level waste liquid is too high, and the specific pH value is 2, so as to obtain a liquid to be extracted;
s2, mixing the obtained liquid to be extracted with 2.5mol/L of N, N, N ', N' -tetraoctyl-3-oxa-glutaramide extractant, performing extraction reaction for 18min at the extraction temperature of 35 ℃, and performing liquid-liquid separation after the reaction is finished to obtain an organic phase rich in metal ions of lanthanide series elements.
In this example, the sodium carbonate solution is an alkaline salt solution, and the pH of the solution during the extraction reaction can be raised, and the ion concentration of the metal ions in the solution can be adjusted, so that the metal ion chelate complex produced by the reaction can be maintained within the appropriate range of the acidity of the solution and the ion concentration of the metal ions, and the metal ion chelate complex can be kept stable.
It will be appreciated that sodium acetate solution, sodium silicate solution, sodium phosphate solution are also common alkaline salts and that the effect of the sodium carbonate of this example may be replaced with an obvious effect.
In the embodiment, the N, N, N ', N' -tetraoctyl-3-oxaglutaramide extractant is one of bisamide pod ether extractants and is used for extracting lanthanide in high-level radioactive waste liquid, so that the nuclear fuel aftertreatment process is facilitated.
Example 2
The embodiment provides a method for extracting metal ions in a strong acid system, which comprises the following steps:
s1, mixing high-level waste liquid obtained by nuclear fuel post-treatment with 1.0mol/L chitosan solution, wherein the acidity of the high-level waste liquid is too high, and the specific pH value is 1, so as to obtain a liquid to be extracted;
s2, mixing the obtained liquid to be extracted with 2.5mol/L of N, N, N ', N' -tetraoctyl-3-oxa-glutaramide extractant, performing extraction reaction for 10min at the temperature of 45 ℃, and performing liquid-liquid separation after the reaction is finished to obtain an organic phase rich in metal ions of lanthanide series elements.
In this embodiment, the chitosan is a porous adsorptive carrier, and by utilizing the characteristic of porous nature, the metal ions dissociated from the metal ion chelate in the organic phase after the extraction reaction are prevented from diffusing into the other phase, so that the stability of the metal ion chelate is improved.
In the embodiment, the N, N, N ', N' -tetraoctyl-3-oxaglutaramide extractant is one of bisamide pod ether extractants and is used for extracting lanthanide in high-level radioactive waste liquid, so that the nuclear fuel aftertreatment process is facilitated.
Example 3
The embodiment provides a method for extracting metal ions in a strong acid system, which comprises the following steps:
s1, mixing high-level waste liquid obtained by nuclear fuel post-treatment with an agar solution of 0.5mol/L, wherein the acidity of the high-level waste liquid is too high, and the specific pH value is 1, so as to obtain a liquid to be extracted;
s2, mixing the obtained liquid to be extracted with 1.5mol/L Me-TODGA (N, N, N ', N' -tetraoctyl-2-methyl-3-oxaglutaramide) extractant, performing extraction reaction for 30min at the extraction temperature of 30 ℃, and performing liquid-liquid separation after the reaction is finished to obtain an organic phase rich in metal ions of lanthanide series, wherein the organic phase is rich in metal ions of lanthanide series.
In this embodiment, the agar is a porous adsorptive carrier, and by utilizing the porous characteristic of the agar, the metal ions dissociated from the metal ion chelate in the organic phase after the extraction reaction are prevented from diffusing into the other phase, so that the stability of the metal ion chelate is improved.
In the embodiment, the Me-TODGA extractant is also one of bisamide pod ether extractants, and is used for extracting lanthanide in high-level waste liquid, so that the nuclear fuel post-treatment process is facilitated.
It is understood that DODDDGA, DMDODGA or DMDDDGA is also a common bisamide pod ether extractant, and that the effect of the alternative Me-TODGA of this example is readily apparent.
Comparative example
This comparative example provides a method for extracting metal ions in a strongly acidic system, which is different from examples 1 to 3 in that the step of mixing a metal ion chelate stabilizer with a nuclear fuel post-treatment high-level waste liquid is not performed, the nuclear fuel post-treatment high-level waste liquid and an N, N, N ', N' -tetraoctyl-3-oxaglutaramide extractant are directly mixed to perform an extraction reaction, and the other steps are the same as example 1.
Example 4
Evaluation of the separation Effect of extraction
This example provides the extraction of lanthanide metal ions from high level waste liquid using the extraction rate to evaluate the extraction effect by the method for extracting metal ions in a strongly acidic system provided in examples 1 to 3 and comparative example, and the extraction result data are shown in table 1.
The extraction rate is used for indicating the complete degree of extraction of metal ions into the organic phase, and the symbol is E, and the calculation formula is as follows:
e=mass number of extracted metal ions in organic phase/total amount of extracted metal ions 100%
The larger E indicates the better extraction effect of the extractant on the metal ions.
TABLE 1 extraction Effect of extraction of lanthanide Metal ions from examples 1-3 and comparative examples
| Project | pH during the extraction reaction | Extraction rate after extraction reaction |
| Example 1 | 6.8 | 48.6％ |
| Example 2 | 6.2 | 40.5％ |
| Example 3 | 6.4 | 45.2％ |
| Comparative example | 0.8 | 12％ |
As can be seen from the extraction result data in Table 1, compared with the comparative examples, the method for extracting metal ions in a strongly acidic system provided in examples 1 to 3 has very high extraction rate, the extraction rate is above 40%, the pH value in the extraction reaction process is above 6, the extraction effect of the comparative example is poor, the pH value in the extraction reaction process is also reduced, and the stability of the metal ion chelate is more unfavorable to be maintained.
The previous description of the disclosed embodiments, and examples, is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A method for extracting metal ions in a strongly acidic system, comprising the steps of:
s1, mixing high-level radioactive waste liquid and a metal ion chelate stabilizer to obtain a liquid to be extracted;
s2, mixing the obtained liquid to be extracted with a bisamide pod ether extractant, performing extraction reaction, and performing liquid-liquid separation after the reaction is finished to obtain an organic phase rich in metal ions.
2. A method for extracting metal ions in a strongly acidic system as claimed in claim 1, wherein the pH of said strongly acidic system is from 1 to 2.
3. A method for extracting metal ions in a strongly acidic system as claimed in claim 1, wherein the bisamide capsular ether extractant is N, N' -tetraoctyl-3-oxaglutaramide, me-TODGA, DODDDGA, DMDODGA or DMDDDGA.
4. A method for extracting metal ions in a strongly acidic system as claimed in claim 1, wherein the metal ion chelate stabilizer is an alkaline salt solution or an adsorptive carrier for the metal ion chelate.
5. The method of extracting metal ions in a strongly acidic system of claim 4, wherein the basic salt solution comprises one or more of sodium carbonate solution, sodium acetate solution, sodium silicate solution, and sodium phosphate solution.
6. The method for extracting metal ions in a strongly acidic system as set forth in claim 4, wherein the adsorptive carrier of the metal ion chelate is one of chitosan and agar.
7. The method for extracting metal ions in a strongly acidic system as set forth in claim 1, wherein the conditions for the extraction reaction in S2 are an extraction time of 10 to 30min and an extraction temperature of 30 to 45 ℃.
8. Use of a method according to any one of claims 1 to 7 for extracting metal ions in a strongly acidic system for extracting lanthanide metal ions.
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