CN108149030A - A kind of extraction equipment and extraction process of highly effective integration lithium ion - Google Patents
A kind of extraction equipment and extraction process of highly effective integration lithium ion Download PDFInfo
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- CN108149030A CN108149030A CN201711129737.3A CN201711129737A CN108149030A CN 108149030 A CN108149030 A CN 108149030A CN 201711129737 A CN201711129737 A CN 201711129737A CN 108149030 A CN108149030 A CN 108149030A
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- extraction
- membrane contactor
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- stoste
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/02—Apparatus therefor
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/40—Mixtures
- C22B3/409—Mixtures at least one compound being an organo-metallic compound
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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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of extraction equipments and extraction process of highly effective integration lithium ion, belong to technical field of inorganic chemical industry.The extraction equipment includes the membrane contactor of about three series connection, and stoste area, extraction section and the scrolling mechanism for being stripped area will be divided into membrane contactor from left to right, the in-house amberplex that scrolls is installed on, further includes and forms the stoste case of reflux, extraction liquid case, back extraction liquid case with stoste area, extraction section, back extraction area respectively.The extraction process includes fluid pre-extracted and classification quintessence takes, and for fluid pre-extracted by the way that the fluid of stoste, extract liquor and anti-stripping agent flow velocity is controlled to obtain suitable extraction ratio, classification quintessence, which takes, by the stage supplements or add adminicle progress fractional extraction.In short, present device is small, continuity is high, extractant not easily runs off, good operation stability.
Description
Technical field
The invention belongs to technical field of inorganic chemical industry, and in particular to a kind of extraction equipment and extraction of highly effective integration lithium ion
Taking technique.
Background technology
Lithium is the important rare element for promoting the development of the related industries such as modernization construction and science and technology, is most potential
One of a kind of novel energy and strategic resource are widely used in high power lithium battery, rubber industry, aerospace, ceramics, swash
The numerous areas such as light, medicine, welding, explosive, cement, smelting and new energy are known as " energy metal of 21 century " by reputation.Especially
It is the energy that 1g lithiums are released by thermonuclear reaction in new energy field, is equivalent to more than 20,000 tons of high-quality coal combustion and is produced
Raw energy, lithium ion battery and nuclear fusion power generation are the hot spot directions nowadays studied, in view of it is in atomic energy industry
Special performance is otherwise known as " high-energy metals ".Many countries have made lithium from economic development needs and the consideration of national security angle
For strategic reserves substance and carry out extensively using technical research.
China is a big country with abundant lithium resource, and the lithium resource reserves that oneself verifies occupy the second in the world, especially
Liquid lithium ore resources are very abundant, account for the 87% of national gross reserves, are mainly distributed on Qinghai, Tibet, Xinjiang and four, the Inner Mongol
Just oneself gross reserves verified is suitable at present with other countries of the world for province, the only prospective reserves of Qinghai and Tibetan Salt Lakes brine lithium,
It is and precious with very high extraction value and huge potential economic benefit and the valuable source of China's Future Development lithium salts industry
Library.But the lithium product especially lithium carbonate in China still depends on import at present, there are no ripe salt lake bitterns to carry
The industrialized unit of lithium.Therefore, it is necessary to strengthen the exploitation of China's brine lithium resource, promote the fast development of China's lithium salts industry.
At present, mainly there is the extractive technique of some following lithiums：
(1) precipitation method：The precipitation method are with making purpose ion selectivity in solution by precipitating reagent in insoluble compound shape
The process of state Precipitation, including carbonate precipitation method, aluminic acid salt precipitation method and hydrated sulfuric acid lithium crystalline deposit method.Wherein apply
Most extensive and most ripe is carbonate precipitation method, and basic principle is first with highly basic as in sodium hydroxide pellets concentrated brine
Calcium and magnesium impurity, then lithium ion is precipitated as lithium carbonate with carbonate, so as to achieve the purpose that separating Li.The method is simple for process, can
By property height, suitable for the salt lake bittern of low Mg/Li ratio.
(2) ion exchange adsorption:Ion exchange adsorption includes the attached technology of organic ion-exchange absorption and inorganic ions is handed over
Adsorption technology is changed, basic principle is the lithium ion utilized in adsorbent adsorbent solution, then lithium ion is eluted, so as to reach
To the purpose of separation.The method is simple for process, selectivity is good, the rate of recovery is high and has fewer environmental impacts, suitable for from low-grade
Extracting lithium from salt lake brine.But restraining factors suffered by the method are more, such as the selectivity of adsorbent, cyclic utilization rate, cost, preparation
Method etc..
(3) carbonizatin method：Carbonizatin method Main Basiss lithium carbonate reacts the larger carbonic acid of generation solubility with carbon dioxide and water
This principle of hydrogen lithium is by the lithium in brine and other element sepatations.The method be suitable for low younger sister's lithium than salt lake bittern, feature exists
In product purity height, it is easy to continuous production, but there is also the problems such as technological process is longer, energy consumption is big.
(4) extraction：Developed the 1980s where Chinese Academy of Sciences Qinghai Salt Lake with TBP systems be neutral ligand from
The technology of lithium chloride is directly extracted in high magnesium lithium salts lake bittern water using solvent extraction.The experimental results showed that lithium extraction yield reaches
99.2%, lithium chloride purity (mass fraction) is 99.0%, and total recovery is more than 90%.But extraction process flow is long, extraction is set
Standby bulky, material burn into poor continuity, extractant such as are easy to run off at the reasons during hybrid separation, cause achievement could not
It promotes.
Invention content
For more than technical problem, the present invention provides a kind of extraction equipment of highly effective integration lithium ion, can solve to extract
Taking equipment is bulky, poor continuity, extractant cause equipment not to be durable when being easy to run off during hybrid separation and because corrosion
The technical issues of.
