CN105349775A - Column leaching method conforming to shrinking core model - Google Patents
Column leaching method conforming to shrinking core model Download PDFInfo
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- CN105349775A CN105349775A CN201410416184.XA CN201410416184A CN105349775A CN 105349775 A CN105349775 A CN 105349775A CN 201410416184 A CN201410416184 A CN 201410416184A CN 105349775 A CN105349775 A CN 105349775A
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Abstract
The invention discloses a column leaching method conforming to a shrinking core model. The method comprises the following steps: 1) by the utilization of a constant-temperature constant-potential column leaching device, an upper packing layer and a lower packing layer are firstly contained with PVC shells respectively, an intermediate ore bed and an intermediate packing layer are contained in a same PVC shell, and the upper packing layer, the intermediate ore bed, the intermediate packing layer and the lower packing layer are successively filled in a mineral leaching column; and 2) a spray liquid is sprayed on the upper packing layer; after uniformly redistributed through the upper packing layer, the spray liquid contacts with the intermediate ore bed to react; after reaction, the liquid passes through the intermediate packing layer and the lower packing layer and then flows into a liquid collection bottle; and the constant-temperature, constant-potential and constant-pH solution in the liquid collection bottle is reused as a spray liquid to be sprayed from a top spray header onto the upper packing layer through a circulating pump. According to the invention, industrial dump leaching can be simulated, and the shrinking core model also can be rapidly satisfied. Key kinetic parameters related to mineral leaching can be solved by the method of the invention.
Description
Technical field
The invention belongs to liquid-solid reaction system leaching of ores dynamics field, particularly, the present invention relates to a kind of post leaching method meeting shrinking core model.
Background technology
Shrinking core model is that liquid in metallurgical process (gas) is Gu the basis of/reaction kinetics, utilizing shrinking core model to solve kinetic parameter is one of method of practicality the most, is thus studying liquid (gas) Gu widely use in/reaction kinetics process.For compact solid reactant, chemical reaction is inwardly carried out gradually by solid surface, has obvious boundary between reactant and product, carry out with reaction, product layer thickness increases gradually and solid reactant core reduces gradually, to the last disappears, and Here it is " shrinking core model ".Dump leaching is industrial common Leaching way, is all widely used in the leaching of ores of copper, gold and uranium etc.Ore deposit heap is a complicated heterogeneous system, and the reaction conditions in heap is often different with position and present larger difference, and heap top and the leaching condition difference at the heap end may be larger, and the factors such as physics, chemistry, biology all can affect the leaching efficiency of ore deposit heap.The leaching of ores kinetics of available data report adopts the mode of agitation leach usually, utilizes shrinking core model matching to solve crucial kinetic parameter.Shrinking core model requires the reaction conditions of stable homogeneous, and the electrochemical conditions of usual agitation leach is comparatively homogeneous, is easy to the requirement meeting shrinking core model, but differs comparatively far away with industry is actual, can not simulate industrial dump leaching really.Post leaching is a kind of laboratory method of conventional, simulation dump leaching reality, leaching post and usually adopts different sizes according to different ore grain sizes, sometimes in order to simulate the industrial ore layer up to tens meters, also can adopt multiple leaching post serial operation.Column leaching test because of close with commercial operating conditions, therefore can obtain leaching yield and the leaching rate of target minreal, and the authentic datas such as pH value and Eh change, for industrial practice provides reference.
Available data utilizes shrinking core model to study the kinetics of leaching of ores under rarely having report post leaching condition, electrochemical conditions heterogeneity in usual leaching post, the reaction conditions difference of top and bottom is larger, is difficult to meet the requirement about stable homogeneous reaction conditions in shrinking core model.Even if meet also often needs for a long time, therefore be difficult to be utilized and solve crucial kinetic parameter.For the deficiency of above method, need a kind of new post leaching method of exploitation badly.
Summary of the invention
The object of the invention is to, provide a kind of post leaching method meeting shrinking core model, the method can simulate industrial dump leaching, faster can meet shrinking core model again, and it can be utilized to solve crucial kinetic parameter about leaching of ores.
