CN106995879A - A kind of low-grade Oxidation Leaching of sodium containing chromic vanadium-titanium ferroferrite extraction vanadium method - Google Patents
A kind of low-grade Oxidation Leaching of sodium containing chromic vanadium-titanium ferroferrite extraction vanadium method Download PDFInfo
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- CN106995879A CN106995879A CN201710215442.1A CN201710215442A CN106995879A CN 106995879 A CN106995879 A CN 106995879A CN 201710215442 A CN201710215442 A CN 201710215442A CN 106995879 A CN106995879 A CN 106995879A
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- vanadium
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- containing chromic
- titanium ferroferrite
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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
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- 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
-
- 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
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/2406—Binding; Briquetting ; Granulating pelletizing
-
- 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
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/242—Binding; Briquetting ; Granulating with binders
- C22B1/243—Binding; Briquetting ; Granulating with binders inorganic
-
- 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
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1218—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry processes
-
- 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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
Abstract
The invention belongs to the vanadium extraction technical field in the low-grade method of comprehensive utilization of powder containing chromic vanadium-titanium ferroferrite, there is provided a kind of extraction vanadium method of the low-grade sodium of powder containing chromic vanadium-titanium ferroferrite Oxidation Leaching.This method step includes batch mixing, pelletizing, roasting, leaching.The low-grade resource of powder containing chromic vanadium-titanium ferroferrite is taken full advantage of, the comprehensive utilization ratio of the low-grade resource containing chromic vanadium-titanium ferroferrite is improved;The sodium oxidation vanadium extracting technique flow is short, and whole process vanadium recovery is high, is all higher than 80%;Sodium acid pellet powder is leached using dilute sulfuric acid, can avoid, due to generating water insoluble calcium vanadate in sodium acid pellet powder in sintering process containing CaO, reducing the leaching rate of vanadium;Sodium acid pellet powder after Leaching Vanadium can contemplate coal blending and carry out direct-reduction magnetic separation process enrichment titanium and be subject to extraction and application.
Description
Technical field
The invention belongs to the vanadium extraction technical field in the low-grade method of comprehensive utilization of powder containing chromic vanadium-titanium ferroferrite, especially relate to
And the low-grade sodium of powder containing chromic vanadium-titanium ferroferrite oxidation vanadium extracting method.
Background technology
V-ti magnetite miberal powder is a kind of many metal intergrowth minerals rich in a variety of valuable constituent elements such as iron, vanadium, titaniums, application value
It is high.At present to common vanadium titano-magnetite research comparatively maturation, but the research containing chromic vanadium-titanium ferroferrite is still needed to
Further systematization, and high-grade is concentrated mainly on to the research containing chromic vanadium-titanium ferroferrite containing chromic vanadium-titanium ferroferrite, and it is right
The low-grade research containing chromic vanadium-titanium ferroferrite is still more deficient, and further development is needed in its correlative study work badly.
Recently as the fast development of China's steel industry, supply falls short of demand for domestic Iron Ore Market, low-grade to contain chromium type
V-ti magnetite ore resources are expected to be produced utilization as a kind of iron ore deposit of potentiality.In order that low-grade v-ti magnetite containing chromium type
Ore deposit is fully used, and is increased economic efficiency, people constantly explore and research and develop it is low-grade containing chromic vanadium-titanium ferroferrite except ironmaking with
Outer new technology and new technology, and low-grade powder containing chromic vanadium-titanium ferroferrite process for extracting vanadium is one of important research side
To.
At present, the yield for vanadium being extracted from vanadium titano-magnetite about account for the 90% of industrial production vanadium total output, but domestic
The method that vanadium is extracted from vanadium titano-magnetite is mainly pyrometallurgical method, this method be based on vanadium titano-magnetite raw material through smelting
The vanadium-bearing hot metal that refining is obtained blows vanadium through converter and obtains vanadium slag, then Roasting And Leaching vanadium extraction.And be expected to direct as vanadium titano-magnetite
It is perfect that sodium oxidation-wet-leaching technical study of effective vanadium extraction needs development badly.Therefore, it is low-grade containing chromium in order to preferably carry out
The research work of type v-ti magnetite miberal powder, forms the low-grade theoretical system containing chromic vanadium-titanium ferroferrite, preferably instructs low product
A kind of low-grade sodium of powder containing chromic vanadium-titanium ferroferrite oxidation vanadium extracting side has been invented containing chromic vanadium-titanium ferroferrite comprehensive utilization in position
Method.
