CN100408193C - Solid-liquid centrifugal separator of leached and extracted coupling resultant - Google Patents
Solid-liquid centrifugal separator of leached and extracted coupling resultant Download PDFInfo
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- CN100408193C CN100408193C CNB2005100115970A CN200510011597A CN100408193C CN 100408193 C CN100408193 C CN 100408193C CN B2005100115970 A CNB2005100115970 A CN B2005100115970A CN 200510011597 A CN200510011597 A CN 200510011597A CN 100408193 C CN100408193 C CN 100408193C
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- solid
- organic solvent
- leaching
- present
- liquid
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- 239000007788 liquid Substances 0.000 title claims abstract description 26
- 238000010168 coupling process Methods 0.000 title claims abstract description 7
- 230000008878 coupling Effects 0.000 title claims description 4
- 238000005859 coupling reaction Methods 0.000 title claims description 4
- 239000003960 organic solvent Substances 0.000 abstract description 26
- 238000002386 leaching Methods 0.000 abstract description 21
- 238000000926 separation method Methods 0.000 abstract description 16
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 15
- 239000007787 solid Substances 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 13
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 7
- 239000011707 mineral Substances 0.000 abstract description 7
- 239000002893 slag Substances 0.000 abstract description 7
- 239000011593 sulfur Substances 0.000 abstract description 7
- 229910052717 sulfur Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract 2
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000005864 Sulphur Substances 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 208000035126 Facies Diseases 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 229950011008 tetrachloroethylene Drugs 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229920001617 Vinyon Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical class C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
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Abstract
The present invention belongs to the field of solid-liquid separation, which particularly relates to a separating device and an operation method when leaching slag, solid sulfur, organic solvent and leaching solution containing valuable metal ions are identical after metal vulcanized mineral substances are leached by means of an oxidizing leaching and organic solvent extracting and sulfur coupling method. The present invention is characterized in that the tube wall of a centrifugal tube in a centrifuge is provided with three circular holes at different heights; the bottom of the centrifugal tube is provided with one circular hole; simultaneously, a closing plug with a screw buckle is arranged at each circular hole. The centrifugal tube is provided with the circular holes at different heights, and therefore, the present invention can respectively discharge multilayer substances which are centrifugally separated without mutual pollution. The device of the present invention can be easily operated in solid-liquid separation.
Description
Technical field
The invention belongs to the Separation of Solid and Liquid field, after being particularly related to metal sulfide ore and adopting oxidation leaching and organic solvent extracting sulphur coupling process to leach, device and method of operating that leaching slag, solid sulfur, organic solvent are separated when identical with the leachate four that contains valuable metal ions.
Background technology
In hydrometallurgy, adopt the leaching unit operations, promptly metal-containing minerals and leaching agent are at high temperature reacted, slag liquid must be separated after the metal-containing minerals leaching, slag is discarded, leachate is collected, leachate after the collection is handled again, and the metal recovery useful becomes product.
In small test and industrial operation, the ore pulp after leaching generally adopts filter method to carry out Separation of Solid and Liquid, for accelerated filtration speed, in the collection container of filter, vacuumizes into negative-pressure operation.The purpose of this way is to strengthen the motive force of liquid by filter cloth, and this is the most frequently used solid-liquid separating method, and the small test filter tunnel has a rotary drum filter industrial, and separator all is by principle design like this basically, operates.As Chinese patent application number: the disclosed separation equipment of multifunctional and composite type solid-liquid rotational flow separation device of 02153487.X is to be provided with cylindrical deflector in the scroll entire body, and this deflector is to be arranged by a plurality of and radially acutangulate flow deflector to form; Chinese patent application number: 96206947.7 disclosed concentrated classifying cyclones are that one group of underflow mouth that bore is different is arranged in the bottom of cyclone.
Tiny especially when running into solid particle, this moment can be because fine grained stops up the filter cloth eyelet when filtering, and the filter cake that forms is when very thin, and the rate of filtration just lowers gradually, even can't operate again.Adopt centrifugal process this moment, because the proportion of liquid and solid has bigger difference, when under certain centrifugal speed, in very short time, solid and liquid separated.Separation of Solid and Liquid can be carried out very soon with centrifuge in the small test chamber, and existing various types centrifuge is used on producing.
But above-mentioned these devices carry out leaching operation at 70～80 ℃, and oxidation leaching and organic solvent extracting sulphur coupling process are adopted in its leaching.After leaching process finishes, except that leached mud, the leachate that also has solid sulfur, organic solvent and contain valuable metal ions.Adopt filtration method to carry out Separation of Solid and Liquid this moment, following problem can occur:
(1) in order to prevent the volatilization of organic solvent, must cool off, when cooling, with decrease of temperature, the powder wrapped of separating out solid sulfur makes solid sulfur to separate on the slag particle surface.
(2) when adopting vacuum decompression suction filtration method, the solution that contains leachate and organic solvent enters in the bottle,suction by filter cloth, owing to be negative-pressure operation, the organic matter volatile quantity is big.
