CN1388256A - Method of recovering Pd from low-concentration waste Pd ion liquid with becteria thallus - Google Patents

Method of recovering Pd from low-concentration waste Pd ion liquid with becteria thallus Download PDF

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Publication number
CN1388256A
CN1388256A CN02102604A CN02102604A CN1388256A CN 1388256 A CN1388256 A CN 1388256A CN 02102604 A CN02102604 A CN 02102604A CN 02102604 A CN02102604 A CN 02102604A CN 1388256 A CN1388256 A CN 1388256A
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China
Prior art keywords
palladium
thalline
reclaim
concentration
waste liquid
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CN02102604A
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CN1166790C (en
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刘月英
傅锦坤
姚炳新
林种玉
古萍英
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Xiamen University
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Xiamen University
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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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  • Manufacture And Refinement Of Metals (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The present invention relates to the recovery of micro amount of noble metal and the used bacteria is lichenoid bacillus No.R08. R08 bacillus thallus solution of 0.4-2.0 g/L concentration and water solution of Pd ion of 30-300 mg/L are first mixed and vibrated at 5-60 deg.c pH 2.0-3.5 and 130 Hz vibration frequency for 3-90 min; the mixed liquid is then filtered; and filtered Pd adsorbing bacillus thallus is set at room temperature for 6-48 hr and burned at 550-800 deg.c for 1.5-3 hr to obtain metal Pd. The simple process is especially suitable for recovering Pd from low concentration solution and the Pd ion adsorbing rate may reach 99%.

