CN114888057A - Harmless treatment method for rare earth radioactive waste residues - Google Patents
Harmless treatment method for rare earth radioactive waste residues Download PDFInfo
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- CN114888057A CN114888057A CN202210554410.5A CN202210554410A CN114888057A CN 114888057 A CN114888057 A CN 114888057A CN 202210554410 A CN202210554410 A CN 202210554410A CN 114888057 A CN114888057 A CN 114888057A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 129
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 82
- 239000002901 radioactive waste Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000002386 leaching Methods 0.000 claims abstract description 94
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 74
- 238000005406 washing Methods 0.000 claims abstract description 71
- 239000002699 waste material Substances 0.000 claims abstract description 57
- 230000002285 radioactive effect Effects 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000012071 phase Substances 0.000 claims description 56
- 238000000605 extraction Methods 0.000 claims description 35
- 239000007788 liquid Substances 0.000 claims description 32
- 239000007791 liquid phase Substances 0.000 claims description 31
- 238000005185 salting out Methods 0.000 claims description 28
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 238000005342 ion exchange Methods 0.000 claims description 17
- 150000007522 mineralic acids Chemical class 0.000 claims description 12
- 230000002378 acidificating effect Effects 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 150000001450 anions Chemical class 0.000 claims description 9
- 239000008139 complexing agent Substances 0.000 claims description 9
- 230000000536 complexating effect Effects 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims 1
- 239000002893 slag Substances 0.000 abstract description 28
- 239000002910 solid waste Substances 0.000 abstract description 14
- 238000003860 storage Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000009270 solid waste treatment Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 16
- 238000000926 separation method Methods 0.000 description 15
- 238000003795 desorption Methods 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 238000001035 drying Methods 0.000 description 11
- 238000001914 filtration Methods 0.000 description 8
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 8
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 230000004913 activation Effects 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000011707 mineral Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 239000003350 kerosene Substances 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 2
- 229910052776 Thorium Inorganic materials 0.000 description 2
- 229910052770 Uranium Inorganic materials 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910052705 radium Inorganic materials 0.000 description 2
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 238000005496 tempering Methods 0.000 description 2
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 2
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical compound CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 description 1
- WBLGXIFKKXGJGJ-UHFFFAOYSA-N CC(CCCCCC)(C)OP(O)(=O)C Chemical compound CC(CCCCCC)(C)OP(O)(=O)C WBLGXIFKKXGJGJ-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 1
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 229910052590 monazite Inorganic materials 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000941 radioactive substance Substances 0.000 description 1
- -1 rare earth nitrate Chemical class 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/70—Chemical treatment, e.g. pH adjustment or oxidation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/80—Destroying solid waste or transforming solid waste into something useful or harmless involving an extraction step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B2101/00—Type of solid waste
- B09B2101/55—Slag
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
Landscapes
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention belongs to the technical field of solid waste treatment, and provides a harmless treatment method of rare earth radioactive waste residues. The harmless treatment method of the invention mixes the rare earth radioactive waste residue and the leaching agent for leaching to obtain the primary purified waste residue; and washing the primarily purified waste residue to obtain harmless waste residue. According to the harmless treatment method provided by the invention, the leaching agent with the concentration of 6-8 mol/L is used for leaching the rare earth radioactive waste residues at the temperature of 60-70 ℃, so that rare earth elements and radioactive elements in the rare earth radioactive waste residues can be leached into a leaching solution; and then the primarily purified waste residue obtained after leaching is washed with water, and the leached rare earth elements and radioactive elements remained in the primarily purified waste residue are transferred into a washing solution, so that the rare earth radioactive waste residue is converted into general solid waste, the storage pressure of a slag warehouse is relieved, and the influence of the rare earth radioactive waste residue on production personnel and the surrounding environment is reduced.
Description
Technical Field
The invention relates to the technical field of solid waste treatment, in particular to a harmless treatment method of rare earth radioactive waste residues.
Background
The rare earth minerals in China are various in variety, and are the only rare earth resource big countries in the world which can supply a large amount of rare earth minerals of different varieties and grades. Rare earth is used as an important mineral resource in the present day, and has wide application in petrochemical industry, glass, ceramics, steel, luminescent materials, hydrogen storage materials and magnetic materials. In recent years, the demand of rare earth products is increasing day by day, the rare earth mining and smelting industry is also rapidly developed, but the rare earth waste residue containing a large amount of radioactive elements is produced in the rare earth separation process.
