CN110106355A - The method of microemulsion extracting gold based on microreactor - Google Patents
The method of microemulsion extracting gold based on microreactor Download PDFInfo
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- CN110106355A CN110106355A CN201910411559.6A CN201910411559A CN110106355A CN 110106355 A CN110106355 A CN 110106355A CN 201910411559 A CN201910411559 A CN 201910411559A CN 110106355 A CN110106355 A CN 110106355A
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- microemulsion
- microreactor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/40—Mixtures
- C22B3/406—Mixtures at least one compound thereof being a heterocyclic compound
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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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- Environmental & Geological Engineering (AREA)
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Abstract
A method of the microemulsion extracting gold based on microreactor, using microemulsion as extraction phase, using the acid solution containing gold as being extracted phase, the two, which is placed in microreactor, completes gold from water phase to the transmitting of micro emulsion liquid phase, obtained micro emulsion liquid phase is stripped with thiocarbamide again, gold is set to realize the purification of gold from micro emulsion liquid phase to water phase, and the micro emulsion liquid phase after back extraction is carried out washing to reuse；Present invention incorporates the technical advantages of microreactor and microemulsion, in which: microreactor has the advantages that biggish specific surface area, mixing efficiency are high, mass transfer velocity is fast and safe operation；Preparation method is simple for microemulsion, and has superior extraction ability and selectivity for gold ion, and extraction time is short, mass tranfer coefficient is high, and hydrophilic ionic-liquid can be reused as extractant.The two combines, it is ensured that under the premise of safety in production, the efficiency of extracting gold is improved with lower energy consumption.
Description
Technical field
The present invention relates to a kind of isolation technics of chemical field, specifically a kind of microemulsion extraction based on microreactor
The method for taking gold.
Background technique
Noble metal has huge practical application value in various fields such as jewelry, hyundai electronics and medicine, from ore and
Extract gold in electronic waste and be increasingly becoming the project to merit attention, but environmental pollution caused by its extraction process and compared with
High energy consumption is still the challenge in golden removal process.There are organic solvent consumptions for the abstraction technique of existing gold greatly, extraction
The defect for taking time length, extractant that cannot be recycled.
Summary of the invention
The present invention is directed to the limitation and defect of the prior art, proposes a kind of side of microemulsion extracting gold based on microreactor
Method improves the efficiency of gold extraction with lower energy consumption, in which: micro- reaction in conjunction with the technical advantage of microreactor and microemulsion
Device has the advantages that biggish specific surface area, mixing efficiency are high, mass transfer velocity is fast and safe operation, and uses microemulsion extractor body
System can reduce the loss of hydrophilic ionic-liquid, the recycling of facilitated extraction agent and the quick separating of target product.
The present invention is achieved by the following technical solutions:
The present invention is placed in micro- reaction as phase, the two is extracted using microemulsion as extraction phase, using the acid solution containing gold
Gold is completed in device to be stripped obtained micro emulsion liquid phase from water phase to the transmitting of micro emulsion liquid phase, then with thiocarbamide, makes Jin Congwei
Lotion mutually arrives the purification that water phase realizes gold, and the micro emulsion liquid phase after back extraction wash and can be reused.
The microreactor includes: T-type threeway and the capillary microchannels that are attached thereto, in which: two of T-type threeway
Input terminal inputs microemulsion and the acid solution containing gold respectively, and the output end of capillary microchannels is connected with separatory funnel.
The internal diameter of the capillary microchannels is 0.25~6mm, using PFA, PTFE material.
Flow rate of liquid control is preferably 0.2~2.4mL/min by capillary microchannels one end connecting fluid pump.
The acid solution is hydrochloric acid solution of the concentration in 0.5~3.0mol/L.
The concentration of the thiocarbamide is 0.1mol/L.
