CN108046325A - A kind of method by the high molten molybdenum trioxide of molybdenum concntrate production catalyst - Google Patents

A kind of method by the high molten molybdenum trioxide of molybdenum concntrate production catalyst Download PDF

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Publication number
CN108046325A
CN108046325A CN201810083931.0A CN201810083931A CN108046325A CN 108046325 A CN108046325 A CN 108046325A CN 201810083931 A CN201810083931 A CN 201810083931A CN 108046325 A CN108046325 A CN 108046325A
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CN
China
Prior art keywords
molybdenum
calcining
concntrate
filter cake
dry
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Application number
CN201810083931.0A
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Chinese (zh)
Inventor
任倩
杨伟
刘锦锐
高志强
方奇
刘阳
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成都虹波钼业有限责任公司
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Priority to CN201810083931.0A priority Critical patent/CN108046325A/en
Publication of CN108046325A publication Critical patent/CN108046325A/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00Compounds of molybdenum
    • C01G39/02Oxides; Hydroxides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction 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
    • C22B3/10Hydrochloric acid, other halogenated acids or salts thereof
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Process efficiency
    • Y02P10/21Process efficiency by recovering materials
    • Y02P10/212Recovering metals from waste
    • Y02P10/234Recovering metals from waste by hydro metallurgy

Abstract

The invention discloses a kind of methods by the high molten molybdenum trioxide of molybdenum concntrate production catalyst, are including step:First, roasting and ball milling;2nd, pickling and filtering;3rd, dry.Granularity D90 is selected to be less than 60um, the molybdenum concntrate of molybdenum content >=55% is roasted after drying using rotary kiln;Dilute hydrochloric acid concentration is prepared in 3~5g/l, the solid-to-liquid ratio 1 of calcining and dilute hydrochloric acid:3~1:6, it is transferred in pressure reaction still, the interior heating of pressure reaction still is simultaneously passed through industrial oxygen, agitator treating;Calcining filter cake after being washed to what is obtained under the conditions of process above is placed in fluidized bed furnace and is carried out at the same time dry and crushes.The calcining of the present invention pressurizes acid wash from the supreme molten molybdenum trioxide of molybdenite production, and technological process is short, and metal recovery rate is high, and about 8000 yuan of production cost is per ton;Production process only generates the acidity feed liquid containing molybdenum that PH is about 2, does not generate ammonia-contaminated gas waste water, environmental-friendly.

Description

A kind of method by the high molten molybdenum trioxide of molybdenum concntrate production catalyst

Technical field

The invention belongs to chemical technology field, more particularly to one kind by the high molten molybdenum trioxide of molybdenum concntrate production catalyst Method.

Background technology

Promotion based on market to petroleum catalyst dosage demand, molybdenum trioxide is as catalyst raw material, and demand is also Increasingly soaring, the approach for seeking simple economy produces the high molten molybdenum trioxide of catalyst as industry focus.Existing report The high oxidizing molybdenum production method of catalyst, the direct material generally selected are ammonium tetramolybdate or ammonium dimolybdate, process characteristic To take method for calcinating, high solvable molybdenum trioxide is obtained, completely producing work technique is:Molybdenite --- roasting --- industry Molybdenum oxide --- ammonia leaching --- ammonium molybdate solution --- ammonium salt removal of impurities --- ammonium sulfide removal of impurities --- acid is heavy --- four molybdic acids Ammonium --- ammonia is molten --- evaporative crystallization --- ammonium dimolybdate --- low temperature calcination --- molybdenum trioxide.

This conventional method has the disadvantage that:

1. calcination method is produced from molybdenite, technological process to finished product is long, metal recovery rate is low, production cost is high, from molybdenum Concentrate is to high molten about 18000 yuan of molybdenum trioxide product per ton cost.

2. in calcination method production process, since ammonia soaks largely consumption ammonia, the heavy a large amount of ammonia for consuming nitric acid, generating a large amount of high concentrations of acid Nitrogen compound, the waste water and exhaust gas that calcining ammonium molybdate dehydration deamination generates are difficult to reach national environmental protection emission request, cause ammonia nitrogen Discharge severely exceeds, and is environmental problem urgently to be resolved hurrily.

