CN104129814A - Method for producing ammonium metavanadate by using petroleum hydrogenation waste catalyst as raw material - Google Patents
Method for producing ammonium metavanadate by using petroleum hydrogenation waste catalyst as raw material Download PDFInfo
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- CN104129814A CN104129814A CN201410339692.2A CN201410339692A CN104129814A CN 104129814 A CN104129814 A CN 104129814A CN 201410339692 A CN201410339692 A CN 201410339692A CN 104129814 A CN104129814 A CN 104129814A
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Abstract
The invention relates to a method for producing ammonium metavanadate by using a petroleum hydrogenation waste catalyst as a raw material. The method relates to the technical field of non-ferrous metallurgy. According to the invention, under a condition of high temperature, the petroleum hydrogenation waste catalyst is oxidized in a rotating rotary kiln by using oxygen, such that an oxide of vanadium is produced; the oxide of vanadium is subjected to a reaction with sodium oxide under a temperature of 850-950 DEG C, such that sodium vanadate is produced; sodium vanadate is cooled and is delivered to a wet ball milling process; high temperature leaching and solid-liquid separation are carried out; nickel-rich slag obtained by separation can be directly used for smelting, and liquid obtained by separation is subjected to ammonium salt vanadium precipitation, such that ammonium metavanadate can be produced. Compared to prior arts, the method provided by the invention has the characteristics of simple production process, convenient operation, low cost, and high safety.
Description
Technical field
The invention belongs to technical field of non-ferrous metallurgy, particularly a kind of method of producing ammonium meta-vanadate.
Background technology
Ammonium meta-vanadate (ammonium metavanadate is called for short AMV), white or slightly light yellow crystalline powder, molecular formula: NH4VO3, molecular weight: 116.98, relatively close 2.326; 200 DEG C of fusing points, are slightly soluble in cold water, hot ethanol and ether, are dissolved in hot water and rare ammonium hydroxide; In air, become Vanadium Pentoxide in FLAKES when calcination, poisonous.Main as chemical reagent, catalyzer, siccative, mordant etc., ceramic industry is widely used as glaze, also can be used for producing Vanadium Pentoxide in FLAKES.Ammonium meta-vanadate is mainly used in main as chemical reagent and catalyzer, also can be used for producing Vanadium Pentoxide in FLAKES.For smelting ferrovanadium, as alloy addition, account for the more than 80% of Vanadium Pentoxide in FLAKES total amount consumed.
The raw material of producing at present ammonium meta-vanadate is all bone coal, slag etc., the high and difficult buying of raw materials cost.Sodium roasting technique is the technology of state-of-the-art extraction vanadium.It has, and technique is simple, the extraction yield low, vanadium that consumes energy is high, is conducive to metal enrichment.Its product ammonium meta-vanadate is all the raw material of domestic urgent need high-tech product.All the time, the method of domestic production ammonium meta-vanadate is all mainly pickling process, first by carrying out after sodium roasting, water logging containing vanadium raw materials, prepare sodium vanadate solution through impurity and purification again, then with stirring and be settled out ammonium meta-vanadate under ammonium salt normal temperature, because the content of impurity is very large, thereby be difficult to prepare highly purified ammonium meta-vanadate.In order to prepare highly purified ammonium meta-vanadate, normally sodium vanadate solution is added under acidic conditions to ammonium salt precipitation ammonium poly-vanadate, then ammonium poly-vanadate is returned molten with sodium salt deamination, obtain sodium vanadate solution, after purification, add ammonium salt, stir and be settled out high-purity ammonium meta-vanadate at normal temperatures.The method exist ammonium salt and sodium salt consumption large, and the high problem of sodium content in the ammonium meta-vanadate obtaining.And its pH value in reaction low (being less than 2), requiring of the equipment to reaction is high, and reaction is all discontinuity, level of automation is low, these problems have increased the production cost of producing ammonium meta-vanadate to a great extent, and the quality of the ammonium meta-vanadate obtaining is unstable, and wastewater flow rate is large.
So this area is needed a kind of new technology badly and is changed such present situation.
Summary of the invention
Technical problem to be solved by this invention: for shortcomings and deficiencies of the prior art, the invention provides that a kind of production technique is simple, convenient operation, with low cost, the safe method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate.
