CN102517454A - Method for recycling Au (III) in industrial waste water by chlorella-microfiltration membrane coupling technique - Google Patents
Method for recycling Au (III) in industrial waste water by chlorella-microfiltration membrane coupling technique Download PDFInfo
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- CN102517454A CN102517454A CN2011104223132A CN201110422313A CN102517454A CN 102517454 A CN102517454 A CN 102517454A CN 2011104223132 A CN2011104223132 A CN 2011104223132A CN 201110422313 A CN201110422313 A CN 201110422313A CN 102517454 A CN102517454 A CN 102517454A
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Abstract
The invention discloses a method for recycling Au (III) in industrial waste water by a chlorella-microfiltration membrane coupling technique, belonging to the recycle technology of heavy metal ions. The method comprises the steps of: culturing the Chlorella miniata by domestic sewage in a semi-continuous operation mode, and filtering the chlorella by an inorganic microfiltration membrane to obtain concentrated chlorella solution; adding the obtained chlorella solution in a reactor for recycling the Au (III) in the industrial waste water, wherein 99.8% of Au (III) can be adsorbed by a biosorbent and the Au (III) is reduced to nanometer level nulvalent gold on the surface of the chlorella; reacting the concentrated chlorella solution obtained by treating the Au (III) with 0.2 M thiourea solution to recycle the gold on the surface of the chlorella, and 99.3% of the gold can be recycled. The method the invention has the advantages of providing a cheap chlorella biosorbent to adsorb the Au (III), and the total recovery of the Au (III) is as high as 99.1%.
Description
Technical field
The present invention relates to the recovery method of a kind of Au (III), particularly relate to a kind of chlorella-microfiltration membrane coupling technique that utilizes and from trade effluent, reclaim the method for Au (III).
Background technology
The trade effluent that contains trivalent gold ion [Au (III)] is mainly derived from the waste water of plating, exploitation of gold deposit and electron trade discharging.These discharged waste water are big, and the concentration of gold is relatively low, as Au (III) not being carried out efficient recovery, causes environmental pollution on the one hand, causes production cost to improve on the other hand.The method of traditional method such as chemical precipitation, galvanic deposit, SX, charcoal absorption and resins exchange can be used for the process that dilute solution reclaims gold; But because low, expensive, the high energy consumption of the recovery or produce problems such as secondary pollution, these technology are restricted in application process.In order further to improve the recovery of Au (III), create bigger economic benefit, need the separation method that a kind of efficient is high, energy consumption is low, cost is little badly.
Biological adsorption technology be a kind of novel, reclaim the heavy metal ion technology efficiently, and up till now the problem of the maximum of technical application was how to reduce its production cost.Our early-stage Study finds that this chlorella has good effect of removing (Han, X.et al., Journal of Colloid and Interface Science, 2006,303,365-371 to Cr (III) and Cr (VI); Han, X.etal., Journal of Hazardous Materials, 2007,146,65-72).We find that also the growth velocity of chlorella Chlorella miniata in sewage will be higher than the growth velocity in the Bristol nutrient solution, and the most of N in the sewage, P and some nutritive ingredients can be removed effectively; Simultaneously, utilize chlorella Chlorellaminiata that sewage turns out to Cr (III) and Cr (VI) have equally very high clearance (Han, X.et al.Water Environment Research, 2008,80,647-653).This will reduce the production cost of biological adsorption agent to a great extent, and result of study proves that fully the research that utilizes sewage cultivation Chlorella miniata and apply it to the precious metal ion recovery is feasible.
The separation of microbial adsorbent is another major issue in the biological adsorption applications.Because mikrobe individual little, therefore insufficient strength is difficult to the suitable tripping device of selection they is separated, this to a great extent limit their application.With microbial biomass carry out immobilization and apply it to fixed bed or fluidized-bed reactor in can overcome this problem; But the immobilization meeting has a strong impact on the mass transfer effect of heavy metal ion at the fixation cell cellular surface, thereby the adsorption rate of heavy metal ion is reduced greatly.In addition, cost and the post-processed thereof as fixation support also will be the important factor that needs consideration in the application.Membrane separation reactor begins to receive publicity in the Biosorption of Heavy Metals field in recent years, and research shows that it can substitute the biological adsorption process that immobilization technology is applied to heavy metal ion.Utilize the crown_interception of ultrafiltration or microfiltration membrane, heavy metal ion can be separated with the biological adsorption agent mixed solution well.Do not see as yet that at present this technology studies the recovery of precious metal ion.
