CN105714114A - Method for adsorbing enriched rare earth ions from low-concentration rare earth lixivium through fungus A-Fu03 thalli - Google Patents
Method for adsorbing enriched rare earth ions from low-concentration rare earth lixivium through fungus A-Fu03 thalli Download PDFInfo
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- CN105714114A CN105714114A CN201610265071.3A CN201610265071A CN105714114A CN 105714114 A CN105714114 A CN 105714114A CN 201610265071 A CN201610265071 A CN 201610265071A CN 105714114 A CN105714114 A CN 105714114A
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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
- C22B3/18—Extraction of metal compounds from ores or concentrates by wet processes with the aid of microorganisms or enzymes, e.g. bacteria or algae
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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
- C22B59/00—Obtaining rare earth metals
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Abstract
The invention relates to a fungus bacterial strain A-FuO3 which can remove metallurgical waste water from rare earth mines or recover rare earth elements from low-concentration rare earth lixivium. The fungus bacterial strain A-FuO3 disclosed by the invention is taxonomically named as Aspergillus oryzae. The fungus bacterial strain A-FuO3 disclosed by the invention is good in effect of adsorbing low-concentration rare earth ions, simple to operate, low in cost and easy to culture. Microorganisms as adsorbents can be regenerated and degraded, and are environmentally-friendly and pollution-free. The fungus bacterial strain A-FuO3 can be applied to reduce the waste water treatment cost, reduce the discharge of ammonia nitrogen, avoid the waste of rare earth resources, and facilitate the water purification and the soil remediation in mineral leaching regions, and is also adaptive to enriched rare earth in the low-concentration rare earth lixivium.
Description
Technical field
The present invention relates to technical field of rare-earth hydrometallurgy, particularly relate to microorganism adsorption enrichment rare earth from
The green extraction of son and Rare-earth Mine metallurgy waste water treatment new method, particularly relate to a kind of fungal bacterial strain
The method of A-Fu03 adsorption of Low Concentration Rare Earth Mine leachate Rare Earth Ion.
Background technology
According to its ion type feature of weathered superficial leaching rare-earth ore, China's ion type rareearth ore uses substantially
The ammonium sulfate leaching technology of ion exchange leaching rare earth.Along with rich ore is the leanest miscellaneous by preferential exploitation utilization
Changing, the problem that highlights brought is that rare earth leaching efficiency is low, and leachate rare earth concentration is more and more lower, foreign ion
Concentration increases, and follow-up leachate middle rare earth extracts and separating difficulty increases the most therewith.Carbon is used in producing at present
The acid hydrogen ammonium sedimentation method are from leachate Extraction of rare earth, owing to re dip solution rare earth concentration is the lowest, rare-earth precipitation rate
Low, rare-earth precipitation is incomplete, and mother liquor of precipitation of ammonium remaining rare earth, precipitant ammonium hydrogen carbonate consumption is excessive, substantial amounts of
The discharge of carbon ammonium precipitation mother solution causes mining area water system ammonia nitrogen to exceed standard, by rainwash and underground migration, infiltration
Enter soil and water body, polluted underground water source." the rare-earth industry pollutant emission standard " that country promulgates,
Ammonia nitrogen discharge is proposed high request, and wherein ammonia nitrogen concentration of emission limit value typically area is 50mg/L, and environment is quick
Sense area is 30mg/L.Therefore, low ammonia nitrogen Extraction of rare earth technology is newly asking of facing of rare-earth wet method Metallurgical Industry Development
Topic.The sedimentation method, because setting up on the basis of ammonia nitrogen, use " without depositing technology ", such as extraction, biological adsorption
The new techniques such as method, are the inevitable directions of Extraction of rare eart technology development.
" sedimentation method " and " non precipitating method " are had from weathered superficial leaching rare-earth ore leaching liquid Extraction of rare earth technology,
Sedimentation method Extraction of rare earth has oxalic acid precipitation rare-earth process, ammonium bicarbonate precipitation rare-earth process and precipitation-floatation
Deng, oxalate precipitation method lacks because oxalic acid cost is high, toxic, pollute environment, do not meet Green Chemistry extraction etc.
Point is the most gradually replaced by additive method.It is nontoxic that ammonium bicarbonate precipitation method has precipitation filtrates, rare-earth precipitation rate
Height, the advantage such as good in economic efficiency, but still suffer from the shortcomings such as high ammonia nitrogen discharge, face environmental conservation new challenge.
