CN106219579B - A kind of extraction element of industrial grade methanol - Google Patents
A kind of extraction element of industrial grade methanol Download PDFInfo
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- CN106219579B CN106219579B CN201610550355.7A CN201610550355A CN106219579B CN 106219579 B CN106219579 B CN 106219579B CN 201610550355 A CN201610550355 A CN 201610550355A CN 106219579 B CN106219579 B CN 106219579B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/04—Halides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention discloses a kind of extraction element of industrial grade methanol, the device includes by pipeline successively along filter press even, the blend tank for adjust acid to handle, extracting system, washing system and the back extraction system being connected in series respectively by multistage centrifugal extracter and iron removal system and oil removing system；Wherein, the stripping workshop output end for being stripped system is also connected with washing system, and the organic phase output terminal for being stripped system is connected with saponification system, and saponification system is connected with extracting system；The extracting system, washing system, back extraction system, saponification system constitute circulation loop.The device is additionally provided with data analysis system, which can be automatically by abnormal centrifugal extractor Switch of working position to standby platform centrifugal extractor.The material input of each system is additionally provided with frequency-variable closed flow control system in the circulation loop, to obtain accurate flow and the input phase ratio by timely adjustment.Extraction efficiency of the present invention is high, balances each other that settling time is fast, solvent acquisition amount is small, solvent consumption is few, process is continuously reliable.
Description
Technical field
The invention belongs to chemical industry of inorganic salt fields, and in particular to a kind of extraction element of industrial grade methanol.
Background technology
Lithium chloride is mainly used for air conditioner dehumidification agent, bleaching powder, insecticide, synthetic fibers, pharmaceuticals industry, lithium battery electrolysis
Secondly matter, metal alloy solder agent or fluxing agent are for producing lithium metal there are one critically important purposes, lithium is national warp
The strategic materials that Ji development and national defense construction are badly in need of, the current unique commercial run for producing lithium metal is to be proposed by rigid thatch for 1893
, i.e. lithium chloride molten salt electrolysis.
Currently, the domestic lithium chloride for being only capable of 99.5% purity of production, the lithium chloride of high-purity, such as 99.995% purity are only capable of
By from external import, seriously constraining the progress of the industries such as China's economic development and aerospace, national defense construction.In the prior art
The method of extraction lithium chloride is mainly the following form both at home and abroad：Calcination method, the precipitation method, ion-exchange, solvent extraction,
Floatation etc..Wherein, solvent extraction obtains industrial grade methanol and can realize that large-scale industrial production has become domestic and international technology
The common recognition of development.Conventional solvent extraction generally uses static extracting slot, extraction compartment as main extractor tool, with following
Disadvantage：1. solvent acquisition amount is big, consumption is more, of high cost；2. extraction efficiency is low, required series is more, it is difficult to obtain the high production of purity
Product；3. settling time of balancing each other is long, extraction process is unstable；4. operation is safeguarded cumbersome, corollary equipment is more, and labor intensity is high, accounts for
Ground area is excessive etc..The above reason hinders popularization and application of the solvent extraction in putting forward lithium technique, also counteracts high-purity chloro
Change the industrialized production of lithium.With the continuous improvement of extractant technology, high distribution coefficient extractant emerges in multitude, because of static extracting
The popularization problem urgent need to resolve of solvent extraction caused by equipment.
Therefore, that it is urgent to provide a kind of extraction efficiencies is high, settling time of balancing each other is fast, solvent acquisition amount by those skilled in the art
It is small, solvent consumption is few, the continuous reliable industrial grade methanol extraction element of process.
Invention content
Against the above deficiency, that the present invention provides a kind of extraction efficiencies is high, settling time of balancing each other is fast, solvent acquisition amount
It is small, solvent consumption is few, the continuous reliable industrial grade methanol extraction element of process.