The rare earth waste slag is a general name of acid dissolving slag, tempering slag and neutralization slag produced in the processes of acid dissolving, tempering, neutralizing and the like of rare earth raw ore, rare earth concentrate and the like. Many rare earth minerals (rare earth raw ore and rare earth concentrate) are associated with radioactive elements, for example, rare earth raw ore and rare earth concentrate such as monazite and bastnaesite used in rare earth smelting separation are associated with radioactive elements such as thorium, uranium and radium, in a rare earth extraction process such as acid dissolution, the mineral structure is damaged, part of the radioactive elements are released and enter rare earth feed liquid, and the associated radioactive elements are further enriched in the ore dressing, smelting and separation of rare earth and are transferred to slag through the processes of acid dissolution, adjustment, neutralization and the like to form rare earth radioactive waste slag. And the rare earth radioactive waste residues are not further treated, and a special rare earth radioactive waste residue library is established by a general rare earth separation enterprise and is uniformly stored. With the continuous operation of rare earth separation enterprises, rare earth radioactive waste residues can be continuously produced, the storage pressure of the slag warehouse is very high, the capability of the slag warehouse for resisting natural disasters is weak, and great potential safety hazards are caused to the surrounding environment and the health of personnel.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for harmless treatment of rare earth radioactive waste residues. The harmless treatment method provided by the invention can convert the rare earth radioactive waste residues into general solid waste, and reduces the influence of the rare earth radioactive waste residues on production personnel and surrounding environment while relieving the storage pressure of a slag warehouse.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a harmless treatment method of rare earth radioactive waste residues, which comprises the following steps:
mixing the rare earth radioactive waste residue with a leaching agent, and leaching to obtain primary purified waste residue;
washing the primarily purified waste residue to obtain harmless waste residue;
the leaching agent comprises an inorganic acid;
the concentration of the leaching agent is 6-8 mol/L;
the leaching temperature is 60-70 ℃, and the heat preservation time is 1-2 h.
Preferably, the dosage ratio of the rare earth radioactive waste residue to the leaching agent is 1 g: 4-6 mL.
Preferably, the number of washing is 2-4.
Preferably, the washed reagent comprises water; the washing temperature is 60-70 ℃, and the washing time is 1-2 h; the washing is carried out under stirring.
Preferably, the leaching also results in a leachate; washing to obtain a washing solution; combining the leaching solution and the washing solution to be used as a liquid phase for radioactive element enrichment;
the radioactive element enrichment comprises:
mixing the liquid phase with a salting-out agent to obtain a salting-out liquid phase;
extracting the salting-out liquid phase by using an extracting agent to obtain an extract phase;
and (3) sequentially washing and back-extracting the extract phase to obtain back-extraction solution.
Preferably, the extracting agent comprises a complexing agent and a diluent, the complexing agent is a neutral complexing extracting agent or an acidic complexing extracting agent, the mass percentage of the complexing agent in the extracting agent is 20-30%, the extracting temperature is 10-20 ℃, and the extracting times are 3-6.
Preferably, the stripping agent for stripping comprises inorganic acid, the concentration of the stripping agent is 0.5-2 mol/L, and the stripping temperature is 60-80 ℃.
Preferably, the extraction also yields a raffinate; washing with water to obtain a washing solution; combining the raffinate and the water washing liquid to be used as a water phase for ion exchange;
the ion exchange comprises: and adjusting the pH value of the water phase to 2.5-3.0, placing the water phase on an ion exchange column, and leaching and analyzing the water phase in sequence.
Preferably, the packing of the ion exchange column comprises a strongly basic anionic resin.
Preferably, the eluted eluting agent comprises a citric acid solution, and the mass concentration of the eluting agent is 0.1-0.5%; the analytic agent comprises inorganic acid, and the concentration of the analytic agent is 1-3 mol/L.
The invention provides a harmless treatment method of rare earth radioactive waste residues, which comprises the following steps: mixing the rare earth radioactive waste residue with a leaching agent, and leaching to obtain primary purified waste residue; washing the primarily purified waste residue to obtain harmless waste residue; the leaching agent comprises an inorganic acid; the concentration of the leaching agent is 6-8 mol/L; the leaching temperature is 60-70 ℃, and the heat preservation time is 1-2 h. According to the harmless treatment method provided by the invention, the leaching agent with the concentration of 6-8 mol/L is used for leaching the rare earth radioactive waste residues at 60-70 ℃, so that most of rare earth elements and radioactive elements in the rare earth radioactive waste residues can be leached into a leaching solution, and meanwhile, the leaching of a large amount of iron, silicon and aluminum can be avoided, and the subsequent separation and enrichment of the rare earth elements and the radioactive elements are facilitated; and then washing the primarily purified waste residue obtained after leaching, transferring the leached rare earth elements and radioactive elements remained in the primarily purified waste residue into washing liquid, so as to convert the rare earth radioactive waste residue into general solid waste, slow down the storage pressure of a slag warehouse and reduce the influence of the rare earth radioactive waste residue on production personnel and the surrounding environment.