Description

From the palladium ion waste liquid of lower concentration, reclaim the method for palladium with the bacterium thalline
(1) technical field
The present invention relates to a kind of recovery method of minute amount of noble metal.
(2) background technology
Precious metals such as palladium are national defence, chemical industry, indispensable important source material in the industrial production such as petroleum refining and electronics.Along with the development of industrial technology, the application of precious metal is more and more extensive.Yet, precious metal resource scarcities and rare such as palladium.Therefore, various countries reclaim the regeneration of precious metal and all take much count of.The method that reclaims precious metals such as palladium at present from solution has activated carbon adsorption, ion-exchange, chemical precipitation, electrolysis and solvent extraction etc.The process of these methods is loaded down with trivial details and easily cause secondary pollution, when precious metal ion content in the solution is low, is uneconomic with above-mentioned recovery method particularly.People such as Brierly (Biohydrometa, Proc Int Symp, 1988,477) once were prepared into the agent of granulous metal removal with dead thalline, from 10mgPd 2+Reclaim palladium in the/L solution.People such as Lloyd (ApplEnviron Microbiol, 1998,4607) report, Desulfovibriodesulfuricanns resting cell can reduce soluble Pd 2+Become palladium metal (Pd 0).It is reported (Mreeoun et al J ApplMicrobiol, 1998,84:63), that live or dead complete microorganism cells and meta-bolites thereof can adsorb soluble and metal particle form efficiently, particularly reclaim precious metal from the metal ion of low solubility.Many studies show that, dead microorganism cells has characteristics (Niu Hui etc., 1993,33 (6): 459) such as speed is fast, selectivity is high, loading capacity is big to the absorption of metal ion.
(3) summary of the invention
Purpose of the present invention aims to provide a kind of method of utilizing the bacterium thalline to reclaim palladium from the palladium ion waste liquid of lower concentration.
The used microbial adsorbent of the present invention is the absorbing and reducing Pa that filters out from metal mining area environment separation 2+The bacterial strain R08 that ability is stronger has been stored in China Committee for Culture Collection of Microorganisms common micro-organisms center through being accredited as this thalline of bacillus licheniformis (Bacillus licheniformis), and that registers on the books is numbered 0503, strain RO8.
The Pd of the present invention in the R08 thalline absorbing and reducing solution 2+, its operation and analysis determining method are as follows:
At first with somatic cells solution and Pd 2+Aqueous solution, cell concentration are preferably 0.8～1.6g/L of 0.4～2.0g/L, Pd 2+Concentration be 30～300mg/L. under 5～60 ℃ of temperature, preferably under the condition of PH2.0～3.5, by 130 times/min of oscillation frequency vibration, 3～90min, preferably 30～60min makes bacterium fully adsorb Pd in PH1.0～3.8 2+Be the membrane filtration Pd of 0.22um then with the aperture 2+-thalline effect liquid makes absorption Pd 2+Thalline and residual Pd 2+Solution separately.The absorption Pd that is obtained will be filtered 2+Thalline under room temperature, place 6～48h, preferably behind 18～36h, through 550～800 ℃ of high temperature sintering 1.5h～3h, promptly recyclable palladium metal.Filtrate is used its residual Pd of WFX-IE2 type atomic absorption spectrophotometer 2+Concentration is calculated as follows thalline to Pd 2+Adsorption rate and adsorptive capacity:
Adsorption rate (%)=(C i-C f)/C i* 100%
Adsorptive capacity (mg/g dry mycelium)=(C i-C f)/C b
C in the formula iAnd C fBe respectively Pd 2+Initial concentration and final concentration (mg/L), C bBe cell concentration (g/L).
Show R08 thalline and Pd with transmission electron microscope (TEM) observation 2+Solution contact 6h～48h after, on cell walls, have Pd 0Particle.Method provided by the invention is easy, and cost is low, is particularly suitable for from lower concentration Pd 2+Reclaim palladium in the solution, Pb 2+Adsorption rate can be up to 99%.
(4) embodiment
The invention will be further described below by embodiment.
Embodiment 1:
With cell concentration is that dead somatic cells solution of R08 and the initial concentration of 1.2g/L is the Pd of 200mg/L 2+Solution mixes, and regulating the pH value is 3.5, under 30 ℃, by the oscillation frequency vibration mixing solutions 45min of 130 times/min, is the filtering membrane filtration Pd of 0.22mm then with the aperture 2+-thalline effect liquid will adsorb Pd 2+Thalline under room temperature, place 24h, after reclaim palladium metal after 600 ℃ of calcinations.Analyze after measured, the R08 thalline is to Pd 2+Adsorptive capacity can reach the 149.0mg/g thalline, adsorption rate is 89.4%.
Embodiment 2～9:
At Pd 2+Initial concentration is the absorption of carrying out different time under 200mg/L, cell concentration 0.8g/L, pH3.0 and the 25 ℃ of conditions, measures adsorption time thalline is adsorbed Pd 2+Influence.Other operation is with embodiment 1, and the result is as follows:
Embodiment time (min) adsorptive capacity (mg/g) adsorption rate (%)
2 3 139.4 58.1
3 8 147.4 61.4
4 11 152.2 63.4
5 15 156.3 65.1
6 30 164.1 68.4
7 45 177.1 70.8
8 60 175.2 70.1
9 90 176.5 70.6
Embodiment 10～13
With PdCl 2Solution transfers to different pH values, at Pd 2+Initial concentration is 100mg/L, and under the condition of bacteria concentration 0.8g/L and 25 ℃, absorption 45min measures thalline to Pd 2+Adsorption rate and adsorptive capacity.Other will adsorb Pb with embodiment 1 2+Thalline filter, place after 18 hours, through 550 ℃ of calcination 3h, promptly can be recycled to palladium metal.The result is as follows:
Embodiment pH value adsorptive capacity (mg/g) adsorption rate (%)
10 1.0 58.8 47.0
11 2.0 87.9 70.3
12 3.0 107.3 85.8
13 3.5 116.5 93.2
Embodiment 14～19
Change adsorbing temperature, at Pd 2+Initial concentration 200mg/L, under the condition of bacteria concentration 0.8g/L and pH3.5, absorption 45min measures temperature thalline is adsorbed Pd 2+Influence.All the other are with embodiment 1, and after last thalline was placed 36h, the calcination 1.5h through 800 ℃ promptly can be recycled to palladium metal.The result is as follows:
The embodiment temperature (℃) adsorptive capacity (mg/g) adsorption rate (%)
14 5 190.4 76.2
15 20 196.0 78.4
16 30 196.7 78.7
17 40 197.6 79.0
18 50 201.3 81.3
19 60 202.2 81.3
Embodiment 20～23
Change adsorbing cell concentration, at Pd 2+Under the condition of initial concentration 200mg/L, pH3.5 and 30 ℃, absorption 45min measures cell concentration thalline is adsorbed Pd 2+Influence.The result is as follows:
Embodiment cell concentration (g/L) C i: C b(mg/g) adsorptive capacity (mg/g) adsorption rate (%)
20 0.4 500 224.8 45.0
21 0.8 250 175.2 70.1
22 1.6 125 115.5 92.4
23 2.0 100 94.4 94.4
C i: C b: Pd 2+The ratio of initial concentration and cell concentration.
Embodiment 24～33
Change adsorbing Pd 2+Initial concentration, under the condition of cell concentration 0.8g/L, pH3.5 and 30 ℃, absorption 45min measures Pd 2+Initial concentration adsorbs Pd to thalline 2+Influence.The result is as follows:
Embodiment Pd 2+Concentration (mg/L) adsorptive capacity (mg/g) adsorption rate (%)
24 30 37.1 99.0
25 60 74.1 98.7
26 90 107.2 95.3
27 120 128.4 85.6
28 150 149.8 79.9
29 180 165.4 73.5
30 210 84.8 70.4
31 240 192.2 64.1
32 270 198.8 59.3
33 300 202.9 55.1
Embodiment 34-38
Pd with the dead palladium catalyst treatment solution 2+Initial concentration transfers to about 200mg/L, adsorbs 60min under cell concentration 2～10g/L and 30 ℃ of conditions, and the result is as follows:
Embodiment cell concentration (g/L) adsorption rate (%)
34 2 11.7
35 4 36.9
36 6 56.1
37 8 68.3
38 10 78.4Pd 2+Initial concentration: 206mg/L

