CN114832762A - High-mixing type continuous rotating reactor and method for preparing aluminum salt lithium adsorbent by using same - Google Patents
High-mixing type continuous rotating reactor and method for preparing aluminum salt lithium adsorbent by using same Download PDFInfo
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- CN114832762A CN114832762A CN202210606385.0A CN202210606385A CN114832762A CN 114832762 A CN114832762 A CN 114832762A CN 202210606385 A CN202210606385 A CN 202210606385A CN 114832762 A CN114832762 A CN 114832762A
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 56
- 238000002156 mixing Methods 0.000 title claims abstract description 45
- FCVHBUFELUXTLR-UHFFFAOYSA-N [Li].[AlH3] Chemical compound [Li].[AlH3] FCVHBUFELUXTLR-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 78
- 238000005070 sampling Methods 0.000 claims abstract description 9
- 238000004891 communication Methods 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims description 22
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 13
- 125000006850 spacer group Chemical group 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 10
- 230000008093 supporting effect Effects 0.000 claims description 3
- 239000011541 reaction mixture Substances 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 37
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 28
- 239000007788 liquid Substances 0.000 description 20
- 239000002245 particle Substances 0.000 description 15
- 238000001179 sorption measurement Methods 0.000 description 15
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 14
- 229910052744 lithium Inorganic materials 0.000 description 14
- 239000002243 precursor Substances 0.000 description 12
- 238000000975 co-precipitation Methods 0.000 description 11
- 238000000926 separation method Methods 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 238000003828 vacuum filtration Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- 239000012267 brine Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- 239000012065 filter cake Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 230000002572 peristaltic effect Effects 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 description 5
- 238000012544 monitoring process Methods 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 210000004243 sweat Anatomy 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000012156 elution solvent Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- -1 aluminum ions Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Images
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28085—Pore diameter being more than 50 nm, i.e. macropores
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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
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- Chemical Kinetics & Catalysis (AREA)
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- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a high-mixing type continuous rotating reactor, which comprises: a housing defining a receiving chamber therein, said housing acting as a stator; the rotor is arranged in the accommodating cavity, the shape of the rotor is matched with that of the accommodating cavity, and a reaction gap is formed between the outer surface of the rotor and the surface of the accommodating cavity at intervals; at least one feed port in communication with the reaction gap; at least one sampling port in communication with the reaction gap; a shim receiving position disposed between the housing and the rotor for receiving shims having a thickness, the reaction gap being adjustable by adjusting the thickness of a single shim or selecting the number of shims. The invention also relates to a method for preparing the aluminum salt lithium adsorbent by using the high-mixing type continuous rotating reactor.
Description
Technical Field
The invention belongs to the field of mixed reactors, and particularly relates to a high-mixing type continuous rotating reactor. The invention also relates to a method for preparing the aluminum salt lithium adsorbent by using the high-mixing type continuous rotating reactor.
Background
At present, with the development of portable lithium batteries, electric vehicles, and the like, the demand for lithium resources is increasing. Most of the lithium resources exist in salt lake brine in China. Because the salt lake brine in China generally has the problem of high magnesium-lithium ratio, the separation and processing of lithium resources are greatly hindered, and the development and utilization of the salt lake resources in China are seriously influenced.
In the prior art, the traditional methods for separating and extracting lithium resources comprise a precipitation method, a solvent extraction method, a membrane separation method and an adsorption method. Wherein the adsorption method has unique advantages in extracting the lithium resource in the brine with the characteristics. The selection of the adsorbent is the most critical step in the adsorption method, and commonly used adsorbents are an ion sieve type adsorbent and an aluminum salt lithium adsorbent.
Lithium aluminate adsorbents, Li/Al-LDHs, have been developed for lithium extraction from aluminum salt precipitates, and the chemical formula of the adsorbent is generally LiCl. mAl (OH) 3 ·nH 2 O, proved to be suitable for the brine resource featuring high magnesium-lithium ratio, has the characteristics of strong selectivity, good adsorption capacity and strong cycling stability, and is widely demanded by the market at present.
