CN114289000B - Salt lake lithium extraction adsorbent and preparation method thereof - Google Patents
Salt lake lithium extraction adsorbent and preparation method thereof Download PDFInfo
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- CN114289000B CN114289000B CN202111618049.XA CN202111618049A CN114289000B CN 114289000 B CN114289000 B CN 114289000B CN 202111618049 A CN202111618049 A CN 202111618049A CN 114289000 B CN114289000 B CN 114289000B
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 77
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 38
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000605 extraction Methods 0.000 title claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 55
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 230000008961 swelling Effects 0.000 claims abstract description 18
- 239000011780 sodium chloride Substances 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 229920000620 organic polymer Polymers 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000010936 titanium Substances 0.000 claims abstract description 12
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 11
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920002545 silicone oil Polymers 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 49
- 239000005995 Aluminium silicate Substances 0.000 claims description 46
- 235000012211 aluminium silicate Nutrition 0.000 claims description 46
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 46
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- 229910001416 lithium ion Inorganic materials 0.000 claims description 24
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 21
- 239000002244 precipitate Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 19
- -1 polypropylene Polymers 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000007731 hot pressing Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 229920001912 maleic anhydride grafted polyethylene Polymers 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 5
- 150000003608 titanium Chemical class 0.000 claims description 5
- 239000003480 eluent Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 4
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 4
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- 244000043261 Hevea brasiliensis Species 0.000 claims 1
- 229920003052 natural elastomer Polymers 0.000 claims 1
- 229920001194 natural rubber Polymers 0.000 claims 1
- 229910003002 lithium salt Inorganic materials 0.000 abstract description 5
- 159000000002 lithium salts Chemical class 0.000 abstract description 5
- 238000001179 sorption measurement Methods 0.000 description 29
- 235000002639 sodium chloride Nutrition 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 16
- 230000035699 permeability Effects 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 12
- 238000004090 dissolution Methods 0.000 description 11
- 239000012267 brine Substances 0.000 description 8
- 239000011148 porous material Substances 0.000 description 8
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical group [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229910001437 manganese ion Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 description 2
- 235000011008 sodium phosphates Nutrition 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The application relates to the technical field of lithium salt extraction, in particular to a salt lake lithium extraction adsorbent and a preparation method thereof, wherein the salt lake lithium extraction adsorbent is prepared from the following raw materials in parts by weight: 40-60 parts of titanium source, 20-30 parts of lithium source, 5-10 parts of swelling organic polymer, 10-15 parts of 10-15% strong acid solution, 5-10 parts of solid carrier, 0.1-0.3 part of dispersing agent, 0.2-0.5 part of first pore-forming agent, 10-15 parts of sodium chloride solution, 5-10 parts of silicone oil, 1-2 parts of cross-linking agent, 5-8 parts of sodium chloride solution and 15-20 parts of 10-15% sodium hydroxide solution.
Description
Technical Field
The application relates to the technical field of lithium salt extraction, in particular to a salt lake lithium extraction adsorbent and a preparation method thereof.
Background
The lithium resource is an important raw material of the lithium battery, is an 'energy metal' with strategic significance, and is mainly distributed in brine and ores, wherein the ratio of the brine lithium resource is more than 60%, and compared with the production of lithium salt by taking the brine lithium resource as a raw material and the production of lithium salt by taking the ores as the raw material, the lithium battery has the advantages of low energy consumption, low cost, 30-50% of comprehensive cost saving, more salt lakes in China, abundant brine lithium resource and high lithium concentration, and is especially suitable for Qinghai and Tibet areas in China. At present, the salt lake lithium extraction in China mainly adopts the technical routes of an ion exchange adsorption method, a solvent extraction method, a membrane separation method, a calcination leaching method, a solar cell method, electrochemistry and the like, and the technical points of the technical methods are that the selectivity, the universality and the reusability of the adsorption extraction material on lithium ions and the device cost under the influence of environmental factors.