The present invention is design like this: a kind of method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate, is characterized in that: comprise the steps,
Step 1, by oil hydrogenation spent catalyst, soda ash with water in 1:(0.3～0.6): the ratio of (0.1～0.2) is mixed;
Step 2, the mixture in step 1 is added in rotary kiln continuously from rotary kiln, the control of rotary kiln revolution is 0.12 rev/min; The long 38m of described rotary kiln, rotary kiln higher than kiln hood, with ground be 3.5 ° of angles, rotary kiln is followed successively by region, preheating zone, the roasting region of 23m and the cooling zone region of 5m of 10m from kiln tail to kiln hood;
Step 3, burner is stretched in rotary kiln and lighted from rotary kiln end, and at the oxygen that passes into 0.2MP pressure apart from 10 meters of of kiln tail;
Region, the preheating zone temperature of step 4, control 10m is (300～500) DEG C, make mixture in step 2 when through region, preheating zone transpiring moisture and and oxygen reaction, 97%～98% vanadium sulfide in oil hydrogenation spent catalyst is oxidized to Vanadium Pentoxide in FLAKES, by all nickelous sulfides be oxidized to nickel oxide, soda ash resolves into sodium oxide, this process time is 2h～3h;
The roasting region temperature of step 5, control 23m is 850 DEG C～950 DEG C, makes all Vanadium Pentoxide in FLAKESs that produce in step 4 when through roasting region, react generation solubility vanadic acid sodium with sodium oxide, and this process time is 5h～6h;
The cooling zone regional temperature of step 6, control 5m is 550 DEG C～600 DEG C, and this process mixture is 1h～1.5h through the time in cooling zone region;
Step 7, mixture are out delivered to afterwards cooler from rotary kiln, and mixture is cooled to 20 DEG C～30 DEG C of room temperatures, and this process time is 2min;
Step 8, the mixture in step 7 is selected to qualified calcining after screening, calcining is delivered to ball mill by wet process, calcining is liquid-solid separation after ball milling and high temperature leach;
The isolated solid of calcining in step 9, step 8 is nickeliferous 5%～8% rich nickel slag, rich nickel slag is delivered to smeltery stand-by; The isolated liquid of calcining adds ammonium chloride reaction to generate ammonium meta-vanadate after purifying.
In described step 1 PetroChina Company Limited. hydrogenation spent catalyst raw material, the mass percent of vanadium is 10%～18%, and the mass percent of nickel is 2%～4%.
Described rotary kiln, cooler and ball mill by wet process is all rotating machinery.
In burner in described step 3, be connected with coal gas.
Oxygen purity used in described step 3 is greater than 98%.
Oxygen flow in described step 3 is 10m
3/ h～15m
3/ h.
350 DEG C～500 DEG C of vanadium in described step 4, the sulfide oxidizing temperatures of nickel.
The reaction conditions that the isolated liquid of calcining in described step 9 adds ammonium chloride reaction to generate ammonium meta-vanadate after purifying is 20 DEG C～30 DEG C of room temperatures, pH8.0～8.5.
By above-mentioned design, the present invention can bring following beneficial effect:
1, the present invention is a kind of is a kind of method of brand-new production ammonium meta-vanadate taking oil hydrogenation spent catalyst as the method for raw material production ammonium meta-vanadate.Oil hydrogenation spent catalyst under the condition at high temperature, with dioxygen oxidation, generates the oxide compound of vanadium in the rotary kiln rotating; The oxide compound of vanadium generates vanadic acid sodium with sodium oxide at the temperature of 850 DEG C～950 DEG C; Vanadic acid sodium is delivered to wet ball grinding through overcooling, then leaches through high temperature, and solid-liquid separation, the rich nickel slag after separation can be directly used in smelting, and liquid carries out producing ammonium meta-vanadate after ammonium salt precipitation.This method reaction conditions gentleness, does not relate to hazardous and noxious substances, operational safety; Process is simple, does not need complicated flow process and loaded down with trivial details equipment, easy and simple to handle; Roasting and combined coefficient are high, 97%～98% vanadium sulfide in oil hydrogenation spent catalyst is used again, instead of buys new starting material, and cost is low.
