CN108821307B - Method for recovering residual ammonium ions in ore body after mining of ion adsorption type rare earth ore - Google Patents
Method for recovering residual ammonium ions in ore body after mining of ion adsorption type rare earth ore Download PDFInfo
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- CN108821307B CN108821307B CN201810777289.6A CN201810777289A CN108821307B CN 108821307 B CN108821307 B CN 108821307B CN 201810777289 A CN201810777289 A CN 201810777289A CN 108821307 B CN108821307 B CN 108821307B
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- magnesium
- ammonium ions
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- -1 ammonium ions Chemical class 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 20
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 15
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 14
- 238000005065 mining Methods 0.000 title claims abstract description 13
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 11
- 150000002500 ions Chemical class 0.000 title claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002386 leaching Methods 0.000 claims abstract description 13
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 9
- MXZRMHIULZDAKC-UHFFFAOYSA-L ammonium magnesium phosphate Chemical compound [NH4+].[Mg+2].[O-]P([O-])([O-])=O MXZRMHIULZDAKC-UHFFFAOYSA-L 0.000 claims abstract description 7
- MHJAJDCZWVHCPF-UHFFFAOYSA-L dimagnesium phosphate Chemical compound [Mg+2].OP([O-])([O-])=O MHJAJDCZWVHCPF-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910052567 struvite Inorganic materials 0.000 claims abstract description 7
- 229910000395 dimagnesium phosphate Inorganic materials 0.000 claims abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 15
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 229910019142 PO4 Inorganic materials 0.000 claims description 12
- 239000012452 mother liquor Substances 0.000 claims description 11
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 10
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 7
- 229960002261 magnesium phosphate Drugs 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 5
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 5
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 238000005915 ammonolysis reaction Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract 2
- 239000006096 absorbing agent Substances 0.000 abstract 1
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 238000000151 deposition Methods 0.000 abstract 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- 239000002734 clay mineral Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Treating Waste Gases (AREA)
- Removal Of Specific Substances (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A method for recovering residual ammonium ions in ore body after mining of ion-adsorption type rare earth ore includes such steps as using magnesium salt solution with a certain concentration as exchanger, using engineering measures and equipment in rare earth mining procedure to complete exchange leaching of ammonium ions, depositing ammonium ions by magnesium ammonium phosphate method, recovering ammonium ions from magnesium ammonium phosphate by alkali-thermal method, volatilizing ammonium ions in the form of ammonia gas, absorbing ammonia water with a certain concentration by absorber for recovery, and using the generated magnesium hydrogen phosphate as precipitant for cyclic use. The method has simple process, can quickly realize the recovery of the ammonium ions in the mining of the ion-adsorption type rare earth ore, and reduces the pollution of the ammonium ions to the environment.
Description
Technical Field
The invention relates to a method for recovering residual ammonium ions in an ore body after the exploitation of an ion adsorption type rare earth ore.
Background
The mining of ion adsorption type rare earth ore in south has been in history for decades, and in recent decades, an in-situ ore leaching mode is adopted, ammonium sulfate is used as an ore leaching agent, ammonium sulfate solution is injected into a certain number of injection wells excavated in situ in a mountain body in the ore body to exchange rare earth ions, and the ammonium ions are adsorbed in the ore body by clay minerals. Due to the activity of ammonium ions, the adsorbed ammonium ions are easy to migrate by natural rainfall and excreted in a water body around an ore body in a slow release form, so that the ammonia nitrogen in surface water exceeds the national specified environmental standard, and in addition, the slow release time is long, and the mining area is wide, so that a method for quickly releasing the ammonium ions remained in the ore body and recycling the ammonium ions is urgently needed to solve the long-term pollution problem.
Disclosure of Invention
The invention aims to provide a method for recovering residual ammonium ions in an ore body after the mining of ion adsorption type rare earth ore, which has simple process and can reduce environmental pollution.