In the prior art, the preparation method of the aluminum salt lithium adsorbent generally comprises a hydrothermal method, a mechanochemical method, a coprecipitation method and the like. Although the aluminum salt lithium adsorbent synthesized by the hydrothermal method has good crystal form and uniform particle size, the aluminum salt lithium adsorbent needs to be carried out in a high-temperature and high-pressure environment, the conditions are strict, and the cost is high; while the mechanochemical method can reduce the use of solvents in the synthesis process, the prepared adsorbent has non-uniform grain diameter; the coprecipitation method can directly obtain powder material with uniform chemical components, small granularity and uniform distribution, and is more suitable for synthesizing the aluminum salt adsorbent.
In recent years, researchers have tried to influence the co-precipitation process of preparing aluminum lithium salt adsorbents by using different reactors, such as stirred tank reactors, hypergravity reactors, micro-reactors, and the like. Although these reactors can achieve some degree of homogenization of the aluminum salt lithium adsorbent, problems still exist in that the reaction space is not suitable, resulting in insufficient micromixing or restricting fluid turbulence.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a high-mixing type continuous rotary reactor which is used for replacing a traditional reaction kettle to prepare an aluminum salt lithium adsorbent by a coprecipitation method, so that the coprecipitation reaction space is limited, a high-speed rotating reaction process is provided, the problems of insufficient micromixing and limited fluid turbulence are solved, and the preparation of the aluminum salt lithium adsorbent with high uniformity is realized.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a highly mixed continuous rotary reactor comprising: a housing defining a receiving chamber therein, said housing acting as a stator; the rotor is arranged in the accommodating cavity, the shape of the rotor is matched with that of the accommodating cavity, and a reaction gap is formed between the outer surface of the rotor and the surface of the accommodating cavity at intervals; at least one feed inlet in communication with the reaction gap; at least one sampling port in communication with the reaction gap; a shim receiving position disposed between the housing and the rotor for receiving shims having a thickness, the reaction gap being adjustable by adjusting the thickness of a single shim or selecting the number of shims.
Specifically, the relative position between the stator and the rotor is adjusted by the supporting action of the spacer, thereby achieving adjustment of the reaction gap.
Preferably, the thickness of the shim is 0.2mm and the reaction gap is increased by 0.05mm for each additional shim.
Preferably, the rotor has a circular truncated cone shape, and the accommodating cavity has an inner cavity of an opposite shape adapted to the rotor.
In an improvement of the above technical solution, the inclination of the circular truncated cone is 60 to 80 degrees, that is, an inclination angle of 60 to 80 degrees exists between a generatrix of the rotor and a horizontal direction, and particularly preferably, the inclination of the circular truncated cone is 75 degrees.
As a further improvement to the above technical solution, the high-mixing continuous rotation reactor further comprises a driving motor for driving the rotor to rotate, and the driving motor is provided with a controller for controlling the driving motor to start, stop, rotate forward, rotate backward, and adjust the rotation speed.
The second purpose of the invention is to provide a method for preparing aluminum salt lithium adsorbent by using the high-mixing type continuous rotating reactor provided by the invention. The high-mixing type continuous rotating reactor is suitable for the existing preparation method of the aluminum salt lithium adsorbent which is mature to be applied in the prior art. Preferably, the method comprises the steps of:
a. adjusting the high-mixing type continuous rotating reactor to a required reaction gap through a gasket;
b. introducing a lithium-aluminum mixed solution prepared in advance and alkali liquor into the high-mixing type continuous rotary reactor;
c. controlling reaction conditions to carry out mixed reaction;
d. and after the reaction is finished, collecting the reaction mixture, aging and drying to obtain the aluminum salt lithium adsorbent.