2, the present invention a kind of taking oil hydrogenation spent catalyst in the method for raw material production ammonium meta-vanadate, the spent catalyst oxidizing roasting of oil hydrogenation and sodium roasting once complete in a rotary kiln device, are conducive to reduce costs, and simplify the operation, meanwhile, reach higher production efficiency.
3, simple, the convenient operation, with low cost, safe of a kind of method production technique taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate of the present invention, can carry out scale operation, in order to substitute existing old technology.
Embodiment
A method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate, is characterized in that: comprises the steps,
Step 1, by oil hydrogenation spent catalyst, soda ash with water in 1:(0.3～0.6): the ratio of (0.1～0.2) is mixed;
Step 2, the mixture in step 1 is added in rotary kiln continuously from rotary kiln, the control of rotary kiln revolution is 0.12 rev/min; The long 30m of described rotary kiln, rotary kiln higher than kiln hood, with ground be 3.5 ° of angles, rotary kiln is followed successively by region, preheating zone, the roasting region of 23m and the cooling zone region of 5m of 10m from kiln tail to kiln hood;
Step 3, burner is stretched in rotary kiln and lighted from rotary kiln, and at the oxygen that passes into 0.2MP pressure apart from 10 meters of of kiln tail;
Region, the preheating zone temperature of step 4, control 10m is (300～500) DEG C, make mixture in step 2 when through region, preheating zone transpiring moisture and and oxygen reaction, 97%～98% vanadium sulfide in oil hydrogenation spent catalyst is oxidized to Vanadium Pentoxide in FLAKES, by all nickelous sulfides be oxidized to nickel oxide, soda ash resolves into sodium oxide, this process time is 2h～3h;
The roasting region temperature of step 5, control 23m is 850 DEG C～950 DEG C, makes all Vanadium Pentoxide in FLAKESs that produce in step 4 when through roasting region, react generation solubility vanadic acid sodium with sodium oxide, and this process time is 5h～6h;
The cooling zone regional temperature of step 6, control 5m is 550 DEG C～600 DEG C, and this process mixture is 1h～1.5h through the time in cooling zone region;
Step 7, mixture are out delivered to afterwards cooler from rotary kiln, and mixture is cooled to room temperature, and this process time is 2min;
Step 8, the mixture in step 7 is selected to qualified calcining after screening, calcining is delivered to ball mill by wet process, calcining is liquid-solid separation after ball milling and high temperature leach;
The isolated solid of calcining in step 9, step 8 is nickeliferous 5%～8% rich nickel slag, rich nickel slag is delivered to smeltery stand-by; The isolated liquid of calcining adds ammonium chloride reaction to generate ammonium meta-vanadate after purifying.
In described oil hydrogenation spent catalyst raw material, the mass percent of vanadium is 10%～18%, and the mass percent of nickel is 2%～4%.
Described rotary kiln, cooler and ball mill is all rotating machinery.
In burner in described step 3, be connected with coal gas.
Oxygen purity used in described step 3 is greater than 98%.
Oxygen flow in described step 3 is 10m
3/ h～15m
3/ h.
350 DEG C～500 DEG C of vanadium in described step 4, the sulfide oxidizing temperatures of nickel.
The reaction conditions that the isolated liquid of calcining in described step 9 adds ammonium chloride reaction to generate ammonium meta-vanadate after purifying is room temperature, pH8.0～8.5.
