CN101224900A - Novel method for spodumene calcining transformation - Google Patents
Novel method for spodumene calcining transformation Download PDFInfo
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- CN101224900A CN101224900A CNA2007100502169A CN200710050216A CN101224900A CN 101224900 A CN101224900 A CN 101224900A CN A2007100502169 A CNA2007100502169 A CN A2007100502169A CN 200710050216 A CN200710050216 A CN 200710050216A CN 101224900 A CN101224900 A CN 101224900A
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Abstract
The invention relates to a method for producing lithium carbonate, lithium hydroxide and lithium chloride with spodumene. Aiming at the defect of the calcination transformation technology of the spodumene concentrate, the invention provides a new method of the fluidization and dynamic calcination transformation of the spodumene concentrate: the spodumene concentrate from a concentration plant is dried and milled to granules with the granularity of minus 250 meshes to minus 350 meshes; then a fluidization dynamic calcinator is adopted to carry out high temperature calcination transformation to the concentrate, the material temperature is controlled between 900 and 1200 DEG C; because the material in the furnace is fluidized and transfers heat and is delivered in the form of air delivery with hot air, the process is rapid in heat transfer rate, high in efficiency and short in calcination time, which overcomes the technical defect of the existing calcination technology that the material is easy to be agglomerated and avoids cooling and ball-milling procedures. When the calcined material is treated by the procedures of leaching, purging, filtering, etc., the obtained filtrate (raw material liquid) can be utilized for producing products such as lithium carbonate, lithium hydroxide, lithium chloride and so on by adopting existing different technologies.
Description
Technical field
The present invention relates to triphane and produce the production method of Quilonum Retard, lithium hydroxide, lithium chloride.
Background technology
Lithium and compound thereof have unique physical and chemical performance, be widely used in fields such as the energy, chemical industry, nuclear power, pottery, metallurgy, especially the widespread use on lithium cell, making the main products of market to lithium---Quilonum Retard, lithium hydroxide and lithium chloride consumption sharply increase, and market value goes up at double.Therefore invent and new, economically viablely produce the lithium method for product from the triphane concentrate, significant.
Produce Quilonum Retard, lithium hydroxide or lithium chloride from triphane, present domestic operational path and principle are:
With the triphane is raw material, no matter produces Quilonum Retard, lithium hydroxide or lithium chloride, all must make it to be converted into the β type from the α type with the triphane concentrate of α type by high-temperature calcination.At present domestic traditional technology be the triphane concentrate through the internal heat type rotary kiln in 1000-1100 ℃ of high-temperature calcination 0.5-2 hour, make the triphane concentrate be converted into the β type from the α type, calcining materials is cooled to below 100 ℃ by water cooler, after the ball mill ball milling is extremely about-200 orders, with sulfuric acid by 0.25-0.32: 1.0 (sulfuric acid is to the lithium concentrate mass ratioes) mix and stir with this material, carried out acidizing fired 0.5 hour in 300-350 ℃ with the acidifying rotary kiln, this acidifying material water after the water cooler cooling leaches, pass through purifying treatment, filter, obtain being rich in the lithium sulfate solution of lithium, be stock liquid, this stock liquid can be produced Quilonum Retard by different production technique, product such as lithium hydroxide or lithium chloride.The main drawback that this traditional technology exists is:
1. rotary kiln high-temperature calcination thermal conduction is poor, and calcination time is long, and throughput is low, the energy consumption height, and facility investment is big, the cost height
The widely used internal heat type rotary kiln of lithium industry carries out calcining transition of triphane at present, material rotates from the kiln tail to kiln hood and the heated air transmission of heat by contact by slow in kiln, be warming up to gradually about 1100 ℃, because heat transfer rate is slow, calcination time is greatly about 30-120 minute, and the being heated evenly property of material is poor, be prone to local sintering, rate transition of material can only reach 95-97%, and cleaned coal (〉=7400Kcal/Kg) consumption is big, makes production cost very high; And this equipment volume is huge, and generally all about 2 meters, length is at 35-40 rice for its diameter, and investment is big, the power consumption height;
2. the tail gas dust collecting system is huge, and investment is high
What the rotary kiln dust collecting system generally adopted at present is cyclone dust collection and wet dust collector, and it is bulky, and floor space is big, and is less economical;
3. ball mill ball milling material energy consumption height is invested greatly the noise height
Ball mill is mainly used in the higher material grinding of hardness, this equipment energy consumption height, and investment is big, the noise height.In system lithium industry, because rotary kiln high-temperature calcination thermal conduction is poor, calcining transformation material thereby partial rigid agglomerate occurs also has to adopt the above-mentioned calcining transformation material of this ball mill ball milling in the existing technology.
