CN109852820A - A method of producing vanadic anhydride - Google Patents
A method of producing vanadic anhydride Download PDFInfo
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- CN109852820A CN109852820A CN201910132960.6A CN201910132960A CN109852820A CN 109852820 A CN109852820 A CN 109852820A CN 201910132960 A CN201910132960 A CN 201910132960A CN 109852820 A CN109852820 A CN 109852820A
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Abstract
The invention discloses a kind of production technologies of even phase method production vanadic anhydride, it is using bone coal or containing vanadium slag as raw material, using catalyst A as auxiliary material, miberal powder is activated by ball milling kinetic energy, under mildly acidic conditions, using duct type super high pressure reactor as core process equipment, under the conditions of the reaction pressure of 1-6, it activates miberal powder and catalyst A acts synergistically, complete to leach.The technique does not need to roast, and generates without poison gas, and clean and environmental protection, stone containing navajoite, slag resolution ratio are up to 90-95%, and whole direct yield is more than 82%, and process flow is short, and even phase precipitation agent B, hydrogen peroxide is added, under the action of precipitation agent B in reaction post mother liquor.Hydrogen peroxide quantitatively discharges oxygen, trivalent vanadium ion in solution is quantitatively oxidized to 5 valence vanadium ions, forms the quantitative even phase precipitating of vanadic acid, the purity of primary sedimentation product is that can reach the requirement of metallurgical grade vanadic anhydride, thus production cost is extremely low, and social efficiency, business efficiency are obvious.
Description
Technical field
The invention belongs to vanadium field of metallurgy, in particular to from Rock coal containing alum, containing the side for producing vanadic anhydride in vanadium slag
Method.
Background technique
Vanadic anhydride is most important barium oxide, and industrial dosage is maximum.It is also important metallurgy and chemical industry is former
One of material can make alloy quality fine and close for manufacturing vanadium steel and other nonferrous alloy, toughness, elasticity, intensity, wearability and resist
Impact improves, thus is widely used in national defence, aviation, aerospace, atomic industry department.Vanadic anhydride is removed to be closed for producing
It is golden outer also and other vfanadium compound be mainly used for glass and ceramic industry colorant, sulfuric acid and petrochemical industry production catalysis
In terms of agent, it is not only inexpensive, active big and is not easy to be poisoned.So how safety, low cost, environmental protection, produce five oxygen on a large scale
Change two vanadium into urgent problem to be solved.
Currently, Rock coal containing alum, containing vanadium slag produce vanadic anhydride, 90% or more all be using plus sodium chloride, sodium carbonate or
Trivalent vanadium in bone coal, slag, is converted to the sodium salt or calcium salt of vanadium by the method for lime-roasting, then is transferred to sour water extraction molten
Liquid precipitates production sodium metavanadate with ammonia salt after removal of impurities and roasts de- ammonium, obtains vanadic anhydride.The whole process of the traditional processing technology is straight
Yield only has 40-50%, and roasting process product per ton need to consume 25 tons or so of sodium salt or calcium salt, generate in roasting a large amount of
Sulfur dioxide, chlorine, hydrogen chloride, carbon dioxide toxic gas, discharge largely contain ammonia, the production waste water containing heavy metal, seriously
Surrounding enviroment are polluted, the ecological balance is destroyed, waste valuable strategic resource, and production process is complicated, leads to higher cost, because
This, the method for finding a kind of production vanadic anhydride of simple controllable environmental protection is necessary.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide a kind of side for producing vanadic anhydride
Method, production method provided by the invention is simple to operation, at low cost, environmental protection and energy saving, is suitble to large-scale production.
The present invention provides a kind of method for producing vanadic anhydride, comprising the following steps:
A) add water for ball milling to crush slurrying in bone coal navajoite stone to obtain miberal powder slurry, catalyst A mixing is added, is then pumped into autoclave
Acid adding pressurization carries out Leach reaction, obtains through being separated by solid-liquid separation containing vanadium mother liquid after reaction；
B it) is put into described in centrifugation decleaning tank containing vanadium mother liquid, cleaner is added, be 1-3 come purification and impurity removal with liquid alkaline tune pH value,
Removal of impurities mother liquor is obtained by filtration；
C) even phase precipitation agent B will be added in the removal of impurities mother liquor, is reacted after mixing, it is molten that the precipitation of dioxygen water management is added dropwise
Liquid current potential is separated by solid-liquid separation obtains filter cake after reaction in 482-500mv, obtains vanadic anhydride after dry.
