CN110387463A - A method of vanadic anhydride is produced using vanadium ferrotianium mineral intergrowth - Google Patents
A method of vanadic anhydride is produced using vanadium ferrotianium mineral intergrowth Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C22B34/20—Obtaining niobium, tantalum or vanadium
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Abstract
The invention discloses a kind of methods using vanadium ferrotianium mineral intergrowth production vanadic anhydride, the present invention is directed to the problem of Land use systems and production process of existing iron ore, the present invention provides a kind of method for preparing vanadic anhydride using vanadium ferrotianium mineral intergrowth miberal powder, and the present invention uses vanadium ferrotianium mineral intergrowth (iron 35~57%, titanium dioxide 15~35%, vanadic anhydride 0.5~1.2%) pass through direct conversion roasting, water extraction, extraction and back extraction, precipitating, calcining, high efficiente callback vanadium therein.The method of the present invention process equipment is simple, and operation is easy, safety is, it can be achieved that sefstromite green chemical industry clean manufacturing, achieves energy-saving and emission reduction purposes.
Description
Technical field
The invention belongs to metallurgical technology fields, and in particular to a kind of side using vanadium ferrotianium mineral intergrowth production vanadic anhydride
Method.
Background technique
Vanadium resource is a kind of very valuable strategic resources, is widely used in machine-building, automobile, aerospace, iron
The fields such as road, bridge.With science and technology constantly development and progress, vanadium is had become in order to indispensable in modern industry and science and technology
Resource.
China's vanadium iron magnetite deposit distribution is extensive, rich reserves, the third position of the national iron ore of reserves and yield residence, oneself
The v-ti magnetite ore reserves verified is about 98.3 hundred million tons, is distributed mainly on Sichuan area, Chengde area, Shan Xihan
The areas such as middle area, Hubei Xiangyang area, Xingning of Guangdong Province and Shanxi Dai County.Wherein, Panzhihua Region is China's vanadium titano-magnetite
Main Metallogenic band, and one of the important producing region in similar mineral deposit in the world has been verified at large-scale, oversized mineral deposit 7, medium-sized mine
At bed 6.China's navajoite resource is compared with horn of plenty, and 25,960,000 tons of reserves (with V2O5Meter), the 3rd, the ranking world, mainly with association
Mineral products form originates in lithotype v-ti magnetite mineral deposit.Currently, mainly being wrapped for the comprehensive utilization of v-ti magnetite ore resources both at home and abroad
Include two steps, the sorting to ore and the smelting to sorted product, wherein the technique of preparing of vanadium titano-magnetite is increasingly
Maturation, and be also difficult to realize for how to make iron, vanadium, titanium resource obtain efficient utilize by subsequent smelting.
Vanadic anhydride is widely used in the industries such as metallurgy, chemical industry, is mainly used for smelting ferrovanadium.As alloy addition, account for
80% or more of vanadic anhydride total flow is followed by used as the catalyst of organic chemical industry, i.e. catalyst, accounts for about the 10% of total amount,
Elsewhere it is used as inorganic chemical, chemical reagent, enamel and magnetic material etc. and accounts for about the 10% of total amount.Therefore, it is efficient to develop a kind of energy
It is very important using the method for the mineral intergrowth of ferrotianium containing vanadium.
Summary of the invention
The purpose of the present invention is to provide a kind of methods using vanadium ferrotianium mineral intergrowth production vanadic anhydride.