(3) when after 70～80 ℃ of leachings; when carrying out heat filtering; organic solvent is from a filter tunnel volatilization part; the organic solvent volatilization is bigger in the subnormal ambient in bottle,suction; and enter in the vavuum pump with gas along pipeline; make that the pumping fluid dilution is rotten, cause vavuum pump often to change oil, even cause vavuum pump to damage.Main organic solvent is because volatilization loss causes the rate of recovery very low.
In order to address the above problem, adopt centrifugal separation method.Metalliferous mineral leaches at 70～80 ℃, under this temperature, the ore pulp after leaching is poured into rapidly in the centrifuge tube, covers the loam cake of centrifuge tube, puts into centrifuge immediately and carries out centrifugally operated, has formed four layers (as shown in Figure 1) after a few minutes in centrifuge tube.
Separation method: through cooled centrifuge tube, with syringe from the top, dividing different height that institute's separator is aspirated then step by step separates, the shortcoming of the method maximum is to operate respectively, when adopt glass or vinyon centrifuge tube the time, this interface can be operated with syringe as can be seen; But when adopting the metal centrifuge tube, owing to can't conclude the accurate position at interface, extraction can't accurately put in place during with syringe pump.
Summary of the invention
A purpose of the present invention is to cause the organic solvent loss serious in order to overcome above-mentioned filtration method; Centrifugal filtration lock out operation complexity, product is introduced the defective of aspects such as impurity easily, provides a kind of simple to operate, the solid-liquid centrifugal separating device that can respectively four kinds of product be separated.
Still a further object of the present invention is to utilize the solid-liquid centrifugal separation equipment, Gu to liquid-liquid-solid-four methods of operating of separating mutually.
To achieve these goals, the present invention improves the centrifuge tube in the centrifuge, has taked following measures:
The solid-liquid centrifugal separating device of leached and extracted coupling resultant of the present invention (as shown in Figure 2), comprise centrifuge tube, centrifuge tube lid, it is characterized in that: the tube wall differing heights place at centrifuge tube has 3 circular holes, has 1 circular hole in the bottom, and each circular hole place is furnished with sealing-plug or minor valve etc.Gu liquid-liquid-solid-four can be poured out from corresponding circular hole respectively mutually, target product purity height is easy and simple to handle.
Have internal thread in the described circular hole, sealing-plug has external screw thread, and both coincide by the spiral shell button.
Described tube wall position of opening is positioned at the bottom of each product layer.
Solid-liquid centrifugal separation equipment of the present invention, Gu the method for operating when carrying out liquid-liquid-solid-four phase centrifugations may further comprise the steps:
(1) sealing-plug is screwed in the hole of centrifuge tube.
(2) metalliferous mineral leached 3～6 hours at 70～80 ℃, after leaching finishes, under this temperature, rapidly the pyrosol that contains solid and organic solvent of pre-separation was poured in the off-the-shelf centrifuge tube, covered the loam cake of centrifuge tube, put into centrifuge.
(3) start centrifuge, shut down after waiting to contain the solution separator well of solid and organic solvent.
(4) take out centrifuge tube, treat the solution cool to room temperature after, uppermost first plug of the centrifuge tube of back-outing is earlier poured out the leachate that ground floor contains valuable metal ions; Then back-outing, first fills in second following plug, pours out pressed powder; The 3rd plug of back-outing poured out organic solvent; Pour out slag by the bottom at last.
The organic solvent rate of recovery of the present invention is 85%～90%, and the organic solvent of pouring out from the duct that communicates with organic solvent can directly recycle, and does not influence the leaching rate of valuable metal.
The present invention is applicable to the separation of the solid-liquid system that contains organic solvent, particularly higher and when adopting the organic solvent be easy to volatilize in temperature, can obviously reduce volatilization because of organic solvent and cause loss when reclaiming, avoid causing environmental pollution, can improve the Recovery of Organic Solvent rate, thereby simplify technological process, reduce equipment investment, improved the quality of target product, solved organic solvent when separating because the problems such as causing economic loss of volatilizing.Also solved simultaneously leached mud, solid sulfur, organic solvent and the leachate that contains valuable metal ions have been carried out four problems that are separated difficulty simultaneously.
The present invention is owing to have circular hole at the differing heights place of centrifuge tube, thereby the multilayer material after centrifugation can be discharged respectively and do not pollute mutually.With respect to the centrifuge tube that only has outlet in the prior art in the bottom, the invention has the advantages that the separative efficiency height, be fit to the multilayer separation, avoid polluting, because after lower floor discharges from the bottom earlier, certainly exist the situation that subnatant is bonded at outlet, when layer second from the bottom once more when the bottom outlet is discharged, will be subjected to remaining in the pollution of ground floor liquid in the outlet.
Description of drawings
Fig. 1. the prior art centrifuge tube separates the product layering schematic diagram behind the solid-liquid.
Fig. 2. centrifuge tube schematic diagram of the present invention.