For realizing above object, the present invention by the following technical solutions:
Meet a post leaching method for shrinking core model, said method comprising the steps of:
1) constant temperature constant potential post bath unit is utilized, first upper strata packing layer and lower floor's packing layer are adopted PVC shell splendid attire respectively, middle seam and intermediate filler layer splendid attire in same PVC shell, then are filled in leaching ore pillar body according to upper strata packing layer, middle seam, intermediate filler layer and lower floor's packing layer successively;
2) spray liquid spray upper strata packing layer, after the even distribution again of upper strata filler, with middle seam contact reacts, flow in liquid-collecting bottle after intermediate filler layer and lower floor's packing layer after reaction, the solution of the constant temperature in liquid-collecting bottle, constant potential and permanent pH value sprays upper strata packing layer as spray liquid again through recycle pump from top spray head;
Described step 1) in PVC shell internal diameter be 4 ~ 6cm, in middle seam, minal add-on is 1 ~ 2g;
Described step 2) in the amount ratio of minal add-on and spray liquid be 1:100 ~ 1:300, spray liquid concentration is 5 ~ 20g/L, and Spraying rates is 3 ~ 10mL/min.
Preferably, described middle seam height≤0.5cm, middle seam and intermediate filler layer total height are at 0.8 ~ 1.5cm.Those skilled in the art can also select other numerical value as required.
Preferably, the height of described upper strata packing layer and lower floor's packing layer is 3 ~ 7cm.Those skilled in the art can also select other numerical value as required.
Preferably, the filler in described upper strata packing layer, intermediate filler layer and lower floor's packing layer is granulated glass sphere or quartz sand.Those skilled in the art can also select other inert filler as required.
In the present invention, controlled the redox potential of spray liquid by redox potential on-line monitoring device and hydrogen peroxide, controlled oxidization reduction potential fluctuation range is ± 10mV.
In the present invention, measured the pH of solution in liquid-collecting bottle by pH meter interval, and regulate pH that its fluctuation range is controlled as ± 0.05 by acid-base solution.
In the present invention, keep leaching the homo(io)thermism in post by heating in water bath chuck layer, kept the homo(io)thermism of solution in liquid-collecting bottle by oil bath heating.
In the present invention, the temperature in described liquid-collecting bottle maintains 30 ~ 60 DEG C.
In the present invention, the sieve plate 9 of described PVC shell is arranged several round sieves 8.
Post leaching method of the present invention significantly can reduce the concentration difference that spray liquid distributes in ore bed, meets the requirement of shrinking core model, and the verification method of shrinking core model is as follows:
1) sample in liquid-collecting bottle every 1 ~ 12h, measure metal ions M in leach liquor with ICP-OES
n+concentration, calculates the leaching yield X of M according to the following formula:
X＝C*V/(G*a)*100％；
Wherein, C is M
n+concentration, unit is g/L; V is liquor capacity, and unit is L; G is minal add-on in leaching ore pillar, and unit is g; A is minal grade;
2) with time t for X-coordinate, control with the reaction controlling in shrinking core model, internal diffusion respectively, the kinetic equation of mixture control maps for ordinate zou, utilize data fitting software to carry out linear fit to the scatter diagram obtained, compare the straight line that matching obtains, linearly dependent coefficient R
2the highest and >0.98 and fitting of a straight line effect through initial point is best.
Wherein, the reaction controlling in shrinking core model, internal diffusion control, the kinetic equation of mixture control is respectively 1-(1-X)
1/3, 3-2X-3 (1-X)
2/3, 1-(1-X)
1/3+ B [3-2X-3 (1-X)
2/3], B=K
c/ K
p, be dimensionless constant.K
cfor chemical reaction rates, unit is min
-1, K
pfor rate of diffusion constant, unit is min
-1.
The present invention adopts " four-layer structure " of leaching ore pillar body, and leaching ore pillar body is divided into upper strata packing layer, middle seam, intermediate filler layer and lower floor's packing layer.Packing layer and lower floor's packing layer contain the inert filler of good penetrability at the middle and upper levels for they; Intermediate filler layer can load quartz sand, the little and minal that grade is narrow of middle seam filling granularity, and mixes with quartz sand.