The difference of and reaction conditions raw materials used according to the present invention, prepare 6 batches of ammonium meta-vanadates:
Embodiment 1
Oil hydrogenation spent catalyst raw material major ingredient:
| V 2O 5 | Ni | Fe | S | Mn | Mg | Zn | Cu | Al 2O 3 | SiO2 |
| 13.5 | 2.3 | 0.066 | 6.36 | 0.08 | 0.01 | 0.013 | 0.003 | 45 | 1.81 |
Rotating in rotary kiln the mixing raw material that adds oil hydrogenation spent catalyst and soda ash, water with the speed of 800kg per hour, raw material moisture content 15%, rotary kiln revolution is decided to be 0.12 rev/min, residence time of material 6h, passes into heating gas during this time and oxygen reacts, and preheating temperature of reaction is controlled at 300 DEG C～500 DEG C, material dewatering, vanadium sulfide is oxidized to Vanadium Pentoxide in FLAKES, and nickelous sulfide is oxidized to nickel oxide, and soda ash is decomposed into sodium oxide; 870 DEG C of calcination temperature, Vanadium Pentoxide in FLAKES reacts with sodium oxide produces vanadic acid sodium.Cooling zone temperature of reaction is 590 DEG C, cooling through cooler pressure, produces qualified calcining, turns the rate of soaking and reaches 96.7%.Qualified calcining is transported to ball mill by wet process to carry out heating after ball milling to 90 DEG C and leaches, and extraction time is 3h.Leaching finishes to carry out press filtration with sheet frame afterwards, and in solid, nickel degree is 5.3%, is transported to smeltery and smelts.Liquor pump adds ammonium chloride to carry out the heavy reaction of ammonium to reactor, and temperature of reaction is room temperature, and the reaction times is 1.5h.The qualified rear press filtration of supernatant liquor after testing, the solid after filtration is ammonium meta-vanadate product, packaging after drying.Product ammonium meta-vanadate purity is 99.91%.Metal recovery rate is 92%.
Embodiment 2
Oil hydrogenation spent catalyst raw material composition:
| V 2O 5 | Ni | Fe | S | Mn | Mg | Zn | Cu | Al 2O 3 | SiO2 |
| 14.5 | 2.7 | 0.042 | 6.38 | 0.03 | 0.01 | 0.007 | 0.003 | 44.7 | 1.66 |
Rotating in rotary kiln the mixing raw material that adds oil hydrogenation spent catalyst and soda ash, water with the speed of 800kg per hour, raw material moisture content 13%, rotary kiln revolution is decided to be 0.12 rev/min, residence time of material 5h, passes into heating gas during this time and oxygen reacts, and preheating temperature of reaction is controlled at 300 DEG C～500 DEG C, material dewatering, vanadium sulfide is oxidized to Vanadium Pentoxide in FLAKES, and nickelous sulfide is oxidized to nickel oxide, and soda ash is decomposed into sodium oxide; 890 DEG C of calcination temperature, Vanadium Pentoxide in FLAKES reacts with sodium oxide produces vanadic acid sodium.Cooling zone temperature of reaction is 590 DEG C, cooling through cooler pressure, produces qualified calcining, turns the rate of soaking and reaches 96.3%.Qualified calcining is transported to ball mill by wet process to carry out heating after ball milling to 90 DEG C and leaches, and extraction time is 3h.Leaching finishes to carry out press filtration with sheet frame afterwards, and in solid, nickel degree is 5.8%, is transported to smeltery and smelts.Liquor pump adds ammonium chloride to carry out the heavy reaction of ammonium to reactor, and temperature of reaction is room temperature, and the reaction times is 1.5h.The qualified rear press filtration of supernatant liquor after testing, the solid after filtration is ammonium meta-vanadate product, packaging after drying.Product ammonium meta-vanadate purity is 99.89%.Metal recovery rate is 93.47%.
Embodiment 3
Oil hydrogenation spent catalyst raw material composition:
| V 2O 5 | Ni | Fe | S | Mn | Mg | Zn | Cu | Al 2O 3 | SiO2 |
| 13.7 | 2.4 | 0.032 | 6.08 | 0.02 | 0.01 | 0.007 | 0.003 | 45.9 | 1.16 |
Rotating in rotary kiln the mixing raw material that adds oil hydrogenation spent catalyst and soda ash, water with the speed of 800kg per hour, raw material moisture content 11%, rotary kiln revolution is decided to be 0.12 rev/min, residence time of material 5.5h, passes into heating gas during this time and oxygen reacts, and preheating temperature of reaction is controlled at 300 DEG C～500 DEG C, material dewatering, vanadium sulfide is oxidized to Vanadium Pentoxide in FLAKES, and nickelous sulfide is oxidized to nickel oxide, and soda ash is decomposed into sodium oxide; 930 DEG C of calcination temperature, Vanadium Pentoxide in FLAKES reacts with sodium oxide produces vanadic acid sodium.Cooling zone temperature of reaction is 580 DEG C, cooling through cooler pressure, produces qualified calcining, turns the rate of soaking and reaches more than 95%.Qualified calcining is transported to ball mill by wet process to carry out heating after ball milling to 90 DEG C and leaches, and extraction time is 3h.Leaching finishes to carry out press filtration with sheet frame afterwards, and in solid, nickel degree is 6.4%, is transported to smeltery and smelts.Liquor pump adds ammonium chloride to carry out the heavy reaction of ammonium to reactor, and temperature of reaction is room temperature, and the reaction times is 1.5h.The qualified rear press filtration of supernatant liquor after testing, the solid after filtration is ammonium meta-vanadate product, packaging after drying.Product ammonium meta-vanadate purity is 99.90%.Metal recovery rate is 92.23%.