The schematic diagram that combines of Fig. 2 A. centrifuge tube circular hole of the present invention and sealing-plug.
Reference numeral
1. leachate 2. pressed powders 3. organic layers that contain valuable metal ions
4. slag 5. pads 6. tube walls
7. sealing-plug
The specific embodiment
Comparative Examples
Filtration method
10g mineral (zinc concentrate), 10ml organic solvent (tetrachloro-ethylene), 100ml leachate (being made up of 2mol/L sulfuric acid and 0.2mol/L nitric acid) are joined in the 250ml reactor.The capping still is opened and is stirred and heat riser, feeds O when temperature reaches 80 ℃
2, and keep O
2Pressure is 0.1MPa, and reaction needs 3～6 hours.After reaction finishes, the ore pulp after leaching is poured into rapidly in the funnel, adopted vacuum decompression suction filtration method to separate, organic facies, sulphur, leaching liquid measure recovering state are as shown in table 1.
Table 1
| Organic amount (ml) | Sulphur (g) | Liquid measure (ml) | |
| Reclaim | 7.0 | 2.0 | 94 |
| Loss | 30％ | 35％ | 6％ |
Embodiment
Centrifugal process
See also Fig. 2 and Fig. 2 A.On the tube wall of the 250ml of centrifuge centrifuge tube, have 3 circular holes that have internal thread, (the tube wall position of opening: distance pipe end 1.0cm, 1.6cm, 2.0cm).Have 1 circular hole that has internal thread in the bottom of centrifuge tube, each circular hole is furnished with the sealing-plug of band spiral shell button.10g mineral (zinc concentrate), 10ml organic solvent (tetrachloro-ethylene), 100ml leachate (being made up of 2mol/L sulfuric acid and 0.2mol/L nitric acid) are joined in the 250ml reactor.The capping still is opened and is stirred and heat riser, feeds O when temperature reaches 80 ℃
2, and keep O
2Pressure is 0.1MPa, and reaction needs 3～6 hours.After reaction finishes, the ore pulp after leaching is poured into rapidly in the device of the present invention, adopted centrifugal separation method to separate (shown in Fig. 2 and Fig. 2 A), organic facies, sulphur, leaching liquid measure recovering state are as shown in table 2.
Table 2
| Organic amount (ml) | Sulphur (g) | Liquid measure (ml) | |
| Reclaim | 8.7 | 2.9 | 98 |
| Loss | 13％ | 5％ | 2％ |
Claims (2)
1. the solid-liquid centrifugal separating device of a leached and extracted coupling resultant comprises centrifuge tube, centrifuge tube lid, and it is characterized in that: the tube wall differing heights place at centrifuge tube has 3 circular holes, has 1 circular hole in the bottom, and each circular hole place is furnished with sealing-plug;
Described tube wall position of opening is positioned at the bottom of each product layer.
2. device according to claim 1 is characterized in that: have internal thread in the described circular hole, sealing-plug has external screw thread.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100115970A CN100408193C (en) | 2005-04-20 | 2005-04-20 | Solid-liquid centrifugal separator of leached and extracted coupling resultant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100115970A CN100408193C (en) | 2005-04-20 | 2005-04-20 | Solid-liquid centrifugal separator of leached and extracted coupling resultant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1853792A CN1853792A (en) | 2006-11-01 |
| CN100408193C true CN100408193C (en) | 2008-08-06 |
Family
ID=37194427
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100115970A Expired - Fee Related CN100408193C (en) | 2005-04-20 | 2005-04-20 | Solid-liquid centrifugal separator of leached and extracted coupling resultant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100408193C (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87201372U (en) * | 1987-02-26 | 1988-01-27 | 王建光 | Separating device for water with dregs |
| CN2257743Y (en) * | 1996-03-30 | 1997-07-16 | 钟会平 | Concentrating grading swirler |
| US6378608B1 (en) * | 1998-02-13 | 2002-04-30 | Framo Engineering A.S. | Apparatus and method for separating oil, water and solids |
| CN1188221C (en) * | 2002-11-29 | 2005-02-09 | 清华大学 | Multifunctional composite type solid-liquid cyclone separator |
-
2005
- 2005-04-20 CN CNB2005100115970A patent/CN100408193C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87201372U (en) * | 1987-02-26 | 1988-01-27 | 王建光 | Separating device for water with dregs |
| CN2257743Y (en) * | 1996-03-30 | 1997-07-16 | 钟会平 | Concentrating grading swirler |
| US6378608B1 (en) * | 1998-02-13 | 2002-04-30 | Framo Engineering A.S. | Apparatus and method for separating oil, water and solids |
| CN1188221C (en) * | 2002-11-29 | 2005-02-09 | 清华大学 | Multifunctional composite type solid-liquid cyclone separator |
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| Publication number | Publication date |
|---|---|
| CN1853792A (en) | 2006-11-01 |
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Granted publication date: 20080806 Termination date: 20110420 |