The method for recovering the residual ammonium ions in the ore body after the mining of the ion adsorption type rare earth ore comprises the following steps:
1. preparing a magnesium sulfate or magnesium chloride solution with the concentration of 0.5-5% in a solution preparation pool for later use;
2. the prepared magnesium sulfate or magnesium chloride solution is conveyed to a head tank by a pump through a pipeline, the head tank is connected with a liquid injection well through a pipeline, and the solution is subjected to drip leaching;
3. leaching liquid is evenly saturated in the ore body, then seeps out from the bottom of the ore body, and is collected by a liquid collecting ditch and conveyed to a mother liquid collecting tank for storage and standby;
4. conveying the mother liquor in the mother liquor collecting tank to a mother liquor adjusting tank through a pipeline, adjusting the pH =6.6-7.3 by magnesium oxide, and then clarifying for later use;
5. leading the supernatant clarified in the step 4 into a sedimentation tank through a pipeline, and sampling to detect Mg2+、NH4 +Determining the quantity of supplemented magnesium salt and phosphate, and the optimal conditions of precipitation: mg (magnesium)2+:NH4 +:PO4 3-The molar ratio is 1.2:1:1.1, magnesium salt and phosphate are added according to the proportion, and then the mixture is self-circulated and stirred in a sedimentation tank by a pump for more than 1 hour and then is clarified for standby;
6. filtering the magnesium ammonium phosphate precipitate generated in the step 5 by using a plate-and-frame filter press, transferring the filtrate into a solution preparation pool for solution preparation, and reserving filter residues for later use;
7. putting the filter residue generated in the step 6 into a steel barrel with stirring function, sealing the barrel body,the upper part is provided with an air outlet connected with the absorption tower, the wall of the barrel is provided with a coil electric heater, water with 2 times of the amount of filter residue is added, then solid sodium hydroxide is added for ammonolysis, and the weight ratio of the added sodium hydroxide is NH4 +The amount is more than 2 times, a stirring and heating device is started, the system is heated to 85-95 ℃ for reaction, an absorption device is started for ammonia absorption, and the reaction time is more than 1 hour;
8. and 7, conveying the magnesium hydrogen phosphate generated after the reaction in the step 7 to a storage barrel with a stirrer through a pipeline for next ammonium ion precipitation, and transporting the generated ammonia water to the outside after reaching a certain concentration.
The invention relates to a method for recovering residual ammonium ions in an ore body after mining of an ion adsorption type rare earth ore, which utilizes a magnesium salt solution with a certain concentration as an exchanger, utilizes engineering measures and equipment in the rare earth mining process to complete the exchange leaching of the ammonium ions, adopts a magnesium ammonium phosphate method to precipitate the ammonium ions, adopts an alkaline thermal method to recover the ammonium ions in the magnesium ammonium phosphate, volatilizes the ammonium ions in the form of ammonia gas, absorbs ammonia water with a certain concentration through an absorption device to be recycled, generates magnesium hydrogen phosphate as a precipitator to be recycled, and has the reaction formula as follows:
Mg2++2NH4 +(A)=Mg2+(A)+2NH4 +(wherein A is a clay mineral)
Mg2++NH4 ++PO4 3-=MgNH4PO4↓
NaOH+MgNH4PO4=NH3↑+MgHPO4+NaOH。
Detailed Description
The method for recovering the residual ammonium ions in the ore body after the mining of the ion adsorption type rare earth ore comprises the following steps of:
the leaching facilities extend to all facilities for leaching rare earth ore, and are as follows:
1. engineering facilities: elevated tank 50m3Liquid injection well, pipeline, liquid collecting ditch, etc.;
2. liquid collection facility: mother liquor collecting tank 400m3 1, mother liquor adjusting tank 200m3 4 are provided with200m in a sedimentation tank3 3, a liquid preparation pool of 400m3 1, the number of the active ingredients is 1;
the absorption device is a filler spray absorption tower made of 1 pp material, three-stage absorption is realized, and the volume is 10m3Absorbed water is stored at 20m3 The pp material is arranged in a closed tank and is connected with the absorption tower by a pipeline.