The technical scheme is that：A kind of extraction equipment of highly effective integration lithium ion, membrane contactor, stoste case, extraction
Liquid case, back extraction liquid case, condensing crystallizing device, condensate recycling device and lithium salts case are taken, it is identical that the membrane contactor is divided into specification
Top membrane contactor, middle part membrane contactor, bottom membrane contactor, membrane contactor include reactor shell, scrolling mechanism, ion and hand over
Film and heating stirring mechanism are changed, totally two, the mechanism of scrolling, longitudinal direction is equidistant respectively and is removably mounted at reactor shell
Inside, and stoste area, extraction section and back extraction area will be in turn divided into inside reactor shell from left to right, the stoste area,
Import is respectively equipped with above extraction section and back extraction area, outlet is respectively arranged below with, sealing valve is equipped in the outlet, in
The import 114 of portion membrane contactor 1b is connected with the outlet of top membrane contactor, and the import of bottom membrane contactor is contacted with middle part film
The outlet of device is connected, and the amberplex is mounted between scrolling mechanism, and can be described by scrolling above and below the mechanism that scrolls
Heating stirring mechanism is respectively fixedly connected in the stoste area, extraction section and the bottom centre position for being stripped area, the stoste
Case is connected respectively by pumping with the stoste area of the top membrane contactor, the stoste area of the bottom membrane contactor, the extraction
Liquid case is connected respectively by pumping with the extraction section of top membrane contactor, the extraction section of bottom membrane contactor, the back extraction liquid case
It is connected respectively by pumping with the back extraction area of top membrane contactor, the back extraction area of bottom membrane contactor, the condensing crystallizing device
It is connected between the back extraction area of bottom membrane contactor and back extraction liquid case by triple valve, the condensate recycling device and concentration
It is connected above crystallizer, back extraction liquid case is recycled to after gas is condensed, the lithium salts case is connected to the lower section of condensing crystallizing device.
Further, the scrolling mechanism includes upper shell, lower shell, drive roll, driven voller, connecting tube one, connecting tube
2nd, reeling driver and power pack, the drive roll are located at the horizontal axis center of the lower shell, and drive roll is with driven voller
Hollow shaft and equal length, the right end of drive roll are connected with the output shaft of the reeling driver, and the power pack is located at actively
The left end of roller, and pass through conducting wire and provide electric energy for reeling driver across drive roll inside, the driven voller is arranged on described
The horizontal axis center of cylinder, the top of upper shell are equipped with film import parallel and equal length with drive roll, the bottom of lower shell
Portion is exported equipped with film parallel and equal length with driven voller, and the connecting tube one and connecting tube two are respectively equipped with inner groovy and outer
Groove is detachably connected on respectively between upper shell and lower shell both ends, and the inner groovy is the movement of the amberplex
Track, the outside groove are connected to by clamping or guide rail on the reactor shell inner wall, because amberplex will be with
Organic extraction is mutually in direct contact, and is easily corroded, and is unfavorable for the longtime running of equipment, and a large amount of ion exchanges are prestored in the mechanism that scrolls
Film substantially increases the service life of equipment, while also ensured the Effec-tive Function of extraction process, it can be achieved that scrolling changes film.
Further, the inner groovy and the width of external groove ratio are 1:5-10, inner groovy are used for amberplex
It is fixed and is oriented to, it is too small easily stuck, film both sides liquid is easily made mutually to flow greatly very much.
Further, the scrolling mechanism is the disposable apparatus handled through waterproof and anticorrosion, and material can be used corrosion-resistant
High molecular material, in order to ensure that internal component is without damage, and scroll mechanism in wound membrane amount can run support long enough when
Between, recycling must be dismantled and be installed again, then the mechanism that scrolls leakproofness is then damaged, and be unfavorable for holding for reaction
It is continuous to carry out.
Further, the heating stirring mechanism includes capsul, heater, heat resisting motor and T-shaped stirring rod, described
The bottom of capsul is fixed on the stoste area, extraction section and the bottom centre position for being stripped area, the heater and Nai Gao
Warm motor is located inside capsul side by side, and passes through capsul and stoste area, extraction section and the bottom and the external electrical that are stripped area
Source is connected, and the T-shaped stirring rod is located at capsul top, and the perpendicular section bottom end of T-shaped stirring rod and the output of heat resisting motor
Axis is connected, and T-shaped stirring rod is internally provided with heating seal wire, and the heating seal wire is connected with heater, and heating and stirring can carry
High extraction yield.
Further, the import of the same membrane contactor is dislocated with outlet, can improve interior stoste area, extraction
The remaining time of each liquid in area, back extraction area, and then increase the contact area of remaining amberplex, improve extraction yield.
Further, the top membrane contactor, middle part membrane contactor, the extraction section of bottom membrane contactor and back extraction area
Top is connected with addition box and supply container by proportioning valve respectively, adds assistance extract to extraction section by adding box, passes through
Supply container back extraction area supplements pure anti-stripping agent, is for reducing the saturation degree of extract liquor and pure back extraction, and then improves extraction
Take rate.
A kind of extraction process using extraction equipment extraction lithium ion includes the following steps：
Mono- Walk：Fluid pre-extracted
S1：Open whole sealing valves, and set the back extraction liquid zone of the triple valve connection bottom membrane contactor with it is anti-
Extract liquid case；
S2：From the stoste case, extraction liquid case, back extraction liquid case extract stoste, extract liquor, anti-stripping agent, from it is described into
Mouth is flowed into top membrane contactor, middle part membrane contactor, stoste area, extraction section and back extraction in the membrane contactor of bottom successively
Area finally from the outlet return to stoste case, extraction liquid case, back extraction liquid case, while uses the heating stirring mechanism pair
Liquid is heated in stoste area, extraction section and back extraction area, and temperature is 30-50 DEG C, total duration 30-60min, wherein, it is former
Liquid, extract liquor, anti-stripping agent flow velocity be followed successively by 2-3m/min, 4-5m/min, 6-7m/min；
Second step:Classification quintessence takes
S1:By top membrane contactor, middle part membrane contactor in the first step, stoste area in the membrane contactor of bottom, extraction section and
The liquid in back extraction area is back to stoste case, extraction liquid case, back extraction liquid case respectively, empties all membrane contactors, and closes complete
The sealing valve in portion；
S2:It is 3 to extract volume ratio from stoste case, extraction liquid case, back extraction liquid case:2:1 stoste, extract liquor, back extraction
In liquid to top membrane contactor, mixed liquor is added to its corresponding extraction section by the addition box above the membrane contactor of top
The volume ratio of body one, the mixing liquid one and the extract liquor is 1:8-10, while pass through the institute above the membrane contactor of top
It states supply container and supplements pure anti-stripping agent, the volume ratio of the pure anti-stripping agent and the anti-stripping agent to its corresponding back extraction area
It is 1:5-6 is 30-50 degree by heating stirring mechanism heats to temperature, stirs 2-3min, rotating speed 200-300r/min；
S3：All sealing valves below the membrane contactor of top are opened, by liquid drain to middle part membrane contactor, and are passed through
Addition box above the membrane contactor of middle part adds mixing liquid two, the mixing liquid two and the extraction to its corresponding extraction section
The volume ratio for taking liquid is 1:12-15, while supplemented by the supply container above the membrane contactor of middle part to its corresponding back extraction area
The volume ratio of pure anti-stripping agent, the pure anti-stripping agent and the anti-stripping agent is 1:7-8, by heating stirring mechanism heats extremely
Temperature is 30-50 degree, stirs 4-5min, rotating speed 300-400r/min；
S4：All sealing valves below the membrane contactor of middle part are opened, by liquid drain to bottom membrane contactor, and are passed through
Addition box above the membrane contactor of bottom adds mixing liquid three, the mixing liquid three and the extraction to its corresponding extraction section
The volume ratio for taking liquid is 1:18-20, while supplemented by the supply container above the membrane contactor of bottom to its corresponding back extraction area
The volume ratio of pure anti-stripping agent, the pure anti-stripping agent and the anti-stripping agent is 1:9-10 passes through heating stirring mechanism heats
It is 30-50 degree to temperature, stirs 5-6min, rotating speed 400-500r/min；
S5：By the back extraction liquid zone of triple valve connection bottom membrane contactor and the condensing crystallizing device, bottom is then opened
All sealing valves below membrane contactor, by liquid in the stoste area of bottom membrane contactor, extraction section be pumped to respectively stoste case,
Liquid case is extracted, and lithium-containing solution in the back extraction area of bottom membrane contactor is drained in condensing crystallizing device；
S6：Above-mentioned S2-S5 steps are repeated, finally using condensing crystallizing device by lithium-containing solution evaporative crystallization, obtained gas warp
The back extraction liquid case is back to after the condensate recycling device condensation, obtained crystal is sent into the lithium salts case.