The content of the invention
Resources characteristic for the low-grade powder containing chromic vanadium-titanium ferroferrite and its sky in terms of application field is studied in vanadium extraction
In vain, the present invention provides a kind of extraction vanadium method of the low-grade sodium of powder containing chromic vanadium-titanium ferroferrite oxidation-leaching.
The low-grade sodium of powder containing chromic vanadium-titanium ferroferrite oxidation vanadium extracting-leaching method of the present invention, comprises the following steps:
Step 1, batch mixing:
Weigh low-grade powder containing chromic vanadium-titanium ferroferrite, binding agent and additive and carry out batch mixing, mixed material is made;Its
In, additive is NaCl, Na2CO3、Na2SO4, NaOH or NaNO3In one or more, the quality of mixed material and additive
Than for 50:1~4;The mass ratio of mixed material and binding agent is 100:1~2;
Step 2, pelletizing:
(1) water is added to mixed material, 30~40min of material is boiled in a covered pot over a slow fire in stirring mixing;Wherein, the mass ratio of mixed material and water
For 100:8~11;
(2) water is added into stewing material, the low-grade pelletizing containing chromic vanadium-titanium ferroferrite that granularity is 7~12mm is made, is made
Low-grade pelletizing containing chromic vanadium-titanium ferroferrite in, the weight content of water is 9~12%;
(3) low-grade pelletizing containing chromic vanadium-titanium ferroferrite is dried;
Step 3, it is calcined:
(1) the low-grade pelletizing containing chromic vanadium-titanium ferroferrite of drying is loaded into crucible, be put into high temperature Muffle furnace;
(2) pelletizing oxidizing roasting process is:In air atmosphere, high temperature Muffle furnace be warming up to 700 with 8~12 DEG C/min~
900 DEG C, then be warming up to 4~6 DEG C/min after 1150 DEG C~1250 DEG C, 0.5~2h of insulation, cool to 700~900 DEG C with stove
When, air cooling is taken out, the low-grade sodium acid pellet containing chromic vanadium-titanium ferroferrite is obtained;
Step 4, leach:
(1) by the sodium acid pellet of cooling, crush, obtain the pelletizing powder that granularity is less than 200 mesh;
(2) sodium acid pellet powder is leached in heating water bath pot, solution used is dilute sulfuric acid in leaching process,
Bath temperature is 80~100 DEG C, and mixing speed is 200~400r/min, and dilute sulfuric acid and the sodium of pH=0.3~0.5 aoxidize ball
The mass ratio of cooking starch is 30~50:1, extraction time is 1~3h;Obtain filtrate containing vanadium and vanadium extraction mine tailing.
Further, the particle mean size of the above-mentioned low-grade powder containing chromic vanadium-titanium ferroferrite is below 200 mesh.
Further, the particle mean size of above-mentioned additive is below 200 mesh.
Further, above-mentioned binding agent is bentonite, and particle mean size accounts for more than 90% below 200 mesh.
Further, in above-mentioned steps 1, batch mixing device therefor is ball mill, and mixing time is no less than 5h.
Further, in above-mentioned steps 2 (2), pelletizing prepares device therefor for balling disk (-sc), and balling disk (-sc) rotating speed is in 17~19r/
min。
Further, in above-mentioned steps 2 (3), the low-grade drying time of pelletizing containing chromic vanadium-titanium ferroferrite is no less than 5h.
Further, in above-mentioned steps 4 (1), it is sealed type sample pulverizer to crush equipment used.