The object of the present invention is achieved like this, the method packet using vanadium ferrotianium mineral intergrowth production vanadic anhydride
Roasting, leaching, extraction, back extraction and post-processing step are included, is specifically included:
A, roast: will in vanadium ferrotianium symbiosis miberal powder be added additive be uniformly mixed obtain material a, will in material a be added vanadium ferrotianium
The carbon of symbiosis powdered ore quality 30 ~ 50% is fired to obtain sintered material b；
B, it leaches: obtaining grinding material c for sintered material b is ground, 3 ~ 5 times of grinding material c mass is added in grinding material c
Water, 3 ~ 6h is leached at 80 ~ 95 DEG C of Yu Wendu, and separation of solid and liquid obtains leachate d and leached mud e；
C, it extracts: organic solvent being added in leachate d, organic extraction phase f and extraction extraction raffinate g is obtained by extraction；
D, it is stripped: Na is added in organic extraction phase f2CO3Solution is stripped to obtain rich vanadium liquid h and lean organic phase i；
E, it post-processes:
1) precipitating reagent is added in rich vanadium liquid h, adjusting pH value is 8 ~ 10, and 1.5 ~ 3h is stirred at 85 ~ 95 DEG C of temperature, is filtered, washed
Obtain vanadium intermediate products j；
2) vanadium intermediate products j is obtained into object vanadic anhydride through calcining；
3) leached mud e obtains ferrous material k and titanium dioxide enrichment material l after magnetic separation；
4) ferrous material k and titanium dioxide enrichment material l are subjected to hydraulic cyclone stirring respectively, reduction is respectively obtained after being separated by filtration
Iron powder and ilmenite concentrate.
The present invention is directed to the problem of Land use systems and production process of existing iron ore, provides a kind of utilization vanadium ferrotianium
The method that mineral intergrowth miberal powder prepares vanadic anhydride, the present invention use vanadium ferrotianium symbiosis miberal powder (iron 35~57%, titanium dioxide 15
~35%, vanadic anhydride 0.5~1.2%) by direct pyrolytic conversion reduction roasting, it leaches, extraction and back extraction, precipitating is forged
It burns, high efficiente callback vanadium therein.The above-mentioned vanadium ferrotianium symbiosis miberal powder of the present invention directlys adopt rotary kiln supplying soda, high
Temperature roasting conversion, obtained material go out to obtain soluble vanadium hydrochlorate through water logging, obtain rich vanadium liquid through extraction and back extraction, and it is heavy to be added
Shallow lake agent generates vanadium intermediate products, and calcining vanadium intermediate products produce vanadic anhydride
The beneficial effects of the present invention are:
(1) the method for the present invention sefstromite powder uses high-temperature roasting, roasting material through water logging, extraction, back extraction, precipitating, calcining,
Obtain the higher vanadic anhydride product of purity；
(2) the method for the present invention uses water logging, extraction and back extraction method, efficient can leach, extract the vanadium contained in raw material simultaneously
With iron, TiO2Equal substances and other impurities separation；
(3) the method for the present invention process equipment is simple, and operation is easy, safety is, it can be achieved that sefstromite green chemical industry clean manufacturing, reaches
To the purpose of energy-saving and emission-reduction.
Detailed description of the invention
Fig. 1 is present invention process flow diagram.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is further illustrated, but is not subject in any way to the present invention
Limitation, based on present invention teach that it is made it is any transform or replace, all belong to the scope of protection of the present invention.
Method of the present invention using vanadium ferrotianium mineral intergrowth production vanadic anhydride includes roasting, leaches, extracts, anti-
Extraction and post-processing step, specifically include:
A, roast: will in vanadium ferrotianium symbiosis miberal powder be added additive be uniformly mixed obtain material a, will in material a be added vanadium ferrotianium
The carbon of symbiosis powdered ore quality 30 ~ 50% is fired to obtain sintered material b；
B, it leaches: obtaining grinding material c for sintered material b is ground, 3 ~ 5 times of grinding material c mass is added in grinding material c
Water, 3 ~ 6h is leached at 80 ~ 95 DEG C of Yu Wendu, and separation of solid and liquid obtains leachate d and leached mud e；
C, it extracts: organic solvent being added in leachate d, organic extraction phase f and extraction extraction raffinate g is obtained by extraction；
D, it is stripped: Na is added in organic extraction phase f2CO3Solution is stripped to obtain rich vanadium liquid h and lean organic phase i；
E, it post-processes:
1) precipitating reagent is added in rich vanadium liquid h, adjusting pH value is 8 ~ 10, and 1.5 ~ 3h is stirred at 85 ~ 95 DEG C of temperature, is filtered, washed
Obtain vanadium intermediate products j；
2) vanadium intermediate products j is obtained into object vanadic anhydride through calcining；
3) leached mud e obtains ferrous material k and titanium dioxide enrichment material l after magnetic separation；
4) ferrous material k and titanium dioxide enrichment material l are subjected to hydraulic cyclone stirring respectively, reduction is respectively obtained after being separated by filtration
Iron powder and ilmenite concentrate.
