CN104232942A - Pretreatment method of tungsten mineral materials - Google Patents

Pretreatment method of tungsten mineral materials Download PDF

Info

Publication number
CN104232942A
CN104232942A CN201410527644.6A CN201410527644A CN104232942A CN 104232942 A CN104232942 A CN 104232942A CN 201410527644 A CN201410527644 A CN 201410527644A CN 104232942 A CN104232942 A CN 104232942A
Authority
CN
China
Prior art keywords
raw material
tungsten
tungsten mineral
leaching
wolframite
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201410527644.6A
Other languages
Chinese (zh)
Other versions
CN104232942B (en
Inventor
李小斌
崔源发
周秋生
李建圃
齐天贵
徐双
刘桂华
林国荣
彭志宏
李继红
徐向明
徐旺
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangxi Rare Earth and Rare Metals Tungsten Group Holding Co Ltd
Central South University
Original Assignee
Jiangxi Rare Earth and Rare Metals Tungsten Group Holding Co Ltd
Central South University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangxi Rare Earth and Rare Metals Tungsten Group Holding Co Ltd, Central South University filed Critical Jiangxi Rare Earth and Rare Metals Tungsten Group Holding Co Ltd
Priority to CN201410527644.6A priority Critical patent/CN104232942B/en
Publication of CN104232942A publication Critical patent/CN104232942A/en
Application granted granted Critical
Publication of CN104232942B publication Critical patent/CN104232942B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

Disclosed is a pretreatment method of tungsten mineral materials. The pretreatment method of the tungsten mineral materials is characterized by including the following steps of raw material preparation and clinker sintering, the raw material preparation includes that the tungsten mineral materials (scheelite, wolframite, scheelite and wolframite mixed mineral and/or tungsten fine silt) are mixed with a certain quantity of calcic substances and mineralizer to be finely ground to obtain raw materials, and the clinker sintering includes that the prepared raw materials are calcinated under special conditions to obtain clinker. The pretreatment method of the tungsten mineral materials has the advantages that the adaptability is wide, and the method is suitable for all tungsten mineral materials, especially scheelite; (2) added calcic substances are cheap and easy to obtain; (3) the calcination temperature is low, the operation is simple, and the industrial application is easy; (4) tungsten in the obtained clinker is good in leaching performance, fully leaching can be achieved by a sodium carbonate solution or an ammonium carbonate salt solution at low temperature, especially when leaching is performed by the ammonium carbonate salt solution, the economical circulation of the solution during APT production can be achieved, and thereby, discharging of wastewater during production can be eliminated.

