CN102851509A - Method for recovering cadmium from flue dust of bottom-blowing furnace - Google Patents
Method for recovering cadmium from flue dust of bottom-blowing furnace Download PDFInfo
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- CN102851509A CN102851509A CN201210290669XA CN201210290669A CN102851509A CN 102851509 A CN102851509 A CN 102851509A CN 201210290669X A CN201210290669X A CN 201210290669XA CN 201210290669 A CN201210290669 A CN 201210290669A CN 102851509 A CN102851509 A CN 102851509A
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- cadmium
- cigarette ash
- bottom convertor
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses a method for recovering cadmium from flue dust of a bottom-blowing furnace and relates to the field of nonferrous metal smelting. The method comprises the following steps of leaching flue dust of a bottom-blowing furnace by water to obtain a leachate and leaching residues, feeding back the leaching residues to the bottom-blowing furnace, recovering Pb, adding zinc blocks into the leachate for replacement to obtain sponge cadmium and a displacement liquid, and sequentially adding flue dust of a bottom-blowing furnace into the displacement liquid for leaching to obtain cadmium in the flue dust. The method does not adopt sulfuric acid, avoids leaching of impurities such as arsenic and antimony, and does not produce arsine gas in displacement. Compared with the prior art, the method has better environmental benefits, realizes sponge cadmium product quality, less impurities of a zinc sulfate solution obtained by the displacement and high lead content of leaching residues, and is conducive to improvement of economic benefits of comprehensive recovery of zinc and lead.
Description
Technical field
The present invention relates to reclaim in a kind of non-ferrous metal smelting field, particularly a kind of bottom convertor cigarette ash the method for cadmium.
Background technology
SKS refining splicer skill, i.e. bottom convertor refining is plumbous, and bottom convertor cigarette ash is through circulation, and some impurity is accumulated to the production that to a certain degree is unfavorable for bottom convertor in the cigarette ash.Bottom convertor lead ore concentrate and cigarette ash composition are carried out chemical analysis, find Cd content pettiness in the lead ore concentrate, and the Cd grade must be processed about 15% in the cigarette ash, the comprehensive recovery.Metal Cd in the cigarette ash is carried out material phase analysis to be found: CdSO wherein
4Account for more than 90%.Mainly be that form with vitriol exists for the Cd in the cigarette ash, the existing technology of cadmium that reclaims in the cigarette ash generally is: acidleach adds the method for zinc dust precipitation, this method consumption acids, strengthened cost, arsenic impurities, antimony etc. also can enter cadmium sulfate solution, owing to a large amount of generate lead sulfates therefore to soak in the slag lead amount not high, in the process of zinc dust precipitation cadmium, have arsine gas to produce, owing to obtain the second-rate of cadmium silk floss after the more displacement of impurity in the liquid.
Summary of the invention
The objective of the invention is to overcome the above-mentioned deficiency of prior art and the method that reclaims cadmium is provided in a kind of bottom convertor cigarette ash, the present invention adopts water logging, do not use sulfuric acid, the impurity such as arsenic, antimony is seldom leached, and the displacement operation does not produce arsine gas substantially, so production environment is better than prior art, the continuous good product quality of cadmium, the solution of zinc sulfate that obtains after the displacement is impure few, the leaded height of leached mud, and this is conducive to improve zinc, the plumbous comprehensive economic benefit that reclaims.
Technical scheme of the present invention is: the method that reclaims cadmium in a kind of bottom convertor cigarette ash, bottom convertor cigarette ash goes out to obtain leach liquor and leached mud by adding water logging, leached mud returns bottom convertor and reclaims Pb, leach liquor adds the spelter displacement and obtains cadmium silk floss and displacement liquid, and displacement liquid can continue to add the cadmium in the bottom convertor cigarette ash leaching bottom convertor cigarette ash.
One, bottom convertor cigarette ash Chemical Composition sees Table 1.
