CN108411127A - The restoring method of niobium concentrate miberal powder - Google Patents
The restoring method of niobium concentrate miberal powder Download PDFInfo
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- CN108411127A CN108411127A CN201810300882.1A CN201810300882A CN108411127A CN 108411127 A CN108411127 A CN 108411127A CN 201810300882 A CN201810300882 A CN 201810300882A CN 108411127 A CN108411127 A CN 108411127A
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- niobium concentrate
- crucible
- reducing agent
- miberal powder
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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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention provides a kind of restoring method of niobium concentrate miberal powder, including：Niobium concentrate miberal powder and reducing agent are dried；The reducing agent for the preset thickness that tiles in crucible bottom, is then divided into three inner ring, middle ring and outer shroud parts by the space in crucible, reducing agent is filled in inner ring and outer rings, in middle ring filling niobium concentrate miberal powder；The space that reducing agent fills the space of remaining inner ring, the space of middle ring and outer shroud is extremely concordant with crucible opening face, covers crucible cover；Crucible is put in micro-wave oven, microwave heating is started；Obtain reduction niobium concentrate.Technical solution through the invention, replace traditional heating mode with microwave heating, utilize niobium concentrate and the good microwave absorbing property of carbon, the carbonaceous reducing agents such as niobium concentrate and semicoke, coal dust or coke powder are made to rely on self-heating under microwave field, heat needed for Chemoselective reduction is provided, the selective reduction that iron in niobium concentrate is rapidly completed in good confined reaction tank is being kept the temperature, low energy consumption, at low cost, the time is short, working environment is good.
Description
Technical field
The present invention relates to metallurgical technology fields, in particular to a kind of restoring method of niobium concentrate miberal powder.
Background technology
Currently, the technique for smelting ferrocolumbium is broadly divided into three steps, i.e. " niobium concentrate selective reduction-richness niobium slag melting-niobium
The method of ferroalloy smelting ", the technique niobium concentrate miberal powder selective reduction stage is usually following two：
Method one：Before rich niobium slag melting, the metallic iron in lower temperature prereduction niobium concentrate reduces reaction energy
Consumption.But since using the traditional heating mode heated from outside to inside, energy consumption of reaction is still higher, works under hard conditions, also
There are more serious pollution problems.
Method two：By ferro-niobium concentrate powder, coal dust and binder Hybrid Heating briquetting, carried out in rotary hearth furnace or High-temp. kiln
Dry, preheating and selective solid state reduction.The complex operation, briquetting process need to heat, and add additional energy consumption, and
Technique needs reducing agent coal dust to be mixed with ferro-niobium concentrate powder, can reduce the grade of niobium in ferro-niobium concentrate.
Invention content
The present invention is directed to solve at least one of the technical problems existing in the prior art or related technologies.
For this purpose, the object of the present invention is to provide a kind of restoring method of niobium concentrate miberal powder.
In view of this, the technical solution of first aspect present invention provides a kind of restoring method of niobium concentrate miberal powder, including：
Niobium concentrate miberal powder and reducing agent are dried, drying temperature is 100~200 DEG C, 8~12h of drying time；It is flat in crucible bottom
The reducing agent for spreading preset thickness, is then divided into three inner ring, middle ring and outer shroud parts, in inner ring and outer rings by the space in crucible
Fill reducing agent, in middle ring filling niobium concentrate miberal powder, wherein the thickness of feed layer of niobium concentrate miberal powder be crucible internal diameter 20~
25%；The space that reducing agent fills the space of remaining inner ring, the space of middle ring and outer shroud is extremely concordant with crucible opening face, covers
Crucible cover；Crucible is put in micro-wave oven, microwave heating is started, heating temperature is 900~1000 DEG C, keeps the temperature 2.5~4.0h；From
So after cooling, reduction niobium concentrate miberal powder is obtained, wherein reducing agent is carbonaceous reducing agent, and the granularity of carbonaceous reducing agent is 0~2mm.
Further, the material of crucible is silicon carbide or corundum.
Further, carbonaceous reducing agent is one kind or combinations thereof in semicoke, coal dust and coke powder.
Beneficial effects of the present invention are as follows：
Replace traditional heating mode with microwave heating, using niobium concentrate and the good microwave absorbing property of carbon, makes niobium concentrate and half
The carbonaceous reducing agents such as burnt, coal dust or coke powder rely on self-heating under microwave field, provide the heat needed for Chemoselective reduction,
The selective reduction that iron in niobium concentrate is rapidly completed in good confined reaction tank is being kept the temperature, low energy consumption, at low cost, the time is short,
Working environment is good.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obviously, or practice through the invention is recognized.