To achieve the above object, present invention employs following technical schemes：
A kind of extraction element of industrial grade methanol, the device include by pipeline successively along even pre- to the progress of brine material
The filter press of processing is connected in series respectively to the blend tank that material after pretreatment carries out that acid is adjusted to handle by multistage centrifugal extracter
Extracting system, washing system and back extraction system, subsequent iron removal system and oil removing system；Wherein, it is stripped the back extraction of system
Solution output end is also connected with washing system, and the organic phase output terminal for being stripped system is connected with saponification system, the saponification system
It is connected with extracting system；The extracting system, washing system, back extraction system, saponification system constitute circulation loop.
Preferably, which is additionally provided with data analysis system, and monitoring itself operating is both provided on the centrifugal extractor
The sensor of situation, sensor are connect with data analysis system real-time communication, and extracting system, washing system, back extraction system are equal
Equipped with standby platform centrifugal extractor；When data analysis system recognizes centrifugal extractor exception by sensor, which can be certainly
It moves its Switch of working position to standby platform centrifugal extractor.
Further, the material input of each system is equipped with frequency-variable closed flow control system in the circulation loop,
The system includes by pipeline successively along variable-frequency control pump even, the flowmeter with flow feedback, with the regulating valve of position feedback
And automatic valve.Variable-frequency control pump is tentatively controlled by frequency control, by flow in required range, is carried out in conjunction with flowmeter
It measures in due course, measured value is fed into data analysis system and required current capacity contrast by signal, controls to adjust valve opening, convection current
Amount carries out trace regulation, can get required accurate flow.
Preferably, the input terminal of the back extraction system is connected with hydrochloric acid refining plant, and the device is by evaporating the essence generated
Salt manufacturing acid inputs back extraction system, as back washing agent.
Preferably, the extracting system be set as 3 grades, washing system be set as 5 grades, back extraction system be set as 4 grades, successively along even structure
At plural serial stage counter-current extraction system；The centrifugal extractor uses centrifugal extractor.
Preferably, the saponification system is set as 3 grades of saponification, and alkali liquor preparing feedway and waste liquid are connected in saponification system
Collect tapping equipment.
Preferably, it is equipped in the iron removal system and removes iron extraction section and 3 grades of stripping sections along 3 grades even, 3 grades extract except iron
Section is added except iron extractant is to remove the ferro element in solution, and pure water is added as back washing agent in 3 grades of stripping sections, so that except iron extracts
Agent is regenerated, and achievees the purpose that recycling.
Preferably, the oil removing system is set as gravity and ultrasonic air-float oil removing system, including gravity in sequential series removes
Oily device and ultrasonic air-float degreasing unit；The gravity oil-removing device includes 3 concatenated gravity settlers, by inverted
" u "-shaped pipe is connected to, and the maximum height of inverted " u "-shaped pipe is less than the height of upper level oil phase crest of weir.
Further, the stripping workshop that the outflow of back extraction system is controlled by frequency-variable closed flow control system enters washing system
The flow of system is the 20% of its total flow, and remaining 80% flow enters iron removal system, and the ratio between flow of the two is 1:4.
Further, when the input phase of centrifugal extractor ratio meets or exceeds 40:When 1, it is equipped with outside the centrifugal extractor
This grade of reflux or the centrifugal extractor are set as carrying the centrifugal extractor of this grade of reflux.By extracting in centrifugation
It takes and carries out this grade of reflux in machine, by the reality of two-phase compared to control 4:1~5:1, increase the area that is in contact in extracter, obtains
Higher extraction efficiency.
