CN113249596B - Method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass material - Google Patents
Method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass material Download PDFInfo
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- CN113249596B CN113249596B CN202110518723.0A CN202110518723A CN113249596B CN 113249596 B CN113249596 B CN 113249596B CN 202110518723 A CN202110518723 A CN 202110518723A CN 113249596 B CN113249596 B CN 113249596B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/22—Electrolytic production, recovery or refining of metals by electrolysis of solutions of metals not provided for in groups C25C1/02 - C25C1/20
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass materials, which comprises the following steps: the biomass material is taken as an adsorbent, and is a persimmon peel base imprinting composite material obtained by modifying persimmon peels by an ion imprinting technology; and (3) loading the persimmon peel-based imprinting composite material into a two-stage dynamic adsorption column, and selectively adsorbing and desorbing gallium in the alumina seed precipitation mother liquor through a gallium extraction dynamic adsorption column 1 and a gallium enrichment dynamic adsorption column 2 respectively to obtain a gallium-rich electrolytic stock solution. According to the method, the persimmon peel of waste biomass is taken as a material, the adsorbent is obtained by surface ion imprinting modification, selective extraction of gallium in the alumina seed precipitation mother liquor is realized through gallium ion specific recognition sites on the surface of the adsorbent, and the method has the advantages of low gallium enrichment cost, high efficiency and the like, and has good economic benefits and environmental benefits.
Description
Technical Field
The invention relates to a gallium extraction and enrichment method, in particular to a method for enriching and extracting gallium from alumina seed precipitation mother liquor based on a biomass material.
Background
Gallium is an important rare metal and has become an important supporting material for new technology development in the fields of national defense, aerospace, medical industry, communication electronics and the like. The content of gallium is low, the distribution is relatively dispersed, and the gallium exists in the form of associated ores together with other metal elements. Due to the trace accompanying relation, the enrichment and extraction level of gallium resources is low, the yield of gallium cannot be improved, and serious shortage will occur within 20-30 years in the future. In the enrichment extraction of gallium, about 90% of the primary gallium is extracted from the alumina production process. The content of gallium in the alumina seed precipitation mother liquor is only 150-250mg/L, while the content of aluminum is 100 times of that of gallium, and the low concentration of gallium in the alumina seed precipitation mother liquor makes the efficient enrichment of gallium difficult.
The resin adsorption method is a gallium enrichment method which is commonly used at home and abroad at present, and the enrichment and extraction of gallium are realized through the customization of specific chelating groups on resin. However, in a complex mixed system, coexisting ions of aluminum and gallium are elements of the same main group, the properties are similar, the selective adsorption efficiency of gallium is influenced by the complex coordination of chelating groups on the surface of the resin and high-concentration aluminum, and meanwhile, the high concentration causes Al (OH)3The crystal precipitation and the blockage of the adsorption layer cause the poor cycle performance of the resin, so that the enrichment and extraction cost of the gallium is increased. The low selectivity-high cost of the extraction process of gallium in the alumina seed precipitation mother liquor becomes a main technical bottleneck restricting the enrichment and extraction of the aluminum oxide seed precipitation mother liquor. Persimmon peel is a biomass waste produced in the production of dried persimmons and dried persimmons, which contains abundant persimmon tannin and mainly contains complex polyphenol substances of catechol and pyrogallol groups. The persimmon tannin can perform ion exchange or complexation reaction with metal ions, thereby realizing the selective recovery of specific metal ions from the solution.
Disclosure of Invention
The invention aims to provide a method for enriching and extracting gallium from alumina seed precipitation mother liquor based on a biomass material, and aims to solve the problems of high cost and poor adsorption selectivity in the gallium extraction process.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass materials is provided, wherein the biomass materials are persimmon peel-based imprinted composite materials obtained by persimmon peel modification through an ion imprinting technology; loading the obtained persimmon peel-based imprinted composite material into a two-stage dynamic adsorption column, and selectively adsorbing and desorbing gallium in the alumina seed precipitation mother liquor through a gallium extraction dynamic adsorption column 1 and a gallium enrichment dynamic adsorption column 2 respectively to obtain a gallium-rich electrolytic stock solution.
