CN101693947B - 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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- CN101693947B CN101693947B CN2009100445998A CN200910044599A CN101693947B CN 101693947 B CN101693947 B CN 101693947B CN 2009100445998 A CN2009100445998 A CN 2009100445998A CN 200910044599 A CN200910044599 A CN 200910044599A CN 101693947 B CN101693947 B CN 101693947B
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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. The additive comprises alkali metal nitrates and hydroxides of aluminum in the mass percent of 1:0.5-3. The method for extracting vanadium by roasting the stone coal ores comprises the following steps: 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 residues in the vanadium extraction process. Compared with the traditional method, the method also greatly reduces waste water discharging, 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
China south extensively is distributed with a large amount of bone coals, wherein is rich in a large amount of Vanadium Pentoxide in FLAKESs.China extracts the most sodium roasting technologies that adopt of vanadium technology from bone coal, produce a large amount of chlorine in roasting process, and hydrogen chloride gas contains a large amount of salinities in the waste water, environment is caused serious pollution, and the total yield of the Vanadium Pentoxide in FLAKES in the ore is low.Then acid consumption of the roasting-acid leaching process that adopts is huge, not only pollutes greatly, and energy consumption is big, and extraction yield is low, the subsequent disposal difficulty.
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:
One of addictive preparation method: will by mass ratio be 1: 0.5～3 saltpetre or/and SODIUMNITRATE and alumag mix, levigate after, in 500～700 ℃ of roastings 3～7 hours.
Two of addictive preparation method: with the aluminum nitrate wiring solution-forming of certain mass, by nitrate and aluminum nitrate mass ratio is to drop into an amount of saltpetre or/and after the SODIUMNITRATE in 1: 2～1: 4, add ammoniacal liquor and be stirred to gel formation, after the drying, in 500～700 ℃ of roastings 3～7 hours.Reaction obtains aluminium hydroxide and ammonium nitrate to aluminum nitrate with ammoniacal liquor, and after the roasting, ammonium nitrate resolves into ammonia, nitrogen, gas evolution such as oxygen, only remaining nitrate and alumag solid.
Adopt one of above-mentioned preparation method to prepare to be used for the additive of bone coal ore deposit roasting vanadium extraction, comprise the oxyhydroxide of base metal nitrate and aluminium in the additive, and the oxyhydroxide mass percent of nitrate and aluminium is 1: 0.5～3.
The method of bone coal ore deposit roasting vanadium extraction is as follows:
Powder ore obtains breeze, and the addition of pressing mass ratio 3～5% adds above-mentioned additive in breeze, mixed evenly after, add the water body ball, make the mixing ore particle; Again with the above-mentioned mixing ore particle that makes in 500～800 ℃ of roastings 2～4 hours, naturally cool to room temperature and get calcining; Calcining through operations such as acidleach, extraction, precipitation, decomposition, makes Vanadium Pentoxide in FLAKES again.
Described bone coal raw ore is crushed to 80～120 orders, and the particle diameter that mixes ore particle is 1.2～1.5cm.
For improving the acidleach operation, its processing condition are: be that 3～5% sulfuric acid leached between 40～100 ℃ 3～12 hours with mass concentration, leaching solid-to-liquid ratio is 1: 1～1: 4.
Each operation after the acidleach can adopt following scheme: leach liquor obtains rich vanadium solution with inhaling after the vanadium resin absorption is separated, and rich vanadium solution adds ammonium salt and obtains the ammonium meta-vanadate precipitation, and ammonium meta-vanadate precipitation thermal degradation can get Vanadium Pentoxide in FLAKES.