The beneficial effects of the present invention are：
1), present invention introduces Hefei General Environment Control Technology Co., Ltd., (former Hefei work of nature scientific and technological development is limited
Company) production the efficient centrifugal extractor of big flow, according to specific process section, by the Centrifugical extraction unit of different number of units
At the extracting system of different series, washing system, back extraction system, counter flow in series extracting system is formed.Wherein extracting system is general
It is formed by 3 grades, 5 grades of washing system, 4 grades of back extraction system.The required efficient centrifugal extractor of big flow according to specific flow,
It can be in 1m3/ h~70m3Concrete model is chosen within the scope of/h to match；It can also be according to the temperature, acidity, organic solvent etc. of material
Feature selects the unlike materials such as stainless steel, dual phase steel, titanium, Hastelloy or steel lining plastic, to meet production needs.Big flow is high
The counter flow in series extracting system of centrifugal extractor composition is imitated, has that extraction efficiency is high, settling time of balancing each other is fast, solvent
The advantages that demand is small, solvent consumption is few, process is continuously reliable solves traditional static extraction tank, the series that extraction compartment is brought
Problem has tamped technical foundation for extensive, industrialized production high-purity lithium chloride products.
2), extracting system is extracted using 3 grades of counter flow in series in the present invention, required compared with traditional static solvent extraction
Extraction series is less, and the dosage of extractant is also few；The solution output end that the present invention is stripped system is connected to washing system, is stripped
The lithium chloride solution obtained afterwards provides its 20% flow, back to washing system as detergent.By washing, lithium has with load
The impurity such as calcium, magnesium, sodium in machine phase are replaced, and the impurity in load organic phases is made to be washed, be removed, anti-to make to enter
The Chlorine in Solution lithium purity for extracting section is higher；The present invention, which is stripped system, makes load organic phases release the lithium of load, iron ion, shape
At lithium chloride and liquor ferri trichloridi, which enters iron removal system, and using oil removing system, the lithium chloride after iron and oil removing is molten
Liquid by processes such as evaporation and concentration, crystallization, separation, drying, packagings, obtains 99.995% high-purity lithium chloride products again.And it is anti-
The organic phase for extracting system output then enters the progress saponification of saponification system except acid regeneration；
Device solvent acquisition amount that the present invention purifies lithium chloride is small, solvent consumption is few；Pass through plural serial stage adverse current
Extraction can get the higher lithium chloride solution of purity, and so that extractant organic phase is regenerated by back extraction, reduce extraction
The dosage of agent；Saponification is generated by adding lye in saponification system, the acid in extractant organic phase is removed so that extraction
It takes agent organic phase distribution coefficient to be restored, can recirculate and be extracted in addition extracting system, ensure that extraction efficiency simultaneously
Reduce production cost；It is stripped by the way that pure water is added in iron removal system, can also make to be regenerated except iron extractant.
3), for the present invention through entering oil removing system except the industrial grade methanol solution after iron, lithium chloride solution enters the 1st grade of sedimentation
After tank because flow is smaller, solution slowly in settling tank assemble, increase, in the process, entrained oil phase factor density compared with
Small gradual floating, water phase generate water-oil separating because of the larger gradual sinking of density.The oil phase of rising enters eventually by oil phase crest of weir
Oil phase collecting chamber is drained, and water phase enters next stage gravitational settling by the discharge pipe of lowest part by the inverse u shape pipe of certain altitude
Tank, the height of inverse u shape pipe are generally below the height of upper level oil phase crest of weir so that water phase can reach in settling tank it is certain
Liquid level；Into after next stage gravity settler, still continue the above oil water separation process, repeatedly, passes through 3 grades of gravitational settlings
Afterwards, removing entrained oil in the lithium chloride solution after iron, mutually major part can remove, and the miscellaneous oil of micro, 100ppm units or so enters
Ultrasonic air-float oil removing system generates the air supporting that aeration is brought by the cavitation of ultrasonic wave and the compressed air of introducing and makees
With, the micro oil of emulsification is broken up, is precipitated, is further removed eventually by modes such as gravity oil skimming, active carbon filter absorption,
Entrained oil in lithium chloride solution is set mutually to be reduced to 10ppm hereinafter, obtaining the lithium chloride solution of high-purity, to obtain 99.995%
High-purity lithium chloride products are laid a good foundation.