Further, it is 1 that the mixing liquid one, which is volume ratio,:1:2 extractant, synergic reagent, sustained release agent；The mixing
Liquid two is that volume ratio is 3:2:5 extractant, synergic reagent, sustained release agent；It is 4 that the mixing liquid three, which is volume ratio,:1:5 extraction
Take agent, synergic reagent, sustained release agent.
Compared with prior art, beneficial effects of the present invention are：
(1) present invention extracts lithium ion using the form of membrane contactor, combines the highly selective and film of extraction
The separation function of material so that extraction and back extraction can be carried out at the same time, due to avoiding the direct of organic extractant phase and water phase
Contact also avoids mixing of the organic phase with water phase with detaching the problem of caused extractant is lost in this.
(2) present invention is that membrane contactor is carried out subregion, and amberplex is mounted in by amberplex
In the mechanism that scrolls, by prestoring a large amount of amberplexes, it can be achieved that scrolling changes film in scrolling mechanism, solves ion exchange
Film substantially increases the service life of equipment, simultaneously because of the problem of being in direct contact with machine extraction phase, easily corrode, need to be replaced frequently
Also the Effec-tive Function of extraction process has been ensured.
(3) present invention is by the way that the import of membrane contactor to be arranged to be dislocated with outlet, for improving interior stoste area, extraction
It takes area, be stripped the remaining time of each liquid in area, and then increase the contact area of remaining amberplex, improve extraction yield.
(4) present invention is connected using three membrane contactors, by controlling stoste, extraction in the fluid pre-extracted of the first step
Liquid, anti-stripping agent flow velocity, and then the contact unit amount of three is controlled, reach reasonable extraction ratio；In the classification of second
Quintessence take in by control batch close sealing valve, and pass through add box to extraction section add assist extract, pass through supply container
It is stripped area and supplements pure anti-stripping agent, be for reducing the saturation degree of extract liquor and pure back extraction, and then improve extraction yield；Its
In, by the successional fluid pre-extracted of the first step, the time that second part grade quintessence takes each can be reduced so that entire technique
Flow keeps continuity run.
In short, the present invention has many advantages, such as that equipment volume is small, continuity is high, extractant not easily runs off, good operation stability,
With good marketing meaning.
Description of the drawings
Fig. 1 is the overall structure diagram of the present invention；
Fig. 2 is the scrolling mechanism longitudinal sectional view of the present invention；
Fig. 3 is Section A-A sectional view in Fig. 2；
Fig. 4 is the structure diagram of the heating stirring mechanism of the present invention.
Wherein, 1- membrane contactors, 1a- tops membrane contactor, 1b- middle parts membrane contactor, 1c- bottoms membrane contactor, 11- are anti-
Answer device housing, 111- stostes area, 112- extraction sections, 1121- addition box, 113- back extraction area, 1131- supply containers, 114- imports,
115- outlets, 116- sealing valves, 12- scrolling mechanism, 121- upper shells, the import of 1211- films, 122- lower shells, 1221- films go out
Mouth, 123- drive rolls, 124- driven vollers, 125- connecting tubes one, 1251- inner groovies, 1252- external grooves, 126- connecting tubes two,
127- reeling drivers, 128- power packs, 13- amberplexes, 14- heating stirrings mechanism, 141- capsuls, 142- heating
Device, 143- heat resisting motors, 144-T types stirring rod, 145- thermal conductivities silk, 2- stostes case, 3- extract liquid case, 4- is stripped liquid case,
5- condensing crystallizings device, 6- condensate recycling devices, 7- lithium salts case, 8- pumps, 9- triple valves.
Specific embodiment
In order to more fully explain the present invention, the present invention is described further below by attached drawing 1-4.
Embodiment 1
As shown in Figure 1, a kind of extraction equipment of highly effective integration lithium ion, membrane contactor 1, stoste case 2, extraction liquid case 3,
Back extraction liquid case 4, condensing crystallizing device 5, condensate recycling device 6 and lithium salts case 7, membrane contactor 1 divide the top-film identical for specification
Contactor 1a, middle part membrane contactor 1b, bottom membrane contactor 1c, membrane contactor 1 include reactor shell 11, scrolling mechanism 12,
Amberplex 13 and heating stirring mechanism 14, scroll totally two, mechanism 12, and longitudinal direction is equidistant respectively and is removably mounted at anti-
It answers inside device housing 11, and stoste area 111, extraction section 112 and anti-will be in turn divided into inside reactor shell 11 from left to right
Extraction section 113.Wherein, scrolling mechanism 12 is the disposable apparatus handled through waterproof and anticorrosion, and corrosion resistant high score can be used in material
Sub- material, in order to ensure that internal component is without damage, and wound membrane amount can run support enough for a long time in the mechanism 12 that scrolls, weight
Multiple using that must be dismantled and installed again, 12 leakproofness of the mechanism that then scrolls then is damaged, and is unfavorable for continuing for reaction
It carries out.
