CN107934980A - The method that lepidolite recirculating fluidized bed roasts defluorinate - Google Patents
The method that lepidolite recirculating fluidized bed roasts defluorinate Download PDFInfo
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- CN107934980A CN107934980A CN201711317357.2A CN201711317357A CN107934980A CN 107934980 A CN107934980 A CN 107934980A CN 201711317357 A CN201711317357 A CN 201711317357A CN 107934980 A CN107934980 A CN 107934980A
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- Prior art keywords
- defluorinate
- fluidized bed
- lepidolite
- miberal powder
- recirculating fluidized
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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
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/42—Micas ; Interstratified clay-mica products
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
-
- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
-
- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Abstract
The invention discloses a kind of method of lepidolite recirculating fluidized bed roasting defluorinate, concretely comprise the following steps：By in levigate miberal powder input recirculating fluidized bed, rise with the water vapour of combustion heat gas and introducing and roast defluorinate, then together into the cyclone separator gas solid separation of fluidized bed top horizontal connection, miberal powder enters circulation discharge groove, part miberal powder is blown into circulation roasting defluorinate in fluid bed through air or steam, and remaining miberal powder is discharged into cooling in cooler and obtains defluorinate lepidolite finished product；The tail gas of cyclonic separation enters dust pelletizing system after afterheat steam recovery system lowered temperature reclamation heat, and air is discharged into after finally carrying out tail gas defluorinate.Method of the present invention, lepidolite miberal powder is with high-temperature water vapor haptoreaction in state is fluidized, and temperature control is uniform, defluorinate stabilization is thorough, temperature control is uniform；Flow is simple, and overall process heat is recycled in the form of steam and preheated air, and heat recovery rate is high.
Description
Technical field
The invention belongs to mineral raw material processing technology field, and in particular to a kind of lepidolite recirculating fluidized bed roasts defluorinate
Method.
Background technology
With the development of new and high technology, lithium is led as a kind of New Green Energy source material in electric automobile, lithium ion battery etc.
The extensive use in domain so that the world is in explosive growth to the demand of lithium and its compound.China is enriched containing lithium minerals, such as lithium brightness
Stone, lepidolite.ɑ-spodumene crystal form is easier to extract elemental lithium therein after being converted to β-spodumene.And lepidolite mineral are typical cases
Layered silicate structure mineral, the lithium in ore is embedded in [Si-O] lattice, and contains fluorine in mineral, straight without processing
It is larger to connect the extraction lithium difficulty from lepidolite concentrate, therefore studies lepidolite defluorination method and lithium industry is proposed to follow-up ore with important
Meaning.
The method of lepidolite recirculating fluidized bed roasting defluorinate proposed by the present invention, using coal tar, natural gas, liquefied gas etc.
Alkanes and coke-stove gas are fuel, contain a large amount of vapor in the high-temperature gas of burning so that miberal powder is in recirculating fluidized bed
Begin to carry out defluorination reaction during being brought rapidly up；Waste heat from tail gas after roasting is directly recovered as steam, and energy consumption is low, hot time
High income；And the flow is simple, process resistance is small.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of lepidolite recirculating fluidized bed roasting defluorinate
Method.Put into by the lepidolite after will be broken in recirculating fluidized bed, water steams during lepidolite miberal powder circulates in recirculating fluidized bed
Gas comes into full contact with miberal powder and the reaction time is enough, and miberal powder defluorinate rate is high；High-temperature tail gas heat recovery steam, heat are fully sharp
With heat loss is few, and the utilization rate of the energy is high.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of method of lepidolite recirculating fluidized bed roasting defluorinate, comprises the following steps：
1）Lepidolite ore is milled down to certain particle diameter with pulverizer, obtains lepidolite miberal powder；
2）Lepidolite miberal powder after will be levigate is incorporated into recirculating fluidized bed, the burning with the generation of recirculating fluidized bed combustion bottom burner
Gas and the vapor of introducing carry out defluorinate roasting together, and subsequent miberal powder enters recirculating fluidized bed top water together with thermal current
The cyclone separator of flushconnection carries out gas solid separation；Separated miberal powder enters in circulation discharge groove, with steam or air part
It is incorporated into recirculating fluidized bed and continues defluorinate roasting with the miberal powder newly added, remaining miberal powder is discharged in cooler with sky through discharge groove
Gas is cooled down and recycles heat, obtains defluorinate lepidolite；The separated tail gas of cyclone separator enters afterheat steam recovery system
Cooling, and participate in defluorination reaction in partially recycled water vapour to recirculating fluidized bed；Gas after cooling is removed through cloth bag or electricity
After dirt, into the rear emptying up to standard of tail gas defluorinate system；Collected in afterheat steam recovery system and the sedimentation of cloth bag or electric precipitation
Miberal powder return to recirculating fluidized bed in continue defluorinate roasting.