The ion exchange adsorption method mainly adopts a selective adsorbent to adsorb Li+, then uses a nanofiltration membrane to remove magnesium under an acidic condition after eluting Li+ by using an eluent, and finally obtains a high-lithium qualified liquid after reverse osmosis concentration and natural evaporation concentration in a salt field, and finally precipitates and filters to obtain a lithium carbonate product. The most important part of the ion exchange adsorption method is an adsorbent, the performance of which determines the process of the ion exchange adsorption method, the adsorbent can remove a large amount of coexisting alkali metals in brine, and selectively adsorb lithium ions in the brine, and commonly used lithium adsorbents can be classified into organic adsorbent resin adsorbents and inorganic adsorbents, and inorganic adsorbents can be classified into ion sieve adsorbents, aluminum salt adsorbents, natural mineral adsorbents and the like.
The ion sieve adsorbent can be divided into a manganese ion sieve and a titanium ion sieve, and the manganese ion sieve has the advantages of good adsorption capacity, good selectivity and stability for lithium ions, but serious manganese dissolution loss problem, high lithium salt impurity, reduced adsorption capacity due to time change and poor cycle performance; in order to solve the problem of manganese dissolution loss, the titanium ion sieve is further developed, and has stable property, low dissolution loss, good acid resistance and large adsorption capacity, but the titanium ion sieve is in powder form, has lower permeability and adsorption rate, has long adsorption period, and can greatly reduce the adsorption capacity after being molded and granulated.
Disclosure of Invention
In order to solve the technical problems, the application provides a salt lake lithium extraction adsorbent and a preparation method thereof.
In a first aspect, the present application provides a salt lake lithium extraction adsorbent, which adopts the following technical scheme:
the salt lake lithium extraction adsorbent is prepared from the following raw materials in parts by weight:
40-60 parts of titanium source
20-30 parts of lithium source
5-10 parts of swelling organic polymer
10 to 15 parts of strong acid solution with mass fraction of 10 to 15 percent
5-10 parts of solid carrier
0.1 to 0.3 part of dispersing agent
0.2 to 0.5 part of first pore-forming agent
10 to 15 parts of sodium chloride solution
5 to 10 parts of silicone oil
1 to 2 portions of cross-linking agent
15 to 20 parts of 10 to 15 percent sodium hydroxide solution.
By adopting the technical scheme, the adsorption capacity of the prepared salt lake lithium extraction adsorbent is increased, the permeability and the adsorption rate are increased, and the adsorption time is shortened. The titanium source reacts with the strong acid solution with the mass fraction of 10-15% to generate titanium ions, then the lithium source is added, the lithium source reacts with the strong acid solution to generate lithium ions, then the pH value in the system is regulated by adding the sodium hydroxide solution with the mass fraction of 10-15%, so that solid precipitate is generated, the generated solid precipitate is fluffy in structure, the content of the lithium ions absorbed by the prepared adsorbent is increased, the strong acid solution with the mass fraction of 10-15% is one of the hydrochloric acid solution with the mass fraction of 10-15%, the sulfuric acid solution with the mass fraction of 10-15% and the nitric acid solution with the mass fraction of 10-15%, and the strong acid solution with the mass fraction of 10-15% reacts with the titanium source and the lithium source more fully.
The generated precipitate can be adhered to the surface of the solid carrier to form larger particles, so that the agglomeration of the precipitate is reduced, the space for absorbing lithium ions is reduced, and the particles are uniformly dispersed in the system, so that the adsorbent can further absorb more lithium ions.
When the swelling organic polymer is soaked in salt lake water, the swelling organic polymer can expand to enable the internal structure to be fluffy, gaps are enlarged, and salt water enters the inside of the adsorbent, so that more lithium ions can be absorbed conveniently.
The solid carrier can be uniformly mixed and connected with the swelling organic polymer, the dispersing agent enables the solid carrier to be uniformly mixed with the swelling organic polymer, the first pore-forming agent increases the number of pores among the swelling organic polymer, and the absorption rate of the adsorbent and the permeability of saline water are improved.
The silicone oil reacts with the cross-linking agent to generate oily matters, so that the oily matters can be stably bonded, meanwhile, the oily matters play a role in lubrication, so that the pores cannot be bonded when the adsorbent is in a dry state, the adsorbent is reused, the pores can be rapidly opened, and the speed of absorbing lithium ions is accelerated.
The sodium chloride provides a solvent environment, so that the solid carrier, the swelling organic polymer, the first pore-forming agent, the dispersing agent and the oily matter are uniformly mixed, and the connection between the solid carrier and the swelling organic polymer is more stable.
