CN105112658A - Method for extracting rare-earth elements through micro channels - Google Patents
Method for extracting rare-earth elements through micro channels Download PDFInfo
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- CN105112658A CN105112658A CN201510538000.1A CN201510538000A CN105112658A CN 105112658 A CN105112658 A CN 105112658A CN 201510538000 A CN201510538000 A CN 201510538000A CN 105112658 A CN105112658 A CN 105112658A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 53
- 239000012074 organic phase Substances 0.000 claims abstract description 44
- 239000012071 phase Substances 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 150000003839 salts Chemical class 0.000 claims description 24
- 239000008346 aqueous phase Substances 0.000 claims description 21
- 238000007127 saponification reaction Methods 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- -1 rare earth nitrate salts Chemical class 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- 239000003085 diluting agent Substances 0.000 abstract 1
- 238000009854 hydrometallurgy Methods 0.000 abstract 1
- 230000005501 phase interface Effects 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005272 metallurgy Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004148 unit process Methods 0.000 description 1
Classifications
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- 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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- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a method for extracting rare-earth elements through micro channels, and belongs to the technical field of hydrometallurgy. The method comprises the steps that firstly, P507 or P204 is added into 260# solvent oil diluents according to the volume ratio of 3:10-10:3 to obtain an organic phase; a rare-earth salt solution serves as a water phase; the organic phase and the water phase are subjected to normal-temperature extraction through the micro channels in a microreactor according to the phase ratio of 5:1-1:5 and at the volume flowing speed of 5.55*10-10-4.17*10-8 m<3>/s; and finally, an extraction phase containing rare-earth elements and raffinate are obtained. In combination with the advantages that the micro channels are high in specific interfacial area, high in mass transfer rate, short in response time and the like, the purpose of achieving high-efficiency rare-earth extraction is realized through contact of two phase interfaces in the micro channels, and the method is safe, efficient and low in consumption.
Description
Technical field
The present invention relates to the method for a kind of microchannel extracting rare-earth element, belong to technical field of wet metallurgy.
Background technology
China's rare earth resources is very abundant, and not only reserves are large, account for first place, the world, and great variety of goods; Simultaneously rare earth element metallurgy, glass, pottery, chemical industry, nuclear industry, electronic industry, agricultural and medical in all have a wide range of applications.Mainly adopt solvent extration, ion-exchange chromatography, extracting resin chromatography etc. in current rare-earth extraction separating process, wherein solvent extration is widely used.Mixing-clarifying tank is extraction equipment the most frequently used in solvent extraction, there is the shortcomings such as mixing time is long, floor space is large, security is low, energy consumption is high.
Micro passage reaction, refers to a kind of by means of special micro-processing technology, and the mean sizes of inside unit structure width is at micron order, and be the fluid channel of tens to hundreds of micron usually containing equivalent diameter, overall dimensions is then at centimetre scale.The principle of its extracting metals ion is the concentration gradient that specific interfacial area that microreactor is higher can strengthen object element in two-phase, extraction impellent is caused greatly to improve, mass-transfer efficiency improves an order of magnitude than traditional operation, two-phase carries out rapid mass transfer by the contact of short period of time, and then enhance metallurgical operations unit process, raise the efficiency, shorten extraction time and reduce energy consumption.
In recent years, the technology of microminiaturized extraction mass transfer rig reaches its maturity, microchannel extraction mass transfer apparatus can increase mass transfer area because of it, shorten the residence time, improve mass-transfer performance, overcome a lot of problems in traditional rare earth extraction process, if be applied in rare earth extraction field, there is good development prospect.
Summary of the invention
The present invention is directed to the problems such as extraction equipment in conventional solvent extraction exists that mixing time is long, floor space is large, security is low and energy consumption is high, propose the method for a kind of microchannel extracting rare-earth element.The advantages such as the present invention is high in conjunction with microchannel specific interfacial area, rate of mass transfer is fast, the time of response is short, the target of efficient extracting rare-earth is realized by two-phase interface contact in microchannel, be a kind of method of safe, efficient, low consumption, the present invention is achieved through the following technical solutions.
A method for microchannel extracting rare-earth element, its concrete steps are as follows:
(1) be first add 260 at 3: 10 ~ 10: 3 by P507 or P204 according to volume ratio
#solvent oil thinner obtains organic phase;
(2) using rare earths salt as aqueous phase, by the organic phase of step (1) and aqueous phase according to being in a ratio of 5:1 ~ 1:5, with 5.55 × 10
-10~ 4.17 × 10
-8m
3the volumetric flow rate of/s carries out normal temperature extraction in the microchannel of microreactor, and final acquisition contains rare earth element extraction phase and raffinate.