The preparation method of the microemulsion specifically includes the following steps:
1) cyclohexane solution as organic phase is added using cetylpyridinium chloride ionic liquid as surfactant
In, add the n-hexyl alcohol as cosurfactant；
2) solution for obtaining step 1) is placed in supersonic cleaning machine and the hydrochloric acid that concentration is 0.1mol/L is added dropwise, until solution
From it is transparent become muddiness when stop being added dropwise；
3) transparent uniform microemulsion will be formed after the product ultrasound 5min of step 2), then microemulsion is placed in a centrifuge
It is centrifuged 5min, non-split-phase.
The volume ratio of the n-hexyl alcohol and hexamethylene is 3:7.
The concentration of the cetylpyridinium chloride ionic liquid is 1.47 × 10-3~10.73 × 10-3mol/L。
Technical effect
Compared with prior art, the present invention has higher selectivity to be superior to iron, copper, nickel, aluminum metal fitting；Compared with Gao Cui
Efficiency is taken to can achieve 99.2%, extraction time is as short as 14.7s；The microemulsion phase that hydrophilic ionic-liquid is constructed can repeat benefit
With.
Detailed description of the invention
Fig. 1 is influence schematic diagram of the concentration of hydrochloric acid to microemulsion extracting gold in microreactor；
In figure: a is the schematic diagram influenced with the raising of concentration of hydrochloric acid on the extraction efficiency of gold；B is various metals ion
The comparison diagram of extraction efficiency；
Fig. 2 is influence schematic diagram of the ionic liquid concentration to microemulsion extracting gold in microreactor；
Fig. 3 is that influence of the residence time to the extraction efficiency and mass tranfer coefficient of microemulsion extracting gold in microreactor is illustrated
Figure；
Fig. 4 is the structural schematic diagram of embodiment device；
In figure: 1 syringe, 2 micro-injection pumps, 3T type micro-mixer, 4 capillary microchannels, 5 waters bath with thermostatic control, 6 liquid separations leakage
Bucket.
Specific embodiment
Embodiment 1
The present embodiment is controlled temperature at 25 DEG C using water bath with thermostatic control, microemulsion as extraction phase, with gold ion, iron from
Son, copper ion or its hybrid ionic include gold ion, iron ion, copper ion, nickel ion, aluminum ions acid solution as being extracted
Phase is taken, the two, which is injected into microreactor, completes metal from water phase to the transmitting of micro emulsion liquid phase.
The microreactor includes: T-type threeway and the capillary microchannels that are attached thereto, wherein T-type threeway and capillary
Pipe microchannel is connected through a screw thread.
The section stream operating range of the capillary microchannels, drop stream operating range flow velocity are respectively 0.2~1.6mL/
Min, 1.6~2.4mL/min.
The T-type threeway uses PEEK material, internal diameter 0.5mm.
The internal diameter of the capillary microchannels is 0.5mm, length 15cm, using PFA material.
The inside of the capillary microchannels is equipped with fluid pump, and flow rate of liquid is controlled as 0.8mL/min.
The preparation method of the microemulsion specifically includes the following steps:
1) being added to be used as surfactant for 0.0067mol/L cetylpyridinium chloride ionic liquid using concentration has
In the cyclohexane solution of machine phase, the n-hexyl alcohol as cosurfactant is added；
2) solution for obtaining step 1) is placed in supersonic cleaning machine and the hydrochloric acid that concentration is 0.1mol/L is added dropwise, until solution
From it is transparent become muddiness when stop being added dropwise；
3) transparent uniform microemulsion will be formed after the product ultrasound 5min of step 2), then microemulsion is placed in a centrifuge
It is centrifuged 5min, non-split-phase.
The volume ratio of the n-hexyl alcohol and hexamethylene is 3:7.
The concentration of golden concentration and other metals is 1.94 × 10 in the acid solution containing gold-3mol/L。
The water phase of the metal ion and the volume ratio of micro emulsion liquid phase are 1.0.
The acid solution is hydrochloric acid solution of the concentration in 0.5~3.0mol/L.
Gold ion in the water phase measures concentration using ultraviolet specrophotometer (UV-VIS), other metal ions are adopted
Concentration is measured with inductive coupling plasma emission spectrograph (ICP-OES).