Summary of the invention
The present invention is directed to above-mentioned triphane concentrate Quilonum Retard, lithium hydroxide or the lithium chloride technology shortcoming in the calcining transformation technology, the novel method that provides a kind of triphane concentrate fluidisation dynamic calcining to make the transition are provided.Principle process flow sheet of the present invention is seen accompanying drawing 1, specifically:
The triphane concentrate (water ratio is generally 12-18%) that will come from the dressing-works, is 0.5-8% with pneumatic drier or other drying plant with this concentrate moisture drying to water ratio, the hot gas that its drying source can produce with the tail gas after the calcining or other heating unit, with pulverizer should dried concentrate be milled to granularity for-250 orders to-350 orders, if the granularity of former concentrate own is-200 orders, also can not carry out ore grinding; If the moisture content of former concentrate also can not carried out this drying less than 8%.With fluidisation dynamic calcining stove above-mentioned concentrate being carried out high-temperature calcination from burner with high-temperature hot air by metering makes the transition, calcining furnace ingress hot air temperature is 800-1500 ℃, calcining furnace exit hot air temperature is 500-1000 ℃, temperature of charge is controlled at 900-1200 ℃, vacuum tightness is 2000-9000Pa in the control stove, and the hot gas flow velocity is 5-40m/s, and the residence time of material in stove is 5 seconds to 5 minutes, material is gas delivery form and hot blast and conducts heat, and calcines and carry.The thermal source of this fluidisation dynamic calcining stove is a fine coal, or Sweet natural gas, or the burning of heavy-oil hot-air stove produces high temperature hot gas.Material is come out of the stove after cyclone dust collection, bag type filtering is collected and gather dust after, sending into acid mixer mixes with sulfuric acid, entering the acidifying kiln again carries out acidizing fired, water leaches then, obtain being rich in the stock liquid of Lithium Sulphate after the filtration, this stock liquid can be produced Quilonum Retard, lithium hydroxide or lithium chloride by different technology after purifying.
The present invention has the following advantages compared with the prior art:
1. fluidisation dynamic calcining heat transfer rate is fast, and material is heated evenly, transition the rate height, calcination time is short, the throughput height, energy consumption is low, facility investment is little, cost is low
Compare with traditional triphane high temperature technology transition, the present invention is owing to adopt fluidisation dynamic calcining new technology to replace traditional internal heat type rotary kiln, make material and heated air be the fluidisation dynamical state and carry out heat exchange, heat transfer rate is fast and even, and be the gas delivery form and carry, calcination time only is the 1-8% of the required calcination time of traditional calcined by rotary kiln technology transition, and saved the calcining materials refrigerating work procedure, throughput has improved tens of times, energy consumption and production cost are descended greatly, and this method investment is little, under the identical throughput, only is the 40-70% of traditional calcined by rotary kiln technological investment transition;
2. the calcining transformation material is loose, has overcome material easy-sintering phenomenon in traditional calcining transformation technology, has saved the ball milling operation, has simplified technology, has reduced cost
3. the tail gas dust collecting system is little, invests for a short time, has overcome the shortcoming that fine dusts is difficult to utilize again
The present invention adopts cyclone dust collection, bag type filtering to gather dust, and its volume is little, and reduced investment is effective, and has overcome the shortcoming that is difficult to reclaim because of dust is tiny in the conventional art.