Further, the chemical composition and its percentage by weight included in above-mentioned low-grade powder containing chromic vanadium-titanium ferroferrite
For Fe3O4:40.0~42.7%, FeO:17.0~19.0%, CaO:3.0~4.0%, SiO2:6.5~7.5%, MgO:0.6~
0.8%, Al2O3:1.5~2.1%, TiO2:20.0~22.0%, V2O5:1.6~1.8%, Cr2O3:0.02~0.2%, S≤
0.05%, P≤0.01%, surplus is inevitable impurity.
The beneficial effects of the invention are as follows:The low-grade resource of powder containing chromic vanadium-titanium ferroferrite is taken full advantage of, low product are improved
The comprehensive utilization ratio of position resource containing chromic vanadium-titanium ferroferrite;The sodium oxidation vanadium extracting technique flow is short, and whole process vanadium recovery is high,
It is all higher than 80%;Sodium acid pellet powder is leached using dilute sulfuric acid, can avoid due in sodium acid pellet powder containing CaO
Water insoluble calcium vanadate is generated in sintering process, the leaching rate of vanadium is reduced;Sodium acid pellet powder after Leaching Vanadium can be with
Consider coal blending be reduced directly-magnetic separation process enrichment titanium and be subject to extraction and application.
Embodiment
The low-grade powder containing chromic vanadium-titanium ferroferrite of the embodiment of the present invention comes from Liaoning Ka Zuo somewheres.
The present invention uses the TFe of the low-grade powder containing chromic vanadium-titanium ferroferrite mass percent for 43.0~45.0%, bag
The chemical composition and its percentage by weight contained is Fe3O4:40.0~42.7%, FeO:17.0~19.0%, CaO:3.0~
4.0%, SiO2:6.5~7.5%, MgO:0.6~0.8%, Al2O3:1.5~2.1%, TiO2:20.0~22.0%, V2O5:
1.6~1.8%, Cr2O3:0.02~0.2%, S≤0.05%, P≤0.01%, surplus are inevitable impurity.
The bentonite of the embodiment of the present invention is commercial products.
Additive NaCl, the Na used in the embodiment of the present invention2CO3、Na2SO4, NaOH and NaNO3For commercial products, purity
For >=98%.
Embodiment 1
A kind of low-grade oxidation vanadium extracting of sodium containing chromic vanadium-titanium ferroferrite method, is carried out according to the following steps:
Step 1, batch mixing:
Weigh low-grade powder containing chromic vanadium-titanium ferroferrite, additive, bentonite to be put into ball mill, carry out batch mixing, batch mixing
Time is 5h, and mixed material is made;Wherein, additive Na2SO4Content is the 4% of the low-grade powder containing chromic vanadium-titanium ferroferrite, swollen
The native content of profit is the 1% of mixed material quality;
Step 2, pelletizing:
(1) to mixed material, water is added, material 30min is boiled in a covered pot over a slow fire in mixing;Wherein, in mass ratio, water is added in mixed material
Amount:Mixed material=8%;
(2) by the material boiled in a covered pot over a slow fire, it is put into the balling disk (-sc) that rotating speed is 18r/min, carries out in pelletizing, balling process, add water,
The low-grade pelletizing containing chromic vanadium-titanium ferroferrite that granularity is 8~12mm is made, wherein, obtained low-grade v-ti magnetite containing chromium type
In ore deposit pelletizing, the weight content of water is 9%;
(3) low-grade pelletizing containing chromic vanadium-titanium ferroferrite is put into baking oven 5h, dried, the pelletizing dried;
Step 3, it is calcined:
(1) pelletizing of drying is put into corundum crucible, be put into high temperature Muffle furnace;
(2) sodium acid pellet high-temperature calcination process is:In air atmosphere, high temperature Muffle furnace is with 8 DEG C/min heating
Speed is warming up to 1200 DEG C to 700 DEG C, then from 700 DEG C with 6 DEG C/min, and high-temperature roasting 60min cools to 900 DEG C with stove afterwards,
Air cooling is taken out, the sodium acid pellet of high-temperature roasting is obtained;
Step 4, leach
(1) the sodium acid pellet of cooling is put into sealed type sample pulverizer, crushed, obtain granularity less than 200 mesh
Sodium acid pellet powder;
(2) it is 90 DEG C with temperature, mixing speed is 300r/min heat collecting type heated at constant temperature water-baths to sodium acid pellet
Powder is leached, and pH=0.5 dilute sulfuric acid and sodium acid pellet powder mass ratio are 50:1, extraction time is 1h, obtains containing vanadium
Filtrate and vanadium extraction mine tailing, wherein, content of vanadium is 0.164% in vanadium extraction mine tailing, and the leaching rate of vanadium is 82.25%.