Preferably, the step A) in, the content of the vanadium from stone coal vanadium is 0.9-1.9%.
Preferably, the step A) in, the dosage of the catalyst A is the 1-5% of bone coal navajoite stone quality, the miberal powder
The solid content of slurry is 700-900g/L, powder particle diameter < 0.074mm.
Preferably, the step A) in, the miberal powder slurry will also enter in transfer pond after moisturizing, and it is equal that catalyst A is just added
Even mixing, the acid adding are the concentrated sulfuric acid for being added 98%, and the pH value of control miberal powder slurry is 5-6；Bone coal navajoite and moisturizing, the concentrated sulfuric acid
Mass ratio be 1:1:0.2-0.3.
Preferably, the step A) in, described be pressurised into is warming up to pressure up to 1-6MPa in kettle.
Preferably, the step A) in, the time of the Leach reaction is uniform stirring 6-8h, and control reaction kettle revolving speed is
100-200 turns/min.
Preferably, the step B) in, the revolving speed control of the centrifugation decleaning tank turns/min in 40-100.
Preferably, the step B) in, the dosage that cleaner is added is 2-3 times of phosphorus content in mother liquor, when removal of impurities
Between be 4-8h.
Preferably, the step C) in, the dosage of the even phase precipitation agent B is containing containing vanadic anhydride in removal of impurities mother liquor
The 20-120% of amount, the concentration of the hydrogen peroxide of dropwise addition are 20-50%.
Preferably, the step C) in, the reaction is arrest reaction, and temperature maintains 90 DEG C or more, time 8-12h.
Beneficial effects of the present invention: (1) compared with prior art, the present invention passes through ball milling using bone coal navajoite stone as raw material
Miberal powder slurry is starched to obtain in crushing, using catalyst A as auxiliary material, under mildly acidic conditions, using autoclave as core process equipment, in 1-
Under the reaction pressure of 6MP, miberal powder slurry with catalyst A synergistic effect complete leach, after filtering into mother liquor be added cleaner dephosphorization,
Silicon obtains that even phase precipitation agent B and hydrogen peroxide is added containing vanadium mother liquid after filtering, and under the action of precipitation agent B, hydrogen peroxide quantitatively discharges
Oxygen, the trivalent vanadium ion in solution are quantitatively oxidized to 5 valence vanadium ions, form the quantitative even phase precipitating of vanadic acid, primary sedimentation product it is pure
Degree can reach the requirement for controlling golden grade vanadic anhydride.The present invention does not need to roast during production method, does not have poison gas
It generates, clean and environmental protection is energy saving, and entire process flow is shortened, and cost reduces, and bone coal navajoite stone resolution ratio is up to 90-
95%, whole direct yield is more than 82%, improves the comprehensive utilization ratio of bone coal navajoite, and whole process is simple to operation, without " three wastes "
It generates, is not necessarily to special installation, cost of investment is few (being 2/3rds of prior art technology), is suitble to large-scale production；
(2) cleaner in the present invention is under conditions of pH value is equal to 1, and selectivity preferably, only precipitates phosphorus and silicon, other metals at
Divide and do not absorb, and deposition efficiency highest, the loss late of vanadium is also below 3%；
(3) the even phase precipitation agent B that this method is used in precipitation process has specificity, precipitates vanadium under strong acid environment, other gold
Category does not precipitate, and the pentoxide content being precipitated out reaches 90%-95%, and the purity of primary sedimentation product can reach metallurgical grade
The requirement of vanadic anhydride, greatly reduces cost, hence it is evident that improves business efficiency；
(4) this method is discharged in entire technique without waste water,waste gas and industrial residue, without roasting in production process, so without exhaust gas
It generates, is filtered after Leach reaction in step A), brick field is supplied after filtered filter residue backwash and produces construction material, waste residue obtains
It makes full use of, is filtered after reaction in step C), it is 7 that filtered solution lime, which is neutralized to pH, solution after filtering again
It is recovered to ball milling workshop after ion exchange resin desorption, carries out leaching recycling.The present invention is in entire production process
Middle nothing " three wastes ", production cost is low, equipment investment is few, the rate of recovery of vanadium is high, is suitble to one of large-scale production really environmental protection
The method of vanadic anhydride is produced in the slave bone coal navajoite of energy-saving low-carbon.
