CN102489393A - Ore dressing method for separation and recovery of scheelite and fluorite from sulfur flotation tailings of polymetallic ore - Google Patents
Ore dressing method for separation and recovery of scheelite and fluorite from sulfur flotation tailings of polymetallic ore Download PDFInfo
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Abstract
The invention discloses an ore dressing method for separation and recovery of scheelite and fluorite from sulfur flotation tailings of polymetallic ore. The ore dressing method can eliminate the shortcomings caused by a preferential flotation process in the prior art by simultaneously performing bulk flotation on the scheelite and the fluorite and further separating the scheelite from the fluorite, further significantly improve the recovery rate of the scheelite and the fluorite and realize high-efficient recovery of two minerals, namely the scheelite and the fluorite in the polymetallic ore. Furthermore, the scheelite and the fluorite are dressed through a rough concentration bulk flotation and fine concentration separation two-stage process, so that indexes in various stages of operations are convenient to stipulate and control, and quantification of the indexes of the ore dressing process of the scheelite and the fluorite and operation management can be effectively realized.
Description
Technical field
The present invention relates to the technique of preparing field, relate in particular to the beneficiation method of scheelite and fluorite in a kind of polymetallic ore.
Background technology
At present, prior art is for comparatively single scheelite or fluorite, and its ore-dressing technique is comparative maturity all, adopts the method for flotation usually, and technology is simple and effectively.For the polymetallic ore that contains mineral such as sulphide ores such as molybdenite, bismuthine, pyrite and scheelite, fluorite; The scheelite wherein and the recovery of fluorite; Prior art adopts the method for diffeential floatation usually, promptly first flotation scheelite, then floating tungsten mine tailing is carried out the flotation of fluorite.And in the diffeential floatation process, prior art is to adopt high alkaline process to realize suppressing the purpose of fluorite scheelite, promptly through adding Na
2CO
3, CaO, NaOH, Na
2SiO
3Regulate and control pH value>=12, suppressing gangue mineral such as fluorite, and with aliphatic acid as collecting agent, the flotation acquisition contains WO
3＜10% white tungsten rough concentrate, and then selected through heating, obtain WO
3>=65% white tungsten fine ore product.
After floatingly selecting white tungsten rough concentrate, and then floating tungsten mine tailing carried out fluorite, prior art fluorite technology is generally following three types:
One, pure floatation process (see figure 1) is promptly carried out roughing flotation and repeatedly selected, and selected number of times is looked the decision of ore character, and the chats that has is regrinding and reconcentration then.
Two, floating--magnetic technology (see figure 2), promptly through roughing flotation with repeatedly selected after, the fluorite concentrate of acquisition carries out strong magnetic operation again, the non magnetic product of magnetic operation is final fluorite concentrate by force.
Three, magnetic--floating technology (see figure 3), promptly floating tungsten mine tailing concentrates earlier, concentrates the back and gets into magnetic concentration working, behind magnetic sorting, non magnetic product is carried out fluorite, through roughing flotation and repeatedly selected after, obtain final fluorite concentrate.
The ore-dressing technique of scheelite and fluorite in the prior art polymetallic ore still exists following technological deficiency at present:
(1) diffeential floatation scheelite under high-alkali condition, pH >=12 of flotation medium at this moment.And the comparatively suitable pH scope of fluorite is 8～9, when therefore floating tungsten mine tailing being carried out fluorite, needs to add acid flotation medium is adjusted to alkalescent, has obviously increased sour consumption greatly.
(2) when the diffeential floatation scheelite, fluorite is that receiving in the floatation process pressed down mineral.Since surface adsorption inhibitor, make floating tungsten mine tailing carried out in the process of fluorite that fluorite falls groove easily, and is especially all the more so in the repeatedly selected operation under low consistency conditions, thereby greatly influenced the raising of the fluorite rate of recovery.
(3) adopt during the diffeential floatation scheelite aliphatic acid as collecting agent, the white tungsten rough concentrate that is obtained contains CaF
220～65%, take away about 15～30% the fluorite rate of recovery, this part fluorite finally runs off in white tungsten is heated refining process, makes that the fluorite overall recovery is difficult to improve.Prior art is for grade WO
30.30 CaF～0.45%,
217～25% give ore deposit, the scheelite concentrate grade WO that is obtained
3About 65%, the rate of recovery is 65～72%, fluorite concentrate grade CaF
2About 97%, the rate of recovery is 50～65%.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art; A kind of beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite is provided; Through scheelite and fluorite bulk flotation are simultaneously come out, carry out again separating of scheelite and fluorite afterwards, to eliminate the drawback that the prior art controling differential flotation process for copper is brought; Thereby significantly improve the rate of recovery of scheelite and fluorite, the high efficiente callback of scheelite and two kinds of mineral of fluorite in the realization polymetallic ore.