Embodiment 4
Oil hydrogenation spent catalyst raw material composition:
| V 2O 5 | Ni | Fe | S | Mn | Mg | Zn | Cu | Al 2O 3 | SiO2 |
| 14.5 | 2.7 | 0.042 | 6.38 | 0.03 | 0.01 | 0.007 | 0.003 | 44.7 | 1.66 |
Rotating in rotary kiln the mixing raw material that adds oil hydrogenation spent catalyst and soda ash, water with the speed of 800kg per hour, raw material moisture content 12.7%, rotary kiln revolution is decided to be 0.12 rev/min, residence time of material 4.5h, passes into heating gas during this time and oxygen reacts, and preheating temperature of reaction is controlled at 300 DEG C～500 DEG C, material dewatering, vanadium sulfide is oxidized to Vanadium Pentoxide in FLAKES, and nickelous sulfide is oxidized to nickel oxide, and soda ash is decomposed into sodium oxide; 887 DEG C of calcination temperature, Vanadium Pentoxide in FLAKES reacts with sodium oxide produces vanadic acid sodium.Cooling zone temperature of reaction is 560 DEG C, cooling through cooler pressure, produces qualified calcining, turns the rate of soaking and reaches 94.6%.Qualified calcining is transported to ball mill by wet process to carry out heating after ball milling to 90 DEG C and leaches, and extraction time is 3h.Leaching finishes to carry out press filtration with sheet frame afterwards, and in solid, nickel degree is 7.17%, is transported to smeltery and smelts.Liquor pump adds ammonium chloride to carry out the heavy reaction of ammonium to reactor, and temperature of reaction is room temperature, and the reaction times is 1.5h.The qualified rear press filtration of supernatant liquor after testing, the solid after filtration is ammonium meta-vanadate product, packaging after drying.Product ammonium meta-vanadate purity is 99.76%.Metal recovery rate is 93.45%.
Embodiment 5
Oil hydrogenation spent catalyst raw material composition:
| V 2O 5 | Ni | Fe | S | Mn | Mg | Zn | Cu | Al 2O 3 | SiO2 |
| 13.3 | 2.1 | 0.022 | 5.38 | 0.03 | 0.02 | 0.009 | 0.002 | 43.1 | 1.41 |
Rotating in rotary kiln the mixing raw material that adds oil hydrogenation spent catalyst and soda ash, water with the speed of 800kg per hour, raw material moisture content 14.7%, rotary kiln revolution is decided to be 0.12 rev/min, residence time of material 4h, passes into heating gas during this time and oxygen reacts, and preheating temperature of reaction is controlled at 300 DEG C～500 DEG C, material dewatering, vanadium sulfide is oxidized to Vanadium Pentoxide in FLAKES, and nickelous sulfide is oxidized to nickel oxide, and soda ash is decomposed into sodium oxide; 910 DEG C of calcination temperature, Vanadium Pentoxide in FLAKES reacts with sodium oxide produces vanadic acid sodium.Cooling zone temperature of reaction is 590 DEG C, cooling through cooler pressure, produces qualified calcining, turns the rate of soaking and reaches 86.7%.Qualified calcining is transported to ball mill by wet process to carry out heating after ball milling to 90 DEG C and leaches, and extraction time is 3h.Leaching finishes to carry out press filtration with sheet frame afterwards, and in solid, nickel degree is 4.58%, is transported to smeltery and smelts.Liquor pump adds ammonium chloride to carry out the heavy reaction of ammonium to reactor, and temperature of reaction is room temperature, and the reaction times is 1.5h.The qualified rear press filtration of supernatant liquor after testing, the solid after filtration is ammonium meta-vanadate product, packaging after drying.Product ammonium meta-vanadate purity is 99.73%.Metal recovery rate is 87.10%.