Description of drawings
Accompanying drawing 1 is a principle process flow sheet of the present invention.
Embodiment
Embodiment 1
With 100 kilograms in triphane concentrate (composition sees Table 1), with pneumatic drier this ore deposit being dried to water ratio is 1.2%, its thermal source is used for the tail gas of self-fluidized type dynamic calcining stove, dried material is milled to 80% with pulverizer and crosses 250 orders, carries out calcining transformation with the fluidisation dynamic calcining stove that designs and make voluntarily then.Calcining temperature is 1050 ℃, the thermal source of this calcining furnace is to spray in the boiler tube with the hot gas that heavy oil combustion produces, the flow that dried triphane concentrate is pressed 25Kg/min adds in the calcining furnace, calcining furnace ingress hot air temperature is 1300 ℃, calcining furnace exit hot air temperature is 700 ℃, and temperature of charge is controlled at 1050 ℃, and vacuum tightness is 5000Pa in the control stove, the hot gas flow velocity is 30m/s, and the hot gas flow is 150Nm
3/ min, the residence time of material in stove is 30 seconds, use cyclone, bag filter is collected and is gathered dust, the tail gas emptying, material after the calcining adds the vitriol oil and mixes and stirs by 0.27: 1.0 (mass ratio), carry out acidizing fired in 330 ℃, the acidizing fired time is 30 minutes, takes out cooling, and water leached 30 minutes down in 60 ℃ by solid-to-liquid ratio 1.0: 2.0 (mass ratio), with industrial stair oxidation calcium this leach liquor pH is transferred to 7.5, filter with vacuum filter, and with 500 kilograms process water washing leaching cake, these washing water are collected the back and are used as the water of sizing mixing.Collect this filtrate and filter cake (filter cake is in 110 ℃ of dry diels), measure the Li in filtrate and the filter cake respectively
2O calculates Li
2The leaching yield of O and transition rate.Its analytical results sees Table 2.
Table 1 triphane concentrate main component (wt%)
| Element | Li 2O | Na 2O | K 2O | Fe 2O 3 | P 2O 5 | Al 2O 3 | SiO 2 | Moisture | Granularity |
| Content (%) | 5.3 | 0.72 | 0.45 | 2.1 | 0.28 | 22.44 | 66.82 | 14.5 | -200 |
Embodiment 2
With 100 kilograms in triphane concentrate (composition sees Table 1), with pneumatic drier this ore deposit being dried to water ratio is 1.2%, and its thermal source is used for the tail gas of self-fluidized type dynamic calcining stove, carries out calcining transformation with the fluidisation dynamic calcining stove that designs and make voluntarily then.Calcining temperature is 1050 ℃, the thermal source of this calcining furnace is to spray in the boiler tube with the warm air that heavy oil combustion produces, calcining furnace ingress hot blast temperature is 1500 ℃, calcining furnace exit hot blast temperature is 850 ℃, temperature of charge is controlled at 900-1200 ℃, vacuum tightness is 6000Pa in the control stove, and the furnace gas flow velocity is 40m/s, and the furnace gas flow is 200Nm
3/ min, the residence time of material in stove is 20 seconds, gather dust with cyclone, bag filter, the tail gas emptying, material after the calcining adds the vitriol oil and mixes and stirs by 0.27: 1.0 (mass ratio), in 330 ℃ of acidizing fired times is 30 minutes, take out cooling, water leached 30 minutes down in 60 ℃ by solid-to-liquid ratio 1.0: 2.0 (mass ratio), with industrial one-level lime carbonate this leach liquor pH is transferred to 7.5, filter with vacuum filter, and with 500 kilograms process water washing leaching cake, these washing water are collected the back and are used as next leach liquor.Collect this filtrate and filter cake, the Li in this filtrate and the filter cake (filter cake is in 110 ℃ of dry diels) is measured in sampling respectively
2O calculates Li
2The leaching yield of O and transition rate.Its analytical results sees Table 2.