Step 1）Described in lepidolite ore be milled down to 1000 μm of particle diameter ＜；Lepidolite ore water content ＜ 10wt%, lepidolite
Lithium content >=0.5wt%, fluorinated volume ＞ 0.5wt% are aoxidized in ore deposit.
Step 2）In, miberal powder is consistent with the thermal current direction of motion in fluid bed；It is 700-950 that miberal powder, which is heated to temperature,
℃；Hot gas flow velocity is 0.5-5m/s；The new miberal powder amount being added in recirculating fluidized bed is the miberal powder total amount circulated in fluid bed
3%-20%；The miberal powder amount that continuation defluorinate roasting in recirculating fluidized bed is incorporated into from circulation discharge groove accounts for ore deposit in circulation discharge groove
The 80%-97% of powder amount；Miberal powder mean residence time total in recirculating fluidized bed is 5-50min；Recirculating fluidized bed whirlwind separates
The temperature of defluorinate baking tail gases afterwards is 700-950 DEG C, and into the tail gas of afterheat steam recovery system, to cool to temperature be 150-
300℃；The air roots-type wind turbine being preheated in cooler is introduced into combustion-supporting in burner or is blown into ore deposit in circulation discharge groove
Powder part brings circulation roasting in recirculating fluidized bed into.
Step 2）Fuel in middle burner is one kind or several in coal tar, natural gas, liquefied gas or coke-stove gas
Kind；1.5 wt % of water vapour content ＞ in burning gases；The amount of the vapor of the introducing is lithium cloud in input recirculating fluidized bed
The 0.2-10% of female miberal powder weight；
Handled using this method, obtained lepidolite defluorinate rate ＞ 95%, the heat of roasting process fuel as a vapor and
The form recycling heat of hot-air, heat recovery rate more than 60%.
Compared with prior art, the present invention tool has the advantage that：
Technique of the present invention, using single-stage circulation fluid bed combination waste heat from tail gas recovered steam, lepidolite is ciculation fluidized
Defluorinate is abundant in bed, and easy to control, hot gas heat recovery steam, improves capacity usage ratio, reduce heat loss；Followed with respect to multistage
Ring fluidized system flow is short, it is easier to controls, small investment, process resistance is small, relative to traditional rotary kiln technology, take up little area,
Energy consumption is low, and equipment investment is few, defluorinate is more thorough.
Brief description of the drawings
Fig. 1 is the process flow chart of the present invention, wherein：1, pulverizer；2, recirculating fluidized bed；3, cyclone separator；4th, follow
Ring discharge groove；5, cooler；6, roots-type wind turbine 7, burner；8, afterheat steam recovery system；9, electric precipitation or bag-type dust
Device；10, tail gas defluorinate system.
Embodiment
The present invention further illustrates the present invention with the following example, but protection scope of the present invention is not limited to following reality
Example.
