CN101693946B - Additive and method for extracting vanadium by roasting stone coal ores and preparation method thereof - Google Patents
Additive and method for extracting vanadium by roasting stone coal ores and preparation method thereof Download PDFInfo
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- CN101693946B CN101693946B CN2009100445945A CN200910044594A CN101693946B CN 101693946 B CN101693946 B CN 101693946B CN 2009100445945 A CN2009100445945 A CN 2009100445945A CN 200910044594 A CN200910044594 A CN 200910044594A CN 101693946 B CN101693946 B CN 101693946B
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Abstract
The invention provides an additive and a method for extracting vanadium by roasting stone coal ores and a preparation method thereof. In the invention, the theory of super acid is firstly used to prepare an environmental protection additive for efficiently extracting the vanadium, wherein the additive comprises titanium oxide (TiO2) and tungsten oxide (WO3) in the mass percent of 100 and 3-5. The method for extracting the vanadium by roasting the stone coal ores comprises the following steps of: adding the additive in the smashed stone coal ores to roast together; and carrying out working procedures on the obtained roasted stone coal ore sand, such as acid-leaching, extracting, precipitating, decomposing and the like to obtain vanadium pentoxide. The method can evidently improve the total recycling rate of the vanadium pentoxide and achieve no discharging of waste gas and waste water in the process of the vanadium extraction process; the finally obtained waste residues of the process are good construction raw materials and can be used for the production of machine-made bricks and concretes; and the invention reduces energy consumption and satisfies the technical requirements on a novel environmental protection technology.
Description
Technical field
The present invention relates to a kind of additive and preparation method and corresponding method of extracting metal oxide that ore extracts metal oxide that be used for, be specifically related to additive and preparation method and the corresponding method of extracting Vanadium Pentoxide in FLAKES that ore extracts vanadium.
Background technology
Vanadium Pentoxide in FLAKES is as a kind of extremely important industrial raw material, at metallurgy, and catalysis, novel pigment, battery technologies etc. are widely used in many fields, and huge demand market is arranged.Yet its production technique still rests on common traditional method with salt roasting or baking acid immersion at present, and this processing method is not only polluted greatly, and energy consumption is big, and extraction yield is low.
Summary of the invention
The present invention aims to provide that a kind of extraction yield that improves vanadium, technology are succinct, the bone coal ore deposit extraction vanadium method of environment-protecting clean.
The present invention adopts following scheme:
Get a certain amount of TiO
2, press TiO
2: H
2SO
4(mass ratio) 100: 25～125 put into an amount of H
2SO
4In the solution; Press TiO again
2: WO
3The incorporation of (mass ratio) 100: 3～5 adds sodium wolframate, soaks 2～8 hours; Mixed slurry after drying, again in 300～500 ℃ of roastings 2～6 hours.Prepare a kind of additive that is used for the roasting vanadium extraction of bone coal ore deposit, comprise titanium oxide and tungsten oxide in the additive, and with TiO
2, WO
3Form is calculated, TiO
2With WO
3Mass ratio is 100: 3～5.
Pulverize the bone coal ore and obtain breeze; 1～3% addition adds above-mentioned additive in the breeze by mass percentage, mixed evenly after, add the water body ball; Again with above-mentioned additive and breeze blended bead in 500～900 ℃ of roastings 2～4 hours, naturally cooling gets calcining; Calcining makes Vanadium Pentoxide in FLAKES after operations such as acidleach operation, extraction, precipitation, decomposition.Described bone coal raw ore is crushed to 100～120 orders, and the particle diameter of described additive and breeze blended bead is 1.2～1.5cm.
For improving the acid leaching process condition, the processing condition of described calcining acidleach operation are preferred: be that 3～5% sulfuric acid leached 3～12 hours at 50～100 ℃ with mass concentration, leaching the solid-liquid mass ratio is 1: 1～1: 4.
Each operation after the acidleach operation can adopt following scheme: with the solid-liquid separation on ore pulp that obtains after the acidleach, containing vanadium solution adsorbs with anionite-exchange resin, obtain rich vanadium solution after the desorb, add the ammonium salt precipitation in the rich vanadium solution, obtain the ammonium meta-vanadate precipitation, the thermal degradation ammonium meta-vanadate obtains Vanadium Pentoxide in FLAKES.