Precipitation precipitation-floatation there is also precipitant and the problem of environmental pollution of organic flotation agent.Non precipitating method is from wind
Change shell ion adsorption type rare earth ore leaching liquid Extraction of rare earth method and have leaching liquid direct extracting rare-earth method, leaching liquid ion
Exchange concentration method, leaching liquid liquid membrane enrichment rare-earth process and the microorganism adsorption method etc. involved by the application.
Many microorganisms can be adsorbed and enriched in metals ion from solution, is superior adsorbent.1949
Ruchhoft, C.C. propose biosorption process and remove the Pu239 in waste water.Mullen M.D is equal to 1989
Have studied Pseudomonas aerations the earliest to La3+Absorption, research shows, microorganism is to rare earth
There are good absorption property and accumulation ability.
Microorganism, as adsorbent, easily produces, and raw material sources are extensive, and adsorption capacity is big, and adsorption efficiency is high,
The rate of adsorption is fast, and ion selectivity is high, environmental friendliness, does not produce secondary pollution, and the pH operated and
Temperature range width (general pH is 3～9, and temperature is 4 DEG C～90 DEG C)；To weak solution (1～100mg/L)
High treating effect；Fund input is few, and running cost is low, uses " non precipitating method " of microorganism adsorption technology
From leachate Extraction of rare earth more efficiently, cheap, environmental protection.
Summary of the invention
The present invention provides a kind of raw material sources extensive, and environmental friendliness does not produce secondary pollution, to weak solution
High treating effect, fund input is few, the preparation of the microbial adsorbent of low cost and adsorption of Low Concentration rare earth thereof
The method of solution Rare Earth Ion, technique is as shown in Figure 1.
The preparation process of this microbial adsorbent is: first trained at special liquid by one fungus strain A-Fu03
Support and base cultivated some skies continuously, in centrifuge solid-liquid separation or in filter cloth sedimentation filtration, bacterium will be leached
Body washing, to pure, be stored in less than 4 DEG C refrigerators, obtain microbial adsorbent.Recycle this micro-life
Thing adsorbent low concentration of rare earth leachate Rare Earth Ion.Specifically include following step:
(1) feed liquid detection: low concentration mischmetal feed liquid is carried out rare earth ion concentration detection, uses EDTA
Volumetric method titrimetry rare earth concentration；Remaining rare earth spectrophotometry in remaining liquid after absorption.
(2) culture medium preparation: take peeled potatoes, be cut into small pieces, adds water boil half an hour, the coldest after use
Double gauze filters, and then supplies dehydration to the most volume required, 121 DEG C of sterilizing 20min, 20% Ma Ling
Potato leaching juice.During preparation, add 2g glucose by every 100ml Rhizoma Solani tuber osi leaching juice, continue heating and melting and mend
Foot dehydration.With conical flask subpackage, jump a queue, wrap up.After high pressure steam sterilization, calorstat is dried, then uses
Ultraviolet irradiates further sterilizing in 20 minutes.
(3) inoculation: by strain Aspergillus oryzae Aspergillus oryzae in aseptic superclean bench
Sp.A-Fu03 is inoculated in step (2) in the Rhizoma Solani tuber osi fluid medium of gained.
(4) cultivate: be vaccinated with strain Aspergillus oryzae Aspergillus oryzae by what step (3) obtained
The conical flask of the potato culture of sp.A-Fu03, after cultivating certain time in constant-temperature shaking incubator,
Thalline is collected in centrifugal filtration, and properly preserves.
(5) absorption: the microbial cells that employing step (2) prepares is as adsorbent, to step (1)
Rare earth ion in the low concentration of rare earth solution of preparation adsorbs.It is specially and throws in low concentration of rare earth solution
Add a certain proportion of microbial adsorbent, in certain temperature range, concussion absorption certain time, use light splitting
Photometer measures rare earth ion concentration before and after absorption respectively, calculates the absorption of adsorbance q Unit Weight thalline
Amount (mg/g) and adsorption rate R (%).
(6) use strippant that the microbial adsorbent after absorption rare earth is carried out desorbing.
In described step (1), low concentration mischmetal leachate rare earth concentration scope 0.1～0.5g/L, acidity
It is 5-7 for pH.
In described step (2), medium component is: Rhizoma Solani tuber osi 20g；Glucose 2g；Water 100mL；Natural pH
Value.