Embodiment 1
A kind of method of lepidolite recirculating fluidized bed roasting defluorinate, concretely comprises the following steps：
By lepidolite ore it is levigate to particle diameter be 80 μm；Then be 8wt% by water content, oxidation lithium content is 0.5wt%, fluorinated volume is
The lepidolite miberal powder of 1.5wt% is put into recirculating fluidized bed, with the hot-air of fluidized-bed bottom burner generation and the water of introducing
Steam rises roasting defluorinate, and water vapour content is 10wt% in burning gases, and the water vapour amount of introducing is in input recirculating fluidized bed
The 2% of lepidolite weight, hot gas flow velocity are 2m/s, and miberal powder is heated to 850 DEG C；Then connect together into fluidized bed top horizontal
The cyclone separator gas solid separation connect, miberal powder are fallen into circulation discharge groove, and 85% miberal powder is blown into fluid bed through air or steam
Circulation roasting, the miberal powder stop reaction time total in recirculating fluidized bed is 40min, and remaining miberal powder, which is discharged into cooler, uses air
Cooling obtains defluorinate lepidolite finished product；The exhaust temperature of cyclonic separation is 850 DEG C, and temperature is cooled into afterheat steam recovery system
Spend for 150 DEG C, after bag-type dust enter tail gas defluorinate system defluorinate it is up to standard after be discharged into air.Whole process lepidolite defluorinate rate
For 97%, heat recovery rate 70%.
Embodiment 2
A kind of method of lepidolite recirculating fluidized bed roasting defluorinate, concretely comprises the following steps：
By lepidolite ore it is levigate to particle diameter be 110 μm；Then be 5wt% by water content, oxidation lithium content is 4.0wt%, fluorinated volume
Put into recirculating fluidized bed for the lepidolite miberal powder of 0.8wt%, hot-air and introducing with the generation of fluidized-bed bottom burner
Water vapour rises roasting defluorinate, and water vapour content is 10wt% in burning gases, and the water vapour amount of introducing is input recirculating fluidized bed
The 8% of interior lepidolite weight, hot gas flow velocity are 3m/s, and miberal powder is heated to 840 DEG C；Then together into fluidized bed top horizontal
The cyclone separator gas solid separation of connection, miberal powder are fallen into circulation discharge groove, and 80% miberal powder is blown into fluid bed through air or steam
Interior circulation roasting, miberal powder stop reaction time total in recirculating fluidized bed are 30min, and remaining miberal powder is discharged into cooler with sky
Air cooling obtains defluorinate lepidolite finished product；The exhaust temperature of cyclonic separation is 840 DEG C, is cooled into afterheat steam recovery system
Temperature be 150 DEG C, after bag-type dust enter tail gas defluorinate system defluorinate it is up to standard after be discharged into air.Whole process lepidolite defluorinate
Rate is 98%, heat recovery rate 80%.
Embodiment 3
A kind of method of lepidolite recirculating fluidized bed roasting defluorinate, concretely comprises the following steps：
By lepidolite ore it is levigate to particle diameter be 60 μm；Then be 8wt% by water content, oxidation lithium content is 0.5wt%, fluorinated volume is
The lepidolite miberal powder of 1.5wt% is put into recirculating fluidized bed, with the hot-air of fluidized-bed bottom burner generation and the water of introducing
Steam rises roasting defluorinate, and water vapour content is 12wt% in burning gases, and the water vapour amount of introducing is in input recirculating fluidized bed
The 5% of lepidolite weight, hot gas flow velocity are 3m/s, and miberal powder is heated to 860 DEG C；Then connect together into fluidized bed top horizontal
The cyclone separator gas solid separation connect, miberal powder are fallen into circulation discharge groove, and 90% miberal powder is blown into fluid bed through air or steam
Circulation roasting, the miberal powder stop reaction time total in recirculating fluidized bed is 30min, and remaining miberal powder, which is discharged into cooler, uses air
Cooling obtains defluorinate lepidolite finished product；The exhaust temperature of cyclonic separation is 860 DEG C, and temperature is cooled into afterheat steam recovery system
Spend for 180 DEG C, after bag-type dust enter tail gas defluorinate system defluorinate it is up to standard after be discharged into air.Whole process lepidolite defluorinate rate
For 96.7%, heat recovery rate 80%.