The meaning of this problem is for the recovery of Au in the trade effluent (III) a kind of environmental protection novel method to be provided.Simultaneously, this problem organically combines the processing of sewage and noble metal trade effluent, China's exploitation is had wastewater processing technology efficient, simple and easy, low consumption have important directive significance.
Summary of the invention
The objective of the invention is to overcome the deficiency in the conventional art, provide a kind of efficiently, chlorella biological adsorption agent cheaply, and utilize chlorella-microfiltration membrane coupling technique of developing from trade effluent, to reclaim Au (III).
Technical scheme of the present invention is summarized as follows:
A kind of chlorella-microfiltration membrane coupling technique that utilizes reclaims the method for Au (III), comprises the steps: from trade effluent
(1) at temperature 25 degree, light intensity is to take semi-continuous operating method to cultivate chlorella Chlorella miniata with the sewage of preparation voluntarily under the condition of 4000lux.Chlorella is taken out half the algae liquid after arriving the stationary phase of growing, and adds isopyknic sewage simultaneously and continues to cultivate.After this all operate with this kind mode every day, the algae liquid process pore size that obtains is that the inorganic micro filtering membrane filtration of 0.5 μ m obtains spissated algae liquid (microfiltration membrane tripping device I).
(2) to join volume be that the adsorptive reactor of 4L is used to adsorb Au (III) to the algae liquid after will concentrating.The starting point concentration of Au (III) is 100mg/L.Operational condition is: initial pH is 1.0-7.0, and stirring velocity is 50-100 rev/min, and temperature of reaction is the 20-40 degree, and the reaction times is 1-3 hour.The inorganic micro filtering membrane filtration that mixed solution after the processing feeds 0.5 μ m obtains the spissated chrysophyceae liquid (microfiltration membrane tripping device II) that contains, and the water after the separation emits.
(3) mix with thiourea solution handling concentrated algae liquid that Au (III) back obtained in (2), after the reaction mixing solutions fed inorganic micro filtering membrane filtration acquisition thiocarbamide-gold solution (microfiltration membrane tripping device III) of 0.5 μ m.
Preferably:
The inoculum density of chlorella is 8 * 10 in the said step (1)
6Frustule/milliliter.
In the said step (2), containing golden initial pH on wastewater is 2.0, and stirring velocity is 85 rev/mins, and temperature of reaction is 30 degree, and the reaction times is 1 hour, and algae liquid concentration is 4g/L.
Thiourea solution is 0.2M in the said step (3), and the reaction times is 1 hour.
The present invention relates to a kind of method that from trade effluent, reclaims Au (III), adopt chlorella absorption-microfiltration membrane to separate coupling technique and from trade effluent, reclaim Au (III).Compare with common Au (III) recovery method, Au of the present invention (III) recovery can reach 99.1%, and simultaneously, the present invention can be with the NH in the sewage
4 +-N and PO
4 3--P processing efficiency reaches 93% and 87% respectively.The present invention not only can handle sewage but also can from trade effluent, reclaim noble metal, greatly reduces the production cost of biological adsorption agent, is a green environmental protection technique.
Description of drawings
Fig. 1 is a process unit synoptic diagram of the present invention.
(Fig. 2 a) and through the ESEM (SEM) after Au (III) (Fig. 2 b) processing compares Fig. 2 chlorella Chlorella miniata without Au (III).