Embodiment 6
Oil hydrogenation spent catalyst raw material composition:
| V 2O 5 | Ni | Fe | S | Mn | Mg | Zn | Cu | Al 2O 3 | SiO2 |
| 12.7 | 3.6 | 0.032 | 6.28 | 0.03 | 0.02 | 0.01 | 0.004 | 44.5 | 1.54 |
Rotating in rotary kiln the mixing raw material that adds oil hydrogenation spent catalyst and soda ash, water with the speed of 800kg per hour, raw material moisture content 12.1%, rotary kiln revolution is decided to be 0.12 rev/min, residence time of material 6h, passes into heating gas during this time and oxygen reacts, and preheating temperature of reaction is controlled at 300 DEG C～500 DEG C, material dewatering, vanadium sulfide is oxidized to Vanadium Pentoxide in FLAKES, and nickelous sulfide is oxidized to nickel oxide, and soda ash is decomposed into sodium oxide; 930 DEG C of calcination temperature, Vanadium Pentoxide in FLAKES reacts with sodium oxide produces vanadic acid sodium.Cooling zone temperature of reaction is 570 DEG C, cooling through cooler pressure, produces qualified calcining, turns the rate of soaking and reaches 88.2%.Qualified calcining is transported to ball mill by wet process to carry out heating after ball milling to 90 DEG C and leaches, and extraction time is 3h.Leaching finishes to carry out press filtration with sheet frame afterwards, and in solid, nickel degree is 6.98%, is transported to smeltery and smelts.Liquor pump adds ammonium chloride to carry out the heavy reaction of ammonium to reactor, and temperature of reaction is room temperature, and the reaction times is 1.5h.The qualified rear press filtration of supernatant liquor after testing, the solid after filtration is ammonium meta-vanadate product, packaging after drying.Product ammonium meta-vanadate purity is 99.91%.Metal recovery rate is 89.60%.
Claims (8)
1. the method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate, is characterized in that:
Comprise the steps
Step 1, by oil hydrogenation spent catalyst, soda ash with water in 1:(0.3～0.6): the ratio of (0.1～0.2) is mixed;
Step 2, the mixture in step 1 is added in rotary kiln continuously from rotary kiln, the control of rotary kiln revolution is 0.12 rev/min; The long 38m of described rotary kiln, rotary kiln higher than kiln hood, with ground be 3.5 ° of angles, rotary kiln is followed successively by region, preheating zone, the roasting region of 23m and the cooling zone region of 5m of 10m from kiln tail to kiln hood;
Step 3, burner is stretched in rotary kiln and lighted from rotary kiln end, and at the oxygen that passes into 0.2MP pressure apart from 10 meters of of kiln tail;
Region, the preheating zone temperature of step 4, control 10m is (300～500) DEG C, make mixture in step 2 when through region, preheating zone transpiring moisture and and oxygen reaction, 97%～98% vanadium sulfide in oil hydrogenation spent catalyst is oxidized to Vanadium Pentoxide in FLAKES, by all nickelous sulfides be oxidized to nickel oxide, soda ash resolves into sodium oxide, this process time is 2h～3h;
The roasting region temperature of step 5, control 23m is 850 DEG C～950 DEG C, makes all Vanadium Pentoxide in FLAKESs that produce in step 4 when through roasting region, react generation solubility vanadic acid sodium with sodium oxide, and this process time is 5h～6h;
The cooling zone regional temperature of step 6, control 5m is 550 DEG C～600 DEG C, and this process mixture is 1h～1.5h through the time in cooling zone region;
Step 7, mixture are out delivered to afterwards cooler from rotary kiln, and mixture is cooled to 20 DEG C～30 DEG C of room temperatures, and this process time is 2min;
Step 8, the mixture in step 7 is selected to qualified calcining after screening, calcining is delivered to ball mill by wet process, calcining is liquid-solid separation after ball milling and high temperature leach;
The isolated solid of calcining in step 9, step 8 is nickeliferous 5%～8% rich nickel slag, rich nickel slag is delivered to smeltery stand-by; The isolated liquid of calcining adds ammonium chloride reaction to generate ammonium meta-vanadate after purifying.
