CN1023693C - Process for extracting of vanadium pentoxide by water immersion from cured mixture of stone coal ash with surfuric acid by heating - Google Patents
Process for extracting of vanadium pentoxide by water immersion from cured mixture of stone coal ash with surfuric acid by heating Download PDFInfo
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- CN1023693C CN1023693C CN 90104669 CN90104669A CN1023693C CN 1023693 C CN1023693 C CN 1023693C CN 90104669 CN90104669 CN 90104669 CN 90104669 A CN90104669 A CN 90104669A CN 1023693 C CN1023693 C CN 1023693C
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Abstract
The present invention relates to a technological process for extracting V205 from difficultly-oxidized stone coal ash slag, which comprises: boiling furnace ash slag is stirred with sulphuric acid to be slaked at 100 to 250 DEG C for 1 to 3 hours, and a V205 product can be obtained by the working procedures of water immersion, solid-liquid separation, crystallization of potassium alum and ammonium alum, reduction, extraction, back-extraction, oxidation, alum precipitation, calcination, etc. The overall recovery rate of V205 of the process of the present invention is over 62%, and 10 tons of pure potassium alum and 55 tons of pure ammonium alum can be recovered by producing one ton of V205.
Description
The present invention relates to stone coal ash and extract Vanadium Pentoxide in FLAKES technology.
According to the seventies integrated survey of geology department, the Vanadium Pentoxide in FLAKES reserves surpass the summation of the explored Vanadium Pentoxide in FLAKES resource of other countries in the world in China's bone coal.When utilizing bone coal to act as a fuel, extracting Vanadium Pentoxide in FLAKES from its lime-ash is a great problem.Zhejiang Province chemical research institute success water logging slag acid heap leaching method and bone coal fluidizing furnace lime-ash extraction Vanadium Pentoxide in FLAKES process integration (" coal processing and comprehensive utilization ", 1989, No.6, P.22-24).Domestic technology is the bone coal boiling direct acidleach of ashes or sodium roasting water logging slag acidleach and stone coal ash alkali soaking technology more basically.(" non-ferrous metal ", 1988, the 4th phase, P.43～46 mainly be illitic bone coal raw material) for containing navajoite stone and since wherein vanadium exist valence state quite complicated, major part is a trivalent vanadium, adopt the direct acidleach of bone coal fluidizing furnace lime-ash, alkali soaks, and normal temperature is mixed technologies such as sour slaking, and the transformation efficiency of its Vanadium Pentoxide in FLAKES is all undesirable.European patent EP-49-064 proposes with peroxosulphuric (H
2SO
5) make vanadium be completely oxidized to the method for pentavalent vanadium with the hydrogen peroxide mixed solution.The transformation efficiency height of this method, but that cost does not have is considerable with fixed attention.
The objective of the invention is to seek a kind of from dysoxidizable stone coal ash the high efficiency extraction Vanadium Pentoxide in FLAKES, cost is low, fully reclaims the technical process of byproduct.
Through lab scale, pilot scale is studied repeatedly, has realized finishing the technical process of task of the present invention finally, and concrete technical process is as follows:
1. raw material:
Generate electricity with 6 tons of boiling furnace combustions in Jiangxi eight all bone coal, collecting dust-removing device flying dust is paid bed overflow slag, main bed overflow slag, and the three is 28: 28: 15 weight ratio fusion in proportion, after 60 mesh sieves, makes 95% lime-ash cross 60 mesh sieves through broken mill.V205 content is greater than 0.8 weight % in the raw material.
2. mix sour slaking:
Admix industrial sulphuric acid.
Lime-ash: sulfuric acid=100: the 35-50(weight ratio),
Curing temperature: 100-250 ℃,
Curing time: 1-3 hour.
3. water logging: the lime-ash water logging after the slaking, wherein:
Liquid-solid ratio=1-3.
Water soaking temperature 60-90 ℃.
1-3 hour water logging time.
The average leaching yield of V205 is 68.2%.