In described step (1), organic phase is sponifiable or non-saponified, according to saponification organic phase, and its saponification deg scope 0 ~ 80%.
Described step (2) middle-weight rare earths salts solution is chlorination, sulfuric acid or rare earth nitrate salts solution, and the concentration of rare earths salt is 0.001 ~ 0.5mol/L, and adjusting pH with acid or alkali in rare earths salt is 1 ~ 5.
In described step (2), the microchannel of microreactor is biparting shape, single rectangle, interdigital, circle or double square cross section, biparting shape, single rectangle, double square characteristic dimension wide (w) are 50 ~ 1000 μm, length (L) is 40 ~ 480mm, and highly (h) is 40 ~ 120 μm.
In described step (2), microchannel can be the parallel combination of multiple microchannel, improves the treatment capacity of microchannel with this; And the microfluid combination after parallel connection can be connected, improve extracting and separating coefficient and Purity of Rare Earth.
The invention has the beneficial effects as follows:
(1) microchannel of the present invention extracting rare-earth has the advantage that the two-phase residence time is short, occupation area of equipment is little.
(2) the present invention adopts microchannel high-efficiency extracting rare-earth, and the reaction times shortens to level scope second, and single-stage extraction rate significantly improves, and decreases extraction progression.
(3) aqueous phase is contacted by two-phase interface with organic phase, avoids the emulsion that conventional extraction violent stirring causes.
(4) break through plant engineering by the mode increasing microchannel quantity in parallel, save the pilot scale time, shorten the equipment development cycle.
(5) microchannel extraction carries out in airtight micro-structured reactor, avoids organic phase and directly contact with air, improve the security of extraction process.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The method of this microchannel extracting rare-earth element, its concrete steps are as follows:
(1) be first add 260 at 10: 3 by P204 according to volume ratio
#solvent oil thinner obtains organic phase; Organic phase is saponification organic phase, carries out saponification with the NaOH of 3mol/L, and its saponification deg is 40%;
(2) using rare earths salt as aqueous phase, by the organic phase of step (1) and aqueous phase according to being in a ratio of 1:1, with 8.33 × 10
-10m
3the volumetric flow rate of/s is through microchannel (the biparting shape cross-section microchannel of Y-Y type of microreactor, wide 160 μm, high 40 μm, long 120mm) in carry out normal temperature extraction, final acquisition is containing rare earth element extraction phase and raffinate, and wherein rare earths salt is the LaCl of 0.2mol/L
3solution, adopts the pH to 4 of dilute hydrochloric acid adjustment solution.
In the present embodiment, La percentage extraction can reach 99.76%, and the extraction equilibrium time is 0.37s.
Embodiment 2
The method of this microchannel extracting rare-earth element, its concrete steps are as follows:
(1) be first add 260 at 3: 10 by P204 according to volume ratio
#solvent oil thinner obtains organic phase; Organic phase is saponification organic phase, carries out saponification with the NaOH of 3mol/L, and its saponification deg is 60%;
(2) using rare earths salt as aqueous phase, by the organic phase of step (1) and aqueous phase according to being in a ratio of 1:1, with 5.55 × 10
-10m
3the volumetric flow rate of/s carries out normal temperature extraction in the microchannel (Y type Rectangular Microchannel, wide 100 μm, high 120 μm, long 200mm) of microreactor, finally obtains containing rare earth element extraction phase and raffinate, and wherein rare earths salt is the NdCl of 0.001mol/L
3solution, adopts the pH to 3 of dilute hydrochloric acid adjustment solution.
In the present embodiment, Nd percentage extraction can reach 99.82%, and extraction equilibrium starting time is 1.5s.
Embodiment 3
The method of this microchannel extracting rare-earth element, its concrete steps are as follows:
(1) be first add 260 at 8: 3 by P507 according to volume ratio
#solvent oil thinner obtains organic phase; Organic phase is non-saponified organic phase;
(2) using rare earths salt as aqueous phase, by the organic phase of step (1) and aqueous phase according to being in a ratio of 2:1, with 8.33 × 10
-9m
3the volumetric flow rate of/s carries out normal temperature extraction in the microchannel (interdigital microchannel) of microreactor, and final acquisition contains rare earth element extraction phase and raffinate, and wherein rare earths salt is the Eu (NO of 0.5mol/L
3)
3solution, adopts the pH to 2 of dilute hydrochloric acid adjustment solution.
In the present embodiment, Eu percentage extraction can reach 99.10%, and the extraction equilibrium time is 1.87s.