Reaction principle of the invention: present invention process method is to pass through ball milling as raw material using Rock coal containing alum or containing vanadium slag
Kinetic energy activation miberal powder under mildly acidic conditions, is set using catalyst A as auxiliary material using duct type super high pressure reactor as core process
Standby, under high pressure, activation miberal powder and catalyst A act synergistically, and complete to leach under the reducing conditions, will be in bone coal navajoite
Trivalent vanadium generation vanadic anhydride soluble in water, then the vanadic sulfate generated under mildly acidic conditions with sulfuric acid are more soluble in water,
It obtains after filtering containing vanadium mother liquid, to containing being added even phase precipitation agent B, hydrogen peroxide in vanadium mother liquid, hydrogen peroxide quantitatively discharges oxygen, in solution
Trivalent vanadium ion be quantitatively oxidized to 5 valence vanadium ions, the formed network of pentavalent vanadium ion under the action of precipitation agent B, in solution
Precipitating is closed, obtains vanadic anhydride for being separated by solid-liquid separation after all vanadium ions precipitating.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of method for producing vanadic anhydride, comprising the following steps:
A) add water for ball milling to crush slurrying in bone coal navajoite stone to obtain miberal powder slurry, catalyst A mixing is added, is then pumped into autoclave
Acid adding pressurization carries out Leach reaction, obtains through being separated by solid-liquid separation containing vanadium mother liquid after reaction；
B it) is put into described in centrifugation decleaning tank containing vanadium mother liquid, cleaner is added, be 1-3 come purification and impurity removal with liquid alkaline tune pH value,
Removal of impurities mother liquor is obtained by filtration；
C) even phase precipitation agent B will be added in the removal of impurities mother liquor, is reacted after mixing, it is molten that the precipitation of dioxygen water management is added dropwise
Liquid current potential is separated by solid-liquid separation obtains filter cake after reaction in 482-500mv, obtains vanadic anhydride after dry.
Production process provided by the invention is simple to operation, and environmental protection and energy saving are at low cost；Five oxidations produced through the invention
Two vanadium purity is high, can be directly used for metallurgy industry.
Bone coal navajoite is put into water mill ball mill by the embodiment of the present invention is ground into miberal powder slurry, into after the moisturizing of transfer pond,
It acts synergistically with catalyst A, it is by carrying out Leach reaction in a high pressure reaction kettle, the trivalent vanadium in bone coal navajoite is soluble in water
Vanadic anhydride is generated, then the vanadic sulfate generated under mildly acidic conditions with sulfuric acid is more soluble in water, is obtained after filtering containing vanadium
Mother liquor supplies brick field and produces construction material after filtered filter residue backwash.
In the present invention, above-mentioned bone coal navajoite is put into water mill ball mill is ground into miberal powder slurry, into the moisturizing of transfer pond
Afterwards, it acts synergistically with catalyst A, by carrying out Leach reaction in a high pressure reaction kettle, the acid adding in reaction kettle is to be added
The mass ratio of 98% concentrated sulfuric acid, bone coal navajoite and moisturizing, the concentrated sulfuric acid is 1:1:0.2-0.3, preferably bone coal navajoite and benefit
Water, the concentrated sulfuric acid mass ratio be 1:1:0.27；The pressure that is warming up in reaction kettle reaches 1-6MPa, preferably 1-4 MPa,
More preferably 1 MPa.In a preferred embodiment of the invention, the time of Leach reaction is uniform stirring 8h, and control reaction kettle turns
Speed is 100 turns/min.
It obtains containing after vanadium mother liquid, the embodiment of the present invention cools down by the way of natural cooling, is added in centrifugation decleaning tank
Cleaner is 1-3 come purification and impurity removal with liquid alkaline tune pH value, and removal of impurities mother liquor is obtained by filtration.
