CN1058995A - Centrifugal extraction process of rare earth ore mother liquor from naphthenic acid - Google Patents
Centrifugal extraction process of rare earth ore mother liquor from naphthenic acid Download PDFInfo
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- CN1058995A CN1058995A CN90107128A CN90107128A CN1058995A CN 1058995 A CN1058995 A CN 1058995A CN 90107128 A CN90107128 A CN 90107128A CN 90107128 A CN90107128 A CN 90107128A CN 1058995 A CN1058995 A CN 1058995A
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- acid
- extraction
- rare earth
- grams per
- mother liquor
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- 238000000605 extraction Methods 0.000 title claims abstract description 32
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 23
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 22
- 239000012452 mother liquor Substances 0.000 title claims abstract description 14
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 title claims abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000012074 organic phase Substances 0.000 claims abstract description 19
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 16
- 239000000654 additive Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 7
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 5
- 238000002386 leaching Methods 0.000 claims description 5
- NEAQRZUHTPSBBM-UHFFFAOYSA-N 2-hydroxy-3,3-dimethyl-7-nitro-4h-isoquinolin-1-one Chemical compound C1=C([N+]([O-])=O)C=C2C(=O)N(O)C(C)(C)CC2=C1 NEAQRZUHTPSBBM-UHFFFAOYSA-N 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- 239000011707 mineral Substances 0.000 claims description 4
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 3
- 235000019257 ammonium acetate Nutrition 0.000 claims description 3
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 claims description 3
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims description 2
- 239000005695 Ammonium acetate Substances 0.000 claims 1
- 229940043376 ammonium acetate Drugs 0.000 claims 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 abstract description 12
- 238000001556 precipitation Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 239000003350 kerosene Substances 0.000 abstract description 4
- 235000006408 oxalic acid Nutrition 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000003916 acid precipitation Methods 0.000 abstract description 2
- 238000004945 emulsification Methods 0.000 abstract description 2
- 238000009854 hydrometallurgy Methods 0.000 abstract description 2
- 239000013064 chemical raw material Substances 0.000 abstract 1
- 239000008139 complexing agent Substances 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- 239000003112 inhibitor Substances 0.000 abstract 1
- 239000012747 synergistic agent Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- OXIKLRTYAYRAOE-CMDGGOBGSA-N (e)-3-(1-benzyl-3-pyridin-3-ylpyrazol-4-yl)prop-2-enoic acid Chemical compound N1=C(C=2C=NC=CC=2)C(/C=C/C(=O)O)=CN1CC1=CC=CC=C1 OXIKLRTYAYRAOE-CMDGGOBGSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 235000015165 citric acid Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004176 ammonification Methods 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- -1 rare-earth chloride Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
Classifications
-
- 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
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- Manufacture And Refinement Of Metals (AREA)
Abstract
A method for extracting rare earth oxide from rare earth ore mother liquor by using naphthenic acid centrifugal extraction method belongs to the field of hydrometallurgy. The present invention adopts the method of mixing high-effective ammonia complexing agent, synergistic agent and extraction inhibitor in naphthenic acid-kerosene extraction system, and utilizes centrifugal extraction technology to overcome the problems of organic phase emulsification loss, etc. compared with conventional oxalic acid precipitation method, it omits the procedures of precipitation, firing, acid dissolution and impurity-removing, and its technological process is simple and continuous, and can save chemical raw material and energy source, reduce environmental pollution, and its rare earth yield is high.
Description
Naphthenic acid (HA) centrifugal extraction method extracts the method for rare earth oxide (REO) concentrated solution from the rare-earth mineral mother liquor, belong to the hydrometallurgy field.
The ion type rareearth ore in sand form soaks ore deposit mother liquor (containing REO 1-2 grams per liter) through ammonium sulfate leaching gained, operations such as molten through oxalic acid precipitation, calcination, acid usually, the removal of impurity obtain the extracting and separating that the thick product of mixed rare-earth oxide (REO) is used for the single rare earth oxide compound, because the harmful and contaminate environment of oxalic acid, relevant precipitation agent improvement has report more.Chinese patent 86100671 discloses the method with Ammonium bicarbonate food grade precipitating rare earth ore deposit mother liquor; 88100113 mixed precipitants that disclose bicarbonate of ammonia and ammonium chloride composition replace oxalic acid.As everyone knows, rare-earth separating generally adopts liquid-liquid technique at present, and naphthenic acid (HA) is as the existing many reports of the technology of the extraction agent of Y, La, Eu etc.
The objective of the invention is to ammonium sulfate leaching liquid to the ion type rareearth ore in sand form without precipitation, technical process such as calcination, acid are molten, the removal of impurity directly obtain spissated RECl with naphthenic acid Centrifugical extraction mother liquor and hydrochloric acid reextraction
3Liquid (containing REO 200-250 grams per liter).This liquid can be directly used in extraction tank and carry out that single rare earth separates or grouping, thereby can realize serialization, automatization, also simplified operation, saves the chemical materials and the energy greatly, has improved labour intensity and has reduced environmental pollution.