The method comprises the following specific steps:
1. preparing a magnesium sulfate or magnesium chloride solution with the concentration of 0.5-5% in a solution preparation pool for later use;
2. the prepared magnesium salt solution is conveyed to a high-level pool by a pump through a pipeline, and an exchanger in the high-level pool is connected with a liquid injection well through a pipeline for drip tank leaching;
3. leaching liquid is evenly saturated in the ore body, then seeps out from the bottom of the ore body, and is collected by a liquid collecting ditch and conveyed to a mother liquid collecting tank for storage and standby;
4. conveying the mother liquor in the mother liquor collecting tank to a mother liquor adjusting tank through a pipeline, adjusting the pH =7 by magnesium oxide, and then clarifying for later use;
5. leading the supernatant clarified in the step 4 into a sedimentation tank through a pipeline, and sampling to detect Mg2+、NH4 +Determining the quantity of supplemented magnesium salt and phosphate, and the optimal conditions of precipitation: mg (magnesium)2+:NH4 +:PO4 3-The molar ratio is 1.2:1:1.1, magnesium salt and phosphate are added according to the proportion, and then the mixture is self-circulated and stirred in a sedimentation tank by a pump for more than 1 hour and then is clarified for standby;
6. filtering the magnesium ammonium phosphate precipitate generated in the step 5 by using a plate-and-frame filter press, transferring the filtrate into a solution preparation pool for solution preparation, and reserving filter residues for later use;
7. putting the filter residue generated in the step 6 into a container with the diameter of 10m3The steel barrel with stirring is closed, the upper part of the steel barrel is provided with an air outlet which is connected with the absorption tower, the wall of the steel barrel is provided with a coil electric heater, water with 2 times of the amount of filter residue is added, then solid sodium hydroxide is added for ammonolysis, and the amount of the added sodium hydroxide is NH4 +The weight ratio of the amount of the ammonia gas is more than 2 times, a stirring and heating device is started, the system temperature is heated to 90 ℃ for reaction, an absorption tower is started for absorbing the ammonia gas, and the reaction is carried out1 hour or more;
8. the magnesium hydrogen phosphate generated after the reaction in the step 7 is conveyed to 1 magnesium hydrogen phosphate with the length of 20m by a pipeline3The storage barrel with the stirring function is used for next ammonium ion precipitation, and the generated ammonia water is transported outside after reaching a certain concentration.
Claims (1)
1. A method for recovering residual ammonium ions in an ore body after mining of ion adsorption type rare earth ore is characterized by comprising the following steps: it comprises the following steps:
(1) preparing a magnesium sulfate or magnesium chloride solution with the concentration of 0.5-5% in a solution preparation pool for later use;
(2) the prepared magnesium sulfate or magnesium chloride solution is conveyed to a high-level pool by a pump through a pipeline, the high-level pool is connected with a liquid injection well through a pipeline, and the solution is subjected to drip leaching;
(3) leaching solution is evenly saturated in the ore body and then seeps out from the bottom of the ore body, and the leaching solution is collected by a liquid collecting ditch and conveyed to a mother liquid collecting tank for storage and standby;
(4) conveying the mother liquor in the mother liquor collecting tank to a mother liquor adjusting tank through a pipeline, adjusting the pH =6.6-7.3 by magnesium oxide, and then clarifying for later use;
(5) introducing the supernatant clarified in the step (4) into a sedimentation tank through a pipeline, and sampling to detect Mg2+、NH4 +Determining the quantity of supplemented magnesium salt and phosphate, and the optimal conditions of precipitation: mg (magnesium)2+:NH4 +:PO4 3-The molar ratio is 1.2:1:1.1, magnesium salt and phosphate are added according to the proportion, and then the mixture is self-circulated and stirred in a sedimentation tank by a pump for more than 1 hour and then is clarified for standby;
(6) filtering the magnesium ammonium phosphate precipitate generated in the step (5) through a plate-and-frame filter press, transferring the filtrate into a solution preparation pool for solution preparation, and reserving filter residues for later use;