Embodiment 4
A kind of method of lepidolite recirculating fluidized bed roasting defluorinate, concretely comprises the following steps：
By lepidolite ore it is levigate to particle diameter be 800 μm；Then be 3wt% by water content, oxidation lithium content is 3.6wt%, fluorinated volume
Put into recirculating fluidized bed for the lepidolite miberal powder of 2.8wt%, hot-air and introducing with the generation of fluidized-bed bottom burner
Water vapour rises roasting defluorinate, and water vapour content is 15wt% in burning gases, and the water vapour amount of introducing is input recirculating fluidized bed
The 5% of interior lepidolite weight, hot gas flow velocity are 1.5m/s, and miberal powder is heated to 880 DEG C；Then together into fluidized bed top water
The cyclone separator gas solid separation of flushconnection, miberal powder are fallen into circulation discharge groove, and 85% miberal powder is blown into fluidisation through air or steam
Circulation roasting in bed, the miberal powder stop reaction time total in recirculating fluidized bed is 45min, and remaining miberal powder, which is discharged into cooler, to be used
Air cooling obtains defluorinate lepidolite finished product；The exhaust temperature of cyclonic separation is 880 DEG C, is cooled down into afterheat steam recovery system
To temperature be 160 DEG C, after bag-type dust enter tail gas defluorinate system defluorinate it is up to standard after be discharged into air.Whole process lepidolite takes off
Fluorine rate is 96%, heat recovery rate 82%.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (5)
- A kind of 1. method of lepidolite recirculating fluidized bed roasting defluorinate, it is characterised in that：Comprise the following steps：1）Lepidolite ore pulverizer is levigate, obtain lepidolite miberal powder；2）Lepidolite miberal powder after will be levigate is incorporated into recirculating fluidized bed, the burning with the generation of recirculating fluidized bed combustion bottom burner Gas and the vapor of introducing carry out defluorinate roasting together, and subsequent miberal powder enters recirculating fluidized bed top water together with thermal current The cyclone separator of flushconnection carries out gas solid separation；Separated miberal powder enters in circulation discharge groove, with steam or air part It is incorporated into recirculating fluidized bed and continues defluorinate roasting with the miberal powder newly added, another part miberal powder is discharged in cooler through discharge groove Cooled down with air and recycle heat, obtain defluorinate lepidolite；The separated tail gas of cyclone separator is recycled into afterheat steam System cools down, and participates in defluorination reaction in partially recycled water vapour to recirculating fluidized bed；Gas after cooling through cloth bag or After electric precipitation, into the rear emptying up to standard of tail gas defluorinate system；Settled in afterheat steam recovery system and cloth bag or electric precipitation The miberal powder of collection, which is returned in recirculating fluidized bed, continues defluorinate roasting.
- 2. the method for lepidolite recirculating fluidized bed roasting defluorinate according to claim 1, it is characterised in that：Step 1）Middle lithium Mica Mine is milled down to 1000 μm of particle diameter ＜；Lepidolite ore water content ＜ 10wt%, aoxidize in lepidolite ore lithium content >= 0.5wt%, fluorinated volume ＞ 0.5wt%.
