CN102676845A - Filter residue obtained after purifying zinc liquid and preparation method of filter residue - Google Patents
Filter residue obtained after purifying zinc liquid and preparation method of filter residue Download PDFInfo
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- CN102676845A CN102676845A CN2012101378615A CN201210137861A CN102676845A CN 102676845 A CN102676845 A CN 102676845A CN 2012101378615 A CN2012101378615 A CN 2012101378615A CN 201210137861 A CN201210137861 A CN 201210137861A CN 102676845 A CN102676845 A CN 102676845A
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Abstract
The invention discloses a filter residue obtained after purifying zinc liquid and a preparation method of the filter residue. Solid zinc with high purity in the filter residue can be used as a zinc powder raw material adopted in use of a zinc powder displacement method during zinc liquid purification; and the weight ratio of solid cadmium to solid zinc in the filter residue is less than 1*10<-5>. The filter residue is obtained by the following zinc liquid purification method consisting of the following steps of: (1) performing colloid removal treatment on neutral lixivium or supernatant obtained by precipitating the neutral lixivium to obtain zinc liquid with colloid content of below 50 mg/L; (2) performing first-section purification on the zinc liquid to at least remove copper and cadmium through a first-time zinc powder displacement method; (3) performing solid-liquid separation filtration on the zinc liquid containing solid impurities of copper and cadmium, wherein the filtration time is controlled within 60 minutes, and filtration accuracy is controlled to be below 10 microns; (4) performing second-section purification on the zinc liquid after the solid-liquid separation filtration to at least remove cobalt and nickel; and (5) performing solid-liquid separation filtration on the zinc liquid containing solid impurities of cobalt and nickel to obtain new liquid and filter residue respectively.
Description
Technical field
The present invention relates to solution of zinc sulfate (the calling zinc liquid in the following text) purification process in the zinc hydrometallurgy, be specifically related to the impurity in the neutral leach liquor is removed to the limit of regulation, when satisfying electrolytic deposition to the process of new liquid requirement.
Background technology
Existing zinc liquid purifying method is neutral leach liquor to be imported in the thickener to carry out concentration earlier mostly, and then the supernatant after the concentration (supernatant promptly) is carried out zinc dust precipitation handle.Such as; The accompanying drawing 1 of CN101994005A promptly shows supernatant is successively carried out three sections purifications, and first section purifies copper removal, and second section purification removes cobalt, nickel; The 3rd section purification removes cadmium, and all obtains the process of the zinc liquid after the removal of impurities through the solid-liquid separating and filtering after each section purification.
The zinc factory that also has directly carries out zinc dust precipitation with neutral leach liquor and handles.Such as, promptly show in the schema of " the clean liquid technological design of electrolytic zinc plant zinc, Yang Lian; engineering design and research, total the 119th phase, in June, 2006 " literary composition neutral leach liquor is successively carried out three sections purifications; First section purifies copper removal, cadmium; Second section purification removes cobalt, nickel, and the 3rd section purification removes cadmium once more, and all obtains the process of the zinc liquid after the removal of impurities through the solid-liquid separating and filtering after each section purification.
In a word; Show from the present research tendency that reflects zinc liquid purification process; People often concentrate on the zinc dust precipitation process to the improvement of zinc liquid purification process, and the supernatant that before replacement(metathesis)reaction begins, just neutral leach liquor or neutral leach liquor post precipitation is obtained handle aspect seldom relate to.
Nonetheless, the deep purifying problem of cadmium does not thoroughly solve all the time.Wherein, the filtering element when important reason is that existing zinc liquid scavenging process all adopts filter cloth basically as the solid-liquid separating and filtering, and the filtering accuracy of general filter cloth is limited, causes cadmium to wear filter easily; Simultaneously, the cadmium that displaces is anti-especially easily again to be dissolved.Therefore, two pieces of reference papers that provide have above all been taked three sections purification process, and final stage purifies and all to relate to except that cadmium, and visible its basic goal still wants to improve the purification level of cadmium.Obviously, the flow process of three sections purification process is longer, and will consume a large amount of zinc powders.
Summary of the invention
The technical problem that the present invention is intended to solve at first provides a kind of zinc liquid and removes cadmium technology in purifying, and removes the cadmium effect preferably to reach.Secondly, a kind of zinc liquid purifying method of ideal purification effect also will be provided in the present invention and by the resulting filter residue of this method, the solid zinc that this filter residue moderate purity is higher is so that later use.