Description

A kind of pretreatment process of tungsten mineral material
Technical field
The present invention relates to a kind of pretreatment process of tungsten mineral material, belong to Tungsten smelting technical field.
Background technology
At present, the technological line of industrial preparation APT mainly comprises: adopt caustic soda or soda high-temperature high-pressure to boil decomposition of tungsten mineral raw material → coarse sodium tungstate → solution purification and the → pure tungsten acid ammonium solution → evaporative crystallization → APT → product washing that makes the transition.In APT preparation process, because solution is difficult to economic circulation, supplies consumption is large, and produces a large amount of waste water, and environmental pollution is heavier.
In recent years, attention is obtained using sal volatile as the Leaching Systems of tungsten mineral material.Regrettably, existing industrial tungsten mineral material is difficult to be decomposed by sal volatile under current technology condition.
In prior art, be with the compound of calcareous material 800 ~ 1400 DEG C of roastings to the pre-treatment of tungstenic raw material, to prepare the Ca with good leaching performance 3wO 6.But roasting time required when temperature is lower is long, though at 800 DEG C roasting 16h, the tungsten in tungstenic raw material is converted into Ca not yet completely 3wO 6; For wolframite or Scheelite-Wolframite Mixed Mine, iron wherein is converted into calcium ferrite at roasting process, cause and allocate calcium amount into greatly, roasting energy consumption is high, and the leaching quantity of slag is many and tungsten leaching yield is low; Meanwhile, maturing temperature is high again, the Ca of acquisition 3wO 6middle tungsten leaching performance is deteriorated on the contrary.
The present inventor's exploration and practice for many years shows, the pre-treatment of tungsten mineral material affects its leaching performance in sal volatile system, relate to multiple factor, the batching of such as compound is selected, granularity and ratio, the selection of mineralizer, maturing temperature, roasting time, calcination atmosphere, etc., these factors are all often restrictions mutually, interactional, be not separate, still infinite may combining is had after orthogonal design, and enough excellent technical scheme can not be predicted, " experiment of limited number of time " can not obtain the suitable value of each factor, enough excellent technical scheme is not " obviously ".
Just because of this, in prior art, also there is no adequate measures, to strengthen the leaching performance of tungsten mineral material in sal volatile system.
Summary of the invention
The object of this invention is to provide a kind of pretreatment process of tungsten mineral material, the method can improve the leaching performance of tungsten mineral material in sal volatile system or similar weakly alkaline system.
Another object of the present invention is to provide a kind of pretreatment process of tungsten mineral material, makes the tungsten in tungsten mineral material can be converted into the high reactivity Ca with good leaching performance completely at lesser temps with in the short period 3wO 6or Ca 2feWO 6or Ca 2mnWO 6, make it to be leached by sodium carbonate or ammonium carbonate salt solution system or similar weakly alkaline system under loose condition.
For this reason, the invention provides a kind of pretreatment process of tungsten mineral material, comprise the following steps:
Raw material are prepared, by tungsten mineral material and a certain amount of calcareous material and mineralizer through being mixed and finely ground acquisition raw material;
The raw material prepared are carried out roasting, obtain grog by sinter leaching.
During raw material preparation, the add-on of calcareous material is at least and generates Ca by the tungsten in tungsten mineral material 3wO 6and/or Ca 2feWO 6and/or Ca 2mnWO 61.0 times of theoretical amount, the 1.1-1.5 being preferably theoretical amount doubly, is more preferably 1.2 times;
During raw material preparation, the mineralizer allocated into is fluorochemical, is preferably Calcium Fluoride (Fluorspan), and the add-on of Calcium Fluoride (Fluorspan) is the 0.5-7% (mass percent) of dry tungsten mineral material amount, preferred 1-3% (mass percent); Raw material granularity is less than 150 μm, is preferably less than 45 μm;
Raw material maturing temperature is not less than 500 DEG C, and preferably, raw material maturing temperature is 800-1050 DEG C, is more preferably 850-950 DEG C;
Preferably, in raw material process for preparation, add mineralizer, be preferably Calcium Fluoride (Fluorspan), to accelerate the reaction between tungsten mineral material and batching, significantly reduce maturing temperature;
Roasting time is not particularly limited, and is fully converted into Ca for making the tungsten in raw material 3wO 6and/or Ca 2feWO 6and/or Ca 2mnWO 6, temperature is low, needs to extend roasting time, and being preferably roasting time is 0.5-8.0h, is preferably 1.0 ~ 3.0h, more preferably roasting 1.0 ~ 2.0h at 850 ~ 950 DEG C.
For sheelite raw material, calcination atmosphere is not particularly limited, and is preferably neutral or oxidizing atmosphere; For wolframite, Scheelite-Wolframite Mixed Mine and/or tungsten slurry raw material, calcination atmosphere is neutral or weak reducing atmosphere, is preferably neutral atmosphere.