Wherein, the step of preparing the lithium-aluminum mixed solution and the alkali liquor in advance comprises the following steps: adding lithium salt and aluminum salt into deionized water for dissolving, and performing ultrasonic treatment to ensure that the molar ratio of lithium to aluminum is (0.15-5): 1, the concentration of lithium ions is 0.01-18 mol/L, and the concentration of aluminum ions is 0.1-10 mol/L; dissolving alkali in deionized water to prepare alkali liquor with the concentration of 2-20 mol/L; the conditions of the ultrasonic treatment were: and carrying out ultrasonic treatment at the temperature of 30-100 ℃ for 10-100 min. Wherein the aluminum salt is at least one of aluminum nitrate, aluminum sulfate and aluminum chloride. The lithium salt is at least one of lithium sulfate, lithium nitrate, lithium hydroxide, lithium chloride and lithium perchlorate. The alkali is at least one of sodium hydroxide, lithium hydroxide, potassium hydroxide, sodium metaaluminate and ammonia water.
Preferably, the step of adjusting the highly mixed continuous rotary reactor to a desired reaction gap by means of a spacer includes adjusting the reaction gap of the highly mixed continuous rotary reactor to 0.15mm to 0.2 mm. After the reaction gap is adjusted, a mixing reaction can be carried out in a high-mixing type continuous rotating reactor, and the method specifically comprises the following steps: respectively pumping the lithium-aluminum mixed solution and the alkali liquor into a high-mixing type continuous rotary reactor through two feed ports under the action of a peristaltic pump, adding an aqueous solution of an organic dispersing agent with the mass fraction of 0.02-8% through any feed port, controlling the feed flow of the lithium-aluminum mixed solution to be 10-200 mL/min, controlling the feed flow of the alkali liquor to be 2-100 mL/min, controlling the temperature in the reaction process to be 20-150 ℃, controlling the range of a reaction gap to be 0.1-5 mm, particularly 0.15-0.2 mm, controlling the rotating speed of the reactor to be 1000-6000 rpm, monitoring the pH value of effluent liquid at an outlet, controlling the pH value to be 2-13, and collecting the effluent liquid. Wherein the organic dispersant is at least one of polyvinyl alcohol, polyethylene glycol and polyacrylamide. Then, aging the effluent, wherein the aging time is preferably 0.4-24 h, the stirring speed is controlled to be 100-400 rpm in the aging process, and the temperature is controlled to be 20-150 ℃, so as to obtain a precursor; cooling the obtained precursor, performing solid-liquid separation after the precursor is cooled to room temperature, washing a filter cake by using a solvent with the temperature of 20-50 ℃, performing vacuum drying, controlling the drying temperature to be 40-150 ℃, drying for 1-48 h, then grinding into powder, performing an elution process in the solvent with the temperature of 20-150 ℃, and controlling the ratio of the powder to the solvent to be 1g: (5-500) mL, controlling the elution time to be 0.5-8 h, performing solid-liquid separation, drying for 1-48 h, and grinding into powder to obtain the aluminum salt lithium adsorbent. Wherein the solid-liquid separation mode is at least one of vacuum filtration, centrifugal separation, gravity sedimentation and decantation; the elution solvent is at least one of ethanol, deionized water, ultrapure water, acetone, methanol and chloroform; the temperature of the vacuum drying is 50-120 ℃, and the time is 4-24 hours; the adding proportion of the precursor to the elution solvent is 1g (5-800) mL.
The molecular formula of the aluminum salt lithium adsorbent prepared by the invention is LiCl. mAl (OH) 3 ·nH 2 O, wherein m is 2 to 10, and n is 0.5 to 10.
Due to the adoption of the technical scheme, the invention has the following advantages and beneficial effects:
the high-mixing type continuous rotating reactor adopted by the invention has the advantages of narrow reaction space, higher fluid flow rate and shear rate, microreactor, impinging stream reactor and hypergravity reactor based on reducing reaction space and improving fluid flow rate to influence the coprecipitation process, and is simple to operate, rapid in reaction, easy to control required conditions, low in energy consumption, free of high temperature and high pressure and the like. In addition, the main raw materials are cheap and easy to obtain, the operation conditions in the synthesis process are high in elasticity, the feeding flow and the rotating speed can be flexibly changed according to actual conditions, and large-scale production is easy to realize.