Embodiment 2
A kind of low-grade oxidation vanadium extracting of sodium containing chromic vanadium-titanium ferroferrite method, is carried out according to the following steps:
Step 1, batch mixing:
Weigh low-grade powder containing chromic vanadium-titanium ferroferrite, additive, bentonite to be put into ball mill, carry out batch mixing, batch mixing
Time is 5h, and mixed material is made;Wherein, additive Na2SO4Content is the 4% of the low-grade powder containing chromic vanadium-titanium ferroferrite, swollen
The native content of profit is the 2% of mixed material quality;
Step 2, pelletizing:
(1) to mixed material, water is added, material 40min is boiled in a covered pot over a slow fire in mixing;Wherein, in mass ratio, water is added in mixed material
Amount:Mixed material=11%;
(2) by the material boiled in a covered pot over a slow fire, it is put into the balling disk (-sc) that rotating speed is 17r/min, carries out in pelletizing, balling process, add water,
The low-grade pelletizing containing chromic vanadium-titanium ferroferrite that granularity is 7~11mm is made, wherein, obtained low-grade v-ti magnetite containing chromium type
In ore deposit pelletizing, the weight content of water is 12%;
(3) low-grade pelletizing containing chromic vanadium-titanium ferroferrite is put into baking oven 5h, dried, the pelletizing dried;
Step 3, it is calcined:
(1) pelletizing of drying is put into corundum crucible, be put into high temperature Muffle furnace;
(2) sodium acid pellet high-temperature calcination process is:In air atmosphere, high temperature Muffle furnace is with 10 DEG C/min heating
Speed is warming up to 1200 DEG C to 900 DEG C, then from 900 DEG C with 5 DEG C/min, and high-temperature roasting 60min cools to 900 DEG C with stove afterwards,
Air cooling is taken out, the sodium acid pellet of high-temperature roasting is obtained;
Step 4, leach
(1) the sodium acid pellet of cooling is put into sealed type sample pulverizer, crushed, obtain granularity less than 200 mesh
Sodium acid pellet powder;
(2) it is 90 DEG C with temperature, mixing speed is 300r/min heat collecting type heated at constant temperature water-baths to sodium acid pellet
Powder is leached, and pH=0.5 dilute sulfuric acid and sodium acid pellet powder mass ratio are 50:1, extraction time is 3h, obtains containing vanadium
Filtrate and vanadium extraction mine tailing, wherein, content of vanadium is 0.163% in vanadium extraction mine tailing, and the leaching rate of vanadium is 82.30%.