4), the input phase ratio in the present invention in centrifugal extractor meets or exceeds 40:When 1, by increasing to centrifugal extractor
If external grade reflux or being directly set to the centrifugal extractor with this grade of reflux；So that material exists
The reflux of this grade is carried out in centrifugal extractor, by the reality of two-phase compared to control 4:1~5:1, it increases in extracter and is in contact
Area improves extraction efficiency.
5) it, is equipped with series sensor, including temperature, rotating speed, vibration etc. on all centrifugal extractors of the present invention, these biographies
Sensor is by the in due course parameter incoming data analysis system of centrifugal extractor；When some of which parameter occurs abnormal, data analysis
System can judge or send out accordingly early warning.If being finally judged as centrifugal extractor exception, system if, can be automatically closed
The exception centrifugal extractor simultaneously automatically turns on standby platform centrifugal extractor, while automatically switching related valve, cuts off abnormal centrifugation extraction
The disengaging material of machine is taken, the inlet and outlet piping of standby platform centrifugal extractor is opened, so that centrifugal extractor series line is steadily switched, do not influence
The output of product is stablized.The steady of the processes such as extraction, washing, back extraction is further ensured, avoids machine occur because of certain extracter
Tool failure and cause whole production line occur fluctuation even stop, improve its application value.
6), the present invention introduces frequency-variable closed flow control system in circulation loop.The system by variable-frequency control pump,
Flow is tentatively controlled in required range；Actual flow is measured by flowmeter in due course again, measured value is anti-by signal
Feed enters data analysis system and is analyzed and determined, the actual flow of acquisition is compared with required flow, according to than
Signal is sent out to value, micro control and regulation valve opening carries out trace regulation to flow.By the closed loop feedback and timely adjustment,
Accurately required flow is can get, makes flow error control ± 0.1, and flow can be as small as 0.2m3/h.It ensure that each system phase
The accurate and stabilization of ratio, technological process is steady, and output of products keeps reliable and stable.
Description of the drawings
Fig. 1 is the device of the invention schematic diagram (Fig. 1 a, 1b are respectively the enlarged drawing of dotted line left and right side part in Fig. 1).
Fig. 2 is the process flow chart of the present invention.
The meaning of label symbol is as follows in figure：
1- hydrochloric acid refining plant 2- filter press 3- blend tank 4- centrifugal extractors
40- is for this grade of reflux 401- sensor of platform centrifugal extractor 400-
4A- extracting system 4B- washing systems 4C- is stripped system 4D- saponification systems
5- frequency-variable closed flow control system 51- variable-frequency control pump 52- flowmeters
53- regulating valve 54- automatic valve 6- iron removal system 7- oil removing systems
70- gravity settler 71- inverse u shape pipe 8- data analysis systems
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, is clearly and completely retouched to the technical solution in the present invention
It states.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
As shown in Figure 1, being a kind of extraction element of industrial grade methanol, which includes by pipeline successively along even to halogen
Water material carries out pretreated filter press 2, to the blend tank 3 that material after pretreatment carries out that acid is adjusted to handle, respectively by multistage centrifugal
Extracting system 4A, the washing system 4B and back extraction system 4C, subsequent iron removal system 6 and oil removing system that extracter 4 is connected in series
System 7；Wherein, the stripping workshop output end of back extraction system 4C is also connected with washing system 4B, the organic phase output of back extraction system 4C
End is connected with saponification system 4D, and the saponification system 4D is connected with extracting system 4A；The extracting system 4A, washing system 4B,
Back extraction system 4C, saponification system 4D constitute circulation loop.
The frequency-variable closed flow control system 5 for adjusting each system material input is additionally provided in the circulation loop, with control
Input flow rate it is accurate with compare it is accurate.The system includes anti-along variable-frequency control pump 51 even, band flow successively by pipeline
The flowmeter 52 of feedback, the regulating valve 53 with position feedback and automatic valve 54；Variable-frequency control pump 51, will be at the beginning of flow by frequency control
Step control is measured in required range in conjunction with flowmeter 52 in due course, and measured value is fed into data point by signal
Analysis system 8 and required current capacity contrast, control to adjust 53 aperture of valve, and trace regulation is carried out to flow, can get accurately required stream
Amount.