Preferably, the solid carrier is a modified solid carrier, and each part of the modified solid carrier is prepared from the following materials in parts by weight:
30-60 parts of kaolin
1 to 2 parts of a second pore-forming agent
2-5 parts of maleic anhydride grafted polyethylene wax
10 to 15 portions of hydrochloric acid solution with the mass fraction of 15 to 20 percent.
By adopting the technical scheme, the prepared modified solid carrier has better adhesiveness, more grooves and holes on the surface, is easier to connect with the sediment, is more stable, and ensures that the prepared adsorbent has good permeability and absorptivity and can increase the absorption capacity of the adsorbent. The second pore-forming agent increases the number of surface furrows of the kaolin, the mass fraction of the second pore-forming agent is 15-20% hydrochloric acid solution enables the surface of the kaolin to have more furrows, the second pore-forming agent is easier to act on carrier kaolin powder, and the maleic anhydride grafted polyethylene wax is adhered to the kaolin, so that the kaolin has better adhesive property and is easier to connect with the solid precipitate.
The second pore-forming agent is sodium chloride, sodium sulfate, sodium phosphate, potassium chloride or potassium sulfate, so that the porosity of the surface of the kaolin can be increased, the specific surface area can be enlarged, and the kaolin can be better connected with the maleic anhydride grafted polyethylene wax.
Preferably, the modified solid support is prepared by the steps of:
1) According to parts by weight, firstly adding 30-60 parts of kaolin and 10-15 parts of hydrochloric acid solution with mass fraction of 15-20% into a reaction kettle, carrying out reflux reaction at 50-60 ℃, stirring for 2-3 hours, filtering, washing with water, and drying to obtain carrier kaolin;
2) Uniformly mixing 1-2 parts by weight of a second pore-forming agent and carrier kaolin, calcining at 850-900 ℃ for 4-5 hours, cooling to 20-30 ℃, and crushing to 50-60 nm to obtain carrier kaolin powder;
3) The carrier kaolin powder is added into a high-speed mixer, the rotating speed is 600-900r/min, and 2-5 parts of maleic anhydride grafted polyethylene wax are uniformly mixed according to parts by weight, so that the modified solid carrier is prepared.
By adopting the technical scheme, the prepared modified solid carrier has better adhesiveness, more holes on the surface, and is easier to connect with the sediment and more stable. Under the condition of 50-60 ℃, the mass fraction of hydrochloric acid solution is 15-20% so that the kaolin surface is more furrows faster, the kaolin surface is easily corroded by hydrochloric acid solution with the mass fraction higher than 20%, the kaolin surface is difficult to be provided with fewer furrows by hydrochloric acid solution with the mass fraction lower than 20%, the amount of solid precipitate connected with the kaolin surface is small, the amount of lithium ions absorbed by the adsorbent is reduced finally, the second pore-forming agent and the carrier kaolin are calcined under the condition of 850-900 ℃ for 4-5 hours, the second pore-forming agent and the carrier kaolin can fully react, the number of furrows on the surface of the carrier kaolin is increased, and the solid precipitate connected with more is facilitated.
Preferably, the swelling organic copolymer is at least one of rubber, polypropylene, polystyrene, ethylene-vinyl acetate copolymer and polyvinyl chloride.
Through adopting above-mentioned swelling organic matter for the adsorbent of preparation has better permeability and absorptivity, and above-mentioned swelling organic matter has good swellability, soaks in solution volume grow, and inner structure is loose, uses the preparation adsorbent with other raw materials cooperation, can make the volume increase of adsorbent in water for the inside space increase of adsorbent, inside the salt solution gets into the adsorbent, is convenient for absorb more lithium ions.
Preferably, the first pore-forming agent is one of ethyl acetate, ethanol, butanone, acetonitrile, isopropanol, trichloroethane or hexane.
The solvent is easy to volatilize, and the solvent can volatilize in the process of preparing the adsorbent, and can not remain in the adsorbent, so that more pores are generated in the adsorbent, and the adsorbent is beneficial to absorbing more lithium ions when in use.
Preferably, the dispersing agent is one of sodium dodecyl sulfate, sodium tripolyphosphate, sodium hexametaphosphate or sodium pyrophosphate.
