CN114807601A - Method for adsorbing rare earth element lanthanum by using phosphoric acid modified kaolin - Google Patents
Method for adsorbing rare earth element lanthanum by using phosphoric acid modified kaolin Download PDFInfo
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- CN114807601A CN114807601A CN202210572009.4A CN202210572009A CN114807601A CN 114807601 A CN114807601 A CN 114807601A CN 202210572009 A CN202210572009 A CN 202210572009A CN 114807601 A CN114807601 A CN 114807601A
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- phosphoric acid
- modified kaolin
- lanthanum
- acid modified
- rare earth
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 125
- -1 phosphoric acid modified kaolin Chemical class 0.000 title claims abstract description 124
- 229910052746 lanthanum Inorganic materials 0.000 title claims abstract description 119
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 112
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 77
- 239000007788 liquid Substances 0.000 claims abstract description 63
- 239000002994 raw material Substances 0.000 claims abstract description 55
- 238000001179 sorption measurement Methods 0.000 claims abstract description 55
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 13
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical class O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 34
- 229910019142 PO4 Inorganic materials 0.000 claims description 23
- 239000010452 phosphate Substances 0.000 claims description 23
- 239000005995 Aluminium silicate Substances 0.000 claims description 20
- 235000012211 aluminium silicate Nutrition 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000003795 desorption Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 239000003607 modifier Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 239000003929 acidic solution Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 6
- 238000000605 extraction Methods 0.000 description 16
- 239000003463 adsorbent Substances 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000009297 electrocoagulation Methods 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000002608 ionic liquid Substances 0.000 description 3
- 229910052747 lanthanoid Inorganic materials 0.000 description 3
- 150000002602 lanthanoids Chemical class 0.000 description 3
- 238000000622 liquid--liquid extraction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 239000006184 cosolvent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 description 1
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 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 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
-
- 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 & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Geology (AREA)
- Geochemistry & Mineralogy (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a method for adsorbing a rare earth element lanthanum by using phosphoric acid modified kaolin, which comprises the following steps: (1) mixing phosphoric acid modified kaolin and lanthanum-containing raw material liquid, then adsorbing in the stirring process, and then carrying out solid-liquid separation to obtain residual liquid and phosphoric acid modified kaolin loaded with rare earth lanthanum; (2) desorbing the rare earth lanthanum-loaded phosphoric acid modified kaolin obtained in the step (1) to obtain desorbed phosphoric acid modified kaolin; and (3) applying the desorbed phosphoric acid modified kaolin obtained in the step (2) to the adsorption in the step (1). The method for adsorbing the rare earth element lanthanum by using the phosphoric acid modified kaolin has the advantages of simple process, stable chemical property, environmental friendliness and the like, the adsorption efficiency of the phosphoric acid modified kaolin on the rare earth element lanthanum is high and can reach 99.9%, the phosphoric acid modified kaolin can be completely desorbed by using dilute hydrochloric acid, and the desorbed phosphoric acid modified kaolin can be recycled.
Description
Technical Field
The invention belongs to the technical field of solid-phase adsorption of rare earth, relates to a method for adsorbing a rare earth element by using modified kaolin, and particularly relates to a method for adsorbing a rare earth element lanthanum by using phosphoric acid modified kaolin.
Background
The rare earth element lanthanum is a typical metal element, is the first rare earth element of lanthanide series, and is widely applied to metallurgy, petroleum, glass, ceramics, agriculture and textile. At present, the extraction process of lanthanum in the industry mainly adopts a liquid-liquid extraction process, the core of the process is a naphthenic acid-kerosene system, and a lanthanum product with higher quality is finally obtained through multi-stage extraction. However, the process still has a plurality of defects, such as discharge of excessive acid-base waste liquid, toxic and heavy use of volatile organic solvent, and the like.
The exploitation of rare earth resources is accompanied with a great deal of environmental protection problems, so that the development of a new rare earth extraction technology with high efficiency, cleanness and low cost becomes the development direction of the rare earth extraction industry in the future.
