CN113105647A - Preparation method of acid-resistant Cu-MOF material for selectively adsorbing divalent palladium - Google Patents
Preparation method of acid-resistant Cu-MOF material for selectively adsorbing divalent palladium Download PDFInfo
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Abstract
A preparation method of an acid-resistant Cu-MOF material capable of selectively adsorbing divalent palladium relates to a preparation method of an MOF material capable of adsorbing divalent palladium. The invention aims to solve the technical problems that the existing MOF material is difficult to stably exist in an aqueous solution, the structure is easy to collapse and collapse, and the noble metal palladium is difficult to selectively separate. The invention disclosesPreparation method of Cu-based MOF (metal organic framework), nitrogen heterocyclic ligand taking tetrazine group as functional mode and V-type ligand containing ether bond, and Cu2+The metal ion coordination constructs a metal organic framework with excellent water stability and certain acid resistance, the excellent water stability and certain acid resistance enable the material to have strong adaptability and potential when treating acidic heavy metal wastewater, the material has good selective adsorption capacity on bivalent palladium in a water body, the adsorption capacity reaches 177mg/g, and the process of recycling precious metal palladium independently is enhanced.
Description
Technical Field
The invention relates to a preparation method of an MOF material for adsorbing divalent palladium.
Background
Noble metals have luxurious appearance, and also have excellent physicochemical properties as materials for making coins and jewelry, so that they are widely used in the fields of catalysis, medicine, and the like. Especially in the field of electronics, noble metals have developed as an important component of high-tech materials, even as an indispensable element of modern industry, the importance of which is seen in vain. In consideration of wide application, high value and limited reserves of the precious metals at present, how to recycle the precious metals from industrial wastewater containing gold and palladium and how to improve the selective extraction technology become urgent. Among all the current recovery technologies applied to the resource utilization of wastewater, the adsorption method is almost the most scientific and economic method. The adsorption method has higher adsorption capacity, higher adsorption rate and higher cycle elution times, so that the adsorption method is preferred in the wastewater resource application. Therefore, the water treatment adsorbing material can be designed according to the actual situation of the noble metal wastewater to recover the noble metal palladium.
Some adsorbents can separate palladium element from waste circuit board liquid of wet processing, the process mostly adopts an oxidation reduction method by utilizing the characteristic that noble metal is easy to reduce, palladium and other noble metals can be recycled, and a subsequent separation step is needed for separating palladium from noble metals such as gold, platinum and the like. Since gold has the highest oxidation potential among these noble metals, the separation of palladium from gold, which has the same higher oxidation potential, cannot be really achieved by conventional reduction processes alone. The irreversibility of oxidation and reduction leads to the fact that the materials cannot be recycled, and the process cost is increased. The direct separation of palladium from heavy metal solutions in which precious metals are present is a technical difficulty. The MOF material has rich designable structure types, adjustable chemical functions, a low-density framework, an ultrahigh specific surface area and a functionalized permanent pore space, and has wide application potential in the fields of gas storage and separation, catalysis, sensing, drug transportation, slow release and the like. Meanwhile, the characteristics of the MOF such as porosity, high specific surface area and the like also enable the MOF to have the potential of becoming an excellent adsorption material. Therefore, the preparation of the MOF material which has better water stability, acid resistance and no reducibility and can selectively adsorb divalent palladium so as to facilitate resource recycling has strong practical significance.
Disclosure of Invention
The invention provides a preparation method of an acid-resistant Cu-MOF material for selectively adsorbing divalent palladium, aiming at solving the technical problems that the existing MOF material is difficult to stably exist in an aqueous solution, the structure is easy to collapse and collapse, and the noble metal palladium is difficult to selectively separate.