By adopting the dispersing agent, dialkyl sodium sulfate, sodium tripolyphosphate, sodium hexametaphosphate and sodium pyrophosphate can be dissolved in the sodium chloride solution, and after the dialkyl sodium sulfate, the sodium tripolyphosphate, the sodium hexametaphosphate and the sodium pyrophosphate are dissolved in the sodium chloride solution, the dispersing effect is increased, so that various raw materials in the adsorbent are uniformly mixed, and the permeability and the absorptivity of the adsorbent are further improved.
Preferably, the silicone oil is at least one of methyl hydrogen polysiloxane, tetraethoxysilane, methyl triethoxysilane and vinyl ethyl trilactate siloxane.
Preferably, the cross-linking agent is one of dicumyl peroxide, benzoyl peroxide, dicumyl hydroperoxide or diethylenetriamine.
Through adopting above-mentioned cross-linking agent and above-mentioned silicone oil, the cross-linking agent makes the connection between the silicone oil become three-dimensional structure for the inside space of adsorbent of preparation increases, is favorable to improving the absorptivity and the permeability of adsorbent, increases the adsorption quantity.
Preferably, the preparation method of the salt lake lithium extraction adsorbent comprises the following steps:
adding 40-60 parts by weight of a titanium source into a reaction bottle, adding 10-15 parts by weight of a strong acid solution into the reaction bottle, heating to 80-90 ℃, and carrying out reflux reaction for 0.5-1 h to obtain a titanium salt solution; adding 20-30 parts of lithium source into the titanium salt solution, dropwise adding 5-8 parts of sodium hydroxide solution with the mass fraction of 10-15%, adjusting the pH value to be 8.0-9.0, preparing a solid precipitate, roasting the solid precipitate, crushing, adding the solid precipitate into an eluent, washing lithium ions, washing with water and drying to obtain powder; according to weight parts, under the condition of 100-120 ℃, 5-10 parts of monomer and 1-2 parts of cross-linking agent are reacted to prepare oily reactant; adding 5-10 parts of modified solid carrier into a reactor with a stirring and temperature controlling device, and uniformly mixing the added powder with the modified solid carrier to prepare a composition;
according to parts by weight, 0.2 to 0.5 part of first pore-forming agent, 5 to 10 parts of swelling organic polymer, 0.1 to 0.3 part of dispersing agent and 5 to 8 parts of sodium chloride solution are uniformly stirred with the composition, the mixture is stirred at the temperature of 80 to 100 ℃ until the dispersing agent is dissolved, then the oily reactant is added to prepare a mixture, and the mixture is hot-pressed into a film to prepare the adsorbent.
Through adopting above-mentioned technical scheme, make the salt lake that makes carry lithium adsorbent adsorption capacity increase, permeability and adsorption rate increase, adsorption time shortens, raise the temperature to 80~90 ℃ and make titanium source, lithium source react with strong acid solution, the dropwise add mass fraction is 10~15% sodium hydroxide solution is in order to produce solid precipitate structure more fluffy, adjust pH=8.0 ~9.0 and make titanium ion and lithium ion can fully precipitate in the form of precipitation, it is more loose to bake the internal structure that is in order to fix the precipitate with solid precipitate, be convenient for smash.
The composition, the first pore-forming agent, the swelling organic polymer, the dispersing agent and the sodium chloride solution are stirred, the mixture is stirred at the temperature of 80-100 ℃ until the dispersing agent is dissolved, and the oily reactant is added to ensure that all the components can be fully and uniformly mixed, thereby improving the permeability and the absorption capacity of the adsorbent.
Through the hot pressing of the mixture into the film, the contact area of the adsorbent and the salt lake water is increased so as to absorb more lithium ions, and meanwhile, the film is easy to arrange and collect and is convenient to use.
Preferably, the hot pressing temperature in the hot pressing process is 100-120 ℃, and the hot pressing pressure is 120-160 MPa.
Through adopting above-mentioned technical scheme, through the mode of hot pressing, make the structure of adsorbent more stable, can keep the inside pore structure of film can not take place great deformation simultaneously for the adsorbent of making has good permeability and absorptivity and can increase the absorption capacity of adsorbent. When the pressure of the hot pressing is more than 160MPa, the pores inside the adsorbent are easy to be closed, so that the number of the pores is reduced, and the permeability and the absorptivity of the adsorbent are reduced; when the hot pressing pressure is less than 120Mpa, the film is possibly insufficient in firmness and is easily torn down, so that the use is affected.