Furthermore, the invention carries out radioactive element enrichment on the leaching solution obtained by leaching and the washing solution obtained by washing, and can enrich the radioactive elements in the liquid phase; meanwhile, the separation of most radioactive elements and rare earth elements is realized.
Furthermore, the invention carries out ion exchange on the raffinate obtained by extraction and the washing liquid obtained by washing, and can realize the separation of the residual radioactive elements and rare earth elements in the water phase; meanwhile, the water dischargeability and the rare earth element enrichment are realized.
Detailed Description
The invention provides a harmless treatment method of rare earth radioactive waste residues, which comprises the following steps:
mixing the rare earth radioactive waste residue with a leaching agent, and leaching to obtain primary purified waste residue;
and washing the primarily purified waste residue to obtain harmless waste residue.
In the present invention, the starting materials used in the present invention are preferably commercially available products unless otherwise specified.
The method mixes the rare earth radioactive waste residue with a leaching agent for leaching to obtain the primary purified waste residue. In the invention, the radioactivity specific activity of the rare earth radioactive waste residue is preferably 1 x 10 3 ～1×10 6 Bq/kg. In the present invention, the radioactivity ratio refers to the radioactivity per unit mass of the solid radioactive substance, and is usually expressed as MBq/mg/(mCi/mg). In the present inventionIn the method, the rare earth radioactive waste residues comprise rare earth elements and radioactive elements; the rare earth elements preferably comprise one or more of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Y, Er, Tm, Yb and Lu. In the present invention, the radioactive element preferably comprises one or more of thorium, uranium and radium.
In the invention, the rare earth radioactive waste residue is preferably pretreated before being leached; the pre-treatment preferably comprises drying and grinding. In the invention, the drying temperature is preferably 100-120 ℃, and more preferably 105-110 ℃; the drying time is preferably 0.5-2 h, and more preferably 1-1.5 h; the drying is preferably carried out in a drying oven. The operation of the grinding is not particularly limited in the present invention as long as it can pass through a 200-mesh sieve.
In the present invention, the leaching agent comprises a mineral acid; the inorganic acid preferably comprises one or more of sulfuric acid, hydrochloric acid and nitric acid. In the invention, the concentration of the leaching agent is 6-8 mol/L, preferably 6.5-7.5 mol/L, and more preferably 7 mol/L. In the invention, the dosage ratio of the rare earth radioactive waste residue to the leaching agent is preferably 1 g: 4-6 mL, more preferably 1 g: 5 mL. In the invention, the leaching temperature is 60-70 ℃, preferably 65 ℃; the heat preservation time is 1-2 h, preferably 1.5 h. In the present invention, the leaching is preferably performed under a stirring condition, and the rotation speed of the stirring is preferably 200 to 500rpm, and more preferably 300 to 400 rpm.
After the leaching, the invention preferably further comprises filtering to obtain a leaching solution and a primary purification waste residue.
After the primary purified waste residue is obtained, the invention washes the primary purified waste residue to obtain harmless waste residue.
In the present invention, the washing agent preferably includes water. In the invention, the washing temperature is preferably 60-70 ℃, and more preferably 65 ℃; the time is preferably 1 to 2 hours, and more preferably 1.5 hours. In the present invention, the washing is preferably performed under a stirring condition, and the rotation speed of the stirring is preferably 200 to 500rpm, and more preferably 300 to 400 rpm. In the present invention, the number of washing is preferably 2 to 4.
After the washing, the invention preferably further comprises filtering to obtain washing liquid and harmless waste residues.
After obtaining the leaching solution and the washing solution, the present invention preferably further comprises combining the leaching solution and the washing solution as a liquid phase for radioactive element enrichment. In the present invention, the radioactive element enrichment preferably includes:
mixing the liquid phase with a salting-out agent to obtain a salting-out liquid phase;
extracting the salting-out liquid phase by using an extracting agent to obtain an extract phase;
and (3) sequentially washing and back-extracting the extract phase to obtain back-extraction solution.
The salting-out liquid phase is obtained by mixing the liquid phase with a salting-out agent. In the present invention, the salting-out agent preferably includes one or more of lithium nitrate, rare earth nitrate, and sodium nitrate. In the present invention, the concentration of the salting-out agent in the salting-out liquid phase is preferably 1 to 3mol/L, and more preferably 2 mol/L.