According to the present invention, have the following advantages: wide adaptability, this method all can be adopted to carry out pre-treatment to all tungsten mineral materials, be particularly useful for processing sheelite; The calcareous material added cheaply is easy to get; The mineralizer added significantly can reduce maturing temperature and shorten roasting time, and maturing temperature is low, simple to operate, is easy to industrial application; Tungsten in gained grog has good leaching performance, can fully leach by ammonium carbonate salt solution at a lower temperature, is conducive to the circulation realizing solution in APT production process economically, thus eliminates the discharge of waste water in production process.
Accompanying drawing explanation
Fig. 1 is the pretreated system architecture schematic diagram of tungsten mineral material according to the present invention.
Embodiment
Below, will in conjunction with specific embodiments, the present invention will be described further.
As shown in Figure 1, raw material preparation facilities 10 has raw mineral materials dosage entrance 11 and dosage entrance 12 (being preferably also provided with mineralising dosage entrance 13), raw material fine mill (containing vortex mixer) 14, raw material outlet 15 and leached mud receiving port 16; Roasting kiln (stove) 20 exports 15 through feeding measurement device with raw material silo and raw material and is communicated with, and has heating unit, attemperator (preferably also comprising refrigerating unit 21) and thick grog outlet 22; Grog fine mill 30 exports 22 through grog storehouse with thick grog and is communicated with, and has ore grinding device and thin grog outlet 31; Leaching device 40 and thin grog outlet 31, there is leaching ore deposit agent entrance 41, leaching slurry outlet 42, feedback gas recovery port, solution recovery port, slag phase washings recovery port 45, crystal seed entrance (preferably, also comprise commercial carbon dioxide and pass into mouth 47) for separating of washing.
According to the present invention, the preprocessing process of tungsten mineral material also comprises:
Raw material preparation controller 100, wherein, under the control of proportion scale controller 101, by tungsten mineral material (sheelite, wolframite, Scheelite-Wolframite Mixed Mine and/or tungsten slurry) and a certain amount of calcareous material and mineralizer through being mixed and finely ground (in other examples, also can levigate after remix even), to obtain raw material.
The raw material prepared, under the effect of maturing temperature controller 401, are carried out roasting, obtain grog by sinter leaching controller 400.Raw material preparation controller 100 makes the add-on of calcareous material be at least by generation Ca 3wO 6and/or Ca 2feWO 6and/or Ca 2mnWO 61.0 times of theoretical amount, are preferably 1.1-1.5 doubly, are more preferably 1.2 times.
When raw material are prepared, the mineralizer allocated into is fluorochemical, is preferably Calcium Fluoride (Fluorspan).Raw material preparation controller 100 makes the add-on of described mineralizer be the 0.5-7% (mass percent) of dry tungsten mineral material amount quality, is preferably 1-3%.
Raw material preparation controller 100 has raw mill fine granularity controller 102, and the granularity making raw material levigate is less than 150 μm, is preferably less than 45 μm.
Sinter leaching controller 200 has maturing temperature controller 201, makes maturing temperature be not less than 500 DEG C, is preferably not less than 800 DEG C (maturing temperature is 800 ~ 1050 DEG C, is preferably 850 ~ 950 DEG C).
Sinter leaching controller 200 has roasting time controller 202, makes roasting time be 0.5-8.0h, is preferably raw material roasting 1.0 ~ 3.0h at 850 ~ 950 DEG C.
Sinter leaching controller 200 has calcination atmosphere controller 203, makes: for sheelite raw material, calcination atmosphere is not particularly limited, and is preferably neutral or oxidizing atmosphere; For wolframite, Scheelite-Wolframite Mixed Mine and/or tungsten slurry raw material, calcination atmosphere is neutral or weak reducing atmosphere, is preferably neutral atmosphere.
According to the present invention, to contain (AO) x(WO 3) y(BO) zthe target product (i.e. grog) that transforms as pre-treatment of material, wherein A, B are divalent metal element, (x+z)/y=3, preferably, x=3, y=1, z=0; Or, x=2, y=1, z=1.
Grog Task-size Controlling device 401 makes the granularity of grog be not more than 200 μm, is preferably less than 45 μm.
Seed charge controller 402 makes Seed charge be 0-15g/L, and preferred Seed charge is 10g/L, and crystal seed is carbonate, preferred calcium carbonate or the material containing calcium carbonate.
The selection principle of leaching agent solution at least comprises: with in the reactant of described raw material containing the material again synthesizing this leaching agent can be participated in, leaching agent itself contains NH 4 +, concentration is greater than 10g-NH 4 +/ 100g-H 2o.
