CN113663736A - Preparation and application of Pd/UiO-66 by strong electrostatic adsorption method - Google Patents
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Abstract
The invention relates to a preparation method and application of Pd/UiO-66 by a strong electrostatic adsorption method, wherein the catalyst uses a zirconium-based metal organic framework UiO-66 as a carrier to load metal palladium; the pH value of the reaction solution is adjusted by hydrochloric acid and ammonia water to positively charge the surface of the UiO-66 carrierCharged, capable of strongly adsorbing negatively charged [ PdCl6]2‑(ii) a The strong interaction of the metal complex and the surface of the carrier enables the Pd to have higher dispersity and smaller Pd nano-particles. The molar ratio of the zirconium element to the organic ligand is 1:1, and the loading capacity of the palladium element is 1% -3%. Compared with the prior art, the catalyst has high hydrothermal stability, high specific surface area and high catalytic performance, and can be applied to catalysis of hexavalent chromium catalytic reduction, bromate catalytic reduction, toluene catalytic oxidation, phenol hydrogenation reaction and the like.
Description
Technical Field
The invention belongs to the field of catalytic materials, and particularly relates to preparation and application of Pd/UiO-66 by a strong electrostatic adsorption method.
Background
The chromium element is present in various media of the environment in different forms, mainly in the form of hexavalent chromium cr (vi) and trivalent chromium cr (iii). Chromium pollution refers to pollution caused by chromium and its compounds in the environment. The natural sources of chromium are mainly rock efflorescence, gradual release of mineral rocks, which releases trivalent chromium mainly in the form of chromite. The artificial source of chromium is used as the main aspect of chromium pollution and mainly consists of industrial behaviors of waste water and waste gas discharged by industrial production such as extraction, smelting, chromium plating parts of metal parts, leather preparations, industrial pigments and the like. Chromium in wastewater exists mainly in the form of positive hexavalent chromium (cr (vi)). Cr (VI) is mainly CrO3Chromate (CrO)4 2-) And dichromate (Cr)2O7 2-) In the form of (1), wherein Cr is2O7 2-Most commonly.
The electrostatic view of the adsorption of metals to the support surface may in many cases not only provide a simple and effective basis for the practical aspects of catalyst preparation, but also may serve as a starting point for rational catalyst design. Since the surface of the support contains terminal hydroxyl groups, the terminal hydroxyl groups are protonated or deprotonated depending on the acidity of the impregnation solution. The pH value at which the hydroxyl groups are totally neutral is called the Point of Zero Charge (PZC). Below this pH, the hydroxyl groups are protonated and positively charged and the surface can adsorb anionic metal complexes, such as hexachloroplatinate [ PtCl ]6]2-(commonly referred to as CPA because it is derived from chloroplatinic acid). Above PZC, the hydroxyl group is deprotonated and negatively charged, cations such as tetraamineplatinum (PTA), [ (NH)3)4Pt]2+Is strongly adsorbed.
Thus, the overall idea of strong electrostatic adsorption is to control the ph of the excess liquid to achieve the optimum ph for the strongest metal complex-surface interaction.
Disclosure of Invention
The invention aims to solve the problems and provide a preparation method and application of a Pd/UiO-66 catalyst.
The invention also aims to provide the application of the Pd/UiO-66 catalyst in the reaction of catalyzing the reduction of Cr (VI) into Cr (III).
In order to achieve the purpose, the invention adopts the following technical scheme.
A preparation method of the Pd/UiO-66 catalyst, which comprises the following steps:
(1) dissolving terephthalic acid in N, N-dimethylformamide solution, dissolving a zirconium source in the solution, and then adding micromolecular acid into the mixed solution;
(2) transferring the obtained mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining for reaction to obtain a reactant;
(3) centrifuging, washing and drying the obtained reactant to obtain a zirconium-based metal organic framework UiO-66;
(4) dissolving a palladium source, loading the palladium source on a zirconium-based metal organic framework UiO-66 by a strong electrostatic adsorption method, and then reducing metal palladium into palladium atoms by using a reducing agent to obtain the catalyst Pd/UiO-66.