The aluminum salt lithium adsorbent prepared by the high-mixing type continuous rotating reactor and the method of the invention conforms to the original crystal structure, the particle size distribution range is narrowed, and the volume average particle size of the particles can reach 784 mu m at most. In addition, the lithium ion battery has stable property, the maximum adsorption capacity to lithium can reach 7.29mg/g, and the lithium ion battery has good lithium adsorption performance.
Drawings
FIG. 1a is a schematic view of a highly mixed continuous rotary reactor provided according to an embodiment of the present invention;
FIG. 1b shows a cross-sectional view of portion A shown in FIG. 1 a;
FIG. 2 is a schematic diagram of a highly-mixed continuous rotary reactor system provided in accordance with an embodiment of the present invention;
FIG. 3 shows lithium aluminate adsorbents LiCl. mAl (OH) synthesized in examples 1 to 4 according to the present invention 3 ·nH 2 An XRD pattern of O, wherein the X-ray diffractometer scans the entire area at an angle of 2 θ;
FIG. 4 shows lithium aluminate adsorbents LiCl. mAl (OH) synthesized in examples 1 to 4 according to the present invention 3 ·nH 2 The particle size distribution map of O;
FIG. 5 shows lithium aluminate adsorbents LiCl. mAl (OH) synthesized in examples 1 to 4 according to the present invention 3 ·nH 2 SEM image of O.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Fig. 1a shows a high-mixing type continuous rotary reactor 100 according to an embodiment of the present invention, and fig. 1b shows a cross-sectional view of a dotted-line box a portion of fig. 1a, in which the high-mixing type continuous rotary reactor 100 includes a housing 1 defining a housing chamber 11 therein, the housing 1 serving as a stator; the rotor 2 is arranged in the accommodating cavity 11, the shape of the rotor 2 is matched with that of the accommodating cavity 11, and a reaction gap 3 is formed between the outer surface of the rotor 2 and the surface of the accommodating cavity 11 at intervals; a first feed opening 31 and a second feed opening 32 communicating with said reaction gap 3; a sampling port 33 communicated with the reaction gap 3, wherein the sampling port 33 is provided with a sampling valve for controlling the opening and closing of the sampling port 33; and a spacer placing position 4 provided between the housing 1 and the rotor 2 for placing a spacer having a thickness, the reaction gap 3 being adjustable by adjusting the thickness of the individual spacers or selecting the number of spacers.
In a preferred embodiment, the rotor 2 has a truncated cone-like shape and the receiving cavity 3 has an inner cavity of opposite shape adapted to the rotor 2, as shown in fig. 1 b.
In a further preferred embodiment, the rotor 2 has a height of 20mm, an upper diameter of 44mm, a lower diameter of 60mm and a cone inclination of 75 degrees.
In a preferred embodiment, the rotor 2 is driven to rotate by a driving motor 5, and the driving motor 5 is provided with a controller 7 which is provided with switches, a rotation speed adjusting button, a rotation speed parameter display screen and the like and is used for controlling the starting, stopping, forward rotation, reverse rotation and rotating speed adjustment of the driving motor 5, wherein the rotating speed adjusting range is 0 rpm-9000 rpm.
In addition, a support frame 6 is provided for mounting the driving motor 6 and supporting the entire high mixing type continuous rotary reactor 100.
Referring to fig. 2, an embodiment of the present invention further provides a high-mixing type continuous rotary reactor system 1000 for preparing an aluminum salt lithium adsorbent, comprising a high-mixing type continuous rotary reactor 100, a first supply system 200 for supplying a lithium-aluminum mixed solution to the high-mixing type continuous rotary reactor 100 through a first feed opening 31 and a second supply system 300 for supplying a lye to the high-mixing type continuous rotary reactor 100 through a second feed opening 32, and a collection system 400 for collecting an effluent. The first supply system 200 and the second supply system 300 control the flow rate of the solution to the highly mixed continuous rotary reactor 100 by means of pumps, in particular peristaltic pumps 201, 302.