Leaching agent add-on controller 403 makes leaching agent add-on be at least to make AO and BO in grog to be converted into 1.0 times of corresponding difficulty soluble salt aequum (theoretical amount), described volatile salt-bicarbonate of ammonia and volatile salt-ammonium tungstate-ammonium bicarbonate soln system, bicarbonate of ammonia add-on is at least 1.0 times of theoretical amount, is preferably 1.1 ~ 1.4 times.
Leaching pH value controller 404 makes Leaching Systems pH be not less than 8.
Leach in confined conditions, absolute pressure controller 405 makes the absolute pressure of Leaching Systems be not less than 1atm, and the absolute pressure of Leaching Systems is preferably 1.5-2.5atm, is more preferably 2atm.
Extraction temperature controller 406 makes extraction temperature be 15 ~ 100 DEG C, is more preferably 30 ~ 50 DEG C.
Extraction time controller makes extraction time be 0.1 ~ 10.0h, is more preferably 0.5 ~ 4.0h.
Initial liquid-solid ratio controller 407 makes the initial liquid-solid ratio of Leaching Systems be not less than 1:1mL/g, is preferably 10:1-4:1mL/g.
The mode of being fed in raw material by multistage reduces the final liquid-solid ratio of Leaching Systems, and after having leached, leaching slurry, through separating, washing, obtains ammonium tungstate solution.Preferably, fed in raw material by two sections, the liquid-solid ratio controlling final Leaching Systems is 3:1 ~ 4:1mL/g.
In the present invention, after pretreatment, tungsten is wherein converted into Ca to tungsten mineral material 3wO 6and/or Ca 2feWO 6and/or Ca 2mnWO 6, become in sodium carbonate or ammonium carbonate salt solution and there is good leaching performance.
Following reaction adds Wingdale for example, and schematically the tungsten of setting forth in tungsten mineral material of the present invention changes Ca in preprocessing process 3wO 6ultimate principle:
CaWO 4+2CaCO 3＝Ca 3WO 6+2CO 2
CaWO 4+2CaCO 3+FeS＝Ca 2FeWO 6+CaS+2CO 2
FeWO 4+2CaCO 3＝Ca 2FeWO 6+2CO 2
MnWO 4+2CaCO 3＝Ca 2MnWO 6+2CO 2
embodiment 1:
By certain sheelite (WO 3mass percentage is 49.53%, Fe mass percentage is 0.57%), generate Ca by tungsten 3wO 6allocate calcium carbonate into, and allocate the Calcium Fluoride (Fluorspan) of sheelite amount 2% into for 1.1 times of theoretical amount, carry out being mixed and finely ground and cross 325 mesh sieves (granularity <45 μm) and obtain raw material.Then, in stoving oven, under air atmosphere, 800 DEG C of roasting 2.0h, obtain grog, and its X-ray diffraction analysis result shows, the tungstenic thing existed in grog only has Ca mutually 3wO 6.
embodiment 2:
By certain sheelite (WO 3mass percentage is 49.53%, Fe mass percentage is 0.57%), by generating Ca 3wO 6allocate calcium carbonate into, after carrying out levigate mixing, obtain raw material for 1.1 times of theoretical amount, and cross 325 mesh sieves.Then, in stoving oven, under air atmosphere, 800 DEG C of roasting 2.0h, obtain grog, and its X-ray diffraction analysis result shows, the tungstenic thing existed in grog has Ca mutually 3wO 6and CaWO 4.
embodiment 3:
By certain sheelite (WO 3mass percentage is 49.53%, Fe mass percentage is 0.57%), by generating Ca 3wO 6allocate calcium carbonate into, and allocate the Calcium Fluoride (Fluorspan) of sheelite amount 7% into, after carrying out levigate mixing, obtain raw material for 1.3 times of theoretical amount, and cross 200 mesh sieves.Then, in stoving oven, under oxidizing atmosphere, 850 DEG C of roasting 1.5h, obtain grog, and its X-ray diffraction analysis result shows, the tungstenic thing existed in grog only has Ca mutually 3wO 6.
embodiment 4:
By certain sheelite (WO 3mass percentage is 60.34%, Fe mass percentage is 4.73%), by generating Ca 3wO 6and Ca 2feWO 6allocate calcium oxide into, after carrying out levigate mixing, obtain raw material for 1.5 times of theoretical amount, and cross 325 mesh sieves.Then, in stoving oven, under weak reducing atmosphere, 950 DEG C of roasting 4.0h, obtain grog, and its X-ray diffraction analysis result shows, the tungstenic thing existed in grog only has Ca mutually 3wO 6and Ca 2feWO 6.
embodiment 5:
By certain Scheelite-Wolframite Mixed Mine (WO 3mass percentage is 58.70%, Fe mass percent is 9.39%), by generating Ca 3wO 6and Ca 2feWO 6allocate calcium hydroxide into for 1.1 times of theoretical amount, and allocate the Calcium Fluoride (Fluorspan) of tungsten ore amount 3% into, raw material are obtained after carrying out levigate mixing, then, move in stoving oven, under neutral atmosphere, roasting 2.0h at 850 DEG C, obtain grog, its X-ray diffraction analysis result shows, the tungstenic thing existed in grog only has Ca mutually 3wO 6and Ca 2feWO 6.
embodiment 6:
By certain black tungsten composite ore (WO 3mass percentage is 60.15%, Fe mass percent is 16.62%), by generating Ca 2feWO 6allocate calcium carbonate into for 1.1 times of theoretical amount, and allocate the Calcium Fluoride (Fluorspan) of tungsten ore amount 1% into, raw material are obtained after carrying out levigate mixing, then, move in stoving oven, under weak reducing atmosphere, roasting 2.0h at 850 DEG C, obtain grog, its X-ray diffraction analysis result shows, the tungstenic thing existed in grog only has Ca mutually 2feWO 6.
embodiment 7:
By certain sheelite (WO 3mass percentage is 49.53%, Fe mass percentage is 0.57%), by generating Ca 3wO 6allocate calcium carbonate into, after carrying out levigate mixing, obtain raw material for 1.0 times of theoretical amount, and cross 325 mesh sieves.Then, in stoving oven, under oxidizing atmosphere, 500 DEG C of roasting 8.0h, obtain grog, and its X-ray diffraction analysis result shows, the thing existed in grog has Ca mutually 3wO 6, CaWO 4and CaCO 3.