4. solid-liquid separation:
Ore pulp after the leaching is sent into vacuum apparatus (40-90 ℃) vacuum filtration while hot immediately and is obtained containing the filtrate of V205, and wet slag is through three sections countercurrent washings, and the once washing water cycle is returned and soaked grog, and two, three times wash water recycles, and residue enters the tailings pond.
5. potassium alum crystallization:
After leaching back stoste placement, separate out along with temperature reduces potassium alum, its Tc is 0-30 ℃, keeps crystallization time 24-140 hour, obtains thick potassium alum crystallization and mother liquor after the filtration./
6. tschermigite crystallization:
Mother liquor after potassium alum filters is sent into neutralizing well and is added bicarbonate of ammonia adjusting pH value 1.8-2.2, at room temperature stirs 30-60 minute, places 1-2 hour after-filtration again and obtains thick tschermigite product.
7. reduction: (vanadium unification in the present invention is in the V205 weight percentage)
The solution that extracts behind the tschermigite is squeezed into header tank with pump, flows into reduction column, filling iron filings and quartz sand in the reduction column, and the control flow velocity, solution potential is reduced to below 250 millivolts more than 400 millivolts by reduction is preceding.Reduction process makes vanadium be reduced into tetravalence, and reduction process V205 yield is more than 97%.
8. extracting vanadium: the mother liquor after the reduction enters extraction tank.
Extraction agent is kerosin (65% kerosene+20%P204+15%TBP), can effectively extract the tetravalence vanadium of P204 and TBP.Extraction procedure is countercurrent flow.Organic phase: water=1: 2.5.Be 5 minutes duration of contact, six grades of extractions.The continuous operation stable operation does not have emulsion, does not have third phase to form yet.Percentage extraction is greater than 98%.
9. the reextraction of vanadium:
Saturated organic phase after extraction flows into the reextraction groove, with the vanadium in the sulfuric acid back extraction organic phase of 3N, and a back extraction vanadium under this acidity and not back extraction molybdenum, impurity such as iron can reach the purpose of purifying effectively.In the reextraction groove, the stream of organic phase and water ratio is 6: 1,5 minutes duration of contact.Pyatyi is stripped.Smooth operation in continuous operation does not produce emulsion.Stripping rate can reach more than 99%.
10. oxidation:
In anti-stripping agent, add 200 grams per liter sodium chlorate solutions, make the tetravalence vanadium in the solution be oxidized to the pentavalent vanadium.Solution potential should be more than 900 millivolts.
11. precipitation:
Through the acidic solution that contains the pentavalent vanadium of oxidation, regulate the pH value to 2-3 with ammoniacal liquor, solution temperature is 90 ℃, 1-1.5 hour precipitation time.After filtering, heavy hall obtains ammonium poly-vanadate.
12. calcining:
The ammonium poly-vanadate filter cake that precipitation obtains, 110-120 ℃ dry 2 hours down, then in oxidizing atmosphere in 450-500 ℃ of calcining 3 hours, obtain yellow powdery Vanadium Pentoxide in FLAKES product.The Vanadium Pentoxide in FLAKES total yield is more than 62%.
The drawing explanation:
Fig. 1 is a process flow sheet of the present invention.
Flow process of the present invention is because through mixing the acid slaking operation of heating. Make the stone coal ash raw material of the valence state complexity of dysoxidizable vanadium obtain oxidation, make the average water logging rate of V205 more than 68%. The reduction process vanadium recovery is more than 97%. Extraction efficiency is more than 98%, and reextraction efficient is more than 99%. Precipitation efficient is more than 99%, and ammonium poly-vanadate acid decomposition yield is more than 98%. Because each operation rate of recovery height makes the vanadic anhydride overall recovery more than 62%, and one ton of vanadic anhydride of every production can obtain 10 tons of smart potassium alums simultaneously, 55 tons of ammonia-alums, examine through pilot scale, the totle drilling cost of vanadic anhydride per ton is more than 53000 yuan, recyclable more than 19000 yuan of byproduct is down to below 30000 yuan the integrated cost of vanadic anhydride per ton.