As shown in Fig. 2, scrolling mechanism 12 includes upper shell 121, lower shell 122, drive roll 123, driven voller 124, connection
Pipe 1, connecting tube 2 126, reeling driver 127 and power pack 128, drive roll 123 are located at the horizontal axis center of lower shell 122
Position, drive roll 123 and driven voller 124 are hollow shaft and equal length, right end and the reeling driver 127 of drive roll 123
Output shaft is connected, and power pack 128 is located at the left end of drive roll 123, and passes through conducting wire and driven across 123 inside of drive roll for spool
Device 127 provides electric energy, and driven voller 124 is arranged on the horizontal axis center of upper shell 121, and the top of upper shell 121 is equipped with and master
Dynamic roller 123 is parallel and film import 1211 of equal length, and the bottom of lower shell 122 is equipped with driven voller 124 parallel and length phase
Deng film outlet 1221.As shown in figure 3, connecting tube 1 and connecting tube 2 126 are respectively equipped with inner groovy 1251 and external groove
1252, the width ratio of inner groovy 1251 and external groove 1252 is 1:5, inner groovy 1251 is used to that amberplex 13 to be fixed
And be oriented to, it is too small easily stuck, film both sides liquid is easily made mutually to flow greatly very much.It is detachably connected on upper shell 121 and lower cylinder respectively
Between 122 both ends of body, inner groovy 1251 is the moving track of amberplex 13, and outside groove 1252 is connected by clamping or guide rail
It is connected on 11 inner wall of reactor shell, because amberplex 13 will be mutually in direct contact with organic extraction, easily corrodes, be unfavorable for
The longtime running of equipment prestores a large amount of amberplexes 13, it can be achieved that scrolling changes film in the mechanism 12 that scrolls, substantially increases and set
The standby service life, while also ensured the Effec-tive Function of extraction process.
As shown in Figure 1, the top in stoste area 111, extraction section 112 and back extraction area 113 is respectively equipped with import 114, lower section
Outlet 115 is respectively equipped with, is equipped with sealing valve 116 in outlet 115, the import 114 of middle part membrane contactor 1b is contacted with top-film
The outlet 115 of device 1a is connected, and the import 114 of bottom membrane contactor 1c is connected with the outlet 115 of middle part membrane contactor 1b, wherein,
The import 114 of same membrane contactor 1 is dislocated with outlet 115, can improve interior stoste area 111, extraction section 112, back extraction
The remaining time of each liquid in area 113, and then increase the contact area of remaining amberplex 13, improve extraction yield.Ion is handed over
It changes film 1 to be mounted between scrolling mechanism 12, and can be by the mechanism scrolling about 12 that scrolls, heating stirring mechanism 14 is fixed respectively
Stoste area 111, extraction section 112 and the bottom centre position for being stripped area 113 are connected to, as shown in figure 4, heating stirring mechanism 14
Including capsul 141, heater 142, heat resisting motor 143 and T-shaped stirring rod 144, the bottom of capsul 141 is fixed on stoste
Area 111, extraction section 112 and the bottom centre position for being stripped area 113, heater 142 and heat resisting motor 143 are located at close side by side
Inside capsule 141, and pass through capsul 141 and stoste area 111, extraction section 112 and the bottom and the external power supply that are stripped area 113
It is connected, T-shaped stirring rod 144 is located at 141 top of capsul, and the perpendicular section bottom end of T-shaped stirring rod 144 and heat resisting motor 143
Output shaft be connected, T-shaped stirring rod 144 be internally provided with heating seal wire 145, heating seal wire 145 be connected with heater 142, add
Heat and stirring can improve extraction yield.
As shown in Figure 1, stoste case 2 passes through the stoste area 111 of pump 8 and top membrane contactor 1a, bottom membrane contactor respectively
The stoste area 111 of 1c is connected, and extraction liquid case 3 is contacted respectively by the extraction section 112 of pump 8 and top membrane contactor 1a, bottom film
The extraction section 112 of device 1c is connected, and back extraction liquid case 4 passes through back extraction area 113, the bottom of pump 8 and top membrane contactor 1a respectively
The back extraction area 113 of membrane contactor 1c is connected, wherein, top membrane contactor 1a, middle part membrane contactor 1b, bottom membrane contactor 1c
Extraction section 112 and back extraction area 113 top addition box 1121 and supply container 1131 are connected with by proportioning valve respectively, by adding
Box 1121 is added to be added to extraction section 112 and assists extract, being stripped area 113 by supply container 1131 supplements pure anti-stripping agent,
It is the saturation degree in order to reduce extract liquor and pure back extraction, and then improves extraction yield.Condensing crystallizing device 5 is connected by triple valve 9
Between the back extraction area 113 of bottom membrane contactor 1c and back extraction liquid case 4, condensate recycling device 6 and 5 top of condensing crystallizing device
It is connected, back extraction liquid case 4 is recycled to after gas is condensed, lithium salts case 7 is connected to the lower section of condensing crystallizing device 5.