embodiment 8:
By certain sheelite (WO 3mass percentage is 60.14%, Fe mass percentage is 0.28%), by generating Ca 3wO 6allocate calcium carbonate into, after carrying out levigate mixing, obtain raw material for 1.2 times of theoretical amount, and cross 100 mesh sieves.Then, in stoving oven, under neutral atmosphere, 750 DEG C of roasting 2.0h, obtain grog, and its X-ray diffraction analysis result shows, the thing existed in grog has Ca mutually 3wO 6, CaWO 4and CaCO 3.
embodiment 9:
By certain sheelite (WO 3mass percentage is 60.14%, Fe mass percentage is 0.28%), by generating Ca 3wO 6allocate calcium carbonate into, after carrying out levigate mixing, obtain raw material for 1.1 times of theoretical amount, and cross 325 mesh sieves.Then, in stoving oven, under reducing atmosphere, 1050 DEG C of roasting 0.5h, obtain grog, and its X-ray diffraction analysis result shows, the tungstenic thing existed in grog is Ca mutually 3wO 6.
Embodiment 10:
By certain tungsten slurry (WO 3mass percentage is 16.22%, Fe mass percentage is 7.85%) by generating Ca 3wO 6and Ca 2feWO 6allocate calcium carbonate into for 1.1 times of theoretical amount, allocate the Calcium Fluoride (Fluorspan) of tungsten slurry amount 5% into simultaneously, raw material are obtained after carrying out levigate mixing, and cross 325 mesh sieves (raw material granularity≤45 μm), then, roasting 3h at stoving oven reducing atmosphere 940 DEG C, obtains grog, its X-ray diffraction analysis result shows, the tungstenic thing existed in grog has Ca mutually 3wO 6and Ca 2feWO 6.
embodiment 11:
By certain sheelite (WO 3mass percentage is 60.14%, Fe mass percentage is 0.28%), by generating Ca 3wO 6and Ca 2feWO 6allocate calcium carbonate and spathic iron ore into, add the Calcium Fluoride (Fluorspan) of sheelite quality 5%, after carrying out levigate mixing, obtain raw material for 1.2 times of theoretical amount, and cross 100 mesh sieves (raw material granularity≤150 μm).Then, in stoving oven, under neutral atmosphere, 850 DEG C of roasting 4.0h, obtain grog, and its X-ray diffraction analysis result shows, the tungstenic thing existed in grog has Ca mutually 3wO 6and Ca 2feWO 6.
embodiment 12:
By certain Scheelite-Wolframite Mixed Mine (WO 3mass percentage is 58.70%, Fe mass percent is 9.39%), by generating Ca 3wO 6and Ca 2feWO 6allocate calcium carbonate into for 2.0 times of theoretical amount, and allocate the Calcium Fluoride (Fluorspan) of tungsten ore amount 0.5% into, raw material are obtained after carrying out levigate mixing, then, move in stoving oven, under weak reducing atmosphere, roasting 2.0h at 850 DEG C, obtain grog, its X-ray diffraction analysis result shows, the tungstenic thing existed in grog only has Ca mutually 3wO 6and Ca 2feWO 6.
embodiment 13:
By certain white tungsten composite ore (WO 3mass percentage is 52.90%), by generating Ca 3wO 6and Ca 2feWO 6and Ca 2mnWO 6allocate calcium carbonate, spathic iron ore and rhodochrosite into for 1.2 times of theoretical amount, and allocate the Calcium Fluoride (Fluorspan) of tungsten ore amount 2% into, raw material are obtained after carrying out levigate mixing, then, move in stoving oven, under weak reducing atmosphere, roasting 2.0h at 850 DEG C, obtain grog, its X-ray diffraction analysis result shows, the tungstenic thing existed in grog only has Ca mutually 3wO 6, Ca 2feWO 6and Ca 2mnWO 6
embodiment 14:
Take the grog 5.0g and 50.0g volatile salt that burn till according to the method in embodiment 1, join in the reactor that 50mL deionized water is housed, airtight and unlatching is stirred, at 70 DEG C, react 4h.After reaction terminates, leach ore pulp and adopt vacuum filtration, with pure water filter cake three times.The leaching yield of tungsten is 97.35%.The X-ray diffraction analysis result of leached mud shows, the dominant in leached mud is CaCO mutually 3.
embodiment 15:
Take the grog 5.0g and 12.0g sodium carbonate that burn till according to the method in embodiment 1, join in the reactor that 50mL deionized water is housed, airtight and unlatching is stirred, at 90 DEG C, react 4h.After reaction terminates, leach ore pulp and adopt vacuum filtration, with pure water filter cake three times.The leaching yield of tungsten is 98.50%.The X-ray diffraction analysis result of leached mud shows, the dominant in leached mud is CaCO mutually 3.
embodiment 16:
Take the grog 10.0g and 25.0g volatile salt that burn till according to the method in embodiment 4, join in the reactor that 50mL deionized water is housed, airtight and unlatching is stirred, at 50 DEG C, react 3h.After reaction terminates, leach ore pulp and adopt vacuum filtration, with pure water filter cake three times.The leaching yield of tungsten is 97.96%.The X-ray diffraction analysis result of leached mud shows, the dominant in leached mud is CaCO mutually 3.
It is important to note that above embodiment is only example, in order to the present invention to be described, instead of limit the scope of the invention.It should be appreciated by those skilled in the art: if do not depart from spirit of the present invention and design, the amendment carry out details and the form of technical solution of the present invention and replacement, all within the protection domain of appended claims.

