CN114479109A - Preparation and application of N, S-containing metal organic framework material - Google Patents
Preparation and application of N, S-containing metal organic framework material Download PDFInfo
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- CN114479109A CN114479109A CN202210121229.5A CN202210121229A CN114479109A CN 114479109 A CN114479109 A CN 114479109A CN 202210121229 A CN202210121229 A CN 202210121229A CN 114479109 A CN114479109 A CN 114479109A
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Abstract
The patent discloses preparation and application of N, S-containing metal organic framework material. The metal organic framework material (Zn-AMT) containing N, S functionalized atoms is prepared by one-step reaction of zinc nitrate hexahydrate and 3-amino-5-mercapto-1, 2, 4-triazole. The preparation method is simple, the prepared material is used as an adsorbent to treat trivalent gold ions in the aqueous solution, the adsorption capacity is high, the adsorption rate is high, the selective adsorption performance on gold is outstanding, the desorption and the reutilization are easy, and a feasible new method is provided for the recovery and the utilization of noble metals.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to synthesis of a metal organic framework material Zn-AMT containing N and S and a method for adsorbing and separating Au (III) ions in an aqueous solution by using the metal organic framework material Zn-AMT.
Background
The content of noble metals in the nature is extremely low, and the noble metals are generally intergrowth with other mineral deposits. The traditional means for obtaining the noble metal has low efficiency and high energy consumption, so that the yield of the recovery of the noble metal is difficult to improve, and the demand of human beings for the noble metal is increasing. In order to deal with the contradiction between the supply and demand of precious metal resources, the recovery of precious metals is bound to become a future development direction. The recovery of the noble metal not only can lead to the repeated use of scarce resources, but also can bring great economic benefit to the society and play a role in promoting the protection of the ecological environment. The measure is beneficial to building an ecological civilized society and promoting national economic development and scientific and technological progress.
Gold is one of the most widely used precious metals, and has excellent physical and chemical properties, such as high temperature oxidation resistance, corrosion resistance, electrical resistance, good electrical conductivity, higher catalytic activity, stronger coordination ability and the like. In industrial applications, gold is called an industrial vitamin because of its wide use and indispensable functions. At present, methods applied to gold ion separation include chemical precipitation, membrane filtration, ion exchange, adsorption, electrolysis, biological treatment and the like. Among the above methods, the adsorption method is widely used for the separation of noble metals because of its advantages such as low running cost, simple operation, little environmental impact, and easy industrialization.
The research utilizes zinc nitrate hexahydrate and 3-amino-5-mercapto-1, 2, 4-triazole to prepare a novel metal organic framework material Zn-AMT, and utilizes N and S exposed on the surface of the novel metal organic framework material as adsorption sites to show high-efficiency selective adsorption to Au (III) in an aqueous solution.
Disclosure of Invention
The invention aims to provide a preparation method of N, S-containing metal organic framework material with excellent adsorption performance on Au (III) in aqueous solution, and the material has high adsorption capacity, rapid adsorption rate, high selectivity and high recycling performance on Au (III). The technical scheme adopted by the invention is as follows:
a certain amount of Zn (NO)3)2·6H2Adding O and 3-amino-5-mercapto-1, 2, 4-triazole into a DMF (dimethyl formamide) and water mixed solvent, heating and reacting for a period of time in a closed manner at a certain temperature, cooling the reaction liquid to room temperature, and then carrying out suction filtration, washing and drying to obtain the Zn-AMT. Adopting Zn-AMT as adsorbent to adsorb and separate Au (III) in water solution, preparing Au (III) solution with certain concentration by using gold trichloride with the purity of 98%, and using 0.1mol/L sodium hydroxide or HNO3After the pH value of the aqueous solution is adjusted, a certain volume of the aqueous solution is added into a centrifuge tube, a certain amount of Zn-AMT is added as an adsorbent, the aqueous solution is placed in a constant-temperature water bath oscillator at a certain temperature and fully stirred for a certain time, after adsorption is completed, a certain amount of samples are taken, the concentrations of the original solution and the residual solution after adsorption are measured by an atomic absorption spectrometer, and the adsorption amount and the adsorption rate are calculated. Adding a certain volume of thiourea solution into a 50mL centrifuge tube for desorptionAdding 5mg of adsorbed Zn-AMT material, placing in a constant-temperature water bath oscillator at 15-55 ℃ for oscillating desorption for 0-45h, taking out a centrifuge tube for centrifugal separation, and adsorbing the desorbed Zn-AMT material again;
preferably, the volume ratio of the mixed solvent DMF and the water for preparing the material is 1:3-3: 1;
preferably Zn (NO)3)2·6H2The molar ratio of O to 3-amino-5-mercapto-1, 2, 4-triazole is 1:2-1: 5;
preferably, the molar concentration of the 3-amino-5-mercapto-1, 2, 4-triazole is 0.03-0.1 mol/L;
preferably, the reaction temperature is 110-180 ℃, and the synthesis time is 12-72 h;
preferably, the concentration of the prepared Au (III) solution is 0-2000 mg/L;
preferably, the pH of the solution is set to 1-6;
preferably, the adsorption temperature is 15-80 ℃;
preferably, the adsorption time is 0-2880 min;
preferably, the concentration of the thiourea solution is more than 0.2 mol/L.
