CN112195336A - Efficient leaching comprehensive recovery process for mixed waste tungsten-molybdenum catalyst - Google Patents
Efficient leaching comprehensive recovery process for mixed waste tungsten-molybdenum catalyst Download PDFInfo
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- CN112195336A CN112195336A CN202010965906.2A CN202010965906A CN112195336A CN 112195336 A CN112195336 A CN 112195336A CN 202010965906 A CN202010965906 A CN 202010965906A CN 112195336 A CN112195336 A CN 112195336A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/54—Preparation of sulfur dioxide by burning elemental sulfur
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- C01G39/06—Sulfides
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- C01G41/00—Compounds of tungsten
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
- C22B34/345—Obtaining molybdenum from spent catalysts
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
- C22B34/365—Obtaining tungsten from spent catalysts
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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Abstract
The invention relates to a high-efficiency leaching comprehensive recovery process for a mixed waste tungsten-molybdenum catalyst, which comprises the following steps of: A. roasting; B. ammonia carbonate leaching; C. evaporating and crystallizing; D. precipitating molybdenum for the first time; E. secondary molybdenum precipitation; F. ammonium paratungstate. The invention adopts the processes of pyrogenic pretreatment and wet leaching, i.e. comprehensive recovery of tungsten and molybdenum by roasting, ammonia carbonate leaching and secondary molybdenum precipitation. The ammonia leaching residue can further separate valuable metals, comprehensively recover valuable components such as cobalt, nickel, aluminum and the like, achieve the aims of effectively utilizing resources, saving energy and preventing pollution, and can obtain the optimal technical and economic effects. Meanwhile, the invention has low implementation cost and reliable technology.
Description
Technical Field
The invention belongs to the field of comprehensive utilization of dangerous solid waste resources, and particularly relates to a high-efficiency leaching comprehensive recovery process for a mixed waste tungsten-molybdenum catalyst.
Background
In modern oil refining and chemical industry, more than 90% of chemical reaction process is realized in the presence of catalyst, the annual production of waste catalyst is about 50-70 ten thousand tons all over the world, and several thousand tons of waste catalyst containing molybdenum only are unloaded from the device every year, so that the recovery and utilization of valuable metals in the waste catalyst are paid more attention. The content of valuable metals in the waste catalyst is not lower than that in the ore, and the recovery of the valuable metals in the waste catalyst has important significance from the aspects of resource recycling and environmental protection. With the progress of science and technology and the development of society, higher requirements are put forward on the utilization degree of resources. At present, national economy is continuously developed and social sustainable development is promoted on the premise of reasonably utilizing resources, greatly saving natural resources and protecting ecological environment.
The random discharge of the waste catalyst not only loses various valuable metals and wastes valuable resources, but also causes serious pollution to the environment. At present, about 20 tons of waste tungsten-molybdenum catalysts are stored in northwest mining and metallurgy research institute, and the catalysts are formed by mixing two types of waste catalysts, namely FH-5A and FH-DS. Since the catalyst belongs to the field of hazardous material management, the comprehensive recovery and treatment of the waste catalyst is urgent.
Disclosure of Invention
The invention aims to provide a high-efficiency leaching comprehensive recovery process for a mixed waste tungsten-molybdenum catalyst, which has high leaching efficiency and reliable technology.