Embodiment 3
A kind of low-grade oxidation vanadium extracting of sodium containing chromic vanadium-titanium ferroferrite method, is carried out according to the following steps:
Step 1, batch mixing:
Weigh low-grade powder containing chromic vanadium-titanium ferroferrite, additive, bentonite to be put into ball mill, carry out batch mixing, batch mixing
Time is 5h, and mixed material is made;Wherein, additive Na2CO3Content is the 4% of the low-grade powder containing chromic vanadium-titanium ferroferrite, swollen
The native content of profit is the 2% of mixed material quality;
Step 2, pelletizing:
(1) to mixed material, water is added, material 40min is boiled in a covered pot over a slow fire in mixing;Wherein, in mass ratio, water is added in mixed material
Amount:Mixed material=8%;
(2) by the material boiled in a covered pot over a slow fire, it is put into the balling disk (-sc) that rotating speed is 19r/min, carries out in pelletizing, balling process, add water,
The low-grade pelletizing containing chromic vanadium-titanium ferroferrite that granularity is 7~12mm is made, wherein, obtained low-grade v-ti magnetite containing chromium type
In ore deposit pelletizing, the weight content of water is 9%;
(3) low-grade pelletizing containing chromic vanadium-titanium ferroferrite is put into baking oven 5h, dried, the pelletizing dried;
Step 3, it is calcined:
(1) pelletizing of drying is put into corundum crucible, be put into high temperature Muffle furnace;
(2) sodium acid pellet high-temperature calcination process is:In air atmosphere, high temperature Muffle furnace is with 12 DEG C/min heating
Speed is warming up to 1200 DEG C to 900 DEG C, then from 900 DEG C with 4 DEG C/min, and high-temperature roasting 60min cools to 900 DEG C with stove afterwards,
Air cooling is taken out, the sodium acid pellet of high-temperature roasting is obtained;
Step 4, leach
(1) the sodium acid pellet of cooling is put into sealed type sample pulverizer, crushed, obtain granularity less than 200 mesh
Sodium acid pellet powder;
(2) it is 80 DEG C with temperature, mixing speed is 1800r/min heat collecting type heated at constant temperature water-baths to sodium acid pellet
Powder is leached, and pH=0.5 dilute sulfuric acid and sodium acid pellet powder mass ratio are 50:1, extraction time is 3h, obtains containing vanadium
Filtrate and vanadium extraction mine tailing, wherein, content of vanadium is 0.155% in vanadium extraction mine tailing, and the leaching rate of vanadium is 83.23%.
Embodiment 4
A kind of low-grade oxidation vanadium extracting of sodium containing chromic vanadium-titanium ferroferrite method, is carried out according to the following steps:
Step 1, batch mixing:
Weigh low-grade powder containing chromic vanadium-titanium ferroferrite, additive, bentonite to be put into ball mill, carry out batch mixing, batch mixing
Time is 5h, and mixed material is made;Wherein, additive Na2CO3Content is the 4% of the low-grade powder containing chromic vanadium-titanium ferroferrite, swollen
The native content of profit is the 1% of mixed material quality;
Step 2, pelletizing:
(1) to mixed material, water is added, material 40min is boiled in a covered pot over a slow fire in mixing;Wherein, in mass ratio, water is added in mixed material
Amount:Mixed material=10%;
(2) by the material boiled in a covered pot over a slow fire, it is put into the balling disk (-sc) that rotating speed is 18r/min, carries out in pelletizing, balling process, add water,
The low-grade pelletizing containing chromic vanadium-titanium ferroferrite that granularity is 8~12mm is made, wherein, obtained low-grade v-ti magnetite containing chromium type
In ore deposit pelletizing, the weight content of water is 11%;
(3) low-grade pelletizing containing chromic vanadium-titanium ferroferrite is put into baking oven 5h, dried, the pelletizing dried;
Step 3, it is calcined:
(1) pelletizing of drying is put into corundum crucible, be put into high temperature Muffle furnace;
(2) sodium acid pellet high-temperature calcination process is:In air atmosphere, high temperature Muffle furnace is with 10 DEG C/min heating
Speed is warming up to 1200 DEG C to 900 DEG C, then from 900 DEG C with 6 DEG C/min, and high-temperature roasting 60min cools to 900 DEG C with stove afterwards,
Air cooling is taken out, the sodium acid pellet of high-temperature roasting is obtained;
Step 4, leach
(1) the sodium acid pellet of cooling is put into sealed type sample pulverizer, crushed, obtain granularity less than 200 mesh
Sodium acid pellet powder;
(2) it is 90 DEG C with temperature, mixing speed is 300r/min heat collecting type heated at constant temperature water-baths to sodium acid pellet
Powder is leached, and pH=0.5 dilute sulfuric acid and sodium acid pellet powder mass ratio are 50:1, extraction time is 1h, obtains containing vanadium
Filtrate and vanadium extraction mine tailing, wherein, content of vanadium is 0.125% in vanadium extraction mine tailing, and the leaching rate of vanadium is 86.47%.
