CN1298872C - Phosphorus-eliminating purification process of vanadium-containing chamotte leachate - Google Patents
Phosphorus-eliminating purification process of vanadium-containing chamotte leachate Download PDFInfo
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- CN1298872C CN1298872C CNB021555125A CN02155512A CN1298872C CN 1298872 C CN1298872 C CN 1298872C CN B021555125 A CNB021555125 A CN B021555125A CN 02155512 A CN02155512 A CN 02155512A CN 1298872 C CN1298872 C CN 1298872C
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Abstract
The present invention relates to a phosphorus removing purification method of a vanadium containing clinker leaching solution. Crystalline aluminum chloride and crystalline calcium chloride are matched and are prepared to be a solution according to a certain proportion, a proper amount of the solution is added to the vanadium containing clinker leaching solution, and mixtures are uniformly stirred. A flocculating agent is added, mixtures are uniformly mixed, and purified vanadium liquid on an upper layer and underflow liquid are obtained by standing sedimentation. Slag and liquid are separated by carrying out press filtration to the underflow liquid, underflow slag is generated, and filtered liquid is added to the purified vanadium liquid. The present invention has the advantages of obvious economic benefit, easy recovery of vanadium in filtered slag, no change of the existing production technology, easy popularization and application and obvious effect of phosphorus removing purification. The underflow slag generated by the phosphorus removing purification has low content of insoluble vanadium, and the vanadium loss caused by the process of the phosphorus removing purification is effectively reduced. The purifying degree of the vanadium liquid can be increased, and conditions are provided by the production of high grade vanadium.
Description
Technical field
The present invention relates to the technical field of wet method vanadium extraction, relate in particular to the dephosphorization purifying method of the vanadium-contained clinker leaching liquor after a kind of wet method vanadium extraction.
Background technology
In the production process of vanadous oxide, Vanadium Pentoxide in FLAKES, contain vanadium solution carry out dephosphorization purify essential, require dephosphorization to purify back vanadium liquid and contain [P] less than 0.015g/L, or [P]/[V] ratio is below 0.0007, [Si], [Fe] and [Al] plasma concentration all have a threshold quantity.Otherwise quality product is defective, and the precipitation rate descends.
Domestic most wet method vanadium extraction producer purifies vanadium bearing slag or the dephosphorization that contains vanadium solution and all adopts calcium chloride separately, and its characteristics have the dephosphorization good purification, the scavenging agent consumption is few, cost is lower.But, exist dephosphorization and purify the insoluble content of vanadium height of underflow slag that the back produces, cause vanadium to decrease shortcomings such as bigger than normal.For example, domestic production adopts the intermittent type extract technology to produce the method for vanadous oxide, be to concentrate the back to add the calcium chloride solution dephosphorization vanadium-contained clinker leaching liquor to purify, vanadous oxide consumption 50kg industry Calcium Chloride Powder Anhydrous per ton produces underflow slag 60kg, the composition of this underflow slag is (wt, %): ∑ V14.60～27.67, wherein sour molten vanadium 3.55～6.84, insoluble vanadium 9.82～22.51, P0.42～2.75, Ca 10.11～18.58.This shows that the vanadium in the underflow slag mainly exists with the form of insoluble vanadium.
Reclaim in the prior art of vanadium in the underflow slag, have following deficiency:
1, washing method can only reclaim most solvable vanadium in the underflow slag, and insoluble vanadium can not reclaim.
2, smelting ferrovanadium is done the batching adding and is reclaimed vanadium, and phosphorus content exceeds standard, and the vanadium iron product is defective.
3, return production line and reclaim vanadium, sneak into the raw material roasting, not only need drying, pulverizing, and batch mixing is irregular, the local Ca height causes whole roasting grog vanadium transformation efficiency on the low side easily.
4, pickling process reclaims vanadium, and not only the vanadium leaching yield is low, and the impurity in the underflow slag enters solution again, and impurity and purification can cause new vanadium loss again.