At first, the step that comprises except that cadmium technology during zinc liquid of the present invention purifies is: 1) remove the colloid processing to neutral leach liquor or by the supernatant that neutral leach liquor post precipitation obtains, obtaining colloidal content is the zinc liquid below the 50mg/L; 2) in zinc liquid, displace cadmium at least through zinc replacement; 3) the zinc liquid that contains inpurity cadmium is carried out the solid-liquid separating and filtering, wherein, filtration time was controlled in 60 minutes, filtering accuracy is controlled at below 10 microns.
Colloid in neutral leach liquor or the supernatant that obtained by neutral leach liquor post precipitation is mainly materials such as silica gel, iron glue, and these colloidalmaterials exist with the form of reuniting in zinc liquid.Colloidal content in general in the supernatant is about about 1g/L, and the colloidal content in the neutral leach liquor is then bigger.Since the existence of these colloidalmaterials, the one, reduced the zinc dust precipitation effect, the 2nd, hinder the solid-liquid separating and filtering, thereby influenced the effect of removing cadmium greatly.In view of this; The elder generation that taked of the invention property removes the colloid processing to neutral leach liquor or supernatant; And then the mode through zinc replacement reinforcing-liquid separating and filtering; And filtration time, these key parameters of filtering accuracy when removing colloid and handle colloidal content and the solid-liquid separating and filtering in the zinc liquid of back have carried out selecting collocation, have confirmed the final cadmium technology of removing.Before the present invention; After carrying out one section purification through zinc replacement to neutral leach liquor or by the supernatant that neutral leach liquor post precipitation obtains in order to remove cadmium, again through the cadmium content in the prepared zinc liquid of solid-liquid separating and filtering generally about 20～50mg/L; Test shows, carry out one section purification through zinc replacement to neutral leach liquor or by the supernatant that neutral leach liquor post precipitation obtains among the present invention after, the content of cadmium ion is below the 2mg/L in the zinc liquid that makes through the solid-liquid separating and filtering again.
Remove in the step 1) of cadmium technology in the present invention, can realize removing colloid through different modes and handle.For example, can in zinc liquid, add flocculation agent or ionogen and make the colloidalmaterial deposition.But as preferred version, this step 1) realizes through neutral leach liquor or supernatant are carried out membrane filtration.Membrane filtration not only can remove the colloidalmaterial in the dezincify liquid, can also remove ZnFeO
2Deng solid impurity, make the preceding zinc liquid quality of replacement(metathesis)reaction better, further improve zinc liquid decontamination effect improving.Form too fast and reduce filtration flux for fear of filter cake, this step 1) preferably realizes through neutral leach liquor or supernatant are carried out crossflow membrane filtration.Cross flow filter has special effect to removing colloid: the shearing force of cross flow filter can effectively prevent colloid attached to cartridge surface, thereby reduces the thickness of cake layer, guarantees filtration flux.
Above-mentioned steps 3) membrane filtration is adopted in suggestion equally.For ease of realizing quick filtration, wherein preferably adopt the terminal membrane filtration.
Zinc liquid purifying method of the present invention, the step that comprises is: 1) remove the colloid processing to neutral leach liquor or by the supernatant that neutral leach liquor post precipitation obtains, obtaining colloidal content is the zinc liquid below the 50mg/L; 2) through the first time zinc replacement zinc liquid carried out one section purify copper removal, cadmium at least; 3) the zinc liquid that contains solid impurity copper, cadmium is carried out the solid-liquid separating and filtering, wherein, filtration time was controlled in 60 minutes, filtering accuracy is controlled at below 10 microns; 4) the zinc liquid behind the solid-liquid separating and filtering is carried out two sections purifications and remove cobalt, nickel at least; 5) the zinc liquid that contains solid impurity cobalt, nickel is carried out the solid-liquid separating and filtering, obtain new liquid and filter residue respectively.
Test shows, is Cu:Cd:Co:Zn=(0.01～0.2) with the weight ratio of solid zinc respectively by copper, cadmium, three kinds of solid matters of cobalt in the resulting filter residue of aforesaid method: (0～0.001): (0.5～1.5): 100.It is thus clear that the weight ratio of solid cadmium and solid zinc is less than 1 * 10 in this filter residue
-5, cadmium content is extremely low.