Preferably, the molar ratio of the zirconium source to the terephthalic acid is 1:1, and the loading amount of the palladium element is 1% -3%.
Preferably, the molar ratio of small molecule acid to terephthalic acid is 6.4: 1.
Preferably, the small molecular acid is one or more of acetic acid, hydrochloric acid or formic acid.
Preferably, the solvent in step (1) is one or more of ethanol, N-dimethylformamide, N-dimethylacetamide or ethylene glycol.
Preferably, the reaction temperature in the step (2) is 110-140 ℃, and the reaction time is 12-36 h.
Preferably, the washing is performed three times with N, N-dimethylformamide and then three times with methanol.
The invention also protects the Pd/UiO-66 catalyst prepared by the preparation method.
It is worth to be noted that the application of the Pd/UiO-66 catalyst in catalysis of hexavalent chromium catalytic reduction, bromate catalytic reduction, toluene catalytic oxidation, phenol hydrogenation reaction and the like is also within the protection scope of the invention.
The invention has the beneficial effects that the catalyst adopts a metal organic framework structure, the material structure is controllable and adjustable, and the catalyst not only has high hydrothermal stability, but also has a large specific surface area.
The zirconium-based metal organic framework UiO-66 Pd-loaded catalyst synthesized by the solvothermal method can not only catalyze the reduction of Cr (VI) into Cr (III), but also maintain high stability. In addition, the catalyst can be used as a catalyst for catalytic reduction of bromate, catalytic oxidation of toluene, hydrogenation of phenol, and the like.
The method has simple preparation process and equipment, good repeatability and good industrial application prospect.
Drawings
FIG. 1 is an IR spectrum of UiO-66 and Pd/UiO-66 prepared in example 1 of the present invention.
FIG. 2 is a sample plot of UiO-66 and Pd/UiO-66 prepared in example 1 of the present invention.
FIG. 3 is a diagram of PZC of UiO-66 prepared by example 1 of the invention.
From FIG. 1 it can be seen that the Pd/UiO-66 catalyst prepared by the present invention, at 1580cm-1And 1400cm-1Is OCO asymmetric and symmetric stretching vibration of terephthalic acid, 1504cm-1Vibration of C = C in benzene ring, 811cm-1、746cm-1And 705cm-1The peak in the vicinity of (A) was a mixed region of C-H, C = C stretch and COC bond in terephthalic acid, 663cm-1And 485cm-1Is Zr6Zr-O in clustersμ3-O and Zr-Oμ3Stretching vibration of-OH, basically consistent with literature reports. It can be seen that the position of the UiO-66 peak is unchanged and the structure is kept intact after the Pd nanoparticles are loaded.
It can be seen from FIG. 2 that the UiO-66 sample is white and the sample after loading Pd is grey black.
From FIG. 3, it can be seen that the PZC of the UiO-66 sample is 3.70.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1 0.1623g of terephthalic acid was weighed and placed in a beaker, 50mL of an N, N-dimethylformamide solution was weighed and placed in the beaker, and dissolved by ultrasound; 0.2332g of zirconium chloride is weighed and ultrasonically dissolved in the solution, then 1mL of 36% acetic acid is added, the mixed solution is placed in a reaction kettle with a polytetrafluoroethylene lining, sealed and placed in a drying oven to be heated for 24h at 120 ℃, then the solution is centrifuged, washed with N, N-dimethylformamide for three times, washed with methanol for three times, and dried in the drying oven at 100 ℃ for 12h, and the zirconium-based metal organic framework is obtained.