After the salting-out liquid phase is obtained, the salting-out liquid phase is extracted by an extracting agent to obtain an extraction phase. In the present invention, the extractant preferably includes a complexing agent and a diluent. In the present invention, the complexing agent is preferably a neutral complexing extractant or an acidic complexing extractant, and further preferably includes an acidic complexing extractant. In the present invention, the neutral complexing extractant preferably comprises one or more of neutral tributyl phosphate, sec-octanol, and methyl isobutyl ketone. In the present invention, the acidic complex extractant preferably comprises one or more of acidic tributyl phosphate (acidic TBP), dimethylheptyl methylphosphonate, bis (2-ethylhexyl) phosphate (P204) and 2-ethylhexyl phosphate (P507). In the invention, the mass percentage of the complexing agent in the extracting agent is preferably 20-30%, and more preferably acidic tributyl phosphate. In the present invention, the diluent preferably comprises kerosene. In the invention, the extraction temperature is preferably 10-20 ℃. In the invention, the number of times of extraction is preferably 3-6 times. In the present invention, the extraction is preferably performed by countercurrent extraction. In the present invention, the extraction preferably also results in a raffinate. In the invention, the extraction can transfer the radioactive elements in the liquid phase into the extracting agent to form an extraction phase, and the rare earth elements and a small amount of radioactive elements exist in the extraction raffinate, so that the preliminary separation of the radioactive elements and the rare earth elements is realized.
After the extraction phase is obtained, the extraction phase is sequentially washed and back-extracted to obtain back-extraction solution. The operation of the water washing is not particularly limited in the present invention as long as the rare earth element in the extraction phase can be transferred to water. In the present invention, the washing preferably also results in a water washing solution. In the invention, the water washing can wash off the rare earth elements in the extraction phase, thereby realizing the purification of radioactive elements. In the present invention, the stripping agent of the stripping preferably comprises an inorganic acid, and the inorganic acid preferably comprises one or more of sulfuric acid, hydrochloric acid and nitric acid. In the invention, the concentration of the stripping agent is preferably 0.5-2 mol/L. More preferably 0.5 to 1 mol/L. In the invention, the temperature of the back extraction is preferably 60-80 ℃, more preferably 65-75 ℃, and more preferably 70 ℃. In the present invention, the stripping is capable of transferring the radioactive elements in the extracted phase to the stripping agent.
After obtaining the raffinate and the water washing liquid, the invention preferably further comprises combining the raffinate and the water washing liquid as an aqueous phase for ion exchange. In the present invention, the ion exchange preferably comprises: and adjusting the pH value of the water phase to 2.5-3.0, placing the water phase on an ion exchange column, and leaching and analyzing the water phase in sequence.
In the present invention, the agent for adjusting the pH of the aqueous phase preferably comprises sodium hydroxide and/or calcium hydroxide. In the present invention, the packing of the ion exchange column preferably comprises a strongly basic anion resin; the strongly basic anion resin preferably comprises a strongly basic anion resin of type 717, a strongly basic anion resin of type D201 or a strongly basic anion resin of type D730. In the present invention, the ion exchange column is preferably subjected to an activation treatment before use, and the operation of the activation treatment in the present invention is not particularly limited, and an ion exchange column activation operation known to those skilled in the art may be used. In the invention, the eluted eluting agent preferably comprises a citric acid solution, and the mass concentration of the eluting agent is preferably 0.1-0.5%. In the present invention, the flow rate of the rinsing is preferably 5 mL/min. In the present invention, the resolving agent for resolving preferably includes an inorganic acid, and the inorganic acid preferably includes one or more of sulfuric acid, hydrochloric acid, and nitric acid. In the present invention, the concentration of the resolving agent is preferably 1 to 3 mol/L. In the invention, rare earth elements can be eluted by leaching, while radioactive elements can be eluted by resolving, so that the separation of residual radioactive elements and rare earth elements is realized.
The method for detoxifying rare earth radioactive waste residues according to the present invention will be described in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Step 1: weighing 100g of rare earth radioactive waste residues stored in a slag warehouse, and drying for 1h at 105 ℃ in a drying box; and grinding the dried rare earth radioactive waste residues by using a mortar, and sieving by using a 200-mesh sieve.
Step 2: adding HNO with the concentration of 6mol/L into the rare earth radioactive waste residue obtained in the step 1 3 400 mL; stirring at 300r/min, heating at 70 deg.C for 1 hr, and filtering to obtain leaching solution and primary purified waste residue.
And step 3: and (3) primarily purifying the waste residues, adding water, washing for 2 times at the rotation speed of 300r/min and at the temperature of 70 ℃, and filtering to obtain washing liquid and harmless waste residues.
And 4, step 4: combining the leaching solution obtained in the step 2 and the washing solution obtained in the step 3 to be used as a liquid phase, and adding lithium nitrate to the liquid phase to be used as a salting-out agent, wherein the concentration of the salting-out agent in the obtained salting-out liquid phase is 2.0 mol/L; extracting the salting-out liquid phase for 3 times by using an extracting agent (a diluting agent in the extracting agent is kerosene) with the mass concentration of 25% of acidic TBP to obtain an extraction phase and an extraction raffinate.