The titanium source in the present application is TiO 2 Or Ti (OC) 4 H 9 ) 4 The lithium source is LiOH, li 2 CO 3 Or CH (CH) 3 COOLi。
In summary, the present application has the following beneficial effects:
1. according to the method, the prepared adsorbent has the advantages of high permeability, high absorption rate, short absorption time and large absorption capacity through the compound use of a titanium source, a lithium source, a swelling organic polymer, a strong acid solution with the mass fraction of 10-15%, a solid carrier, a dispersing agent, a first pore-forming agent, a sodium chloride solution, silicone oil, a cross-linking agent, a sodium chloride solution and a sodium hydroxide solution with the mass fraction of 10-15%.
2. The modified solid carrier is prepared from kaolin, a second pore-forming agent, maleic anhydride grafted polyethylene wax and a hydrochloric acid solution with mass fraction of 15-20%, has good adhesiveness, is easier to be connected with other substances, and enables the structure of the adsorbent to be more stable.
3. The application prepares the adsorbent by adopting the hot-pressing film forming, so that the structure of the adsorbent is more stable, and meanwhile, the internal pore structure of the film can be kept from larger deformation, so that the prepared adsorbent has good permeability and absorptivity and the absorption capacity of the adsorbent can be increased.
Detailed Description
The following examples and comparative examples are provided to illustrate the present application in further detail, wherein the raw materials are commercially available, and wherein table 1 shows the source and model of some of the raw materials:
TABLE 1 sources and types of partial materials
Preparation example of modified solid Carrier
Preparation example 1
A modified solid support prepared by the method comprising:
weighing 300g of kaolin and 100g of hydrochloric acid solution with mass fraction of 15-20%, adding into a reaction kettle, carrying out reflux reaction at 50 ℃, stirring for 2h, filtering, washing with water, and drying to obtain carrier kaolin;
weighing 10g of sodium chloride, uniformly mixing with carrier kaolin, calcining at 850 ℃ for 4 hours, cooling to 20 ℃, and crushing to 50nm to obtain carrier kaolin powder;
and adding the carrier kaolin powder into a high-speed mixer at the rotating speed of 600r/min, weighing 20g of maleic anhydride grafted polyethylene wax, and uniformly mixing with the carrier kaolin powder to prepare the modified solid carrier.
Preparation example 2
A modified solid support prepared by the method comprising:
450g of kaolin and 125g of hydrochloric acid solution with mass fraction of 15-20% are weighed and added into a reaction kettle, and reflux reaction is carried out at 55 ℃, stirring is carried out for 2.5h, filtering, washing with water and drying are carried out, thus obtaining carrier kaolin;
weighing 15g of sodium sulfate, uniformly mixing with carrier kaolin, calcining at 880 ℃ for 4.5 hours, cooling to 25 ℃, and crushing to 55nm to obtain carrier kaolin powder;
and adding the carrier kaolin powder into a high-speed mixer at the rotating speed of 800r/min, weighing 40g of maleic anhydride grafted polyethylene wax, and uniformly mixing with the carrier kaolin powder to prepare the modified solid carrier.
Preparation example 3
A modified solid support prepared by the method comprising:
600g of kaolin and 150g of hydrochloric acid solution with mass fraction of 15-20% are weighed and added into a reaction kettle, and reflux reaction is carried out at 60 ℃, stirring is carried out for 3 hours, filtering, washing with water and drying are carried out, thus obtaining carrier kaolin;
weighing 50g of sodium phosphate, uniformly mixing with carrier kaolin, calcining at 900 ℃ for 5 hours, cooling to 30 ℃, and crushing to 60nm to obtain carrier kaolin powder;
and adding the carrier kaolin powder into a high-speed mixer at the rotating speed of 900r/min, weighing 50g of maleic anhydride grafted polyethylene wax, and uniformly mixing with the carrier kaolin powder to prepare the modified solid carrier.