Technique using the extraction equipment extraction lithium ion of the present embodiment includes the following steps：
Mono- Walk：Fluid pre-extracted
S1：Whole sealing valves 116 is opened, and the back extraction liquid zone 113 of the connection of triple valve 9 bottom membrane contactor 1c is set
With being stripped liquid case 4；
S2：Stoste, extract liquor, anti-stripping agent are extracted from stoste case 2, extraction liquid case 3, back extraction liquid case 4, from import 114
It is flowed into top membrane contactor 1a, middle part membrane contactor 1b, the stoste area 111 in the membrane contactor 1c of bottom, extraction section 112 successively
With back extraction area 113, stoste case 2, extraction liquid case 3, back extraction liquid case 4 finally are back to from outlet 115, while stir using heating
It mixes mechanism 14 to heat liquid in stoste area 111, extraction section 112 and back extraction area 113, temperature is 30 DEG C, and total duration is
30min, wherein, stoste, extract liquor, anti-stripping agent flow velocity be followed successively by 2m/min, 4m/min, 6m/min；
Second step:Classification quintessence takes
S1:By stoste area 111 in top membrane contactor 1a in the first step, middle part membrane contactor 1b, bottom membrane contactor 1c,
The liquid in extraction section 112 and back extraction area 113 is back to stoste case 2, extraction liquid case 3, back extraction liquid case 4 respectively, and emptying is all
Membrane contactor 1, and close whole sealing valves 116；
S2:It is 3 to extract volume ratio from stoste case 2, extraction liquid case 3, back extraction liquid case 4:2:1 stoste, extract liquor, back extraction
It takes in liquid to top membrane contactor 1a, by the addition box 1121 above the membrane contactor 1a of top to its corresponding extraction section 112
The volume ratio of addition mixing liquid one, mixing liquid one and extract liquor is 1:8, wherein, mixing liquid one is that volume ratio is 1:1:2
Extractant (triisopropyl phosphate), synergic reagent 1- butyl -3- methyl (limidazolium hexafluorophosphate), sustained release agent (n-hexane),
Pure anti-stripping agent is supplemented to its corresponding back extraction area 113 by the supply container 1131 above the membrane contactor 1a of top simultaneously
(1mol/LHCl solution), pure anti-stripping agent (1mol/LHCl solution) and the volume of anti-stripping agent (hydrochloric acid solution containing lithium ion)
Than being 1:5, it is 30 degree to be heated to temperature by heating stirring mechanism 14, stirs 2min, rotating speed 200r/min；
S3：All sealing valves 116 below the membrane contactor 1a of top are opened, by liquid drain to middle part membrane contactor 1b
It is interior, and pass through the addition box 1121 above the membrane contactor 1b of middle part and add mixing liquid two, mixing to its corresponding extraction section 112
The volume ratio of liquid two and extract liquor is 1:12, wherein, mixing liquid two is that volume ratio is 3:2:5 extractant (triisopropyl
Phosphate), synergic reagent 1- butyl -3- methyl (limidazolium hexafluorophosphate), sustained release agent (n-hexane), while contacted by middle part film
Supply container 1131 above device 1b supplements pure anti-stripping agent (1mol/LHCl solution), pure back extraction to its corresponding back extraction area 113
The volume ratio for taking liquid (1mol/LHCl solution) and anti-stripping agent (hydrochloric acid solution containing lithium ion) is 1:7, pass through heating stirring machine
It is 40 degree that structure 14, which is heated to temperature, stirs 4min, rotating speed 300r/min；
S4：All sealing valves 116 below the membrane contactor 1b of middle part are opened, by liquid drain to bottom membrane contactor 1c
It is interior, and pass through the addition box 1121 above the membrane contactor 1c of bottom and add mixing liquid three, mixing to its corresponding extraction section 112
The volume ratio of liquid three and extract liquor is 1:18, wherein, mixing liquid three is that volume ratio is 4:1:5 extractant (triisopropyl
Phosphate), synergic reagent 1- butyl -3- methyl (limidazolium hexafluorophosphate), sustained release agent (n-hexane), while contacted by bottom film
Supply container 1131 above device 1c supplements pure anti-stripping agent (1mol/LHCl solution), pure back extraction to its corresponding back extraction area 113
The volume ratio for taking liquid (1mol/LHCl solution) and anti-stripping agent (hydrochloric acid solution containing lithium ion) is 1:9, pass through heating stirring machine
It is 50 degree that structure 14, which is heated to temperature, stirs 5min, rotating speed 400r/min；
S5：Triple valve 9 is connected into the back extraction liquid zone 113 of bottom membrane contactor 1c and condensing crystallizing device 5, then opens bottom
All sealing valves 116 below portion membrane contactor 1c, by liquid in the stoste area 111 of bottom membrane contactor 1c, extraction section 112 point
It is not pumped to stoste case 2, extraction liquid case 3, and lithium-containing solution in the back extraction area 113 of bottom membrane contactor 1c is drained to concentration
In crystallizer 5；
S6：Above-mentioned S2-S5 steps are repeated, finally using condensing crystallizing device 5 by lithium-containing solution evaporative crystallization, obtained gas warp
Condensate recycling device 6 is back to back extraction liquid case 4 after condensing, obtained crystal is sent into lithium salts case 7.
Test result：Lithium extraction yield is up to 99.3%, and lithium chloride purity (mass fraction) is 99.2%, total recovery 91%.
Embodiment 2
The present embodiment is substantially the same manner as Example 1, the difference lies in：
Technique using the extraction equipment extraction lithium ion of embodiment 1 includes the following steps：
Mono- Walk：Fluid pre-extracted
S1：Whole sealing valves 116 is opened, and the back extraction liquid zone 113 of the connection of triple valve 9 bottom membrane contactor 1c is set
With being stripped liquid case 4；
S2：Stoste, extract liquor, anti-stripping agent are extracted from stoste case 2, extraction liquid case 3, back extraction liquid case 4, from import 114
It is flowed into top membrane contactor 1a, middle part membrane contactor 1b, the stoste area 111 in the membrane contactor 1c of bottom, extraction section 112 successively
With back extraction area 113, stoste case 2, extraction liquid case 3, back extraction liquid case 4 finally are back to from outlet 115, while stir using heating
It mixes mechanism 14 to heat liquid in stoste area 111, extraction section 112 and back extraction area 113, temperature is 40 DEG C, and total duration is
45min, wherein, stoste, extract liquor, anti-stripping agent flow velocity be followed successively by 2.5m/min, 4.5m/min, 6.5m/min；
Second step:Classification quintessence takes
S1:By stoste area 111 in top membrane contactor 1a in the first step, middle part membrane contactor 1b, bottom membrane contactor 1c,
The liquid in extraction section 112 and back extraction area 113 is back to stoste case 2, extraction liquid case 3, back extraction liquid case 4 respectively, and emptying is all
Membrane contactor 1, and close whole sealing valves 116；