By utilizing the high-mixing type continuous rotating reactor provided by the invention, the coprecipitation reaction is completed at one step, and the reaction product is directly collected at the sampling port. Meanwhile, the rotating speed of the reactor can be adjusted, so that the high-mixing type continuous rotating reactor can carry out reaction under the condition of different rotating speeds. The outer stator is fixed and the inner rotor can rotate at a stable rotational speed. The reactor with the structure has the advantages of narrow reaction space, higher fluid flow rate and shear rate, and the advantages of a micro reactor, an impinging stream reactor and a hypergravity reactor, and can enable reaction products to be more fully and uniformly mixed compared with the existing mixing reactor (such as a jacketed reaction kettle) under the same reaction condition, so that the reaction in the reactor is more fully and thoroughly. The reactor is particularly suitable for coprecipitation reaction, such as coprecipitation method for preparing aluminum salt lithium adsorbent.
The high-mixing continuous rotary reactor 100 provided in this example operates as follows:
first, the size of the required reaction gap 3 is determined, and a corresponding number of shims is placed at the shim placement position 4. In a preferred embodiment, each spacer is 0.2mm thick, and at the spacer placement site 4, no less than 2 spacers are placed in reaction. The reaction gap increases by 0.05mm for each additional shim. In a preferred embodiment, the reaction gap is adjusted to 0.15mm to 0.2 mm.
Taking the preparation of aluminum-salt lithium adsorbent as an example, the operation of the reactor of the present invention is as follows:
the lithium-aluminum mixed solution and the alkali liquor which are prepared in advance are respectively placed in the first supply system 200 and the second supply system 300 and are respectively introduced into the high mixing type continuous rotating reactor 100 through the first feeding port 31 and the second feeding port 32; controlling the reaction conditions to carry out mixing reaction in a high-mixing type continuous rotating reactor 100; the effluent is collected through sampling port 33 to collection system 400.
The effluent treatment also includes an aging step and a drying separation step.
In order to verify the performance of the high-mixing continuous rotary reactor provided by the invention, the following examples provide that aluminum salt lithium adsorbent samples 1 to 4 are prepared in the high-mixing continuous rotary reactor provided by the invention by adopting different reaction proportions and reaction conditions, and the prepared aluminum salt lithium adsorbent samples 1 to 4 are subjected to XRD and SEM characterization and tested for particle size distribution diagrams and adsorption capacity.
Example 1
Firstly, preparing lithium-aluminum mixed solution and alkali liquor
Aluminum chloride (56g, 0.42mol) and lithium chloride (7g, 0.16mol) were dissolved in 500mL of deionized water, where Al 3+ Concentration of 0.84mol/L, Li + The concentration was 0.33 mol/L. And (3) placing the solution in a heating and stirring table, stirring for half an hour, and then performing ultrasonic treatment in an ultrasonic instrument at the temperature of 75 ℃ for 60min to ensure that the solution is fully and uniformly mixed to obtain the lithium-aluminum mixed solution.
320g of sodium hydroxide is put into 1L of deionized water to prepare 8M sodium hydroxide lye.
Second, mixed reaction
Pumping 8M sodium hydroxide lye with the feeding flow of 10.5mL/min and lithium-aluminum mixed solution with the feeding flow of 30mL/min into a high-mixing type continuous rotary reactor 100 through a first feeding port 31 and a second feeding port 32 respectively under the action of peristaltic pumps 201 and 301, controlling the temperature in the reaction process at 20 ℃, the reaction gap at 0.2mm, controlling the rotating speed of the high-mixing type continuous rotary reactor at 1000rpm, adding a polyvinyl alcohol aqueous solution with the polyvinyl alcohol mass fraction of 0.5% of an organic dispersing agent from any one feeding port, monitoring the pH value of an outlet by using a pH meter after feeding for 15min, controlling the pH value of the effluent to be 5, and collecting the effluent.