CN 108893625A discloses a process for preparing high-purity lanthanum by an extraction method, which takes a 3N industrial-grade lanthanum chloride aqueous solution as a feed liquid and P204-TBP as a composite extractant, and specifically comprises five steps of fractional extraction separation of Na Mg Ca Pb Zn La/La Ce Pr Nd Sm Fe, fractional extraction separation of Na Mg Ca Pb Zn/La, fractional extraction separation of La/Ce Pr Nd Sm Fe, and a back extraction section 1 and a back extraction section 2. CN105506284A discloses a lanthanide extraction body, an extraction method and its application, wherein the extraction system comprises an organic phase and an aqueous phase, the organic phase comprises an ionic liquid, a cosolvent and an extractant: the aqueous phase comprises a lanthanide and nitric acid; wherein the cation of the ionic liquid is imidazole cation; the anion of the ionic liquid is [ NTf 2 ] - Or [ PF ] 6 ] - (ii) a The cosolvent is one or more of ethanol, benzene, dichloromethane, n-octanol, toluene or acetonitrile; the extraction agent is selected from R-BTP, R-BTBP, R-One or more of BTPhen, CA-BTP, CA-BTBP or CA-BTPhen, wherein the content of nitric acid in water phase is 0-3 mol 1.L -1 。
The liquid-liquid extraction process is adopted to extract and separate the metal lanthanum, compared with the liquid-liquid extraction process, the solid phase adsorption process is simple, the adsorption efficiency of the rare earth elements is higher, the use of organic solvents such as naphthenic acid, kerosene and toluene is avoided, the method is environment-friendly, the method has huge application potential in the extraction aspect of the rare earth elements, and the difficulty and the core of the method lie in the design and preparation of high-efficiency solid adsorbent materials.
Kaolin is a common clay mineral in the nature, is often used as a raw material for developing a solid phase adsorbent, has the advantages of low price, easy obtainment, strong adsorption performance, environmental friendliness and the like, and is widely used in the aspects of metal ion extraction, wastewater treatment and the like. CN 105126742a discloses a method for treating fluorine-containing wastewater by using a modified kaolin adsorbent, which comprises the following preparation processes: adding water into kaolin to prepare first ore pulp, adding sodium hexametaphosphate and sodium hydroxide, stirring in a water bath, and standing; taking the upper layer slurry for centrifugal separation, drying, immersing in a hydrophobic acid solution, and performing suction filtration; adding water to prepare a second ore pulp, adding polydimethyldiallyl ammonium chloride, stirring for reaction, filtering, drying, crushing and sieving to obtain the modified kaolin adsorbent; the method for treating the fluorine-containing wastewater by using the modified kaolin adsorbent comprises the following steps: s1, flocculating and settling: collecting fluorine-containing wastewater, naturally settling, sending into a sedimentation tank, adding a mixed solution of polymeric aluminum hydrophosphate and calcium hydroxide into the sedimentation tank, uniformly mixing, controlling the pH value in the sedimentation tank to be 7-9, standing, performing solid-liquid separation, introducing the liquid after the solid-liquid separation into a flocculation tank, adding a combined flocculant of PFC and PAM, uniformly mixing, and standing for sedimentation; s2, electrocoagulation: introducing the wastewater subjected to flocculation precipitation in the step S1 into an electrolytic bath, adding electrolyte, electrifying for electrocoagulation, standing, draining water into a water outlet pool, adding alkali to adjust the pH value to 9-11, adding activated carbon powder, and uniformly stirring; s3, adsorption: and (3) introducing the wastewater subjected to electrocoagulation treatment in S3 into an adsorption tank, adding acid to adjust the pH value to 4-6, adding the modified kaolin adsorbent, heating, stirring, standing and separating. The patent provides a modified kaolin applied to the field of wastewater treatment, but does not show the high-efficiency adsorption effect of kaolin on rare earth ions. Therefore, the application of the modified kaolin to the adsorption of rare earth ions requires further research.