The present invention is from the blank roasting-process for extracting vanadium by acid leaching of bone coal navajoite, by to after having added special additive in the bone coal navajoite, carry out high-temperature roasting, roasting condition to the roasting material is controlled, the high conversion and the leaching yield of Vanadium Pentoxide in FLAKES have been realized, step of acid dipping can make the leaching yield of Vanadium Pentoxide in FLAKES reach more than 90%, and total yield is more than 85%.Compare with traditional technology, the present invention can obviously improve the total yield of Vanadium Pentoxide in FLAKES, and accomplishes not have substantially waste gas, discharge of wastewater in the vanadium extraction process, and the last gained waste residue of technology then is a kind of good building material, can be used for machine made brick, Cement Production; During high-temperature roasting, be to heat up, need not replenish other fuel, so reduced energy consumption with the contained carbonaceous burning of bone coal self.This shows that the present invention has embodied the requirement of novel environment friendly Technology.
Embodiment
The present invention is further specified but not to further restriction of the present invention below in conjunction with example:
Embodiment 1:
Get 100 gram TiO
2Be dispersed in the H of 500 milliliters of 1mol/L
2SO
4In, TiO wherein
2: H
2SO
4(mass ratio) 100: 49; Press TiO again
2: WO
3(mass ratio) WO of 100: 3
3Incorporation adds sodium wolframate (Na
2WO
4).Soak after 6 hours in 100 ℃ of dryings, 500 ℃ of roastings 5 hours are prepared into additive.Comprise titanium oxide and tungsten oxide in this additive, and with TiO
2, WO
3Form is calculated, TiO
2With WO
3Mass ratio is 100: 3.
Get somewhere, Hunan bone coal sample ore 100 grams, the Vanadium Pentoxide in FLAKES grade is 1.2% after measured, being crushed to granularity is 80～120 orders, toward wherein adding above-mentioned additive powder 1 gram, be that addition is 1% (mass percent), after stirring, adding water body, to become diameter be 1.2～1.5 centimetres bead, the above-mentioned mixing bead that makes is placed 700 ℃ of roastings of retort furnace 3 hours, naturally cool to room temperature, it is in 4% the sulfuric acid that calcining after the roasting is joined 150 milliliters of mass concentrations, leaching the solid-liquid mass ratio is 1: 2,75 ℃ heat leach 5 hours after solid-liquid separation, repeatedly wash slag with less water, to wash scoriaceous water and sneak in the former leach liquor, obtaining concentration is the vanadium aqueous solution 300ml (the vanadium water concentration is in Vanadium Pentoxide in FLAKES) of 3.7g/L.Leaching yield reaches 92.5%, gets the ammonium meta-vanadate precipitation after inhaling vanadium resins exchange absorption-desorption, ammonium salt precipitation, and the sedimentary purity of thermal degradation is 99% Vanadium Pentoxide in FLAKES, 1.05 grams, and total yield reaches 86.6%.
Embodiment 2:
Get 100 gram TiO
2Be dispersed in the H of 500 milliliters of 2.5mol/L
2SO
4In, TiO wherein
2: H
2SO
4(mass ratio) 100: 122.5; Press TiO again
2: WO
3(mass ratio) WO of 100: 5
3Incorporation adds sodium wolframate (Na
2WO
4).Soak after 8 hours after 100 ℃ of dryings, 400 ℃ of roastings 6 hours prepare additive.Comprise titanium oxide and tungsten oxide in this additive, and with TiO
2, WO
3Form is calculated, TiO
2With WO
3Mass ratio is 100: 5.
Get the sample ore 500g identical with embodiment 1, through being crushed to after granularity is 80～120 orders, add the above-mentioned additive of 15 grams, be that addition is that 3% (mass percent) mixes, group's ball roasting, roasting mechanism is basic identical with example 1, maturing temperature is 900 ℃, roasting time is 4 hours, is that 4% sulfuric acid leaches with the calcining mass concentration after the roasting, and leaching the solid-liquid mass ratio is 1: 2, heat 100 ℃ and leach solid-liquid separation after 4 hours, repeatedly wash slag with less water, will wash scoriaceous water and sneak in the former leach liquor, obtaining concentration is 3.6g/L vanadium aqueous solution 1500mL (the vanadium water concentration is in Vanadium Pentoxide in FLAKES).Leaching yield is 90%, through inhaling vanadium resins exchange absorption-desorption, gets the ammonium meta-vanadate precipitation after the ammonium salt precipitation, and thermal degradation precipitates to such an extent that purity is 99% Vanadium Pentoxide in FLAKES, 5.18 grams, and total yield reaches 85.5%.