Further, the preparation process of the biomass material comprises the following steps: firstly, dry persimmon peel with the granularity of less than 74 mu m and GaCl with the concentration of 0.01-0.05mol/L3Mixing the solution, and uniformly stirring at room temperature for 2-4h to ensure that Ga in the solution is3+Completely chelating persimmon tannin on the surface of the persimmon peel; adding a cross-linking agent glutaraldehyde into the mixed solution, stirring for 12-36h in a water bath at 50-70 ℃ to perform aldol condensation reaction of the residual hydroxyl and aldehyde group; washing the obtained product with deionized water, soaking with acid, and drying to obtain the biomass material.
Further, the step of selective adsorption and desorption of gallium by the adsorption column comprises:
(1) loading the persimmon peel-based imprinting composite material into a gallium extraction dynamic adsorption column 1 and a gallium enrichment dynamic adsorption column 2 respectively, enabling aluminum oxide seed precipitation mother liquor containing gallium to flow through the gallium extraction dynamic adsorption column 1, and stopping adsorption when the concentration of gallium at the outlet of the gallium extraction dynamic adsorption column 1 is basically the same as the concentration of gallium in the aluminum oxide mother liquor, namely the gallium extraction dynamic adsorption column 1 reaches adsorption saturation;
(2) enabling a pre-prepared acid solution to flow through the gallium extraction dynamic adsorption column 1 in the step (1) in a forward direction by using a pump, stopping elution when the gallium content in an effluent liquid of the gallium extraction dynamic adsorption column 1 is less than 10mg/L, washing with water until the pH value of an outlet is 5-7, and performing repeated adsorption operation to obtain an acidic desorption liquid;
(3) adjusting the acid concentration of the acidic desorption solution obtained in the step (2) to 3-7mol/L by using hydrochloric acid, enabling the acidic desorption solution to flow through the gallium-enriched dynamic adsorption column 2, and stopping adsorption when the gallium concentrations at the inlet and the outlet of the gallium-enriched dynamic adsorption column 2 are the same;
(4) preparing a hydrochloric acid-thiourea mixed solution with a certain concentration, reversely entering a gallium enrichment dynamic adsorption column 2 at a certain temperature and a certain flow rate for desorption, and taking the gallium concentration in an effluent liquid less than 50mg/L as a desorption end point to obtain a gallium-rich electrolytic stock solution; after the desorption is finished, the resin is washed by water until the pH value of the effluent liquid is 5-7;
(5) and neutralizing and electrolyzing the gallium-rich electrolytic stock solution to obtain the gallium metal.
Preferably, in the step (1), the operating temperature is 35-55 ℃ when the gallium extraction dynamic adsorption column 1 adsorbs gallium from the alumina seed precipitation mother liquor.
Preferably, in the step (2), the acid solution is one of hydrochloric acid, sulfuric acid, nitric acid and acetic acid, and the concentration of the acid solution is 1 mol/L.
Preferably, in the step (3), the acid concentration in the acidic desorption solution is 6mol/L, and the adsorption effect is optimal.
Preferably, in the step (4), the molar ratio of the hydrochloric acid to the thiourea in the hydrochloric acid-thiourea mixed solution is 50: 1.
more preferably, the concentration of hydrochloric acid in the hydrochloric acid-thiourea mixed solution is 0.5-3 mol/L.
Preferably, in the step (4), the temperature of the desorption gallium enrichment dynamic adsorption column 2 is 35-60 ℃.
Preferably, in the step (1), the flow rate of the alumina seed precipitation mother liquor containing gallium flowing through the gallium extraction dynamic adsorption column 1 is 5-15 BV/h; in the step (3), the flow rate of the acid desorption solution flowing through the gallium enrichment dynamic adsorption column 2 is 5-15 BV/h.
The invention provides a low-cost biomass adsorbing material which is designed by taking waste biomass persimmon peels as a material and modifying through ion imprinting; and the biomass adsorption material is used as an adsorbent, and the high-efficiency enrichment of low-concentration gallium in the alumina seed precipitation mother liquor is realized through the secondary adsorption and desorption acid concentration adjustment of the dynamic extraction adsorption column 1 and the dynamic enrichment adsorption column 2. Within the research range of the invention, the maximum concentration of gallium in the gallium-rich solution obtained by the method can reach 6244 mg/L.
Compared with the prior art, the invention has the following beneficial effects:
1. the method adopts waste biomass persimmon peels as raw materials, obtains the adsorbent through surface ion imprinting modification, and realizes selective extraction of gallium in the alumina seed precipitation mother liquor through gallium ion specific recognition sites on the surface of the adsorbent.