The present invention by to after adding special additive in the bone coal navajoite, carries out high-temperature roasting from the blank roasting-process for extracting vanadium by acid leaching of bone coal navajoite, the roasting condition of roasting material is controlled, because super base can activate formation K in the high-temperature calcination process
2O or Na
2The sandwich structure of O, thereby make the silicate sturcture that contains vanadium minerals in the bone coal navajoite suffer strong destruction, cause that the Vanadium Pentoxide in FLAKES of inclusion is exposed to mineral surface in the ore, therefore when acidleach, can access good leaching, can realize the high conversion and the leaching yield of Vanadium Pentoxide in FLAKES.Step of acid dipping can make the leaching yield of Vanadium Pentoxide in FLAKES reach more than 85%, and the vanadium extraction total yield is more than 80%.Compare with traditional method, can improve the total yield of Vanadium Pentoxide in FLAKES significantly; Wastewater discharge also reduces greatly.And accomplish non-exhaust emission in the vanadium extraction process substantially, the slag after the vanadium extraction also can be used for cement, the production of material of construction such as machine made brick.Required roasting high temperature is supplied with by bone coal self burning, need not add other fuel, greatly reduces energy consumption.This shows that the present invention has reached 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 saltpetre 10 grams, aluminium hydroxide 30 grams, mixing is pulverized.700 ℃ of roastings are 5 hours in retort furnace, obtain additive, and comprise saltpetre and aluminium hydroxide in this additive, saltpetre: the aluminium hydroxide mass percent is 1: 3.
Get somewhere, Hunan bone coal sample ore 100 grams, the Vanadium Pentoxide in FLAKES taste is 1.2% after measured, and being crushed to granularity is between 80～120 orders; Toward wherein adding above-mentioned additive 3 grams, addition is equivalent to 3%, and after stirring, adding water body, to become diameter be 1.2～1.5 centimetres bead, makes the mixing ore particle; Above-mentioned mixing ore particle is placed 700 ℃ of roastings of retort furnace 3 hours, naturally cool to room temperature and get calcining, it is in 4% the sulphuric acid soln that above-mentioned calcining is joined 150 milliliters of mass concentrations, leaching the solid-liquid mass ratio is 1: 2, heated leaching after 3 hours at 75 ℃, solid-liquid separation, the washing slag is incorporated into wash water in the leach liquor.Obtaining concentration is the vanadium aqueous solution 300ml of 3.5g/L, and leaching yield reaches 87%, and through inhaling the absorption of vanadium resins exchange, desorb gets the ammonium meta-vanadate precipitation after the ammonium salt precipitation, and the sedimentary purity of thermal degradation is 99% Vanadium Pentoxide in FLAKES, 1.02 grams, and total yield reaches 84.2%.
Embodiment 2:
Get aluminium hydroxide 30 grams, saltpetre 9 grams, SODIUMNITRATE 6 grams, mixing is pulverized.650 ℃ of roastings are 7 hours in retort furnace, obtain additive, comprise saltpetre, SODIUMNITRATE and aluminium hydroxide in this additive, and nitrate (containing saltpetre and SODIUMNITRATE total mass): the aluminium hydroxide mass percent is 1: 2.
Adopt above-mentioned additive, other condition method substantially the same manner as Example 1 is extracted Vanadium Pentoxide in FLAKES from the bone coal ore, and its total yield can reach 81.6%.
Embodiment 3
With the aluminum nitrate wiring solution-formings of 30 grams, by SODIUMNITRATE and aluminum nitrate mass ratio be drop into the SODIUMNITRATE of 10 grams at 1: 3 after, adding ammoniacal liquor is stirred to gel formation, after the drying, 500 ℃ of roastings 7 hours.Obtain additive, comprise SODIUMNITRATE and aluminium hydroxide in this additive, SODIUMNITRATE: the aluminium hydroxide mass percent is about 1: 1.1.
Get above-mentioned sample ore 200g, being crushed to granularity is between 80～120 orders; Add massfraction afterwards and be the additive among 5% the embodiment 1, after stirring, adding water body, to become diameter be 1.2～1.5 centimetres bead, makes the mixing ore particle; Above-mentioned mixing ore particle is placed 500 ℃ of roastings of retort furnace 4 hours, naturally cool to room temperature and get calcining, is that 4% sulfuric acid leaches with above-mentioned calcining with the 300ml mass concentration, leaching the solid-liquid mass ratio is 1: 2, heat 50 ℃ and leached 10 hours, solid-liquid separation, the washing slag is incorporated into wash water in the leach liquor.Obtaining concentration is 4.1g/L vanadium aqueous solution 500mL.Leaching yield is 85.4%, and through inhaling the absorption of vanadium resins exchange, desorb gets the ammonium meta-vanadate precipitation after the ammonium salt precipitation, and it is 99% Vanadium Pentoxide in FLAKES, 2.02 grams that the thermal degradation precipitation obtains purity, and total yield reaches 83.3%.