In order to achieve the purpose, the invention discloses a high-efficiency leaching comprehensive recovery process for a mixed waste tungsten-molybdenum catalyst, which is characterized by comprising the following steps of:
A. roasting: grinding the mixed type waste tungsten-molybdenum catalyst to 180-400 meshes, adding 1kg of material into a crucible, uniformly spreading, placing in a fully-closed muffle furnace, heating to 200-700 ℃, preserving heat for 2-6 hours, and slowly cooling to room temperature to obtain calcine for later use;
B. ammonia carbonate leaching: taking the calcine obtained in the step A, and mixing water: baking: 5 parts of ammonia carbonate by weight: 1: 0.01-0.25, mixing and stirring, heating to 20-40 ℃ in a leaching tank, and leaching for 1-6 hours; filtering to obtain filtrate I for later use, and recycling filter residues;
C. evaporation and crystallization: b, taking the filtrate I in the step B, heating and stirring the filtrate I in a leaching tank with the volume of 1L to the temperature of 80-95 ℃ for 1-4 hours, adding 5-15 ml of hydrochloric acid in the evaporation process, controlling the pH value to be 2-5, stopping stirring, naturally cooling at room temperature, separating out an ammonia molybdate product, and filtering to obtain a filtrate II for later use;
D. primary molybdenum precipitation: taking the filtrate II obtained in the step C, and mixing the filtrate II with the ammonium sulfide according to the weight ratio of 10: 0.01-0.15, mixing and stirring, heating to 20-40 ℃, and reacting for 1-5 hours; filtering to obtain filtrate III, and recovering molybdenum sulfide from the filter residue;
E. secondary molybdenum precipitation: taking the filtrate III obtained in the step D, and mixing the filtrate III with sodium sulfide according to a weight ratio of 10: 0.01-0.10, mixing and stirring, heating to 80-95 ℃, and reacting for 1-5 hours; filtering to obtain filtrate IV for later use, and recovering molybdenum sulfide from filter residue;
F. preparation of ammonium paratungstate: taking the filtrate IV obtained in the step E, and mixing the filtrate IV with nitric acid according to the volume ratio of 10: 0.1-0.5, mixing and stirring, heating to 30-50 ℃, and reacting for 1-5 hours; filtering to obtain filtrate V, and recovering ammonium paratungstate from the filter residue.
In the technical scheme of the high-efficiency leaching comprehensive recovery process of the mixed waste tungsten-molybdenum catalyst, the further preferable technical scheme is characterized in that:
1. heating to 400 ℃ in the step A, and keeping the temperature for 4 hours;
2. and B, water: baking: 5 parts of ammonia carbonate by weight: 1: 0.15 mixing and stirring; heating to 30 ℃ in a leaching tank, and leaching for 3.5 hours;
3. c, heating to 90 ℃ for 2.5 hours in the step C, adding 10ml of hydrochloric acid in the evaporation process, and controlling the pH value to be 3;
4. in the step D, the filtrate II and the ammonia sulfide are mixed according to the weight ratio of 10: 0.08, mixing and stirring, heating to 30 ℃, and reacting for 3 hours;
5. in the step E, the weight ratio of the filtrate III to sodium sulfide is 10: 0.05, mixing and stirring, heating to 88 ℃, and reacting for 3 hours;
6. in the step F, the volume ratio of the filtrate IV to nitric acid is 10: 0.3, mixing and stirring, heating to 40 ℃, and reacting for 3 hours.
Compared with the prior art, the invention has the beneficial effects that:
1. the process flow is short, the equipment is simple, the actual operation condition requirement is loose, and the process is convenient to control; the process has high automation degree and low labor intensity, is easy to realize scale production, and can be completely popularized in the industry.
2. The used device is simple, the waste tungsten-molybdenum catalyst is crushed and ground and then directly enters a furnace to enter a roasting treatment process, and the treatment capacity can reach 0.1 t/h. The technical requirements of the furnace charging materials are as follows: the granularity of the materials is 180-400 meshes, other materials have no special requirements, and the adaptability of the raw materials is strong.
3. The roasting treatment of the invention can be completed in one step in the rotary kiln, and the generated flue gas SO2High concentration, small smoke amount, less matched environment-friendly facilities and high sulfur recovery rate. The wet leaching process has simple equipment, basically no pollutant and little environmental pollution, and each emission index is lower than the related national standard;
4. the invention only needs a single rotary kiln and a part of leaching tanks, the process requires the materials to be the waste tungsten-molybdenum catalyst, the ammonium carbonate, the sodium sulfide, the ammonium sulfide, the nitric acid and the like, and the production cost is lower.
5. The rotary kiln type adopted by the invention is of a fully-closed structure, has good heat preservation, good environmental condition and high heat energy utilization rate, saves energy and completely meets the national requirements of energy conservation and emission reduction. The process pulverized coal consumes 50 Kg/t.
