CN108046297A - The method for recycling rotary kiln exhaust gas production lithium carbonate - Google Patents
The method for recycling rotary kiln exhaust gas production lithium carbonate Download PDFInfo
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- CN108046297A CN108046297A CN201711378097.XA CN201711378097A CN108046297A CN 108046297 A CN108046297 A CN 108046297A CN 201711378097 A CN201711378097 A CN 201711378097A CN 108046297 A CN108046297 A CN 108046297A
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- tail gas
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- rotary kiln
- lithium carbonate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- 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
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Abstract
The method for recycling rotary kiln exhaust gas production lithium carbonate, comprises the technical steps that：The high-temperature tail gas that the rotary kiln of A calcining spodumenes comes out enters waste heat boiler, recycles tail gas heat quantity；The kiln tail gas that B waste heat boilers come out enters bag-type dust collector, removes the dust in tail gas, and control outlet tail gas dust content is less than 50 mg/m3, exhaust temperature is 140 ~ 150 DEG C；Tail gas after C bag-type dusts enters desulfurization removing nitric tower, and tail gas is directly entered roots blower pressure charging system after desulfurization removing nitric drying process；The purified tail gas of D, which enters after roots blower pressurizes in tail gas pressurized tank, to be stored, and the pressure control of storage tank is 70 ~ 90kPa；Cleaning of off-gas in storage tank is passed through carbonizing trough and is reacted with lithium hydroxide mother liquor by E, and wherein lithium hydroxide mother liquid concentration is controlled as 105 ~ 120g/L, pH value 6.8 ~ 7.5,85~92 DEG C of carburizing temperature, 1 ~ 1.5h of reaction time；Slurries obtained by the reaction are centrifuged dry finished product lithium carbonate.
Description
Technical field
The invention belongs to lithium hydroxide and lithium carbonate production technical field and a kind of kiln tail gas disposal technique, specifically
It is related to a kind of method for recycling carbon dioxide production lithium carbonate in calcining spodumene rotary kiln exhaust gas.
Background technology
Sulfuric acid process extracts the ore that lithium carbonate is current comparative maturity from spodumene and puies forward lithium technique.Its technological process：First
Natural spodumene at 950~1100 DEG C is roasted, makes its α-spodumene transformed β-spodumene by monoclinic system, since crystal form turns
Become, the physicochemical properties of mineral generate significant change also with the variation of crystal structure, and chemism increases energy and soda acid
The various reactions of generation.Then sulfuric acid is roasted with β-spodumene at 250 ~ 300 DEG C, it is anti-that displacement occurs by sulfating roasting
It should, you can the soluble lithium sulfate of generation and insoluble gangue.Lithium sulfate solution carries out metathesis reaction with caustic soda, forms sodium sulphate
With lithium hydroxide solution mixture.Using the significant difference of sodium sulphate and Lithium hydroxide monohydrate solubility at low temperature by the two point
It is carbonized high purity lithium carbonate from obtaining the solution of lithium hydroxide, then with carbon dioxide.
Rotary kiln carries out that in high-temperature calcination spodumene processing procedure substantial amounts of high temperature kiln tail gas will be generated.Tail gas it is main
Ingredient is carbon dioxide, nitrogen oxides, sulfide, nitrogen, flue dust etc..Manufacturing enterprise generally after the heat in recycling tail gas,
It is arranged directly outer after tail gas desulfurization denitration, substantial amounts of carbon dioxide is contained in last efflux gas.Carbon dioxide is that the whole world is most heavy
The greenhouse gases wanted account for the 50% of whole greenhouse gases to the contribution of greenhouse effects, are the main originals for causing climate warming
Cause., it is necessary to which outsourcing carbon dioxide, is finally converted lithium hydroxide using carbon dioxide in follow-up pure Lithium Carbonate production technology
For lithium carbonate.Containing substantial amounts of carbon dioxide in rotary kiln exhaust gas, therefore carbon dioxide separation therein can be recycled completely,
For the production of lithium carbonate in subsequent technique.
It is all related in existing disclosed patent to recycling carbon dioxide in various tail gas, but does not have and be generally applicable in
Property, it is had not been reported especially with regard to using carbon dioxide preparation lithium carbonate in the rotary kiln exhaust gas for calcining spodumene.
The content of the invention
The present invention is intended to provide a kind of method for recycling rotary kiln exhaust gas production lithium carbonate, the revolution of recycling calcining spodumene
Carbon dioxide in kiln exhaust gas, for producing lithium carbonate.