The preparation method of the acid-resistant Cu-MOF material for selectively adsorbing divalent palladium is carried out according to the following steps:
fully mixing a nitrogen heterocyclic ligand containing a tetrazine group, a V-type carboxylic acid ligand containing an ether bond and copper salt in an organic solvent, then reacting for 12-72 h under the condition of sealing and 80-150 ℃, carrying out solid-liquid separation on the product, and then drying the solid to obtain purple transparent single crystals, namely Cu-MOF;
the nitrogen heterocyclic ligand containing tetrazine group is 3, 6-di (4-pyridyl) -1,2,4, 5-tetrazine;
the V-type carboxylic acid ligand containing ether bonds is 4, 4' -dicarboxydiphenyl ether;
the mole ratio of the nitrogen heterocyclic ligand containing tetrazine group to the V-type carboxylic acid ligand containing ether bond is 1 (0.5-2);
the molar ratio of the nitrogen heterocyclic ligand containing the tetrazine group to the copper element in the copper salt is 1 (0.5-2);
the volume ratio of the molar weight of the nitrogen heterocyclic ligand containing tetrazine group to the organic solvent is 1mmol (200 mL-220 mL).
The Cu is selected as the metal center in the invention because the Cu-O bond is stronger, a paddle wheel type metal cluster structure can be formed, and the water stability is better.
The invention selects DPT (3, 6-di (4-pyridyl) -1,2,4, 5-tetrazine with CAS number of 1671-87-0) as ligand, firstly, uses tetrazine group as functional group to selectively adsorb bivalent palladium; and secondly, the tetrazine group has certain affinity with hydrogen ions, so that the material has better capability of coping with an acidic environment.
Selection of H in the invention2OBA (4, 4' -dicarboxydiphenyl ether) is used as a ligand, and the first one is that the OBA and DPT are used together as a connecting bridge to form a three-dimensional structure together with a copper paddle wheel type metal cluster; second is type V ligand H2The frame structure formed by the OBA causes steric hindrance, and different heavy metal ions can be separated.
The invention discloses a preparation method of Cu-based MOF, which utilizes tetrazine group as nitrogen heterocyclic ligand of a functional mode and V-type ligand containing ether bond, and Cu2+The metal ions are coordinated, a Metal Organic Framework (MOF) with excellent water stability and certain acid resistance is constructed, and the material has strong adaptability and potential when being used for treating acidic heavy metal wastewater due to the excellent water stability and certain acid resistance. The material has almost no reducing capability, avoids the reduction process of noble metal ions with higher oxidation potential such as gold and the like, and is beneficial to the process of selectively adsorbing palladium ions by utilizing acting forces such as coordination, electrostatic attraction and the like. The Cu-MOF provided by the invention is used as a novel water treatment functional material, has good selective adsorption capacity for divalent palladium in a water body, has good adsorption capacity for divalent palladium, and enhances the independent recycling process of noble metal palladium, wherein the adsorption capacity reaches 177 mg/g.
Drawings
FIG. 1 is a schematic diagram of the structure of an experiment one prepared Cu-MOF;
FIG. 2 is a crystal morphology of Cu-MOF prepared in experiment one under a microscope at 50 times magnification;
FIG. 3 is a TEM image of an experiment one prepared Cu-MOF;
FIG. 4 is an XRD image;
FIG. 5 is an XRD pattern of the adsorbent of test two after soaking for one week at different pH conditions;
figure 6 is a graph of the results of sorbent test data in test three.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of an acid-resistant Cu-MOF material for selectively adsorbing divalent palladium, which is specifically carried out according to the following steps:
fully mixing a nitrogen heterocyclic ligand containing a tetrazine group, a V-type carboxylic acid ligand containing an ether bond and copper salt in an organic solvent, then reacting for 12-72 h under the condition of sealing and 80-150 ℃, carrying out solid-liquid separation on the product, and then drying the solid to obtain purple transparent single crystals, namely Cu-MOF;
the nitrogen heterocyclic ligand containing tetrazine group is 3, 6-di (4-pyridyl) -1,2,4, 5-tetrazine;
the V-type carboxylic acid ligand containing ether bonds is 4, 4' -dicarboxydiphenyl ether;
the mole ratio of the nitrogen heterocyclic ligand containing tetrazine group to the V-type carboxylic acid ligand containing ether bond is 1 (0.5-2);
the molar ratio of the nitrogen heterocyclic ligand containing the tetrazine group to the copper element in the copper salt is 1 (0.5-2);
the volume ratio of the molar weight of the nitrogen heterocyclic ligand containing tetrazine group to the organic solvent is 1mmol (200 mL-220 mL).