The quality proportioning of the vanadium ferrotianium symbiosis miberal powder and additive is 1:(0.5 ~ 1).
The additive is sodium carbonate.
The temperature of the roasting is 750 ~ 1050 DEG C, and the time of roasting is 4 ~ 7h.
At 10 ~ 30 DEG C, milling time is 0.5 ~ 2h for the temperature control ground in step B.
Organic solvent described in step C is N235The mixed extractant constituted with sulfonated kerosene, N235Concentration 10%~30%,
Extraction phase ratio A:O=1:0.5~1.
Na in D step2CO3The concentration of solution is 0.5 ~ 1.0mol/L, extraction phase ratio A:O=0.5~1:2.
Precipitating reagent described in E step 1) is (NH4)2SO4。
The temperature of calcining described in E step 2 is 500 ~ 800 DEG C, and the time of calcining is 1 ~ 3h.
E step 4) is the hydraulic cyclone stirred tank that ferrous material k and titanium dioxide enrichment material l are respectively delivered to adjustable speed
In 1 and 2, distinguishes at room temperature first high-speed stirred 0.5~2.0 hour, then mix slowly 0.5~2.0 hour, then mixing slowly
Under the conditions of the extraction of the material of hydraulic cyclone stirred tank lower part 60% is separated by filtration, respectively obtain reduced iron powder and ilmenite concentrate；It is described
High-speed stirred revolving speed be 300 ~ 500r/min；The revolving speed mixed slowly is 100 ~ 200r/min.
Case is embodied, the present invention will be further described below:
Embodiment 1
(1) sefstromite powder, sodium carbonate 1:0.5 in mass ratio are put into Horizontal type helical ribbon mixer and are uniformly mixed, it is interior to match vanadium titanium
Then the carbon of Iron Ore Powder quality 40% is delivered to the roasting of 1 high temperature of rotary kiln by belt conveyor, controls furnace zone temperature 750
DEG C, the sintered material after being converted for the material lagging time 7 hours；
(2) sintered material that step (1) obtains is sent into ball mill, is ground 1.0 hours at normal temperature, is obtained grinding material
(3) grinding material that step (2) obtains is transferred in high-order material storage bin by belt conveyor, then by high-order object
Material storage bin is added in leaching tanks under agitation, is previously added water by liquid-solid ratio 3:1 in leaching tanks, stirs at a temperature of 80 DEG C
After mixing leaching 6 hours, it is separated by solid-liquid separation through band filter, is cooled to room temperature to obtain the leachate of the hydrochlorate containing soluble vanadium and leaching
Slag；
(4) leachate that step (3) obtains is transferred to extraction tank 1 through pipeline using liquid phase pump, is added by extraction phase ratio A:O=1:1
N235Concentration is 10% sulfonated kerosene organic extractant, and room temperature extracts 1 hour under agitation, stratification, then from extraction
Trench bottom is released water phase respectively and is mutually separated with organic phase, and the organic extraction phase and extraction extraction raffinate containing vanadium are obtained；
(5) the organic extraction phase transfer for being obtained step (4) through pipeline using liquid phase pump is into extraction tank 2, under agitation
The Na of 0.5mol/L is added by extraction phase ratio A:O=1:22CO3Solution is stripped 3 hours, stratification, from extraction trench bottom difference
It releases water phase mutually to be separated with organic phase, obtains rich vanadium liquid and lean organic phase；
(6) the rich vanadium liquid that step (5) obtains is transferred in sedimentation basin using liquid phase pump through pipeline, is added and is precipitated by liquid-solid ratio 6:1
Agent (NH4)2SO4, regulation system pH is 8,85 DEG C of temperature, is stirred to react 1.5h, is filtered, washed to obtain using membrane pressure filter
Vanadium intermediate products ammonium metavanadate；
(7) the vanadium intermediate products for obtaining step (6) are sent into rotary kiln 2 through belt conveyor, calcine 3 hours, obtain at 500 DEG C
Vanadic anhydride product；
(8) leached mud that step (3) obtains is delivered to magnetic separator through belt conveyor and carries out magnetic separation, obtains ferrous material and two
Titanium oxide enrichment material；
(9) ferrous material and titanium dioxide the enrichment material obtained step (8), is respectively delivered to the hydraulic cyclone stirring of adjustable speed
In slot 1 and 2, distinguish at room temperature first high-speed stirred 1.0 hours, then mixes slowly 2.0 hours, it then will under the conditions of mixing slowly
The material extraction of hydraulic cyclone stirred tank lower part 60% is separated by filtration, and respectively obtains reduced iron powder and ilmenite concentrate.