The object of the invention is achieved through following technical scheme:
A kind of beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite provided by the invention may further comprise the steps:
(1) said floating sulphur mine tailing carries out the bulk flotation of scheelite and fluorite
Under weak basic condition, preferred pH 8～9.5 adds gangue inhibitor and fatty acid collecting agent, and the froth pulp of acquisition is the mixed crude concentrate of scheelite and fluorite;
(2) mixed crude concentrate of said scheelite and fluorite carries out fluorite
Add white tungsten inhibitor and fatty acid collecting agent, the froth pulp of acquisition is the fluorite rough concentrate, and product is white tungsten rough concentrate in the groove;
(3) said fluorite rough concentrate carries out acidleach and obtains the fluorite concentrate product;
(4) said white tungsten rough concentrate obtains the white tungsten fine ore product through gravity treatment.
Recovery for scheelite and fluorite in the floating sulphur mine tailing of polymetallic ore separates, and the present invention carries out through two flotation sections of sorting, and promptly the section of roughly selecting mixed floats and selected period separate.
The section of roughly selecting is the bulk flotation process of scheelite and fluorite; The surperficial cation of scheelite and fluorite is calcium ion; Under weak basic condition, mix floating through inhibition gangue mineral, use fatty acid collecting agent; The very first time with scheelite and fluorite emersion together, thereby avoid fluorite floating tungsten process in the past be suppressed and be difficult to again floating occurred be prone to the groove phenomenon, help the raising of the fluorite rate of recovery.
Selected section for pressing down the separation process of the floating fluorite of tungsten,, avoids being prone to floating fluorite and take away the loss that is caused in floating tungsten process in the past with tungsten rough concentrate emersion the fluorite emersion through suppressing scheelite, can effectively improve the rate of recovery of fluorite.The fluorite rough concentrate of emersion just can obtain the fluorite concentrate product through acidleach.And being mainly white tungsten rough concentrate by separating the bottom land thing that obtains behind the selected section floating fluorite, its mineral that contain intermediate density are few, thereby strengthened the density contrast between scheelite and the gangue mineral, can stablize through gravity treatment to obtain the white tungsten fine ore product.
For further obtaining high-quality fluorite concentrate product; In the step according to the invention (3); The fluorite rough concentrate is at first regrinded, is added then white tungsten inhibitor and carries out the floating more floating again concentrate of acquisition fluorite that separates of fluorite with fatty acid collecting agent, afterwards the floating again concentrate of fluorite is carried out acidleach and obtains the fluorite concentrate product.Like this, the fluorite rough concentrate can improve liberation degree of minerals through regrinding, and through removing the gangue mineral that has dissociated floating the separation again, the floating again concentrate of fluorite carries out acidleach and just can obtain high-quality fluorite concentrate product.Preferred version is: the grinding particle size of fluorite coarse concentrate regrinding is-400 orders 75～85%, and fluorite adopts one slightly to sweep one or two smart flow processs floating again the separation, and total time is 5～15 minutes.
The present invention specifically can take following further measure: said fatty acid collecting agent is olein by weight: the modified fat acid of sodium carbonate=1: 0.1～0.3 is 25～1500g/t by floating its consumption of sulphur mine tailing.Said gangue inhibitor adopts waterglass, and its consumption is 0～1500g/t.Said white tungsten inhibitor is a waterglass by weight: sulfuric acid: calgon: the combination of acidic waterglass of oxalic acid=1: 0.1～0.5: 0.1～0.25: 0.1～0.25, its consumption are 0～2500g/t.
Further, bulk flotation adopts one thick two slightly to sweep a smart flow process in the step according to the invention (1), and total time is 10～20 minutes.Fluorite adopts one slightly to sweep five smart flow processs in the said step (2), and total time is 15～25 minutes.
