CN113289690A - Pd/UiO-66 catalyst and preparation method and application thereof - Google Patents
Pd/UiO-66 catalyst and preparation method and application thereof Download PDFInfo
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- CN113289690A CN113289690A CN202110716915.2A CN202110716915A CN113289690A CN 113289690 A CN113289690 A CN 113289690A CN 202110716915 A CN202110716915 A CN 202110716915A CN 113289690 A CN113289690 A CN 113289690A
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- 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
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
- B01J31/2239—Bridging ligands, e.g. OAc in Cr2(OAc)4, Pt4(OAc)8 or dicarboxylate ligands
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- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
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- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/40—Complexes comprising metals of Group IV (IVA or IVB) as the central metal
- B01J2531/48—Zirconium
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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Abstract
The invention relates to a preparation method and application of a Pd/UiO-66 catalyst, wherein the catalyst uses a zirconium-based metal organic framework UiO-66 as a carrier to load metal palladium, the loaded catalyst is subjected to reduction of the metal palladium by sodium borohydride to form palladium atoms entering pores of the UiO-66, the zirconium-based metal organic framework UiO-66 is prepared by reaction of 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%. 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, selective catalytic reduction of nitrogen oxides, catalytic oxidation of toluene, phenol hydrogenation reaction and the like.
Description
Technical Field
The invention belongs to the field of catalytic materials, and particularly relates to a Pd/UiO-66 catalyst, and a preparation method and application thereof.
Background
With the development of modern industry, environmental pollution is becoming more and more serious, and the prevention of environmental pollution has become a major issue related to the nation's county. Heavy metal pollutants have become one of the main sources of water body pollution, and Cr (VI) is one of the heavy metal pollutants. Cr (VI) has been proved to be an extremely harmful toxic substance, has high solubility in water, strong migration ability, mutagenicity and carcinogenicity. Studies have shown that the toxicity of Cr (VI) is about 100 times that of Cr (III) because of its great solubility and flowabilityThe result is. Cr (III) is absorbed to a very low extent in the human intestinal tract, and although a large amount of Cr (III) is a trace element essential for life, it is dangerous for human sensitization. Human beings need Cr (III) to maintain normal sugar metabolism, and lack of Cr (III) causes diseases such as hyperlipidemia, hypercholesterolemia and diabetes. In addition, Cr (III) has a weak migration ability and can form a hydroxide of Cr (III) (Cr (OH))3pKap = 30.2) to precipitate.
A Metal-Organic framework compound (MOFs for short) is a highly ordered low-density crystal material with an infinitely expanded network structure, which is formed by self-assembly and connection of transition Metal ions and Organic ligands through coordination bonds, and is a novel porous material. Over the past decade, research on MOFs has advanced greatly and has gained important applications in the fields of catalysis and adsorption. Among various MOFs, the structure of the UiO series compound has very good thermal stability, and meanwhile, the UiO series compound has the advantages of structural diversity, adjustable pore volume, functional pore channels and the like, and has attracted extensive attention of researchers.
Commonly used noble metal nanocatalysts can be divided into two broad categories: noble metal nanopowder catalysts and supported noble metal nanoparticle catalysts. Currently, the MOFs supported noble metal nano-catalyst can be applied to a series of catalytic reactions, such as hexavalent chromium catalytic reduction, selective catalytic reduction of nitrogen oxides, catalytic oxidation of toluene, and catalysis of phenol hydrogenation reaction.
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 an impregnation 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 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 hexavalent chromium catalytic reduction, nitrogen oxide selective catalytic reduction, toluene catalytic oxidation, phenol hydrogenation reaction and other catalysis 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 selective catalytic reduction of nitrogen oxides, 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.
The method uses a metal organic framework as a carrier to load noble metal Pd, and uses formic acid as a hydrogen source, so that the catalyst has high stability and catalytic performance under a very low load.
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 transmission electron micrograph of Pd/UiO-66 and original UiO-66 (a) prepared in example 1 (b), example 10 (c) and example 11 (d) of the present invention.
From FIG. 1, it can be seen that the Pd @ UiO-66 catalyst prepared by the present invention is 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.