Claims (8)

1. from the palladium ion waste liquid of lower concentration, reclaim the method for palladium with the bacterium thalline, it is characterized in that said bacterium is Bacillus licheniformis (Bacillus lichemiformis), strain R08, recovery method is as follows: the somatic cells solution and the concentration that at first with cell concentration are 0.4～2.0g/L are the Pd of 30～300mg/L 2+Aqueous solution, in 5～60 ℃, under the condition of pH value 2.0～3.5, the oscillation frequency vibration 3～90min by 130 times/min filters Pd then 2+-thalline effect liquid is with the absorption Pd after filtering 2+Thalline under room temperature, place 6～48h, after behind 550～800 ℃ of calcination 1.5～3h palladium metal.
2. the method for using the bacterium thalline to reclaim palladium from the palladium ion waste liquid of lower concentration as claimed in claim 1 is characterized in that cell concentration is 0.8～1.6g/L.
3. the method for using the bacterium thalline to reclaim palladium from the palladium ion waste liquid of lower concentration as claimed in claim 1 is characterized in that the adsorption temperature is 20～50 ℃.
4. the method for using the bacterium thalline to reclaim palladium from the palladium ion waste liquid of lower concentration as claimed in claim 1 is characterized in that the adsorption pH value is 2.0～3.5.
5. the method for using the bacterium thalline to reclaim palladium from the palladium ion waste liquid of lower concentration as claimed in claim 1 is characterized in that the adsorption duration of oscillation is 30～60min.
6. the method for using the bacterium thalline to reclaim palladium from the palladium ion waste liquid of lower concentration as claimed in claim 1 is characterized in that the thalline after the adsorption is placed 18～36h under room temperature.
7. the method for using the bacterium thalline to reclaim palladium from the palladium ion waste liquid of lower concentration as claimed in claim 1 is characterized in that with the aperture being the membrane filtration Pd of 0.22mm 2+Thalline effect liquid.
8. the method for using the bacterium thalline to reclaim palladium from the palladium ion waste liquid of lower concentration as claimed in claim 1 is characterized in that the dead somatic cells of R08 thalline for doing that adopts.
CNB021026041A 2002-01-16 2002-01-16 Method of recovering Pd from low-concentration waste Pd ion liquid with becteria thallus Expired - Fee Related CN1166790C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100441300C (en) * 2006-12-31 2008-12-10 厦门大学 Method of preparing loading type silver catalyst by micro-reduction
CN100500335C (en) * 2007-02-15 2009-06-17 厦门大学 Preparing process of water-soluble nano silver powder containing biomass
CN105714114A (en) * 2016-04-22 2016-06-29 江西省科学院应用化学研究所 Method for adsorbing enriched rare earth ions from low-concentration rare earth lixivium through fungus A-Fu03 thalli

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100441300C (en) * 2006-12-31 2008-12-10 厦门大学 Method of preparing loading type silver catalyst by micro-reduction
CN100500335C (en) * 2007-02-15 2009-06-17 厦门大学 Preparing process of water-soluble nano silver powder containing biomass
CN105714114A (en) * 2016-04-22 2016-06-29 江西省科学院应用化学研究所 Method for adsorbing enriched rare earth ions from low-concentration rare earth lixivium through fungus A-Fu03 thalli

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