The device is additionally provided with data analysis system 8, is both provided on the centrifugal extractor 4 and monitors itself operational situation
Sensor 401, sensor 401 are connect with 8 real-time communication of data analysis system, and extracting system 4A, washing system 4B, back extraction system
System 4C is equipped with standby platform centrifugal extractor 40；When data analysis system 8 recognizes 4 exception of centrifugal extractor by sensor 401
When, which can be automatically by its Switch of working position to standby platform centrifugal extractor 40.
Specifically, the input terminal of the back extraction system 4C is connected with hydrochloric acid refining plant 1, the device is by evaporating generation
Refined hydrochloric acid inputs back extraction system 4C, as back washing agent；
The extracting system 4A be set as 3 grades, washing system 4B be set as 5 grades, back extraction system 4C be set as 4 grades, successively along even structure
At plural serial stage counter-current extraction system；The centrifugal extractor 4 is (former using Hefei General Environment Control Technology Co., Ltd.
Hefei Talentgroup Science ＆ Technology Development Co., Ltd.) production the efficient centrifugal extractor of big flow；
The saponification system 4D is set as 3 grades of saponification, and alkali liquor preparing feedway is connected on saponification system 4D and waste liquid is received
Collect tapping equipment；
It is equipped in the iron removal system 6 along 3 grades even except iron extracts and 3 grades of back extraction, 3 grades are removed iron except iron extraction section is added
For extractant to remove the ferro element in solution, pure water is added as back washing agent in 3 grades of back extraction, so that except iron extractant is regenerated,
Achieve the purpose that recycling.
The oil removing system 7 was set as gravity and ultrasonic air-float oil removing system, including gravity oil-removing in sequential series dress
It sets and ultrasonic air-float degreasing unit；The gravity oil-removing device 70 includes 3 concatenated gravity settlers 70, passes through inverted " u "
Shape pipe 71 is connected to, and the maximum height of inverted " u "-shaped pipe 71 is less than the height of upper level oil phase crest of weir.
The stripping workshop that the 4C outflows of back extraction system are controlled by frequency-variable closed flow control system 5 enters washing system 4B's
Flow is 1 with the ratio between the flow for entering iron removal system 6:4.That is the stripping workshop of back extraction system 4C outflows, the 20% of flow returns
Washing system 4B is moved back into as detergent, remaining 80% flow, which enters iron removal system 6, handled except iron.
When the input phase ratio of centrifugal extractor 4 meets or exceeds 40:When 1, this grade of reflux is equipped with outside the centrifugal extractor 4
Device 400 (referring to Chinese patent literature CN 104771932A) or the centrifugal extractor 4 are set as carrying this grade of reflux dress
The centrifugal extractor set (referring to Chinese patent literature CN104784967A).
Apparatus of the present invention make the course of work of industrial grade methanol with reference to concrete technology (as shown in Figure 2) as follows
Detailed description.