In embodiments of the present invention, the revolving speed control of the centrifugation decleaning tank turns/min, preferably 60-80 in 40-100
Turn/min, more preferably 65 turns/min；Above-mentioned with liquid alkaline tune pH value is 1-3, and preferably tune pH value is 1；The addition cleaner
Dosage be 2-3 times of phosphorus content in mother liquor, except miscellaneous time is 4-8h, the dosage of preferably addition cleaner contains for phosphorus in mother liquor
2 times of amount, except miscellaneous time is 4h.
After obtaining removal of impurities mother liquor, even phase precipitation agent B is added, forms complex-precipitation with the pentavalent vanadium ion in solution, is added dropwise
Three tetravalent vanadium ions in solution are oxidized to the vanadium ion of pentavalent by hydrogen peroxide, and all vanadium ions are precipitated to form vanadic anhydride
It is separated by solid-liquid separation afterwards and obtains filter cake, obtain vanadic anhydride after dry.
In embodiments of the present invention, the dosage of the even phase precipitation agent B is the content containing vanadic anhydride in removal of impurities mother liquor
20-120%, the concentration of the hydrogen peroxide of dropwise addition is 20-50%, and the dosage of preferably even phase precipitation agent B is to contain five in removal of impurities mother liquor
The 40-100% of the content of V 2 O, the concentration of the hydrogen peroxide of dropwise addition are 30-40%.
Reaction of the embodiment of the present invention terminates after being separated by solid-liquid separation, it is preferred to use converter drying machine dry cake obtains five oxidations two
Vanadium, it is 7 that filtrate lime, which is neutralized to pH, and solution is recovered to ball milling workshop after ion exchange resin desorption after filtering, carries out
It leaches and recycles, all filterings or separation of solid and liquid are all operated using chamber-type press filter in the present embodiment.
Miberal powder slurry is obtained, cooperates with work with catalyst A in conclusion bone coal navajoite stone is added water for ball milling to crush slurrying by the present invention
With, carry out Leach reaction in a high pressure reaction kettle, be obtained by filtration containing vanadium mother liquid, then centrifugation decleaning tank in be added cleaner remove
It is miscellaneous that removal of impurities mother liquor is obtained by filtration, then the vanadium ion complexing in solution is generated into precipitating with even phase precipitation agent B, the hydrogen peroxide of addition will
The vanadium ion of trivalent and tetravalence is oxidized to the vanadium ion of pentavalent, and last filtration drying obtains vanadic anhydride.The oxidation of gained five two
Vanadium purity is high, is used directly for metallurgy industry.Entire method does not need to roast, and environmental protection and energy saving, process is simple to operation, obtains
Large-scale industrial production may be implemented in good product quality.
Catalyst A is sodium chlorate in embodiments of the present invention, and even phase precipitation agent B is potassium hydroxide, and cleaner is zirconium oxide.
For a further understanding of the application, below with reference to embodiment and table 1, table 2 to five oxidation of production provided by the present application
The method of two vanadium is specifically described.
Embodiment 1:
Water for ball milling is added to crush 1 ton of bone coal navajoite that grade containing vanadium is 1.21%, powder particle diameter < 0.074mm, the solid of miberal powder slurry
Content is 700g/L, and into the water for mending 1000L in transfer pond, 50 kg catalyst A of investment after mixing, are pumped into reaction under high pressure
In kettle, stirring is started, controls 100 revs/min of revolving speed, the concentrated sulfuric acid that 150L98% is added is warming up to pressure in axe and reaches 1MPa, uniformly
Stirring 8 hours is brown ore pulp in agitator tank, ore pulp is put into chamber-type press filter after natural cooling, through filters pressing solid-liquid at this time
Separating, washing, filter residue are that vanadium content is that 0.07% slag is baked bricks as brick field auxiliary material, and mother liquor enters centrifugation decleaning tank, start stirring,
Revolving speed is controlled at 65 revs/min, 33 kilograms of cleaner is added, with liquid alkaline tune PH to 1 purification and impurity removal 4 hours, filtration washing, after purification
Mother liquor is added even B3 kilograms of agent of phase precipitation, and 20% hydrogen peroxide 100L is added dropwise, and controls precipitation current potential 485mv, static 8h after mixing, temperature
Degree maintains 90 DEG C or more, filters to obtain vanadic anhydride filter cake, obtains 11.23 kilograms of vanadic anhydride after being dried with converter drying machine.