Table 1 bottom convertor cigarette ash chemical ingredients (%)
| Numbering | Pb | Zn | As | Sb | Cd | CdSO 4 | CdS | CdO | Cu |
| The end-1 | 46.87 | 0.50 | 0.24 | 0.029 | 14.80 | ? | ? | ? | 0.069 |
| The end-2 | 39.88 | 0.42 | 0.38 | 0.028 | 18.16 | 16.83 | 0.23 | 0.93 | 0.023 |
| Numbering | Fe | TL | Hg | Ge | Te | F | CL | S | ? |
| The end-1 | 0.23 | 0.25 | 0.00043 | Little | 0.044 | 0.0252 | 0.22 | ? | ? |
| The end-2 | 0.015 | 0.047 | 0.0004 | 0.041 | 0.081 | 0.0199 | 0.205 | 11.20 | ? |
Two, technical process determines and each operation ultimate principle and technical qualification
Bottom convertor cigarette ash leaches operation: adding water in bottom convertor cigarette ash, is that 0 ℃-60 ℃ water logging goes out CdSO with water temperature
4, the control liquid-solid ratio is 3:1, makes cadmium enter solution as far as possible, As, Sb do not leach extraction time simultaneously: 1 to 4 hour, can choose 2 hours, replace with spelter, control beginning PH2.5 ~ 3.0, more than the whole PH5.0,10 ℃-60 ℃ of temperature, 1 to 4 hour time, choose 2 hours, make zinc displace cadmium, the main chemical reactions of displacement operation is:
ZnO+?H
2SO
4=ZnSO
4+?H
2O
Zn+?CdSO
4=?Cd+?ZnSO
4
Three, test-results and analysis
Leaching condition test materials 200 grams have carried out the test of different acidity and liquid-solid ratio.Not acid adding has been carried out in the acidity test, and 1:1,2:1, four gradient condition tests of 3:1,4:1 have been carried out in following three gradient condition test of PH2.0, PH1.0, liquid-solid ratio test, and the acidity test-results sees Table 2.
Table 2 acidity condition test-results
| Acidity | Cd leaching yield (%) | As leaching yield (%) | Sb leaching yield (%) | Slag rate (%) |
| Acid adding not | 90.09 | Do not leach | Do not leach | 64.5 |
| PH2.0 | 89.47 | 50 | 50 | 63.75 |
| Below the PH1.0 | 95.67 | 70 | 70 | 61 |
As can be seen from Table 2, acid adding As, Sb do not leach, and can save cleaning section one, and the leaching yield of Cd can reach 90.09%, in view of to the continuous quality of cadmium, reduce cost and environmental requirement is considered, it is rational selecting not the direct water of acid adding to leach.The liquid-solid ratio test-results sees Table 3.
Table 3 liquid-solid ratio condition test result
| Liquid-solid ratio | The Cd leaching yield | Filter difficulty or ease |
| 1:1 | 85.90 | Difficulty |
| 2:1 | 81.94 | Difficulty |
| 3:1 | 88.31 | Easily |
| 4:1 | 88.29 | Easily |
As can be seen from Table 3, when liquid-solid ratio is 1:1,2:1, the leaching yield of Cd is low, the leached mud filtration difficulty, when liquid-solid ratio was 3:1,4:1, the leaching yield of Cd was suitable, and adopting the ratio of liquid and solid during leaching is that 1:1 is between the 4:1, in view of the consideration that zinc sulfate is recycled, select liquid-solid ratio 3:1 more suitable.
The test of displacement process conditions
By having carried out zinc powder and spelter displacement contrast condition test, the test-results situation sees Table 4.
Table 4 zinc powder and spelter displacement simultaneous test data sheet
As can be seen from Table 4, the zine plate displacement cadmium silk floss that produces contains Cd94.79%, and Zn1.45%, zinc dust precipitation produce the cadmium silk floss and contain Cd81.14%, Zn11.73%, zine plate replace the cadmium that produces silk floss quality be better than zinc dust precipitation far away and produce the cadmium silk floss, should adopt zine plate or spelter so cadmium is replaced.