Table 2 shows the amounts of materials used in preparation examples 1 to 3
Examples
Example 1
A salt lake lithium extraction adsorbent is prepared by the following method:
weigh 400g TiO 2 Adding into a reaction bottle, adding 100g of sulfuric acid solution with the mass fraction of 10% into the reaction bottle, heating to 80 ℃, and carrying out reflux reaction for 0.5h to obtain a titanium salt solution; and 200 to 200gLi 2 CO 3 Adding into titanic acid solution, dripping 150g of 15% sodium hydroxide solution, adjusting pH=8.0 to obtain solid precipitate, roasting the solid precipitate,
crushing, namely, putting the solid precipitate into eluent, washing away lithium ions, washing with water, and drying to obtain powder;
reacting 50g of methyl hydrogen-containing polysiloxane with 10g of dicumyl peroxide at the temperature of 100 ℃ to prepare an oily reactant; adding 50g of solid carrier into a reactor with a stirring and temperature controlling device, adding powder and uniformly mixing 50g of solid carrier,
preparing a composition;
2g of butanone, 50g of polyvinyl chloride, 1g of sodium tripolyphosphate and 100g of sodium chloride solution are weighed and uniformly stirred with the composition, the mixture is stirred uniformly at 80 ℃, the oily reactant is added to prepare a mixture, and the mixture is hot-pressed into a film to prepare the adsorbent.
Example 2
This embodiment differs from embodiment 1 in that: the procedure of example 1 was followed except that 50g of the solid support was replaced with the modified solid support obtained in preparation example 1.
The raw materials and amounts of examples 3 to 7 were partially different from those of example 1, as shown in Table 2:
TABLE 3 raw materials and materials for examples 1 to 7
Comparative example
Comparative example 1
This comparative example differs from example 4 in that: equal amounts of fibers were used in equal amounts of polytetrafluoroethylene bags, the remainder of the amounts and procedure being as in example 4.
Comparative example 2
This comparative example differs from example 4 in that: after the mixture is prepared, the mixture is granulated.
Table 4 examples and comparative examples sources in modified solid supports
| Examples | Source |
| Example 1 | Kaolin clay |
| Example 2 | Preparation example 1 |
| Example 3 | Preparation example 2 |
| Example 4 | Preparation example 3 |
| Example 5 | Preparation example 3 |
| Example 6 | Preparation example 2 |
Performance test
And detecting the adsorption quantity and the dissolution loss rate of the adsorbent.
Detection method/test method adsorption amount: 100g of each of the adsorbents prepared in examples 1 to 6 and comparative examples 1 to 2 was weighed and placed in a solution having a pH=10 and a lithium ion concentration of 180mg/L, and stirred at 40℃for 5 hours, and the concentration of lithium ions absorbed by the adsorbent was measured.
Wherein the adsorption capacity is calculated as follows:
adsorption capacity = lithium content in brine before adsorption-lithium content loss rate in brine after adsorption: 100g of each of the adsorbents prepared in examples 1 to 6 and comparative examples 1 to 2 was weighed and placed in a solution having a pH=10 and a lithium ion concentration of 180mg/L, and stirred at 40℃for 5 hours. Repeating the adsorption and desorption steps for 20 times, pouring out the adsorbent, vacuum drying, weighing, and calculating the dissolution loss rate.
Wherein the solution loss rate calculation formula is as follows:
percent dissolution loss = (initial adsorbent particle mass-mass of adsorbent particles after cycling)/initial adsorbent particle mass x 100%
The test results are shown in Table 4:
TABLE 5 Performance test data
| Lithium ion adsorption capacity (mg/L) | Loss on dissolution (%) | |
| Example 1 | 40 | ≤0.20 |
| Example 2 | 50 | ≤0.10 |
| Example 3 | 51 | ≤0.11 |
| Example 4 | 50 | ≤0.09 |
| Example 5 | 52 | ≤0.10 |
| Example 6 | 51 | ≤0.10 |
| Comparative example 1 | 30 | ≥0.4 |
| Comparative example 2 | 32 | ≥0.5 |
As can be seen from the combination of examples 1 to 6 and comparative examples 1 to 2 and table 5, the adsorption amount and adsorption rate of lithium ions in examples 1 to 6 are greater than those in comparative examples 1 to 2, indicating that the adsorbents prepared by the present application have large adsorption amount, high adsorption rate and good permeability; compared with examples 2-6, the adsorbent prepared by adopting the modified solid carrier has large absorption capacity and good absorption efficiency; example 4 shows that the adsorbent prepared by the preparation method of the present application has a large absorption capacity and good absorption efficiency, compared with comparative example 2.