Embodiment 4
The method of this microchannel extracting rare-earth element, its concrete steps are as follows:
(1) first P507 is added 260 according to volume ratio 7: 3
#solvent oil thinner obtains organic phase; Organic phase is non-saponified organic phase;
(2) using rare earths salt as aqueous phase, by the organic phase of step (1) and aqueous phase according to being in a ratio of 5:1, with 1.52 × 10
-9m
3the volumetric flow rate of/s carries out normal temperature extraction in the microchannel (Y type rectangular cross section microchannel, wide 250 μm, high 120 μm, long 240mm) of microreactor, finally obtains containing rare earth element extraction phase and raffinate, and wherein rare earths salt is the YCl of 0.3mol/L
3solution, adopts the pH to 2.5 of dilute hydrochloric acid adjustment solution.
In the present embodiment, Y percentage extraction can reach 99.23%, and the extraction equilibrium time is 0.79s.
Embodiment 5
The method of this microchannel extracting rare-earth element, its concrete steps are as follows:
(1) be first add 260 at 2: 1 by P507 according to volume ratio
#solvent oil thinner obtains organic phase; Organic phase is non-saponified organic phase;
(2) using rare earths salt as aqueous phase, by the organic phase of step (1) and aqueous phase according to being in a ratio of 3:1, with 4.17 × 10
-8m
3the volumetric flow rate of/s carries out normal temperature extraction in the microchannel (circular cross-section microchannel, diameter 300 μm, long 120mm) of microreactor, and final acquisition contains rare earth element extraction phase and raffinate, and wherein rare earths salt is the SmCl of 0.05mol/L
3solution, adopts the pH to 3 of dilute hydrochloric acid adjustment solution.
In the present embodiment, Sm percentage extraction can reach 98.76%, and the extraction equilibrium time is 1.06s.
Embodiment 6
The method of this microchannel extracting rare-earth element, its concrete steps are as follows:
(1) be first add 260 at 1: 1 by P507 according to volume ratio
#solvent oil thinner obtains organic phase; Organic phase is non-saponified organic phase;
(2) using rare earths salt as aqueous phase, by the organic phase of step (1) and aqueous phase according to being in a ratio of 4:1, with 7.28 × 10
-10m
3the volumetric flow rate of/s is through microchannel (the double square cross-section microchannel of microreactor, wide 170 μm, high 100 μm, long 80mm) in carry out normal temperature extraction, final acquisition is containing rare earth element extraction phase and raffinate, and wherein rare earths salt is the Er (NO of 0.1mol/L
3)
3solution, adopts the pH to 2 of dilute hydrochloric acid adjustment solution.
In the present embodiment, Er percentage extraction can reach 99.56%, and the extraction equilibrium time is 0.57s.
Embodiment 7
The method of this microchannel extracting rare-earth element, its concrete steps are as follows:
(1) be first add 260 at 4: 3 by P507 according to volume ratio
#solvent oil thinner obtains organic phase; Organic phase is non-saponified organic phase;
(2) using rare earths salt as aqueous phase, by the organic phase of step (1) and aqueous phase according to being in a ratio of 1:5, with 10 × 10
-9m
3the volumetric flow rate of/s is through microchannel (the double square cross-section microchannel of microreactor, wide 1000 μm, high 100 μm, long 480mm) in carry out normal temperature extraction, final acquisition is containing rare earth element extraction phase and raffinate, and wherein rare earths salt is the Er (NO of 0.001mol/L
3)
3solution, adopts the pH to 3 of dilute hydrochloric acid adjustment solution.
In the present embodiment, Er percentage extraction can reach 99.78%, and the extraction equilibrium time is 0.12s.
Embodiment 8
The method of this microchannel extracting rare-earth element, its concrete steps are as follows:
(1) be first add 260 at 8: 3 by P507 according to volume ratio
#solvent oil thinner obtains organic phase; Organic phase is non-saponified organic phase;
(2) using rare earths salt as aqueous phase, by the organic phase of step (1) and aqueous phase according to being in a ratio of 1:3, with 4.17 × 10
-8m
3the volumetric flow rate of/s is through microchannel (the double square cross-section microchannel of microreactor, wide 50 μm, high 100 μm, long 40mm) in carry out normal temperature extraction, final acquisition is containing rare earth element extraction phase and raffinate, and wherein rare earths salt is the Er (NO of 0.5mol/L
3)
3solution, adopts the pH to 2 of dilute hydrochloric acid adjustment solution.
In the present embodiment, Er percentage extraction can reach 99.63%, and the extraction equilibrium time is 0.34s.