The present invention adopts large Spraying rates, be beneficial to spray liquid to be evenly distributed in the packing layer of upper strata, the liquid phase reaction agent concentration in spray liquid is high, ensures that in reaction process, reagent is greatly excessive, its concentration can be considered constant, meets requirement constant for liquid phase reaction agent concentration in shrinking core model; The solution that upper strata packing layer can get off to leaching in spray header carries out evenly distributing again, ensures that the electrochemical conditions of the solution contacted with middle seam is homogeneous; Middle seam uses minal to mix with quartz, highly little, and by controlling Spraying rates, the height of reactant density and middle seam reduces the concentration difference of reagent in middle seam; The minal granularity used is little, and grade is narrow, meets the requirement for solid reactant particle diameter in shrinking core model; Intermediate filler layer can effectively stop the mineral caused due to large Spraying rates to run off, and lower floor's packing layer can stop mineral to run off further.The two-layer inert filler all adopting good penetrability, significantly reduces the adsorptive capacity of solution in filler up and down, contributes to the leaching yield more accurately calculating target minreal; Use PVC shell to contain, what be convenient to mineral and packing layer is separated the analysis of soaking slag with mineral.
The present invention is by utilizing the device of constant temperature constant potential, and the solution in circulating system maintains the electrochemical conditions of stable homogeneous, and " four-layer structure " that leach post can meet the requirement of shrinking core model preferably.By the method, both simulated industrial dump leaching, shrinking core model can be utilized again to solve affects the crucial kinetic factor of minal leaching, for industrial practice provides reference.
Handling object of the present invention is minal, by " four layers of design " and the requirement that can meet shrinking core model to the control of reaction conditions (Spraying rates, spray liquid concentration) comparatively fast, preferably.
Accompanying drawing explanation
Fig. 1 is the structural representation of constant temperature constant potential post bath unit in the present invention;
Fig. 2 is the filling structure schematic diagram soaking ore pillar in the present invention;
Fig. 3 is PVC shell vertical view in the present invention;
Fig. 4 is the reaction controlling fitted figure of shrinking core model in embodiment 1;
Fig. 5 is that the internal diffusion of shrinking core model in embodiment 1 controls fitted figure;
Fig. 6 is the mixture control fitted figure of shrinking core model in embodiment 1;
Fig. 7 is the reaction controlling fitted figure of shrinking core model in embodiment 2;
Fig. 8 is that the internal diffusion of shrinking core model in embodiment 2 controls fitted figure;
Fig. 9 is the mixture control fitted figure of shrinking core model in embodiment 2;
Figure 10 is the reaction controlling fitted figure of shrinking core model in embodiment 3;
Figure 11 is that the internal diffusion of shrinking core model in embodiment 3 controls fitted figure;
Figure 12 is the mixture control fitted figure of shrinking core model in embodiment 3;
Figure 13 is Arrhenius equation model figure in embodiment 4;
Reference numeral: 1, upper strata filler; 2, middle seam; 3, intermediate filler; 4, lower floor's filler; 5, spray header; 6, bearing; 7, PVC shell; 8, sieve aperture; 9, sieve plate; 10, circulating water inlet; 11, circulating water outlet pipe; 12, chuck; 13, magnetic stir bar; 14, liquid collection type magnetic stirring apparatus; 15, liquid-collecting bottle liquid outlet; 16, recycle pump; 17, ORP electrode; 18, ORP controller; 19, control of Electric potentials liquid storage bottle; 20, dosing peristaltic pump; 21, leach liquor leakage fluid dram; 22, constant temperature water bath; 23, liquid-collecting bottle.
Embodiment
With the drawings and specific embodiments, the present invention is further detailed explanation below.