The preparation of the absorption thalline of above-mentioned steps (4): by strain Aspergillus oryzae Aspergillus oryzae
Sp.A-Fu03 is inoculated into amplification culture in potato culture (PDA) fluid medium, and shaking table temperature is arranged
Being 30 DEG C, rotating speed is set to 150rpm, after cultivating 2-3 days continuously, 8000rpm be centrifuged 5min (or
Filter paper filtering) collect thalline, it is washed with deionized 3 times, claims weight in wet base, and save backup in 4 DEG C of refrigerators.
Fig. 2 is thalline micro-image.
In above-mentioned steps (5), it is 0.5～1g/L for (in terms of dry weight, mg) that optimal thalline adds ratio, 30 DEG C,
150rpm shaking table vibration absorption 2h, after absorption, 4000rpm is centrifuged 10min (or directly with filter paper filtering), uses
The rare earth ion concentration of residual in spectrophotometry supernatant.
By the thalline having adsorbed a certain amount of rare earth ion collected by above-mentioned steps (5), use 0.5-1M HCl respectively
After 200rpm vibration desorbing 2h, filter, measure the rare earth ion concentration of enrichment in filtrate with EDTA,
To rare earth ion enriched products, calculate desorption efficiency.
Accompanying drawing explanation
Fig. 1 is from low concentration of rare earth leachate adsorption and enrichment rare-earth process flow chart.Fig. 2 is through expanding training
The aspergillus oryzae Aspergillus oryzae sp.A-Fu03 mycelium microgram supported.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, but is not intended to protection scope of the present invention
And application.
Embodiment 1
A kind of fungus A-Fu03 thalline method of adsorption and enrichment rare earth ion from low concentration of rare earth feed liquid, including
Following steps:
(1) rare earth feed liquid: take from Southern Jiangxi Rare Earth Mine lean ore and leach gained leachate through ammonium sulfate, use
EDTA volumetric method titration rare earth ion concentration.The feed liquid titrated is configured to containing rare earth ion about 40mg/L
There is optimal adsorption effective concentration value.PH value is 6.
(2) culture medium preparation: add the ratio of 2g glucose with 20% Rhizoma Solani tuber osi leaching juice by every 100ml Rhizoma Solani tuber osi
Example, continues heating and melting and supplies dehydration.With conical flask subpackage, jump a queue, wrap up.High pressure steam sterilization half
Take out after hour, be dried in calorstat, then irradiate further sterilizing in 20 minutes with ultraviolet.
(3) inoculation: by strain Aspergillus oryzae Aspergillus oryzae in aseptic superclean bench
Sp.A-Fu03 is inoculated in step (2) in the Rhizoma Solani tuber osi fluid medium of gained.
(4) cultivate: will step (3) obtain equipped with inoculated strain Aspergillus oryzae Aspergillus oryzae
The conical flask of the potato culture of sp.A-Fu03, cultivates 72h, 8000rpm in constant-temperature shaking incubator
Centrifugal 5min or filter-cloth filtering collect thalline, are washed with deionized 3 times, claim weight in wet base, and in less than 4 DEG C ice
Case saves backup.
(5) absorption: use the microbial cells prepared by step (4) as adsorbent,
Particularly as follows: add 15mg/50mL thalline (in terms of dry weight) in low concentration (40mg/L) earth solution,
It is 6 that pH value controls, and temperature is set to 30 DEG C, and 150rpm shaking table vibration absorption 2h, 4000rpm are centrifuged 10min
(quantitative filter paper filtration) collects the thalline having adsorbed rare earth ion.Before measuring absorption respectively with spectrophotography
Rear rare earth ion concentration, calculating adsorbance is 39.52mg/g, and adsorption rate reaches 80%.
(6) desorbing: by the thalline having adsorbed rare earth ion collected by above-mentioned steps (5), use 0.5M respectively
HCl, in 200rpm vibration desorbing 2h, leaches thalline.The rare earth ion concentration of enrichment in filtrate is measured with EDTA,
Obtain rare earth ion enriched products, calculate desorption efficiency.
Embodiment 2
A kind of fungus A-Fu03 thalline adsorption and enrichment rare earth ion from the metallurgy waste liquid of low concentration of rare earth mine
Method, comprises the following steps:
(1) detection of rare earth waste liquid is with preparation: carry out rare earth to from Southern Jiangxi rare-earth mining area Metallurgical Waste Water
Ion concentration detects, and uses the titration of EDTA volumetric method.The waste liquid titrated is configured to containing rare earth ion
About 2.5mg/L concentration value, solution ph is 6.