Embodiment
Processing contains 5 tons of the bone coal fluidizing furnace lime-ash of V205 average grade 1.05 weight %, obtains 7.25 tons in grog, and wherein 4 tons of grogs are through water logging, and the vanadium leachate that contains that obtains 5.5 cubic metres extracts continuous operation.Expanding test result shows: in acid consumption 45% o'clock for ash weight, the transformation efficiency of V205 is 68.6%, and the total yield of Vanadium Pentoxide in FLAKES is 62.2%, and smart vanadium product pentoxide content is greater than 98%, and quality product meets the requirement of national standard " GB3283-82 ".
Pilot scale bone coal chemical ingredients (weight %), main V205 0.84%, the SiO of containing
258.45%, Al
2O
37.5%, Fe
2O
32.29%, FeO1.23%, K
2O1.99%, CaO2.65%, MgO1.27% etc., the volatile content in the bone coal are 16.60%.
Bone coal generates electricity through 6 tons of boiling furnace combustions, V205 in the main bed overflow slag of collecting is 0.83 weight %, V205 content in the attached bed overflow slag is 1.09 weight %, V205 content in the fly-ash separator flying dust is 1.12 weight %, with the fly-ash separator flying dust, pay a bed overflow stream slag, main bed overflow slag makes 95% lime-ash by 60 orders by 28: 28: 15 weight ratio fusion through broken mill.Average V205 content in the raw material is 1.05 weight %, SiO
263.83 weight %, Al
2O
39.80 weight %, Fe
2O
35.35 weight % etc.
Mixed ash mixes with 45% sulfuric acid, sends into the revolution curing oven after stirring, and grey slag charge adds from stove tail opening for feed, and 230-250 ℃ hot blast blasts from burner, and both are countercurrent flow.00-120 ℃ of feed end temperature, interior temperature 150-200 ℃ of stove, 180-200 ℃ ℃ of discharge end temperature, 5 kilograms/hour of input speeds, the ash slag charge is 2 hours at residing time in furnace, the material outward appearance of being discharged by discharge gate is a cobble shape not of uniform size, it is cellular that inside is, circuitous water is frangible, the grog of discharging does not need to send into the water logging reactor through fragmentation again, water soaking temperature is 70-80 ℃, time is 2 hours, and liquid-solid ratio is to contain V2051.05 weight % in the lime-ash before 2 leachings, leach that to contain V205 in the leach liquor of back be 3.56 grams per liter sulfuric acid, 107.3 grams per liters, leaching yield be 68.2% and same acids to consume the leaching yield of direct pickling process only be 45%, ore pulp after the leaching is sent into the vacuum apparatus filtered while hot immediately, since eight all in the rock ballast lime-ash potassium content higher, be lower than 30 ℃ when filtering temperature, potassium alum is separated out blocking pipe and is caused the tailings after filtration difficulty filters to carry out three sections countercurrent washings in steel basin, washing back tailings discards a wash water and returns the ripe rice of leaching, two, three times wash water recycles.V205 content is in the analysis wash water: wash water 0.725 grams per liter, and secondary wash water 0.276 grams per liter, three wash water 0.086 grams per liters, washing effect is 99.6%.Leach rear filtrate through placing, separate out successively along with temperature reduces potassium alum, the crystallisation by cooling temperature of potassium alum is 25 ℃, 140 hours time.The filtrate compositional analysis result that potassium alum is separated out before and after the test is: leach rear filtrate and contain V2053.42 grams per liter, H
2SO
4101.9 grams per liter.Potassium alum filters in the mother liquor of back and contains the V2053.37 grams per liter, H
2SO
4102.3 grams per liter, thick potassium alum productive rate is 13.69 tons of/ton V205.Mother liquor after potassium alum filters is sent into neutralizing well and is added bicarbonate of ammonia adjusting pH1.8-2.2.At room temperature stirred 1 hour, tschermigite is separated out successively, and centrifuging obtains thick tschermigite product after placing hour.Tschermigite is separated out the mother liquor composition analysis revealed before and after the test, contains V205 in the potassium alum filtrated stock, 3.37 grams per liters, H
2SO
4102.3 filtering in the mother liquor of back, grams per liter, tschermigite contain the V2053.42 grams per liter, H
2SO
411 grams per liters, thick tschermigite productive rate is 58.82 tons of/ton V205.The thick potassium alum that obtains adds the hot water dissolving, removes by filter insoluble substance, and crystallisation by cooling obtains the refining thick tschermigite of potassium alum product and obtains technical grade tschermigite product after with saturated tschermigite solution washing.