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the copper salt is CuCl2、Cu(NO3)2、CuSO4And Cu (CH)3COO)2One or a mixture of several of them. Other toolsThe first embodiment is the same.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the organic solvent is C2H5OH、CH3One or a mixture of more of OH, DMF, DMA and DMSO. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the drying temperature is 150 ℃, and the drying time is 12 h. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: the solid-liquid separation is completed by a suction filtration method. The rest is the same as the fourth embodiment.
The invention was verified with the following tests:
test one: the test is a preparation method of the acid-resistant Cu-MOF material for selectively adsorbing divalent palladium, and is specifically carried out according to the following steps:
35.4mg of a nitrogen heterocyclic ligand containing a tetrazine group, 38.7mg of a V-type carboxylic ligand containing an ether bond and 36mg of Cu (NO)3)2·3H2Fully mixing O together in 15mL of DMF and 15mL of methanol mixed solvent, then reacting for 72h under the condition of sealing and 90 ℃, filtering the product, and then drying the filter cake at the drying temperature of 150 ℃ for 12h to obtain purple transparent single crystals, namely Cu-MOF;
the nitrogen heterocyclic ligand containing tetrazine group is 3, 6-di (4-pyridyl) -1,2,4, 5-tetrazine;
the V-type carboxylic acid ligand containing ether bonds is 4, 4' -dicarboxydiphenyl ether.
FIG. 1 is a schematic diagram of the structure of a Cu-MOF prepared by experiment, wherein an acting group tetrazinyl is introduced into the MOF, and the group has certain affinity with hydrogen ions, so that the prepared Cu-MOF has better tolerance under acidic conditions.
Table 1 shows the crystallographic data of the Cu-MOF prepared in the first experiment, and the Cu-MOF crystals belong to the monoclinic P2/c space group. Four terephthalic acid and two aminomethyl pyridine ligands are assembled with a copper paddle wheel type structure to form a monoclinic metal organic polyhedron, and finally the porous three-dimensional MOF is assembled.
TABLE 1
Fig. 2 and 3 are the crystal morphology and TEM image of experiment-prepared Cu-MOF under a microscope at 50 x magnification, respectively, showing that the experimental preparation method is stable and efficient.
Fig. 4 is an XRD image, curve 1 is theoretically fitted Cu-MOF, curve 2 is Cu-MOF prepared in the first test, and curve 3 is a product of drying the filter cake in the first test at 55 ℃ for 3 hours, which shows that the Cu-MOF maintains good consistency with the theoretically fitted XRD diffraction pattern before and after drying, thus proving that the method for preparing Cu-MOF in the first test can obtain pure-phase material, the dried material can maintain the original skeleton characteristics, and the Cu-MOF skeleton can have good stability after removing unreacted reactants and solvent molecules in the pore channels (i.e. after drying).
And (2) test II: the test is to evaluate the water stability of Cu-MOF:
preparing 10 beakers, adding 50mL of deionized water into each beaker, and adjusting the pH of the aqueous solution in the 10 beakers to 3, 4,5, 6, 7, 8, 9, 10, 11 and 12 by hydrochloric acid and sodium hydroxide; respectively weighing 10 parts of 20mg of Cu-MOF prepared in the first test as an adsorbent, adding the adsorbent into 10 beakers, soaking for one week, separating the adsorbent after one week, and inspecting XRD images of the adsorbent.