Embodiment 5
A kind of low-grade oxidation vanadium extracting of sodium containing chromic vanadium-titanium ferroferrite method, is carried out according to the following steps:
Step 1, batch mixing:
Weigh low-grade powder containing chromic vanadium-titanium ferroferrite, additive, bentonite to be put into ball mill, carry out batch mixing, batch mixing
Time is 6h, and mixed material is made;Wherein, additive Na2SO4Content is the 4% of the low-grade powder containing chromic vanadium-titanium ferroferrite, swollen
The native content of profit is the 2% of mixed material quality;
Step 2, pelletizing:
(1) to mixed material, water is added, material 40min is boiled in a covered pot over a slow fire in mixing;Wherein, in mass ratio, water is added in mixed material
Amount:Mixed material=8%;
(2) by the material boiled in a covered pot over a slow fire, it is put into the balling disk (-sc) that rotating speed is 17r/min, carries out in pelletizing, balling process, add water,
The low-grade pelletizing containing chromic vanadium-titanium ferroferrite that granularity is 8~12mm is made, wherein, obtained low-grade v-ti magnetite containing chromium type
In ore deposit pelletizing, the weight content of water is 9%;
(3) low-grade pelletizing containing chromic vanadium-titanium ferroferrite is put into baking oven 5h, dried, the pelletizing dried;
Step 3, it is calcined:
(1) pelletizing of drying is put into corundum crucible, be put into high temperature Muffle furnace;
(2) sodium acid pellet high-temperature calcination process is:In air atmosphere, high temperature Muffle furnace is with 10 DEG C/min heating
Speed is warming up to 1200 DEG C to 900 DEG C, then from 900 DEG C with 5 DEG C/min, and high-temperature roasting 60min cools to 700 DEG C with stove afterwards,
Air cooling is taken out, the sodium acid pellet of high-temperature roasting is obtained;
Step 4, leach
(1) the sodium acid pellet of cooling is put into sealed type sample pulverizer, crushed, obtain granularity less than 200 mesh
Sodium acid pellet powder;
(2) it is 90 DEG C with temperature, mixing speed is 300r/min heat collecting type heated at constant temperature water-baths to sodium acid pellet
Powder is leached, and pH=0.3 dilute sulfuric acid and sodium acid pellet powder mass ratio are 50:1, extraction time is 1h, obtains containing vanadium
Filtrate and vanadium extraction mine tailing, wherein, content of vanadium is 0.103% in vanadium extraction mine tailing, and the leaching rate of vanadium is 88.85%.
Embodiment 6
A kind of low-grade oxidation vanadium extracting of sodium containing chromic vanadium-titanium ferroferrite method, is carried out according to the following steps:
Step 1, batch mixing:
Weigh low-grade powder containing chromic vanadium-titanium ferroferrite, additive, bentonite to be put into ball mill, carry out batch mixing, batch mixing
Time is 7h, and mixed material is made;Wherein, additive Na2CO3Content is the low-grade amount of silty containing chromic vanadium-titanium ferroferrite
4%, bentonite content is the 2% of mixed material quality;
Step 2, pelletizing:
(1) to mixed material, water is added, material 40min is boiled in a covered pot over a slow fire in mixing;Wherein, in mass ratio, water is added in mixed material
Amount:Mixed material=8%;
(2) by the material boiled in a covered pot over a slow fire, it is put into the balling disk (-sc) that rotating speed is 17r/min, carries out in pelletizing, balling process, add water,
The low-grade pelletizing containing chromic vanadium-titanium ferroferrite that granularity is 8~12mm is made, wherein, obtained low-grade v-ti magnetite containing chromium type
In ore deposit pelletizing, the weight content of water is 9%;
(3) low-grade pelletizing containing chromic vanadium-titanium ferroferrite is put into baking oven 5h, dried, the pelletizing dried;
Step 3, it is calcined:
(1) pelletizing of drying is put into corundum crucible, be put into high temperature Muffle furnace;
(2) sodium acid pellet high-temperature calcination process is:In air atmosphere, high temperature Muffle furnace is with 10 DEG C/min heating
Speed is warming up to 1200 DEG C to 900 DEG C, then from 900 DEG C with 5 DEG C/min, and high-temperature roasting 60min cools to 900 DEG C with stove afterwards,
Air cooling is taken out, the sodium acid pellet of high-temperature roasting is obtained;
Step 4, leach
(1) the sodium acid pellet of cooling is put into sealed type sample pulverizer, crushed, obtain granularity less than 200 mesh
Sodium acid pellet powder;
(2) it is 90 DEG C with temperature, mixing speed is 300r/min heat collecting type heated at constant temperature water-baths to sodium acid pellet
Powder is leached, and pH=0.3 dilute sulfuric acid and sodium acid pellet powder mass ratio are 50:1, extraction time is 1h, obtains containing vanadium
Filtrate and vanadium extraction mine tailing, wherein, content of vanadium is 0.063% in vanadium extraction mine tailing, and the leaching rate of vanadium is 93.28%.