As shown in Figure 1, constant temperature constant potential post bath unit of the present invention, described device comprises leaching ore pillar and constant potential system;
Described leaching ore pillar top arranges spray header 5, and on post, arrange chuck 12, and chuck 12 is arranged circulating water inlet 10 and circulating water outlet pipe 11, circulating water inlet 10 is connected with constant temperature water bath 22 respectively with circulating water outlet pipe 11;
Leach liquor leakage fluid dram 21 bottom described leaching ore pillar is connected with the bottleneck of liquid-collecting bottle 23, the built-in magnetic stir bar 13 of liquid-collecting bottle 23, and is positioned on liquid collection type magnetic stirring apparatus 14;
Described constant potential system comprises ORP electrode 17, ORP controller 18, dosing peristaltic pump 20 and control of Electric potentials liquid storage bottle 19; The signal input part of ORP controller 18 is connected with ORP electrode 17, and the signal output part of ORP controller 18 is connected with dosing peristaltic pump 20, and described control of Electric potentials liquid storage bottle 19 carries control of Electric potentials liquid after dosing peristaltic pump in liquid-collecting bottle;
Liquid-collecting bottle liquid outlet 15 in liquid-collecting bottle 23 soaks capital end after recycle pump 16 spray header 5 with post is connected.
As shown in Figures 2 and 3, the present invention utilizes constant temperature constant potential post bath unit, first upper strata packing layer 1 and lower floor's packing layer 4 are adopted PVC shell 7 splendid attire respectively, middle seam 2 and intermediate filler layer 3 splendid attire are in same PVC shell, be filled in leaching ore pillar body successively according to upper strata packing layer 1, middle seam 2, intermediate filler layer 3 and lower floor's packing layer 4 again, the bearing 6 of post leaching column bottom is for supporting lower floor's packing layer 4; After filling, concentration is that the spray liquid of 5 ~ 20g/L is with the Spraying rates of 3 ~ 10ml/min spray upper strata packing layer, after the even distribution again of upper strata filler, with middle seam contact reacts, flow in liquid-collecting bottle after intermediate filler layer and lower floor's packing layer after reaction, the solution of the constant temperature in liquid-collecting bottle, constant potential and permanent pH value sprays upper strata packing layer as spray liquid again through recycle pump from top spray head.
Sieve plate 9 in the present invention bottom PVC shell is arranged several round sieves 8.
Embodiment 1:
Certain secondary copper sulfide minal 1.5g, granularity 30 ~ 55 μm accounts for 75%, the Fe of spray liquid to be concentration be 10g/L
2(SO
4)
3solution 300ml, Spraying rates is 5ml/min, and spray liquid ORP controls at 750 ± 10mV (vsSHE), spray liquid pH controls 1.00 ± 0.05, and temperature controls at 30 DEG C, and upper strata bed stuffing height is 4.5cm, middle seam height is 0.5cm, intermediate filler layer height is 0.5cm, and lower floor's bed stuffing height is that 4.5cm, PVC shell internal diameter is 4.5cm, filler is granulated glass sphere, utilize said apparatus to react, sample every 12h, measure Cu in leach liquor with ICP-OES
2+concentration, calculates the leaching yield X of Cu according to X=C*V/ (G*a) * 100%.Utilize the kinetic equation 1-(1-X) in shrinking core model respectively
1/3, 3-2X-3 (1-X)
2/3, 1-(1-X)
1/3+ B [3-2X-3 (1-X)
2/3] carry out matching, result is as shown in Figure 4, Figure 5 and Figure 6.
As can be seen from Fig. 4, Fig. 5 and Fig. 6, Fig. 4 is reaction controlling matching, linearly poor and without initial point, and Fig. 5 is that internal diffusion controls matching, although linear coefficient R
2very high, but without initial point, therefore fitting effect is bad, Fig. 6 is the fitting result of mixture control kinetic equation, linearly dependent coefficient R
2=0.995 and through initial point, compare other two fitting of a straight line better effects if, illustrate and well met Hybrid Control Model, available reaction rate constant K=0.00133h from Fig. 6
-1, it is defined as K
1.From mixture control kinetics fit equation good linearity, cross initial point, from leaching to end 0 ~ 12h all meet shrinking core model.