And 5: washing the extract phase with water to obtain a washing liquid and a washing extract phase; with 0.5mol/L HNO at 60 DEG C 3 The water-washed extract phase is subjected to back extraction,and collecting the stripping solution.
Step 6: combining the raffinate obtained in the step 4 and the water washing liquid obtained in the step 5 to be used as a water phase, adjusting the pH value of the water phase to be 2.5-3.0, and pouring the water phase into an ion exchange column filled with 717 type strongly basic anion resin (through activation); leaching with 0.1 wt% citric acid as leaching agent at a leaching speed of 5mL/min, and collecting the leaching solution; then adding 1mol/L HNO 3 And (4) taking the solution as a desorption agent for desorption, and collecting desorption liquid.
The specific activity and the content of main elements of the rare earth radioactive waste residue obtained in the step 1 and the harmless waste residue obtained in the step 3 are measured, and the results are shown in tables 1 and 2.
TABLE 1 specific activity of radioactivity of slag (Bq/kg)
| Item | α | β | α+β | Radioactive sorting of solid waste |
| Before leaching | 4.19×10 5 | 2.52×10 5 | 6.71×10 5 | Low level of waste |
| After leaching | 530 | 349 | 879 | General waste |
From table 1, it can be seen: compared with the original rare earth radioactive waste residue, the radioactivity of the harmless waste residue is reduced by 99.87 percent, reaches the standard of common solid waste, and can be treated according to the common solid waste.
TABLE 2 main element composition of slag
As can be seen from table 2: the leaching process does not cause a great amount of leaching loss of iron, silicon and aluminum; meanwhile, after leaching, the contents of rare earth elements and radioactive elements are very low, which indicates that most of the rare earth elements and the radioactive elements are leached by leaching.
The elemental contents of the stripping solution and the stripping solution were measured and the results are shown in Table 3. The content of the main elements in the leacheate was measured, and the results are shown in table 4.
TABLE 3 content of elements in the enriched phase
| U | Ra | Th | K-40 | |
| Reextraction liquid (Bq/kg) | 58634 | 468520 | 2724 | 231 |
| Desorption liquid (Bq/kg) | 12756 | 152698 | 1214 | 140 |
TABLE 4 content of major elements in the enriched phase
As can be seen from tables 3 and 4: the stripping solution and the analysis solution do not contain rare earth elements; the leacheate does not contain radioactive elements, and the method provided by the invention realizes the separation of rare earth elements and the radioactive elements.
According to the volume and the material content of the obtained leacheate and based on the content of the rare earth elements in the original rare earth radioactive waste residues, the recovery rate of the rare earth elements obtained by the method is 89.4%.
Example 2
Step 1: weighing 100g of rare earth radioactive waste residues stored in a slag warehouse, and drying for 1h at 105 ℃ in a drying box; and grinding the dried rare earth radioactive waste residues by using a mortar, and sieving by using a 200-mesh sieve.
Step 2: h with the concentration of 6mol/L is added into the rare earth radioactive waste residue obtained in the step 1 2 SO 4 And (2) stirring at 400mL, heating at the stirring speed of 300r/min, keeping the temperature at 60 ℃ for 1h, and filtering to obtain an extract and primary purified waste residues.
And step 3: and (3) primarily purifying the waste residues, adding water, washing for 2 times at the rotation speed of 300r/min and the temperature of 60 ℃, and filtering to obtain washing liquid and harmless waste residues.
And 4, step 4: combining the leaching solution obtained in the step 2 and the washing solution obtained in the step 3 to serve as a liquid phase, and adding lithium nitrate to the liquid phase to serve as a salting-out agent, wherein the concentration of the salting-out agent in the obtained salting-out liquid phase is 2.0 mol/L; extracting the salting-out liquid phase for 3 times by using an extracting agent (a diluting agent in the extracting agent is kerosene) with the mass concentration of 25% of acidic TBP to obtain an extraction phase and an extraction raffinate.
And 5: washing the extract phase with water to obtain a washing liquid and a washing extract phase; with 0.5mol/L HNO at 70 DEG C 3 And (4) performing back extraction on the water-washed extract phase, and collecting back extraction liquid.
Step 6: combining the raffinate obtained in the step 4 and the water washing liquid obtained in the step 5 to be used as a water phase, adjusting the pH value of the water phase to be 2.5-3.0, and pouring the water phase into a column filled with 717 type strongly basic anion resin (after activation); leaching with 0.1 wt% citric acid as leaching agent at a leaching speed of 5mL/min, and collecting the leaching solution; then adding 1mol/L HNO 3 And (4) taking the solution as a desorption agent for desorption, and collecting desorption liquid.