The content of the invention

Goal of the invention:The defects of overcoming the method for conventional calcination production molybdenum oxide, for using high-grade molybdenite concentrate as original Material provides a kind of method of the brief high molten molybdenum trioxide of production catalyst so that product indices are satisfied by client's mark It is accurate and environmentally friendly, efficient, cost-effective.

Technical solution:A kind of method by the molten molybdenum trioxide of molybdenum concntrate production catalyst height is including step:First, roast Burning and ball milling;2nd, pickling and filtering;3rd, dry.

It concretely comprises the following steps:

First, roasting and ball milling

Granularity D90 is selected to be less than 60um, the molybdenum concntrate of molybdenum content >=55% is roasted after drying using rotary kiln; Temperature control is at 580~630 DEG C during roasting, and for the molybdenum calcining after being roasted by 20 mesh sieves, oversize is mixed into molybdenum concntrate raw material In it is levigate after roast again, screenings through ball mill it is levigate to D90 be less than 40um;

2nd, pickling and filtering

Dilute hydrochloric acid concentration is prepared in 3~5g/l, the solid-to-liquid ratio 1 of calcining and dilute hydrochloric acid:3~1:6, it is transferred to pressure reaction still In, the interior heating of pressure reaction still is simultaneously passed through industrial oxygen, agitator treating;Process conditions:150~200 DEG C of temperature, partial pressure of oxygen 1.0 ~1.5MPa, 300~350r/min of speed of agitator, wash time 2h, after reaction kettle release, press filtration generates filter cake and filtrate;Filter Cake penetrates filter cake cleaning again using tap water at the end of filtering;Gained filtrate is used to recycle metal molybdenum.

3rd, dry

Calcining filter cake after being washed to what is obtained under the conditions of process above is placed in fluidized bed furnace and is carried out at the same time dry and crushes; Fluidized bed furnace job parameter:Air compartment temperature:250~310 DEG C, air quantity is 240~250m3/ h, loading frequency are 20~25Hz;Drying Product granularity D90 afterwards is less than 60um.

Beneficial effects of the present invention:The calcining pressurization acid wash of the present invention produces supreme molten molybdenum trioxide, work from molybdenite Skill flow is short, and metal recovery rate is high, and about 8000 yuan of production cost is per ton;Production process only generates the acidity material containing molybdenum that PH is about 2 Liquid does not generate ammonia-contaminated gas waste water, environmental-friendly.

Description of the drawings

Fig. 1 is the method process flow chart of the high molten molybdenum trioxide of present invention production catalyst.

Specific embodiment

It is right in the following with reference to the drawings and specific embodiments in order to make the object, technical solutions and advantages of the present invention clearer The present invention is described in detail.

As shown in Figure 1, a kind of method by the high molten molybdenum trioxide of molybdenum concntrate production catalyst, is including step:First, roast Burning and ball milling;2nd, pickling and filtering;3rd, dry.

It concretely comprises the following steps:

First, roasting and ball milling

Granularity D90 is selected to be less than 60um, the molybdenum concntrate of molybdenum content >=55% is roasted after drying using rotary kiln; Temperature control is at 580~630 DEG C during roasting, and for the molybdenum calcining after being roasted by 20 mesh sieves, oversize is mixed into molybdenum concntrate raw material In it is levigate after roast again, screenings through ball mill it is levigate to D90 be less than 40um;

2nd, pickling and filtering

Dilute hydrochloric acid concentration is prepared in 3~5g/l, the solid-to-liquid ratio 1 of calcining and dilute hydrochloric acid:3~1:6, it is transferred to pressure reaction still In, the interior heating of pressure reaction still is simultaneously passed through industrial oxygen, agitator treating;Process conditions:150~200 DEG C of temperature, partial pressure of oxygen 1.0 ~1.5MPa, 300~350r/min of speed of agitator, wash time 2h, after reaction kettle release, press filtration generates filter cake and filtrate;Filter Cake penetrates filter cake cleaning again using tap water at the end of filtering;Gained filtrate is used to recycle metal molybdenum.