The present invention compared with prior art has following features: the technique that water logging goes out, spelter replacement Treatment SKS cigarette ash is produced the cadmium silk floss, and flow process is simple, and is easy to implement, the cadmium rate of recovery is high, but the lead enrichment, the continuous good product quality of cadmium, good in economic efficiency, a kind of practicable method of the treatment S of can yet be regarded as KS cigarette ash
Below in conjunction with the drawings and specific embodiments detailed construction of the present invention is further described.
Description of drawings
Accompanying drawing 1 is schema of the present invention.
Embodiment
As shown in Figure 1: bottom convertor cigarette ash goes out to obtain leach liquor and leached mud by adding water logging, leached mud returns bottom convertor and reclaims Pb, leach liquor adds the spelter displacement and obtains cadmium silk floss and displacement liquid, and displacement liquid can continue to add the cadmium in the bottom convertor cigarette ash leaching bottom convertor cigarette ash.
One, bottom convertor cigarette ash Chemical Composition sees Table 1.The end-1 is bottom convertor cigarette ash, and be on November 20th, 2007 sample time; The end-2 are bottom convertor cigarette ash, and be on January 8th, 2008 sample time.The test main agents is: autogamy dilute sulphuric acid (H
2SO
4: 184g/L), analytical pure zinc powder, spelter.
Table 1 eight factory's bottom convertor cigarette ash chemical ingredientss (%)
| Numbering | Pb | Zn | As | Sb | Cd | CdSO 4 | CdS | CdO | Cu |
| The end-1 | 46.87 | 0.50 | 0.24 | 0.029 | 14.80 | ? | ? | ? | 0.069 |
| The end-2 | 39.88 | 0.42 | 0.38 | 0.028 | 18.16 | 16.83 | 0.23 | 0.93 | 0.023 |
| Numbering | Fe | TL | Hg | Ge | Te | F | CL | S | ? |
| The end-1 | 0.23 | 0.25 | 0.00043 | Little | 0.044 | 0.0252 | 0.22 | ? | ? |
| The end-2 | 0.015 | 0.047 | 0.0004 | 0.041 | 0.081 | 0.0199 | 0.205 | 11.20 | ? |
Two, technical process determines and each operation ultimate principle and technical qualification
From bottom convertor cigarette ash Chemical Composition as can be known, wherein Pb, Cd have recovery value, analyze the phase of Cd in the end-2, wherein CdSO
4Cd account for 92.68% of total Cd amount, CdSO
4Soluble in water, in the time of 0 ℃ in water solubleness be 755g/L, the solubleness in the time of 25 ℃ is 772 g/L,
Bottom convertor cigarette ash leaches operation: adding water in bottom convertor cigarette ash, is that 0 ℃-60 ℃ water logging goes out CdSO with water temperature
4, the control liquid-solid ratio is 3:1, makes cadmium enter solution as far as possible, As, Sb do not leach simultaneously, extraction time: 2 hours, with the spelter displacement, control beginning PH2.5 ~ 3.0 were more than the whole PH5.0, below the temperature 60 C, time 2 h makes zinc displace cadmium, and the main chemical reactions of displacement operation is:
ZnO+?H
2SO
4=ZnSO
4+?H
2O
Zn+?CdSO
4=?Cd+?ZnSO
4
Three, test-results and analysis
Leaching condition test materials 200 grams have carried out the test of different acidity and liquid-solid ratio.Not acid adding has been carried out in the acidity test, and 1:1,2:1, four gradient condition tests of 3:1,4:1 have been carried out in following three gradient condition test of PH2.0, PH1.0, liquid-solid ratio test, and the acidity test-results sees Table 2.