Through analyzing, the present embodiment vanadium overall recovery 80.75%, product vanadic anhydride V2O5Content 98.32%；Reduced iron powder
Product TFe content reaches 98.38%；Ilmenite concentrate content of titanium dioxide reaches 50.91%.
Embodiment 2
(1) sefstromite powder, sodium carbonate 1:1 in mass ratio are put into Horizontal type helical ribbon mixer and are uniformly mixed, it is interior to match vanadium ferrotianium
Then the carbon of powdered ore quality 30% is delivered to the roasting of 1 high temperature of rotary kiln by belt conveyor, controls furnace zone temperature 850
DEG C, the sintered material after being converted for the material lagging time 6 hours；
(2) sintered material that step (1) obtains is sent into ball mill, is ground 0.5 hour at normal temperature, is obtained grinding material
(3) grinding material that step (2) obtains is transferred in high-order material storage bin by belt conveyor, then by high-order object
Material storage bin is added in leaching tanks under agitation, is previously added water by liquid-solid ratio 5:1 in leaching tanks, stirs at a temperature of 85 DEG C
After mixing leaching 4 hours, it is separated by solid-liquid separation through band filter, is cooled to room temperature to obtain the leachate of the hydrochlorate containing soluble vanadium and leaching
Slag；
(4) leachate that step (3) obtains is transferred to extraction tank 1 through pipeline using liquid phase pump, adds by extraction phase ratio A:O=1:0.5
Enter N235Concentration is 30% sulfonated kerosene organic extractant, and room temperature extracts 2 hours under agitation, stratification, then from extraction
It takes trench bottom to release water phase respectively mutually to be separated with organic phase, obtains the organic extraction phase and extraction extraction raffinate containing vanadium；
(5) the organic extraction phase transfer for being obtained step (4) through pipeline using liquid phase pump is into extraction tank 2, under agitation
The Na of 1.0mol/L is added by extraction phase ratio A:O=0.5:22CO3Solution is stripped 9 hours, stratification, from extraction trench bottom point
Not Fang Chu water phase mutually separated with organic phase, obtain rich vanadium liquid and lean organic phase；
(6) the rich vanadium liquid that step (5) obtains is transferred in sedimentation basin using liquid phase pump through pipeline, is added and is precipitated by liquid-solid ratio 8:1
Agent (NH4)2SO4, regulation system pH is 10,95 DEG C of temperature, is stirred to react 1.5h, is filtered, washed to obtain using membrane pressure filter
Vanadium intermediate products ammonium metavanadate；
(7) the vanadium intermediate products for obtaining step (6) are sent into rotary kiln 2 through belt conveyor, calcine 1 hour, obtain at 800 DEG C
Vanadic anhydride product；
(8) leached mud that step (3) obtains is delivered to magnetic separator through belt conveyor and carries out magnetic separation, obtains ferrous material and two
Titanium oxide enrichment material；
(9) ferrous material and titanium dioxide the enrichment material obtained step (8), is respectively delivered to the hydraulic cyclone stirring of adjustable speed
In slot 1 and 2, distinguish at room temperature first high-speed stirred 0.5 hour, then mixes slowly 1.0 hours, it then will under the conditions of mixing slowly
The material extraction of hydraulic cyclone stirred tank lower part 60% is separated by filtration, and respectively obtains reduced iron powder and ilmenite concentrate.