Because scheelite and fluorite have obtained enrichment timely in the above-mentioned mixed floating section of roughly selecting; And obtained effective separation for selected section at fluorite; So most of scheelite is to be enriched in the interior product of groove of fluorite, and the mineral composition of the interior product of this time slot is simple relatively, WO
3＞1%, it is not high to contain fluorite, and behind gravity treatment acquisition white tungsten fine ore, the mine tailing of gravity treatment helps adopting the flotation mode of normal temperature to be handled.For this reason further; The gravity tailings of step according to the invention (4) can carry out white tungsten flotation and obtain the tungsten ore product after concentrating; Be after product obtains white tungsten fine ore through gravity treatment in the groove of fluorite, the mine tailing of gravity treatment adopts not to be had the further processing of the floatation process (yet can adopt the technology of heating) of heating and just can obtain the tungsten ore product.
In the such scheme, step according to the invention can adopt shaking table equipment in (4), carries out reselection operation through one thick one smart flow process.
The present invention has following beneficial effect:
(1) the present invention at first comes out scheelite and fluorite disposable bulk flotation simultaneously; Avoided prior art high-alkali press down the fluorite scheelite and in weak alkaline medium the required pH that carries out of flotation fluorite adjust repeatedly, the height alternation procedure, greatly reduce the acid consumption and consume with medicine.
(2) through the section of roughly selecting the disposable bulk flotation simultaneously of scheelite and fluorite is come out after, the selected section method of taking to press down tungsten flotation fluorite, make scheelite and fluorite be able to high efficiente callback and separate.
(3) reduced and be prone to floating fluorite and when diffeential floatation scheelite in the past, be entrained into white tungsten rough concentrate and the loss in white tungsten is heated refining process; Simultaneously, eliminated in the past in the diffeential floatation scheelite process, be difficult to behind the fluorite surface adsorption inhibitor to float and be prone to the phenomenon of groove, effectively improved the rate of recovery of fluorite.
(4) mineral that contain intermediate density through selected section isolated white tungsten rough concentrate are few, make the density contrast between scheelite and the gangue mineral big, can stablize, obtain to contain with high yield WO through the method for gravity treatment
3>=65% scheelite concentrate product.And that gravity tailings contains fluorite is not high, just can obtain a tungsten ore product through the normal temperature flotation, has solved the selected difficult problem of heating that contains the white tungsten rough concentrate of fluorite in the prior art.
(5) scheelite of the present invention is taked to roughly select to mix to float with fluorite and is sorted with the selected two-stage process that separates, and is convenient to formulate, control the index of each section operation, thereby can effectively realizes the quantification and the operational administrative of scheelite, processing of fluorspar ores technic index.
Description of drawings
To combine embodiment and accompanying drawing that the present invention is made further detailed description below:
Fig. 1 is the white tungsten flotation of prior art--a fluorite principle process chart;
Fig. 2 is the strong magnetic principle process chart of the white tungsten flotation of prior art--fluorite--;
Fig. 3 is the white tungsten flotation of prior art--strong magnetic--fluorite principle process chart;
Fig. 4 is the principle process chart of the embodiment of the invention from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite;
Fig. 5 is that scheelite and fluorite mix floating-separating flotation process chart again in the embodiment of the invention;
Fig. 6 is that the fluorite coarse concentrate regrinding floats-the acid leaching process flow chart again in the embodiment of the invention;
Fig. 7 is white tungsten rough concentrate gravity treatment-flotation process figure in the embodiment of the invention.
The specific embodiment
With persimmon bamboo plantation Chai Shan fork in the road, Hunan polymetallic ore is example, and its mineral deposit is many metals of tungsten bismuth skarn type mineral deposit.Major metal mineral in the ore are scheelite, fluorite, molybdenite, bismuthine, cassiterite, wolframite and magnetic iron ore, and main gangue mineral is garnet, calcite, quartz, hornblend, chlorite, biotite, sericite and diopside.Tungsten in the ore is to be main with scheelite, and material phase analysis shows that its apportionment ratio accounts for more than 90%.
Main Containing Sulfur ore deposit and oxide ore two parts in the raw ore ore behind conventional sulfide flotation, contain WO in the floating sulphur mine tailing
30.17 CaF～0.35%,
216～29%.