The present invention adopts and mixes with multiple-effect ammonia composite additive in naphthenic acid-kerosene extraction system (hereinafter to be referred as organic phase), by the Centrifugical extraction technology, the compound action effect of performance additive has overcome the problems such as emulsification loss of organic phase, reach branch lover and the high effect of extraction efficiency, saved in the conventional extraction that organic phase is given first ammonification and mother liquor gives operations such as the first removal of impurity.
Extracted organic phase consists of 30～40%HA-70～60% kerosene-0.1～0.5% hydroxamic acid or petrolenum sulfoxide among the present invention, the add-on of ammonia composite additive is calculated as 1-5% by REO, it specifically consists of the ammoniacal liquor of 7N, 10 grams per liter citric acids, 15 grams per liter ammonium acetates, 15 grams per liter sulfo group water acid, 25 grams per liter ammonium sulfate.Feed liquid is for containing REO1.0-1.2% grams per liter, P
HValue is the rare-earth mine sulfuric acid ammonium leaching mother liquor of 4-4.6, and composition and foreign matter content see Table 1.
Technology of the present invention is extracted organic phase to be gone into Xiang Kou (heavy liquid inlet) with ore deposit liquid mother liquor from another from the same Xiang Kou of going into (gently entering the mouth mutually) together with the ammonia recombiner flow into centrifugal extractor simultaneously, and its throughput ratio (or claiming to compare) is ore deposit liquid (Va): organic phase (Vo): ammonia composite additive (Vc) equals 8-15: 1: 0.03-0.05.Amount control balance water P with ammonia recombiner additive
HIn the 6.5-7.0 scope.One-stage centrifugal extraction, extraction can be greater than 97%, and cascade extraction also can improve the rate of getting, and load organic phases is used 6.0-7.0N HCL half countercurrent reextraction again through three grades of washings then, obtains containing the RECl of REO 200-250 grams per liter through 4-6 level and three grades of washings
3Solution (composition sees Table 1) can go up directly that extraction tank divides into groups or rare-earth separating.
The used rare-earth original ore sand of the present invention sees Table 1 through the composition of the leach liquor of ammonium sulfate infiltration.
The present invention has successfully solved first from low concentration of rare earth feed liquid (1.0-1.5 grams per liter) and has dragged for the also technical process problem of concentrated rare earth entirely with the naphthenic acid Centrifugical extraction.
Centrifugal extracting process of the present invention is only used Centrifugical extraction, hydrochloric acid back extraction two step main technique can obtain rare-earth chloride solution separates for the extraction grouping and uses, and the precipitation rule must → calcination → packing → acid air-dry molten through precipitation → clarification or filtration → pack → removal of impurity → filtration washing → RECl
3Nine step of batching operation just can obtain entering the RECl of segregation section
3Solution, this technology have that flow process is simple, serialization, step are few, save industrial chemicals and
The energy, minimizing environmental pollution, rare earth yield advantages of higher obtain tangible economic and social benefit, are applicable to all separation plant uses that rare-earth ore resource is arranged.
The advantage of technology of the present invention is that treatment capacity is big, the extraction efficiency height, and floor space is little, and by powerful centrifugal force and phase-splitting can overcome organic phase emulsive problem, the organic phase burden is little also to can be recycled.
Embodiments of the invention are as follows:
Embodiment 1:
Get Dingnan County's rare-earth mineral mother liquor, it is formed as table 1 sequence number 1, contains REO 1.0-1.2 grams per liter, P
H=4～4.6, adopt organic phase to consist of 30% naphthenic acid-0.5% hydroxamic acid-～70% kerosene, the ammonia composite additive is ammonia concn 7N, 10 grams per liter citric acids, 15 grams per liter ammonium acetates, 15 gram/sulfo group water acid, 25 grams per liter ammonium sulfate, continuous extraction in φ 85 centrifugal extractors, feed liquid adds from the heavy liquid inlet, and organic phase and mouthful adding on the lenient side mutually of ammonia composite additive are respectively by under meter and control valve monitoring and dominant discharge, 500 liters/hour of total fluxs are in a ratio of V
Have: V
Material=1: 10, control composite additive flow velocity makes balance outlet water P
HValue is 7.0, behind Centrifugical extraction, two-phase is flowed out by heavy phase and light phase export respectively, and aqueous phase extracted contains REO＜30 milligram after testing, percentage extraction is greater than 97%, load organic phases contains the about 12-14 grams per liter of REO, and load organic phases is through 3 grades of washings then, 4 grade of half adverse current 6.0NHCl back extraction, again through 3 grades of washings, organic phase recycles, and it is 250 grams per liters that strip liquor contains REO, and this strip liquor can be used as the raw material of the finished product Rare Earth Separation of the present invention factory.
Embodiment 2:
Get the rare-earth mineral mother liquor, it is formed as table 1 sequence number 2, and other technology is with embodiment 1.
Embodiment 3:
Except that adopting organic phase to consist of 40% naphthenic acid-0.1% hydroxamic acid-～60% kerosene other technology with embodiment 1 or 2.