The calculation formula of the extraction yield of the gold are as follows:Wherein: Caq,initTo extract preceding water phase
The initial concentration of gold, Caq,outFor the concentration of water phase gold after extraction.
As shown in Figure 1a, influence of the hydrochloric acid to the extraction efficiency of gold is smaller, although higher concentration of hydrochloric acid is help to obtain
The extraction yield of higher gold, but biggish acidity can cause to corrode to equipment.Meanwhile it determining at identical conditions single
The extraction efficiency of metallic iron and copper, discovery is with the variation of concentration of hydrochloric acid, and the extraction efficiency of iron and copper is almost without changing.
As shown in Figure 1 b, microemulsion verifies golden extraction selectivity, i.e., by gold ion and nickel ion, copper from
Son, iron ion and aluminium ion are mixed, and together as phase is extracted, are extracted by microemulsion, and the extraction of gold is calculated
Rate is 99.2%, and the extraction yield of nickel is 7.8%, and the extraction yield of iron is 3.3%, and the extraction yield of copper is 0.30%, the extraction yield of aluminium
It is 0.10%.It follows that extraction system of the invention has excellent extraction efficiency and selectivity to fitting.
Embodiment 2
Compared with Example 1, the concentration of the cetylpyridinium chloride ionic liquid of the present embodiment be respectively 0.00147,
0.00378,0.0067,0.0084,0.01073mol/L, golden concentration are 1.94 × 10-3Mol/L, flow rate of liquid control are
0.8mL/min, the internal diameter of pipe are 0.5mm, length 15cm.
As shown in Fig. 2, with the increase of ionic liquid concentration, golden extraction yield is gradually increased, when the concentration of ionic liquid
When for 0.0067mol/L, golden extraction yield reaches maximum, is further added by the concentration of ionic liquid, golden extraction efficiency remains unchanged.
Therefore, the concentration of ionic liquid is selected as 0.0067mol/L.
Embodiment 3
Compared with Example 1, the extraction phase in capillary microchannels is by the present embodiment with the flow control for being extracted phase
0.1mL/min, golden concentration are 1.94 × 10-3Mol/L, the internal diameter of pipeline are 0.5mm, capillary channel length is respectively 2.5,5,
10,15,20,25,30cm, the concentration of ionic liquid are 0.0067mol/L.
As shown in figure 3, golden extraction yield becomes larger with the extension of residence time.When the residence time is 14.7s,
The extraction yield of gold reaches maximum value 99.2%.Calculating gold constant interval of the volume transmission quality coefficient of extractor in extraction process is
0.33-2.9s-1, compared to other extraction systems, microemulsion extracting gold can obtain bigger volumetric mass transfer system in microreactor
Number.
The calculation formula of the volume transmission quality coefficient are as follows:Wherein: Caq,initBefore extraction
Water phase gold, Caq,outFor extraction after water phase gold concentration,For the concentration in water phase when gold balance.
Above-mentioned specific implementation can by those skilled in the art under the premise of without departing substantially from the principle of the invention and objective with difference
Mode carry out local directed complete set to it, protection scope of the present invention is subject to claims and not by above-mentioned specific implementation institute
Limit, each implementation within its scope is by the constraint of the present invention.
Claims (8)
1. a kind of method of the microemulsion extracting gold based on microreactor, which is characterized in that using microemulsion as extraction phase, will contain
For the acid solution of gold as phase is extracted, the two, which is placed in microreactor, completes gold from water phase to the transmitting of micro emulsion liquid phase, then uses
Thiocarbamide is stripped obtained micro emulsion liquid phase, so that gold is realized the purification of gold from micro emulsion liquid phase to water phase, and will be after back extraction
Micro emulsion liquid phase carry out washing can reuse；
The microreactor includes: T-type threeway and the capillary microchannels that are attached thereto, in which: two inputs of T-type threeway
End inputs microemulsion and the acid solution containing gold respectively.