Claims (10)
1. a kind of low-grade sodium containing chromic vanadium-titanium ferroferrite aoxidizes-leach extraction vanadium method, it is characterised in that including walking as follows
Suddenly:
Step 1, batch mixing:
Weigh low-grade powder containing chromic vanadium-titanium ferroferrite, binding agent and additive and carry out batch mixing, mixed material is made;Wherein, add
Plus agent is NaCl, Na2CO3、Na2SO4, NaOH or NaNO3In one or more, the mass ratio of mixed material and additive is
50:1~4;The mass ratio of mixed material and binding agent is 100:1~2;
Step 2, pelletizing:
(1) water is added to mixed material, 30~40min of material is boiled in a covered pot over a slow fire in stirring mixing;Wherein, the mass ratio of mixed material and water is
100:8~11;
(2) water is added into stewing material, the low-grade pelletizing containing chromic vanadium-titanium ferroferrite that granularity is 7~12mm is made, it is obtained low
In grade pelletizing containing chromic vanadium-titanium ferroferrite, the weight content of water is 9~12%;
(3) low-grade pelletizing containing chromic vanadium-titanium ferroferrite is dried;
Step 3, it is calcined:
(1) the low-grade pelletizing containing chromic vanadium-titanium ferroferrite of drying is loaded into crucible, be put into high temperature Muffle furnace;
(2) pelletizing oxidizing roasting process is:In air atmosphere, high temperature Muffle furnace is warming up to 700~900 with 8~12 DEG C/min
DEG C, then be warming up to 4~6 DEG C/min after 1150 DEG C~1250 DEG C, 0.5~2h of insulation, when cooling to 700~900 DEG C with stove, take
Go out air cooling, obtain the low-grade sodium acid pellet containing chromic vanadium-titanium ferroferrite;
Step 4, leach:
(1) by the sodium acid pellet of cooling, crush, obtain the pelletizing powder that granularity is less than 200 mesh;
(2) sodium acid pellet powder is leached in heating water bath pot, solution used is dilute sulfuric acid, water-bath in leaching process
Temperature is 80~100 DEG C, and mixing speed is 200~400r/min, dilute sulfuric acid and the sodium acid pellet powder of pH=0.3~0.5
Mass ratio be 30~50:1, extraction time is 1~3h;Obtain filtrate containing vanadium and vanadium extraction mine tailing.
2. the low-grade sodium containing chromic vanadium-titanium ferroferrite of one kind according to claim 1 aoxidizes-extraction vanadium method is leached, it is special
Levy and be, the particle mean size of the low-grade powder containing chromic vanadium-titanium ferroferrite is below 200 mesh.
3. the low-grade sodium containing chromic vanadium-titanium ferroferrite of one kind according to claim 1 or 2 aoxidizes-extraction vanadium method is leached,
Characterized in that, the particle mean size of the additive is below 200 mesh.
4. the low-grade sodium containing chromic vanadium-titanium ferroferrite of one kind according to claim 1 or 2 aoxidizes-extraction vanadium method is leached,
Characterized in that, described binding agent is bentonite, particle mean size accounts for more than 90% below 200 mesh.
5. the low-grade sodium containing chromic vanadium-titanium ferroferrite of one kind according to claim 3 aoxidizes-extraction vanadium method is leached, it is special
Levy and be, described binding agent is bentonite, and particle mean size accounts for more than 90% below 200 mesh.