Embodiment 3
With 100 kilograms in triphane concentrate (composition sees Table 1), carry out calcining transformation with small-sized rotary kiln.Calcining temperature is 1050 ℃, the thermal source of this calcining furnace is to spray into the warm air that the kiln internal combustion produces with fine coal, the residence time of material in kiln is 40 minutes, use cyclone, wet cleaner gathers dust, the tail gas emptying, material after the calcining is after the cooling of external-cooling type watercooler, enter ball mill and be milled to 80% (quality)-200 order, adding the vitriol oil mixes and stirs by 0.27: 1.0 (mass ratio), in 330 ℃ of acidizing fired times is 30 minutes, take out cooling, water leached 30 minutes down in 60 ℃ by solid-to-liquid ratio 1.0: 2.0 (mass ratio), with industrial stair oxidation calcium this leach liquor pH was transferred to 7.5, filtered with vacuum filter, and with 500 kilograms process water washing leaching cake, these washing water are collected the back as next leach liquor.Collect this filtrate and filter cake, the Li in this filtrate and the filter cake (filter cake is in 110 ℃ of dry diels) is measured in sampling respectively
2O calculates Li
2The leaching yield of O and transition rate.Its analytical results sees Table 2.
Table 2 embodiment result
| Embodiment | Dried filter cake Li 2O content (wt%) | Filtrate Li 2O content (g/l) | Rate transition (%) | Li 2O leaching yield (%) |
| Embodiment 1 | 0.28 | 24.2 | 98.7 | 92.04 |
| Embodiment 2 | 0.31 | 23.6 | 97.2 | 89.83 |
| Embodiment 3 | 0.38 | 22.8 | 96.0 | 86.97 |
Claims (3)
1. a spodumene calcining transformation is produced Quilonum Retard, lithium hydroxide or lithium chloride method, it is characterized in that: the triphane concentrate is behind air stream drying, material is by the calcining of fluidisation dynamic high temperature, α type lithium concentrate is made the transition be β type lithium concentrate, material is come out of the stove after after cyclone dust collection, bag type filtering are gathered dust, do not need ore grinding, directly sending into acid mixer mixes with sulfuric acid, entering the acidifying kiln again carries out acidizing fired, water leaches then, obtain being rich in the stock liquid of Lithium Sulphate after the filtration, this stock liquid can be produced Quilonum Retard, lithium hydroxide or lithium chloride by different technology after purifying.
2. according to the triphane transition method of claim 1, it is characterized in that: said air stream drying is that a kind of solid powder is scattered in the drying mode in the warm air, the thermal source that its drying source can produce with the tail gas after the calcining or other heating unit, with pulverizer should dried concentrate be milled to granularity for-250 orders to-350 orders, if the granularity of former concentrate own is-200 orders, also can not carry out this ore grinding; If the moisture content of former concentrate also can not carried out this drying less than 8%.The pneumatic drier inlet temperature is 150-700 ℃, and air outlet temperature is 50-200 ℃, uses cyclone and bagroom to collect material and gather dust.
3. according to the triphane transition method of claim 1, it is characterized in that: said fluidisation dynamic calcining is that triphane concentrate powder is scattered in and is gas delivery form and hot gas in the hot gas and conducts heat, and carries out high-temperature calcination transition and carry.The thermal source of this fluidisation dynamic calcining is a fine coal, or Sweet natural gas, or the burning of heavy-oil hot-air stove produces high temperature hot gas, calcining furnace ingress hot air temperature is 800-1500 ℃, and calcining furnace exit hot air temperature is 500-1000 ℃, and temperature of charge is controlled at 900-1200 ℃, vacuum tightness is 2000-9000Pa in the control stove, hot gas flow velocity in calcining furnace is 5-40m/s, and the residence time of material in stove is 5 seconds to 5 minutes, collects material and gathers dust with cyclone and bagroom.