In conclusion, the use of the cheap kaolin is accelerated and strengthened, and the development of the novel solid phase adsorbent for extracting the rare earth element lanthanum has great practical value.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for adsorbing rare earth element lanthanum by using phosphoric acid modified kaolin, wherein the phosphoric acid modified kaolin in the method has the advantages of simple process, stable chemical property, environmental friendliness and the like, the adsorption efficiency of the phosphoric acid modified kaolin on the rare earth element lanthanum is high and can reach 99.9%, the phosphoric acid modified kaolin can be completely desorbed by using dilute hydrochloric acid, and the desorbed phosphoric acid modified kaolin can be recycled.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for adsorbing a rare earth element lanthanum by using phosphoric acid modified kaolin, which comprises the following steps:
(1) mixing phosphoric acid modified kaolin and lanthanum-containing raw material liquid, then adsorbing in the stirring process, and then carrying out solid-liquid separation to obtain residual liquid and phosphoric acid modified kaolin loaded with rare earth lanthanum;
(2) desorbing the rare earth lanthanum-loaded phosphoric acid modified kaolin obtained in the step (1) to obtain desorbed phosphoric acid modified kaolin;
and (3) applying the desorbed phosphoric acid modified kaolin obtained in the step (2) to the adsorption in the step (1).
According to the method provided by the invention, the phosphoric acid modified kaolin is used for adsorbing the rare earth element lanthanum, the adsorption efficiency is high, and the phosphoric acid modified kaolin has the advantages of simple process, stable chemical property, environmental friendliness and the like, and can be desorbed and regenerated.
The method provided by the invention modifies the surface phosphate radical functional group (PO) of the kaolin powder by phosphoric acid 4 3- ) With lanthanum ion (La) 3+ ) The bonding effect between the La and the La in the solution is realized 3+ High-efficiency adsorption. Using a desorption solvent for PO 4 3- And (4) carrying out desorption and regeneration on the kaolin, wherein the regenerated phosphoric acid modified kaolin powder can be recycled.
Preferably, the solid-to-liquid ratio of the phosphoric acid modified kaolin to the lanthanum-containing raw material liquid in step (1) is (1.5-6) g:1L, and may be, for example, 1.5g:1L, 2g:1L, 2.5g:1L, 3g:1L, 3.5g:1L, 4g:1L, 4.5g:1L, 5g:1L, 5.5g:1L, or 6g:1L, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the stirring comprises magnetic stirring or shaking stirring.
Preferably, the stirring speed is 150-300r/min, such as 150r/min, 180r/min, 200r/min, 220r/min, 240r/min, 260r/min, 280r/min or 300r/min, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the adsorption time is 1 to 3 hours, for example 1 hour, 1.2 hours, 1.4 hours, 1.6 hours, 1.8 hours, 2 hours, 2.2 hours, 2.4 hours, 2.6 hours, 2.8 hours or 3 hours, but not limited to the recited values, and other values not recited in the numerical ranges are also applicable.
Preferably, the adsorption temperature is 25-35 ℃, for example, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃, 30 ℃, 31 ℃, 32 ℃, 33 ℃, 34 ℃ or 35 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the desorbent used in the desorption of step (2) comprises an acidic solution.
Preferably, the acidic solution comprises any one of or a combination of at least two of dilute hydrochloric acid, dilute sulfuric acid, or dilute nitric acid, typical but non-limiting combinations including a combination of dilute hydrochloric acid and dilute sulfuric acid, a combination of dilute hydrochloric acid and dilute nitric acid, a combination of dilute sulfuric acid and dilute nitric acid, or a combination of dilute hydrochloric acid, dilute sulfuric acid, and dilute nitric acid.
Preferably, the concentration of the acidic solution is 0.02 to 0.06mol/L, and may be, for example, 0.02mol/L, 0.025mol/L, 0.03mol/L, 0.035mol/L, 0.04mol/L, 0.045mol/L, 0.05mol/L, 0.055mol/L or 0.06mol/L, but not limited to the values listed, and other values not listed within the numerical range are equally applicable.
Preferably, (1) the concentration of the lanthanum-containing raw material solution is 10 to 100ppm, and may be, for example, 10ppm, 20ppm, 30ppm, 40ppm, 50ppm, 60ppm, 70ppm, 80ppm, 90ppm or 100ppm, but is not limited to the recited values, and other values not recited in the numerical ranges are also applicable.
