CN114574709A - Method for recovering precious metal based on floating covalent organic polymer material - Google Patents
Method for recovering precious metal based on floating covalent organic polymer material Download PDFInfo
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- CN114574709A CN114574709A CN202210200356.4A CN202210200356A CN114574709A CN 114574709 A CN114574709 A CN 114574709A CN 202210200356 A CN202210200356 A CN 202210200356A CN 114574709 A CN114574709 A CN 114574709A
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 229920000620 organic polymer Polymers 0.000 title claims abstract description 8
- 239000002861 polymer material Substances 0.000 title claims abstract description 7
- 239000010970 precious metal Substances 0.000 title claims description 11
- 239000000463 material Substances 0.000 claims abstract description 55
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 150000002500 ions Chemical class 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000007146 photocatalysis Methods 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 125000003277 amino group Chemical group 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 230000000737 periodic effect Effects 0.000 claims abstract description 6
- 125000000524 functional group Chemical group 0.000 claims abstract description 5
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 5
- 230000009286 beneficial effect Effects 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 238000013329 compounding Methods 0.000 claims abstract description 3
- 238000000967 suction filtration Methods 0.000 claims abstract description 3
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 229910052763 palladium Inorganic materials 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004729 solvothermal method Methods 0.000 claims description 4
- 230000001699 photocatalysis Effects 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 239000013310 covalent-organic framework Substances 0.000 claims 12
- 150000002739 metals Chemical class 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000010793 electronic waste Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
- 229960001553 phloroglucinol Drugs 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010926 waste battery Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
-
- 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]
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/60—Reduction reactions, e.g. hydrogenation
- B01J2231/62—Reductions in general of inorganic substrates, e.g. formal hydrogenation, e.g. of N2
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- 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
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Abstract
A method for recovering noble metals based on a floating covalent organic polymer material belongs to the field of noble metal recovery. The floating type adsorption-photocatalysis material with certain hydrophobic property is obtained through compounding the COF with the nitrogen-rich structure and the flexible material catkin and performing suction filtration, the floating type COF material can utilize functional groups such as surface amino groups to efficiently adsorb noble metal ions through electrostatic attraction, and meanwhile, the COF with the periodic pi conjugated system is beneficial to electronic delocalization, so that the floating type COF has excellent photoconductivity, the COF floating on the water surface can greatly absorb visible light to excite the separation of electron-hole pairs, and the noble metal ions adsorbed on the surface of the floating type COF material are reduced into nano metal simple substances, thereby realizing the recycling of the noble metal.
Description
Technical Field
The invention designs a noble metal recovery method, and particularly relates to a floating covalent organic polymer (COF) photocatalytic material for recovering noble metals.
Background
Noble metals (Pd, Pt, Au, etc.) are widely used in the fields of electronic devices and industrial catalysis because of their physical properties such as good ductility, conductivity, etc. However, with the upgrading of electronic products, electronic wastes such as waste batteries and mobile phones are growing in multiples, so that a material is designed to recover precious metals in the electronic wastes to prevent environmental pollution, and the material also has great economic benefits.
At present, the recovery methods of noble metals mainly comprise hydrometallurgy, thermal metallurgy, ion exchange and the like. However, most of these methods are limited by various conditions to reduce operability, such as high cost and low recovery efficiency, and the use of a large amount of organic solvent causes environmental pollution. Among the recovery methods, the adsorption method has the advantages of simplicity, high efficiency, environmental friendliness and the like, and is widely concerned, but most of adsorption materials have low reusability and low functional group density, and the recovered noble metal ions need to be further reduced to obtain a metal simple substance, so that the cost and the complexity are greatly increased. Therefore, based on the advantages of adsorption and the disadvantages of the existing material method, the development of a floating type adsorption-photocatalytic reduction integrated method for recycling and reusing precious metals is urgently needed.
Disclosure of Invention
The invention aims to provide a method for recovering noble metal based on a floating COF material aiming at the defects of the existing method
In order to solve the above problems, the present invention provides the following technical solutions: a method for recovering precious metals based on floating COF materials is characterized by comprising the following steps:
(1) compounding COF with a nitrogen-rich structure with a flexible material catkin, and performing suction filtration to obtain a floating type adsorption-photocatalysis material with certain hydrophobic property;
(2) the floating type adsorption-photocatalysis material is placed in a noble metal ion solution, the COF material can adsorb noble metal ions, and noble metal ions (Au, Pt, Pd and the like) are reduced into a nano metal simple substance through photocatalysis.