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115101A (en) * | 2011-01-05 | 2011-07-06 | 屈俊鸿 | Novel method for producing lithium carbonate and lithium hydroxide |
| WO2011148040A1 (en) * | 2010-05-25 | 2011-12-01 | Outotec Oyj | Method for processing spodumene |
| CN102509790A (en) * | 2011-10-20 | 2012-06-20 | 四川天齐锂业股份有限公司 | LiFePO4 (lithium iron phosphate) positive electrode material with specific morphology and structure and lithium secondary battery |
| CN103183366A (en) * | 2013-01-05 | 2013-07-03 | 江西赣锋锂业股份有限公司 | Method for extracting lithium salt from spodumene by soda ash pressure leach method |
| CN103204510A (en) * | 2013-04-24 | 2013-07-17 | 成都正远机电设备有限公司 | Spodumene roasting transformation method |
| CN103332858A (en) * | 2013-07-09 | 2013-10-02 | 海门容汇通用锂业有限公司 | Preparation method of microcrystalline glass-grade beta-type spodumene |
| CN103849761A (en) * | 2014-03-17 | 2014-06-11 | 河南省岩石矿物测试中心 | Method for extracting lithium from low-grade lithium-containing clay ore |
| CN104071811A (en) * | 2014-06-06 | 2014-10-01 | 江西江锂新材料科技有限公司 | Process for extracting lithium salt from spodumene by adopting sulfuric acid pressure boiling method |
| CN106044804A (en) * | 2016-05-26 | 2016-10-26 | 四川思达能环保科技有限公司 | Novel process for producing lithium salt by aid of sulfuric acid methods |
| CN106904577A (en) * | 2017-03-21 | 2017-06-30 | 西北工业大学 | A kind of powder prepares high temperature gas flow impact thermal decomposition processing method and its device |
| CN107034355A (en) * | 2017-05-05 | 2017-08-11 | 江西南氏锂电新材料有限公司 | A kind of method that rubidium and caesium are extracted from lepidolite ore |
| CN107089674A (en) * | 2017-07-03 | 2017-08-25 | 福州大学 | A kind of spodumene sodium sulphate pressure leaching puies forward lithium technique |
| CN107640779A (en) * | 2017-11-15 | 2018-01-30 | 天元锂电材料河北有限公司 | Spodumene produces lithium carbonate technique |
| CN107739847A (en) * | 2017-10-16 | 2018-02-27 | 福州大学 | A kind of crystal formation conversion method of natural spodumene suspension roasting |
| CN108423694A (en) * | 2017-12-27 | 2018-08-21 | 攀枝花兴辰钒钛有限公司 | The method for producing lithium sulfate mother liquor or lithium carbonate as raw material using spodumene |
| CN109354044A (en) * | 2018-10-22 | 2019-02-19 | 天齐锂业(射洪)有限公司 | The method that lithium is recycled in lithium sodium sulfate byproduct is proposed from spodumene sulfuric acid process |
| WO2019086511A1 (en) * | 2017-11-03 | 2019-05-09 | Thyssenkrupp Industrial Solutions Ag | Method and facility for the thermal treatment of a lithium ore |
| CN110331280A (en) * | 2019-08-19 | 2019-10-15 | 四川卡森科技有限公司 | A kind of amblygonite roasting acidification system and its roasting acidization tool |
| CN113149039A (en) * | 2021-04-30 | 2021-07-23 | 四川万邦胜辉新能源科技有限公司 | Method for preparing lithium oxide by thermally reducing spodumene |
| CN115304073A (en) * | 2022-07-14 | 2022-11-08 | 北京凯盛建材工程有限公司 | Spodumene calcination transformation system and method |
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- 2007-10-11 CN CNA2007100502169A patent/CN101224900A/en active Pending
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| WO2011148040A1 (en) * | 2010-05-25 | 2011-12-01 | Outotec Oyj | Method for processing spodumene |