Description of the drawings
The above-mentioned and/or additional aspect and advantage of the present invention will become in the description from combination following accompanying drawings to embodiment
Obviously and it is readily appreciated that, wherein：
Fig. 1 shows the flow diagram of the restoring method of niobium concentrate miberal powder according to an embodiment of the invention；
Specific implementation mode
It is below in conjunction with the accompanying drawings and specific real in order to be more clearly understood that aforementioned aspect of the present invention, feature and advantage
Mode is applied the present invention is further described in detail.It should be noted that in the absence of conflict, the implementation of the application
Feature in example and embodiment can be combined with each other.
Many details are elaborated in the following description to facilitate a thorough understanding of the present invention, still, the present invention may be used also
To be implemented different from other modes described here using other, therefore, protection scope of the present invention is not by described below
Specific embodiment limitation.
Embodiment 1：
As shown in Figure 1, the restoring method of niobium concentrate miberal powder according to an embodiment of the invention, including：Step S102, by niobium
Concentrate miberal powder and reducing agent are dried, and drying temperature is 100~200 DEG C, 8~12h of drying time；Step S1044, in crucible
The reducing agent of bottom tiling preset thickness, is then divided into three inner ring, middle ring and outer shroud parts, in inner ring by the space in crucible
With outer ring filling reducing agent, in middle ring filling niobium concentrate miberal powder, wherein the thickness of feed layer of niobium concentrate miberal powder be crucible internal diameter 20
~25%；Step S106, the space that reducing agent fills the space of remaining inner ring, the space of middle ring and outer shroud are open to crucible
Face is concordant, covers crucible cover；Step S108, crucible is put in micro-wave oven, start microwave heating, heating temperature be 900~
1000 DEG C, keep the temperature 2.5~4.0h；Step S110 after natural cooling, obtains reduction niobium concentrate miberal powder, wherein reducing agent is carbonaceous
The granularity of reducing agent, carbonaceous reducing agent is 0~2mm.
Replace traditional heating mode with microwave heating, using niobium concentrate and the good microwave absorbing property of carbon, makes niobium concentrate and half
The carbonaceous reducing agents such as burnt, coal dust or coke powder rely on self-heating under microwave field, provide the heat needed for Chemoselective reduction,
The selective reduction that iron in niobium concentrate is rapidly completed in good confined reaction tank is being kept the temperature, low energy consumption, at low cost, the time is short,
Working environment is good.The thickness of feed layer of niobium concentrate miberal powder is the 20~25% of crucible internal diameter, and the surrounding of niobium concentrate miberal powder is by carbon
Matter reducing agent is covered, and the heat that carbonaceous reducing agent generates fully influences niobium concentrate miberal powder, and niobium concentrate miberal powder is made fully to restore.
Embodiment 2：
1) the present embodiment is raw materials used
Niobium concentrate：Using niobium concentrate miberal powder of the Bayan Obo tailing after sorting enrichment, main chemical compositions (wt%):
Nb2O55.1、FeO1.2、TFe42.2、TiO28.24、SiO221.87、CaO1.34、F0.85。
Coke powder：Fixed carbon content 69.39wt%, ash content 17.22wt%, volatile matter 12.6wt%, 0~2mm of granularity.
2) feedstock processing
Niobium concentrate miberal powder and coke powder are dried in drying box, drying temperature is 120 DEG C, drying time 10h.
3) it feeds
Crucible used in the present embodiment is crystalline silicon carbide silica crucible, crucible outer diameter 60mm, internal diameter 48mm, high 70mm.When charging
10~12mm of niobium concentrate thickness of feed layer is controlled, corresponding charging quality is 58~67g.
Crystalline silicon carbide crucible bottom tile 5mm thickness coke powder, then by the space in crucible be divided into inner ring, middle ring and
Three parts of outer shroud, the ring filling 58g niobiums concentrate miberal powder in crucible, crucible inner ring, outer shroud and remaining space are filled completely with coke powder,
Cover crucible cover.
4) microwave carbon thermal reduction
Charged crucible is placed in micro-wave oven, microwave heating is started, temperature is risen to 900 DEG C, is reacted after keeping the temperature 4h
Terminate, is taken out after natural cooling.Reduction niobium concentrate 48.8g, average assay Nb is obtained2O5Content 6.09wt%, FeO content
11.6wt%, MFe content 50.1wt%.
