CN111001392A - Preparation method and application of modified zirconium-based metal organic framework adsorbent for gold ion adsorption - Google Patents
Preparation method and application of modified zirconium-based metal organic framework adsorbent for gold ion adsorption Download PDFInfo
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- 239000010931 gold Substances 0.000 title claims abstract description 52
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 52
- 239000003463 adsorbent Substances 0.000 title claims abstract description 37
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 31
- 239000013096 zirconium-based metal-organic framework Substances 0.000 title claims abstract description 24
- 150000003754 zirconium Chemical class 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 75
- -1 gold ion Chemical class 0.000 claims abstract description 42
- 239000013207 UiO-66 Substances 0.000 claims abstract description 31
- 239000000243 solution Substances 0.000 claims abstract description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- GPNNOCMCNFXRAO-UHFFFAOYSA-N 2-aminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC=C1C(O)=O GPNNOCMCNFXRAO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000010992 reflux Methods 0.000 claims abstract description 16
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000011084 recovery Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims description 33
- 238000000926 separation method Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- 238000001291 vacuum drying Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 5
- 230000000274 adsorptive effect Effects 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical group [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 9
- 239000012621 metal-organic framework Substances 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000010793 electronic waste Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 231100000915 pathological change Toxicity 0.000 description 1
- 230000036285 pathological change Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
-
- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a modified zirconium-based metal organic framework adsorbent for gold ion adsorption and a preparation method and application thereof, belonging to the technical field of adsorbent preparation. Namely zirconium tetrachloride, 2-amino terephthalic acid and hydrochloric acid inN,NAnd (4) refluxing and reacting in a dimethylformamide solution to obtain Amino-UiO-66. And then carrying out reflux reaction on the 2-Amino-5-aldehyde thiazole and Amino-UiO-66 under a certain condition to obtain the adsorbent AF-UiO-66. The preparation method of the adsorbent is simple and feasible, the operation is simple, and the reagent is cheap and easy to obtain. The obtained novel modified metal organic framework adsorbent has excellent stability, can be applied to high-efficiency and selective adsorption of gold ions in aqueous solution, and can be repeatedly used. The invention relates to the recovery of secondary gold-containing resourcesProvides a green and efficient adsorbent, and simultaneously brings a new idea for the design and synthesis of a novel adsorbent.
Description
Technical Field
The invention relates to a modified zirconium-based metal organic framework adsorbent for gold ion adsorption, and a preparation method and application thereof, and belongs to the technical field of adsorbent preparation.
Background
As a noble metal, gold has been popular with various industries since ancient times. Along with the development of society, gold is increasingly becoming an indispensable material. Meanwhile, gold is widely applied to industries such as electronic and electric appliances, chemical and chemical industries, medical treatment, financial securities and the like due to unique physical and chemical properties of gold. However, gold production is far below social demand. With the progress of smelting technology, the recovery and utilization of gold from various secondary resources, such as tailings, electronic wastes, leaching residues and the like, attract wide attention. Meanwhile, the presence of gold ions in the waste can cause environmental pollution, enter organisms, pose a threat to health and cause pathological changes. Therefore, the efficient selective recovery of gold ions not only meets the social requirements, but also meets the environmental requirements. At present, the main gold recovery methods include a biological enrichment method, an electrochemical method, an ion exchange method, a membrane filtration method, a solvent extraction method, an adsorption method and the like. In contrast, the adsorption method is considered to be one of the most effective methods due to the advantages of simple operation, good selectivity, no secondary pollution and the like. The common adsorbent comprises resin, natural minerals, metal organic framework, nano silicon dioxide, biochar and the like. In contrast, Metal Organic Frameworks (MOFs) are one of the most promising adsorbent materials to choose from due to their advantages of ultra-high specific surface area, simple operation, diverse structures, tunable functional groups, and long-lasting porosity. However, unmodified MOFs are less selective and less efficient in adsorption.
Disclosure of Invention
Aiming at the problems and the defects of the prior art, the invention provides a preparation method and application of a modified zirconium-based metal organic framework adsorbent for gold ion adsorption. The modified zirconium-based metal organic framework adsorbent can be used for selectively recovering gold ions in an aqueous solution, and has the advantages of low cost of used reagents, simple and easy synthesis process, easy separation from the aqueous solution, high adsorption capacity and high selectivity, and repeated use.