6. a kind of low-grade sodium containing chromic vanadium-titanium ferroferrite according to claim 1 or 2 or 5 aoxidizes-leach vanadium extraction side
Method, it is characterised in that in step 1, batch mixing device therefor is ball mill, and mixing time is no less than 5h.
7. a kind of low-grade sodium containing chromic vanadium-titanium ferroferrite according to claim 1 or 2 or 5 aoxidizes-leach vanadium extraction side
Method, it is characterised in that in the step 2 (2), pelletizing prepares device therefor for balling disk (-sc), and balling disk (-sc) rotating speed is in 17~19r/
min。
8. a kind of low-grade sodium containing chromic vanadium-titanium ferroferrite according to claim 1 or 2 or 5 aoxidizes-leach vanadium extraction side
Method, it is characterised in that in the step 2 (3), the low-grade drying time of pelletizing containing chromic vanadium-titanium ferroferrite is no less than 5h.
9. a kind of low-grade sodium containing chromic vanadium-titanium ferroferrite according to claim 1 or 2 or 5 aoxidizes-leach vanadium extraction side
Method, it is characterised in that the chemical composition and its percentage by weight that described low-grade powder containing chromic vanadium-titanium ferroferrite is included be
Fe3O4:40.0~42.7%, FeO:17.0~19.0%, CaO:3.0~4.0%, SiO2:6.5~7.5%, MgO:0.6~
0.8%, Al2O3:1.5~2.1%, TiO2:20.0~22.0%, V2O5:1.6~1.8%, Cr2O3:0.02~0.2%, S≤
0.05%, P≤0.01%, surplus is inevitable impurity.
10. a kind of low-grade sodium containing chromic vanadium-titanium ferroferrite according to claim 1 or 2 or 5 aoxidizes-leach vanadium extraction side
Method, it is characterised in that comprise the following steps:
Step 1, batch mixing:
Weigh low-grade powder containing chromic vanadium-titanium ferroferrite, additive, bentonite to be put into ball mill, carry out batch mixing, mixing time
For 5h, mixed material is made;Wherein, additive Na2CO3Content is the 4% of the low-grade amount of silty containing chromic vanadium-titanium ferroferrite, swollen
The native content of profit is the 2% of mixed material quality;
Step 2, pelletizing:
(1) water mixing is added to mixed material, boils in a covered pot over a slow fire material 40min;The amount of water is added in mixed material:Mixed material=8%;
(2) by the material boiled in a covered pot over a slow fire, it is put into the balling disk (-sc) that rotating speed is 17r/min, carries out in pelletizing, balling process, add water, be made
Granularity is 8~12mm low-grade pelletizing containing chromic vanadium-titanium ferroferrite, wherein, obtained low-grade ball containing chromic vanadium-titanium ferroferrite
In group, the weight content of water is 9%;
(3) low-grade pelletizing containing chromic vanadium-titanium ferroferrite is put into baking oven 5h, the pelletizing dried;
Step 3, it is calcined:
(1) pelletizing of drying is put into corundum crucible, be put into high temperature Muffle furnace;
(2) sodium acid pellet high-temperature calcination process is:In air atmosphere, high temperature Muffle furnace is with 10 DEG C/min programming rate
1200 DEG C are warming up to 900 DEG C, then from 900 DEG C with 5 DEG C/min, high-temperature roasting 60min cools to 900 DEG C, taking-up with stove afterwards
Air cooling, obtains the sodium acid pellet of high-temperature roasting;
Step 4, leach
(1) the sodium acid pellet of cooling is put into sealed type sample pulverizer, crushed, obtain the sodium that granularity is less than 200 mesh
Change acid pellet powder;
(2) it is 90 DEG C with temperature, mixing speed leaches for 300r/min water-bath to sodium acid pellet powder, pH=
0.3 dilute sulfuric acid is 50 with sodium acid pellet powder mass ratio:1, extraction time is 1h, obtains filtrate containing vanadium and vanadium extraction mine tailing.
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