Adopt the continous way extract technology to produce the method for Vanadium Pentoxide in FLAKES, it is to add calcium chloride in leaching process that dephosphorization purifies, its consumption rate vanadous oxide is produced much higher, Vanadium Pentoxide in FLAKES per ton needs 155kg calcium chloride, produce more than the underflow slag 180kg, insoluble content of vanadium is greater than 15.12%, underflow slag is together discharged with the leaching residue, underflow slag weight accounts for and leaches 2% of residue total amount, cause and leach that ∑ V content increases nearly 0.3% in the residue, therefore, the residue ∑ V content of Vanadium Pentoxide in FLAKES production discharge is generally more higher than the residue ∑ V content of vanadous oxide production discharge.
Reduce the vanadium loss that vanadium bearing slag leaches vanadium liquid dephosphorization scavenging process, basic way is to change the performance of dephosphorization scavenging agent and supporting operative technique thereof, promptly adopt the dephosphorization decontamination effect improving to get well, the dephosphorization scavenging agent that the insoluble vanadium of underflow slag that produces will lack directly drops on production line, operates and get final product.
Summary of the invention
The objective of the invention is,, provide a kind of dephosphorization purifying method, decrease to reduce vanadium to the vanadium-contained clinker leaching liquor after the wet method vanadium extraction at problems of the prior art.
The dephosphorization purifying method of the vanadium-contained clinker leaching liquor after a kind of wet method vanadium extraction, its spy is to comprise following step:
The employing weight ratio is 1～2: 3～4 crystal aluminum chloride and crystallization calcium chloride, and it makes the dephosphorization decontaminant solutions that contains aluminum chloride and calcium chloride gross weight 10%～15% with the industrial aqueous solution;
It is in 8.5～11.0 the vanadium-contained clinker leaching liquor that the dephosphorization decontaminant solutions for preparing is joined pH value, determines the size of dephosphorization scavenging agent add-on according to the vanadium-contained clinker leaching liquor phosphorus content;
Above-mentioned solution is heated to 80 ± 5 ℃, stirred insulation reaction 10～15 minutes;
Contain vanadium solution with every cubic metre and add 1 liter of neutral polyacrylamide solution that concentration is 3g/L, flocculate, leave standstill clarification;
With the press filtration of sedimentation underflow input plate-and-frame filter press, filtrate is incorporated upper strata purifying vanadium liquid into, and underflow slag reclaims solvable vanadium through washing and filter pressing.
The present invention is containing grog or is containing vanadium solution when being heated to 80 ± 5 ℃, height according to phosphorus content drops into the dephosphorization scavenging agent, continues heated and stirred 10～15 minutes, allows phosphorus, aluminium, iron, calcium plasma fully react, under alkaline condition, produce co-precipitation, reach the purpose that dephosphorization purifies vanadium liquid.
The used flocculation agent of the present invention, for non-ionic polyacrylamide is mixed with the aqueous solution that concentration is about 3.0g/L, every cubic metre of vanadium bearing slag or contain vanadium solution and add 1 liter stirs and leaves standstill, flocculates, clarifies after 10～15 minutes, slag, liquid separation.
Phosphorus, aluminium, iron plasma content are all less than 10mg/L in the dephosphorization purification vanadium liquid of the present invention, and silicone content reduces more than 60%.
The present invention be applicable to leach continuously after the wet method vanadium extraction and intermittently the dephosphorization of extract technology meta-alkalescence vanadium liquid purify, according to the size of the height decision input amount of phosphorus content.Generally, when the intermittent type extract technology concentrates vanadium liquid to handle, V per ton
2O
5Or V
2O
3Product consumes 100～130Kg.Contain that the following purification of [P] 1.0g/L all can obtain the higher purifying vanadium liquid of quality in the vanadium solution.
The invention has the advantages that:
1, technology is simple, and operation is reliable, easily applies.
2, utilize production line dephosphorization cleaning section, directly drop into this technology and get final product, do not need to increase in addition construction investment.
3, dephosphorization good purification, vanadium liquid purifying quality height, particularly the vanadium loss is low, remarkable in economical benefits.
Description of drawings
Fig. 1 is the dephosphorization purification process schema of vanadium-contained clinker leaching liquor.