The invention is realized by the following technical scheme.
A modified zirconium-based metal organic framework adsorbent for gold ion adsorption has a structural formula as follows:
The invention also aims to provide a preparation method of the modified zirconium-based metal organic framework adsorbent for gold ion adsorption, which comprises the following specific steps:
(1) sequentially adding 2-aminoterephthalic acid and zirconium tetrachloride into an N, N-dimethylformamide solution, dropwise adding a certain amount of hydrochloric acid, carrying out reflux reaction in a round bottom three-necked bottle, carrying out liquid-solid separation, washing the obtained solid with the N, N-dimethylformamide solution, centrifuging, and carrying out vacuum drying to obtain the Amino-UiO-66. The synthetic route is as follows:
(2) and (2) sequentially adding the product Amino-UiO-66 and 2-Amino-5-aldehyde thiazole obtained in the step (1) into an N, N-dimethylformamide solution for reflux reaction, performing liquid-solid separation, washing the obtained solid with the N, N-dimethylformamide solution, centrifuging, and performing vacuum drying to obtain the AF-UiO-66. The synthetic route is as follows:
preferably, in the above production method: in the step (1), the solid-to-liquid ratio of the 2-aminoterephthalic acid to the N, N-dimethylformamide is 1: 30-1: 50g/mL, the liquid-to-solid ratio of the hydrochloric acid to the 2-aminoterephthalic acid is 1: 1-1: 10mL/g, and the mass ratio of the 2-aminoterephthalic acid to the zirconium tetrachloride is 1: 1-1.2: 1.
Preferably, in the above production method: in the step (2), the liquid-solid ratio of the N, N-dimethylformamide to the Amino-UiO-66 is 30: 1-50: 1mL/g, and the mass ratio of the Amino-UiO-66 to the 2-Amino-5-aldehyde thiazole is 1: 1-1: 1.2.
Preferably, in the above production method: the reflux in the step (1) is carried out for 12-24 h at the temperature of 110-130 ℃. And (3) the reflux in the step (2) is carried out for 12-24 hours at the temperature of 50-70 ℃.
The modified zirconium-based metal organic framework adsorbent is applied to selective adsorption of gold ions in a solution.
The organic and inorganic reagents were commercially available analytical grade.
Compared with the prior art, the invention has the following beneficial effects:
(1) the modified zirconium-based metal organic framework adsorbent for gold ion adsorption has good selectivity and reusability for gold ion adsorption, and has high adsorption capacity and recovery rate.
(2) The adsorbent provided by the invention is simple and feasible in preparation process, easy to synthesize and low in raw material cost.
(3) The modified zirconium-based metal organic framework adsorbent for gold ion adsorption has the advantages of no toxicity, stable performance, easy separation, reutilization and no secondary pollution to the environment.
(4) The modified zirconium-based metal organic framework adsorbent has good economic and practical values. Has great popularization potential in the aspect of selective recovery of gold ions.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1:
the modified zirconium-based metal organic framework adsorbent for gold ion adsorption has the structural formula:
The preparation method of the gold ion adsorbed modified zirconium-based metal organic framework adsorbent comprises the following specific steps:
(1) uniformly mixing 2-aminoterephthalic acid and N, N-dimethylformamide solution according to the solid-to-liquid ratio of 1:30 g/mL; adding zirconium tetrachloride according to the mass ratio of the 2-amino terephthalic acid to the zirconium tetrachloride of 1: 1; and then adding hydrochloric acid according to the liquid-solid ratio of 1:1mL/g of hydrochloric acid and 2-Amino terephthalic acid, carrying out reflux reaction at 110 ℃ for 12h, carrying out liquid-solid separation, washing the obtained solid with an N, N-dimethylformamide solution, centrifuging, and carrying out vacuum drying to obtain Amino-UiO-66. The synthetic route is as follows:
(2) uniformly mixing N, N-dimethylformamide and Amino-UiO-66 at a liquid-solid ratio of 30:1mL/g, adding 2-Amino-5-aldehyde thiazole according to the mass ratio of the Amino-UiO-66 to the 2-Amino-5-aldehyde thiazole of 1:1, carrying out reflux reaction at 50 ℃ for 12 hours, carrying out liquid-solid separation, washing the obtained solid with N, N-dimethylformamide solution, centrifuging, and carrying out vacuum drying to obtain AF-UiO-66. The synthetic route is as follows:
and (3) testing the performance of adsorbing gold ions:
10mg of the AF-UiO-66 adsorbent in the embodiment is put into a gold ion solution with the initial concentration of 100mg/L for oscillation adsorption for 5h, centrifugal separation is carried out, the concentration of gold ions in the supernatant is measured by AAS to be 5.41mg/L, and the adsorption rate is 94.59%. Desorbing the bottom layer solid with thiourea solution (10 wt%) for 12h, centrifuging, washing, drying at 65 deg.C for 12h, adding into 100mg/L gold ion solution again, shaking for 5h, centrifuging, and determining the gold ion concentration in the supernatant to be 7.89mg/L and the adsorption rate to be 92.11% by AAS. The 2-amino-5-aldehyde thiazole modified zirconium-based metal organic framework adsorbent AF-UiO-66 can be repeatedly used for removing gold ions in aqueous solution.