The third step, aging
Aging the effluent liquid in the second step for 24h, wherein the stirring speed is controlled to be 300rpm in the aging process, and the temperature is controlled to be 80 ℃ to obtain 5g of precursor;
the fourth step, drying and separating
After the third step of aging is finished, 5g of the obtained precursor is cooled to room temperature, vacuum filtration solid-liquid separation is carried out on a vacuum filtration pump, 200mL of deionized water at the room temperature is used for washing a filter cake in the process, then the filter cake is dried for 24 hours at the temperature of 80 ℃, an agate mortar is used for grinding the filter cake into powder, and 4g of aluminum-salt-lithium adsorbent sample 1 is obtained, wherein the chemical formula of the sample is LiCl. mAl (OH) 3 ·nH 2 O, wherein m is 4.1 and n is 5.2.
Example 2
The procedure of "lithium-aluminum mixed solution and lye preparation" in this example was exactly the same as in example 1.
Second, mixed reaction
Pumping 8M sodium hydroxide lye with a feeding flow of 14.5mL/min and lithium-aluminum mixed solution with a feeding flow of 45mL/min into a high-mixing type continuous rotary reactor 100 through a first feeding port 31 and a second feeding port 32 respectively under the action of peristaltic pumps 201 and 301, controlling the temperature in the reaction process at 20 ℃, the reaction gap at 0.2mm, controlling the rotating speed of the high-mixing type continuous rotary reactor at 2000rpm, adding an organic dispersion solution with the mass fraction of 2% of polyvinyl alcohol into the reaction gap from any feeding port, monitoring the pH value of an effluent liquid outlet by using a pH meter after feeding for 10min, controlling the pH value of the effluent liquid at 5, and collecting the effluent liquid.
The third step, aging
Aging the effluent liquid in the second step for 24h, wherein the stirring speed is controlled to be 300rpm in the aging process, and the temperature is controlled to be 80 ℃ to obtain 5g of precursor;
the fourth step, drying and separating
After the third step of aging is finished, cooling the obtained 5g of precursor to room temperature, carrying out vacuum filtration solid-liquid separation on a vacuum filtration pump, flushing filter cakes by 200mL of deionized water at normal temperature in the process, and then drying for 24 hours at the temperature of 80 DEG CPulverized using an agate mortar to obtain 4g of an aluminum lithium salt adsorbent sample 2 having a chemical formula of LiCl. mAl (OH) 3 ·nH 2 O, wherein m is 3.7 and n is 4.
Example 3
The procedure of "lithium aluminum mixed solution and lye preparation" in this example was exactly the same as in example 1.
Second, mixed reaction
Pumping 8M sodium hydroxide alkaline liquor with the feeding flow of 18mL/min and lithium-aluminum mixed solution with the feeding flow of 60mL/min into a high-mixing type continuous rotary reactor 100 through a first feeding port 31 and a second feeding port 32 under the action of peristaltic pumps 201 and 301, controlling the temperature in the reaction process to be 20 ℃, the reaction gap to be 0.2mm, controlling the rotating speed of the high-mixing type continuous rotary reactor to be 3000rpm, adding organic dispersion solution with the mass fraction of polyacrylamide of 3% into a reaction space from any feeding port, monitoring the pH value of effluent liquid at an outlet by using a pH meter after feeding the sample for 10min, controlling the pH value of the effluent liquid to be 5, and collecting the effluent liquid.