Claims (3)
1, extracts the method for mixed rare-earth oxide from the ammonium sulfate leaching mother liquor of rare-earth mineral, the invention is characterized in and adopt naphthenic acid Centrifugical extraction mother liquor and hydrochloric acid reverse-extraction method to obtain spissated mixed rare-earth oxide liquid.
2, as the described Centrifugical extraction method of claim 1, it is characterized in that with 30-40% naphthenic acid-70～60% kerosene-0.1～0.5% hydroxamic acid be extracted organic phase, add the ammonia composite additive; Feed liquid is for containing rare earth oxide 1.0～1.2 grams per liters, P
HValue is 4～4.6 rare earth sulfuric acid ammonium leaching mother liquor, the extraction have camera with the ammonia recombiner together from the same Xiang Kou of going into, feed liquid is gone into mutually from another, and mouth flows into centrifugal extractor together simultaneously, its throughput ratio or title are in a ratio of: ore deposit liquid (Va): organic phase (Vo): ammonia composite additive (Vc) is 8-15: 1: 0.03～0.05, and with the amount control balance water P of ammonia composite additive
HIn the 6.5-7.0 scope, through single-stage or tandem Centrifugical extraction, load organic phases is used 6.0-7.0N HCl half countercurrent reextraction then through three grades of washings, obtains containing the RECl of REO200-250g/l through 4-6 level and three grades of washings
3Solution.
3, method according to claim 2 is characterized in that described ammonia composite additive is the ammoniacal liquor of 7N, the citric acid of 10 grams per liters, the ammonium acetate of 15 grams per liters, the sulfo group water acid of 15 grams per liters, the ammonium sulfate of 25 grams per liters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90107128A CN1029630C (en) | 1990-08-15 | 1990-08-15 | Centrifugal extraction process of rare earth ore mother liquor from naphthenic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90107128A CN1029630C (en) | 1990-08-15 | 1990-08-15 | Centrifugal extraction process of rare earth ore mother liquor from naphthenic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1058995A true CN1058995A (en) | 1992-02-26 |
| CN1029630C CN1029630C (en) | 1995-08-30 |
Family
ID=4880412
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN90107128A Expired - Fee Related CN1029630C (en) | 1990-08-15 | 1990-08-15 | Centrifugal extraction process of rare earth ore mother liquor from naphthenic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1029630C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824535B (en) * | 2009-03-03 | 2012-11-14 | 北京有色金属研究总院 | Process for gathering trace rare earth from phosphoric acid by using centrifugal extracting equipment |
| CN103773955A (en) * | 2013-11-04 | 2014-05-07 | 中铝广西有色金源稀土股份有限公司 | Method for removing aluminium in tombarthite feed liquid |
| CN105803207A (en) * | 2016-04-11 | 2016-07-27 | 河南师范大学 | Recycling and reusing method for Bayer process red mud |
| CN106521194A (en) * | 2016-11-14 | 2017-03-22 | 贵州大学 | Extraction agent used for extracting rare earth through emulsion liquid membrane and using method thereof |
| CN109680166A (en) * | 2017-10-19 | 2019-04-26 | 厦门稀土材料研究所 | A kind of technique that centrifugal extraction method leaches recovering rare earth in mother liquor from ion type rareearth ore |
-
1990
- 1990-08-15 CN CN90107128A patent/CN1029630C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824535B (en) * | 2009-03-03 | 2012-11-14 | 北京有色金属研究总院 | Process for gathering trace rare earth from phosphoric acid by using centrifugal extracting equipment |
| CN103773955A (en) * | 2013-11-04 | 2014-05-07 | 中铝广西有色金源稀土股份有限公司 | Method for removing aluminium in tombarthite feed liquid |
| CN103773955B (en) * | 2013-11-04 | 2016-08-31 | 中铝广西有色金源稀土股份有限公司 | A kind of remove the method for aluminium in rare earth feed liquid |
| CN105803207A (en) * | 2016-04-11 | 2016-07-27 | 河南师范大学 | Recycling and reusing method for Bayer process red mud |
| CN105803207B (en) * | 2016-04-11 | 2018-06-26 | 河南师范大学 | A kind of recycling reuse method of Bayer process red mud |
| CN106521194A (en) * | 2016-11-14 | 2017-03-22 | 贵州大学 | Extraction agent used for extracting rare earth through emulsion liquid membrane and using method thereof |
| CN106521194B (en) * | 2016-11-14 | 2018-09-07 | 贵州大学 | A kind of extractant and its application method for emulsion liquid membrane extracting rare earth |
| CN109680166A (en) * | 2017-10-19 | 2019-04-26 | 厦门稀土材料研究所 | A kind of technique that centrifugal extraction method leaches recovering rare earth in mother liquor from ion type rareearth ore |
| CN109680166B (en) * | 2017-10-19 | 2021-05-18 | 厦门稀土材料研究所 | Process for recovering rare earth from ionic rare earth ore leaching mother liquor by centrifugal extraction method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1029630C (en) | 1995-08-30 |
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