S1, pretreatment：Brine material is pre-processed by filter press 2, remove material in boric acid, solid impurity and
Suspended matter；
S2, acid is adjusted：Pretreated material is added to a concentration of 31% technical hydrochloric acid, is stirred by blend tank 3
It carries out adjusting sour processing, makes material PH=2；
S3, multi-stage counter current extraction：The material (water phase) after acid is adjusted to enter extraction system by frequency-variable closed flow control system 5
The heavy liquid inlet of 4 first order of plural serial stage centrifugal extractor in system 4A, meanwhile, extractant (oil phase) is closed also by frequency conversion
Circulation amount control system 5 enters the light phase inlet of 4 afterbody of plural serial stage centrifugal extractor, forms counter-current extraction；
The two compares control in oil phase:Water phase=2:1, wherein using complex compound N523 ((the 2- ethyls of N, N- bis- of high distribution coefficient
Hexyl) acetamide) sulfonated kerosene is added as diluent and trichlorine as extractant in+TBP (tributyl phosphate) organic solvent
Change iron as synergic reagent；After extraction, load organic phases and raffinate phase are obtained；
S4, multi-stage countercurrent washing：Load organic phases (oil phase) pass through frequency-variable closed flow control after extracting system 4A comes out
System 5 processed enters the light phase inlet of 4 afterbody of plural serial stage centrifugal extractor in washing system 4B；Meanwhile detergent (water
Phase is stripped 20% flow distributed in the lithium chloride solution of system output) enter also by frequency-variable closed flow control system 5
The heavy liquid inlet of 4 first order of plural serial stage centrifugal extractor forms countercurrent washing；Washing system 4B is oil compared to control
Phase:Water phase=200:1；After washing of the load organic phases by washing system 4B centrifugal extractors, eliminate calcium with which,
The impurity such as magnesium, sodium make load organic phases contain only lithium, iron ion；
S5, multi-stage countercurrent back extraction：Load organic phases (oil phase) after washing are closed after washing system 4B comes out by frequency conversion
Circulation amount control system 5 enters the light phase inlet of 4 afterbody of plural serial stage centrifugal extractor in back extraction system 4C；Back washing agent
(water phase) uses the refined hydrochloric acid of 6mol/L, back washing agent to enter in back extraction system 4C also by frequency-variable closed flow control system 5
The heavy liquid inlet of 4 first order of plural serial stage centrifugal extractor；Back extraction system 4C is oil phase compared to control:Water phase=40:1.Pass through
After back extraction, load organic phases release the lithium of load, iron ion, form lithium chloride and liquor ferri trichloridi；And it is obtained after being stripped
20% flow backs into washing system 4B as detergent in the lithium chloride solution obtained, and the washed of load organic phases is added
Journey；Remaining 80% solution enters lower step process iron removal system 6, and organic phase then enters saponification system 4D and carries out saponification deacidification
Regeneration；
S6, saponification：Saponification agent (water phase) uses the lye of 4mol/L, the organic phase (oil phase) of back extraction system 4C outputs to enter
Saponification system 4D, by saponification to remove the hydrochloric acid wherein contained, the two compares control in oil phase:Water phase=40:1,
The entrance of two-phase is by frequency-variable closed flow control system 5 to control the flow entered, to which control is compared；Having after saponification
Machine is mutually regenerated, and distribution coefficient is restored, and is returned into extracting system 4A；Water phase after saponification is arranged as waste liquid
Go out；
The raffinate phase that extracting system 4A is obtained also enters saponification system 4D with saponification agent lye together, wherein may with obtaining
The organic phase contained.
S7, iron is removed：The lithium chloride and liquor ferri trichloridi obtained after back extraction, wherein 20% flow is returned as detergent shunting
Washing system 4B is returned, the flow (water phase) of residue 80% enters in iron removal system 6；N523 organic solvents are added as extractant
(oil phase), and sulfonated kerosene is added as diluent, which is oil phase compared to control:Water phase=2:1, to remove the iron in solution
Ionic impurity obtains the lithium chloride solution of high-purity；
Except iron extractant (oil phase) is stripped by the way that pure water (water phase) is added, which is oil phase compared to control:Water phase=
2:1, make to be regenerated except iron extractant, and reuse；
The entrance of above workshop section's water phase and an oil phase by frequency-variable closed flow control system 5 with control enter flow, from
And it controls and compares；
S8, oil removing：Except the lithium chloride solution after iron passes through gravity and ultrasonic air-float oil removing system 7, lithium chloride solution again
After initially entering the 1st grade of gravity settler 70, because flow is smaller, solution slowly aggregation, raising in gravity settler 70,
In the process, the smaller gradual floating of entrained oil phase factor density, water phase generate water-oil separating because of the larger gradual sinking of density.