In the above-mentioned zinc liquid purifying method, both can carry out two sections purifications to zinc liquid and remove cobalt, nickel, also can add xanthate, β-Nai Fen except that cobalt, nickel through the zinc replacement second time.
Based on alleged cause, said step 1) realizes through neutral leach liquor or supernatant are carried out membrane filtration.
Based on alleged cause, said step 1) realizes through neutral leach liquor or supernatant are carried out crossflow membrane filtration.
As further improvement to above-mentioned zinc liquid purifying method, with the filter residue of gained in the step 5) as carrying out the employed zinc powder raw material of zinc replacement in the above-mentioned steps.After carrying out the solid-liquid separating and filtering through one section purification and to the zinc liquid that contains solid impurity copper, cadmium; The content of cadmium ion the earth to the utmost descends in the zinc liquid that filters out; Therefore; Through only containing the cadmium of minute quantity in two sections filter residues that purify and the zinc liquid that contains solid impurity cobalt, nickel carried out the solid-liquid separating and filtering; In this case, can this filter residue be turned back in the step of front as carrying out the employed zinc powder raw material of zinc replacement fully, thereby under the situation that hardly zinc liquid scavenging process is caused any disadvantageous effect (mainly being in zinc liquid, to introduce inpurity cadmium hardly), reduce the consumption of zinc powder significantly.In the past, because cadmium content is higher in the filter residue after the purification of zinc liquid, so those skilled in the art can not use this filter residue as the zinc powder raw material.
Wherein, for said step 3) and step 4), adopted membrane filtration in the step 3) at least.
Wherein, for said step 3) and step 4), adopted the terminal membrane filtration at least in the step 3).
A kind of zinc liquid provided by the present invention purifies back gained filter residue, and wherein the weight ratio of solid cadmium and solid zinc is less than 1 * 10
-5
This filter residue is the zinc powder raw material that is adopted when using zinc replacement in purifying as zinc liquid.
This filter residue is resultant by following zinc liquid purifying method, and the step that this method comprises is: 1) remove the colloid processing to neutral leach liquor or by the supernatant that neutral leach liquor post precipitation obtains, obtaining colloidal content is the zinc liquid below the 50mg/L; 2) through the first time zinc replacement zinc liquid carried out one section purify copper removal, cadmium at least; 3) the zinc liquid that contains solid impurity copper, cadmium is carried out the solid-liquid separating and filtering, wherein, filtration time was controlled in 60 minutes, filtering accuracy is controlled at below 10 microns; 4) the zinc liquid behind the solid-liquid separating and filtering is carried out two sections purifications and remove cobalt, nickel at least; 5) the zinc liquid that contains solid impurity cobalt, nickel is carried out the solid-liquid separating and filtering, obtain new liquid and filter residue respectively.
Wherein, said step 1) realizes through neutral leach liquor or supernatant are carried out membrane filtration.
Wherein, said step 1) realizes through neutral leach liquor or supernatant are carried out crossflow membrane filtration.
Further be that to obtain colloidal content after colloid is handled be the zinc liquid below the 10mg/L through neutral leach liquor or supernatant are removed in the said step 1).
Wherein, through the second time zinc replacement zinc liquid carried out two sections purifications remove cobalt, nickel at least.
Wherein, for said step 3) and step 4), adopted membrane filtration in the step 3) at least.
Wherein, for said step 3) and step 4), adopted the terminal membrane filtration at least in the step 3).
Above-mentioned zinc liquid purifies the preparation method of back gained filter residue, and the step that comprises is: 1) remove the colloid processing to neutral leach liquor or by the supernatant that neutral leach liquor post precipitation obtains, obtaining colloidal content is the zinc liquid below the 50mg/L; 2) through the first time zinc replacement zinc liquid carried out one section purify copper removal, cadmium at least; 3) the zinc liquid that contains solid impurity copper, cadmium is carried out the solid-liquid separating and filtering, wherein, filtration time was controlled in 60 minutes, filtering accuracy is controlled at below 10 microns; 4) the zinc liquid behind the solid-liquid separating and filtering is carried out two sections purifications and remove cobalt, nickel at least; 5) the zinc liquid that contains solid impurity cobalt, nickel is carried out the solid-liquid separating and filtering, obtain new liquid and filter residue respectively.
Description of drawings
Fig. 1 is the process flow sheet of zinc liquid purifying method embodiment of the present invention.