2. a kind of method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate according to claim 1, it is characterized in that: in described step 1 PetroChina Company Limited. hydrogenation spent catalyst raw material, the mass percent of vanadium is 10%～18%, and the mass percent of nickel is 2%～4%.
3. a kind of method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate according to claim 1, is characterized in that: described rotary kiln, cooler and ball mill by wet process is all rotating machinery.
4. a kind of method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate according to claim 1, is characterized in that: in the burner in described step 3, be connected with coal gas.
5. a kind of method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate according to claim 1, is characterized in that: oxygen purity used in described step 3 is greater than 98%.
6. a kind of method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate according to claim 1, is characterized in that: the oxygen flow in described step 3 is 10m
3/ h～15m
3/ h.
7. a kind of method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate according to claim 1, is characterized in that: 350 DEG C～500 DEG C of the vanadium in described step 4, the sulfide oxidizing temperatures of nickel.
8. a kind of method taking oil hydrogenation spent catalyst as raw material production ammonium meta-vanadate according to claim 1, it is characterized in that: the reaction conditions that the isolated liquid of calcining in described step 9 adds ammonium chloride reaction to generate ammonium meta-vanadate after purifying is 20 DEG C～30 DEG C of room temperatures, pH8.0～8.5.
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| CN104528825A (en) * | 2014-12-17 | 2015-04-22 | 武汉源宸再生资源科技有限公司 | Method for producing ammonium metavanadate, lanthanum oxalate, cerium oxalate and nickel sulfide by using spent catalytic cracking catalyst from oil refinery |
| CN104609470A (en) * | 2014-12-17 | 2015-05-13 | 武汉源宸再生资源科技有限公司 | Method using oil refining plant catalytic cracking waste catalyst for production of ammonium metavanadate, lanthanum oxalate and cerous oxalate |
| CN107805716A (en) * | 2017-11-08 | 2018-03-16 | 大连东泰资源再生有限公司 | A kind of nickel aluminium powder recovery method |
| CN109628765A (en) * | 2018-12-27 | 2019-04-16 | 大连博融新材料有限公司 | A kind of recovery method of vpo catalyst |
| KR20210150899A (en) * | 2020-06-04 | 2021-12-13 | 한국지질자원연구원 | Recovery method of vanadium from aqueous solution containing vanadium |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528825A (en) * | 2014-12-17 | 2015-04-22 | 武汉源宸再生资源科技有限公司 | Method for producing ammonium metavanadate, lanthanum oxalate, cerium oxalate and nickel sulfide by using spent catalytic cracking catalyst from oil refinery |
| CN104609470A (en) * | 2014-12-17 | 2015-05-13 | 武汉源宸再生资源科技有限公司 | Method using oil refining plant catalytic cracking waste catalyst for production of ammonium metavanadate, lanthanum oxalate and cerous oxalate |
| CN104528825B (en) * | 2014-12-17 | 2016-08-24 | 武汉源宸再生资源科技有限公司 | Ammonium metavanadate, lanthanum oxalate, Sedemesis. and the method for nickel sulfide is produced by oil plant catalytic cracking spent catalyst |
| CN107805716A (en) * | 2017-11-08 | 2018-03-16 | 大连东泰资源再生有限公司 | A kind of nickel aluminium powder recovery method |
| CN107805716B (en) * | 2017-11-08 | 2019-07-23 | 大连东泰资源再生有限公司 | A kind of nickel aluminium powder recovery method |
| CN109628765A (en) * | 2018-12-27 | 2019-04-16 | 大连博融新材料有限公司 | A kind of recovery method of vpo catalyst |
| CN109628765B (en) * | 2018-12-27 | 2021-06-15 | 大连博融新材料有限公司 | Method for recovering VPO catalyst |
| KR20210150899A (en) * | 2020-06-04 | 2021-12-13 | 한국지질자원연구원 | Recovery method of vanadium from aqueous solution containing vanadium |
| KR102362942B1 (en) | 2020-06-04 | 2022-02-15 | 한국지질자원연구원 | Recovery method of vanadium from aqueous solution containing vanadium |
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