Embodiment one:
Present embodiment with above-mentioned floating sulphur mine tailing as giving the ore deposit, the beneficiation method of Separation and Recovery scheelite and fluorite, as shown in Figure 4, its step is following:
(1) floating sulphur mine tailing carries out the bulk flotation (section of roughly selecting) of scheelite and fluorite
Feed preparation unit size is-200 orders 82%; Add waterglass as gangue inhibitor; Collecting agent is an olein by weight: the modified fat acid of sodium carbonate=1: 0.2; Under pH 9 conditions, slightly sweep a smart flow process (see figure 5) through one thick two, total time is 14 minutes, and the froth pulp of acquisition is the mixed crude concentrate of scheelite and fluorite;
(2) mixed crude concentrate of scheelite and fluorite carries out fluorite (selected section)
With waterglass by weight: sulfuric acid: calgon: oxalic acid=1: 0.3: 0.1: 0.15 combination of acidic waterglass is as white tungsten inhibitor; Collecting agent is the same; Slightly sweep five smart flow process (see figure 5)s through one; Total time is 18 minutes, and the froth pulp of acquisition is the fluorite rough concentrate, and product is white tungsten rough concentrate in the groove;
(3) the fluorite rough concentrate carries out acidleach to the floating again concentrate of fluorite then and obtains the fluorite concentrate product through the floating floating again concentrate of fluorite that obtains of regrinding again
The grinding particle size of (3-1) regrinding is-400 orders 82.69%, and fluorite adopts one slightly to sweep a smart flow process (see figure 6) floating again the separation, and total time is 10 minutes, obtains the floating again concentrate of fluorite, and the shaking table mine tailing that floating again mine tailing merges to step (4) carries out white tungsten flotation;
(3-2) dripping hydrochloric acid in the floating again concentrate of fluorite also stirs 0.5h again till still, just obtains the fluorite concentrate product through washing and filtering;
(4) as shown in Figure 7, white tungsten rough concentrate adopts shaking table, and feed ore concentration is 25%, obtains the white tungsten fine ore product through one thick one smart flow process; The shaking table mine tailing carries out white tungsten flotation after concentrating, and sweeps three smart flow processs through one thick three and obtains the tungsten ore product.
Embodiment two:
Present embodiment and embodiment one difference are:
1, step (1), feed preparation unit size are-200 orders 85%, and collecting agent is an olein by weight: the modified fat acid of sodium carbonate=1: 0.1; Total time is 20 minutes.
2, step (2), with waterglass by weight: sulfuric acid: calgon: oxalic acid=1: 0.1: 0.2: 0.25 combination of acidic waterglass is as white tungsten inhibitor; Total time is 25 minutes.
3, step (3-1), the grinding particle size of fluorite coarse concentrate regrinding are-400 orders 85%; Total time is 15 minutes.
4, step (4), the feed ore concentration of shaking table is 30%.
Embodiment three:
Present embodiment and embodiment one difference are:
1, step (1), feed preparation unit size are-200 orders 90%, and collecting agent is an olein by weight: the modified fat acid of sodium carbonate=1: 0.3; Flotation under pH 8.5 conditions, total time is 10 minutes.
2, step (2), with waterglass by weight: sulfuric acid: calgon: oxalic acid=1: 0.5: 0.25: 0.1 combination of acidic waterglass is as white tungsten inhibitor; Total time is 15 minutes.
3, step (3-1), the grinding particle size of fluorite coarse concentrate regrinding are-400 orders 75%; Total time is 5 minutes.
4, step (4), the feed ore concentration of shaking table is 35%.
Embodiment four:
Present embodiment and embodiment one difference are:
1, step (1), feed preparation unit size are-200 orders 83%, and collecting agent is an olein by weight: the modified fat acid of sodium carbonate=1: 0.25; Total time is 15 minutes.
2, step (2), with waterglass by weight: sulfuric acid: calgon: oxalic acid=1: 0.3: 0.15: 0.2 combination of acidic waterglass is as white tungsten inhibitor; Total time is 18 minutes.
3, step (3-1), the grinding particle size of fluorite coarse concentrate regrinding are-400 orders 80%; Total time is 10 minutes.
4, step (4), the feed ore concentration of shaking table is 30%.
The regime of agent of each embodiment flotation operation is seen table 1 (consumption is by floating sulphur mine tailing).
The regime of agent of table 1 embodiment one～four flotation operation
The mineral processing index that each embodiment obtains is seen table 2.