Table 2 acidity condition test-results
| Acidity | Cd leaching yield (%) | As leaching yield (%) | Sb leaching yield (%) | Slag rate (%) |
| Acid adding not | 90.09 | Do not leach | Do not leach | 64.5 |
| PH2.0 | 89.47 | 50 | 50 | 63.75 |
| Below the PH1.0 | 95.67 | 70 | 70 | 61 |
As can be seen from Table 2, acid adding As, Sb do not leach, and can save cleaning section one, and the leaching yield of Cd can reach 90.09%, in view of to the continuous quality of cadmium, reduce cost and environmental requirement is considered, it is rational selecting not the direct water of acid adding to leach.The liquid-solid ratio test-results sees Table 3.
Table 3 liquid-solid ratio condition test result
| Liquid-solid ratio | The Cd leaching yield | Filter difficulty or ease |
| 1:1 | 85.90 | Difficulty |
| 2:1 | 81.94 | Difficulty |
| 3:1 | 88.31 | Easily |
| 4:1 | 88.29 | Easily |
As can be seen from Table 3, when liquid-solid ratio was 1:1,2:1, the leaching yield of Cd was low, the leached mud filtration difficulty, and when liquid-solid ratio was 3:1,4:1, the leaching yield of Cd was suitable, in view of the consideration that zinc sulfate is recycled, selected liquid-solid ratio 3:1 more suitable.
The test of displacement process conditions
By having carried out zinc powder and spelter displacement contrast condition test, the test-results situation sees Table 4.
Table 4 zinc powder and spelter displacement simultaneous test data sheet
As can be seen from Table 4, the zine plate displacement cadmium silk floss that produces contains Cd94.79%, and Zn1.45%, zinc dust precipitation produce the cadmium silk floss and contain Cd81.14%, Zn11.73%, zine plate replace the cadmium that produces silk floss quality be better than zinc dust precipitation far away and produce the cadmium silk floss, should adopt zine plate so cadmium is replaced.
The whole process round-robin test
The test portion of whole process round-robin test is SKS cigarette ash (end-2) 1000 grams, Cd grade 18.16% and (end-1) 1000 grams, Cd grade 14.80%.(end-2) cigarette ash is done the first five cycle, and (end-1) cigarette ash is done rear five cycles, why gets the cigarette ash of one high and one low two kinds of grades and does experiment, and wants exactly to do between the different cigarette ash of grade a comparison.
The technical indicator such as leaching yield, the rate of recovery
The technical indicator such as leaching yield, rate of recovery contrast situation sees Table 5
Table 5 leaching yield, rate of recovery index contrast information slip
| Cycle | Cd leaching yield (%) | The Cd rate of recovery (%) | Cd direct yield (%) | Slag rate (%) |
| The first five cycle | 85.37 | 84.81 | 84.79 | 67.25 |
| Rear five cycles | 85.69 | 82.35 | 82.35 | 75.20 |
| Total ten cycles | 85.46 | 83.68 | 83.63 | 71.22 |
As can be seen from Table 5, it is lower to contain Cd grade low the test portion rate of recovery, direct yield, and the slag rate is higher.
The product Chemical Composition
The continuous product Chemical Composition of each cycle cadmium sees Table 6,1-10 cycle whole process test displacement liquid zinc accumulation sees Table 7, the average Chemical Composition of other product sees Table 8, as known from Table 6, ten cycle master composition average out to 90.75%(cadmium silk flosses are oven for drying, and some cadmium is oxidized, and actual cadmium grade should be more than 90.75%), Zn average out to 1.79%, the content of the impurity such as Pb, As, Cu, Fe is all lower.