Embodiment 2:
Certain secondary copper sulfide minal 2g, granularity 30 ~ 55 μm accounts for 75%, and spray liquid adopts concentration to be the Fe of 20g/L
2(SO
4)
3solution 200ml, Spraying rates is 3ml/min, solution O RP controls at 750mV ± 10mV (vsSHE), pH value of solution controls 1.00 ± 0.05, temperature controls at 45 DEG C, upper strata bed stuffing height is 7cm, and middle seam height is 0.4cm, and intermediate filler layer height is 1.1cm, lower floor's bed stuffing height is 7cm, PVC shell internal diameter is 6cm, and filler is quartz sand, utilizes said apparatus to react, reaction sampling in early stage is comparatively intensive, elongated (, every 1h, 10 ~ 50h is every 3h for 0 ~ 10h) samples at later time interval, measures Cu in leach liquor with ICP-OES
2+concentration, calculates the leaching yield X of Cu according to X=C*V/ (G*a) * 100%.Utilize the kinetic equation 1-(1-X) in shrinking core model respectively
1/3, 3-2X-3 (1-X)
2/3, 1-(1-X)
1/3+ B [3-2X-3 (1-X)
2/3] carry out matching, result is as shown in Figure 7, Figure 8 and Figure 9.
As can be seen from Fig. 7, Fig. 8 and Fig. 9, Fig. 7 is reaction controlling matching, linearly poor and without initial point, and Fig. 8 is that internal diffusion controls matching, although linear coefficient R
2very high, but without initial point, therefore fitting effect is bad, Fig. 9 is the fitting result of mixture control kinetic equation, utilizes the linearly dependent coefficient R of Hybrid Control Model matching gained straight line
2=0.999 and through initial point, compare other two fitting of a straight line better effects if, illustrate and well met Hybrid Control Model, available reaction rate constant K=0.0068h from Fig. 9
-1, it is defined as K
2.From mixture control kinetics fit equation good linearity, cross initial point, from leaching to end 0 ~ 45h all meet shrinking core model.
Embodiment 3:
Certain secondary copper sulfide minal 1g, granularity 30 ~ 55 μm accounts for 75%, and spray liquid adopts concentration to be the Fe of 5g/L
2(SO4)
3solution 300ml, Spraying rates is that 10ml/min, solution O RP control at 750mV ± 10mV (vsSHE), pH value of solution controls 1.00 ± 0.05, and temperature controls at 60 DEG C, and upper strata bed stuffing height is 3cm, middle seam height is 0.3cm, intermediate filler layer height is 0.5cm, and lower floor's bed stuffing height is that 3cm, PVC shell internal diameter is 4cm, filler is quartz sand, utilize said apparatus to react, sample every about 1h, measure Cu in leach liquor with ICP-OES
2+concentration, calculates the leaching yield X of Cu according to X=C*V/ (G*a) * 100%.Utilize the kinetic equation 1-(1-X) in shrinking core model respectively
1/3, 3-2X-3 (1-X)
2/3, 1-(1-X)
1/3+ B [3-2X-3 (1-X)
2/3] carry out matching, result is as shown in Figure 10, Figure 11 and Figure 12.
As can be seen from Figure 10, Figure 11 and Figure 12, Figure 10 is reaction controlling matching, linearly poor and without initial point, and Figure 11 is that internal diffusion controls matching, although linear coefficient R
2very high, but without initial point, therefore fitting effect is bad, Figure 12 is the fitting result of mixture control kinetic equation, utilizes the linearly dependent coefficient R of Hybrid Control Model matching gained straight line
2=0.999 and through initial point, compare other two fitting of a straight line better effects if, illustrate and well met Hybrid Control Model, available reaction rate constant K=0.02329h from Figure 12
-1, and it is defined as K
3.From mixture control kinetics fit equation good linearity, cross initial point, from leaching to end 0 ~ 240h all meet shrinking core model.
Embodiment 4:
Utilize the reaction rate constant k that the experimental result in embodiment 1,2,3 obtains
1, k
2, k
3, carry out matching in conjunction with Arrhenius equation, K is reaction rate constant, and T is temperature of reaction, and can obtain the activation energy that this Secondary Sulfide under leaching condition dissolves in acid ferrum sulfuricum oxydatum solutum, result as shown in figure 13.In figure, X-coordinate is 1/T*1000; Ordinate zou is LnK, K is reaction rate constant, K required namely
1, K
2, K
3, matching obtains straight line, and the slope * R of activation energy=straight line, R are universal constant 8.314J/ (mol*K).
As seen from Figure 13, matching obtains straight line, and linear coefficient is 0.994, and activation energy is 80.17KJ/mol.The mixture control that this secondary copper sulfide mineral dissolving in acid ferrum sulfuricum oxydatum solutum is taken as the leading factor by chemical reaction under leaching condition can be judged according to activation energy size and the matching of retract mixture control.