3rd, dry

Calcining filter cake after being washed to what is obtained under the conditions of process above is placed in fluidized bed furnace and is carried out at the same time dry and crushes; Fluidized bed furnace job parameter:Air compartment temperature:250~310 DEG C, air quantity is 240~250m3/ h, loading frequency are 20~25Hz;Drying Product granularity D90 afterwards is less than 60um.

Through being overpressurized pickling, the MoS in calcining2And MoO2It is fully converted to molybdenum trioxide, and metals content impurity therein It is greatly reduced.Table 1 is the raw material of embodiment and the elemental analysis data of product.

Table 1

The foregoing is merely the preferred embodiments of the present invention, are not intended to limit the invention, in the spiritual and former of invention Any modifications, equivalent replacements and improvements are made within then should be included within the system structure and method of the present invention.

Claims (2)

  1. A kind of 1. method by the high molten molybdenum trioxide of molybdenum concntrate production catalyst, which is characterized in that be including step:First, roast Burning and ball milling;2nd, pickling and filtering;3rd, dry.
  2. 2. the method according to claim 1 by the high molten molybdenum trioxide of molybdenum concntrate production catalyst, which is characterized in that tool Body step is:
    First, roasting and ball milling
    Granularity D90 is selected to be less than 60um, the molybdenum concntrate of molybdenum content >=55% is roasted after drying using rotary kiln;Roasting Shi Wendu is controlled at 580~630 DEG C, and the molybdenum calcining after being roasted is mixed into molybdenum concntrate raw material and grinds by 20 mesh sieves, oversize It is roasted again after thin, screenings is less than 40um to D90 through ball mill is levigate;
    2nd, pickling and filtering
    Dilute hydrochloric acid concentration is prepared in 3~5g/l, the solid-to-liquid ratio 1 of calcining and dilute hydrochloric acid:3~1:6, it is transferred in pressure reaction still, presses The interior heating of power reaction kettle is simultaneously passed through industrial oxygen, agitator treating;Process conditions:150~200 DEG C of temperature, partial pressure of oxygen 1.0~ 1.5MPa, 300~350r/min of speed of agitator, wash time 2h, after reaction kettle release, press filtration generates filter cake and filtrate;Filter cake Penetrate filter cake cleaning at the end of filtering again using tap water;Gained filtrate is used to recycle metal molybdenum.
    3rd, dry
    Calcining filter cake after being washed to what is obtained under the conditions of process above is placed in fluidized bed furnace and is carried out at the same time dry and crushes;Boiling Stove job parameter:Air compartment temperature:250~310 DEG C, air quantity is 240~250m3/ h, loading frequency are 20~25Hz;After drying Product granularity D90 is less than 60um.
CN201810083931.0A 2018-01-29 2018-01-29 A kind of method by the high molten molybdenum trioxide of molybdenum concntrate production catalyst CN108046325A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810083931.0A CN108046325A (en) 2018-01-29 2018-01-29 A kind of method by the high molten molybdenum trioxide of molybdenum concntrate production catalyst

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Application Number Priority Date Filing Date Title
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914678A (en) * 2010-08-20 2010-12-15 西北有色金属研究院 Method for producing industry molybdenum oxide from molybdenum concentrate
CN107585789A (en) * 2017-09-26 2018-01-16 河南科技大学 A kind of method that high-purity molybdenum trioxide is prepared using hydrometallurgy molybdenum concntrate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914678A (en) * 2010-08-20 2010-12-15 西北有色金属研究院 Method for producing industry molybdenum oxide from molybdenum concentrate
CN107585789A (en) * 2017-09-26 2018-01-16 河南科技大学 A kind of method that high-purity molybdenum trioxide is prepared using hydrometallurgy molybdenum concntrate

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张文钲: ""工业氧化钼生产研讨"", 《中国钼业》 *

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