The oil phase of rising enters oil phase collecting chamber eventually by oil phase crest of weir and drains, and water phase passes through certain altitude by the discharge pipe of lowest part
Inverse u shape pipe 71 enter next stage gravity settler 70, the height of inverse u shape pipe 71 is generally below upper level oil phase crest of weir
Highly, so that water phase reaches certain liquid level in settling tank；Into after next stage gravity settler 70, still continue the above grease
Separation process after 3 grades of gravitational settlings, can be gone repeatedly except entrained oil is mutually most of in the lithium chloride solution after iron
Remove, the miscellaneous oil of micro, 100ppm units or so enters ultrasonic air-float oil removing system, by the cavitation of ultrasonic wave and
The compressed air of introducing generates the air supporting effect that aeration is brought, and the micro oil of emulsification is broken up precipitation, eventually by gravity oil skimming,
The modes such as active carbon filter absorption are further removed, and entrained oil in lithium chloride solution is made mutually to be reduced to 10ppm hereinafter, into one
Step improves the purity of lithium chloride solution；
It is S9, final, by evaporation and concentration, crystallization, separation, drying, packaging process, obtain 99.995% it is high-purity anhydrous
Lithium chloride products.
Claims (7)
1. a kind of extraction element of industrial grade methanol, it is characterised in that：The device includes by pipeline successively along even to material
Brine carries out pretreated filter press (2), to the blend tank (3) that material after pretreatment carries out that acid is adjusted to handle, respectively by more from
Multi-stage counter current extraction system (4A), washing system (4B) and the back extraction system (4C) that heart extracter (4) is connected in series, subsequently remove iron
System (6) and oil removing system (7)；Wherein, the stripping workshop output end of back extraction system (4C) is also connected with washing system (4B),
Organic phase output terminal of back extraction system (4C) is connected with saponification system (4D), the saponification system (4D) and extracting system (4A) phase
Even；The extracting system (4A), washing system (4B), back extraction system (4C), saponification system (4D) constitute circulation loop；
The extracting system (4A) be set as 3 grades, washing system (4B) be set as 5 grades, back extraction system (4C) be set as 4 grades, successively along even
Constitute plural serial stage counter-current extraction system；The centrifugal extractor (4) uses centrifugal extractor；
The stripping workshop that back extraction system (4C) flows out, which is controlled, by frequency-variable closed flow control system (5) enters washing system (4B)
Flow be the 20% of its total flow, remaining 80% flow enters iron removal system (6), and the ratio between flow of the two is 1:4；
The oil removing system (7) is set as gravity and ultrasonic air-float oil removing system, including gravity oil-removing device in sequential series and
Ultrasonic air-float degreasing unit；The gravity oil-removing device includes 3 concatenated gravity settlers (70), passes through inverted " u "-shaped pipe
(71) it is connected to, and the maximum height of inverted " u "-shaped pipe (71) is less than the height of upper level oil phase crest of weir.
2. a kind of extraction element of industrial grade methanol according to claim 1, it is characterised in that：The device is additionally provided with data
Analysis system (8) is both provided with the sensor (401) for monitoring itself operational situation, sensor on the centrifugal extractor (4)
(401) it is connect with data analysis system (8) real-time communication, and extracting system (4A), washing system (4B), back extraction system (4C) are equal
Equipped with standby platform centrifugal extractor (40)；When by sensor (401) to recognize centrifugal extractor (4) different for data analysis system (8)
Chang Shi, the system can be automatically by its Switch of working position to standby platform centrifugal extractor (40).
3. a kind of extraction element of industrial grade methanol according to claim 2, it is characterised in that：It is each in the circulation loop
The material input of system is equipped with frequency-variable closed flow control system (5), which includes by pipeline successively along change even
Frequency governor impeller (51), the flowmeter (52) with flow feedback, the regulating valve (53) with position feedback and automatic valve (54)；Become frequency modulation
Flow is tentatively controlled in required range, is surveyed in due course in conjunction with flowmeter (52) by frequency control by speed pump (51)
Amount, measured value is fed into data analysis system (8) and required current capacity contrast by signal, then is opened by controlling to adjust valve (53)
Degree carries out trace regulation to flow, can get required accurate flow.