This technology is selected the tetravalence vanadium in the phosphine kind of extractants P204 energy selective extraction solution for use.Therefore the essential reduction of solution before extraction.Solution behind the extraction tschermigite is squeezed into header tank with pump, flows into reduction column, is filled with iron filings and quartz sand in the reduction column, and the control flow velocity makes solution pass through reduction column, and the solution variation sees Table 1 before and after the reduction.(table is seen the literary composition back)
Extraction agent is the kerosin (its weight ratio is: 20: 15: 65) of P204 and TBP.Organic extractant and extraction stoste are countercurrent flow in the extraction process, two-phase flow ratio: organic phase: be 5 minutes water=1: 2.5 duration of contact, six grades of extractions, stable operation in continuous operation, do not have emulsification or third phase to form, the Vanadium Pentoxide in FLAKES change in concentration of two-phase outlet sees Table 2.(table is seen the literary composition back)
Saturated organic phase after extraction flows into the reextraction groove, with the vanadium in the sulfuric acid back extraction organic phase of 3N, a back extraction vanadium under this acidity and impurity such as not back extraction molybdenum, iron can reach the purpose of purifying, effectively in the reextraction groove, the stream ratio of organic phase and water is 6: 1,5 minutes duration of contact, Pyatyi is stripped, smooth operation in continuous operation, do not produce emulsion, the partial results of two-phase outlet V205 concentration analysis is listed in table 3 after the reextraction balance.(table is seen the literary composition back)
As seen from the experiment: when the V205 mean concns was 8.67 grams per liters in the saturated organic phase, the V205 mean concns was 0.038 grams per liter in the poor organic phase after the Pyatyi back extraction, and stripping rate reaches 99.56%.
Vanadium is oxidized to the pentavalent vanadium earlier with 200 grams per liter sodium chlorate solution oxidations for making the tetravalence vanadium in the solution in the anti-stripping agent, and current potential should be regulated the pH value to 2-3 with ammoniacal liquor again more than 900 millivolts, and the precipitation temperature is 90 ℃, and time 1-1.5 hour, experimental result was listed in table 4.(table is seen the literary composition back)
The resulting ammonium poly-vanadate in back is filtered in precipitation.110-120 ℃ dry 2 hours down, then in oxidizing atmosphere in 450-500 ℃ of calcining 3 hours, obtain yellow powdery Vanadium Pentoxide in FLAKES product.Calcining yield 98%.Its mass analysis result is for listing in table 5.(table is seen the literary composition back)
By table 5 as seen, can reach metallurgical V20598 level during product matter of the present invention.
Through cost keeping, the total cost of Vanadium Pentoxide in FLAKES per ton is 53621.8 yuan, and one ton of V205 of every production can obtain 9 tons of potassium alums, can take in 4500 yuan, can obtain 55 tons of tschermigites, can take in 19250 yuan, so the comprehensive cost of V205 per ton is 29871.8 yuan.Realized the comprehensive utilization of bone coal.Technology of the present invention is owing to V205 transformation efficiency height, and cost is low, and byproduct has been recycled, therefore improved economic benefit, strengthen the competitive capacity of product, under the situation that current world market vanadium valency drops significantly, more demonstrated the vitality of technical process of the present invention.