Using conventional vanadium detection method (such as ferrous ammonium sulfate titration) and silicon, phosphorus detection method analysis vanadium, silicon, phosphorus each
The content in a stage analyzes result referring to Tables 1 and 2.
Embodiment 2:
Water for ball milling is added to crush 1 ton of bone coal navajoite that grade containing vanadium is 1.81%, powder particle diameter < 0.074mm, the solid of miberal powder slurry
Content is 800g/L, and into the water for mending 1000L in transfer pond, 50 kg catalyst A of investment after mixing, are pumped into reaction under high pressure
In kettle, stirring is started, controls 100 revs/min of revolving speed, the concentrated sulfuric acid that 150L98% is added is warming up to pressure in axe and reaches 1MPa, uniformly
Stirring 8 hours is brown ore pulp in agitator tank, ore pulp is put into chamber-type press filter after natural cooling, through filters pressing solid-liquid at this time
Separating, washing, filter residue are that vanadium content is that 0.1% slag is baked bricks as brick field auxiliary material, and mother liquor enters centrifugation decleaning tank, start stirring,
Revolving speed is controlled at 65 revs/min, 33 kilograms of cleaner is added, with liquid alkaline tune PH to 1 purification and impurity removal 4 hours, filtration washing, after purification
Mother liquor is added even B3 kilograms of agent of phase precipitation, and 30% hydrogen peroxide 100L is added dropwise, and controls precipitation current potential 482mv, static 8h, mistake after mixing
Vanadic anhydride filter cake is filtered to obtain, obtains 17.5 kilograms of vanadic anhydride after being dried with converter drying machine.Using conventional vanadium detection side
The content of method and silicon, phosphorus detection method analysis vanadium, silicon, phosphorus in each stage, analyzes result referring to Tables 1 and 2.
Embodiment 3:
Water for ball milling is added to crush 1 ton of bone coal navajoite that grade containing vanadium is 0.97%, powder particle diameter < 0.074mm, the solid of miberal powder slurry
Content is 900g/L, and into the water for mending 1000L in transfer pond, 40 kg catalyst A of investment after mixing, are pumped into reaction under high pressure
In kettle, stirring is started, controls 200 revs/min of revolving speed, the concentrated sulfuric acid that 109L98% is added is warming up to pressure in axe and reaches 2MPa, uniformly
Stirring 6 hours is brown ore pulp in agitator tank, ore pulp is put into chamber-type press filter after natural cooling, through filters pressing solid-liquid at this time
Separating, washing, filter residue are that vanadium content is that 0.08% slag is baked bricks as brick field auxiliary material, and mother liquor enters centrifugation decleaning tank, start stirring,
Revolving speed is controlled at 40 revs/min, 35 kilograms of cleaner is added, with liquid alkaline tune PH to 2 purification and impurity removal 6 hours, filtration washing, after purification
Mother liquor is added even B5 kilograms of agent of phase precipitation, and 50% hydrogen peroxide 100L is added dropwise, and controls precipitation current potential 500mv, static 10h, mistake after mixing
Vanadic anhydride filter cake is filtered to obtain, obtains 8.74 kilograms of vanadic anhydride after being dried with converter drying machine.Using conventional vanadium detection side
The content of method and silicon, phosphorus detection method analysis vanadium, silicon, phosphorus in each stage, analyzes result referring to Tables 1 and 2.