1-is with vanadium-contained clinker leaching liquor or contain vanadium solution adding mixing tank; 2-adds the dephosphorization scavenging agent; 3-adds flocculation agent; 4-with mixture mixing, heating, stir, leave standstill; 5-upper strata purifying vanadium liquid; 6-underflow liquid; The 7-press filtration; 8-filtrate; The 9-underflow slag; After purifying, the 10-dephosphorization contains vanadium solution.
Embodiment
Below in conjunction with drawings and Examples technical scheme of the present invention is described further.
Embodiment 1
Raw materials used, contain [V] 35.63g/L, [P] 59mg/L, [Fe] 28mg/L, [Al] 21mg/L, [Si] 810mg/L, pH are 10 vanadium-contained clinker leaching liquor 50m
3The input mixing tank is opened steam heating simultaneously, when treating the vanadium-contained clinker leaching liquor capacity, opens pressurized air and stirs, and quantitatively heats the dephosphorization decontaminant solutions 0.9m for preparing
3(about 80Kg) continues heated and stirred it fully reacted, and restir is 10 minutes when treating solution to 80 ± 5 ℃, and then add concentration and be 50 liters of the polyacrylamide solutions of 3g/L, stirred 10 minutes, be input to the settling tank clarification behind the mixing, obtain [V] 35.51g/L, [P]＜10mg/L, [Fe]＜10mg/L, [Al]＜10mg/L, the purifying vanadium liquid of [Si] 281mg/L, the underflow slag that produces through press filtration contains ∑ V 8.27%, sour molten vanadium 6.38%, insoluble vanadium 1.89%, P2.37%.
Embodiment 2
Raw materials used, contain [V] 27.46g/L, [P] 39mg/L, [Fe] 23mg/L, [Al] 19mg/L, [Si] 785mg/L, pH are 9.5 vanadium-contained clinker leaching liquor 50m
3The input mixing tank is opened steam heating simultaneously, when treating the vanadium-contained clinker leaching liquor capacity, opens pressurized air and stirs, and quantitatively heats the dephosphorization decontaminant solutions 0.8m for preparing
3(about 71Kg) continues heated and stirred it fully reacted, and restir is 10 minutes when treating solution to 80 ± 5 ℃, and then add concentration and be 50 liters of the polyacrylamide solutions of 3g/L, stirred 10 minutes, be input to the settling tank clarification behind the mixing, obtain [V] 27.34g/L, [P]＜10mg/L, [Fe]＜10mg/L, [Al]＜10mg/L, the purifying vanadium liquid of [Si] 298mg/L, the underflow slag that produces through press filtration contains ∑ V 7.65%, sour molten vanadium 6.03%, insoluble vanadium 1.62%, P 2.24%.
Embodiment 3
Raw materials used, contain [V] 33.50g/L, [P] 61mg/L, [Fe] 25mg/L, [Al] 18mg/L, [Si] 698mg/L, pH are 10 vanadium-contained clinker leaching liquor 50m
3The input mixing tank is opened steam heating simultaneously, when treating the vanadium-contained clinker leaching liquor capacity, opens pressurized air and stirs, and quantitatively heats the dephosphorization decontaminant solutions 0.8m for preparing
3(about 71Kg) continues heated and stirred it fully reacted, and restir is 10 minutes when treating solution to 80 ± 5 ℃, and then add concentration and be 50 liters of the polyacrylamide solutions of 3g/L, stirred 10 minutes, be input to the settling tank clarification behind the mixing, obtain [V] 33.39g/L, [P]＜10mg/L, [Fe]＜10mg/L, [Al]＜10mg/L, the purifying vanadium liquid of [Si] 244mg/L, the underflow slag that produces through press filtration contains ∑ V 8.81%, sour molten vanadium 6.81%, insoluble vanadium 1.92%, P 3.75%.