Solution changes (concentration grams per liter) before and after table 1 reduction
V205 Fe Fe H
2SO
4Current potential (millivolt) pH
Reduce preceding 3.57 12.15 6.45 8.23 410 1.72
Reduction back 3.50 little 23.90 6.14 218 2.14
Two-phase outlet vanadium change in concentration behind table 2 extraction equilibrium
Sequence number collection stoste V grams per liter saturated organic phase V grams per liter raffinate water V grams per liter percentage extraction %
1 3.48 8.66 0.038 98.91
16 3.55 8.37 0.063 98.22
20 3.49 8.72 0.028 99.20
25 3.44 8.58 0.052 98.49
Average 3.50 8.67 0.044 98.74
Two-phase outlet V205 concentration after the table 3 reextraction balance
Water after the poor organic phase back extraction of saturated organic phase
Stripping rate %
V205 grams per liter V205 grams per liter V205 grams per liter
0.038 52.40 99.56
0.026 52.40 99.70
8.72
0.031 52.40 99.64
0.046 52.40 99.47
0.037 50.32 99.57
0.048 50.32 99.44
8.61
0.046 50.32 99.47
0.031 50.32 99.64
Table 4 ammonium depositing in water vanadium test-results
Reaction water is formed grams per liter ammonia volume liter/mother liquor V205 before the precipitation
Mother liquor pH precipitation rate %
Premium on currency phase V205 grams per liter
The total Fe H of V205
2SO
4
0.235 2.62 0.34 99.34
0.230 2.47 0.38 99.27
51.8 0.75 138.4
0.237 2.55 0.34 99.34
0.234 2.54 0.35 99.32
The smart vanadium quality level of table 5
Scope of application chemical metallurgy expands the smart vanadium of examination
Trade mark product
Composition V205 99 V205 98 V205 97
V205 99.0 98.0 97.0 98.02
Si 0.15 0.25 0.50 ＜0.1
Fe 0.20 0.40 0.30 0.29
P 0.03 0.05 0.30 0.032
S 0.01 0.03 0.30
AS 0.01 0.02 0.02 0.0026
Na
2O+K
2O 1.0 1.5 1.0 K
2O0.01
Na
2O0.24
V
2O
42.5
Physical condition sheet sheet powdery powdery
Claims (9)
1, a kind of stone coal ash extracts Vanadium Pentoxide in FLAKES technology, the invention is characterized in: the lime-ash raw material makes 95% lime-ash can cross 60 mesh sieves through broken mill, lime-ash and sulfuric acid weight ratio are 100: 35-50, mix acid after 100-250 ℃ slaking 1-3 hour, water soaking temperature is 60-90 ℃, time 1-3 hour, ore pulp 40-90 after the leaching ℃ is carried out vacuum filtration, through three washings, thick potassium alum is separated out in the filtrate cooling, filters the back mother liquor and regulates pH1.8-2.2 with bicarbonate of ammonia, filtration obtains thick tschermigite, filtrate is used iron reduction, makes into the tetravalence vanadium, the mother liquor after the reduction P204 and six grades of extractions of TBP kerosin adverse current, the tetravalence vanadium enters organic phase, use the tetravalence vanadium in the 3N sulfuric acid back extraction organic phase again, Pyatyi is stripped, and anti-stripping agent is oxidized to the pentavalent vanadium with sodium chlorate (200 grams per liter), regulate pH to 2-3 with ammoniacal liquor, complete until heavy hall, filter the ammonium poly-vanadate drying that obtains and be 400-550 ℃ of calcining 2-4 hour again, obtain the Vanadium Pentoxide in FLAKES product.
2, technical process according to claim 1 is characterized in that, fly-ash separator flying dust in the lime-ash: pay bed overflow slag: main bed overflow slag=28: 28: 15.
3, technical process according to claim 1, it is characterized in that preferred acid consumption is 45% of ash weight, send into the revolution curing oven after stirring, grey slag charge adds from stove tail opening for feed, and 230-250 ℃ hot blast blasts from burner, both are countercurrent flow, 00-120 ℃ of feed end temperature, interior temperature 150-200 ℃ of stove, 180-200 ℃ of discharge end temperature, 5 kilograms/hour of input speeds, grey slag charge stopped in stove 2 hours.