Compared with the prior art, the invention has the following advantages:
(1) the metal organic framework material containing functional atoms N and S is prepared by adopting a one-step method, the reaction solvent is green, the reaction temperature is moderate, and the raw material cost is low. (2) Zn-AMT can effectively adsorb Au (III) ions in the aqueous solution, the adsorption amount is up to 2878mg/g, and the adsorption amount of the material can be continuously increased by increasing the temperature. (3) The Zn-AMT material is easy to elute and can be repeatedly recycled after desorption, thereby being a saving material and bringing higher economic benefit. (4) The Zn-AMT material has better selectivity to Au (III), which is beneficial to the selective adsorption of trivalent gold ions in the complex practical solution.
[ detailed description ] according to the present embodiment
Example 1
Adding 600mg of zinc nitrate hexahydrate (2 mmol) and 700mg of 3-amino-5-mercapto-1, 2, 4-triazole (6 mmol) into a 250mL beaker, adding a mixed solvent containing 100mL of DMF and 50mL of water, and stirring until the mixture is completely dissolved; the solution was transferred to a reaction vessel which had been preheated to 140 ℃ and reacted at 140 ℃ for 12-72 hours. After the reaction is finished, cooling to room temperature, performing suction filtration to obtain solid powder, washing with DMF (dimethyl formamide), deionized water and an anhydrous methanol solvent for multiple times, and performing suction filtration; the solid was dried overnight in a vacuum oven at 80 ℃ and ground to give Zn-AMT as a white powder.
Example 2
Preparing Au (III) solution with the concentration of 10.9mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in the example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating and adsorbing, setting the temperature to be 25 ℃, performing fixed-point sampling detection, measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, and after 20min, obtaining the adsorption capacity of 43.6mg/g and the adsorption rate of 100%.
Example 3
Preparing Au (III) solution with the concentration of 10.9mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in the example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating adsorption, setting the temperature to be 25 ℃, taking a certain amount of sample after 8min, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 41.1mg/g, and the adsorption rate is 94.2%.
Example 4
Preparing Au (III) solution with the concentration of 10.9mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in the example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating adsorption, setting the temperature to be 25 ℃, taking a certain amount of sample after 2min, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 30.4mg/g, and the adsorption rate is 49.7%.
Example 5
Preparing Au (III) solution with the concentration of 93mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in the example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating and adsorbing, setting the temperature to be 25 ℃, taking a certain amount of sample after 30min, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 372.6mg/g, and the adsorption rate is 100%.
Example 6
Preparing Au (III) solution with the concentration of 243.7mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in the example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating and adsorbing, setting the temperature to be 25 ℃, after 4.5 hours, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 939mg/g, and the adsorption rate is 96.3%.
Example 7
Preparing an Au (III) solution with the concentration of 89mg/L by using gold trichloride with the purity of 98%, adding 20mL of the Au (III) solution into a 50mL centrifuge tube, adjusting the pH to 5.22 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating adsorption, setting the temperature to be 25 ℃, after 18 hours, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 343mg/g, and the adsorption rate is 96%.
Example 8
Preparing an Au (III) solution with the concentration of 89mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 7.57 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating and adsorbing, setting the temperature to be 25 ℃, after 18h, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 193.4mg/g, and the adsorption rate is 54.2%.
Example 9
Preparing Au (III) solution with the concentration of 5 mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in the example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating and adsorbing, setting the temperature to be 25 ℃, after 48 hours, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 20mg/g, and the adsorption rate is 100%.
Example 10
Preparing Au (III) solution with the concentration of 58mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in the example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating and adsorbing, setting the temperature to be 25 ℃, after 48 hours, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 232mg/g, and the adsorption rate is 100%.
Example 11
Preparing Au (III) solution with the concentration of 105 mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating adsorption, setting the temperature to be 25 ℃, after 48 hours, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 419.2mg/g, and the adsorption rate is 99.6%.
Example 12
Preparing an Au (III) solution with the concentration of 292.7mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in the example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating adsorption, setting the temperature to be 25 ℃, after 48 hours, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 1154.6mg/g, and the adsorption rate is 98.6%.
Example 13
Preparing an Au (III) solution with the concentration of 965.1mg/L by using gold trichloride with the purity of 98%, adding 20mL of the Au (III) solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in the embodiment 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating and adsorbing, setting the temperature to be 25 ℃, and after 48 hours, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 2040.2mg/g, and the adsorption rate is 52.8%.
Example 14
Preparing an Au (III) solution with the concentration of 1021mg/L by using gold trichloride with the purity of 98%, adding 20mL of the Au (III) solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating adsorption, setting the temperature to be 15 ℃, after 48 hours, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 1317mg/g, and the adsorption rate is 32.2%.
Example 15
Preparing an Au (III) solution with the concentration of 1021mg/L by using gold trichloride with the purity of 98%, adding 20mL of the solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating adsorption, setting the temperature to 35 ℃, after 48 hours, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 2605mg/g, and the adsorption rate is 63.8%.