Example 2:
the modified zirconium-based metal organic framework adsorbent for gold ion adsorption has the structural formula:
The preparation method of the gold ion adsorbed modified zirconium-based metal organic framework adsorbent comprises the following specific steps:
(1) uniformly mixing 2-aminoterephthalic acid and N, N-dimethylformamide solution according to the solid-to-liquid ratio of 1:40 g/mL; adding zirconium tetrachloride according to the mass ratio of 1.1:1 between 2-amino terephthalic acid and zirconium tetrachloride; and then adding hydrochloric acid according to the liquid-solid ratio of 1:5mL/g of hydrochloric acid to 2-Amino terephthalic acid, carrying out reflux reaction at 120 ℃ for 18h, carrying out liquid-solid separation, washing the obtained solid with an N, N-dimethylformamide solution, centrifuging, and carrying out vacuum drying to obtain Amino-UiO-66. The synthetic route is as follows:
(2) uniformly mixing N, N-dimethylformamide and Amino-UiO-66 at a liquid-solid ratio of 40:1mL/g, adding 2-Amino-5-aldehyde thiazole according to the mass ratio of the Amino-UiO-66 to the 2-Amino-5-aldehyde thiazole of 1:1.1, carrying out reflux reaction at 55 ℃ for 18h, carrying out liquid-solid separation, washing the obtained solid with N, N-dimethylformamide solution, centrifuging, and carrying out vacuum drying to obtain the AF-UiO-66. The synthetic route is as follows:
and (3) testing the performance of adsorbing gold ions:
10mg of the AF-UiO-66 adsorbent in the embodiment is put into a gold ion solution with the initial concentration of 100mg/L for oscillation adsorption for 5h, centrifugal separation is carried out, the concentration of gold ions in the supernatant is determined to be 3.99mg/L by AAS, and the adsorption rate is 96.01%. Desorbing the bottom layer solid with thiourea solution (10 wt%) for 12h, centrifuging, washing, drying at 65 deg.C for 12h, adding into 100mg/L gold ion solution again, shaking for 5h, centrifuging, and determining the gold ion concentration in the supernatant as 5.44mg/L by AAS, with the adsorption rate of 94.56%. The 2-amino-5-aldehyde thiazole modified zirconium-based metal organic framework adsorbent AF-UiO-66 can be repeatedly used for removing gold ions in aqueous solution.