Weighing 20mg of palladium chloride, adding into 30mL of distilled water, dissolving by ultrasonic treatment for 20min, adding 0.6g of UiO-66, adjusting the pH value to 3 by using hydrochloric acid, and stirring for 12 h; filtering with 0.45um filter membrane, washing with distilled water to neutrality, calcining in muffle furnace at 200 deg.C for 4 hr, and reducing with hydrogen at 200 deg.C for 4 hr.
The activity evaluation of the catalyst is carried out in a self-made reactor; the catalytic hydrogenation reduction reaction of Cr (VI) is carried out in a 500mL three-necked flask, and the reaction temperature is controlled at 25 ℃ by using a thermostatic water bath. 40mL of 21.20 mM potassium dichromate and 360mL of water were added to a three-necked flask, the pH was adjusted to 2 with sulfuric acid, and 8mg of the catalyst was added to the three-necked flask. Introducing nitrogen (flow rate of 200 mL/min), and magnetically stirring for 30min to remove oxygen in the solution; thereafter, the intake air is switched to H2The catalytic reaction is started (the flow is 200 mL/min), the timing is started, samples are taken at certain time intervals, the samples are filtered by a filter membrane with the diameter of 0.45 mu m, and the pollutant concentration is analyzed by an ultraviolet-visible spectrophotometer after the reaction is carried out for 60 min. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can completely reduce Cr (VI) into Cr (III) within 60min, the conversion rate is 100%, and the structure of the catalyst is not changed after the catalyst is used.
Example 2 the process of the invention of example 1 was followed, the pH of the reaction solution was adjusted to 1 with sulfuric acid, and the catalyst was evaluated in the same manner as in example 1. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can completely reduce Cr (VI) into Cr (III) within 40min, the conversion rate is 100%, and the structure of the catalyst is not changed after the catalyst is used.
Example 3 the process of the invention of example 1 was followed to adjust the pH of the reaction solution to 2.50 with sulfuric acid and evaluate the catalyst in the same manner as in example 1. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can reduce Cr (VI) into Cr (III) within 60min, the conversion rate is 11%, and the structure of the catalyst is not changed after the catalyst is used.
Example 4 the preparation process of the invention of example 1 was followed with a catalyst amount of 4 mg. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can reduce Cr (VI) into Cr (III) within 60min, the conversion rate is 95%, and the structure of the catalyst is not changed after the catalyst is used.
Example 5 the preparation process of the invention according to example 1 was followed, the catalyst amount being 16 mg and the catalyst being evaluated in the same manner as in example 1. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can completely reduce Cr (VI) into Cr (III) within 40min, the conversion rate is 100%, and the structure of the catalyst is not changed after the catalyst is used.
Example 6 the preparation process of the invention according to example 1 was followed, the catalyst amount being 24 mg and the catalyst being evaluated in the same manner as in example 1. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can completely reduce Cr (VI) into Cr (III) within 30min, the conversion rate is 100%, and the structure of the catalyst is not changed after the catalyst is used.
Example 7 the procedure of the invention of example 1 was followed to evaluate the catalyst by varying the Pd loading to 1% as in example 1. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can reduce Cr (VI) into Cr (III) within 60min, the conversion rate is 90 percent, and the structure of the catalyst is not changed after the catalyst is used.
Example 8 the procedure of the invention of example 1 was followed with a change in Pd loading of 3% and the catalyst evaluated in the same manner as in example 1. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can completely reduce Cr (VI) into Cr (III) within 40min, the conversion rate is 100%, and the structure of the catalyst is not changed after the catalyst is used.
Example 9 the process of the invention of example 1 was followed to evaluate the catalyst at a molar contaminant concentration of 0.55 mM as in example 1. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can completely reduce Cr (VI) into Cr (III) within 30min, the conversion rate is 100%, and the structure of the catalyst is not changed after the catalyst is used.
Example 10 the process of the invention of example 1 was followed to evaluate a catalyst having a molar concentration of contaminants of 1.04 mM and the same procedure as in example 1. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can completely reduce Cr (VI) into Cr (III) within 40min, the conversion rate is 100%, and the structure of the catalyst is not changed after the catalyst is used.