The continuous product Chemical Composition of each cycle cadmium of table 6 whole process round-robin test
| Cycle | Cd(%) | Zn(%) | Pb(%) | As(%) | Cu(%) | Fe(%) |
| 1 | 88.42 | 1.24 | 0.0608 | Little | Little | 0.011 |
| 2 | 96.61 | 1.25 | 0.10 | Little | Little | Little |
| 3 | 95.75 | 2.01 | 0.10 | Little | 0.10 | Little |
| 4 | 89.86 | 2.27 | 0.10 | Little | Little | Little |
| 5 | 88.75 | 2.34 | 0.11 | Little | Little | 0.0072 |
| 6 | 91.10 | 1.99 | 0.076 | Little | Little | Little |
| 7 | 88.60 | 1.36 | 0.057 | Little | Little | Little |
| 8 | 89.18 | 1.52 | 0.067 | Little | Little | 0.0048 |
| 9 | 87.52 | 1.69 | 0.074 | Little | Little | Little |
| 10 | 91.74 | 2.21 | 0.15 | Little | 0.0468 | 0.0098 |
| On average | 90.75 | 1.79 | 0.089 | Little | 0.073 | 0.0087 |
Table 7 1-10 cycle whole process test displacement liquid zinc accumulation table
| Cycle | Quantity (mL) | Contain zinc (g/L) | Zinc amount (g) | Cycle | Quantity (mL) | Contain zinc (g/L) | Zinc amount (g) |
| 1 | 525 | 13.55 | 7.11 | 6 | 500 | 74.22 | 37.11 |
| 2 | 600 | 40.03 | 24.02 | 7 | 520 | 81.49 | 42.37 |
| 3 | 560 | 62.75 | 35.14 | 8 | 550 | 76.16 | 41.89 |
| 4 | 520 | 71.43 | 37.14 | 9 | 370 | 93.86 | 34.73 |
| 5 | 490 | 65.44 | 32.06 | 10 | 450 | 76.68 | 34.51 |
Zinc amount from top 1-10 cycle displacement liquid, the accumulation of 1-3 cycle zinc is more obvious, the accumulation of 3-10 cycle zinc is just reacted not out, the 9-10 cycle also descends to some extent, why can this situation appear in sample? because each cycle displacement liquid sampling 100mL of chemical examination, the amount of solution of original displacement liquid is just few, each periodic sampling loss 100mL, 10 cycles get off, the loss of zinc amount is just large, if small-sized production just can this situation not occur, the zinc accumulation just can reflect in the displacement liquid.
Table 8 1-10 cycle whole process is tested the average Chemical Composition of other product
| Title | Cd | Zn | As | Sb | Cu | Fe | Mn | Ni | Co | Pb | F | Cl | Ge |
| Leach liquor (g/L) | 46.08 | ? | 0.05 | ? | ? | 0.0019 | ? | ? | ? | ? | ? | ? | ? |
| Leached mud (g/L) | 3.40 | ? | 0.51 | ? | ? | 0.45 | ? | ? | ? | 58.32 | ? | ? | ? |
| Displacement liquid (g/L) | 0.295 | 65.56 | Little | Little | Little | Little | Little | Little | Little | Little | Little | Little | Little |
As can be seen from Table 8, the impurity of displacement liquid is all very low, if Zn has been accumulated to a certain degree, can directly advance electric Zn system, or produces the zinc sulfate product after further removing cadmium.
The method that reclaims cadmium in the bottom convertor cigarette ash adopts the technique that water logging goes out, spelter replacement Treatment SKS cigarette ash is produced the cadmium silk floss, and flow process is simple, and is easy to implement, the cadmium rate of recovery is high, but the lead enrichment, the continuous good product quality of cadmium, good in economic efficiency, a kind of practicable method of the treatment S of can yet be regarded as KS cigarette ash.
Claims (5)
1. reclaim the method for cadmium in the bottom convertor cigarette ash, it is characterized in that: bottom convertor cigarette ash goes out to obtain leach liquor and leached mud by adding water logging; Leached mud returns bottom convertor and reclaims Pb; Leach liquor adds the spelter displacement and obtains cadmium silk floss and displacement liquid; Displacement liquid can continue to add the cadmium in the bottom convertor cigarette ash leaching bottom convertor cigarette ash.
2. reclaim the method for cadmium in a kind of bottom convertor cigarette ash according to claim 1, it is characterized in that:
Bottom convertor cigarette ash Chemical Composition content drops between the end-1 and the end-2;
Table 1 bottom convertor cigarette ash chemical ingredients (%).