S2:It is 3 to extract volume ratio from stoste case 2, extraction liquid case 3, back extraction liquid case 4:2:1 stoste, extract liquor, back extraction
It takes in liquid to top membrane contactor 1a, by the addition box 1121 above the membrane contactor 1a of top to its corresponding extraction section 112
The volume ratio of addition mixing liquid one, mixing liquid one and extract liquor is 1:9, wherein, mixing liquid one is that volume ratio is 1:1:2
Extractant (butyl phosphoric acid dibutyl ester), synergic reagent (cyclohexanone), sustained release agent (isobutyrone), while pass through top-film
Supply container 1131 above contactor 1a supplements pure anti-stripping agent (1mol/LHCl solution) to its corresponding back extraction area 113, pure
The volume ratio of anti-stripping agent (1mol/LHCl solution) and anti-stripping agent (hydrochloric acid solution containing lithium ion) is 1:5, it is stirred by heating
It is 45 degree to mix mechanism 14 and be heated to temperature, stirs 2min, rotating speed 250r/min；
S3：All sealing valves 116 below the membrane contactor 1a of top are opened, by liquid drain to middle part membrane contactor 1b
It is interior, and pass through the addition box 1121 above the membrane contactor 1b of middle part and add mixing liquid two, mixing to its corresponding extraction section 112
The volume ratio of liquid two and extract liquor is 1:14, wherein, mixing liquid two is that volume ratio is 3:2:5 extractant (butyl phosphoric acid
Dibutyl ester), synergic reagent (cyclohexanone), sustained release agent (isobutyrone), while pass through the benefit above the membrane contactor 1b of middle part
It fills box 1131 and supplements pure anti-stripping agent (1mol/LHCl solution), pure anti-stripping agent (1mol/ to its corresponding back extraction area 113
LHCl solution) with the volume ratio of anti-stripping agent (hydrochloric acid solution containing lithium ion) it is 1:7.5, it is heated by heating stirring mechanism 14
It is 45 degree to temperature, stirs 4min, rotating speed 350r/min；
S4：All sealing valves 116 below the membrane contactor 1b of middle part are opened, by liquid drain to bottom membrane contactor 1c
It is interior, and pass through the addition box 1121 above the membrane contactor 1c of bottom and add mixing liquid three, mixing to its corresponding extraction section 112
The volume ratio of liquid three and extract liquor is 1:19, wherein, mixing liquid three is that volume ratio is 4:1:5 extractant (butyl phosphoric acid
Dibutyl ester), synergic reagent (cyclohexanone), sustained release agent (isobutyrone), while pass through the benefit above the membrane contactor 1c of bottom
It fills box 1131 and supplements pure anti-stripping agent (1mol/LHCl solution), pure anti-stripping agent (1mol/ to its corresponding back extraction area 113
LHCl solution) with the volume ratio of anti-stripping agent (hydrochloric acid solution containing lithium ion) it is 1:9.5, it is heated by heating stirring mechanism 14
It is 50 degree to temperature, stirs 5min, rotating speed 450r/min；
S5：Triple valve 9 is connected into the back extraction liquid zone 113 of bottom membrane contactor 1c and condensing crystallizing device 5, then opens bottom
All sealing valves 116 below portion membrane contactor 1c, by liquid in the stoste area 111 of bottom membrane contactor 1c, extraction section 112 point
It is not pumped to stoste case 2, extraction liquid case 3, and lithium-containing solution in the back extraction area 113 of bottom membrane contactor 1c is drained to concentration
In crystallizer 5；
S6：Above-mentioned S2-S5 steps are repeated, finally using condensing crystallizing device 5 by lithium-containing solution evaporative crystallization, obtained gas warp
Condensate recycling device 6 is back to back extraction liquid case 4 after condensing, obtained crystal is sent into lithium salts case 7.
Test result：Lithium extraction yield is up to 99.7%, and lithium chloride purity (mass fraction) is 99.5%, total recovery 96%.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, the difference lies in：
Technique using the extraction equipment extraction lithium ion of embodiment 1 includes the following steps：
Mono- Walk：Fluid pre-extracted
S1：Whole sealing valves 116 is opened, and the back extraction liquid zone 113 of the connection of triple valve 9 bottom membrane contactor 1c is set
With being stripped liquid case 4；
S2：Stoste, extract liquor, anti-stripping agent are extracted from stoste case 2, extraction liquid case 3, back extraction liquid case 4, from import 114
It is flowed into top membrane contactor 1a, middle part membrane contactor 1b, the stoste area 111 in the membrane contactor 1c of bottom, extraction section 112 successively
With back extraction area 113, stoste case 2, extraction liquid case 3, back extraction liquid case 4 finally are back to from outlet 115, while stir using heating
It mixes mechanism 14 to heat liquid in stoste area 111, extraction section 112 and back extraction area 113, temperature is 50 DEG C, and total duration is
60min, wherein, stoste, extract liquor, anti-stripping agent flow velocity be followed successively by 3m/min, 5m/min, 7m/min；
Second step:Classification quintessence takes
S1:By stoste area 111 in top membrane contactor 1a in the first step, middle part membrane contactor 1b, bottom membrane contactor 1c,
The liquid in extraction section 112 and back extraction area 113 is back to stoste case 2, extraction liquid case 3, back extraction liquid case 4 respectively, and emptying is all
Membrane contactor 1, and close whole sealing valves 116；
S2:It is 3 to extract volume ratio from stoste case 2, extraction liquid case 3, back extraction liquid case 4:2:1 stoste, extract liquor, back extraction
It takes in liquid to top membrane contactor 1a, by the addition box 1121 above the membrane contactor 1a of top to its corresponding extraction section 112
The volume ratio of addition mixing liquid one, mixing liquid one and extract liquor is 1:10, wherein, mixing liquid one is that volume ratio is 1:1:
2 extractant (TBP), synergic reagent (N- methyl), sustained release agent (D70 special solvent oils), while by the membrane contactor 1a of top
The supply container 1131 of side supplements pure anti-stripping agent (1mol/LHCl solution), pure anti-stripping agent to its corresponding back extraction area 113
The volume ratio of (1mol/LHCl solution) and anti-stripping agent (hydrochloric acid solution containing lithium ion) is 1:6, pass through heating stirring mechanism 14
It is 40 degree to be heated to temperature, stirs 3min, rotating speed 300r/min；
S3：All sealing valves 116 below the membrane contactor 1a of top are opened, by liquid drain to middle part membrane contactor 1b
It is interior, and pass through the addition box 1121 above the membrane contactor 1b of middle part and add mixing liquid two, mixing to its corresponding extraction section 112
The volume ratio of liquid two and extract liquor is 1:15, wherein, mixing liquid two is that volume ratio is 3:2:5 extractant (TBP) assists extraction
Agent (N- methyl), sustained release agent (D70 special solvent oils), at the same it is right to its by the supply container 1131 above the membrane contactor 1b of middle part
The back extraction area 113 answered supplements pure anti-stripping agent (1mol/LHCl solution), pure anti-stripping agent (1mol/LHCl solution) and back extraction