Claims (10)

1. a pretreatment process for tungsten mineral material, is characterized in that, said method comprising the steps of:
Raw material are prepared, and mix, tungsten mineral material (sheelite, wolframite, Scheelite-Wolframite Mixed Mine and/or tungsten slurry) and a certain amount of calcareous material and the levigate extremely suitable granularity of mineralizer to obtain raw material; And
The raw material prepared are carried out roasting, obtain grog by sinter leaching under given conditions.
2. method according to claim 1, is characterized in that, for sheelite raw material, calcination atmosphere is not particularly limited, and is preferably neutral or oxidizing atmosphere; For wolframite, Scheelite-Wolframite Mixed Mine and/or tungsten slurry raw material, calcination atmosphere is neutral or weak reducing atmosphere, is preferably neutral atmosphere; And/or, during raw material preparation, simultaneously containing ferro element and/or manganese element in described calcareous material.
3. method according to claim 1, is characterized in that, when raw material are prepared, the calcareous material allocated into is calcium carbonate or calcium oxide or calcium hydroxide or iron calcium cpd or their any mixture, is preferably calcium carbonate; The mineralizer allocated into is fluorochemical, is preferably Calcium Fluoride (Fluorspan).
4. method according to claim 3, is characterized in that, the add-on of described mineralizer is the 0.5-7% (mass percent) of dry tungsten mineral material amount quality, is preferably 1-3%.
5. method according to claim 1, is characterized in that, described raw material are levigate and mixing process is that various batching is first distinguished levigate rear remix, or by levigate mixing together after various batching mixing; The granularity that raw material are levigate is less than 150 μm, is preferably less than 45 μm.
6. method according to claim 1, is characterized in that, maturing temperature, for being not less than 500 DEG C, is preferably not less than 800 DEG C.
7. method according to claim 1, is characterized in that, maturing temperature is 800 ~ 1050 DEG C, is preferably 850 ~ 950 DEG C.
8. method according to claim 1, is characterized in that, roasting time is 0.5-8.0h, is preferably 1.0-3.0h.
9. method according to claim 1, is characterized in that, raw material are roasting 1.0 ~ 2.0h at 850-950 DEG C.
10. method according to claim 1, is characterized in that, during raw material preparation, the add-on of calcareous material is at least and generates Ca by the tungsten in tungsten mineral material 3wO 6and/or Ca 2feWO 6and/or Ca 2mnWO 61.0 times of theoretical amount, are preferably 1.1-1.5 doubly, are more preferably 1.2 times.
CN201410527644.6A 2014-10-09 2014-10-09 A kind of preprocess method of tungsten mineral material Active CN104232942B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410527644.6A CN104232942B (en) 2014-10-09 2014-10-09 A kind of preprocess method of tungsten mineral material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410527644.6A CN104232942B (en) 2014-10-09 2014-10-09 A kind of preprocess method of tungsten mineral material