Through analyzing, the present embodiment vanadium overall recovery 84.46%, product vanadic anhydride V2O5Content 98.56%；Reduced iron powder
Product TFe content reaches 98.02%；Ilmenite concentrate content of titanium dioxide reaches 50.68%.
Embodiment 3
(1) sefstromite powder, sodium carbonate 1:0.8 in mass ratio are put into Horizontal type helical ribbon mixer and are uniformly mixed, it is interior to match vanadium titanium
Then the carbon of Iron Ore Powder quality 50% is delivered to the roasting of 1 high temperature of rotary kiln by belt conveyor, controls furnace zone temperature
1050 DEG C, the sintered material after being converted for the material lagging time 4 hours；
(2) sintered material that step (1) obtains is sent into ball mill, is ground 0.75 hour at normal temperature, is obtained grinding material
(3) grinding material that step (2) obtains is transferred in high-order material storage bin by belt conveyor, then by high-order object
Material storage bin is added in leaching tanks under agitation, is previously added water by liquid-solid ratio 4:1 in leaching tanks, stirs at a temperature of 95 DEG C
After mixing leaching 3 hours, it is separated by solid-liquid separation through band filter, is cooled to room temperature to obtain the leachate of the hydrochlorate containing soluble vanadium and leaching
Slag；
(4) leachate that step (3) obtains is transferred to extraction tank 1 through pipeline using liquid phase pump, adds by extraction phase ratio A:O=1:0.6
Enter N235Concentration is 20% sulfonated kerosene organic extractant, and room temperature extracts 3 hours under agitation, stratification, then from extraction
It takes trench bottom to release water phase respectively mutually to be separated with organic phase, obtains the organic extraction phase and extraction extraction raffinate containing vanadium；
(5) the organic extraction phase transfer for being obtained step (4) through pipeline using liquid phase pump is into extraction tank 2, under agitation
The Na of 0.7mol/L is added by extraction phase ratio A:O=0.8:22CO3Solution is stripped 5 hours, stratification, from extraction trench bottom point
Not Fang Chu water phase mutually separated with organic phase, obtain rich vanadium liquid and lean organic phase；
(6) the rich vanadium liquid that step (5) obtains is transferred in sedimentation basin using liquid phase pump through pipeline, is added and is precipitated by liquid-solid ratio 7:1
Agent (NH4)2SO4, regulation system pH is 9,90 DEG C of temperature, is stirred to react 3.0h, is filtered, washed to obtain using membrane pressure filter
Vanadium intermediate products ammonium metavanadate；
(7) the vanadium intermediate products for obtaining step (6) are sent into rotary kiln 2 through belt conveyor, calcine 2 hours, obtain at 700 DEG C
Vanadic anhydride product；
(8) leached mud that step (3) obtains is delivered to magnetic separator through belt conveyor and carries out magnetic separation, obtains ferrous material and two
Titanium oxide enrichment material；
(9) ferrous material and titanium dioxide the enrichment material obtained step (8), is respectively delivered to the hydraulic cyclone stirring of adjustable speed
In slot 1 and 2, distinguish at room temperature first high-speed stirred 2.0 hours, then mixes slowly 0.5 hour, it then will under the conditions of mixing slowly
The material extraction of hydraulic cyclone stirred tank lower part 60% is separated by filtration, and respectively obtains reduced iron powder and ilmenite concentrate.
Through analyzing, the present embodiment vanadium overall recovery 85.72%, product vanadic anhydride V2O5Content 99.20%；Reduced iron powder
Product TFe content reaches 98.07%；Ilmenite concentrate content of titanium dioxide reaches 51.36%.