6. The invention can generate better environmental benefit and has good development prospect.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Embodiment 1, a high-efficiency leaching comprehensive recovery process for a mixed waste tungsten-molybdenum catalyst, comprising the following steps: A. roasting: grinding the mixed type waste tungsten-molybdenum catalyst to 180-400 meshes, adding 1kg of material into a crucible, uniformly spreading, placing in a fully-closed muffle furnace, heating to 200-700 ℃, preserving heat for 2-6 hours, and slowly cooling to room temperature to obtain calcine for later use; B. ammonia carbonate leaching: taking the calcine obtained in the step A, and mixing water: baking: 5 parts of ammonia carbonate by weight: 1: 0.01-0.25, mixing and stirring, heating to 20-40 ℃ in a leaching tank, and leaching for 1-6 hours; filtering to obtain filtrate I for later use, and recycling filter residues; C. evaporation and crystallization: b, taking the filtrate I in the step B, heating and stirring the filtrate I in a leaching tank with the volume of 1L to the temperature of 80-95 ℃ for 1-4 hours, adding 5-15 ml of hydrochloric acid in the evaporation process, controlling the pH value to be 2-5, stopping stirring, naturally cooling at room temperature, separating out an ammonia molybdate product, and filtering to obtain a filtrate II for later use; D. primary molybdenum precipitation: taking the filtrate II obtained in the step C, and mixing the filtrate II with the ammonium sulfide according to the weight ratio of 10: 0.01-0.15, mixing and stirring, heating to 20-40 ℃, and reacting for 1-5 hours; filtering to obtain filtrate III, and recovering molybdenum sulfide from the filter residue; E. secondary molybdenum precipitation: taking the filtrate III obtained in the step D, and mixing the filtrate III with sodium sulfide according to a weight ratio of 10: 0.01-0.10, mixing and stirring, heating to 80-95 ℃, and reacting for 1-5 hours; filtering to obtain filtrate IV for later use, and recovering molybdenum sulfide from filter residue; F. preparation of ammonium paratungstate: taking the filtrate IV obtained in the step E, and mixing the filtrate IV with nitric acid according to the volume ratio of 10: 0.1-0.5, mixing and stirring, heating to 30-50 ℃, and reacting for 1-5 hours; filtering to obtain filtrate V, and recovering ammonium paratungstate from the filter residue. Because the mixed waste tungsten-molybdenum catalyst contains W, Mo, Co, Ni and Al, the waste tungsten-molybdenum catalyst can be used for extracting metal tungsten, molybdenum and the like. Phase analysis of the waste tungsten-molybdenum catalyst: wherein, the waste tungsten-molybdenum catalyst is a mixed material of various compounds with complex components. Aiming at the phase characteristics, the invention adopts the processes of pyrogenic pretreatment and wet leaching, namely, the tungsten and the molybdenum are comprehensively recovered through roasting, ammonia carbonate leaching and secondary molybdenum precipitation. The ammonia leaching residue can further separate valuable metals, comprehensively recover valuable components such as cobalt, nickel, aluminum and the like, achieve the aims of effectively utilizing resources, saving energy and preventing pollution, and can obtain the optimal technical and economic effects. Meanwhile, the implementation cost of the invention is low, the technology is reliable, the leaching rate of the metal tungsten and molybdenum can reach more than 95%, and the recovery rate of the tungsten and the molybdenum is about 85%.
Embodiment 2, according to the comprehensive recovery process of the mixed type waste tungsten-molybdenum catalyst by high-efficiency leaching described in embodiment 1, in the step a, heating is performed to 400 ℃, and the temperature is maintained for 4 hours.
Example 3, in the mixed type waste tungsten-molybdenum catalyst high-efficiency leaching comprehensive recovery process according to example 1 or 2, the water in the step B: baking: 5 parts of ammonia carbonate by weight: 1: 0.15 mixing and stirring; heating to 30 ℃ in a leaching tank, and leaching for 3.5 hours.
Embodiment 4, in the process for efficiently leaching and comprehensively recovering the mixed type waste tungsten-molybdenum catalyst according to embodiment 1, 2 or 3, in the step C, the temperature is increased to 90 ℃ for 2.5 hours, 10ml of hydrochloric acid is added during evaporation, and the PH value is controlled to be 3.