The COF is a periodic pi conjugated system with a nitrogen-rich structure.
The COF with the nitrogen-rich structure and the flexible material catkin obtained in the step (1) are prepared by mixing (1): 1, adding dimethyl sulfoxide as a solvent, and carrying out ultrasonic treatment for 20 min; (2) and carrying out solvothermal reaction on the obtained mixture at 160 ℃ to obtain the composite material. The floating type adsorption-photocatalysis material adopts a flexible substrate catkin loaded with a photocatalyst COF, and utilizes the strong hydrophobic property of the catkin to support the COF to float on the water surface.
The surface of the floating COF material is provided with a nitrogen-rich group, and the nitrogen-rich group is an amino group;
the floating COF material is placed in water containing noble metal ions, the noble metal ions are efficiently adsorbed by utilizing functional groups such as surface amino groups through electrostatic attraction, and meanwhile, the COF with a periodic pi conjugated system is beneficial to electron delocalization, so that the excellent photoelectric conductivity is achieved, the COF floating on the water surface can greatly absorb visible light, the separation of electron-hole pairs is excited, and the noble metal ions adsorbed on the surface of the floating COF material are reduced into a nano metal simple substance.
The floating type COF material can be adjusted in size, thickness, shape and the like according to actual conditions.
The floating COF material can be recycled by a simple flushing method, so that the material has excellent recycling performance.
Compared with the existing adsorbing material, the floating COF material is used for recovering the precious metals, the surface amino groups of the COF efficiently adsorb the precious metal ions through the electrostatic effect, and then the COF material floating on the water surface can fully absorb visible light and reduce the precious metal ions, so that the sewage purification is realized by using the cheap material, and meanwhile, the high economic benefit is brought.
The floating COF material can be simply recycled after being used, the reduced precious metal can be recycled and then put into use again, extra mechanical treatment such as stirring is not needed in the using process, and the cost can be effectively reduced.
Drawings
FIG. 1: schematic of floating COF materials;
FIG. 2: the drawings of the floating COF material for Au, Pt and Pd are shown in the figure;
FIG. 3: and recycling the floating COF material.
Detailed Description
The technical solutions of the present invention will be further explained with reference to the accompanying drawings, and the described embodiments are only some of the embodiments of the present invention.
Example 1 referring to fig. 1, a COF and a flexible material catkin were combined to obtain a floating COF material, and a sheet-like COF material was obtained by solvothermal synthesis and filtration, and the shape and size thereof were freely adjusted according to the shape and size of a filter bowl. The floating COF material is placed in water containing noble metal ions, the noble metal ions are efficiently adsorbed by utilizing functional groups such as surface amino groups through the electrostatic attraction effect, meanwhile, the COF with a periodic pi conjugated system is beneficial to electron delocalization, so that the excellent photoelectric conductivity is achieved, the COF floating on the water surface can greatly absorb visible light, the separation of electron-hole pairs is excited, and the noble metal ions adsorbed on the surface of the floating COF material are reduced into a nano metal simple substance.
The floating COF material is prepared by taking melamine, trialdehyde phloroglucinol, p-phenylenediamine and the like as monomers and taking a flexible material catkin as a carrier through a solvothermal reaction.
Example 2, referring to fig. 2, the floating COF materials were added to Au (iii), Pt (iv), Pd (ii) solutions each having a volume of 50ml and a concentration of 10mg/L, and adsorbed for 24 hours under a dark condition, and then the resulting solutions were subjected to AES-ICP test, and found to have excellent adsorption properties for Au, Pt, Pd. The floating COF material is a circle with the diameter of 3.5cm and the thickness of 1mm, the shape, the thickness and the size of the floating COF material can be adjusted randomly according to practical application, the floating COF material can absorb visible light, and noble metal ions adsorbed on the surface are reduced into simple metal substances.
Example 3, referring to fig. 3, the floating COF material can be easily recycled and has excellent recyclability.
Finally, it should be noted that the above-mentioned examples are only examples for explaining the present invention, and do not limit the embodiments, and in this document, terms such as "comprising", "including", and the like are used to include a series of methods, processes, and other elements. The noble metal ions include, but are not limited to, Au, Pt, Pd, and also include metal ions such as Fe, Co, Ni, Cu, Zn, etc. In addition, although practical examples of the present invention have been clearly shown, it will be apparent to those skilled in the art that changes, modifications and substitutions may be made in the embodiments based on the principles of the present description, and thus the changes may be made within the scope of the present invention.