Embodiment 4
(1) sefstromite powder, sodium carbonate 1:0.7 in mass ratio are put into Horizontal type helical ribbon mixer and are uniformly mixed, it is interior to match vanadium titanium
Then the carbon of Iron Ore Powder quality 40% is delivered to the roasting of 1 high temperature of rotary kiln by belt conveyor, controls furnace zone temperature 950
DEG C, the sintered material after being converted for the material lagging time 5 hours；
(2) sintered material that step (1) obtains is sent into ball mill, is ground 1.0 hours at normal temperature, is obtained grinding material
(3) grinding material that step (2) obtains is transferred in high-order material storage bin by belt conveyor, then by high-order object
Material storage bin is added in leaching tanks under agitation, water is previously added by liquid-solid ratio 4.5:1 in leaching tanks, at a temperature of 90 DEG C
After stirring leaching 5 hours, it is separated by solid-liquid separation through band filter, is cooled to room temperature to obtain the leachate of the hydrochlorate containing soluble vanadium and leaching
It slags tap；
(4) leachate that step (3) obtains is transferred to extraction tank 1 through pipeline using liquid phase pump, adds by extraction phase ratio A:O=1:0.8
Enter N235Concentration be 15% sulfonated kerosene organic extractant, under agitation room temperature extract 1.5 hours, stratification, then from
Extraction trench bottom is released water phase respectively and is mutually separated with organic phase, and the organic extraction phase and extraction extraction raffinate containing vanadium are obtained；
(5) the organic extraction phase transfer for being obtained step (4) through pipeline using liquid phase pump is into extraction tank 2, under agitation
The Na of 0.9mol/L is added by extraction phase ratio A:O=0.6:22CO3Solution is stripped 7 hours, stratification, from extraction trench bottom point
Not Fang Chu water phase mutually separated with organic phase, obtain rich vanadium liquid and lean organic phase；
(6) the rich vanadium liquid that step (5) obtains is transferred in sedimentation basin using liquid phase pump through pipeline, is added and is precipitated by liquid-solid ratio 7:1
Agent (NH4)2SO4, regulation system pH is 8.5,85 DEG C of temperature, is stirred to react 2.5h, is filtered, washed using membrane pressure filter
To vanadium intermediate products ammonium metavanadate；
(7) the vanadium intermediate products for obtaining step (6) are sent into rotary kiln 2 through belt conveyor, calcine 1.5 hours, obtain at 600 DEG C
To vanadic anhydride product；
(8) leached mud that step (3) obtains is delivered to magnetic separator through belt conveyor and carries out magnetic separation, obtains ferrous material and two
Titanium oxide enrichment material；
(9) ferrous material and titanium dioxide the enrichment material obtained step (8), is respectively delivered to the hydraulic cyclone stirring of adjustable speed
In slot 1 and 2, distinguish at room temperature first high-speed stirred 1.5 hours, then mixes slowly 1.5 hours, it then will under the conditions of mixing slowly
The material extraction of hydraulic cyclone stirred tank lower part 60% is separated by filtration, and respectively obtains reduced iron powder and ilmenite concentrate.
Through analyzing, the present embodiment vanadium overall recovery 86.46%, product vanadic anhydride V2O5Content 99.50%；Reduced iron powder
Product TFe content reaches 97.94%；Ilmenite concentrate content of titanium dioxide reaches 51.82%.
Above the embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment party
Formula can also be made without departing from the purpose of the present invention within the knowledge of a person skilled in the art
Various change out.