4. a kind of extraction element of industrial grade methanol according to claim 1, it is characterised in that：The back extraction system (4C)
Input terminal be connected with hydrochloric acid refining plant (1).
5. a kind of extraction element of industrial grade methanol according to claim 1, it is characterised in that：The saponification system (4D)
3 grades of saponification are set as, alkali liquor preparing feedway and waste collection tapping equipment are connected in saponification system (4D).
6. a kind of extraction element of industrial grade methanol according to claim 1, it is characterised in that：The iron removal system (6)
In be equipped with along even 3 grades remove iron extraction section and 3 grades of stripping sections, 3 grades except iron extraction section be added except iron extractant to remove solution
In ferro element, pure water are added as back washing agent in 3 grades of stripping sections so that except iron extractant is regenerated, realization recycling.
7. according to a kind of extraction element of industrial grade methanol of claim 1~6 any one of them, it is characterised in that：Work as centrifugation
The input phase ratio of extracter (4) meets or exceeds 40:When 1, it is equipped with this grade of reflux (400) outside the centrifugal extractor (4),
Or the centrifugal extractor (4) is set as carrying the centrifugal extractor of this grade of reflux；By being carried out in centrifugal extractor
This grade flows back, by the reality of two-phase compared to control 4:1~5:1, increase the area that is in contact in extracter.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610550355.7A CN106219579B (en) | 2016-07-13 | 2016-07-13 | A kind of extraction element of industrial grade methanol |
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| CN106629788B (en) * | 2017-02-13 | 2019-04-30 | 青海盐湖工业股份有限公司 | A kind of production technology of lithium chloride |
| CN107760885B (en) * | 2017-11-16 | 2019-09-20 | 中国科学院青岛生物能源与过程研究所 | A method of extracting low concentration lithium from the original brine of salt lake |
| CN108217697A (en) * | 2018-01-31 | 2018-06-29 | 上海易信生物科技有限公司 | A kind of method that high-purity lithium salts is extracted from brine containing lithium |
| CN109574047B (en) * | 2018-10-22 | 2021-03-12 | 天齐锂业（江苏）有限公司 | Method for recovering high-purity efavirenz and lithium chloride from medical lithium-containing waste liquid |
| CL2020001650A1 (en) | 2019-06-18 | 2021-01-29 | Schlumberger Technology Bv | Lithium extraction |
| CN111013191A (en) * | 2019-12-25 | 2020-04-17 | 四川星明能源环保科技有限公司 | Stripping agent circulating device for low-cost vanadium electrolyte production line |
| CN113247864B (en) * | 2021-05-24 | 2022-11-15 | 中国成达工程有限公司 | Automatic continuous production system and method for calcium-process bleaching powder fine chlorination unit |
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| CN102001692B (en) * | 2010-12-03 | 2012-11-07 | 中国科学院青海盐湖研究所 | Coordinate extracting system for extracting lithium from salt lake brine by extraction method |
| CN204237845U (en) * | 2013-12-19 | 2015-04-01 | 宜兴新威利成稀土有限公司 | Rare earth chloride extraction plant |
| CN105439176B (en) * | 2014-09-28 | 2017-10-13 | 中国科学院上海高等研究院 | It is a kind of that the process for preparing high-purity lithium salts is extracted from high-Mg Li-contained bittern |
| CN104451145B (en) * | 2014-11-25 | 2017-08-11 | 中国科学院青海盐湖研究所 | Extraction is except the method for iron in a kind of mixed solution from chloride |
| CN104784967B (en) * | 2015-03-25 | 2016-09-14 | 合肥通用机械研究院 | One is the most adjustable level reflow type centrifugal extractor and a control method thereof |
| CN105420521B (en) * | 2015-12-30 | 2018-04-24 | 江阴加华新材料资源有限公司 | A kind of organic extractant phase Rare Earth Separation technique |
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