As can be seen by combining examples 1-6 and comparative examples 1-2 and combining Table 5, the dissolution loss rate of examples 2-6 is less than 0.11, the dissolution loss rate of example 1 is less than 0.2, and the dissolution loss rate of comparative examples 1-2 is greater than 0.4, which indicates that the adsorbents prepared by the method have low dissolution loss rate and good use effect.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (1)
1. The salt lake lithium extraction adsorbent is characterized in that: the salt lake lithium extraction adsorbent is prepared from the following raw materials in parts by weight:
40-60 parts of titanium source
20-30 parts of lithium source
5-10 parts of swelling organic polymer
10-15 parts of strong acid solution with mass fraction of 10-15%
5-10 parts of solid carrier
0.1 to 0.3 part of dispersant
0.2-0.5 part of first pore-forming agent
5-10 parts of silicone oil
1-2 parts of cross-linking agent
5-8 parts of sodium chloride solution
15-20 parts of sodium hydroxide solution with the mass fraction of 10-15%;
the solid carrier is a modified solid carrier, and each part of the modified solid carrier is prepared from the following materials in parts by weight:
30-60 parts of kaolin
1-2 parts of a second pore-forming agent
2-5 parts of maleic anhydride grafted polyethylene wax
10-15 parts of 15-20% hydrochloric acid solution by mass fraction;
the modified solid carrier is prepared by the following steps:
1) According to parts by weight, firstly adding 30-60 parts of kaolin and 10-15 parts of hydrochloric acid solution with mass fraction of 15-20% into a reaction kettle, carrying out reflux reaction at 50-60 ℃, stirring for 2-3 hours, filtering, washing with water, and drying to obtain carrier kaolin;
2) Uniformly mixing 1-2 parts by weight of a second pore-forming agent and carrier kaolin, calcining at 850-900 ℃ for 4-5 hours, cooling to 20-30 ℃, and crushing to 50-60 nm to obtain carrier kaolin powder;
3) Adding carrier kaolin powder into a high-speed mixer, mixing 2-5 parts by weight of maleic anhydride grafted polyethylene wax uniformly at the rotating speed of 600-900r/min, and preparing a modified solid carrier;
the swelling organic copolymer is at least one of natural rubber, polypropylene, polystyrene, ethylene-vinyl acetate copolymer and polyvinyl chloride;
the first pore-forming agent is one of ethyl acetate, ethanol and butanone;
the dispersing agent is one of sodium dodecyl sulfate, sodium tripolyphosphate, sodium hexametaphosphate or sodium pyrophosphate;
the silicone oil is at least one of methyl hydrogen polysiloxane, tetraethoxysilane and methyltriethoxysilane;
the cross-linking agent is one of dicumyl peroxide, benzoyl peroxide or dicumyl hydroperoxide;
the preparation method of the salt lake lithium extraction adsorbent comprises the following steps:
adding 40-60 parts by weight of a titanium source into a reaction bottle, adding 10-15 parts by weight of a strong acid solution into a reaction kettle, heating to 80-90 ℃, and carrying out reflux reaction for 0.5-1 h to obtain a titanium salt solution; adding 20-30 parts of lithium source into the titanium salt solution, dropwise adding 5-8 parts of sodium hydroxide solution with the mass fraction of 10-15%, adjusting the pH value to be 8.0-9.0, preparing a solid precipitate, roasting the solid precipitate, crushing, adding the solid precipitate into an eluent, washing lithium ions, washing with water, and drying to obtain powder;
according to parts by weight, reacting 5-10 parts of silicone oil with 1-2 parts of cross-linking agent at the temperature of 100-120 ℃ to prepare an oily reactant;
adding 5-10 parts of modified solid carrier into a reactor with a stirring and temperature controlling device, adding powder and uniformly mixing the modified solid carrier to prepare a composition;
uniformly stirring 0.2-0.5 part by weight of a first pore-forming agent, 5-10 parts by weight of a swelling organic polymer, 0.1-0.3 part by weight of a dispersing agent and 5-8 parts by weight of sodium chloride solution with the composition, stirring at 80-100 ℃ until the dispersing agent is dissolved, adding the oily reactant to prepare a mixture, and hot-pressing the mixture into a film to prepare the adsorbent;
the hot pressing temperature in the hot pressing process is 100-120 ℃, and the hot pressing pressure is 120-160 MPa.
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