Example 5, in the process for recovering the mixed type waste tungsten-molybdenum catalyst through high-efficiency leaching according to any one of examples 1 to 4, in the step D, the weight ratio of the filtrate ii to the ammonium sulfide is 10: 0.08, mixing and stirring, heating to 30 ℃, and reacting for 3 hours.
Example 6, the combined recovery process for high-efficiency leaching of mixed waste tungsten and molybdenum catalysts according to any one of examples 1 to 5: in the step E, the weight ratio of the filtrate III to sodium sulfide is 10: 0.05 stirring, heating to 88 ℃ and reacting for 3 hours.
Example 7, the combined recovery process for high-efficiency leaching of mixed spent tungsten-molybdenum catalyst according to any one of examples 1 to 6: in the step F, the volume ratio of the filtrate IV to nitric acid is 10: 0.3, mixing and stirring, heating to 40 ℃, and reacting for 3 hours.
Example 8, the combined recovery process for high-efficiency leaching of mixed spent tungsten-molybdenum catalyst according to any one of examples 1 to 7: the method comprises the following specific steps:
a: roasting: grinding the mixed waste tungsten-molybdenum catalyst to 180-400 meshes, adding 1Kg of material into a crucible, uniformly spreading, placing in a fully-closed muffle furnace, heating to 200 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃ or 700 ℃, keeping for 2, 3, 4, 5 or 6 hours, heating, slowly cooling to room temperature to obtain calcine for later use; the sulfur in the catalyst mainly exists in a simple substance form, and after roasting, the sulfur and the like in the slag are oxidized into sulfur dioxide, and other metals are oxidized into metal oxides and exist in the slag. The process principle is as follows:
b: ammonia carbonate leaching: taking calcine and water from A: slag: 5 parts of ammonia carbonate by weight: 1: 0.01-0.25, mixing and stirring, heating to 20, 30 or 40 ℃, and leaching for 1, 2, 3, 4 or 5 hours; filtering to obtain filtrate containing ammonium molybdate and ammonium tungstate for later use, and separately treating filter residues containing cobalt, nickel and the like; and the filtrate is sampled and sent for analysis. Calculating the leaching rate of tungsten and molybdenum to 95%; the process principle is as follows:
c: evaporation and crystallization: taking the filtrate in the B, adding the filtrate with the volume of 1L into a leaching tank, heating and stirring the filtrate to 20, 30 or 40 ℃, and stirring the filtrate for 1, 2, 3, 4 or 5 hours; adding 5-10 Ml of hydrochloric acid in the process, controlling the pH value to be 2, 3, 4 or 5, stopping stirring, naturally cooling at room temperature, separating out ammonia molybdate to be a product, and keeping the residual liquid containing a small amount of ammonia molybdate for later use; sampling the liquid and analyzing;
d: primary molybdenum precipitation: taking the filtrate in the step C, liquid: ammonia sulfide according to the weight ratio of 10: 0.01-0.15, heating to 20, 30 or 40 ℃, and stirring for 1, 2, 3, 4 or 5 hours; filtering to obtain filtrate for later use, and recovering molybdenum sulfide as a product from filter residue; sampling the filtrate, and analyzing;
e: secondary molybdenum precipitation: taking the filtrate in step D, liquid: sodium sulfide according to the weight ratio of 10: 0.01-0.10, mixing and stirring, heating to 50, 60, 70, 80 or 90 ℃, and stirring for 1, 2, 3, 4 or 5 hours; filtering to obtain filtrate for later use, and recovering molybdenum sulfide as a product from filter residue; sampling the filtrate, and analyzing;
f: preparation of ammonium paratungstate: taking the filtrate in the step E, and liquid: nitric acid according to the volume ratio of 5: 0.1-0.5, mixing and stirring, heating to 20, 30 or 40 ℃, and stirring for 1, 2, 3, 4 or 5 hours; filtering to obtain filter residue ammonium paratungstate as a product, and recycling the filtrate.
The above description is only for the preferred embodiments of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and the inventive concept thereof within the scope of the present invention.