The third step, aging
Aging the effluent liquid in the second step for 24h, wherein the stirring speed is controlled to be 300rpm in the aging process, and the temperature is controlled to be 80 ℃ to obtain 5g of precursor;
the fourth step, drying and separating
After the third step of aging, cooling the obtained 5g of precursor to room temperature, carrying out vacuum filtration solid-liquid separation on a vacuum filtration pump, adding 200mL of normal-temperature deionized water to wash a filter cake in the process, then drying for 24 hours at the temperature of 80 ℃, and grinding into powder by using an agate mortar to obtain 4g of aluminum-salt-lithium adsorbent sample 3, wherein the chemical formula of the sample is LiCl. mAl (OH) 3 ·nH 2 O, wherein m is 2.9 and n is 4.
Example 4
The procedure of "lithium-aluminum mixed solution and lye preparation" in this example was exactly the same as in example 1.
Second, mixed reaction
Pumping 8M sodium hydroxide lye with the feeding flow of 28.5mL/min and lithium-aluminum mixed solution with the feeding flow of 90mL/min into a high-mixing type continuous rotary reactor 100 through a first feeding port 31 and a second feeding port 32 respectively under the action of peristaltic pumps 201 and 301, controlling the temperature in the reaction process at 20 ℃, the reaction gap at 0.2mm, controlling the rotating speed of the high-mixing type continuous rotary reactor at 5000rpm, adding organic dispersion solution with the mass fraction of polyethylene glycol of 8% into a reaction space from any feeding port, monitoring the pH value of effluent at an outlet by using a pH meter after feeding for 10min, controlling the pH value of the effluent to be 5, and collecting the effluent.
The third step, aging
Aging the effluent liquid in the second step for 24h, wherein the stirring speed is controlled to be 300rpm in the aging process, and the temperature is controlled to be 80 ℃ to obtain 5g of precursor;
the fourth step, drying and separating
After the third step of aging is finished, cooling the obtained 5g of precursor to room temperature, carrying out vacuum filtration solid-liquid separation on a vacuum filtration pump, adding 200mL of normal-temperature deionized water to wash a filter cake in the process, then drying for 24 hours at the temperature of 80 ℃, and grinding into powder by using an agate mortar to obtain 4g of aluminum-salt-lithium adsorbent sample 4, wherein the chemical formula of the sample is LiCl. mAl (OH) 3 ·nH 2 O, wherein m is 4 and n is 5.2.
After the lithium aluminate adsorbent samples 1-4 were prepared, XRD, SEM and particle size tests were performed on each product, and the results are shown in fig. 3-5.
FIG. 3 shows the synthesized AlLi-aluminate adsorbents LiCl. mAl (OH) in examples 1 to 4 3 ·nH 2 An XRD pattern of O, wherein the X-ray diffractometer scans the entire area at an angle of 2 θ; FIG. 4 shows the synthesized aluminum-salt lithium adsorbents LiCl. mAl (OH) in examples 1 to 4 3 ·nH 2 The particle size distribution map of O; FIG. 5 shows the synthesized AlLi-aluminate adsorbents LiCl. mAl (OH) in examples 1 to 4 3 ·nH 2 SEM image of O.
The XRD pattern in figure 3 shows that the prepared adsorbent well conforms to the peak shape of the lithium-aluminum layered hydroxide, the diffraction peak is weaker, the peak shape is low and flat, the half-peak width is wider, the crystal form is good, and no other substance impurity peak appears. As can be seen from fig. 4 and 5, the particle size distribution range of the adsorbent is narrow, and the adsorbent is distributed in a droplet aggregation state.
The adsorption capacity of the aluminum salt lithium adsorbent samples 1-4 is tested, and the specific test results are as follows:
adding the prepared aluminum salt lithium adsorbent into Carer sweat brine according to the solid-to-liquid ratio of 1g/30mL, wherein the composition of the Carer sweat brine is shown in Table 1, reacting in a constant-temperature air shaking table at 25 ℃ and 150rpm for 48 hours, taking out, and measuring Li in the lithium-containing solution before and after adsorption of the aluminum salt lithium adsorbent by ICP (inductively coupled plasma) + The adsorption capacity is calculated according to the concentration change of the aluminum salt lithium adsorbent, and the adsorption capacity of the aluminum salt lithium adsorbent samples 1-4 is shown in table 2.