FIG. 5 is an XRD image of the adsorbent of test two after one week of soaking at different pH conditions, and it can be seen that the XRD pattern remains substantially unchanged, demonstrating the excellent water stability and acid resistance of Cu-MOF.
And (3) test III: the test is used for evaluating the adsorption capacity of Cu-MOF:
respectively preparing 12 parts of 50mL of aqueous solutions of trivalent Au ions, divalent Pd ions, monovalent Ag ions, divalent Co ions, divalent Ni ions, hexavalent Cr ions, divalent Cu ions, trivalent Sb ions, pentavalent Sb ions, divalent Cd ions and pentavalent P ions, wherein the ion concentrations of the trivalent Au ions, the divalent Pd ions, the monovalent Ag ions, the divalent Co ions, the divalent Ni ions, the hexavalent Cr ions, the divalent Cu ions, the trivalent Sb ions, the pentavalent Sb ions, the divalent Cd ions and the pentavalent P ions are 200mg/L, respectively placing the aqueous solutions into 12 sample bottles, respectively adding 20mg of Cu-MOF material prepared in the first test into each sample bottle as an adsorbent, then oscillating all the sample bottles at a constant temperature of 25 ℃ for 24 hours, finally detecting the concentration of metal ions in the supernatant of each sample bottle, and.
FIG. 6 is a graph of the results of sorbent test data in test three, and not only can the Cu-MOF material prepared in test one be seen versus Pd in FIG. 62+The characteristics of high adsorption capacity (177mg/g) and strong selectivity of adsorption show that the first experiment shows that the prepared Cu-MOF material is used for adsorbing and recovering Pd in heavy metal wastewater2+Separation of Pd from waste liquid of noble metals2+Has great potential in all aspects.
Claims (5)
1. A preparation method of an acid-resistant Cu-MOF material for selectively adsorbing divalent palladium is characterized in that the preparation method of the acid-resistant Cu-MOF material for selectively adsorbing divalent palladium is carried out according to the following steps:
fully mixing a nitrogen heterocyclic ligand containing a tetrazine group, a V-type carboxylic acid ligand containing an ether bond and copper salt in an organic solvent, then reacting for 12-72 h under the condition of sealing and 80-150 ℃, carrying out solid-liquid separation on the product, and then drying the solid to obtain purple transparent single crystals, namely Cu-MOF;
the nitrogen heterocyclic ligand containing tetrazine group is 3, 6-di (4-pyridyl) -1,2,4, 5-tetrazine;
the V-type carboxylic acid ligand containing ether bonds is 4, 4' -dicarboxydiphenyl ether;
the mole ratio of the nitrogen heterocyclic ligand containing tetrazine group to the V-type carboxylic acid ligand containing ether bond is 1 (0.5-2);
the molar ratio of the nitrogen heterocyclic ligand containing the tetrazine group to the copper element in the copper salt is 1 (0.5-2);
the volume ratio of the molar weight of the nitrogen heterocyclic ligand containing tetrazine group to the organic solvent is 1mmol (200 mL-220 mL).
2. The method of claim 1, wherein the copper salt is CuCl2、Cu(NO3)2、CuSO4And Cu (CH)3COO)2One or a mixture of several of them.
3. The method of claim 1, wherein the organic solvent is C2H5OH、CH3One or a mixture of more of OH, DMF, DMA and DMSO.
4. The method for preparing the acid-resistant Cu-MOF material for selectively adsorbing the divalent palladium according to claim 1, wherein the drying temperature is 150 ℃ and the drying time is 12 hours.
5. The method for preparing the acid-resistant Cu-MOF material for selectively adsorbing the divalent palladium according to claim 1, wherein the solid-liquid separation is performed by suction filtration.
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| CN111545171A (en) * | 2020-04-16 | 2020-08-18 | 南昌航空大学 | Preparation method of acid-resistant Zr-MOF material for selectively adsorbing hexavalent chromium |
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