Preferably, the lanthanum-containing raw material solution in step (1) has a pH of 4 to 7, which may be, for example, 4, 4.3, 4.6, 4.9, 5.2, 6.5, 5.8, 6.1, 6.4, 6.7 or 7, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the preparation method of the phosphoric acid modified kaolin in the step (1) is as follows:
mixing kaolin raw materials and a modifier, carrying out ball milling, and then sequentially washing and drying to obtain the phosphate modified kaolin.
The invention provides mechanical force through ball milling, and the phosphate radical is fixed on the surface of kaolin particles under the action of the mechanical force.
Preferably, the modifying agent comprises phosphoric acid.
The phosphoric acid is commercially available concentrated phosphoric acid, and the chemical molecular formula of the phosphoric acid is H 3 PO 4 。
The kaolin raw material is commercially available or prepared water-washed kaolin powder, and the chemical molecular formula of the kaolin raw material is Al 2 SiO 5 (OH) 4 。
Preferably, the mass ratio of the modifier to the kaolin clay raw material is 1 (5-20), and may be, for example, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, or 1:20, but is not limited to the recited values, and other values not recited within the numerical range are also applicable.
Preferably, the rotation speed of the ball mill is 350-400rpm, such as 350rpm, 360rpm, 370rpm, 380rpm, 390rpm or 400rpm, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the ball milling time is 10-120min, such as 10min, 30min, 50min, 70min, 90min, 110min or 120min, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the ball-to-feed ratio in the ball mill is (40-50):1, and may be, for example, 40:1, 41:1, 42:1, 43:1, 44:1, 45:1, 46:1, 47:1, 48:1, 49:1 or 50:1, but is not limited to the recited values, and other values not recited within the numerical range are equally applicable.
Preferably, the drying temperature is 20-30 ℃, for example, 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃ or 30 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the drying time is 6-8h, for example 6h, 6.2h, 6.4h, 6.6h, 6.8h, 7h, 7.2h, 7.4h, 7.6h, 7.8h or 8h, but not limited to the recited values, and other values not recited in the numerical ranges are equally applicable.
Preferably, the washing liquid used in the washing comprises water.
The invention uses water to wash to remove excess phosphoric acid.
As a preferred technical scheme, the method for adsorbing the rare earth element lanthanum by using the phosphate modified kaolin provided by the invention comprises the following steps:
(1) mixing phosphoric acid modified kaolin and lanthanum-containing raw material liquid with the concentration of 10-100ppm and the pH value of 4-7, then adsorbing for 1-3h in the stirring process at the rotating speed of 150-; the solid-liquid ratio of the phosphoric acid modified kaolin to the lanthanum-containing raw material liquid is (1.5-6) g: 1L;
(2) desorbing the rare earth lanthanum-loaded phosphoric acid modified kaolin obtained in the step (1) by using a desorption agent with the concentration of 0.02-0.06mol/L to obtain desorbed phosphoric acid modified kaolin;
the phosphate modified kaolin obtained in the step (2) after desorption is used for adsorption in the step (1);
the preparation method of the phosphoric acid modified kaolin in the step (1) is as follows:
mixing a modifier and a kaolin raw material according to a mass ratio of 1 (5-20), ball-milling at a rotation speed of 350-400rpm for 10-120min, then washing with water, and drying at 20-30 ℃ for 6-8h to obtain the phosphoric acid modified kaolin.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method for adsorbing the rare earth element lanthanum by using the phosphoric acid modified kaolin has the adsorption efficiency of the rare earth element lanthanum as high as 99.9 percent;
(2) according to the method for adsorbing the rare earth element lanthanum by using the phosphoric acid modified kaolin, the acid solution is used as the desorbent, so that the complete desorption of the rare earth lanthanum can be realized, the adsorption efficiency of the desorbed phosphoric acid modified kaolin on the rare earth lanthanum is basically kept unchanged, and the cyclic utilization of the phosphoric acid modified kaolin is realized;
(3) the method for adsorbing the rare earth element lanthanum by using the phosphoric acid modified kaolin has the advantages of high efficiency, low cost and environmental friendliness.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
In the specific embodiment of the invention, after the adsorption and desorption are completed, the content of the rare earth element lanthanum in the solution is measured by an ICP method.