| CN102906022A (en) * | 2010-05-25 | 2013-01-30 | 奥图泰有限公司 | Method for processing spodumene |
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| CN102906022B (en) * | 2010-05-25 | 2015-11-25 | 奥图泰有限公司 | The working method of triphane |
| CN102115101B (en) * | 2011-01-05 | 2013-09-04 | 屈俊鸿 | Novel method for producing lithium carbonate and lithium hydroxide |
| CN102115101A (en) * | 2011-01-05 | 2011-07-06 | 屈俊鸿 | Novel method for producing lithium carbonate and lithium hydroxide |
| CN102509790A (en) * | 2011-10-20 | 2012-06-20 | 四川天齐锂业股份有限公司 | LiFePO4 (lithium iron phosphate) positive electrode material with specific morphology and structure and lithium secondary battery |
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| CN103204510A (en) * | 2013-04-24 | 2013-07-17 | 成都正远机电设备有限公司 | Spodumene roasting transformation method |
| CN103332858A (en) * | 2013-07-09 | 2013-10-02 | 海门容汇通用锂业有限公司 | Preparation method of microcrystalline glass-grade beta-type spodumene |
| CN103332858B (en) * | 2013-07-09 | 2016-08-10 | 江苏容汇通用锂业股份有限公司 | A kind of preparation method of devitrified glass level β-type spodumene |
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| CN106044804A (en) * | 2016-05-26 | 2016-10-26 | 四川思达能环保科技有限公司 | Novel process for producing lithium salt by aid of sulfuric acid methods |
| CN106904577A (en) * | 2017-03-21 | 2017-06-30 | 西北工业大学 | A kind of powder prepares high temperature gas flow impact thermal decomposition processing method and its device |
| CN107034355A (en) * | 2017-05-05 | 2017-08-11 | 江西南氏锂电新材料有限公司 | A kind of method that rubidium and caesium are extracted from lepidolite ore |
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| CN107089674A (en) * | 2017-07-03 | 2017-08-25 | 福州大学 | A kind of spodumene sodium sulphate pressure leaching puies forward lithium technique |
| CN107739847A (en) * | 2017-10-16 | 2018-02-27 | 福州大学 | A kind of crystal formation conversion method of natural spodumene suspension roasting |
| WO2019086511A1 (en) * | 2017-11-03 | 2019-05-09 | Thyssenkrupp Industrial Solutions Ag | Method and facility for the thermal treatment of a lithium ore |
| CN107640779A (en) * | 2017-11-15 | 2018-01-30 | 天元锂电材料河北有限公司 | Spodumene produces lithium carbonate technique |
| CN108423694A (en) * | 2017-12-27 | 2018-08-21 | 攀枝花兴辰钒钛有限公司 | The method for producing lithium sulfate mother liquor or lithium carbonate as raw material using spodumene |
| CN109354044A (en) * | 2018-10-22 | 2019-02-19 | 天齐锂业(射洪)有限公司 | The method that lithium is recycled in lithium sodium sulfate byproduct is proposed from spodumene sulfuric acid process |
| CN110331280A (en) * | 2019-08-19 | 2019-10-15 | 四川卡森科技有限公司 | A kind of amblygonite roasting acidification system and its roasting acidization tool |
| CN113149039A (en) * | 2021-04-30 | 2021-07-23 | 四川万邦胜辉新能源科技有限公司 | Method for preparing lithium oxide by thermally reducing spodumene |
| CN113149039B (en) * | 2021-04-30 | 2023-03-03 | 四川万邦胜辉新能源科技有限公司 | Method for preparing lithium oxide by thermal reduction of spodumene |
| CN115304073A (en) * | 2022-07-14 | 2022-11-08 | 北京凯盛建材工程有限公司 | Spodumene calcination transformation system and method |
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