2. The method adopts two sections of dynamic adsorption columns to selectively extract gallium in the alumina mother liquor, and realizes the high-efficiency enrichment of gallium by regulating and controlling the acid concentration of the desorption liquor.
3. The method has the advantages of simple operation, low cost and obvious extraction and enrichment effects, realizes the value-added utilization of the biomass, is easy for large-scale industrial application, and has good economic and environmental benefits.
Drawings
FIG. 1 is a flow chart of the present invention.
FIG. 2 is an SEM image of the biomass material before pickling in example 1 of the present invention.
FIG. 3 is an EDX spectrum of the biomass material before acid washing in example 1 of the present invention.
FIG. 4(a) shows the adsorption efficiency of the biomass material to the metal ions in the alumina seed precipitation mother liquor in example 2 of the present invention.
FIG. 4(b) shows the desorption efficiency of each metal ion of the biomass material in example 2 of the present invention.
Fig. 5(a) is an absorption penetration curve of the gallium-rich dynamic adsorption column 2 on each metal ion in the desorption solution of the adsorption column 1 in example 3 of the present invention.
FIG. 5(b) is a graph showing the desorption breakthrough curves of the metal ions on the gallium-rich dynamic adsorption column 2 in example 3 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Example 1: production of biomass material
(1) Adopts surface imprinting technology, uses persimmon tannin on the surface of persimmon peel as a functional monomer, Ga3+Coating persimmon tannin cross-linked polymer on the surface of persimmon peel under the action of a cross-linking agent glutaraldehyde as a template: collecting 0.4g dried persimmon peel with particle size less than 74 μm, and adding 30mL GaCl with concentration of 0.05mol/L3The solution was stirred for 2h, then 2mL of the crosslinker glutaraldehyde was added and stirred for 24h in a water bath at 55 ℃.
(2) Washing the product obtained in the step (1) by deionized water, and soaking the product in 1mol/L HCl solution for 2 hours until Ga can not be detected in the soaking solution3+And washing with deionized water, and drying to obtain the persimmon peel imprinted composite material.
FIG. 2 is an SEM image of a persimmon peel imprinted composite material before pickling; FIG. 3 is an EDX chart of the imprinted composite material of persimmon peel before acid washing. From fig. 2 and 3, it can be seen that the biomass adsorbing material has been successfully constructed.
Example 2: dynamic adsorption performance of biomass material on gallium in alumina seed precipitation mother liquor
The implementation steps are shown in fig. 1.
(1) Loading the biomass material obtained in the example 1 into a dynamic glass adsorption column with the column length of 300mm and the inner diameter of 10mm to obtain a gallium extraction dynamic adsorption column 1, enabling an alumina seed precipitation mother liquor with the gallium concentration of 187mg/L to flow through the gallium extraction dynamic adsorption column 1 at the temperature of 40 ℃ at the speed of 10BV/h, and stopping adsorption after 13.3h when the outlet gallium concentration of the gallium extraction dynamic adsorption column 1 is basically the same as the gallium concentration in the alumina seed precipitation mother liquor;
(2) and (3) allowing the HCl solution with the concentration of 1mol/L to flow through the gallium extraction dynamic adsorption column 1 in the step (1) in a forward direction by using a pump, stopping elution when the gallium content in an effluent liquid of the gallium extraction dynamic adsorption column 1 is less than 10mg/L, and washing with water until the pH value of an outlet is 6.
(3) ICP-MS is respectively adopted to measure the concentration of each metal ion in the alumina seed precipitation mother liquor and the desorption liquor, and the absorption and desorption efficiencies of the gallium extraction dynamic adsorption column 1 to gallium and interference ions are shown in a figure 4(a) and a figure 4(b), wherein the absorption and desorption efficiencies of gallium are respectively 56% and 100%.
Example 3: adsorption performance of biomass material on desorption liquid of gallium extraction dynamic adsorption column 1
The implementation steps are shown in fig. 1.