Embodiment
The content of copper, cadmium, cobalt ion is respectively 400mg/L, 550mg/L, 25mg/L in the supernatant that the neutral leach liquor post precipitation of certain zinc factory obtains, and through surveying, the colloidal content in this solution is about 1g/L.This zinc factory adopts at present three sections purification process, at first, through the first time zinc replacement supernatant carried out one section purify copper removal, cadmium at least; Then, the zinc liquid that contains solid impurity copper, cadmium is carried out the solid-liquid separating and filtering, adopt flame filter press during filtration, the filtering accuracy of filter cloth is the 40-50 micron in this flame filter press, and filtration time is 60 minutes; After this, through the second time zinc replacement zinc liquid carried out two sections purifications remove cobalt, nickel at least; Then, the zinc liquid that contains solid impurity cobalt, nickel is carried out the solid-liquid separating and filtering, adopt identical flame filter press during filtration, filtration time is 40 minutes; After this, through zinc replacement for the third time zinc liquid is carried out three sections purifications again and remove cadmium at least; Adopt identical flame filter press that the zinc liquid that contains the solid impurity cadmium is carried out the solid-liquid separating and filtering then, obtain new liquid and filter residue respectively.Through surveying, the content of copper, cadmium, cobalt ion is respectively 12mg/L, 50mg/L, 20mg/L in the zinc liquid after one section purifies and filters; Two sections content that purify and filter copper, cadmium, cobalt ion in the zinc liquid of back are respectively 0.4mg/L, 2.0mg/L, 1.5mg/L; Three sections content that purify and filter copper, cadmium, cobalt ion in the zinc liquid of back are respectively 0.1mg/L, 0.8mg/L, 1.0mg/L.
As shown in Figure 1, the present invention is directed to same supernatant and adopted following method, the steps include: 1) adopted crossflow membrane filtration that supernatant is removed the colloid processing, obtaining colloidal content is the zinc liquid below the 50mg/L; 2) through the zinc replacement first time (adopting the processing condition of existing zinc replacement copper removal, cadmium) zinc liquid is carried out one section and purify copper removal, cadmium at least; 3) adopted the terminal membrane filtration that the zinc liquid that contains solid impurity copper, cadmium is carried out the solid-liquid separating and filtering, wherein, filtration time had been controlled in 60 minutes, filtering accuracy has been controlled at below 10 microns; 4) through the zinc replacement second time (adopting existing zinc replacement to remove the processing condition of cobalt, nickel) the zinc liquid behind the solid-liquid separating and filtering is carried out two sections purifications and remove cobalt, nickel at least; 5) adopt the terminal membrane filtration that the zinc liquid that contains solid impurity cobalt, nickel is carried out the solid-liquid separating and filtering, obtained new liquid and filter residue respectively; Thereby this filter residue turns back to one section purification and two sections cleaning sections as carrying out the employed zinc powder raw material of zinc replacement in the above-mentioned steps; Filter the slag that produces in the whole zinc liquid scavenging process and pass through the discharging of terminal membrane filtration outlet for the first time.Below through 5 groups of embodiment (numbering 1～5) zinc liquid purifying method of the present invention is done specifying, details is seen table 1.
In addition; Through surveying; Copper, cadmium, three kinds of solid matters of cobalt are Cu:Cd:Co:Zn=(0.01～0.2) with the weight ratio of solid zinc respectively in the filter residue of above-mentioned 5 groups of embodiment behind two sections cleaning sections: (0～0.001): (0.5～1.5): 100, promptly in the filter residue weight ratio of solid cadmium and solid zinc all less than 1 * 10
-5, cadmium content is extremely low.
Specify:
1, above-mentioned term " filtration time " be meant specified quantitative zinc liquid from beginning to be filled into the time that whole filtrations are accomplished.
2, can adopt methods such as weighting method in the turbidity measurement, spectrophotometry to measure to the colloidal content of zinc liquid.
Table 1
Annotate: " calm " refers to detect less than this element through polarograph.
Claims (10)
1. zinc liquid purifies back gained filter residue, and it is characterized in that: the weight ratio of solid cadmium and solid zinc is less than 1 * 10 in this filter residue.
2. zinc liquid as claimed in claim 1 purifies back gained filter residue, it is characterized in that: this filter residue is the zinc powder raw material that is adopted when using zinc replacement in purifying as zinc liquid.