Publications (2)

Publication Number Publication Date
CN104232942A true CN104232942A (en) 2014-12-24
CN104232942B CN104232942B (en) 2016-07-13

Family

ID=52221831

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410527644.6A Active CN104232942B (en) 2014-10-09 2014-10-09 A kind of preprocess method of tungsten mineral material

Country Status (1)

Country Link
CN (1) CN104232942B (en)

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104805314A (en) * 2015-05-13 2015-07-29 中南大学 Method for extracting tungsten from raw materials containing wolframite
CN104843791A (en) * 2015-05-06 2015-08-19 江西稀有金属钨业控股集团有限公司 Tungsten-contained material treating method
CN104878223A (en) * 2015-05-13 2015-09-02 中南大学 Method for extracting tungsten from wolframite or scheelite and wolframite mixed ores
CN105112691A (en) * 2015-10-10 2015-12-02 江西理工大学 Method for extracting tungsten from tungsten minerals through alkaline decomposition
CN105907993A (en) * 2016-07-05 2016-08-31 江西理工大学 Method for extracting tungsten from fluorine-containing scheelite
CN105969977A (en) * 2016-07-05 2016-09-28 江西理工大学 Method for extracting tungsten from scheelite
CN106011504A (en) * 2016-07-05 2016-10-12 江西理工大学 Method for resolving scheelite
CN106587158A (en) * 2016-12-14 2017-04-26 衡阳市南东有色金属有限公司 Method for highly-efficient and environmentally-friendly production of ammonium paratungstate through using low-degree tungstic acid and alkali
CN106636681A (en) * 2016-11-23 2017-05-10 江西稀有金属钨业控股集团有限公司 Tungsten-contained raw ore pretreatment system for realizing green metallurgy
CN109439929A (en) * 2018-12-17 2019-03-08 江西理工大学 A kind of method that alkaline system decomposes Scheelite-Wolframite Mixed Mine
CN113428902A (en) * 2021-07-09 2021-09-24 崇义章源钨业股份有限公司 Method for preparing ammonium paratungstate
CN113737027A (en) * 2021-08-19 2021-12-03 长沙矿冶研究院有限责任公司 Method for recovering valuable metal from tungsten-containing slag
CN115055263A (en) * 2022-06-01 2022-09-16 浙江艾领创矿业科技有限公司 Fine grinding process for tungsten-containing mineral

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102649995A (en) * 2012-05-24 2012-08-29 崇义章源钨业股份有限公司 Method for transforming wolframite into scheelite
CN103614545A (en) * 2013-11-22 2014-03-05 中南大学 Method for treating low-grade tungsten concentrate and tungsten slag

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102649995A (en) * 2012-05-24 2012-08-29 崇义章源钨业股份有限公司 Method for transforming wolframite into scheelite
CN103614545A (en) * 2013-11-22 2014-03-05 中南大学 Method for treating low-grade tungsten concentrate and tungsten slag