3. reclaim the method for cadmium in a kind of bottom convertor cigarette ash according to claim 1 and 2, it is characterized in that: in bottom convertor cigarette ash, add water, go out CdSO with 10 ℃ of-60 ℃ of water loggings
4, control liquid-solid ratio be 1:1 between the 4:1, extraction time is 1-4 hour, replaces with zinc.
4. reclaim the method for cadmium in a kind of bottom convertor cigarette ash according to claim 1 and 2, it is characterized in that: the zinc that is used for displacement is spelter or zine plate.
5. reclaim the method for cadmium in a kind of bottom convertor cigarette ash according to claim 1 and 2, it is characterized in that: the best 3:1 of being of liquid-solid ratio, extraction time the best is 2 hours.
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| CN201210290669XA CN102851509A (en) | 2012-08-15 | 2012-08-15 | Method for recovering cadmium from flue dust of bottom-blowing furnace |
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|---|---|---|---|
| CN201210290669XA CN102851509A (en) | 2012-08-15 | 2012-08-15 | Method for recovering cadmium from flue dust of bottom-blowing furnace |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105200242A (en) * | 2015-10-27 | 2015-12-30 | 中南大学 | Method for revering cadmium from arsenic-containing lead-smelting oxygen bottom-blown furnace dust |
| CN105925808A (en) * | 2016-04-28 | 2016-09-07 | 河南金利金铅集团有限公司 | Method for improving grade of by-product sponge cadmium in heptahydrate production |
| CN105925810A (en) * | 2016-04-21 | 2016-09-07 | 西北矿冶研究院 | Method for preparing sponge cadmium from cadmium rectification alkaline residue |
| CN108913910A (en) * | 2018-07-18 | 2018-11-30 | 河南金利金铅集团有限公司 | A kind of method that lead smelts the recycling of bottom convertor cigarette ash cadmium metal |
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| GB392374A (en) * | 1932-06-29 | 1933-05-18 | American Smelting Refining | Improvements relating to a process for separating cadmium from material containing cadmium and other metals or compounds thereof |
| GB419507A (en) * | 1933-03-29 | 1934-11-13 | American Smelting Refining | Process for producing cadmium |
| CN101255502A (en) * | 2008-04-02 | 2008-09-03 | 河南豫光金铅股份有限公司 | Process for comprehensive recovery of indium, cadmium, thallium and zinc from lead system smoke |
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2012
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| GB392374A (en) * | 1932-06-29 | 1933-05-18 | American Smelting Refining | Improvements relating to a process for separating cadmium from material containing cadmium and other metals or compounds thereof |
| GB419507A (en) * | 1933-03-29 | 1934-11-13 | American Smelting Refining | Process for producing cadmium |
| CN101255502A (en) * | 2008-04-02 | 2008-09-03 | 河南豫光金铅股份有限公司 | Process for comprehensive recovery of indium, cadmium, thallium and zinc from lead system smoke |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105200242A (en) * | 2015-10-27 | 2015-12-30 | 中南大学 | Method for revering cadmium from arsenic-containing lead-smelting oxygen bottom-blown furnace dust |
| CN105200242B (en) * | 2015-10-27 | 2017-06-23 | 中南大学 | A kind of method that cadmium is reclaimed from containing arsenic refining lead oxygen bottom blown furnace cigarette ash |
| CN105925810A (en) * | 2016-04-21 | 2016-09-07 | 西北矿冶研究院 | Method for preparing sponge cadmium from cadmium rectification alkaline residue |
| CN105925808A (en) * | 2016-04-28 | 2016-09-07 | 河南金利金铅集团有限公司 | Method for improving grade of by-product sponge cadmium in heptahydrate production |
| CN108913910A (en) * | 2018-07-18 | 2018-11-30 | 河南金利金铅集团有限公司 | A kind of method that lead smelts the recycling of bottom convertor cigarette ash cadmium metal |
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Application publication date: 20130102 |