Embodiment 3：
1) the present embodiment is raw materials used
Niobium concentrate：Using niobium concentrate miberal powder of the Bayan Obo tailing after sorting enrichment, main chemical compositions (wt%):
Nb2O55.1、FeO1.2、TFe42.2、TiO28.24、SiO221.87、CaO1.34、F0.85。
Coke powder：Fixed carbon content 69.39wt%, ash content 17.22wt%, volatile matter 12.6wt%, 0~2mm of granularity.
2) feedstock processing
Niobium concentrate miberal powder and coke powder are dried in drying box, drying temperature is 120 DEG C, drying time 10h.
3) it feeds
Crucible used in the present embodiment is crystalline silicon carbide silica crucible, crucible outer diameter 60mm, internal diameter 48mm, high 70mm.When charging
10~12mm of niobium concentrate thickness of feed layer is controlled, corresponding charging quality is 58~67g.
Crystalline silicon carbide crucible bottom tile 5mm thickness coke powder, then by the space in crucible be divided into inner ring, middle ring and
Three parts of outer shroud, the ring filling 62g niobiums concentrate miberal powder in crucible, crucible inner ring, outer shroud and remaining space are filled completely with coke powder,
Cover crucible cover.
4) microwave carbon thermal reduction
Charged crucible is placed in micro-wave oven, microwave heating is started, temperature is risen to 950 DEG C, is reacted after keeping the temperature 3h
Terminate, is taken out after natural cooling.Reduction niobium concentrate 50.2g, average assay Nb is obtained2O5Content 6.5wt%, FeO content
9.18wt%, MFe content 51.1wt%.
Embodiment 4：
1) the present embodiment is raw materials used
Niobium concentrate：Using niobium concentrate miberal powder of the Bayan Obo tailing after sorting enrichment, main chemical compositions (wt%):
Nb2O55.1、FeO1.2、TFe42.2、TiO28.24、SiO221.87、CaO1.34、F0.85。
Coke powder：Fixed carbon content 69.39wt%, ash content 17.22wt%, volatile matter 12.6wt%, 0~2mm of granularity.
2) feedstock processing
Niobium concentrate miberal powder and coke powder are dried in drying box, drying temperature is 120 DEG C, drying time 10h.
3) it feeds
Crucible used in the present embodiment is crystalline silicon carbide silica crucible, crucible outer diameter 60mm, internal diameter 48mm, high 70mm.When charging
10~12mm of niobium concentrate thickness of feed layer is controlled, corresponding charging quality is 58~67g.
Crystalline silicon carbide crucible bottom tile 5mm thickness coke powder, then by the space in crucible be divided into inner ring, middle ring and
Three parts of outer shroud, the ring filling 67g niobiums concentrate miberal powder in crucible, crucible inner ring, outer shroud and remaining space are filled completely with coke powder,
Cover crucible cover.
4) microwave carbon thermal reduction
Charged retort is placed in micro-wave oven, microwave heating is started, temperature is risen to 1000 DEG C, after keeping the temperature 2.5h
Reaction terminates, and is taken out after natural cooling.Reduction niobium concentrate 55.8g, average assay Nb is obtained2O5Content 6.26wt%, FeO contain
Measure 10.2wt%, MFe contents 50.67wt%.
Above in association with technical scheme of the present invention has been illustrated, technical solution through the invention is taken with microwave heating
Make the carbonaceous such as niobium concentrate and semicoke, coal dust or coke powder also using niobium concentrate and the good microwave absorbing property of carbon for traditional heating mode
Former agent relies on self-heating under microwave field, provides the heat needed for Chemoselective reduction, is keeping the temperature good confined reaction
The selective reduction of iron in niobium concentrate is rapidly completed in tank, low energy consumption, at low cost, the time is short, working environment is good.
In the description of this specification, the description of term " one embodiment ", " some embodiments ", " specific embodiment " etc.