Example 11 the process of the invention of example 1 was followed to evaluate a catalyst having a molar concentration of contaminants of 1.63 mM and the same procedure as in example 1. The activity test shows that the Pd/UiO-66 catalyst prepared by the method can completely reduce Cr (VI) into Cr (III) within 50min, the conversion rate is 100%, and the structure of the catalyst is not changed after the catalyst is used.
Example 12 the process of example 1 was followed to prepare a catalyst preparation solution having a pH of 2 adjusted with hydrochloric acid, and the catalyst was evaluated in the same manner as in example 1. The activity test shows that the prepared Pd/UiO-66 catalyst can reduce Cr (VI) into Cr (III) within 60min, the conversion rate is 79 percent, and the structure of the catalyst is not changed after the catalyst is used.
Example 13 the process of the invention of example 1 was followed to adjust the catalyst preparation solution to pH 5 with ammonia, and the catalyst was evaluated in the same manner as in example 1. The activity test shows that the prepared Pd/UiO-66 catalyst can reduce Cr (VI) into Cr (III) within 60min, the conversion rate is 60 percent, and the structure of the catalyst is not changed after the catalyst is used.
Claims (9)
- The Pd/UiO-66 catalyst is characterized in that metal palladium is loaded on the catalyst by taking a zirconium-based metal organic framework UiO-66 as a carrier, the zirconium-based metal organic framework UiO-66 is prepared by reacting an organic ligand and a zirconium element, the molar ratio of the zirconium element to the organic ligand is 1:1, and the loading amount of the palladium element is 1% -3%.
- 2. The process for preparing the Pd/UiO-66 catalyst as claimed in, wherein the process comprises the steps of(1) Dissolving terephthalic acid in N, N-dimethylformamide solution, dissolving a zirconium source in the solution, and then adding micromolecular acid into the mixed solution;(2) transferring the obtained mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining for reaction to obtain a reactant;(3) centrifuging, washing and drying the obtained reactant to obtain a zirconium-based metal organic framework UiO-66;(4) dissolving a palladium source, loading the palladium source on a zirconium-based metal organic framework UiO-66 by a strong electrostatic adsorption method, and then reducing metal palladium into palladium atoms by using a reducing agent to obtain the catalyst Pd/UiO-66.
- 3. A method of preparing the Pd/UiO-66 catalyst of claim 2 wherein the zirconium source of step (1) is one of zirconium chloride or zirconium oxychloride.
- 4. The method for preparing the Pd/UiO-66 catalyst as claimed in claim 2, wherein the solvent in step (1) is one or more of ethanol, N-dimethylformamide, N-dimethylacetamide and ethylene glycol.
- 5. The method for preparing the Pd/UiO-66 catalyst as claimed in claim 2, wherein the small-molecule acid in step (1) is one or more of acetic acid, hydrochloric acid and formic acid.
- 6. The preparation method of the Pd/UiO-66 catalyst as claimed in claim 2, wherein the reaction temperature in the step (2) is 110-140 ℃, and the reaction time is 12-36 h.
- 7. The method for preparing the Pd/UiO-66 catalyst as claimed in claim 2, wherein the reducing agent in step (4) is one or more of sodium borohydride, ascorbic acid, potassium borohydride or hydrogen.
- 8. A method for preparing the Pd/UiO-66 catalyst according to claim 2, wherein the palladium source in step (4) is one of palladium nitrate, palladium sulfate or palladium chloride.
- 9. The method for preparing the Pd/UiO-66 catalyst as claimed in claim 1, wherein the catalyst uses hydrogen as a reducing agent to reduce metallic Pd to Pd atoms after loading, and is used for catalysis of hexavalent chromium catalytic reduction, bromate catalytic reduction, toluene catalytic oxidation, phenol hydrogenation reaction, etc.
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