CN104404275B - A kind of method of counterflow leaching continuous decomposition sheelite - Google Patents
A kind of method of counterflow leaching continuous decomposition sheelite Download PDFInfo
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- CN104404275B CN104404275B CN201410706456.XA CN201410706456A CN104404275B CN 104404275 B CN104404275 B CN 104404275B CN 201410706456 A CN201410706456 A CN 201410706456A CN 104404275 B CN104404275 B CN 104404275B
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Abstract
The present invention relates to a kind of method of counterflow leaching continuous decomposition sheelite, comprise the steps: 1) sheelite and mother liquor are added reaction 1 district continuously, be fully uniformly mixed, gained slurry enters reaction 2 district; 2) in reaction 2 district, add sulfuric acid, phosphoric acid continuously, be fully uniformly mixed, gained slurry enters reaction 3 district; 3) in reaction 3 district, slurry is shunted, and a part of backflow of slurry is to reaction 1st district, and another part slurry enters reaction 4 district; 4) by gained slurries filtration in reaction 4 district, tungsten carried by leach liquor, and mother liquid obtained reaction 1 district that returns continues to mix with sheelite.Acid is mended continuously by adopting to leach continuously to combine, avoid the fluctuation of sheelite leaching condition, and part leaching ore pulp is directly returned, on the one hand can oscillation suppression further, the gypsum tailings returned in a steady working condition in ore pulp can be used as crystal seed on the other hand, simplify operation, improve effect, thus achieve extensive stably manufactured.
Description
Technical field
The present invention relates to a kind of method of counterflow leaching continuous decomposition sheelite, belong to technical field of wet metallurgy.
Background technology
Tungsten resource reserves the first in the world of China, wherein sheelite accounts for tungsten resource reserves more than 2/3.Develop efficient sheelite smelting technology and just become the key promoting Chemical analysis development.
ZL201010605095.1, international monopoly PCT application (PCT/CN2011/001895) propose the method adopting sulfuric-phosphoric to work in coordination with decompose tunstite.Wherein, ZL201010605095.1 decomposes extract tungsten by adding sheelite in mixed acid system, and fills into phosphoric acid and sulfuric acid returns leaching to carrying in the mother liquor after tungsten.
Following defect is there is: (1) adopts intermittent operation owing to leaching in the process of above-mentioned phosphorus acid-sulfur acid system decompose tunstite, production efficiency is low, poor stability: when sheelite feeds intake, on the one hand because vigorous reaction causes solution acidity to decline rapidly, the acidity of the areas adjacent that particularly feeds intake declines more so instantaneously.On the other hand vigorous reaction causes calcium sulfate concentration in solution to rise rapidly forming large degree of supersaturation.Reaction violent in addition also causes local temperature too high, and the crystal formation affecting calcium sulfate controls.These problems are more outstanding when process association has the low grade wolfram of a large amount of calcic gangue, often make leaching process off-target working conditions, cause caking phenomenon in slip, make discomposing effect undesirable; (2) acid concentration is higher when each leaching cycle starts, but consumes along with reaction and constantly decline, and is difficult to provide stable physicochemical environment for crystal of calcium sulfate, and then impact is leached.If strengthen reaction liquid-solid ratio, acid concentration can be stablized to a certain extent, but significantly reduce device processes ability; (3) for improving the crystallization behavior of calcium sulfate and the preparation specially of the crystal seed needs that add, the crystal seed made also wants meticulous filtration washing in order to avoid reunite and impact effect, and this makes again process complexity tediously long, is sometimes also difficult to the leaching effect reached.
Summary of the invention
For overcoming the problems referred to above, the invention provides a kind of method that high performance counter current leaches continuous decomposition sheelite.Acid is mended continuously by adopting to leach continuously to combine, avoid the fluctuation of sheelite leaching condition, and part leaching ore pulp is directly returned, on the one hand can oscillation suppression further, the gypsum tailings returned in a steady working condition in ore pulp can be used as crystal seed on the other hand, simplify operation, improve effect, thus achieve extensive stably manufactured.
To achieve these goals, the present invention adopts following technical scheme:
A method for counterflow leaching continuous decomposition sheelite, comprises the steps:
1) sheelite and mother liquor are added reaction 1 district continuously, be fully uniformly mixed, gained slurry enters reaction 2 district;
2) in reaction 2 district, add sulfuric acid, phosphoric acid continuously, be fully uniformly mixed, gained slurry enters reaction 3 district;
3) in reaction 3 district, slurry is shunted, and a part of backflow of slurry is to reaction 1st district, and another part slurry enters reaction 4 district;
4) by gained slurries filtration in reaction 4 district, tungsten carried by leach liquor, and mother liquid obtained reaction 1 district that returns continues to mix with sheelite.
Wherein, in step 1) in, the mass volume ratio of described sheelite and mother liquor is 1:2 ~ 10 (kg/L).
Wherein, in step 1) in, WO in described sheelite
3mass percent is 10-70%, and 98% granularity is not more than 50 orders.
In step 1) in, stirring velocity 70 ~ 180rmp; Preferred 90-100rmp.
Wherein, in step 2) in, in reaction 2 district after acid adding, to be converted to P
2o
5meter, concentration is 15%-30%, and sulfate concentration is 50-150g/L.
In step 2) in, stirring velocity 70 ~ 180rmp; Preferred 90-100rmp.
Wherein, in step 3) in, the stock quality being back to reaction 1 district accounts for the 20%-80% of the total stock quality of reaction 3 Qu.