TABLE 1
| Components | Li + | Mg 2+ | Na + | K + | Ca 2+ |
| Concentration (ppm) | 350 | 112242 | 1555 | 564 | 48 |
TABLE 2
| Example 1 | Example 2 | Example 3 | Example 4 | |
| q e (mg/g) | 7.29 | 6.87 | 6.56 | 7.11 |
When a common jacketed reaction kettle is used as a coprecipitation reactor to prepare the aluminum salt lithium adsorbent, the reaction space is large, the reaction process is only mixed by a stirring paddle, and the problems of overlarge reaction space, insufficient reaction mixing and the like exist. The aluminum salt lithium adsorbent prepared by the traditional reaction kettle coprecipitation has wide particle size distribution range, the average particle size of the particle volume is 76.4 mu m, and the lithium adsorption amount to the Carlo sweat brine is about 6 mg/g. Correspondingly, as shown in fig. 4 and table 2, the aluminum salt lithium adsorbent prepared by the high-mixing continuous rotating reactor provided by the invention has a narrow particle size distribution range, a particle volume average particle size of 784 μm, and a lithium adsorption amount of about 7mg/g, which is as high as 7.29mg/g, and is increased to a certain extent compared with the adsorption amount of the adsorbent prepared by a general jacketed reactor, i.e., the aluminum salt lithium adsorbent prepared by the reactor has higher uniformity and good lithium adsorption performance.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A highly mixed continuous rotary reactor, comprising:
a housing defining a receiving chamber therein, said housing acting as a stator;
the rotor is arranged in the accommodating cavity, the shape of the rotor is matched with that of the accommodating cavity, and a reaction gap is formed between the outer surface of the rotor and the surface of the accommodating cavity at intervals;
at least one feed port in communication with the reaction gap;
at least one sampling port in communication with the reaction gap;
a shim receiving position disposed between the housing and the rotor for receiving shims having a thickness, the reaction gap being adjustable by adjusting the thickness of a single shim or selecting the number of shims.
2. The highly-mixed continuous rotary reactor according to claim 1, wherein the adjustment of the reaction gap is achieved by adjusting the relative position between the stator and the rotor by the supporting action of the spacers.
3. The highly-mixed continuous rotary reactor according to claim 1, wherein the thickness of the spacer is 0.2 mm.
4. The highly-mixed continuous rotary reactor according to claim 3, wherein the reaction gap is increased by 0.05mm for each additional shim.
5. The highly mixed continuous rotary reactor of claim 1, wherein the rotor has a frustoconical shape and the receiving cavity has an inner cavity of opposite shape that fits the rotor.
6. The highly-mixed continuous rotary reactor according to claim 5, wherein the inclination of the circular truncated cone is 60 to 80 degrees.
7. The highly-mixed continuous rotary reactor according to claim 1, further comprising a driving motor for driving the rotor to rotate.
8. The highly-mixed continuous rotary reactor according to claim 7, wherein the drive motor is provided with a controller for controlling the start, stop, forward rotation, reverse rotation, and adjustment of the rotation speed of the drive motor.
9. A method for preparing an aluminum salt lithium adsorbent using the highly mixed continuous rotary reactor according to any one of claims 1 to 8, comprising the steps of:
a. adjusting the high-mixing type continuous rotating reactor to a required reaction gap through a gasket;
b. introducing a lithium-aluminum mixed solution prepared in advance and alkali liquor into the high-mixing type continuous rotary reactor;
c. controlling reaction conditions to carry out mixed reaction;
d. and after the reaction is finished, collecting the reaction mixture, aging and drying to obtain the aluminum salt lithium adsorbent.
10. The method of claim 9, wherein in step a, the reaction gap is adjusted to 0.15mm to 0.2 mm.
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