It should be noted last that, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted.Although with reference to embodiment to invention has been detailed description, will be understood by those skilled in the art that, modify to technical scheme of the present invention or equivalent replacement, do not depart from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (10)
1. meet a post leaching method for shrinking core model, said method comprising the steps of:
1) constant temperature constant potential post bath unit is utilized, first upper strata packing layer and lower floor's packing layer are adopted PVC shell splendid attire respectively, middle seam and intermediate filler layer splendid attire in same PVC shell, then are filled in leaching ore pillar body according to upper strata packing layer, middle seam, intermediate filler layer and lower floor's packing layer successively;
2) spray liquid spray upper strata packing layer, after the even distribution again of upper strata filler, with middle seam contact reacts, flow in liquid-collecting bottle after intermediate filler layer and lower floor's packing layer after reaction, the solution of the constant temperature in liquid-collecting bottle, constant potential and permanent pH value sprays upper strata packing layer as spray liquid again through recycle pump from top spray head;
Described step 1) in PVC shell internal diameter be 4 ~ 6cm, in middle seam, minal add-on is 1 ~ 2g;
Described step 2) in the amount ratio of minal add-on and spray liquid be 1:100 ~ 1:300, spray liquid concentration is 5 ~ 20g/L, and Spraying rates is 3 ~ 10mL/min.
2. the post leaching method meeting shrinking core model according to claim 1, is characterized in that, described middle seam height≤0.5cm, middle seam and intermediate filler layer total height are 0.8 ~ 1.5cm.
3. the method meeting post leaching shrinking core model according to claim 1, it is characterized in that, the height of described upper strata packing layer and lower floor's packing layer is 3 ~ 7cm.
4. the post leaching method meeting shrinking core model according to claim 1, is characterized in that, the filler in described upper strata packing layer, intermediate filler layer and lower floor's packing layer is granulated glass sphere or quartz sand.
5. the post leaching method meeting shrinking core model according to claim 1, is characterized in that, controlled the redox potential of spray liquid by redox potential on-line monitoring device and hydrogen peroxide, controlled oxidization reduction potential fluctuation range is ± 10mV.
6. the post leaching method meeting shrinking core model according to claim 1, is characterized in that, is measured the pH of solution in liquid-collecting bottle by pH meter interval, and regulates pH that its fluctuation range is controlled as ± 0.05 by acid-base solution.
7. the post leaching method meeting shrinking core model according to claim 1, is characterized in that, keeps leaching the homo(io)thermism in post by heating in water bath chuck layer, is kept the homo(io)thermism of solution in liquid-collecting bottle by oil bath heating.
8. the post leaching method meeting shrinking core model according to claim 1, it is characterized in that, the temperature in described liquid-collecting bottle maintains 30 ~ 60 DEG C.
9. the post leaching method meeting shrinking core model according to claim 1, it is characterized in that, described middle seam mixes with quartz sand.
10. the post leaching method meeting shrinking core model according to claim 1, is characterized in that, the sieve plate (9) of described PVC shell arranges several round sieves (8).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4701309A (en) * | 1984-11-30 | 1987-10-20 | Umetco Minerals Corporation | Method of operating a heap leach for recovering uranium and vanadium |
| CN202047109U (en) * | 2011-01-12 | 2011-11-23 | 紫金矿业集团股份有限公司 | Ore leaching test device |
| CN203569160U (en) * | 2013-10-31 | 2014-04-30 | 中国科学院过程工程研究所 | Constant-temperature and constant-potential column leaching experiment device |
-
2014
- 2014-08-21 CN CN201410416184.XA patent/CN105349775B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4701309A (en) * | 1984-11-30 | 1987-10-20 | Umetco Minerals Corporation | Method of operating a heap leach for recovering uranium and vanadium |
| CN202047109U (en) * | 2011-01-12 | 2011-11-23 | 紫金矿业集团股份有限公司 | Ore leaching test device |
| CN203569160U (en) * | 2013-10-31 | 2014-04-30 | 中国科学院过程工程研究所 | Constant-temperature and constant-potential column leaching experiment device |
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