3. according to claim 1 or claim 2 zinc liquid purifies back gained filter residue; It is characterized in that: this filter residue is resultant by following zinc liquid purifying method; The step that this method comprises is: 1) remove the colloid processing to neutral leach liquor or by the supernatant that neutral leach liquor post precipitation obtains, obtaining colloidal content is the zinc liquid below the 50mg/L; 2) through the first time zinc replacement zinc liquid carried out one section purify copper removal, cadmium at least; 3) the zinc liquid that contains solid impurity copper, cadmium is carried out the solid-liquid separating and filtering, wherein, filtration time was controlled in 60 minutes, filtering accuracy is controlled at below 10 microns; 4) the zinc liquid behind the solid-liquid separating and filtering is carried out two sections purifications and remove cobalt, nickel at least; 5) the zinc liquid that contains solid impurity cobalt, nickel is carried out the solid-liquid separating and filtering, obtain new liquid and filter residue respectively.
4. zinc liquid as claimed in claim 3 purifies back gained filter residue, it is characterized in that: said step 1) realizes through neutral leach liquor or supernatant are carried out membrane filtration.
5. zinc liquid as claimed in claim 4 purifies back gained filter residue, it is characterized in that: said step 1) realizes through neutral leach liquor or supernatant are carried out crossflow membrane filtration.
6. zinc liquid as claimed in claim 3 purifies back gained filter residue, it is characterized in that: it is characterized in that: to obtain colloidal content after the colloid processing be the zinc liquid below the 10mg/L through neutral leach liquor or supernatant are removed in the said step 1).
7. zinc liquid as claimed in claim 3 purifies back gained filter residue, it is characterized in that: through the second time zinc replacement zinc liquid carried out two sections purifications remove cobalt, nickel at least.
8. zinc liquid as claimed in claim 3 purifies back gained filter residue, for said step 3) and step 4), has adopted membrane filtration in the step 3) at least.
9. zinc liquid as claimed in claim 8 purifies back gained filter residue, for said step 3) and step 4), has adopted the terminal membrane filtration at least in the step 3).
10. claim 1 or 2 described zinc liquid purify the preparation method of back gained filter residue, and the step that comprises is: 1) remove the colloid processing to neutral leach liquor or by the supernatant that neutral leach liquor post precipitation obtains, obtaining colloidal content is the zinc liquid below the 50mg/L; 2) through the first time zinc replacement zinc liquid carried out one section purify copper removal, cadmium at least; 3) the zinc liquid that contains solid impurity copper, cadmium is carried out the solid-liquid separating and filtering, wherein, filtration time was controlled in 60 minutes, filtering accuracy is controlled at below 10 microns; 4) the zinc liquid behind the solid-liquid separating and filtering is carried out two sections purifications and remove cobalt, nickel at least; 5) the zinc liquid that contains solid impurity cobalt, nickel is carried out the solid-liquid separating and filtering, obtain new liquid and filter residue respectively.
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Cited By (4)
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| CN103194600A (en) * | 2013-04-23 | 2013-07-10 | 吴鋆 | Method for purifying zinc sulfide solution |
| CN106244813A (en) * | 2016-08-29 | 2016-12-21 | 江西铜业股份有限公司 | A kind of zinc abstraction nickel cobalt slag recoverying and utilizing method |
| CN106893872A (en) * | 2016-12-27 | 2017-06-27 | 河南豫光锌业有限公司 | A kind of method of zinc hydrometallurgy deeply purifying and removing cobalt |
| CN107012326A (en) * | 2017-03-29 | 2017-08-04 | 四环锌锗科技股份有限公司 | Improve the method that zinc hydrometallurgy neutrality leaches press filtration |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194600A (en) * | 2013-04-23 | 2013-07-10 | 吴鋆 | Method for purifying zinc sulfide solution |
| CN106244813A (en) * | 2016-08-29 | 2016-12-21 | 江西铜业股份有限公司 | A kind of zinc abstraction nickel cobalt slag recoverying and utilizing method |
| CN106893872A (en) * | 2016-12-27 | 2017-06-27 | 河南豫光锌业有限公司 | A kind of method of zinc hydrometallurgy deeply purifying and removing cobalt |
| CN107012326A (en) * | 2017-03-29 | 2017-08-04 | 四环锌锗科技股份有限公司 | Improve the method that zinc hydrometallurgy neutrality leaches press filtration |
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