4, technical process according to claim 1 is characterized in that: preferred water logging technology is that liquid-solid ratio equals 2, and water soaking temperature is 70-80 ℃, 2 hours water logging time.
5, technical process according to claim 1 is characterized in that: the wet slag that vacuum filtration obtains is washed through three sections adverse currents, and one time wash water returns the leaching grog, and two, three times wash water recycles.
6, technical process according to claim 1 is characterized in that: the crystallisation by cooling temperature of potassium alum is 25 ℃, and 140 hours time, thick potassium alum productive rate is 13 tons of/ton V205.When regulating the pH value to 2-3 with bicarbonate of ammonia, tschermigite is separated out, and the productive rate of thick tschermigite is 58 tons of/ton V205.
7, technical process according to claim 1, it is characterized in that: P204 in the extraction agent: TBP: kerosene=20: 15: 65, organic phase: water=1: 2.5, the saturated organic phase after extraction is stripped with the sulfuric acid of 3N, organic phase is 6: 1 with the stream ratio of water, and be 5 hours duration of contact.
8, technical process according to claim 1 is characterized in that: the solution potential of sodium chlorate solution's oxidation should be more than 900 millivolts, and the precipitation condition is that the pH value is 2-3,90 ℃ of precipitation temperature, time 1-1.5 hour.
9, technical process according to claim 1 is characterized in that: the ammonium poly-vanadate filter cake is calcined in oxidizing atmosphere through 110-120 ℃ of drying 2 hours.
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|---|---|---|---|
| CN 90104669 CN1023693C (en) | 1990-07-12 | 1990-07-12 | Process for extracting of vanadium pentoxide by water immersion from cured mixture of stone coal ash with surfuric acid by heating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90104669 CN1023693C (en) | 1990-07-12 | 1990-07-12 | Process for extracting of vanadium pentoxide by water immersion from cured mixture of stone coal ash with surfuric acid by heating |
Publications (2)
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| CN1049642A CN1049642A (en) | 1991-03-06 |
| CN1023693C true CN1023693C (en) | 1994-02-09 |
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Cited By (3)
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|---|---|---|---|---|
| CN100422357C (en) * | 2007-01-29 | 2008-10-01 | 中经九丰（北京）投资有限公司 | Method for electrolyzing vanadium slurry and extracting vanadium pentexide using film |
| CN100465307C (en) * | 2007-06-29 | 2009-03-04 | 黎吉星 | Stone-like coal gas phase vanadium extracting method |
| CN101585553B (en) * | 2009-07-06 | 2010-09-22 | 云南俊驰环保科技有限公司 | Method for producing vanadium pentoxide by ore containing vanadium and intermediate material containing vanadium |
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| CN1040132C (en) * | 1992-08-12 | 1998-10-07 | 湖南省洪江市黔城钒厂 | Settling process for extracting vanadium from bone coal |
| CN1319863C (en) * | 2004-09-24 | 2007-06-06 | 刘亚光 | Method of producing ranadium pentoxide using vanadium containing waste catalyst |
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| CN102912144A (en) * | 2012-09-12 | 2013-02-06 | 北京矿冶研究总院 | Method for leaching vanadium pentoxide from vanadium-containing soot |
| CN117327930B (en) * | 2023-12-01 | 2024-02-27 | 中国恩菲工程技术有限公司 | Method for recovering vanadium from primary shale stone coal |
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1990
- 1990-07-12 CN CN 90104669 patent/CN1023693C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100422357C (en) * | 2007-01-29 | 2008-10-01 | 中经九丰（北京）投资有限公司 | Method for electrolyzing vanadium slurry and extracting vanadium pentexide using film |
| CN100465307C (en) * | 2007-06-29 | 2009-03-04 | 黎吉星 | Stone-like coal gas phase vanadium extracting method |
| CN101585553B (en) * | 2009-07-06 | 2010-09-22 | 云南俊驰环保科技有限公司 | Method for producing vanadium pentoxide by ore containing vanadium and intermediate material containing vanadium |
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|---|---|
| CN1049642A (en) | 1991-03-06 |
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