The specific activity and the content of main elements of the rare earth radioactive waste residue in the step 1 and the harmless waste residue obtained in the step 3 were measured, and the results are shown in tables 5 and 6.
TABLE 5 specific activity of radioactivity of slag (Bq/kg)
| Item | α | β | α+β | Radioactive sorting of solid waste |
| Before leaching | 4.19×10 5 | 2.52×10 5 | 6.71×10 5 | Low level of waste |
| After leaching | 564 | 390 | 954 | General waste |
As can be seen from table 5: the radioactivity ratio activity of the harmless waste residue is 954Bq/kg, which is reduced by 99.86% compared with the radioactivity ratio activity of the original rare earth radioactive waste residue, and the harmless waste residue reaches the standard of common solid waste and can be treated according to the common solid waste.
TABLE 6 main elemental composition of slag
As can be seen from table 6: the leaching process does not cause leaching loss of a large amount of iron, silicon and aluminum; meanwhile, after leaching, the contents of rare earth elements and radioactive elements are very low, which indicates that most of the rare earth elements and the radioactive elements are leached by leaching.
The elemental contents of the stripping solution and the stripping solution were measured and the results are shown in Table 7. The content of the main elements in the leacheate was measured, and the results are shown in table 8.
TABLE 7 content of elements in the enriched phase
| U | Ra | Th | K-40 | |
| Reextraction liquid (Bq/kg) | 64552 | 488647 | 2411 | 234 |
| Desorption liquid (Bq/kg) | 14208 | 102456 | 857 | 96 |
TABLE 8 content of major elements in the enriched phase
As can be seen from tables 7 and 8: the stripping solution and the analysis solution do not contain rare earth elements; the leacheate does not contain radioactive elements, and the method provided by the invention realizes the separation of rare earth elements and the radioactive elements.
According to the volume and the material content of the obtained leacheate and based on the content of the rare earth elements in the original rare earth radioactive waste residues, the recovery rate of the rare earth elements obtained by the method is 86.57%.
Example 3
Step 1: weighing 100g of rare earth radioactive waste residues stored in a slag warehouse, and drying for 1h at 105 ℃ in a drying box; and grinding the dried rare earth radioactive waste residues by using a mortar, and sieving by using a 200-mesh sieve.
Step 2: adding HCl400mL with the concentration of 6mol/L into the rare earth radioactive waste residue obtained in the step 1; stirring at 300r/min, heating at 60 deg.C for 1 hr, and filtering to obtain leaching solution and primary purified waste residue.
And step 3: and (3) primarily purifying the waste residues, adding water, washing for 2 times at the rotation speed of 300r/min and the temperature of 60 ℃, and filtering to obtain washing liquid and harmless waste residues.
And 4, step 4: combining the leaching solution obtained in the step 2 and the washing solution obtained in the step 3 to be used as a liquid phase, and adding lithium nitrate to the liquid phase to be used as a salting-out agent, wherein the concentration of the salting-out agent in the obtained salting-out liquid phase is 2.0 mol/L; extracting the salting-out liquid phase for 3 times by using an extracting agent (a diluting agent in the extracting agent is kerosene) with the mass concentration of 25% of acidic TBP to obtain an extraction phase and an extraction raffinate.
And 5: washing the extract phase with water to obtain a washing liquid and a washing extract phase; with 0.5mol/L HNO at 70 DEG C 3 And (4) performing back extraction on the water-washed extract phase, and collecting back extraction liquid.
And 6: combining the raffinate obtained in the step 4 and the water washing liquid obtained in the step 5 to be used as a water phase, adjusting the pH value of the water phase to be 2.5-3.0, and pouring the water phase into an ion exchange column filled with 717 type strongly basic anion resin (through activation); leaching with 0.1 wt% citric acid as leaching agent at a leaching speed of 5mL/min, and collecting the leaching solution; then adding 1mol/L HNO 3 And (4) taking the solution as a desorption agent for desorption, and collecting desorption liquid.
The specific activity and the content of main elements of the rare earth radioactive waste residue in the step 1 and the harmless waste residue obtained in the step 3 were measured, and the results are shown in tables 9 and 10.
TABLE 9 specific activity of radioactivity of slag (Bq/kg)
| Item | α | β | α+β | Radioactive sorting of solid waste |
| Before leaching | 4.19×10 5 | 2.52×10 5 | 6.71×10 5 | Low level of waste |
| After leaching | 532 | 456 | 988 | General waste |
As can be seen from table 9: the radioactivity ratio activity of the harmless waste residue is 988Bq/kg, is reduced by 99.85 percent compared with the radioactivity ratio activity of the original rare earth radioactive waste residue, reaches the standard of common solid waste, and can be treated according to the common solid waste.