Embodiment 4
With the aluminum nitrate wiring solution-formings of 30 grams, by saltpetre and aluminum nitrate mass ratio be drop into the saltpetre of 20 grams at 1: 1.5 after, adding ammoniacal liquor is stirred to gel formation, after the drying, 600 ℃ of roastings 6.5 hours.Obtain additive, comprise saltpetre and aluminium hydroxide in this additive, saltpetre: the aluminium hydroxide mass percent is about 1: 0.55.
Get bone coal sample ore 500 grams, the Vanadium Pentoxide in FLAKES taste is 1.2% after measured, and being crushed to granularity is between 80～120 orders; Toward wherein adding above-mentioned additive 20 grams, addition is equivalent to 4%, and after stirring, adding water body, to become diameter be 1.2～1.5 centimetres bead, makes the mixing ore particle; Above-mentioned mixing ore particle is placed 800 ℃ of roastings of retort furnace 2 hours, naturally cool to room temperature and get calcining, it is in 5% the sulphuric acid soln that above-mentioned calcining is joined 1000 milliliters of mass concentrations, leaching the solid-liquid mass ratio is 1: 2.5, heated leaching after 12 hours at 100 ℃, the washing slag is incorporated into wash water in the leach liquor.Obtaining concentration is the vanadium aqueous solution 1600ml of 3.3g/L, and leaching yield reaches 88%, and through inhaling the absorption of vanadium resins exchange, desorb 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, 4.87 grams, and total yield reaches 81.2%.
Claims (6)
1. additive that is used for the roasting vanadium extraction of bone coal ore deposit is characterised in that: comprise saltpetre in the additive or/and the oxyhydroxide of SODIUMNITRATE and aluminium, and the oxyhydroxide mass percent of nitrate and aluminium is 1: 0.5～3.
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: will by mass ratio be 1: 0.5～3 saltpetre or/and SODIUMNITRATE and alumag mix, levigate after, in 500～700 ℃ of roastings 3～7 hours.
3. 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: with the aluminum nitrate wiring solution-forming of certain mass, by nitrate and aluminum nitrate mass ratio is to drop into an amount of saltpetre or/and after the SODIUMNITRATE in 1: 2～1: 4, add ammoniacal liquor and be stirred to gel formation, after the drying, in 500～700 ℃ of roastings 3～7 hours.
4. the method for a bone coal ore deposit roasting vanadium extraction, it is characterized in that: powder ore obtains breeze; Adopt claim 2 or the 3 described preparation methods that are used for bone coal ore deposit roasting additive for extracting vanadium to make additive; The addition of pressing mass ratio 3～5% adds above-mentioned additive in breeze, mixed evenly after, add the water body ball, make the mixing ore particle; Again with the above-mentioned mixing ore particle that makes in 500～800 ℃ of roastings 2～4 hours, naturally cool to room temperature and get calcining; Calcining through acidleach, extraction, precipitation, decomposition process, makes Vanadium Pentoxide in FLAKES again.
5. the method for bone coal as claimed in claim 4 ore deposit roasting vanadium extraction is characterized in that: described calcining acid leaching process condition is: be that 3～5% sulfuric acid leached between 40～100 ℃ 3～12 hours with mass concentration, leaching the solid-liquid mass ratio is 1: 1～1: 4.
6. as the method for claim 4 or 5 described bone coal ore deposit roasting vanadium extractions, it is characterized in that: described ore must be crushed to 80～120 orders, and the particle diameter that mixes ore particle is 1.2～1.5cm.
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| CN2009100445998A CN101693947B (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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