The formula for calculating the adsorption efficiency of the rare earth element lanthanum is as follows:
wherein A represents adsorption efficiency, [ M ]] i Represents the concentration of lanthanum, a rare earth element, in a lanthanum-containing raw material solution, [ M ]] f The concentration of the rare earth element lanthanum in the raffinate is shown.
Example 1
The embodiment provides a method for adsorbing a rare earth element lanthanum by using phosphoric acid modified kaolin, which comprises the following steps:
(1) mixing 0.2g of phosphoric acid modified kaolin and 100mL of lanthanum-containing raw material liquid with the concentration of 30ppm and the pH value of 4.45, adsorbing for 2 hours at the water bath temperature of 25 ℃ in the stirring process at the rotating speed of 200r/min, and then carrying out solid-liquid separation to obtain residual liquid and phosphoric acid modified kaolin loaded with rare earth lanthanum;
(2) desorbing the rare earth lanthanum-loaded phosphoric acid modified kaolin obtained in the step (1) by using dilute hydrochloric acid with the concentration of 0.05mol/L to obtain desorbed phosphoric acid modified kaolin;
the phosphate modified kaolin obtained in the step (2) after desorption is used for adsorption in the step (1);
the preparation method of the phosphoric acid modified kaolin in the step (1) is as follows:
mixing 0.2g of phosphoric acid and 2g of kaolin raw material, ball-milling at the rotating speed of 350rpm for 120min, then washing with water, and drying at 25 ℃ for 7h to obtain the phosphoric acid modified kaolin.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 99.9%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 99.4%.
Example 2
The embodiment provides a method for adsorbing a rare earth element lanthanum by using phosphoric acid modified kaolin, which comprises the following steps:
(1) mixing 0.3g of phosphoric acid modified kaolin and 150mL of lanthanum-containing raw material liquid with the concentration of 60ppm and the pH value of 4.25, adsorbing for 3 hours in an oscillating and stirring process at the water bath temperature of 30 ℃ and the rotating speed of 200r/min, and then carrying out solid-liquid separation to obtain residual liquid and phosphoric acid modified kaolin loaded with rare earth lanthanum;
(2) desorbing the rare earth lanthanum-loaded phosphoric acid modified kaolin obtained in the step (1) by using dilute hydrochloric acid with the concentration of 0.04mol/L to obtain desorbed phosphoric acid modified kaolin;
the phosphate modified kaolin obtained in the step (2) after desorption is used for adsorption in the step (1);
the preparation method of the phosphoric acid modified kaolin in the step (1) is as follows:
mixing 0.3g of phosphoric acid and 3g of kaolin raw material, ball-milling for 90min at the rotating speed of 380rpm, washing with water, and drying at 25 ℃ for 8h to obtain the phosphoric acid modified kaolin.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 99.6%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 98.7%.
Example 3
The embodiment provides a method for adsorbing a rare earth element lanthanum by using phosphoric acid modified kaolin, which comprises the following steps:
(1) mixing 0.3g of phosphoric acid modified kaolin and 100mL of lanthanum-containing raw material liquid with the concentration of 70ppm and the pH value of 3.35, adsorbing for 3 hours in an oscillating and stirring process at the water bath temperature of 35 ℃ and the rotating speed of 200r/min, and then carrying out solid-liquid separation to obtain residual liquid and phosphoric acid modified kaolin loaded with rare earth lanthanum;
(2) desorbing the rare earth lanthanum-loaded phosphoric acid modified kaolin obtained in the step (1) by using dilute hydrochloric acid with the concentration of 0.02mol/L to obtain desorbed phosphoric acid modified kaolin;
the phosphate modified kaolin obtained in the step (2) after desorption is used for adsorption in the step (1);
the preparation method of the phosphoric acid modified kaolin in the step (1) is as follows:
mixing 0.25g of phosphoric acid and 2.5g of kaolin raw material, ball-milling at the rotating speed of 390rpm for 120min, then washing with water, and drying at 30 ℃ for 6h to obtain the phosphoric acid modified kaolin.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 98.9%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 98.3%.