Above the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (4)
1. a method for microchannel extracting rare-earth element, is characterized in that concrete steps are as follows:
(1) be first add 260 at 3: 10 ~ 10: 3 by P507 or P204 according to volume ratio
#solvent oil thinner obtains organic phase;
(2) using rare earths salt as aqueous phase, by the organic phase of step (1) and aqueous phase according to being in a ratio of 5: 1 ~ 1: 5, with 5.55 × 10
-10~ 4.17 × 10
-8m
3the volumetric flow rate of/s carries out normal temperature extraction in the microchannel of microreactor, and final acquisition contains rare earth element extraction phase and raffinate.
2. the method for microchannel according to claim 1 extracting rare-earth element, is characterized in that: in described step (1), organic phase is sponifiable or non-saponified, according to saponification organic phase, and its saponification deg scope 0 ~ 80%.
3. the method for microchannel according to claim 1 extracting rare-earth element, it is characterized in that: described step (2) middle-weight rare earths salts solution is chlorination, sulfuric acid or rare earth nitrate salts solution, the concentration of rare earths salt is 0.001 ~ 0.5mol/L, and adjusting pH with acid or alkali in rare earths salt is 1 ~ 5.
4. the method for microchannel according to claim 1 extracting rare-earth element, it is characterized in that: in described step (2), the microchannel of microreactor is biparting shape, single rectangle, interdigital, circle or double square cross section, biparting shape, single rectangle, double square characteristic dimension wide are 50 ~ 1000 μm, length is 40 ~ 480mm, is highly 40 ~ 120 μm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105732422A (en) * | 2016-04-15 | 2016-07-06 | 浙江大学 | Method for utilizing microchannel for extracting diacetylmonoxime in ammonium sulfate water solution |
| CN106214838A (en) * | 2016-07-20 | 2016-12-14 | 南京工业大学 | A kind of method utilizing microchannel extraction equipment to reclaim total flavonoids extract from vegetable polysaccharides Aqueous extracts |
| CN108359811A (en) * | 2018-03-07 | 2018-08-03 | 昆明理工大学 | A method of being stripped cobalt using micro-fluidic technologies |
| CN108654138A (en) * | 2017-04-01 | 2018-10-16 | 四川大学 | A kind of centrifugal force microfluid extraction equipment and its extracting process |
| CN114525418A (en) * | 2022-03-10 | 2022-05-24 | 福州大学 | Method for enhancing extraction of rare earth neodymium ions at high phase ratio by using series-connected pore throat microchannels |
| CN116251380A (en) * | 2023-03-16 | 2023-06-13 | 福州大学 | Extraction method for high-phase-ratio system |
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| CN101319275A (en) * | 2007-06-04 | 2008-12-10 | 北京有色金属研究总院 | Process for solvent extraction separation purification of rare earth element |
| CN103060559A (en) * | 2013-01-30 | 2013-04-24 | 昆明理工大学 | Microfluid extraction method for extracting and separating In, Fe and Zn |
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2015
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105732422A (en) * | 2016-04-15 | 2016-07-06 | 浙江大学 | Method for utilizing microchannel for extracting diacetylmonoxime in ammonium sulfate water solution |
| CN105732422B (en) * | 2016-04-15 | 2017-12-15 | 浙江大学 | The method that diacetylmonoxime in ammonium sulfate solution is extracted using microchannel |
| CN106214838A (en) * | 2016-07-20 | 2016-12-14 | 南京工业大学 | A kind of method utilizing microchannel extraction equipment to reclaim total flavonoids extract from vegetable polysaccharides Aqueous extracts |
| CN106214838B (en) * | 2016-07-20 | 2020-04-07 | 南京工业大学 | Method for recovering total flavone extract from plant polysaccharide water extract by using microchannel extraction device |
| CN108654138A (en) * | 2017-04-01 | 2018-10-16 | 四川大学 | A kind of centrifugal force microfluid extraction equipment and its extracting process |
| CN108654138B (en) * | 2017-04-01 | 2023-06-16 | 四川大学 | Centrifugal force micro-fluid extraction device and extraction method thereof |
| CN108359811A (en) * | 2018-03-07 | 2018-08-03 | 昆明理工大学 | A method of being stripped cobalt using micro-fluidic technologies |
| CN114525418A (en) * | 2022-03-10 | 2022-05-24 | 福州大学 | Method for enhancing extraction of rare earth neodymium ions at high phase ratio by using series-connected pore throat microchannels |
| CN114525418B (en) * | 2022-03-10 | 2023-10-03 | 福州大学 | Method for strengthening rare earth neodymium ion extraction under high phase ratio by utilizing serial pore throat micro-channel |
| CN116251380A (en) * | 2023-03-16 | 2023-06-13 | 福州大学 | Extraction method for high-phase-ratio system |
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