Example 16
Preparing an Au (III) solution with the concentration of 1021mg/L by using gold trichloride with the purity of 98%, adding 20mL of the Au (III) solution into a 50mL centrifuge tube, adjusting the pH to 3.19 by using 0.1mol/L NaOH, adding 5mg of Zn-AMT material obtained in example 1 as an adsorbent, placing the solution into a constant-temperature water bath oscillator for oscillating adsorption, setting the temperature to be 42 ℃, after 48 hours, taking a certain amount of sample, and measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, wherein the adsorption amount is 2878mg/g, and the adsorption rate is 70.4%.
Example 17
5mg of Zn-AMT material is added into 20mL of mixed solution containing Au (III), Ni (II), Zn (II), Cu (II), Cd (II) and Co (II) ions with the concentration of 100mg/L and the pH value of 3.19, the mixed solution is shaken in a constant-temperature water bath shaker at the temperature of 25 ℃ for 24 hours, and after filtration by a microporous filter membrane, the absorbance of each ion solution before and after adsorption is measured by an atomic absorption spectrophotometer. In this example, the material adsorbed Au (III) in an amount of 400mg/g, and hardly adsorbed other coexisting metal ions.
Example 18
Adding 20mL of 0.5mol/L thiourea aqueous solution into a 50mL centrifuge tube as a desorption agent, adding 5mg of the adsorbed Zn-AMT material, placing the mixture in a constant-temperature water bath oscillator for oscillating desorption at the set temperature of 25 ℃, filtering and drying after 24 hours, and adsorbing the desorbed Zn-AMT material again. After repeated use for 3 times, the adsorption performance is only reduced by 4 percent.
The above examples merely express several embodiments of the present invention, and the description thereof is more specific and detailed, but the technical scope thereof is not limited to the above embodiments. It will be apparent to those skilled in the art that various modifications and embodiments can be made without departing from the spirit of the invention, and these are within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of N, S-containing metal organic framework material Zn-AMT and a method for applying the same to absorb Au (III) in aqueous solution are characterized in that a certain amount of Zn (NO) is added3)2·6H2Adding O and 3-amino-5-mercapto-1, 2, 4-triazole into a DMF (dimethyl formamide) and water mixed solvent, heating and reacting for a period of time in a closed manner at a certain temperature, cooling the reaction liquid to room temperature, and then carrying out suction filtration, washing and drying to obtain Zn-AMT; adopting Zn-AMT as adsorbent to adsorb and separate Au (III) in water solution, preparing Au (III) solution with certain concentration by using gold trichloride with the purity of 98%, and using 0.1mol/L sodium hydroxide or HNO3After the pH value of the aqueous solution is adjusted, adding a certain volume of the aqueous solution into a centrifuge tube, adding a certain amount of Zn-AMT (zinc-ammonium mechanical Transmission) serving as an adsorbent, placing the aqueous solution into a constant-temperature water bath oscillator at a certain temperature, fully stirring the aqueous solution for a certain time, taking a certain amount of sample after adsorption is finished, measuring the concentrations of the original solution and the residual solution after adsorption by using an atomic absorption spectrometer, and calculating the adsorption amount and the adsorption rate; a certain volume of thiourea solution was added into a 50mL centrifuge tubeAdding 5mg of adsorbed Zn-AMT material as a desorption agent, placing the desorption agent in a 15-55 ℃ constant-temperature water bath oscillator for oscillating desorption for 0-45h, taking out a centrifuge tube for centrifugal separation, and adsorbing the desorbed Zn-AMT material again.
2. The method of claim 1, wherein the material is prepared by using a volume ratio of the mixed solvent DMF and water of 1:3-3: 1.
3. The method of claim 1, wherein Zn (NO)3)2·6H2The molar ratio of O to 3-amino-5-mercapto-1, 2, 4-triazole is 1:2-1: 5.
4. The method of claim 1, wherein the molar concentration of 3-amino-5-mercapto-1, 2, 4-triazole is 0.03-0.1 mol/L.
5. The method as claimed in claim 1, wherein the reaction temperature is 110-180 ℃ and the synthesis time is 12-72 h.
6. The method of claim 1, wherein the Au (III) solution is prepared at a concentration of 0-2000 mg/L.
7. The method of claim 1, wherein the pH of the solution is set to 1 to 6.
8. The process of claim 1, wherein the adsorption temperature is 15 to 80 ℃.
9. The process according to claim 1, wherein the adsorption time is from 0 to 2880 min.
10. The method of claim 1, wherein the thiourea solution has a concentration of greater than 0.2 mol/L.
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| CN104151335A (en) * | 2014-08-01 | 2014-11-19 | 南开大学 | MOFs (Metal-Organic Frameworks) with ph stability as well as preparation method and application of MOFs |
| CN107442078A (en) * | 2017-03-16 | 2017-12-08 | 浙江工商大学 | Novel color-changing fiber AMTF PAR preparation and application |
| CN108559098A (en) * | 2018-05-11 | 2018-09-21 | 西北大学 | A kind of metal organic framework compound and preparation method and application |
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