Embodiment 3:
Get 100 gram TiO
2Be dispersed in the H of 500 milliliters of 0.5mol/L
2SO
4In, TiO wherein
2: H
2SO
4(mass ratio) 100: 24.5; Press TiO again
2: WO
3(mass ratio) WO of 100: 4
3Incorporation adds sodium wolframate (Na
2WO
4).Soak after 2 hours after 100 ℃ of dryings, 300 ℃ of roastings 6 hours prepare additive.Comprise titanium oxide and tungsten oxide in this additive, and with TiO
2, WO
3Form is calculated, TiO
2With WO
3Mass ratio is 100: 4.
Get the sample ore 400g identical with embodiment 1, through being crushed to after granularity is 80～120 orders, add the above-mentioned additive of 8 grams, be that addition is that 2% (mass percent) mixes, group's ball roasting, roasting mechanism is basic identical with example 1, maturing temperature is 800 ℃, roasting time is 3.5 hours, is that 3.5% sulfuric acid leaches with the calcining mass concentration after the roasting, and leaching the solid-liquid mass ratio is 1: 4, heat 50 ℃ and leach solid-liquid separation after 12 hours, repeatedly wash slag with less water, will wash scoriaceous water and sneak in the former leach liquor, obtaining concentration is 2.2g/L vanadium aqueous solution 2000mL (the vanadium water concentration is in Vanadium Pentoxide in FLAKES).Leaching yield is 91.7%, through inhaling vanadium resins exchange absorption-desorption, gets the ammonium meta-vanadate precipitation after the ammonium salt precipitation, and thermal degradation precipitates to such an extent that purity is 99% Vanadium Pentoxide in FLAKES, 4.13 grams, and total yield reaches 86%.
Claims (4)
1. additive that is used for the roasting vanadium extraction of bone coal ore deposit is characterised in that: comprise titanium oxide and tungsten oxide in the additive, and with TiO
2, WO
3Form is calculated, TiO
2With WO
3Mass ratio is 100: 3～5.
2. one kind prepares the preparation method who is used for bone coal ore deposit roasting additive for extracting vanadium as claimed in claim 1, it is characterized in that: get a certain amount of TiO
2, press TiO
2: H
2SO
4(mass ratio) 100: 25～125 put into an amount of H
2SO
4In the solution; Press TiO again
2: WO
3The incorporation of (mass ratio) 100: 3～5 adds sodium wolframate, soaks 2～8 hours; Mixed slurry after drying, again in 300～500 ℃ of roastings 2～6 hours.
3. the method for a bone coal ore deposit roasting vanadium extraction, it is characterized in that: powder ore obtains breeze; Adopt the described preparation method who is used for bone coal ore deposit roasting additive for extracting vanadium of claim 2 to make additive; 1～3% addition adds above-mentioned additive in the breeze by mass percentage, mixed evenly after, add the water body ball; Again with the above-mentioned bead that makes in 500～900 ℃ of roastings 2～4 hours, naturally cooling gets calcining; Calcining through acidleach, extraction, precipitation, decomposition process, makes Vanadium Pentoxide in FLAKES again.
4. the method for bone coal as claimed in claim 3 ore deposit roasting vanadium extraction is characterized in that: described calcining acid leaching process condition is: be that 3～5% sulfuric acid leached between 50～100 ℃ 3～12 hours with mass concentration, leaching the solid-liquid mass ratio is 1: 1～4: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100445945A CN101693946B (en) | 2009-10-22 | 2009-10-22 | Additive and method for extracting vanadium by roasting stone coal ores and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100445945A CN101693946B (en) | 2009-10-22 | 2009-10-22 | Additive and method for extracting vanadium by roasting stone coal ores and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101693946A CN101693946A (en) | 2010-04-14 |
| CN101693946B true CN101693946B (en) | 2011-05-04 |
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ID=42092942
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100445945A Expired - Fee Related CN101693946B (en) | 2009-10-22 | 2009-10-22 | Additive and method for extracting vanadium by roasting stone coal ores and preparation method thereof |
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| CN107287410B (en) * | 2017-06-30 | 2019-04-09 | 重庆康普化学工业股份有限公司 | It is a kind of for roasting the compound additive and its application method of vanadium extraction |
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Granted publication date: 20110504 Termination date: 20121022 |