Wherein, in whole successive reaction, temperature controls at 60-100 DEG C, and total reaction time controls at 1 ~ 6h, and flow rate of slurry controls between 124-128L/h, while guarantee slurry fully reacts, improve reaction efficiency.
It is as follows that the present invention has beneficial effect: 1, part size is back to reaction 1 district and participates in countercurrent reaction, can reduce the decomposition acid consumption of tungsten ore, realize the efficient-decomposition of sheelite; 2, the calcium sulfate containing generation in backflow slurry, can be used as crystal seed to reduce the degree of supersaturation of calcium sulfate; 3, in reaction system, acid concentration is relatively stable, can obtain the crystal of calcium sulfate of thick rule, not only can improve tungsten ore rate of decomposition, also makes solid-liquid separation easy handling.
Accompanying drawing explanation
Fig. 1 is successive reaction schematic flow sheet described in the embodiment of the present invention 1.
Fig. 2 is continuous reaction apparatus vertical view described in the embodiment of the present invention 1.
Embodiment
Be described further below in conjunction with embodiment, following examples are intended to the present invention instead of limitation of the invention further are described.
The method of embodiment 1 counterflow leaching continuous decomposition sheelite
The present embodiment provides a kind of method of counterflow leaching continuous decomposition sheelite, as shown in Figure 1 and Figure 2, comprises the steps:
1) by sheelite (wherein WO
3mass percent is that 30%, 98% granularity is not more than 50 orders), mother liquor adds reaction 1 district continuously with mass volume ratio 1:5 (kg/L), be fully uniformly mixed, gained slurry enters reaction 2 district;
2) in reaction 2 district, add sulfuric acid, phosphoric acid continuously, be fully uniformly mixed, gained slurry enters reaction 3 district;
In reaction 2 district after acid adding, with P
2o
5meter concentration is 16.8%, and sulfate concentration is 55g/L;
3) in reaction 3 district, the part size accounting for slurry total mass 30% is back to reaction 1 district, and remaining slurry enters reaction 4 district;
4) by gained slurries filtration in reaction 4 district, tungsten carried by leach liquor, and mother liquid obtained reaction 1 district that returns continues to mix with sheelite.
Wherein, in whole successive reaction, temperature controls at 62 DEG C.
React 1st district, the stirring velocity in 2nd district is 95rmp, slurry flow rate is 125L/h.
Adopt production breakdown sheelite described in embodiment 1, reaction total residence time controls at 6h.
Embodiment 2-9
According to the method counterflow leaching continuous decomposition sheelite of embodiment 1.Wherein, the stirring velocity controlling each reaction zone is 90-100rmp, and slurry flow rate is 124-128L/h.Concrete operations parameter and result as shown in table 1.
The concrete operations of table 1. successive reaction groove decompose tunstite and result
Compared with traditional rhythmic reaction technique, adopt treatment process of the present invention, the continuous leaching of sheelite can be realized, not only reduce the labour intensity of operator, and also obtain unusual effect in energy-conserving action.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (7)
1. a method for counterflow leaching continuous decomposition sheelite, is characterized in that, comprises the steps:
1) sheelite and mother liquor are added reaction 1 district continuously, be fully uniformly mixed, gained slurry enters reaction 2 district;
2) in reaction 2 district, add sulfuric acid, phosphoric acid continuously, be fully uniformly mixed, gained slurry enters reaction 3 district;
3) in reaction 3 district, slurry is shunted, and a part of backflow of slurry is to reaction 1st district, and another part slurry enters reaction 4 district;
4) by gained slurries filtration in reaction 4 district, tungsten carried by leach liquor, and mother liquid obtained reaction 1 district that returns continues to mix with sheelite;
In step 2) in, in reaction 2 district after acid adding, to be converted to P
2o
5meter, concentration is 15%-30%;
In step 2) in, in reaction 2 district after acid adding, sulfate concentration is 50-150g/L;
In step 3) in, the stock quality being back to reaction 1 district accounts for the 20%-80% of the total stock quality of reaction 3 Qu.
2. the method for counterflow leaching continuous decomposition sheelite according to claim 1, is characterized in that, in step 1) in, the mass volume ratio of described sheelite and mother liquor is 1:2 ~ 10kg/L.
3. the method for counterflow leaching continuous decomposition sheelite according to claim 1, is characterized in that, in step 1) in, WO in described sheelite
3mass percent is 10-70%, and 98% granularity is not more than 50 orders.
4. the method for counterflow leaching continuous decomposition sheelite according to claim 1, it is characterized in that, in whole successive reaction, temperature controls at 60-100 DEG C.
5. the method for counterflow leaching continuous decomposition sheelite according to claim 1, is characterized in that, in step 1), step 2) in, stirring velocity 70 ~ 180rmp.
6. the method for counterflow leaching continuous decomposition sheelite according to claim 5, is characterized in that, in step 1), step 2) in, stirring velocity 90-100rmp.
7. the method for counterflow leaching continuous decomposition sheelite according to claim 1, it is characterized in that, the flow rate control of described slurry is between 124-128L/h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021328A (en) * | 2010-12-24 | 2011-04-20 | 中南大学 | Method for extracting tungsten from scheelite |
| CN102080157A (en) * | 2010-12-24 | 2011-06-01 | 中南大学 | Method for decomposing scheelite |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021328A (en) * | 2010-12-24 | 2011-04-20 | 中南大学 | Method for extracting tungsten from scheelite |
| CN102080157A (en) * | 2010-12-24 | 2011-06-01 | 中南大学 | Method for decomposing scheelite |
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