2. the method for the microemulsion extracting gold according to claim 1 based on microreactor, characterized in that the micro emulsion
The preparation method of liquid specifically includes the following steps:
1) it is added cetylpyridinium chloride ionic liquid as surfactant as in the cyclohexane solution of organic phase, then
The n-hexyl alcohol as cosurfactant is added；
2) solution for obtaining step 1) is placed in supersonic cleaning machine and the hydrochloric acid that concentration is 0.1mol/L is added dropwise, until solution is by saturating
It is bright to become stopping being added dropwise when muddiness；
3) transparent uniform microemulsion will be formed after the product ultrasound 5min of step 2), then microemulsion is placed in a centrifuge centrifugation
5min, non-split-phase.
3. the method for the microemulsion extracting gold according to claim 2 based on microreactor, characterized in that it is described just oneself
The volume ratio of alcohol and hexamethylene is 3:7.
4. the method for the microemulsion extracting gold according to claim 2 based on microreactor, characterized in that the chlorination
The concentration of cetyl pyridinium ionic liquid is 1.47 × 10-3~10.73 × 10-3mol/L。
5. the method for the microemulsion extracting gold according to claim 1 based on microreactor, characterized in that the acidity
Solution is hydrochloric acid solution of the concentration in 0.5~3.0mol/L.
6. the method for the microemulsion extracting gold according to claim 1 based on microreactor, characterized in that the thiocarbamide
Concentration be 0.1mol/L.
7. the method for the microemulsion extracting gold according to claim 1 based on microreactor, characterized in that the capillary
The internal diameter of pipe microchannel is 0.25~6mm；The inside of capillary microchannels be equipped with fluid pump with control flow rate of liquid be 0.2~
2.4mL/min。
8. the method for the microemulsion extracting gold according to claim 1 or claim 7 based on microreactor, characterized in that described
The section stream operating range of capillary microchannels, drop stream operating range flow velocity are respectively 0.2~1.6mL/min, 1.6~2.4mL/
min。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113392596A (en) * | 2021-04-25 | 2021-09-14 | 四川大学 | Method for extracting and separating scandium-iron solution by using microchannel reactor |
| CN115305359A (en) * | 2022-08-23 | 2022-11-08 | 成都先进金属材料产业技术研究院股份有限公司 | Method for selectively extracting copper from sulfur-cobalt concentrate leaching solution based on microemulsion |
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| WO2007076392A2 (en) * | 2005-12-22 | 2007-07-05 | Shell Oil Company | A method for reusing rhenium from a donor spent epoxidation catalyst |
| CN103882231A (en) * | 2014-02-21 | 2014-06-25 | 周千里 | Method for extracting gold from electronic wastes by using novel microemulsion |
| CN107841623A (en) * | 2017-10-20 | 2018-03-27 | 昆明理工大学 | It is a kind of using micro-fluidic technologies from nickel and cobalt solution extract and separate manganese, zinc method |
-
2019
- 2019-05-17 CN CN201910411559.6A patent/CN110106355A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007076392A2 (en) * | 2005-12-22 | 2007-07-05 | Shell Oil Company | A method for reusing rhenium from a donor spent epoxidation catalyst |
| CN103882231A (en) * | 2014-02-21 | 2014-06-25 | 周千里 | Method for extracting gold from electronic wastes by using novel microemulsion |
| CN107841623A (en) * | 2017-10-20 | 2018-03-27 | 昆明理工大学 | It is a kind of using micro-fluidic technologies from nickel and cobalt solution extract and separate manganese, zinc method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113392596A (en) * | 2021-04-25 | 2021-09-14 | 四川大学 | Method for extracting and separating scandium-iron solution by using microchannel reactor |
| CN115305359A (en) * | 2022-08-23 | 2022-11-08 | 成都先进金属材料产业技术研究院股份有限公司 | Method for selectively extracting copper from sulfur-cobalt concentrate leaching solution based on microemulsion |
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Application publication date: 20190809 |
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