TABLE 10 main elemental composition of slag
As can be seen from table 10: the leaching process does not cause leaching loss of a large amount of iron, silicon and aluminum; meanwhile, after leaching, the contents of rare earth elements and radioactive elements are very low, which indicates that most of the rare earth elements and the radioactive elements are leached by leaching.
The elemental contents of the stripping solution and the stripping solution were measured and the results are shown in Table 11. The content of the main elements in the leacheate was measured, and the results are shown in table 12.
TABLE 11 content of elements in the enriched phase
| U | Ra | Th | K-40 | |
| Reextraction liquid (Bq/kg) | 59577 | 482567 | 2401 | 234 |
| Desorption liquid (Bq/kg) | 12114 | 104506 | 873 | 96 |
TABLE 12 content of essential elements in the enriched phase
As can be seen from tables 11 and 12: the stripping solution and the analysis solution do not contain rare earth elements; the leacheate does not contain radioactive elements; the method provided by the invention realizes the separation of rare earth elements and radioactive elements.
According to the volume and the material content of the obtained leacheate and based on the content of the rare earth elements in the original rare earth radioactive waste residues, the recovery rate of the rare earth elements obtained by the method is 87.69%.
Comparative example 1
The differences from example 1 are: the concentration of nitric acid in the step 2 is 4 mol/L.
The specific activity and the content of main elements of the rare earth radioactive waste residue in the step 1 and the waste residue obtained in the step 3 were measured, and the results are shown in tables 13 and 14.
TABLE 13 specific activity of radioactivity of slag (Bq/kg)
| Item | α | β | α+β | Radioactive sorting of solid waste |
| Before leaching | 4.19×10 5 | 2.52×10 5 | 6.71×10 5 | Low level of waste |
| After leaching | 1156 | 604 | 1760 | Low level of waste |
As can be seen from table 13: the specific activity of the leached waste residue is 1760Bq/kg, which is reduced by 99.74 percent compared with the original rare earth radioactive waste residue.
TABLE 14 main elemental composition of slag
As can be seen from table 14: the leaching process does not cause leaching loss of a large amount of iron, silicon and aluminum; however, the leached slag contains a large amount of rare earth elements and radioactive elements, and the harmless treatment of the slag is not completely realized.
The elemental contents of the stripping solution and the stripping solution were measured and the results are shown in Table 15. The content of the main element in the leacheate was measured, and the results are shown in Table 16.
TABLE 15 content of elements in enriched phase
| U | Ra | Th | K-40 | |
| Reextraction liquid (Bq/kg) | 67854 | 435247 | 2789 | 189 |
| Desorption liquid (Bq/kg) | 11745 | 87965 | 764 | 82 |
TABLE 16 content of essential elements in the enriched phase
As can be seen from tables 15 and 16: the stripping solution and the analysis solution do not contain rare earth elements; the leacheate does not contain radioactive elements, and the method provided by the invention realizes the separation of rare earth elements and the radioactive elements.
According to the volume and the material content of the obtained leacheate and based on the content of the rare earth elements in the original rare earth radioactive waste residues, the recovery rate of the rare earth elements obtained by the method is 52.38 percent and is lower than that of the rare earth elements obtained by the embodiments 1-3.
Comparative example 2
The differences from example 1 are: the temperature in step 2 was 40 ℃.
The specific activity and the content of main elements of the rare earth radioactive waste residue in the step 1 and the harmless waste residue obtained in the step 3 were measured, and the results are shown in tables 17 and 18.
TABLE 17 specific activity of radioactivity of slag (Bq/kg)
| Item | α | β | α+β | Radioactive sorting of solid waste |
| Before leaching | 4.19×10 5 | 2.52×10 5 | 6.71×10 5 | Low level of waste |
| After leaching | 1864 | 592 | 2456 | Low level of waste |
As can be seen from table 17: the radioactivity ratio of the harmless waste residue is 2456Bq/kg, and is reduced by 99.64 percent compared with the radioactivity ratio of the original rare earth radioactive waste residue.
TABLE 18 main elemental composition of slag
As can be seen from table 18: the leaching process does not cause leaching loss of a large amount of iron, silicon and aluminum; however, the leached slag contains a large amount of rare earth elements and radioactive elements, and the harmless treatment of the slag is not completely realized.
The elemental contents of the stripping solution and the stripping solution were measured and the results are shown in Table 19. The content of the main elements in the leacheate was measured, and the results are shown in table 20.
TABLE 19 content of elements in the enriched phase
| U | Ra | Th | K-40 | |
| Reextraction liquid (Bq/kg) | 59798 | 467175 | 2356 | 156 |
| Desorption liquid (Bq/kg) | 15886 | 95627 | 896 | 91 |
TABLE 20 content of essential elements in the enriched phase
As can be seen from tables 19 and 20: the stripping solution and the analysis solution do not contain rare earth elements; the leacheate does not contain radioactive elements, and the method provided by the invention realizes the separation of rare earth elements and the radioactive elements.