Claims (10)
1. a kind of method using vanadium ferrotianium mineral intergrowth production vanadic anhydride, it is characterised in that described utilizes the symbiosis of vanadium ferrotianium
The method that mine produces vanadic anhydride includes roasting, leaching, extraction, back extraction and post-processing step, is specifically included:
A, roast: will in vanadium ferrotianium symbiosis miberal powder be added additive be uniformly mixed obtain material a, will in material a be added vanadium ferrotianium
The carbon of symbiosis powdered ore quality 30 ~ 50% is fired to obtain sintered material b；
B, it leaches: obtaining grinding material c for sintered material b is ground, 3 ~ 5 times of grinding material c mass is added in grinding material c
Water, 3 ~ 6h is leached at 80 ~ 95 DEG C of Yu Wendu, and separation of solid and liquid obtains leachate d and leached mud e；
C, it extracts: organic solvent being added in leachate d, organic extraction phase f and extraction extraction raffinate g is obtained by extraction；
D, it is stripped: Na is added in organic extraction phase f2CO3Solution is stripped to obtain rich vanadium liquid h and lean organic phase i；
E, it post-processes:
1) precipitating reagent is added in rich vanadium liquid h, adjusting pH value is 8 ~ 10, and 1.5 ~ 3h is stirred at 85 ~ 95 DEG C of temperature, is filtered, washed
Obtain vanadium intermediate products j；
2) vanadium intermediate products j is obtained into object vanadic anhydride through calcining；
3) leached mud e obtains ferrous material k and titanium dioxide enrichment material l after magnetic separation；
4) ferrous material k and titanium dioxide enrichment material l are subjected to hydraulic cyclone stirring respectively, reduction is respectively obtained after being separated by filtration
Iron powder and ilmenite concentrate.
2. the method according to claim 1 using vanadium ferrotianium mineral intergrowth production vanadic anhydride, it is characterised in that described
Vanadium ferrotianium symbiosis miberal powder and additive quality proportioning be 1:(0.5 ~ 1).
3. the method according to claim 1 or 2 using vanadium ferrotianium mineral intergrowth production vanadic anhydride, it is characterised in that institute
The additive stated is sodium carbonate.
4. the method according to claim 1 using vanadium ferrotianium mineral intergrowth production vanadic anhydride, it is characterised in that described
The temperature of roasting be 750 ~ 1050 DEG C, time of roasting is 4 ~ 7h.
5. the method according to claim 1 using vanadium ferrotianium mineral intergrowth production vanadic anhydride, it is characterised in that step B
At 10 ~ 30 DEG C, milling time is 0.5 ~ 2h for the temperature control of middle grinding.
6. the method according to claim 1 using vanadium ferrotianium mineral intergrowth production vanadic anhydride, it is characterised in that step C
Described in organic solvent be N235The mixed extractant constituted with sulfonated kerosene, N235Concentration 10%~30%, extraction phase ratio A:O=
1:0.5~1.
7. the method according to claim 1 using vanadium ferrotianium mineral intergrowth production vanadic anhydride, it is characterised in that D step
Middle Na2CO3The concentration of solution is 0.5 ~ 1.0mol/L, extraction phase ratio A:O=0.5~1:2.
8. the method according to claim 7 using vanadium ferrotianium mineral intergrowth production vanadic anhydride, it is characterised in that E step
1) precipitating reagent described in is (NH4)2SO4。
9. the method according to claim 1 using vanadium ferrotianium mineral intergrowth production vanadic anhydride, it is characterised in that E step
2) temperature of the calcining described in is 500 ~ 800 DEG C, and the time of calcining is 1 ~ 3h.
10. the method according to claim 1 using vanadium ferrotianium mineral intergrowth production vanadic anhydride, it is characterised in that E step
4) rapid is that ferrous material k and titanium dioxide enrichment material l are respectively delivered in the hydraulic cyclone stirred tank 1 and 2 of adjustable speed, room temperature
It is lower high-speed stirred 0.5~2.0 hour first respectively, then mix slowly 0.5~2.0 hour, then by water under the conditions of mixing slowly
The material extraction of power cyclone mixing slot lower part 60% is separated by filtration, and respectively obtains reduced iron powder and ilmenite concentrate；The high-speed stirred
Revolving speed be 300 ~ 500r/min；The revolving speed mixed slowly is 100 ~ 200r/min.
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