Embodiment 4:
Water for ball milling is added to crush 1 ton of bone coal navajoite that grade containing vanadium is 1.35%, powder particle diameter < 0.074mm, the solid of miberal powder slurry
Content is 850g/L, and into the water for mending 1000L in transfer pond, 25 kg catalyst A of investment after mixing, are pumped into reaction under high pressure
In kettle, stirring is started, controls 150 revs/min of revolving speed, the concentrated sulfuric acid that 163L98% is added is warming up to pressure in axe and reaches 6MPa, uniformly
Stirring 7 hours is brown ore pulp in agitator tank, ore pulp is put into chamber-type press filter after natural cooling, through filters pressing solid-liquid at this time
Separating, washing, filter residue are that vanadium content is that 0.09% slag is baked bricks as brick field auxiliary material, and mother liquor enters centrifugation decleaning tank, start stirring,
Revolving speed is controlled at 100 revs/min, is added 40 kilograms of cleaner, with liquid alkaline tune PH to 3 purification and impurity removal 8 hours, filtration washing, purification
Post mother liquor is added even B6 kilograms of agent of phase precipitation, and 20% hydrogen peroxide 100L is added dropwise, and controls precipitation current potential 490mv, static 12h after mixing,
Vanadic anhydride filter cake is filtered to obtain, obtains 12.41 kilograms of vanadic anhydride after being dried with converter drying machine.It is detected using conventional vanadium
The content of method and silicon, phosphorus detection method analysis vanadium, silicon, phosphorus in each stage, analyzes result referring to Tables 1 and 2.
Embodiment 5:
Water for ball milling is added to crush 1 ton of bone coal navajoite that grade containing vanadium is 1.5%, powder particle diameter < 0.074mm, the solid of miberal powder slurry
Content is 800g/L, and into the water for mending 1000L in transfer pond, 50 kg catalyst A of investment after mixing, are pumped into reaction under high pressure
In kettle, stirring is started, controls 100 revs/min of revolving speed, the concentrated sulfuric acid that 150L98% is added is warming up to pressure in axe and reaches 1MPa, uniformly
Stirring 8 hours is brown ore pulp in agitator tank, ore pulp is put into chamber-type press filter after natural cooling, through filters pressing solid-liquid at this time
Separating, washing, filter residue are that vanadium content is that 0.07% slag is baked bricks as brick field auxiliary material, and mother liquor enters centrifugation decleaning tank, start stirring,
Revolving speed is controlled at 70 revs/min, 33 kilograms of cleaner is added, with liquid alkaline tune PH to 1 purification and impurity removal 4 hours, filtration washing, after purification
Mother liquor is added even B3 kilograms of agent of phase precipitation, and 35% hydrogen peroxide 100L is added dropwise, and controls precipitation current potential 495mv, static 8h, mistake after mixing
Vanadic anhydride filter cake is filtered to obtain, obtains 13.86 kilograms of vanadic anhydride after being dried with converter drying machine.Using conventional vanadium detection side
The content of method and silicon, phosphorus detection method analysis vanadium, silicon, phosphorus in each stage, analyzes result referring to Tables 1 and 2.
Embodiment 6:
Water for ball milling is added to crush 1 ton of bone coal navajoite that grade containing vanadium is 1.32%, powder particle diameter < 0.074mm, the solid of miberal powder slurry
Content is 700g/L, and into the water for mending 1000L in transfer pond, 50 kg catalyst A of investment after mixing, are pumped into reaction under high pressure
In kettle, stirring is started, controls 100 revs/min of revolving speed, the concentrated sulfuric acid that 150L98% is added is warming up to pressure in axe and reaches 1MPa, uniformly
Stirring 6 hours is brown ore pulp in agitator tank, ore pulp is put into chamber-type press filter after natural cooling, through filters pressing solid-liquid at this time
Separating, washing, filter residue are that vanadium content is that 0.1% slag is baked bricks as brick field auxiliary material, and mother liquor enters centrifugation decleaning tank, start stirring,
Revolving speed is controlled at 75 revs/min, 33 kilograms of cleaner is added, with liquid alkaline tune PH to 1 purification and impurity removal 6 hours, filtration washing, after purification
Mother liquor is added even B5 kilograms of agent of phase precipitation, and 30% hydrogen peroxide 100L is added dropwise, and controls precipitation current potential 485mv, static 8h, mistake after mixing
Vanadic anhydride filter cake is filtered to obtain, obtains 12.26 kilograms of vanadic anhydride after being dried with converter drying machine.Using conventional vanadium detection side
The content of method and silicon, phosphorus detection method analysis vanadium, silicon, phosphorus in each stage, analyzes result referring to Tables 1 and 2.
The content of phosphorus, silicon and vanadium in the removal of impurities post mother liquor of table 1
Content analysis of the vanadium ingredient in each stage in 2 production process of table
The above-mentioned description to embodiment is understood for the ease of those skilled in the art and using the present invention.It is familiar with
Those skilled in the art easily can make various modifications to these embodiments, and General Principle application described herein
Into other embodiments, without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments.Art technology
Personnel's principle according to the present invention, does not depart from improvement that scope of the invention is made and modification all should be in protection of the invention
Within the scope of.