Claims (7)
1. The high-efficiency leaching comprehensive recovery process of the mixed waste tungsten-molybdenum catalyst is characterized by comprising the following steps of:
A. roasting: grinding the mixed type waste tungsten-molybdenum catalyst to 180-400 meshes, adding 1kg of material into a crucible, uniformly spreading, placing in a fully-closed muffle furnace, heating to 200-700 ℃, preserving heat for 2-6 hours, and slowly cooling to room temperature to obtain calcine for later use;
B. ammonia carbonate leaching: taking the calcine obtained in the step A, and mixing water: baking: 5 parts of ammonia carbonate by weight: 1: 0.01-0.25, mixing and stirring, heating to 20-40 ℃ in a leaching tank, and leaching for 1-6 hours; filtering to obtain filtrate I for later use, and recycling filter residues;
C. evaporation and crystallization: b, taking the filtrate I in the step B, heating and stirring the filtrate I in a leaching tank with the volume of 1L to the temperature of 80-95 ℃ for 1-4 hours, adding 5-15 ml of hydrochloric acid in the evaporation process, controlling the pH value to be 2-5, stopping stirring, naturally cooling at room temperature, separating out an ammonia molybdate product, and filtering to obtain a filtrate II for later use;
D. primary molybdenum precipitation: taking the filtrate II obtained in the step C, and mixing the filtrate II with the ammonium sulfide according to the weight ratio of 10: 0.01-0.15, mixing and stirring, heating to 20-40 ℃, and reacting for 1-5 hours; filtering to obtain filtrate III, and recovering molybdenum sulfide from the filter residue;
E. secondary molybdenum precipitation: taking the filtrate III obtained in the step D, and mixing the filtrate III with sodium sulfide according to a weight ratio of 10: 0.01-0.10, mixing and stirring, heating to 80-95 ℃, and reacting for 1-5 hours; filtering to obtain filtrate IV for later use, and recovering molybdenum sulfide from filter residue;
F. preparation of ammonium paratungstate: taking the filtrate IV obtained in the step E, and mixing the filtrate IV with nitric acid according to the volume ratio of 10: 0.1-0.5, mixing and stirring, heating to 30-50 ℃, and reacting for 1-5 hours; filtering to obtain filtrate V, and recovering ammonium paratungstate from the filter residue.
2. The high-efficiency leaching comprehensive recovery process of the mixed type waste tungsten-molybdenum catalyst as claimed in claim 1, which is characterized in that: and heating to 400 ℃ in the step A, and keeping the temperature for 4 hours.
3. The high-efficiency leaching comprehensive recovery process of the mixed type waste tungsten-molybdenum catalyst as claimed in claim 1, which is characterized in that: and B, water: baking: 5 parts of ammonia carbonate by weight: 1: 0.15 mixing and stirring; heating to 30 ℃ in a leaching tank, and leaching for 3.5 hours.
4. The high-efficiency leaching comprehensive recovery process of the mixed type waste tungsten-molybdenum catalyst as claimed in claim 1, which is characterized in that: and C, heating to 90 ℃ in the step C for 2.5 hours, adding 10ml of hydrochloric acid in the evaporation process, and controlling the pH value to be 3.
5. The high-efficiency leaching comprehensive recovery process of the mixed type waste tungsten-molybdenum catalyst as claimed in claim 1, which is characterized in that: in the step D, the filtrate II and the ammonia sulfide are mixed according to the weight ratio of 10: 0.08, mixing and stirring, heating to 30 ℃, and reacting for 3 hours.
6. The high-efficiency leaching comprehensive recovery process of the mixed type waste tungsten-molybdenum catalyst as claimed in claim 1, which is characterized in that: in the step E, the weight ratio of the filtrate III to sodium sulfide is 10: 0.05 stirring, heating to 88 ℃ and reacting for 3 hours.
7. The high-efficiency leaching comprehensive recovery process of the mixed type waste tungsten-molybdenum catalyst as claimed in claim 1, which is characterized in that: in the step F, the volume ratio of the filtrate IV to nitric acid is 10: 0.3, mixing and stirring, heating to 40 ℃, and reacting for 3 hours.
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