In order to achieve the goal above, the present invention takes following technical scheme：
The method for recycling rotary kiln exhaust gas production lithium carbonate, comprises the technical steps that：
The high-temperature tail gas that the rotary kiln of A calcining spodumenes comes out enters waste heat boiler, tail gas heat quantity is recycled, after recycling heat
Exhaust temperature is 140 ~ 160 DEG C.
The kiln tail gas that B waste heat boilers come out enters bag-type dust collector, removes the dust in tail gas, control outlet tail
Gas dust content is less than 50 mg/Nm3, exhaust temperature is 140 ~ 150 DEG C.
Tail gas after C bag-type dusts enters desulfurization removing nitric tower, and content of sulfur dioxide is less than 10 in control gained cleaning of off-gas
mg/Nm3, amount of nitrogen oxides is less than 5mg/Nm3, water content is reduced to 30mg/Nm3, tail gas dust content is less than 5 mg/Nm3,
Tail gas is cooled to 70 ~ 80 DEG C；Tail gas is directly entered roots blower pressure charging system after desulfurization removing nitric drying process.The desulfurization takes off
The nitrogen tower tower is double-deck packed tower, and lower floor's filling sodium carbonate, for removing the sulfur dioxide and nitrogen oxides in tail gas, upper strata is filled out
Fill the moisture in 3A molecular sieves removal tail gas.
The purified tail gas of D, which enters after roots blower pressurizes in tail gas pressurized tank, to be stored, and the pressure control of storage tank is
70~90kPa。
Cleaning of off-gas in storage tank is passed through carbonizing trough and is reacted with lithium hydroxide mother liquor by E, wherein lithium hydroxide mother liquid concentration
It controls as 105 ~ 120g/L, pH value 6.8 ~ 7.5,85~92 DEG C of carburizing temperature, 1 ~ 1.5h of reaction time；By slurries obtained by the reaction
It is centrifuged dry finished product lithium carbonate（LITHIUM BATTERY）.
Description of the drawings
Fig. 1 is present invention process flow chart.
Specific embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1：
Spodumene 6t calcines per hour in certain enterprise, and each component content is after testing such as table 1 in spodumene rotary kiln exhaust gas.
Each component content in spodumene rotary kiln exhaust gas in 1 embodiment 1 of table（%）
Processing step includes：
High temperature kiln tail gas is sent into waste heat boiler, boiler recycling wherein most heat, the tail gas come out from waste heat boiler by A
Amount is about 7400 m3/ h, temperature are 146 DEG C, pressure 2080Pa, roll over 4922 Nm3/ h。
Then tail gas is sent into bag-type dust removal system by B, remove the dust in tail gas, 24 mg/ of outlet tail gas dust content
Nm3, exhaust temperature is 142 DEG C.
Tail gas after C will remove chalk dust removing is sent into desulfurization removing nitric drying tower bottom, removes sulfur dioxide therein and nitrogen oxidation
Object, while remove moisture therein.Inner exhaust gas on the 10th（It is every 4 it is small when sampling once）Average content sulfur dioxide 7.3mg/Nm3, nitrogen
4.6 mg/Nm of oxide3, 28 mg/Nm of water3, 4.7 mg/Nm of dust3, tail gas mean temperature is to 74 DEG C；
By treated, tail gas is blasted in tail gas storage tank for use D with roots blower.Carbon dioxide content is in treated tail gas
18.4%, nitrogen content 81.5%, content of sulfur dioxide is 3 mg/Nm3, amount of nitrogen oxides is less than 6 mg/Nm3, water content drop
Down to 15 mg/Nm3。
Tail gas in tail gas storage tank is passed through in carbonization kettle by E again, with the lithium hydroxide mother liquor that concentration therein is 116g/L
Reaction, it is 7.0 to control reaction pH, and reaction temperature is 85 DEG C, is stirred to react 1h.Solid is centrifuged after reaction obtains wet carbon
Then sour lithium carries out drying drying again, finally obtain product lithium carbonate（LITHIUM BATTERY）.
Embodiment 2：
Spodumene 15.5t calcines per hour in certain enterprise, and each component content is after testing such as table 2 in spodumene rotary kiln exhaust gas.
Each component content in spodumene rotary kiln exhaust gas in 2 embodiment 2 of table（%）
Processing step includes：
High temperature kiln tail gas is sent into waste heat boiler, boiler recycling wherein most heat, the tail gas come out from waste heat boiler by A
Amount is about 18500 m3, temperature is 144 DEG C, pressure 2060Pa, rolls over 12362.6 Nm3/ h。
Then tail gas is sent into bag-type dust removal system by B, remove the dust in tail gas, 22 mg/ of outlet tail gas dust content
m3, exhaust temperature is 140 DEG C.