(2) culture medium preparation: add the ratio of 2g glucose with 20% Rhizoma Solani tuber osi leaching juice by every 100ml Rhizoma Solani tuber osi
Example, continues heating and melting and supplies dehydration.With conical flask subpackage, jump a queue, wrap up.High pressure steam sterilization half
Take out after hour, be dried in calorstat, then irradiate further sterilizing in 20 minutes with ultraviolet.
(3) inoculation: by strain Aspergillus oryzae Aspergillus oryzae in aseptic superclean bench
Sp.A-Fu03 is inoculated in step (2) in the Rhizoma Solani tuber osi fluid medium of gained.
(4) cultivate: will step (3) obtain equipped with inoculated strain Aspergillus oryzae Aspergillus oryzae
The conical flask of the potato culture of sp.A-Fu03, cultivates 72h, 8000rpm in constant-temperature shaking incubator
Centrifugal 5min or filter-cloth filtering collect thalline, are washed with deionized 3 times, claim weight in wet base, and in less than 4 DEG C ice
Case saves backup.
(5) absorption: use the microbial cells prepared by step (4) as adsorbent, to step
Suddenly the rare earth ion in the low concentration of rare earth solution that (1) prepares adsorbs.It is specially to low concentration
(2.5mg/L) adding 15mg/50mL thalline (in terms of dry weight) in earth solution, it is 6 that pH value controls, temperature
Being set to 30 DEG C, 150rpm shaking table vibration absorption 2h, 4000rpm are centrifuged 10min (quantitative filter paper filtration), use
Spectrophotography measures rare earth ion concentration before and after absorption respectively, and calculating adsorbance is 61.96mg/g, absorption
Rate is up to 95%.
(6) desorbing: by the thalline having adsorbed rare earth ion collected by above-mentioned steps (5), use 0.5M respectively
HCl, in 200rpm vibration desorbing 2h, leaches thalline.The rare earth ion concentration of enrichment in filtrate is measured with EDTA,
Obtain rare earth ion enriched products, calculate desorption efficiency.
Claims (5)
1. one kind utilizes aspergillus oryzae side of thalline adsorption of Low Concentration rare earth liquid Rare Earth Ion after cultivating
Method, it is characterised in that described yeast culture method is: aspergillus oryzae is inoculated in special liquid culture
In base, 30 DEG C, 150rpm, shaking table is cultivated 3～4 days, 8000rpm is centrifuged 5min (or filter paper mistake
Filter, staticly settles 10-30min) collect thalline, it is washed with deionized 3 times, for fungus A-FuO3 thalline.
Utilize aspergillus oryzae thalline adsorption of Low Concentration rare earth liquid after cultivating the most according to claim 1
The method of Rare Earth Ion, it is characterised in that: described special liquid medium component is: every 1L liquid training
Support the 20g Han glucose in base, peeled potatoes 200g, water 1000ml, natural ph.
Utilize aspergillus oryzae thalline adsorption of Low Concentration rare earth liquid after cultivating the most according to claim 1
The method of Rare Earth Ion, the method utilizes fungus A-FuO3 thalline to mix with low concentration of rare earth solution stirring
0.5 hour, being then centrifuged for filtering, collect the thalline of absorption, filtrate checks earth solution, as also containing rare earth
Ion, repeats said process absorption, till filtrate can't check rare earth ion remnants.
4. according to claim 1 and 3, utilize aspergillus oryzae thalline adsorption of Low Concentration rare earth after cultivating
The method of liquid Rare Earth Ion, mixes the fungus A-FuO3 thalline dilute hydrochloric acid of above-mentioned absorption rare earth ion
Desorbing in 0.5 hour, centrifugal filtration, filtrate is rare earth concentrated solution product.
5. according to claim 1,3 and 4, utilize aspergillus oryzae thalline adsorption of Low Concentration after cultivating
Rare earth liquid Rare Earth Ion and desorption method, be washed with deionized above-mentioned desorbing fungus A-FuO3 thalline,
Until filtrate is neutrality, after being centrifuged to wash, filtering residue returns and reuses.