Example 3:
the gold ion-adsorbed modified zirconium-based metal organic framework adsorbent has the structural formula:
The preparation method of the gold ion adsorbed modified zirconium-based metal organic framework adsorbent comprises the following specific steps:
(1) uniformly mixing 2-aminoterephthalic acid and N, N-dimethylformamide solution according to the solid-to-liquid ratio of 1:50 g/mL; adding zirconium tetrachloride according to the mass ratio of 1.2:1 of 2-amino terephthalic acid to zirconium tetrachloride; and then adding hydrochloric acid according to the liquid-solid ratio of 1:10mL/g of hydrochloric acid to 2-Amino terephthalic acid, carrying out reflux reaction at 130 ℃ for 24 hours, carrying out liquid-solid separation, washing the obtained solid with an N, N-dimethylformamide solution, centrifuging, and carrying out vacuum drying to obtain Amino-UiO-66. The synthetic route is as follows:
(2) uniformly mixing N, N-dimethylformamide and Amino-UiO-66 at a liquid-solid ratio of 50:1mL/g, adding 2-Amino-5-aldehyde thiazole according to the mass ratio of the Amino-UiO-66 to the 2-Amino-5-aldehyde thiazole of 1:1.2, carrying out reflux reaction at 65 ℃ for 24 hours, carrying out liquid-solid separation, washing the obtained solid with N, N-dimethylformamide solution, centrifuging, and carrying out vacuum drying to obtain the AF-UiO-66. The synthetic route is as follows:
and (3) testing the performance of adsorbing gold ions:
10mg of the AF-UiO-66 adsorbent in the embodiment is put into a gold ion solution with the initial concentration of 100mg/L for shaking adsorption for 5 hours, and then centrifugal separation is carried out, the gold ion concentration in the supernatant is measured to be 0.54mg/L by AAS, and the adsorption rate is 99.46%. Desorbing the bottom layer solid with thiourea solution (10 wt%) for 12h, centrifuging, washing, vacuum drying at 65 deg.C for 12h, adding into 100mg/L gold ion solution again, shaking for 5h, centrifuging, and determining the gold ion concentration in the supernatant to be 1.15mg/L by AAS, with the adsorption rate of 98.85%. The 2-amino-5-aldehyde thiazole modified zirconium-based metal organic framework adsorbent AF-UiO-66 can be repeatedly used for removing gold ions in aqueous solution.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (6)
1. A modified zirconium-based metal organic framework adsorbent for gold ion adsorption is characterized in that the structural formula is as follows:
2. the method for preparing a modified zirconium-based metal organic framework adsorbent for gold ion adsorption according to claim 1, comprising the steps of:
(1) sequentially adding 2-aminoterephthalic acid and zirconium tetrachloride into an N, N-dimethylformamide solution, dropwise adding hydrochloric acid, carrying out reflux reaction in a round-bottom three-necked bottle, carrying out liquid-solid separation, washing the obtained solid with the N, N-dimethylformamide solution, centrifuging, and carrying out vacuum drying to obtain Amino-UiO-66;
(2) and (2) sequentially adding the product Amino-UiO-66 and 2-Amino-5-aldehyde thiazole obtained in the step (1) into an N, N-dimethylformamide solution for reflux reaction, performing liquid-solid separation, washing the obtained solid with the N, N-dimethylformamide solution, centrifuging, and performing vacuum drying to obtain the AF-UiO-66.
3. The method of claim 2, wherein: in the step (1), the solid-to-liquid ratio of the 2-aminoterephthalic acid to the N, N-dimethylformamide is 1: 30-1: 50g/mL, the liquid-to-solid ratio of the hydrochloric acid to the 2-aminoterephthalic acid is 1: 1-1: 10mL/g, and the mass ratio of the 2-aminoterephthalic acid to the zirconium tetrachloride is 1: 1-1.2: 1.
4. The method of claim 2, wherein: in the step (2), the liquid-solid ratio of the N, N-dimethylformamide to the Amino-UiO-66 is 30: 1-50: 1mL/g, and the mass ratio of the Amino-UiO-66 to the 2-Amino-5-aldehyde thiazole is 1: 1-1: 1.2.
5. The method of claim 2, wherein: the reflux in the step (1) is carried out for 12-24 h at the temperature of 110-130 ℃; and (3) the reflux in the step (2) is carried out for 12-24 hours at the temperature of 50-70 ℃.
6. Use of the modified zirconium based metal organic framework adsorbent for gold ion adsorption according to claims 1 to 5 for selective adsorptive recovery of gold ions in aqueous solution.
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| CN115490879A (en) * | 2022-11-03 | 2022-12-20 | 江苏海洋大学 | EDTA (ethylene diamine tetraacetic acid) -modified UIO-66 (Zr) metal organic framework material as well as preparation method and application thereof |
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