The XRD figure spectrum analysis of the chlorella Chlorella miniata of Fig. 3 after Au (III) handles.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is further described:
Embodiment 1
The sewage 12L of preparation is voluntarily fed chlorella culture apparatus (Fig. 1).Sewage consists of: 47.71mg L
-1NH
4 +-N (ammonia nitrogen), 1.34mg L
-1NO
x --N (nitre nitrogen), 51.71mg L
-1TKN (total triumphant formula nitrogen), 4.85mg L
-1PO
4 3--P (inorganic phosphorus), 7.56mg L
-1Total P (total phosphorus) and 317mg L
-1COD (COD).In nutrient solution, add chlorella Chlorella miniata then, the inoculum density of chlorella is 5 * 10
5-5 * 10
7Frustule/milliliter.At temperature 25 degree, adopt semi-continuous operating method to cultivate under the condition of light intensity 4000lux, and be that the growth of chlorella provides required CO through the mode that blasts air in bottom of device
2Take out half the algae liquid after arriving the stationary phase of growing, add isopyknic sewage simultaneously and continue to cultivate.After this all operate with this kind mode every day, the pore size of the algae liquid process of obtaining is that the inorganic micro filtering membrane filtration of 0.5 μ m obtains spissated algae liquid.Behind the stable operation, can obtain 1.7g (dry weight algae)/rise sewage every day.The diameter of chlorella culture apparatus is 120mm, highly is 1.8m.Preferred operational condition is: the inoculum density of chlorella is 8 * 10
6Frustule/milliliter.The long 0.5m of inorganic micro filtering membrane film device, diameter 10cm, pore size are 0.5 μ m.
Embodiment 2
It is that the chlorella reactor drum of 4L is used to adsorb Au (III) (Fig. 1) that algae liquid after concentrating among the embodiment 1 is joined volume, forms the algae liquid of 4g/L at last.The starting point concentration of Au (III) is 100mg/L.Operational condition is: initial pH is 1.0-7.0, and stirring velocity is 50-100 rev/min, and temperature of reaction is the 20-40 degree, and the reaction times is 1-5 hour.Mixed solution after the processing feeds inorganic micro filtering membrane film device (the long 0.5m of inorganic micro filtering membrane film device, the diameter 10cm) filtration of aperture 0.5 μ m and obtains spissated algae liquid, and the water after the separation emits.Preferred operational condition is: initial pH is 2.0, and stirring velocity is 85 rev/mins, and temperature of reaction is 25 degree, and the reaction times is 1 hour.Under the peak optimization reaction condition, 99.8% Au (III) can be adsorbed by chlorella.Sem analysis shows that the chlorella surface after handling through Au (III) generates the particle (Fig. 2) of Nano grade.XRD analysis further shows, several positions that go out the peak are respectively 2 θ=38.0,44.3,64.53, and 77.50and 81.61, prove that this nanoparticle is Au (a 0) nanoparticle (Fig. 3).
Embodiment 3
Be mixed in gold and reclaim reactor drum (volume is 1L) handling concentrated algae liquid that Au (III) back the obtained thiourea solution with 0.5L among the embodiment 2, reaction was carried out 1-5 hour, and the gold surperficial to chlorella reclaims.The inorganic micro filtering membrane film device (the long 0.3m of inorganic micro filtering membrane film device, diameter 6cm) that reaction back mixed solution feeds aperture 0.5 μ m carries out liquid-solid separation.Preferred operational condition is: thiourea solution is 0.3L, and concentration is 0.2M, and the reaction times is 1 hour, and the gold on chlorella surface 99.3% is recovered.Therefore, in the waste water altogether 99.1% Au (III) can be recovered.
Claims (6)
1. a chlorella-microfiltration membrane coupling technique reclaims the method for Au (III) in the trade effluent, it is characterized in that may further comprise the steps:
(1) at temperature 25 degree; Light intensity is to take semi-continuous operating method to cultivate chlorella Chlorella miniata with the sewage of preparation voluntarily under the condition of 4000lux; Chlorella is taken out half the algae liquid after arriving the stationary phase of growing, and adds isopyknic sewage simultaneously and continues to cultivate; After this all operate with this kind mode every day, the algae liquid process pore size that obtains is that the inorganic micro filtering membrane filtration of 0.5 μ m obtains spissated algae liquid;
(2) the algae liquid after will concentrating joins the Au that volume is 4L (III) reactor drum and is used for Au (III) absorption, and Au (III) starting point concentration is 100mg/L; Operational condition is: initial pH is 1.0-7.0, and stirring velocity is 50-100 rev/min, and temperature of reaction is the 20-40 degree, and the reaction times is 1-3 hour; Au (III) is reduced into the Au (0) of Nano grade on the chlorella surface; The inorganic micro filtering membrane filtration that mixed solution after the processing feeds 0.5 μ m obtains the spissated chrysophyceae liquid that contains;
(3) reclaim handling the gold that concentrated algae liquid that Au (III) back obtained mixes with thiourea solution the chlorella surface in (2), after the reaction mixing solutions fed inorganic micro filtering membrane filtration acquisition thiocarbamide-gold solution of 0.5 μ m.