- 3. the method for lepidolite recirculating fluidized bed roasting defluorinate according to claim 1, it is characterised in that：Step 2）In, Miberal powder is consistent with the thermal current direction of motion in fluid bed；Miberal powder is heated to temperature as 700-950 DEG C；Hot gas flow velocity is 0.5- 5m/s；The new miberal powder amount being added in recirculating fluidized bed is the 3%-20% of the miberal powder total amount circulated in fluid bed；Arranged from circulation It is incorporated into hopper and continues the 80%-97% that the miberal powder amount that defluorinate roasts accounts for miberal powder amount in circulation discharge groove in recirculating fluidized bed；Ore deposit Powder mean residence time total in recirculating fluidized bed is 5-50min；The temperature of the separated tail gas of cyclone separator is 700-950 DEG C, the tail gas into afterheat steam recovery system cools to temperature as 150-300 DEG C；The sky being preheated in cooler Gas roots-type wind turbine is introduced into combustion-supporting in burner or is blown into circulation discharge groove and brings in recirculating fluidized bed miberal powder part into and follow Ring roasts.
- 4. the method for lepidolite recirculating fluidized bed roasting defluorinate according to claim 1, it is characterised in that：Step 2）Middle combustion Fuel in burner is the one or more in coal tar, natural gas, liquefied gas or coke-stove gas；Vapor in burning gases 1.5 wt % of content ＞；The amount of the vapor of the introducing is the 0.2-10% of lepidolite miberal powder weight in input recirculating fluidized bed.
- A kind of 5. defluorinate lepidolite obtained such as claim 1-4 any one of them methods, it is characterised in that：Obtained lithium Mica defluorinate rate ＞ 95%, the heat of roasting process fuel as a vapor and hot-air form recycling heat, heat recovery rate More than 60%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114790006A (en) * | 2022-06-09 | 2022-07-26 | 沈阳鑫博工业技术股份有限公司 | Suspension roasting method for lepidolite mineral powder |
| CN114933309A (en) * | 2022-05-25 | 2022-08-23 | 江西博瑞新材料科技有限公司 | Method for extracting enriched lepidolite based on lithium ore pressed tail mud |
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| US20030159994A1 (en) * | 2000-02-23 | 2003-08-28 | Marc Blachman | Defluorinator catalyst and process for removing fluorides from fluids |
| CN102530874A (en) * | 2012-03-02 | 2012-07-04 | 宜春合纵锂业科技有限公司 | Method for preparing hydrogen fluoride and fluoride product from lepidolite defluorinated tail gas |
| CN102586587A (en) * | 2012-03-24 | 2012-07-18 | 宜春合纵锂业科技有限公司 | Novel method for treating lepidolite ore |
| CN105331803A (en) * | 2015-10-27 | 2016-02-17 | 中国科学院过程工程研究所 | Roasting defluorination device and technology |
| CN106987708A (en) * | 2016-01-21 | 2017-07-28 | 中国科学院过程工程研究所 | A kind of defluorinate calciner and technique containing lithium minerals |
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2017
- 2017-12-12 CN CN201711317357.2A patent/CN107934980B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20030159994A1 (en) * | 2000-02-23 | 2003-08-28 | Marc Blachman | Defluorinator catalyst and process for removing fluorides from fluids |
| CN102530874A (en) * | 2012-03-02 | 2012-07-04 | 宜春合纵锂业科技有限公司 | Method for preparing hydrogen fluoride and fluoride product from lepidolite defluorinated tail gas |
| CN102586587A (en) * | 2012-03-24 | 2012-07-18 | 宜春合纵锂业科技有限公司 | Novel method for treating lepidolite ore |
| CN105331803A (en) * | 2015-10-27 | 2016-02-17 | 中国科学院过程工程研究所 | Roasting defluorination device and technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114933309A (en) * | 2022-05-25 | 2022-08-23 | 江西博瑞新材料科技有限公司 | Method for extracting enriched lepidolite based on lithium ore pressed tail mud |
| CN114933309B (en) * | 2022-05-25 | 2023-08-25 | 江西博瑞新材料科技有限公司 | Method for extracting and enriching lepidolite based on lithium ore pressed tail mud |
| CN114790006A (en) * | 2022-06-09 | 2022-07-26 | 沈阳鑫博工业技术股份有限公司 | Suspension roasting method for lepidolite mineral powder |
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