(1) Loading the biomass material obtained in the example 1 into a dynamic glass adsorption column with the column length of 300mm and the inner diameter of 10mm to obtain a gallium enrichment dynamic adsorption column 2, adjusting the acid concentration in the acidic desorption solution obtained in the example 2 to 6mol/L by using concentrated hydrochloric acid, flowing through the gallium enrichment dynamic adsorption column 2 at the rate of 10BV/h, and stopping adsorption when the gallium concentrations at the inlet and the outlet of the gallium enrichment dynamic adsorption column 2 are the same;
(2) adopting hydrochloric acid-thiourea desorption solution with the hydrochloric acid concentration of 1.5mol/L (the molar ratio of the hydrochloric acid to the thiourea is 50: 1), reversely flowing into a gallium enrichment dynamic adsorption column 2 at 40 ℃ for desorption, and taking the gallium concentration in effluent liquid less than 50mg/L as a desorption end point to obtain gallium-rich electrolytic stock solution; after the desorption is finished, the resin is washed by water until the pH of the effluent liquid is 5;
(4) and directly neutralizing and electrolyzing the gallium-rich electrolytic stock solution to obtain the gallium metal.
Fig. 5(a) and 5(b) are absorption penetration curves and desorption elution penetration curves of the biomass material for gallium, respectively, and it can be seen that when the hydrochloric acid concentration is 6mol/L, the biomass material has a good selective absorption effect on gallium, no absorption occurs to coexisting ions of aluminum, vanadium and iron, gallium is easily desorbed in a hydrochloric acid-thiourea system, and the concentration after desorption can reach 6244 mg/L.
Example 4: adsorption performance of biomass material to desorption liquid of adsorption column 1
The adsorption step of the desorption solution of the adsorption column 1 in this example is substantially the same as that of example 3, except that the acid concentration of the acidic desorption solution is 5 mol/L.
The concentration of gallium in the desorption solution obtained in the embodiment was 5918 mg/L.
Example 5: adsorption performance of biomass material to desorption liquid of adsorption column 1
The adsorption step of the desorption solution of the adsorption column 1 in this example is substantially the same as that of example 3, except that the acid concentration of the acidic desorption solution is 4 mol/L.
The concentration of gallium in the desorption solution obtained in this example was 5247 mg/L.
Example 6: adsorption performance of biomass material to desorption liquid of adsorption column 1
The adsorption step of the desorption solution of the adsorption column 1 in this example is substantially the same as that of example 3, except that the acid concentration in the acidic desorption solution is 3 mol/L.
The concentration of gallium in the desorption solution obtained in this example was 4715 mg/L.
Example 7: adsorption performance of biomass material to desorption liquid of adsorption column 1
The adsorption step of the desorption solution of the adsorption column 1 in this example is substantially the same as that of example 3, except that the acid concentration in the acidic desorption solution is 7 mol/L.
The concentration of gallium in the desorption solution obtained in the embodiment is 6127 mg/L.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (9)
1. A method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass materials is characterized in that the biomass materials are persimmon peel-based imprinted composite materials obtained by persimmon peel modification through an ion imprinting technology; loading the persimmon peel-based imprinting composite material into a two-stage dynamic adsorption column, and respectively performing selective adsorption and desorption on gallium in the alumina seed precipitation mother liquor by a gallium extraction dynamic adsorption column 1 and a gallium enrichment dynamic adsorption column 2 to obtain gallium-rich electrolytic stock solution;
wherein the selective adsorption and desorption of gallium by the adsorption column comprises the following steps:
(1) loading the persimmon peel-based imprinting composite material into a gallium extraction dynamic adsorption column 1 and a gallium enrichment dynamic adsorption column 2 respectively, enabling aluminum oxide seed precipitation mother liquor containing gallium to flow through the gallium extraction dynamic adsorption column 1, and stopping adsorption when the concentration of gallium at the outlet of the gallium extraction dynamic adsorption column 1 is the same as the concentration of gallium in the aluminum oxide mother liquor, namely the gallium extraction dynamic adsorption column 1 reaches adsorption saturation;
(2) enabling a pre-prepared acid solution to flow through the gallium extraction dynamic adsorption column 1 in the step (1) in a forward direction by using a pump, stopping elution when the gallium content in an effluent liquid of the gallium extraction dynamic adsorption column 1 is less than 10mg/L, washing with water until the pH value of an outlet is 5-7, and performing repeated adsorption operation to obtain an acidic desorption liquid;
(3) adjusting the acid concentration of the acidic desorption solution obtained in the step (2) to 3-7mol/L by using hydrochloric acid, enabling the acidic desorption solution to flow through the gallium-enriched dynamic adsorption column 2, and stopping adsorption when the gallium concentrations at the inlet and the outlet of the gallium-enriched dynamic adsorption column 2 are the same;
(4) preparing a hydrochloric acid-thiourea mixed solution with a certain concentration, reversely entering a gallium enrichment dynamic adsorption column 2 at a certain temperature and a certain flow rate for desorption, and taking the gallium concentration in an effluent liquid less than 50mg/L as a desorption end point to obtain a gallium-rich electrolytic stock solution; after the desorption is finished, the resin is washed by water until the pH value of the effluent liquid is 5-7;
(5) and neutralizing and electrolyzing the gallium-rich electrolytic stock solution to obtain the gallium metal.