2. a kind of chlorella according to claim 1-microfiltration membrane coupling technique reclaims the method for Au (III) in the trade effluent; It is characterized in that described in step (1), (2) and (3): adopt sewage to cultivate chlorella Chlorella miniata, and utilize chlorella absorption-microfiltration membrane to separate coupling technique and reclaim the Au (III) in the trade effluent as biological adsorption agent.
3. a kind of chlorella according to claim 1-microfiltration membrane coupling technique reclaims the method for Au (III) in the trade effluent, it is characterized in that described in step (1), (2) and (3): algae liquid process pore size is that the inorganic micro filtering membrane filtration of 0.5 μ m obtains spissated algae liquid.
4. a kind of chlorella according to claim 1-microfiltration membrane coupling technique reclaims the method for Au (III) in the trade effluent, and it is characterized in that described in the step (1): the initial inoculation concentration of chlorella in sewage is 8 * 10
6Frustule/milliliter sewage.
5. a kind of chlorella according to claim 1-microfiltration membrane coupling technique reclaims the method for Au (III) in the trade effluent; It is characterized in that described in the step (2): contain golden initial pH on wastewater and be controlled to be 2.0; Stirring velocity is 85 rev/mins; Temperature of reaction is 30 degree, and the time is 1 hour, and Chlorella miniata algae liquid concentration is 4g/L.
6. a kind of chlorella according to claim 1-microfiltration membrane coupling technique is reclaimed the method for Au (III) in the trade effluent, it is characterized in that described in the said step (3): adopt 0.3L 0.2M thiourea solution with mix, react and carried out 1 hour.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2947163A4 (en) * | 2013-01-21 | 2016-05-11 | Mitsubishi Rayon Co | Method for metal concentration, method for metal recovery, device for metal concentration, and device for metal recovery |
| CN106391006A (en) * | 2016-09-10 | 2017-02-15 | 天津大学 | Preparation method of heat-resistant anti-coking load-type gold nanoparticle catalyst |
| CN106448791A (en) * | 2016-12-12 | 2017-02-22 | 河北工业大学 | Exploiting absorbent means purge simulating emission sewage trial method |
| CN109844144A (en) * | 2016-10-31 | 2019-06-04 | 新技术管理创新公司 | Metal recovery processes |
| CN114590899A (en) * | 2022-02-24 | 2022-06-07 | 北京科技大学 | Dynamic control device and method for fully mixing and reacting active algae and metal ions |
| WO2024053487A1 (en) * | 2022-09-06 | 2024-03-14 | 株式会社Ihi | Metal recovery agent, metal recovery member, metal recovery liquid agent and metal recovery method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2947163A4 (en) * | 2013-01-21 | 2016-05-11 | Mitsubishi Rayon Co | Method for metal concentration, method for metal recovery, device for metal concentration, and device for metal recovery |
| EP3162905A1 (en) * | 2013-01-21 | 2017-05-03 | Mitsubishi Rayon Co. Ltd. | Method for metal concentration, method for metal recovery, device for metal concentration, and device for metal recovery |
| CN106391006A (en) * | 2016-09-10 | 2017-02-15 | 天津大学 | Preparation method of heat-resistant anti-coking load-type gold nanoparticle catalyst |
| CN106391006B (en) * | 2016-09-10 | 2019-06-18 | 天津大学 | A kind of preparation method of high temperature resistant anti-coking load type gold nanocatalyst |
| CN109844144A (en) * | 2016-10-31 | 2019-06-04 | 新技术管理创新公司 | Metal recovery processes |
| CN106448791A (en) * | 2016-12-12 | 2017-02-22 | 河北工业大学 | Exploiting absorbent means purge simulating emission sewage trial method |
| CN114590899A (en) * | 2022-02-24 | 2022-06-07 | 北京科技大学 | Dynamic control device and method for fully mixing and reacting active algae and metal ions |
| CN114590899B (en) * | 2022-02-24 | 2023-10-20 | 北京科技大学 | Dynamic control device and method for fully mixing reaction of active algae and metal ions |
| WO2024053487A1 (en) * | 2022-09-06 | 2024-03-14 | 株式会社Ihi | Metal recovery agent, metal recovery member, metal recovery liquid agent and metal recovery method |
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Application publication date: 20120627 |