The volume ratio for taking liquid (hydrochloric acid solution containing lithium ion) is 1:8, it is 45 degree to be heated to temperature by heating stirring mechanism 14, stirring
5min, rotating speed 400r/min；
S4：All sealing valves 116 below the membrane contactor 1b of middle part are opened, by liquid drain to bottom membrane contactor 1c
It is interior, and pass through the addition box 1121 above the membrane contactor 1c of bottom and add mixing liquid three, mixing to its corresponding extraction section 112
The volume ratio of liquid three and extract liquor is 1:20, wherein, mixing liquid three is that volume ratio is 4:1:5 extractant (TBP) assists extraction
Agent (N- methyl), sustained release agent (D70 special solvent oils), at the same it is right to its by the supply container 1131 above the membrane contactor 1c of bottom
The back extraction area 113 answered supplements pure anti-stripping agent (1mol/LHCl solution), pure anti-stripping agent (1mol/LHCl solution) and back extraction
The volume ratio for taking liquid (hydrochloric acid solution containing lithium ion) is 1:10, it is 50 degree to be heated to temperature by heating stirring mechanism 14, is stirred
Mix 6min, rotating speed 500r/min；
S5：Triple valve 9 is connected into the back extraction liquid zone 113 of bottom membrane contactor 1c and condensing crystallizing device 5, then opens bottom
All sealing valves 116 below portion membrane contactor 1c, by liquid in the stoste area 111 of bottom membrane contactor 1c, extraction section 112 point
It is not pumped to stoste case 2, extraction liquid case 3, and lithium-containing solution in the back extraction area 113 of bottom membrane contactor 1c is drained to concentration
In crystallizer 5；
S6：Above-mentioned S2-S5 steps are repeated, finally using condensing crystallizing device 5 by lithium-containing solution evaporative crystallization, obtained gas warp
Condensate recycling device 6 is back to back extraction liquid case 4 after condensing, obtained crystal is sent into lithium salts case 7.
Test result：Lithium extraction yield is up to 99.4%, and lithium chloride purity (mass fraction) is 99.3%, total recovery 93%.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
To modify to the technical solution recorded in previous embodiment or carry out equivalent replacement to which part technical characteristic；And
These modifications are replaced, the spirit and model of technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (9)
1. a kind of extraction equipment of highly effective integration lithium ion, which is characterized in that mainly including membrane contactor (1), stoste case
(2), extraction liquid case (3), back extraction liquid case (4), condensing crystallizing device (5), condensate recycling device (6) and lithium salts case (7), the film
Contactor (1) is divided into the identical top membrane contactor (1a) of specification, middle part membrane contactor (1b), bottom membrane contactor (1c), film
Contactor (1) includes reactor shell (11), scrolling mechanism (12), amberplex (13) and heating stirring mechanism (14), institute
Totally two, scrolling mechanism (12) is stated, longitudinal direction is equidistant respectively and is removably mounted at reactor shell (11) inside, and will reaction
Stoste area (111), extraction section (112) and back extraction area (113), the original are in turn divided into inside device housing (11) from left to right
Import (114) is respectively equipped with above liquid zone (111), extraction section (112) and back extraction area (113), is respectively arranged below with outlet
(115), sealing valve (116) is equipped on the outlet (115), the import (114) of middle part membrane contactor (1b) connects with top-film
The outlet (115) of tentaculum (1a) is connected, the import (114) of bottom membrane contactor (1c) and the outlet of middle part membrane contactor (1b)
(115) it is connected, the amberplex (13), and can be by the mechanism that scrolls (12) up and down between scrolling mechanism (12)
Scrolling, the heating stirring mechanism (14) are respectively fixedly connected in the stoste area (111), extraction section (112) and back extraction area
(113) bottom centre position, the stoste case (2) is respectively by pumping (8) and the stoste area of the top membrane contactor (1a)
(111), the stoste area (111) of the bottom membrane contactor (1c) is connected, and the extraction liquid case (3) is respectively by pumping (8) and top
The extraction section (112) of portion's membrane contactor (1a), the extraction section (112) of bottom membrane contactor (1c) are connected, the back extraction liquid case
(4) respectively by pumping the back extraction area (113) of (8) and top membrane contactor (1a), the back extraction area of bottom membrane contactor (1c)
(113) it is connected, the condensing crystallizing device (5) is connected to the back extraction area (113) of bottom membrane contactor (1c) by triple valve (9)
Between back extraction liquid case (4), it is connected above the condensate recycling device (6) and condensing crystallizing device (5), is returned after gas is condensed
It send to back extraction liquid case (4), the lithium salts case (7) is connected to the lower section of condensing crystallizing device (5).
A kind of 2. extraction equipment of highly effective integration lithium ion as described in claim 1, which is characterized in that the scrolling mechanism
(12) including upper shell (121), lower shell (122), drive roll (123), driven voller (124), connecting tube one (125), connecting tube
Two (126), reeling driver (127) and power pack (128), the drive roll (123) is positioned at the horizontal axis of the lower shell (122)
Center, drive roll (123) and driven voller (124) are hollow shaft and equal length, right end and the volume of drive roll (123)
The output shaft of axis driver (127) is connected, and the power pack (128) and passes through conducting wire and pass through positioned at the left end of drive roll (123)
Electric energy is provided for reeling driver (127) inside drive roll (123), the driven voller (124) is arranged on the upper shell (121)
Horizontal axis center, the top of upper shell (121) is equipped with film import parallel and equal length with drive roll (123)
(1211), the bottom of lower shell (122) is equipped with film parallel and equal length with driven voller (124) and exports (1221), the company
Take over one (125) and connecting tube two (126) are respectively equipped with inner groovy (1251) and external groove (1252), are detachably connected on respectively
Between upper shell (121) and lower shell (122) both ends, the inner groovy (1251) is the moving rail of the amberplex (13)
Road, the outside groove (1252) are connected to by clamping or guide rail on the reactor shell (11) inner wall.
A kind of 3. extraction equipment of highly effective integration lithium ion as claimed in claim 2, which is characterized in that the inner groovy
(1251) it is 1 with the width ratio of external groove (1252):5-10.
A kind of 4. extraction equipment of highly effective integration lithium ion as described in claims 1 or 2 or 3, which is characterized in that the volume
Page mechanism (12) is the disposable apparatus handled through waterproof and anticorrosion.