Example 4
The embodiment provides a method for adsorbing a rare earth element lanthanum by using phosphoric acid modified kaolin, which comprises the following steps:
(1) mixing 0.6g of phosphoric acid modified kaolin and 300mL of lanthanum-containing raw material liquid with the concentration of 100ppm and the pH value of 4.00, adsorbing for 3 hours in an oscillating and stirring process at the water bath temperature of 28 ℃ and the rotating speed of 200r/min, and then carrying out solid-liquid separation to obtain residual liquid and phosphoric acid modified kaolin loaded with rare earth lanthanum;
(2) desorbing the rare earth lanthanum-loaded phosphoric acid modified kaolin obtained in the step (1) by using dilute hydrochloric acid with the concentration of 0.03mol/L to obtain desorbed phosphoric acid modified kaolin;
the phosphate modified kaolin obtained in the step (2) after desorption is used for adsorption in the step (1);
the preparation method of the phosphoric acid modified kaolin in the step (1) is as follows:
mixing 0.4g of phosphoric acid and 45g of kaolin raw material, ball-milling for 180min at the rotating speed of 400rpm, then washing with water, and drying at 30 ℃ for 6.5h to obtain the phosphoric acid modified kaolin.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 98.5%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 98.1%.
Example 5
This example provides a method for adsorbing lanthanum, a rare earth element, by using phosphate modified kaolin, which differs from example 1 only in that: in this example, the amount of the phosphoric acid-modified kaolin added in the step (1) was changed to 2 g.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 98.7%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 96.5%.
Example 6
This example provides a method for adsorbing lanthanum, a rare earth element, by using phosphate modified kaolin, which differs from example 1 only in that: in the embodiment, the concentration of the dilute hydrochloric acid in the step (2) is changed to 0.06 mol/L.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 99.9%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 98.4%.
Example 7
This example provides a method for adsorbing lanthanum, a rare earth element, by using phosphate modified kaolin, which differs from example 1 only in that: in the embodiment, the concentration of the dilute hydrochloric acid in the step (2) is changed to 0.1 mol/L.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 99.9%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 98.6%.
Example 8
This example provides a method for adsorbing lanthanum, a rare earth element, by using phosphate modified kaolin, which differs from example 1 only in that: in this example, the amount of phosphoric acid added in the process for producing phosphoric acid-modified kaolin was changed to 0.4 g.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 99.8%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 97.6%.
Example 9
This example provides a method for adsorbing lanthanum, a rare earth element, by using phosphate modified kaolin, which differs from example 1 only in that: in this example, the amount of phosphoric acid added in the process for producing phosphoric acid-modified kaolin was changed to 0.05 g.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 99.6%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 96.8%.
Example 10
This example provides a method for adsorbing lanthanum, a rare earth element, by using phosphate modified kaolin, which differs from example 1 only in that: in the embodiment, the rotating speed in the stirring in the step (1) is changed to 50 r/min.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 98.9%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 96.9%.
Example 11
This example provides a method for adsorbing lanthanum, a rare earth element, by using phosphate modified kaolin, which differs from example 1 only in that: in this example, the ball milling time in the preparation method of the phosphoric acid modified kaolin was changed to 10 min.
The method provided by the embodiment is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 99.5%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed phosphoric acid modified kaolin, wherein the adsorption rate is 98.3%.
Comparative example 1
This comparative example provides a method for adsorbing lanthanum, a rare earth element, by modified kaolin, which differs from example 1 only in that: this comparative example changed the phosphate modified kaolin to unmodified kaolin.
The method provided by the comparative example is adopted to adsorb the lanthanum-containing raw material liquid, and the adsorption rate of the rare earth element lanthanum is 4.2%;
and (3) adsorbing the lanthanum-containing raw material liquid in the step (1) again by using the desorbed unmodified kaolin, wherein the adsorption rate is 4.5%.