Claims (6)
1. A method for recovering precious metals based on a floating covalent organic polymeric material, comprising the steps of:
(1) compounding COF with a nitrogen-rich structure with flexible material catkin, and performing suction filtration to obtain a floating adsorption-photocatalysis material with certain hydrophobic property;
(2) placing the floating type adsorption-photocatalysis material in a noble metal ion solution, wherein the COF material can adsorb noble metal ions and reduce the noble metal ions into a nano metal simple substance through photocatalysis;
the COF is a periodic pi conjugated system with a nitrogen-rich structure.
2. The method for recovering noble metals based on floating covalent organic polymer materials according to claim 1, wherein the COF with nitrogen-rich structure is composited with flexible material catkin in a ratio of 1: 1, adding dimethyl sulfoxide as a solvent, and carrying out ultrasonic treatment for 20 min; carrying out solvothermal reaction on the obtained mixture at 160 ℃ to obtain the composite material; the floating type adsorption-photocatalysis material adopts a flexible substrate catkin loaded with a photocatalyst COF, and utilizes the strong hydrophobic property of the catkin to support the COF to float on the water surface.
3. The method for recovering noble metals based on floating covalent organic polymer materials of claim 1, wherein the floating COF material has nitrogen-rich groups on the surface, and the nitrogen-rich groups are amino groups.
4. The method for recovering noble metals based on floating covalent organic polymer materials according to claim 1, wherein the floating COF materials are placed in water containing noble metal ions, the noble metal ions are efficiently adsorbed by functional groups such as surface amino groups through electrostatic attraction, and meanwhile, COFs with periodic pi conjugated systems are beneficial to electron delocalization, so that the COFs floating on the water surface can greatly absorb visible light to excite electron-hole pair separation, and the noble metal ions adsorbed on the surface of the floating COF materials are reduced into nano elemental metals.
5. The method according to claim 1, wherein the noble metal is selected from the group consisting of Au, Pt, and Pd.
6. The method for recovering precious metals based on floating covalent organic polymer materials according to claim 1, wherein the floating COF materials can be recovered by simple washing method, so that the materials have excellent recyclability.
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| CN202210200356.4A CN114574709B (en) | 2022-03-02 | 2022-03-02 | Method for recycling noble metal based on floating covalent organic polymer material |
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| CN202210200356.4A CN114574709B (en) | 2022-03-02 | 2022-03-02 | Method for recycling noble metal based on floating covalent organic polymer material |
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| CN110215905A (en) * | 2019-07-16 | 2019-09-10 | 福州大学 | A kind of magnetic adsorbent and preparation method thereof removing Nano silver grain |
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| CN113149123A (en) * | 2021-03-31 | 2021-07-23 | 清华大学 | Treatment method for selectively adsorbing and recovering precious metal ions in wastewater by using modified polymer adsorbent |
| CN113209307A (en) * | 2021-04-09 | 2021-08-06 | 山东师范大学 | Au & Ag alloy doped nano covalent organic framework material and preparation method and application thereof |
| CN113832354A (en) * | 2020-06-24 | 2021-12-24 | 武汉理工大学 | Method for efficiently reducing and recovering precious metals in leachate by piezoelectric photocatalysis method |
| CN113831491A (en) * | 2021-09-30 | 2021-12-24 | 南昌大学 | Preparation method and adsorption application of pyrimidazole covalent organic framework |
-
2022
- 2022-03-02 CN CN202210200356.4A patent/CN114574709B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110215905A (en) * | 2019-07-16 | 2019-09-10 | 福州大学 | A kind of magnetic adsorbent and preparation method thereof removing Nano silver grain |
| CN111057863A (en) * | 2019-12-24 | 2020-04-24 | 湖北千里材料科技有限公司 | Application of environment-friendly precious metal adsorption resin material |
| CN113832354A (en) * | 2020-06-24 | 2021-12-24 | 武汉理工大学 | Method for efficiently reducing and recovering precious metals in leachate by piezoelectric photocatalysis method |
| CN113149123A (en) * | 2021-03-31 | 2021-07-23 | 清华大学 | Treatment method for selectively adsorbing and recovering precious metal ions in wastewater by using modified polymer adsorbent |
| CN113209307A (en) * | 2021-04-09 | 2021-08-06 | 山东师范大学 | Au & Ag alloy doped nano covalent organic framework material and preparation method and application thereof |
| CN113831491A (en) * | 2021-09-30 | 2021-12-24 | 南昌大学 | Preparation method and adsorption application of pyrimidazole covalent organic framework |
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