2. The method for enriching and extracting gallium from alumina seed precipitation solution based on biomass material as claimed in claim 1, wherein the preparation process of the biomass material is as follows: firstly, dry persimmon peel with the granularity of less than 74 mu m and GaCl with the concentration of 0.01-0.05mol/L3Mixing the solution, and uniformly stirring at room temperature for 2-4h to ensure that Ga in the solution is3+Completely chelating persimmon tannin on the surface of the persimmon peel; adding a cross-linking agent glutaraldehyde into the mixed solution, stirring for 12-36h in a water bath at 50-70 ℃ to perform aldol condensation reaction of the residual hydroxyl and aldehyde group; washing the obtained product with deionized water, soaking with acid, and drying to obtain the biomass material.
3. The method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass material as claimed in claim 1, wherein in the step (1), the operating temperature of the gallium extraction dynamic adsorption column 1 for adsorbing gallium from alumina seed precipitation mother liquor is 35-55 ℃.
4. The method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass material as claimed in claim 1, wherein in step (2), the acid solution is one of hydrochloric acid, sulfuric acid, nitric acid and acetic acid, and the concentration of the acid solution is 1 mol/L.
5. The method for enriching and extracting gallium from alumina seed pregnant solution based on biomass material as claimed in claim 1, wherein in step (3), the acid concentration in the acidic desorption solution is 6 mol/L.
6. The method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass material as claimed in claim 1, wherein in the step (4), the molar ratio of hydrochloric acid to thiourea in the hydrochloric acid-thiourea mixed solution is 50: 1.
7. the method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass material as claimed in claim 6, wherein the concentration of hydrochloric acid in the hydrochloric acid-thiourea mixed solution is 0.5-3 mol/L.
8. The method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass material as claimed in claim 1, wherein in the step (4), the temperature of the desorption gallium enrichment dynamic adsorption column 2 is 35-60 ℃.
9. The method for enriching and extracting gallium from alumina seed precipitation mother liquor based on biomass material as claimed in claim 1, wherein in step (1), the flow rate of the alumina seed precipitation mother liquor containing gallium flowing through the gallium extraction dynamic adsorption column 1 is 5-15 BV/h; in the step (3), the flow rate of the acid desorption liquid flowing through the gallium enrichment dynamic adsorption column 2 is 5-15 BV/h.
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| CN102321802A (en) * | 2011-08-25 | 2012-01-18 | 西安蓝晓科技有限公司 | New method for extracting gallium from Bayer mother liquor through chelating resin |
| CN103382531A (en) * | 2012-05-04 | 2013-11-06 | 中国科学院过程工程研究所 | Method for enriching gallium from mother-liquor in technology for producing alumina from high-alumina fly ash |
| CN105289519A (en) * | 2015-10-19 | 2016-02-03 | 辽宁大学 | Persimmon tannin adsorbent and preparing method and application thereof |
| CN112452302A (en) * | 2020-11-06 | 2021-03-09 | 辽宁大学 | Three-dimensional gallium imprinted Chinese gall tannin silicon-based composite material and application thereof in gallium recovery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321802A (en) * | 2011-08-25 | 2012-01-18 | 西安蓝晓科技有限公司 | New method for extracting gallium from Bayer mother liquor through chelating resin |
| CN103382531A (en) * | 2012-05-04 | 2013-11-06 | 中国科学院过程工程研究所 | Method for enriching gallium from mother-liquor in technology for producing alumina from high-alumina fly ash |
| CN105289519A (en) * | 2015-10-19 | 2016-02-03 | 辽宁大学 | Persimmon tannin adsorbent and preparing method and application thereof |
| CN112452302A (en) * | 2020-11-06 | 2021-03-09 | 辽宁大学 | Three-dimensional gallium imprinted Chinese gall tannin silicon-based composite material and application thereof in gallium recovery |
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