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104843791A (en) * 2015-05-06 2015-08-19 江西稀有金属钨业控股集团有限公司 Tungsten-contained material treating method
CN104878223A (en) * 2015-05-13 2015-09-02 中南大学 Method for extracting tungsten from wolframite or scheelite and wolframite mixed ores
CN104805314A (en) * 2015-05-13 2015-07-29 中南大学 Method for extracting tungsten from raw materials containing wolframite
CN105112691A (en) * 2015-10-10 2015-12-02 江西理工大学 Method for extracting tungsten from tungsten minerals through alkaline decomposition
CN105907993B (en) * 2016-07-05 2018-01-02 江西理工大学 A kind of method that tungsten is extracted from fluorine-containing scheelite
CN105907993A (en) * 2016-07-05 2016-08-31 江西理工大学 Method for extracting tungsten from fluorine-containing scheelite
CN105969977A (en) * 2016-07-05 2016-09-28 江西理工大学 Method for extracting tungsten from scheelite
CN106011504A (en) * 2016-07-05 2016-10-12 江西理工大学 Method for resolving scheelite
CN105969977B (en) * 2016-07-05 2018-06-22 江西理工大学 A kind of method that tungsten is extracted from scheelite
CN106636681A (en) * 2016-11-23 2017-05-10 江西稀有金属钨业控股集团有限公司 Tungsten-contained raw ore pretreatment system for realizing green metallurgy
CN106587158A (en) * 2016-12-14 2017-04-26 衡阳市南东有色金属有限公司 Method for highly-efficient and environmentally-friendly production of ammonium paratungstate through using low-degree tungstic acid and alkali
CN109439929A (en) * 2018-12-17 2019-03-08 江西理工大学 A kind of method that alkaline system decomposes Scheelite-Wolframite Mixed Mine
CN109439929B (en) * 2018-12-17 2020-07-28 江西理工大学 Method for decomposing wolframite and wolframite mixed ore by alkaline system
CN113428902A (en) * 2021-07-09 2021-09-24 崇义章源钨业股份有限公司 Method for preparing ammonium paratungstate
CN113737027A (en) * 2021-08-19 2021-12-03 长沙矿冶研究院有限责任公司 Method for recovering valuable metal from tungsten-containing slag
CN115055263A (en) * 2022-06-01 2022-09-16 浙江艾领创矿业科技有限公司 Fine grinding process for tungsten-containing mineral

Also Published As

Publication number Publication date
CN104232942B (en) 2016-07-13

Similar Documents

Publication Publication Date Title
CN104232942A (en) Pretreatment method of tungsten mineral materials
CN104805314A (en) Method for extracting tungsten from raw materials containing wolframite
CN102627305A (en) Method using alkaline process to extract alumina in coal ash
CN105925823A (en) Method for processing scheelite concentrate through sulfuric acid to prepare tungstate solution
CN104818395A (en) Method for treating wolframite ore or scheelite and wolframite mixed ore
CN104263973B (en) The method being prepared APT by the many closed loops of tungsten mineral material
CN105925822A (en) Method for processing scheelite concentrate through sulfuric acid to prepare tungstate solution
CN204162450U (en) A kind of system preparing ammonium tungstate solution
CN103112963B (en) Acidolysis laterite nickel ore wastewater treatment and slag utilization method
CN104928502A (en) Method for extracting tungsten from wolframite or scheelite and wolframite mixture ore through adding of high-phosphorus scheelite
CN104263975B (en) There is the tungsten mineral material metallurgical technology of multiple closed loop
CN104878223B (en) A kind of method that tungsten is extracted from wolframite or Scheelite-Wolframite Mixed Mine
CN108752005A (en) The technique that a kind of ardealite and red mud prepare composite ceramic material co-producing sulfuric acid
CN104263976B (en) The tungsten mineral material metallurgical technology of omnidistance non-pollution discharge
CN204401085U (en) A kind of pretreatment system of tungsten mineral material
CN101008047A (en) Method for electrolyzing vanadium slurry and extracting vanadium pentexide using film
CN104263972B (en) There is the tungsten mineral material metallurgical system of multiple closed loop
CN204162765U (en) The metallurgical system of the tungsten mineral material of omnidistance non-pollution discharge
CN204162756U (en) The metallurgical system of the tungsten mineral material of no pollution discharge can be realized
CN102115813B (en) Comprehensive utilization method for low-grade magnesite
CN104263971B (en) The system of APT is prepared by tungsten mineral material no pollution
CN104388670B (en) The tungsten mineral material metallurgical system of omnidistance non-pollution discharge
CN108275714A (en) A kind of method that sodium chloride-ammonia joint leaches production feed grade zinc oxide
CN104386754A (en) Technology for preparing ammonium tungstate solution
RU2657149C1 (en) Method of rare earth metals and scandium extraction from slag wastes

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant