CN203513300U - Preparation system of high-purity lithium carbonate - Google Patents

Preparation system of high-purity lithium carbonate Download PDF

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Publication number
CN203513300U
CN203513300U CN201320568542.XU CN201320568542U CN203513300U CN 203513300 U CN203513300 U CN 203513300U CN 201320568542 U CN201320568542 U CN 201320568542U CN 203513300 U CN203513300 U CN 203513300U
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tank
consummate
water
bittern
preparation system
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朱彬元
余昊
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TIBET JINRUI ASSET MANAGEMENT Co Ltd
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TIBET JINRUI ASSET MANAGEMENT Co Ltd
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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    • Y02P20/129Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

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Abstract

The utility model discloses a preparation system of high-purity lithium carbonate, which comprises a bittern concentration crystallizer and a refiner, wherein the bittern concentration crystallizer is provided with a heat storage tank and a heating tank; the heat storage tank and the heating tank are both provided with a heat exchange device respectively; the heat exchange devices are connected with a heat absorption end and a heat release end of a heat pump respectively; a bittern inlet and a tail bittern outlet are formed in the heating tank; the tail bittern outlet is connected with the heat storage tank through a pipeline; the refiner comprises a refining and purifying tank; a water outlet and a water inlet are formed in the refining and purifying tank; radial filter screens are arranged at the upper and lower parts in the refining and purifying tank. The system disclosed by the utility model can finish the refining and purifying of lithium carbonate through physical operation to obtain over 95% high-purity lithium carbonate, and remarkably reduces the later transportation cost and purifying cost. The system disclosed by the utility model can sufficiently recycle the water vapor byproduct distilled water and is used for purifying lithium carbonate. After use, the distilled water can enter a salt lake again to supplement water, and the ecological problem caused by the drop of water level of the salt lake is avoided.

Description

The preparation system of high purity carbonic acid lithium
Technical field
The utility model relates to a kind of purification system of Quilonum Retard.
Background technology
Because the electrochemical activity of lithium is strong, be again light metal, thereby tool have been widely used.The Application Areas of lithium comprises at present: pottery and glass, synthetic rubber, aluminium production, plastics, medicine, lubricant, air conditioning machinery, TV (window of tube), lithium cell, lithium alloy and nuclear industry etc.; Consumption reaches several ten thousand tons/year, and also in continuous growth.
In world's lithium total resources, bittern lithium ore deposit accounts for 75%, and hard rock lithium ore deposit accounts for 25%; In China's lithium total resources, bittern lithium ore deposit accounts for 72%, and hard rock lithium ore deposit accounts for 28%.Before the sixties, lithium resource is mainly from kieserohalosylvite lithium ore.Salt lake carry lithium cost compared with the low 1-1.5 of hard rock doubly more than, the lithium salts of producing from salt lake has at present surpassed hard rock lithium ore deposit, from salt lake brine, extracting lithium salts has become development megatrend.
Due to different with economic technology condition containing lithium salts lake water chemical type, so the operational path adopting is also different.The method of carrying lithium in prior art from bittern has: organic ion (TBP, i.e. tributyl phosphate etc.) exchange resin method, inorganic ion exchanger method, aluminate method, hydrogenchloride saltout method, aluminate method and the precipitator method (being phosphate process) and carbon method etc.But these methods all exist that energy consumption is higher, feed consumption is more, some systematic lectotypes are difficult, the problems such as production capacity is low or technical process is complicated, contaminate environment.
In addition, the Sulphate lakes such as Chilean Atacama lake, U.S. Yin Feng lake adopt saltpan method to carry out pre-concentration, and then are transported to factory process; Yet because the main salt lake of China is sulphate lake, the above-mentioned saltpan method that is suitable for Sulphate lake is not suitable for China's sulphate lake.Last century Mo, China has expert to propose to be suitable for extracting in sulphate lake the saltpan method of lithium, and is applied to the extraction of lithium salts.Yet after practice, find, there is following shortcoming in this technology, results in a loss:
1, need big area to build salt pan, laid down cost and later maintenance cost are quite large; Artificially significantly increased salt lake additional issue amount, destroyed the liquid level equilibrium in salt lake, may affect the ecology of Salt Lake Area simultaneously;
2, be subject to effect of natural conditions large;
3, the lithium salts purity making is low, and impurity is many, need to be transported to factory's reprocessing; Like this, transportation cost is very high; And wherein most of for transporting " the useless transportation " of impurity;
4, the salt manufacturing time is long; Technological process can not realize automatization, and efficiency is low.
In addition, existing salt lake substantially all, in remote area, has inconvenient traffic, and the shortages such as the energy, fresh water have further strengthened the difficulty of purifying.
For this reason, need to provide a kind of improved system of extracting lithium salts from sulphate lake.
Utility model content
The purpose of this utility model is to provide a kind of preparation system of Quilonum Retard.
Technical solution adopted in the utility model is:
The preparation system of high purity carbonic acid lithium, system comprises bittern condensing crystal device and treater, bittern condensing crystal device is provided with heat storage can and heating tank, heat storage can and heating tank are all independently provided with heat exchanger, the heat exchanger of heat storage can and heating tank is connected with release end of heat with the heat absorbing end of heat pump respectively, heating tank is provided with bittern entrance and tail halogen relief outlet, and tail halogen relief outlet is connected to heat storage can by pipeline; Treater comprises consummate tank, and consummate tank is provided with water outlet and water inlet, and bottom is provided with the radially filter screen for the crystallization of support Quilonum Retard in consummate tank, and consummate tank internal upper part is provided with the detachably filter screen radially that prevents that Quilonum Retard crystallization from flowing out.
As further improvement of the utility model, bittern condensing crystal device is connected with vacuum extractor, and vacuum extractor is connected with steam condenser, and steam condenser is connected with the temporary tank of distilled water.Vacuum extractor can be extracted water vapor out, reduces the pressure of fluid surface, contributes to accelerate the concentrated of liquid.The water vapor of extracting out is through condensation, and by-product distilled water is specially adapted to lack the remote districts of pure water.
As further improvement of the utility model, bittern evaporation and the temporary tank of the distilled water reclaiming when concentrated are provided with the water-in that is connected to consummate tank.
As further improvement of the utility model, before tail halogen relief outlet, be provided with filter screen.
As further improvement of the utility model, between the water outlet of consummate tank and water inlet, be provided with recycle pump.
As further improvement of the utility model, treater is provided with heat exchanger.
As further improvement of the utility model, in heating tank, be provided with dismountable Inner filter net layer.
As further improvement of the utility model, consummate tank is provided with hot-air drying unit.Hot-air drying unit can be simply for being arranged on hot-wind inlet and the outlet of consummate tank.
As further improvement of the utility model, the water outlet of consummate tank is provided with T-valve, and one end of T-valve is connected to heat storage can by pipeline.
As further improvement of the utility model, before the water outlet of consummate tank, water inlet, be provided with filter screen.
The beneficial effects of the utility model are:
The utility model system, need not be used chemical reagent, by physical operations, can complete the consummate of Quilonum Retard, and the Quilonum Retard purity after consummate, up to more than 95%, contributes to the transportation cost that reduces the later stage to become the cost of further purifying.
The utility model system, utilizes vacuum extractor, can fully recycle the water vapor producing when salt lake brine evaporates, concentrates by condensed steam by-product distilled water, and be condensed into pure distilled water when acceleration bittern is concentrated.The distilled water obtaining can be further used for the purification of Quilonum Retard refined salt.Effectively solve the problem that remote Salt Lake Area lacks fresh water (distilled water), further reduced the cost of purifying.Distilled water, after using, can reenter salt lake, effectively to salt lake moisturizing, avoids or reduces the ecological problem that declines and cause because of salt lake water level.
System of the present utility model, easy to use, can prepare highly purified Quilonum Retard.Meanwhile, can be in heat storage can by-product natrium potassium salt.
System of the present utility model, without the extra chemicals that supplements, energy utilization rate is high.
Accompanying drawing explanation
Fig. 1 is the structural representation of the utility model system condensing crystal device;
Fig. 2 is the structural representation of the utility model system treater.
Embodiment
See figures.1.and.2, the preparation system of high purity carbonic acid lithium, comprise bittern condensing crystal device and treater, bittern condensing crystal device is provided with heat storage can 1 and heating tank 2, heat storage can 1 and heating tank 2 are all independently provided with heat exchanger 41, the heat exchanger of heat storage can 1 and heating tank 2 is connected with release end of heat with the heat absorbing end of heat pump 4 respectively, and heating tank 2 is provided with bittern entrance 21 and tail halogen relief outlet 22, and tail halogen relief outlet 22 is connected to heat storage can 1 by pipeline; Treater comprises consummate tank 3, and consummate tank is provided with water outlet 32 and water inlet 31, and the interior bottom of consummate tank 3 is provided with the radially filter screen 33 for the crystallization of support Quilonum Retard, and consummate tank 3 internal upper parts are provided with the detachably filter screen 34 radially that prevents that Quilonum Retard crystallization from flowing out.
As further improvement of the utility model, bittern condensing crystal device is connected with vacuum extractor 5, and vacuum extractor 5 is connected with steam condenser, and steam condenser is connected with the temporary tank 6 of distilled water.Vacuum extractor can be extracted water vapor out, reduces the pressure of fluid surface, contributes to accelerate the concentrated of liquid.The water vapor of extracting out is through condensation, and by-product distilled water is specially adapted to lack the remote districts of pure water.
As further improvement of the utility model, the temporary tank 6 of distilled water is provided with the water-in 31 that is connected to consummate tank.Certain, in order to improve consummate efficiency, before distilled water is imported to consummate tank, distilled water can be preheated to temperature required.Further, treater is provided with heat exchanger 41, to guarantee that the temperature in tank keeps stable when rinsing.Heat exchanger 41 both can be arranged in consummate tank, also can be arranged in outside pipeline or recycle pump, more preferably can be arranged in distilled water storage tank, or in a plurality of positions, arrange simultaneously, and while guaranteeing to rinse, the temperature of distilled water remains on required temperature.
As further improvement of the utility model, before tail halogen relief outlet, be provided with filter screen, can avoid like this, when discharging tail halogen, Quilonum Retard crystallization refined salt being taken out of, affect yield.
As further improvement of the utility model, in heating tank, be provided with dismountable Inner filter net layer.Can guarantee that so most Quilonum Retard crystallizations are all deposited in filter screen, can easily the Quilonum Retard obtaining be taken out.The Quilonum Retard taking out can be transferred to consummate tank and be further purified.
As further improvement of the utility model, between the water outlet 32 of consummate tank and water inlet 31, be provided with recycle pump 7.Hot water circulation can be rinsed to Quilonum Retard crystallization refined salt like this, accelerate purifying process.The water that recycle pump is discharged preferably upwards rinses Quilonum Retard crystallization refined salt from bottom, can avoid crystallization deposition like this, and bottom crystallization is difficult to be flushed to, and affects purification effect.Certainly, also can adopt other backwashing manners, as rinsed from top to bottom, spin rinse etc., or multiple backwashing manner combines.
As further improvement of the utility model, consummate tank is provided with hot-air drying unit.Hot-air drying unit can be simply for being arranged on hot-wind inlet and the outlet of consummate tank.Hot blast is preferably blown into from the bottom of Quilonum Retard crystallization, from top, blows out, like this can be quickly that the Quilonum Retard after purifying is dry.
As further improvement of the utility model, the water outlet of consummate tank is provided with T-valve, and one end of T-valve is connected to heat storage can by pipeline.T-valve can be controlled the flow direction of water easily as required.Rinse complete hot water and import in heat storage can, use afterwards heat pump utilization waste heat wherein, contribute to improve the utilization ratio of the energy, be specially adapted to remote districts.
As further improvement of the utility model, before the water outlet of consummate tank, water inlet, be provided with filter screen.Contribute to like this to prevent that crystallization from entering pipeline, the yield of the normal operation of the equipment that affects and Quilonum Retard.
The preparation method of high purity carbonic acid lithium, comprises the steps:
1) calcareous type salt lake brine is concentrated, heat up Quilonum Retard saturated crystallization is separated out afterwards, collect crystallization and obtain Quilonum Retard refined salt;
2) distilled water flushing reclaiming with 60 ℃ of above bittern evaporations with when concentrated is collected the Quilonum Retard refined salt obtaining, and dissolves natrium potassium salt wherein;
3) the dry high purity carbonic acid lithium that obtains.
Preferably, by reduction vaporization, salt lake brine is concentrated, be warming up to afterwards more than 60 ℃, preferably 65 ℃, 70 ℃ above insulations make Quilonum Retard crystallization.Temperature during crystallization is higher, is more conducive to separate out more highly purified Quilonum Retard refined salt, is conducive to reduce the difficulty of subsequent purification operation.
While using distilled water flushing Quilonum Retard refined salt to its quality to be reduced to without obvious minimizing.Generally speaking, Quilonum Retard refined salt be flushed to quality be reduced to its proper mass (dry weight) 20~30% time, its quality is basicly stable, can't be because of continuing to rush Xian 1~2 hour significantly reduces.In this case, the meaning that continues to rinse can not significantly improve the purity of finished product high purity carbonic acid lithium, can stop rinsing, and to save water and other energy, enhances productivity simultaneously.
Preferably, when rinsing, regularly switch and rinse direction.As changed and rinse direction every 10 seconds, 20 seconds, be more conducive to improve flush efficiency, prevent Crystallization Plugging filter screen simultaneously.
embodiment 1:
Li ionic concn 1.29g/L bittern, the 60 ℃ of above thick lithium salts of crystallization and bittern mixing wet salts issued additional, 897.6g weighs after simple removal supernatant liquor, with 80 ℃ of disposable mixing of distilled water 3000g, fully stir afterwards 3 minutes, through suction filtration and oven dry, obtain purity and be 62% Quilonum Retard 47.4g, from thick lithium salts, obtaining Quilonum Retard yield is 73.5%.
embodiment 2:
Li ionic concn 1.29g/L bittern, the 60 ℃ of above thick lithium salts of crystallization and bittern mixing wet salts issued additional, 877.9g weighs after simple removal supernatant liquor, with 70 ℃ of distilled water 2250g, with 1200g, 600g, 300g, 150g, in embodiment 1 mode, rinse for 4 times altogether respectively, each fully stirring amounts to 2 minutes in 30 seconds, obtains dry purity and be 91.3% Quilonum Retard 37.56g through suction filtration and after drying, and from thick lithium salts, obtaining Quilonum Retard yield is 85.7%.
embodiment 3:
Li ionic concn 1.29g/L bittern, the 60 ℃ of above thick lithium salts of crystallization and bittern mixing wet salts issued additional, 986.7g weighs after simple removal supernatant liquor, be placed in consummate tank, add 90 ℃ of distilled water 1800g, within every 10 seconds, change first power to iterative cycles 1 minute, passing into and after warm air dries up, obtaining dry purity is 97.6% Quilonum Retard 39.74g, and from thick lithium salts, obtaining Quilonum Retard yield is 96.97%.
From the data of above-described embodiment, the purification link that consummate tank can be fast, water-saving continues to carry out Quilonum Retard refined salt.Change direction is rinsed, and both can improve flush efficiency, has also avoided accumulation crystallization in pipeline or consummate tank, can realize automatically cleaning, facilitates the use of equipment, also contributes to reduce and safeguards.
The purification operations time of this link to Quilonum Retard crude salt, tapered to 1/3rd of traditional method; Self-cleaning designs traditional scouring mode must frequent maintenance disadvantage; The amount of flushing distilled water used has tapered to 60% of traditional method, and has avoided the systematicness loss of Quilonum Retard in traditional technology, has obtained grade more than 97%, the particularly preferred lithium carbonate product of more than 96% purity of yield.

Claims (9)

1. the preparation system of high purity carbonic acid lithium, it is characterized in that: described system comprises bittern condensing crystal device and treater, bittern condensing crystal device is provided with heat storage can and heating tank, heat storage can and heating tank are all independently provided with heat exchanger, the heat exchanger of heat storage can and heating tank is connected with release end of heat with the heat absorbing end of heat pump respectively, heating tank is provided with bittern entrance and tail halogen relief outlet, and tail halogen relief outlet is connected to heat storage can by pipeline; Treater comprises consummate tank, and consummate tank is provided with water outlet and water inlet, and bottom is provided with the radially filter screen for the crystallization of support Quilonum Retard in consummate tank, and consummate tank internal upper part is provided with the detachably filter screen radially that prevents that Quilonum Retard crystallization from flowing out.
2. preparation system according to claim 1, is characterized in that: bittern condensing crystal device is connected with vacuum extractor, and vacuum extractor is connected with steam condenser, and steam condenser is connected with the temporary tank of distilled water.
3. preparation system according to claim 1, is characterized in that: the temporary tank of distilled water is provided with the water-in that is connected to consummate tank.
4. preparation system according to claim 1, is characterized in that: between the water outlet of consummate tank and water inlet, be provided with recycle pump.
5. preparation system according to claim 1, is characterized in that: treater is provided with heat exchanger.
6. preparation system according to claim 1, is characterized in that: in heating tank, be provided with dismountable Inner filter net layer.
7. preparation system according to claim 1, is characterized in that: before tail halogen relief outlet, be provided with filter screen.
8. according to the preparation system described in claim 1~7 any one, it is characterized in that: consummate tank is provided with hot-air drying unit.
9. according to the preparation system described in claim 1~7 any one, it is characterized in that: the water outlet of consummate tank is provided with T-valve, one end of T-valve is connected to heat storage can by pipeline.
CN201320568542.XU 2013-09-13 2013-09-13 Preparation system of high-purity lithium carbonate Withdrawn - After Issue CN203513300U (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103482660A (en) * 2013-09-13 2014-01-01 西藏金睿资产管理有限公司 Method and system for preparing high-purity lithium carbonate
WO2015035929A1 (en) * 2013-09-13 2015-03-19 西藏金睿资产管理有限公司 Highly effective thermal energy recovery method and system, and high-purity lithium carbonate preparation method and system based on same
CN108176124A (en) * 2018-02-09 2018-06-19 上海安赐环保科技股份有限公司 A kind of filtration system and its technique applied to the washing of carbonic acid powder for lithium
CN108283831A (en) * 2018-04-11 2018-07-17 宜春市鼎鑫高能科技有限公司 A kind of filter-pressing device and lithium carbonate production equipment
CN114288694A (en) * 2021-12-31 2022-04-08 天津农学院 Flash steam compression type continuous crystallization system and process for high-purity lithium carbonate
WO2024066297A1 (en) * 2022-09-30 2024-04-04 比亚迪股份有限公司 Energy supply system suitable for salt lake lithium extraction and method for supplying energy by using same

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103482660A (en) * 2013-09-13 2014-01-01 西藏金睿资产管理有限公司 Method and system for preparing high-purity lithium carbonate
WO2015035929A1 (en) * 2013-09-13 2015-03-19 西藏金睿资产管理有限公司 Highly effective thermal energy recovery method and system, and high-purity lithium carbonate preparation method and system based on same
CN103482660B (en) * 2013-09-13 2015-06-24 西藏金睿资产管理有限公司 Method and system for preparing high-purity lithium carbonate
CN108176124A (en) * 2018-02-09 2018-06-19 上海安赐环保科技股份有限公司 A kind of filtration system and its technique applied to the washing of carbonic acid powder for lithium
CN108283831A (en) * 2018-04-11 2018-07-17 宜春市鼎鑫高能科技有限公司 A kind of filter-pressing device and lithium carbonate production equipment
CN114288694A (en) * 2021-12-31 2022-04-08 天津农学院 Flash steam compression type continuous crystallization system and process for high-purity lithium carbonate
WO2024066297A1 (en) * 2022-09-30 2024-04-04 比亚迪股份有限公司 Energy supply system suitable for salt lake lithium extraction and method for supplying energy by using same

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