In conclusion, the method for adsorbing the rare earth element lanthanum by using the phosphoric acid modified kaolin provided by the invention has the advantages of simple process, stable chemical property, environmental friendliness and the like, the adsorption efficiency of the phosphoric acid modified kaolin on the rare earth element lanthanum is high and can reach 99.9%, the phosphoric acid modified kaolin can be completely desorbed by using dilute hydrochloric acid, and the desorbed phosphoric acid modified kaolin can be recycled.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for adsorbing a rare earth element lanthanum by using phosphoric acid modified kaolin is characterized by comprising the following steps:
(1) mixing phosphoric acid modified kaolin and lanthanum-containing raw material liquid, then adsorbing in the stirring process, and then carrying out solid-liquid separation to obtain residual liquid and phosphoric acid modified kaolin loaded with rare earth lanthanum;
(2) desorbing the rare earth lanthanum-loaded phosphoric acid modified kaolin obtained in the step (1) to obtain desorbed phosphoric acid modified kaolin;
and (3) applying the desorbed phosphoric acid modified kaolin obtained in the step (2) to the adsorption in the step (1).
2. The method for adsorbing lanthanum as claimed in claim 1, wherein the solid-to-liquid ratio of the phosphate-modified kaolin to the lanthanum-containing raw material liquid in step (1) is (1.5-6) g: 1L.
3. The method for adsorbing the rare earth element lanthanum by using the phosphoric acid modified kaolin as claimed in claim 1 or 2, wherein the stirring comprises magnetic stirring or shaking stirring;
preferably, the rotation speed of the stirring is 150-300 r/min;
preferably, the adsorption time is 1-3 h;
preferably, the temperature of the adsorption is 25-35 ℃.
4. The method for adsorbing lanthanum as a rare earth element by using phosphoric acid modified kaolin according to any one of claims 1 to 3, wherein the desorbent used in the desorption of the step (2) comprises an acidic solution;
preferably, the acidic solution comprises any one of or a combination of at least two of dilute hydrochloric acid, dilute sulfuric acid, or dilute nitric acid;
preferably, the concentration of the acidic solution is 0.02-0.06 mol/L.
5. The method for adsorbing lanthanum as a rare earth element by using phosphoric acid modified kaolin according to any one of claims 1 to 4, wherein the concentration of the lanthanum-containing raw material solution in the step (1) is 10 to 100 ppm;
preferably, the lanthanum-containing raw material liquid in the step (1) has a pH value of 4 to 7.
6. The method for adsorbing lanthanum as a rare earth element by using phosphate modified kaolin according to any one of claims 1 to 5, wherein the preparation method of the phosphate modified kaolin in the step (1) is as follows:
mixing kaolin raw materials and a modifier, carrying out ball milling, and then sequentially washing and drying to obtain the phosphate modified kaolin.
7. The method of claim 6, wherein the modifier comprises phosphoric acid;
preferably, the mass ratio of the modifier to the kaolin raw material is 1 (5-20).
8. The method as claimed in claim 6 or 7, wherein the ball milling speed is 350-400 rpm;
preferably, the ball milling time is 10-120 min;
preferably, the ball-to-material ratio in the ball mill is (40-50): 1.
9. The method for adsorbing lanthanum as a rare earth element by using phosphoric acid modified kaolin according to any one of claims 6 to 8, wherein the drying temperature is 20 to 30 ℃;
preferably, the drying time is 6-8 h;
preferably, the washing liquid used in the washing comprises water.
10. The method for adsorbing lanthanum, which is a rare earth element, by using phosphoric acid modified kaolin according to any one of claims 1 to 9, characterized in that it comprises the following steps:
(1) mixing phosphoric acid modified kaolin and lanthanum-containing raw material liquid with the concentration of 10-100ppm and the pH value of 4-7, then adsorbing for 1-3h in the stirring process at the rotating speed of 150-; the solid-liquid ratio of the phosphoric acid modified kaolin to the lanthanum-containing raw material liquid is (1.5-6) g: 1L;
(2) desorbing the phosphate modified kaolin loaded with the rare earth lanthanum obtained in the step (1) by using a desorption agent with the concentration of 0.02-0.06mol/L to obtain desorbed phosphate modified kaolin;
the phosphate modified kaolin obtained in the step (2) after desorption is used for adsorption in the step (1);
the preparation method of the phosphoric acid modified kaolin in the step (1) is as follows:
mixing a modifier and a kaolin raw material according to a mass ratio of 1 (5-20), ball-milling at a rotation speed of 350-400rpm for 10-120min, then washing with water, and drying at 20-30 ℃ for 6-8h to obtain the phosphoric acid modified kaolin.
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