Table 2 embodiment one～Sibai tungsten ore and processing of fluorspar ores index
Claims (10)
1. beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite is characterized in that may further comprise the steps:
(1) said floating sulphur mine tailing carries out the bulk flotation of scheelite and fluorite
Under weak basic condition, add gangue inhibitor and fatty acid collecting agent, the froth pulp of acquisition is the mixed crude concentrate of scheelite and fluorite;
(2) mixed crude concentrate of said scheelite and fluorite carries out fluorite
Add white tungsten inhibitor and fatty acid collecting agent, the froth pulp of acquisition is the fluorite rough concentrate, and product is white tungsten rough concentrate in the groove;
(3) said fluorite rough concentrate carries out acidleach and obtains the fluorite concentrate product;
(4) said white tungsten rough concentrate obtains the white tungsten fine ore product through gravity treatment.
2. the beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite according to claim 1; It is characterized in that: in the said step (3); The fluorite rough concentrate is at first regrinded, is added then white tungsten inhibitor and carries out the floating more floating again concentrate of acquisition fluorite that separates of fluorite with fatty acid collecting agent, afterwards the floating again concentrate of fluorite is carried out acidleach and obtains the fluorite concentrate product.
3. the beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite according to claim 1 and 2; It is characterized in that: said fatty acid collecting agent is olein by weight: the modified fat acid of sodium carbonate=1: 0.1～0.3 is 25～1500g/t by floating its consumption of sulphur mine tailing; Said step (1) weak basic condition is pH 8～9.5.
4. the beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite according to claim 1, it is characterized in that: said gangue inhibitor is a waterglass, is 0～1500g/t by floating its consumption of sulphur mine tailing.
5. the beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite according to claim 1 and 2; It is characterized in that: said white tungsten inhibitor is waterglass by weight: sulfuric acid: calgon: the combination of acidic waterglass of oxalic acid=1: 0.1～0.5: 0.1～0.25: 0.1～0.25 is 0～2500g/t by floating its consumption of sulphur mine tailing.
6. the beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite according to claim 1, it is characterized in that: the bulk flotation section adopts one thick two slightly to sweep a smart flow process in the said step (1), and total time is 10～20 minutes.
7. the beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite according to claim 1, it is characterized in that: fluorite adopts one slightly to sweep five smart flow processs in the said step (2), and total time is 15～25 minutes.
8. the beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite according to claim 2; It is characterized in that: the grinding particle size of fluorite coarse concentrate regrinding is-400 orders 75～85% in the said step (3); Fluorite adopts one slightly to sweep one or two smart flow processs floating again the separation, and total time is 5～15 minutes.
9. the beneficiation method from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite according to claim 1 is characterized in that: carry out white tungsten flotation after the gravity tailings of said step (4) is concentrated and obtain the tungsten ore product.
10. according to claim 1 or 9 described beneficiation methods, it is characterized in that: adopt shaking table equipment in the said step (4), carry out reselection operation through one thick one smart flow process from floating sulphur mine tailing Separation and Recovery scheelite of polymetallic ore and fluorite.
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| CN105149105A (en) * | 2015-07-13 | 2015-12-16 | 中南大学 | Method for desulfurizing, refining and purifying fluorite concentrate |
| CN105289852A (en) * | 2015-10-30 | 2016-02-03 | 中南大学 | Method for flotation after acid etching pretreatment of high-calcium fluorite |
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| CN106944245A (en) * | 2017-03-29 | 2017-07-14 | 江西省宏兴选矿设备制造有限公司 | A kind of complicated many golden metallic ores of W, mo, bi fluorite select technique |
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| CN108435429A (en) * | 2018-03-30 | 2018-08-24 | 中南大学 | A kind of ore-dressing technique recycling tungsten, fluorite from low-grade tungsten flotation high calcium rough concentrate |
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| CN103706485B (en) * | 2013-12-25 | 2016-02-24 | 昆明理工大学 | A kind of beneficiation method of high carbon acid calcium type fluorite ore |
| CN103706485A (en) * | 2013-12-25 | 2014-04-09 | 昆明理工大学 | Beneficiation method of high calcium carbonate content type fluorite ore |
| CN105149105A (en) * | 2015-07-13 | 2015-12-16 | 中南大学 | Method for desulfurizing, refining and purifying fluorite concentrate |
| CN105149105B (en) * | 2015-07-13 | 2017-12-08 | 中南大学 | A kind of method of fluorite concentrate desulfurization purifying |
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| CN105289852A (en) * | 2015-10-30 | 2016-02-03 | 中南大学 | Method for flotation after acid etching pretreatment of high-calcium fluorite |
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