Claims (10)
1. a kind of process for producing vanadic anhydride, which is characterized in that the process the following steps are included:
A) add water for ball milling to crush slurrying in bone coal navajoite stone to obtain miberal powder slurry, catalyst A mixing is added, is then pumped into autoclave
Acid adding pressurization carries out Leach reaction, obtains through being separated by solid-liquid separation containing vanadium mother liquid after reaction；
B it) is put into described in centrifugation decleaning tank containing vanadium mother liquid, cleaner is added, be 1-3 come purification and impurity removal with liquid alkaline tune pH value,
Removal of impurities mother liquor is obtained by filtration；
C) even phase precipitation agent B will be added in the removal of impurities mother liquor, is reacted after mixing, it is molten that the precipitation of dioxygen water management is added dropwise
Liquid current potential is separated by solid-liquid separation obtains filter cake after reaction in 482-500mv, obtains vanadic anhydride after dry.
2. a kind of process for producing vanadic anhydride according to claim 1, which is characterized in that the step A)
In, the content of the vanadium from stone coal vanadium is 0.9-1.9%.
3. a kind of process for producing vanadic anhydride according to claim 1, which is characterized in that the step A)
In, the dosage of the catalyst A is the 1-5% of bone coal navajoite stone quality, and the solid content of the miberal powder slurry is 700-900g/L,
Its powder particle diameter < 0.074mm.
4. a kind of process for producing vanadic anhydride according to claim 1, which is characterized in that the step A)
In, the miberal powder slurry will also enter in transfer pond after moisturizing, and catalyst A is just added and uniformly mixes, and the acid adding is to be added 98%
The pH value of the concentrated sulfuric acid, control miberal powder slurry is 5-6；Bone coal navajoite and the mass ratio of moisturizing, the concentrated sulfuric acid are 1:1:0.2-0.3.
5. a kind of process for producing vanadic anhydride according to claim 1, which is characterized in that the step A)
In, described be pressurised into is warming up to pressure up to 1-6MPa in kettle.
6. a kind of process for producing vanadic anhydride according to claim 1, which is characterized in that the step A)
In, the time of the Leach reaction is uniform stirring 6-8h, and control reaction kettle revolving speed is that 100-200 turns/min.
7. a kind of process for producing vanadic anhydride according to claim 1, which is characterized in that the step B)
In, the revolving speed control of the centrifugation decleaning tank turns/min in 40-100.
8. a kind of process for producing vanadic anhydride according to claim 1, which is characterized in that the step B)
In, the dosage that cleaner is added is 2-3 times of phosphorus content in mother liquor, except miscellaneous time is 4-8h.
9. a kind of process for producing vanadic anhydride according to claim 1, which is characterized in that the step C)
In, the dosage of the even phase precipitation agent B is the 20-120% of the content containing vanadic anhydride in removal of impurities mother liquor, the hydrogen peroxide of dropwise addition
Concentration be 20-50%.
10. a kind of process for producing vanadic anhydride according to claim 1, which is characterized in that the step C)
In, the reaction is arrest reaction, and temperature maintains 90 DEG C or more, time 8-12h.
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Cited By (2)
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| CN112010347A (en) * | 2020-07-23 | 2020-12-01 | 中信锦州金属股份有限公司 | Method for improving yield by precipitating vanadium from high-chromium vanadium solution ammonium salt |
| CN113737025A (en) * | 2021-07-23 | 2021-12-03 | 中南大学 | Efficient vanadium extraction method and efficient vanadium extraction device for high-silicon refractory stone coal vanadium ore |
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| CN112010347B (en) * | 2020-07-23 | 2022-07-26 | 中信锦州金属股份有限公司 | Method for improving yield by precipitating vanadium from high-chromium vanadium solution ammonium salt |
| CN113737025A (en) * | 2021-07-23 | 2021-12-03 | 中南大学 | Efficient vanadium extraction method and efficient vanadium extraction device for high-silicon refractory stone coal vanadium ore |
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