Claims (1)
1, the dephosphorization purifying method of the vanadium-contained clinker leaching liquor after a kind of wet method vanadium extraction is characterized in that comprising following step:
(1) the employing weight ratio is 1～2: 3～4 crystal aluminum chloride and crystallization calcium chloride, makes the dephosphorization decontaminant solutions that contains aluminum chloride and calcium chloride gross weight 10%～15% with the industrial aqueous solution;
(2) the dephosphorization decontaminant solutions for preparing being joined pH value is in 8.5～11.0 the vanadium-contained clinker leaching liquor, determines the size of dephosphorization scavenging agent add-on according to phosphorus content in the vanadium-contained clinker leaching liquor;
(3) above-mentioned solution is heated to 80 ± 5 ℃, stirred insulation reaction 10～15 minutes;
(4) contain vanadium solution with every cubic metre and add 1 liter of neutral polyacrylamide solution that concentration is 3g/L, flocculate, leave standstill clarification;
(5) with the press filtration of sedimentation underflow input plate-and-frame filter press, filtrate is incorporated upper strata purifying vanadium liquid into, and underflow slag reclaims solvable vanadium through washing and filter pressing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021555125A CN1298872C (en) | 2002-12-09 | 2002-12-09 | Phosphorus-eliminating purification process of vanadium-containing chamotte leachate |
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| CNB021555125A CN1298872C (en) | 2002-12-09 | 2002-12-09 | Phosphorus-eliminating purification process of vanadium-containing chamotte leachate |
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| CN1506474A CN1506474A (en) | 2004-06-23 |
| CN1298872C true CN1298872C (en) | 2007-02-07 |
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| CNB021555125A Expired - Fee Related CN1298872C (en) | 2002-12-09 | 2002-12-09 | Phosphorus-eliminating purification process of vanadium-containing chamotte leachate |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182037B (en) * | 2007-11-23 | 2011-05-11 | 攀钢集团攀枝花钢铁研究院 | Method for reclaiming vanadium oxide from dephosphorization underflow slag |
| CN102251113A (en) * | 2011-07-12 | 2011-11-23 | 河北钢铁股份有限公司承德分公司 | Method for purifying vanadium leaching solution |
| CN103014378B (en) * | 2011-09-21 | 2014-07-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium liquid purification method |
| CN103014377B (en) * | 2011-09-21 | 2014-07-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium liquid purification method |
| AU2012386620B2 (en) * | 2012-08-01 | 2017-02-02 | Obshestvo S Ogranichennoy Otvetstvennost'yu "Obedinennaya Kompania Rusal Inzhenerno-Tekhnologicheskiy Tsentr" | Method for producing alumina |
| CN103643039B (en) * | 2013-11-29 | 2016-06-22 | 四川省川威集团有限公司 | A kind of solution containing vanadium body defecation method |
| CN104129838B (en) * | 2014-07-18 | 2017-10-24 | 河北钢铁股份有限公司承德分公司 | Leach the sedimentation method of vanadium mud in vanadium liquid |
| CN104310551A (en) * | 2014-11-03 | 2015-01-28 | 天津大沽化工股份有限公司 | Method for removing phosphorus in sewage |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4243639A (en) * | 1979-05-10 | 1981-01-06 | Tosco Corporation | Method for recovering vanadium from petroleum coke |
| DE3524703A1 (en) * | 1985-07-11 | 1987-01-22 | Elektrometallurgie Gmbh | Process for preparing low-phosphorus vanadium compounds from high-phosphorus vanadium slags |
| CN1321782A (en) * | 2000-04-28 | 2001-11-14 | 四川川投峨眉铁合金（集团）有限责任公司 | Wet process for extracting vanadium from waste catalyst |
-
2002
- 2002-12-09 CN CNB021555125A patent/CN1298872C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4243639A (en) * | 1979-05-10 | 1981-01-06 | Tosco Corporation | Method for recovering vanadium from petroleum coke |
| DE3524703A1 (en) * | 1985-07-11 | 1987-01-22 | Elektrometallurgie Gmbh | Process for preparing low-phosphorus vanadium compounds from high-phosphorus vanadium slags |
| CN1321782A (en) * | 2000-04-28 | 2001-11-14 | 四川川投峨眉铁合金（集团）有限责任公司 | Wet process for extracting vanadium from waste catalyst |
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