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Cited By (11)
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| CN108441630A (en) * | 2018-07-01 | 2018-08-24 | 广西那神晞途环保科技有限公司 | Application and sandworm culture rare earth ore leachate of the sandworm culture in leaching rare earth |
| CN108754188A (en) * | 2018-07-01 | 2018-11-06 | 广西那神晞途环保科技有限公司 | Application and sandworm culture rare-earth precipitation liquid of the sandworm culture in precipitating rare earth |
| CN108823407A (en) * | 2018-07-01 | 2018-11-16 | 广西那神晞途环保科技有限公司 | Ionic mineral soak mine agent and preparation method thereof |
| CN109161684A (en) * | 2018-11-12 | 2019-01-08 | 江西理工大学 | A method of utilizing spirulina recovering rare earth |
| CN110408801A (en) * | 2019-09-04 | 2019-11-05 | 贵州理工学院 | A kind of method of the dump leaching leaching recovering rare earth of ardealite containing rare earth |
| CN110408788A (en) * | 2019-09-04 | 2019-11-05 | 贵州理工学院 | A method of the leaching slag of acidolysis containing rare earth recovering rare earth |
| CN110607443A (en) * | 2019-10-14 | 2019-12-24 | 中铝广西有色稀土开发有限公司 | Method for recovering rare earth from ionic rare earth ore leaching solution |
| CN110791437A (en) * | 2019-11-29 | 2020-02-14 | 江西师范大学 | Filamentous fungus and method for enriching rare earth yttrium ions by using same |
| CN112877252A (en) * | 2021-03-09 | 2021-06-01 | 中南大学 | Composite microbial agent for leaching weathering crust leaching type rare earth ore and preparation method thereof |
| CN113046554A (en) * | 2021-03-09 | 2021-06-29 | 中南大学 | Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism |
| CN113061758A (en) * | 2021-03-26 | 2021-07-02 | 中国科学院广州地球化学研究所 | Method for extracting rare earth elements from phosphorite type rare earth ore by using phosphorus solubilizing bacteria |
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| CN108754188A (en) * | 2018-07-01 | 2018-11-06 | 广西那神晞途环保科技有限公司 | Application and sandworm culture rare-earth precipitation liquid of the sandworm culture in precipitating rare earth |
| CN108823407A (en) * | 2018-07-01 | 2018-11-16 | 广西那神晞途环保科技有限公司 | Ionic mineral soak mine agent and preparation method thereof |
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| CN109161684B (en) * | 2018-11-12 | 2020-07-24 | 江西理工大学 | Method for recovering rare earth by using spirulina |
| CN109161684A (en) * | 2018-11-12 | 2019-01-08 | 江西理工大学 | A method of utilizing spirulina recovering rare earth |
| CN110408801A (en) * | 2019-09-04 | 2019-11-05 | 贵州理工学院 | A kind of method of the dump leaching leaching recovering rare earth of ardealite containing rare earth |
| CN110408788A (en) * | 2019-09-04 | 2019-11-05 | 贵州理工学院 | A method of the leaching slag of acidolysis containing rare earth recovering rare earth |
| CN110607443A (en) * | 2019-10-14 | 2019-12-24 | 中铝广西有色稀土开发有限公司 | Method for recovering rare earth from ionic rare earth ore leaching solution |
| CN110607443B (en) * | 2019-10-14 | 2021-09-10 | 中铝广西有色稀土开发有限公司 | Method for recovering rare earth from ionic rare earth ore leaching solution |
| CN110791437A (en) * | 2019-11-29 | 2020-02-14 | 江西师范大学 | Filamentous fungus and method for enriching rare earth yttrium ions by using same |
| CN110791437B (en) * | 2019-11-29 | 2022-11-01 | 江西师范大学 | Filamentous fungus and method for enriching rare earth yttrium ions by using same |
| CN112877252A (en) * | 2021-03-09 | 2021-06-01 | 中南大学 | Composite microbial agent for leaching weathering crust leaching type rare earth ore and preparation method thereof |
| CN113046554A (en) * | 2021-03-09 | 2021-06-29 | 中南大学 | Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism |
| CN113046554B (en) * | 2021-03-09 | 2022-03-11 | 中南大学 | Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism |
| CN112877252B (en) * | 2021-03-09 | 2022-05-10 | 中南大学 | Composite microbial agent for leaching weathering crust leaching type rare earth ore and preparation method thereof |
| CN113061758A (en) * | 2021-03-26 | 2021-07-02 | 中国科学院广州地球化学研究所 | Method for extracting rare earth elements from phosphorite type rare earth ore by using phosphorus solubilizing bacteria |
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