(7) putting the filter residue generated in the step (6) into a steel barrel with stirring function, sealing the barrel body, arranging an air outlet at the upper part to be connected with an absorption tower, arranging a coil electric heater on the barrel wall, adding water with the amount of 2 times of the filter residue, then putting solid sodium hydroxide for ammonolysis, and putting the sodium hydroxide into the barrel with the weight ratio of NH4 +The amount is more than 2 times, a stirring and heating device is started, the system is heated to 85-95 ℃ for reaction, an absorption tower is started for ammonia absorption, and the reaction time is more than 1 hour;
(8) and (4) after the reaction in the step (7) is finished, the generated magnesium hydrogen phosphate is conveyed to a storage barrel with stirring through a pipeline for ammonium ion precipitation next time, and the generated ammonia water is transported outside after reaching a certain concentration.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810777289.6A CN108821307B (en) | 2018-07-16 | 2018-07-16 | Method for recovering residual ammonium ions in ore body after mining of ion adsorption type rare earth ore |
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| CN201810777289.6A CN108821307B (en) | 2018-07-16 | 2018-07-16 | Method for recovering residual ammonium ions in ore body after mining of ion adsorption type rare earth ore |
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| CN110479747B (en) * | 2019-08-30 | 2021-06-29 | 江西理工大学 | A kind of in-situ leaching rare earth mining area soil ammonia nitrogen pollution removal method and system |
| CN111088054A (en) * | 2019-12-09 | 2020-05-01 | 武汉工程大学 | Weathering crust elution agent for rare earth ore and elution method thereof |
| CN111482452B (en) * | 2020-04-03 | 2022-05-10 | 武汉工程大学 | Gradient leaching technology for residual leaching agent of weathering crust leaching type rare earth ore |
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|---|---|---|---|---|
| CN102190325A (en) * | 2010-03-17 | 2011-09-21 | 北京有色金属研究总院 | Method for recovering rare earth from ionic type rare earth crude ore |
| CN102674395A (en) * | 2012-05-22 | 2012-09-19 | 河海大学 | Method for preparing ammonia gas from ammonia-nitrogen-containing wastewater |
| CN103695670A (en) * | 2013-11-21 | 2014-04-02 | 南昌大学 | Method for improving ionic rare earth extraction rate and mine tailing safety |
| CN107217139A (en) * | 2017-05-31 | 2017-09-29 | 赣州稀土开采技术服务有限公司 | Southern ion type rareearth ore is without ammonia production practice |
-
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- 2018-07-16 CN CN201810777289.6A patent/CN108821307B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190325A (en) * | 2010-03-17 | 2011-09-21 | 北京有色金属研究总院 | Method for recovering rare earth from ionic type rare earth crude ore |
| CN102674395A (en) * | 2012-05-22 | 2012-09-19 | 河海大学 | Method for preparing ammonia gas from ammonia-nitrogen-containing wastewater |
| CN103695670A (en) * | 2013-11-21 | 2014-04-02 | 南昌大学 | Method for improving ionic rare earth extraction rate and mine tailing safety |
| CN107217139A (en) * | 2017-05-31 | 2017-09-29 | 赣州稀土开采技术服务有限公司 | Southern ion type rareearth ore is without ammonia production practice |
Non-Patent Citations (2)
| Title |
|---|
| Solution, exchangeable and clay-fixed ammonium in south coast British Columbia soils;C. G. Kowalenko and S. Yu;《Canadian Journal of Soil Science》;19961231;第76卷(第4期);第473-483页 * |
| 杨帅.离子型稀土矿开采过程中氨氮吸附解吸行为研究 .《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》.2016, * |
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Effective date of registration: 20210525 Address after: 341099 Unit 2, Building 1, 25 Hongqi Avenue, Zhanggong District, Ganzhou City, Jiangxi Province Applicant after: Sun Dongjiang Applicant after: Wang Qiang Applicant after: You Yilin Applicant after: Wang Zhiyong Applicant after: Cheng Zhe Address before: 341099 Unit 2, Building 1, 25 Hongqi Avenue, Zhanggong District, Ganzhou City, Jiangxi Province Applicant before: Sun Dongjiang Applicant before: Wang Zhiyong |
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Application publication date: 20181116 Assignee: Longnan Xiang'an Materials Co.,Ltd. Assignor: Sun Dongjiang|Wang Qiang|You Yilin|Wang Zhiyong|Cheng Zhe Contract record no.: X2023980035206 Denomination of invention: Recovery method for residual ammonium ions in ore bodies after ion adsorption rare earth mining Granted publication date: 20210611 License type: Exclusive License Record date: 20230504 |