Mean that particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one reality of the present invention
It applies in example or example.In the present specification, schematic expression of the above terms are not necessarily referring to identical embodiment or reality
Example.Moreover, description particular features, structures, materials, or characteristics can in any one or more of the embodiments or examples with
Suitable mode combines.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of restoring method of niobium concentrate miberal powder, which is characterized in that including：
The niobium concentrate miberal powder and reducing agent are dried, drying temperature is 100~200 DEG C, 8~12h of drying time；
Crucible bottom tile preset thickness the reducing agent, then by the space in the crucible be divided into inner ring, middle ring and
Three parts of outer shroud, in the inner ring and the outer ring filling reducing agent, the niobium concentrate miberal powder described in the middle ring filling,
In, the thickness of feed layer of the niobium concentrate miberal powder is the 20~25% of the crucible internal diameter；
The reducing agent fill the space in the space of the remaining inner ring, the space of the middle ring and the outer shroud to and crucible
Opening face is concordant, covers crucible cover；
The crucible is put in micro-wave oven, microwave heating is started, heating temperature is 900~1000 DEG C, keeps the temperature 2.5~4.0h；
After natural cooling, reduction niobium concentrate miberal powder is obtained,
Wherein, the reducing agent is carbonaceous reducing agent, and the granularity of the carbonaceous reducing agent is 0~2mm.
2. the restoring method of niobium concentrate miberal powder according to claim 1, which is characterized in that the material of the crucible is carbonization
Silicon or corundum.
3. the restoring method of niobium concentrate miberal powder according to claim 1, which is characterized in that the carbonaceous reducing agent is half
One kind or combinations thereof in burnt, coal dust and coke powder.
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| CN201810300882.1A CN108411127A (en) | 2018-04-04 | 2018-04-04 | The restoring method of niobium concentrate miberal powder |
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| CN201810300882.1A CN108411127A (en) | 2018-04-04 | 2018-04-04 | The restoring method of niobium concentrate miberal powder |
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Citations (6)
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|---|---|---|---|---|
| CN101157961A (en) * | 2007-11-06 | 2008-04-09 | 东北大学 | Preparation method for producing low-grade ferroniobium by using ferroniobium concentrate |
| CN102168173A (en) * | 2011-03-29 | 2011-08-31 | 内蒙古科技大学 | Method for extracting niobium from tailings |
| CN102994738A (en) * | 2012-12-06 | 2013-03-27 | 内蒙古科技大学 | Method for preparing niobium-enriched ore by employing X-fluorescence sorting-microwave carbon thermal reduction |
| CN103160864A (en) * | 2013-03-25 | 2013-06-19 | 上海大学 | Method for preparing niobium-iron alloy by electrolysis of molten salts of niobium concentrate |
| BR102012027128A2 (en) * | 2012-10-23 | 2014-07-15 | Univ Sao Paulo | PROCESS FOR PRODUCTION OF REFINED CONCENTRATE OF NIOBIO ORE; NIOBIO ORE CONCENTRATE AGGLOMERATES; AND PROCESS FOR PRODUCTION OF NIOBIO ORE CONCENTRATE AGGLOMERATES |
| CN104498737A (en) * | 2014-12-31 | 2015-04-08 | 包钢集团矿山研究院（有限责任公司） | Method for enriching niobium by high-temperature roasting and low-intensity magnetic separation |
-
2018
- 2018-04-04 CN CN201810300882.1A patent/CN108411127A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157961A (en) * | 2007-11-06 | 2008-04-09 | 东北大学 | Preparation method for producing low-grade ferroniobium by using ferroniobium concentrate |
| CN102168173A (en) * | 2011-03-29 | 2011-08-31 | 内蒙古科技大学 | Method for extracting niobium from tailings |
| BR102012027128A2 (en) * | 2012-10-23 | 2014-07-15 | Univ Sao Paulo | PROCESS FOR PRODUCTION OF REFINED CONCENTRATE OF NIOBIO ORE; NIOBIO ORE CONCENTRATE AGGLOMERATES; AND PROCESS FOR PRODUCTION OF NIOBIO ORE CONCENTRATE AGGLOMERATES |
| CN102994738A (en) * | 2012-12-06 | 2013-03-27 | 内蒙古科技大学 | Method for preparing niobium-enriched ore by employing X-fluorescence sorting-microwave carbon thermal reduction |
| CN103160864A (en) * | 2013-03-25 | 2013-06-19 | 上海大学 | Method for preparing niobium-iron alloy by electrolysis of molten salts of niobium concentrate |
| CN104498737A (en) * | 2014-12-31 | 2015-04-08 | 包钢集团矿山研究院（有限责任公司） | Method for enriching niobium by high-temperature roasting and low-intensity magnetic separation |
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| 刘玉宝等: "包头含铌铁精矿选择性还原试验", 《钢铁》 * |
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