According to the volume and the material content of the obtained leacheate and based on the content of the rare earth elements in the original rare earth radioactive waste residues, the recovery rate of the rare earth elements obtained by the method is 43.81%, which is lower than the recovery rate of the rare earth elements obtained by the embodiments 1-3.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A harmless treatment method of rare earth radioactive waste residues is characterized by comprising the following steps:
mixing the rare earth radioactive waste residue with a leaching agent, and leaching to obtain primary purified waste residue;
washing the primarily purified waste residue to obtain harmless waste residue;
the leaching agent comprises an inorganic acid;
the concentration of the leaching agent is 6-8 mol/L;
the leaching temperature is 60-70 ℃, and the heat preservation time is 1-2 h.
2. The innocent treatment method according to claim 1, wherein the dosage ratio of the rare earth radioactive waste residue to the leaching agent is 1 g: 4-6 mL.
3. The method according to claim 1 or 2, wherein the number of washing is 2 to 4.
4. The innocent treatment method according to claim 1, wherein the washing reagent comprises water; the washing temperature is 60-70 ℃, and the washing time is 1-2 h; the washing is carried out under stirring.
5. The innocent treatment method according to claim 1, wherein the leaching also produces a leachate; washing to obtain a washing solution; combining the leaching solution and the washing solution to be used as a liquid phase for radioactive element enrichment;
the radioactive element enrichment comprises:
mixing the liquid phase with a salting-out agent to obtain a salting-out liquid phase;
extracting the salting-out liquid phase by using an extracting agent to obtain an extract phase;
and (3) sequentially washing and back-extracting the extract phase to obtain back-extraction solution.
6. The innocent treatment method according to claim 5, wherein the extractant comprises a complexing agent and a diluent, the complexing agent is a neutral complexing extractant or an acidic complexing extractant, the mass percentage of the complexing agent in the extractant is 20-30%, the temperature of the extraction is 10-20 ℃, and the extraction times are 3-6.
7. The innocent treatment method according to claim 5, wherein the stripping agent for stripping comprises inorganic acid, the concentration of the stripping agent is 0.5-2 mol/L, and the temperature of the stripping is 60-80 ℃.
8. The innocent treatment method according to claim 5, wherein the extraction further yields a raffinate; washing with water to obtain a washing solution; combining the raffinate and the water washing liquid to be used as a water phase for ion exchange;
the ion exchange comprises: and adjusting the pH value of the water phase to 2.5-3.0, placing the water phase on an ion exchange column, and leaching and analyzing the water phase in sequence.
9. The method according to claim 8, wherein the filler of the ion exchange column comprises a strongly basic anion resin.
10. The innocent treatment method according to claim 8, wherein the eluted eluting agent includes a citric acid solution, and the eluting agent has a mass concentration of 0.1-0.5%; the analytic agent comprises inorganic acid, and the concentration of the analytic agent is 1-3 mol/L.
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| CN103184343A (en) * | 2013-03-08 | 2013-07-03 | 包头稀土研究院 | Method for recovering rare earth, thorium and iron in waste residue of rare earth acid technological process |
| CN106957966A (en) * | 2016-01-12 | 2017-07-18 | 厦门稀土材料研究所 | A kind of method that thorium and rare earth element are reclaimed from rare earth waste |
| CN110373556A (en) * | 2019-07-05 | 2019-10-25 | 湖南稀土金属材料研究院 | The method of radioactive element is recycled from zirconium industrial residue |
| WO2019212420A1 (en) * | 2018-05-02 | 2019-11-07 | Apli.Kal, Druzstvo | Method for repurposing of the waste product from the production of heat or electricity from solid fuels and method of use of this repurposed waste product |
| CN114250367A (en) * | 2021-12-29 | 2022-03-29 | 五矿稀土江华有限公司 | Method for comprehensively recovering valuable elements in ionic rare earth impurity removal slag |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103184343A (en) * | 2013-03-08 | 2013-07-03 | 包头稀土研究院 | Method for recovering rare earth, thorium and iron in waste residue of rare earth acid technological process |
| CN106957966A (en) * | 2016-01-12 | 2017-07-18 | 厦门稀土材料研究所 | A kind of method that thorium and rare earth element are reclaimed from rare earth waste |
| WO2019212420A1 (en) * | 2018-05-02 | 2019-11-07 | Apli.Kal, Druzstvo | Method for repurposing of the waste product from the production of heat or electricity from solid fuels and method of use of this repurposed waste product |
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