Tail gas after C will remove chalk dust removing is sent into desulfurization removing nitric drying tower bottom, removes sulfur dioxide therein and nitrogen oxidation
Object, while remove moisture therein.Inner exhaust gas on the 10th（It is every 4 it is small when sampling once）Average content sulfur dioxide 6.6mg/Nm3, nitrogen
3.2 mg/Nm of oxide3, 24 mg/Nm of water3, 4.2 mg/Nm of dust3, tail gas mean temperature is to 72 DEG C；
By treated, tail gas is blasted in tail gas storage tank for use D with roots blower.Treated tail gas inner exhaust gas on the 10th（Every 4 is small
When sampling once）Average content carbon dioxide is 22.6%, nitrogen content 77.2%, content of sulfur dioxide 5mg/Nm3, nitrogen oxygen
Compound content is less than 10 mg/Nm3, water content is reduced to 28 mg/Nm3。
Tail gas in tail gas storage tank is passed through in carbonization kettle by E again, with the lithium hydroxide mother liquor that concentration therein is 116g/L
Reaction, it is 7.0 to control reaction pH, and reaction temperature is 85 DEG C, is stirred to react 1h.Solid is centrifuged after reaction obtains wet carbon
Then sour lithium carries out drying drying again, finally obtain product lithium carbonate（LITHIUM BATTERY）.
Claims (1)
1. recycling the method for rotary kiln exhaust gas production lithium carbonate, comprise the technical steps that：
A. calcine the high-temperature tail gas of the rotary kiln of spodumene out and enter waste heat boiler, tail gas heat quantity is recycled, after recycling heat
Exhaust temperature is 140 ~ 160 DEG C；
B. the kiln tail gas that waste heat boiler comes out enters bag-type dust collector, removes the dust in tail gas, control outlet tail gas powder
Dust content is less than 50 mg/Nm3, exhaust temperature is 140 ~ 150 DEG C；
C. the tail gas after bag-type dust enters desulfurization removing nitric tower, and content of sulfur dioxide is less than 10 in control gained cleaning of off-gas
mg/Nm3, amount of nitrogen oxides is less than 5mg/Nm3, water content is reduced to 30mg/Nm3, tail gas dust content is less than 5 mg/Nm3,
Tail gas is cooled to 70 ~ 80 DEG C；Tail gas is directly entered roots blower pressure charging system after desulfurization removing nitric drying process；
D. purified tail gas after roots blower pressurizes into storing in tail gas pressurized tank, pressure of storage tank control for 70 ~
90kPa；
E. the cleaning of off-gas in storage tank is passed through carbonizing trough to react with lithium hydroxide mother liquor, wherein lithium hydroxide mother liquid concentration control
It is made as 105 ~ 120g/L, pH value 6.8 ~ 7.5,85~92 DEG C of carburizing temperature, 1 ~ 1.5h of reaction time；Slurries obtained by the reaction are passed through
Centrifuge dry finished product lithium carbonate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108923095A (en) * | 2018-08-24 | 2018-11-30 | 广西师范大学 | A method of recycling negative electrode material of waste lithium ion battery |
| CN114835142A (en) * | 2022-05-11 | 2022-08-02 | 江苏容汇通用锂业股份有限公司 | Method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate |
| CN115304086A (en) * | 2022-07-20 | 2022-11-08 | 山西大学 | Method for producing lithium carbonate by mineralizing aluminum-lithium slag with flue gas |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800715A (en) * | 2004-12-31 | 2006-07-12 | 李志恒 | Comprehensive recovery and utilization method for exhaust gas |
| CN103073039A (en) * | 2013-03-01 | 2013-05-01 | 兰州理工大学 | Method for preparing superfine carbonate powder material |
-
2017
- 2017-12-19 CN CN201711378097.XA patent/CN108046297A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800715A (en) * | 2004-12-31 | 2006-07-12 | 李志恒 | Comprehensive recovery and utilization method for exhaust gas |
| CN103073039A (en) * | 2013-03-01 | 2013-05-01 | 兰州理工大学 | Method for preparing superfine carbonate powder material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108923095A (en) * | 2018-08-24 | 2018-11-30 | 广西师范大学 | A method of recycling negative electrode material of waste lithium ion battery |
| CN114835142A (en) * | 2022-05-11 | 2022-08-02 | 江苏容汇通用锂业股份有限公司 | Method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate |
| CN115304086A (en) * | 2022-07-20 | 2022-11-08 | 山西大学 | Method for producing lithium carbonate by mineralizing aluminum-lithium slag with flue gas |
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Application publication date: 20180518 |