A kind of 5. extraction equipment of highly effective integration lithium ion as described in claim 1, which is characterized in that the heating stirring
Mechanism (14) includes capsul (141), heater (142), heat resisting motor (143) and T-shaped stirring rod (144), the sealing
The bottom of shell (141) is fixed on the bottom centre position of the stoste area (111), extraction section (112) and back extraction area (113),
The heater (142) and heat resisting motor (143) are located at capsul (141) inside, and pass through capsul (141) and original side by side
The bottom of liquid zone (111), extraction section (112) and back extraction area (113) is connected with external power supply, T-shaped stirring rod (144) position
It is connected in the perpendicular section bottom end on capsul (141) top, and T-shaped stirring rod (144) with the output shaft of heat resisting motor (143), T
Type stirring rod (144) is internally provided with heating seal wire (145), and the heating seal wire (145) is connected with heater (142).
A kind of 6. extraction equipment of highly effective integration lithium ion as described in claim 1, which is characterized in that the same film
The import (114) of contactor (1) is dislocated with outlet (115).
7. a kind of extraction equipment of highly effective integration lithium ion as described in claim 1, which is characterized in that the top-film connects
Divide above tentaculum (1a), middle part membrane contactor (1b), the extraction section (112) of bottom membrane contactor (1c) and back extraction area (113)
Addition box (1121) and supply container (1131) are not connected with by proportioning valve.
8. a kind of extraction process using extraction equipment extraction lithium ion includes the following steps：
Mono- Walk：Fluid pre-extracted
S1：Whole sealing valves (116) is opened, and the back extraction of the triple valve (9) connection bottom membrane contactor (1c) is set
Liquid zone (113) and back extraction liquid case (4)；
S2：Stoste, extract liquor, anti-stripping agent are extracted from the stoste case (2), extraction liquid case (3), back extraction liquid case (4), from institute
It states import (114) and is flowed into top membrane contactor (1a), middle part membrane contactor (1b), the original in bottom membrane contactor (1c) successively
Liquid zone (111), extraction section (112) and back extraction area (113) are finally back to stoste case (2), extraction from the outlet (115)
Liquid case (3), back extraction liquid case (4), while using the heating stirring mechanism (14) to stoste area (111), extraction section (112) and
Back extraction area (113) interior liquid heated, temperature be 30-50 DEG C, total duration 30-60min, wherein, stoste, extract liquor,
The flow velocity of anti-stripping agent is followed successively by 2-3m/min, 4-5m/min, 6-7m/min；
Second step:Classification quintessence takes
S1:By top membrane contactor (1a), middle part membrane contactor (1b), the interior stoste area of bottom membrane contactor (1c) in the first step
(111), the liquid of extraction section (112) and back extraction area (113) is back to stoste case (2), extraction liquid case (3), back extraction respectively
Liquid case (4) empties all membrane contactors (1), and closes whole sealing valve (116)；
S2:It is 3 to extract volume ratio from stoste case (2), extraction liquid case (3), back extraction liquid case (4):2:It is 1 stoste, extract liquor, anti-
In extract liquor to top membrane contactor (1a), corresponded to by the addition box (1121) above top membrane contactor (1a) to it
Extraction section (112) addition mixing liquid one, the volume ratio of the mixing liquid one and the extract liquor is 1:8-10 leads to simultaneously
The supply container (1131) crossed above top membrane contactor (1a) supplements pure back extraction to its corresponding back extraction area (113)
The volume ratio of liquid, the pure anti-stripping agent and the anti-stripping agent is 1:5-6 is heated to temperature by heating stirring mechanism (14)
For 30-50 degree, 2-3min, rotating speed 200-300r/min are stirred；
S3：All sealing valves (116) below top membrane contactor (1a) are opened, by liquid drain to middle part membrane contactor (1b)
It is interior, and pass through the addition box (1121) above middle part membrane contactor (1b) and add mixing liquid to its corresponding extraction section (112)
Two, the volume ratio of the mixing liquid two and the extract liquor is 1:12-15, at the same by middle part membrane contactor (1b) above
Supply container (1131) supplements pure anti-stripping agent, the pure anti-stripping agent and the back extraction to its corresponding back extraction area (113)
The volume ratio of liquid is 1:7-8 is heated to temperature as 30-50 degree by heating stirring mechanism (14), stirs 4-5min, rotating speed is
300-400r/min；
S4：All sealing valves (116) below middle part membrane contactor (1b) are opened, by liquid drain to bottom membrane contactor (1c)
It is interior, and pass through the addition box (1121) above bottom membrane contactor (1c) and add mixing liquid to its corresponding extraction section (112)
Three, the volume ratio of the mixing liquid three and the extract liquor is 1:18-20, at the same by bottom membrane contactor (1c) above
Supply container (1131) supplements pure anti-stripping agent, the pure anti-stripping agent and the back extraction to its corresponding back extraction area (113)
The volume ratio of liquid is 1:9-10 is heated to temperature as 30-50 degree by heating stirring mechanism (14), stirs 5-6min, rotating speed is
400-500r/min；
S5：Triple valve (9) is connected into the back extraction liquid zone (113) of bottom membrane contactor (1c) and the condensing crystallizing device (5), so
Open all sealing valves (116) below bottom membrane contactor (1c) afterwards, by the stoste area (111) of bottom membrane contactor (1c),
Extraction section (112) interior liquid is pumped to stoste case (2), extraction liquid case (3) respectively, and by the back extraction of bottom membrane contactor (1c)
Area (113) interior lithium-containing solution is drained in condensing crystallizing device (5)；
S6：Repeat above-mentioned S2-S5 step, last condensing crystallizing device (5) is by lithium-containing solution evaporative crystallization, and obtained gas is through described cold
The back extraction liquid case (4) is back to after solidifying retracting device (6) condensation, obtained crystal is sent into the lithium salts case (7).
A kind of 9. extraction equipment of highly effective integration lithium ion as claimed in claim 8, which is characterized in that the mixing liquid
One be volume ratio is 1:1:2 extractant, synergic reagent, sustained release agent；It is 3 that the mixing liquid two, which is volume ratio,:2:5 extraction
Agent, synergic reagent, sustained release agent；It is 4 that the mixing liquid three, which is volume ratio,:1:5 extractant, synergic reagent, sustained release agent.
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