As can be seen from FIG. 2, the UiO-66 material has regular morphology, tends to be spherical as a whole, and has a size of about 50 nm; the TEM surface appearance of the Pd @ UiO-66 after being compared and loaded is not changed; from the TEM of Pd @ UiO-66, it can be seen that Pd nanoparticles are supported on the surface of UiO-66.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
Weighing 0.1623 g of terephthalic acid, placing the terephthalic acid in a beaker, weighing 50 mL of N, N-dimethylformamide solution, placing the N, N-dimethylformamide solution in the beaker, and carrying out ultrasonic dissolution; 0.2332 g of zirconium chloride is weighed and ultrasonically dissolved in the solution, then 1 mL 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 24 h 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 12 h, and the zirconium-based metal organic framework is obtained.
0.3 g of UiO-66 is weighed and ultrasonically dispersed in 30 mL of methanol, and 10 mg of palladium chloride is weighed and ultrasonically dissolved in 3 mL of deionized water; dropwise adding the chloropalladate solution into the UiO-66 suspension, and stirring for 10 hours; weighing 0.064 g of sodium borohydride and dissolving in 5 mL of methanol; dropwise adding the sodium borohydride solution into the UiO-66 suspension, and continuously stirring for 10 h. After the reaction is finished, the mixed solution is centrifuged, washed with ethanol for three times, and dried in an oven at 60 ℃ for 12 hours to obtain the Pd/UiO-66 catalyst.
The activity evaluation of the catalyst is carried out in a self-made reactor, the amount of the catalyst is 4 mg, the molar concentration of pollutants is 3.22 mM, the volume of a reaction solution is 50 mL, the pH value is adjusted to be 2 by using sulfuric acid, and the addition amount of formic acid is 1.50 mL; after reacting for 60 min, the pollutant concentration is analyzed by an ultraviolet-visible spectrophotometer. The activity test shows that 2% Pd/UiO-66 of the Pd-based catalyst prepared by the method and taking UiO-66 as a precursor is subjected to sodium borohydride reduction treatment, formic acid is taken as a hydrogen source, Cr (VI) can be completely reduced to Cr (III) within 50 min, the conversion rate is 100%, and the structure of the catalyst is not changed after the catalyst is used.
Example 2
According to the preparation method of the invention in example 1, the amount of formic acid added was changed to 0.50 mL. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 2% Pd/UiO-66 prepared by the method can reduce Cr (VI) to Cr (III) in 60 min after reduction treatment by sodium borohydride, the conversion rate is 69.87%, and the structure of the catalyst is not changed after use.
Example 3
According to the preparation method of the invention in example 1, the amount of formic acid added was changed to 1.00 mL. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 2% Pd/UiO-66 prepared by the method can reduce Cr (VI) to Cr (III) in 60 min after reduction treatment by sodium borohydride, the conversion rate is 98.94%, and the structure of the catalyst is not changed after use.
Example 4
According to the preparation method of the invention in example 1, the amount of formic acid added was changed to 2.00 mL. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 2% Pd/UiO-66 prepared by the method can reduce Cr (VI) to Cr (III) within 50 min after reduction treatment by sodium borohydride, the conversion rate is 100%, and the structure of the catalyst is not changed after use.
Example 5
The preparation according to the invention of example 1 was followed, with sulfuric acid to adjust the pH = 6. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 2% Pd/UiO-66 prepared by the method can reduce Cr (VI) to Cr (III) in 60 min after reduction treatment by sodium borohydride, the conversion rate is 99.70%, and the structure of the catalyst is not changed after use.
Example 6
The preparation according to the invention of example 1 is carried out with sulfuric acid to adjust the pH = 10. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 2% Pd/UiO-66 prepared by the method can reduce Cr (VI) to Cr (III) in 60 min after reduction treatment by sodium borohydride, the conversion rate is 94.41%, and the structure of the catalyst is not changed after use.
Example 7
The preparation process according to the invention of example 1 was followed, the catalyst amount being 2 mg. The catalyst was evaluated in the same manner as in example 1. The activity test shows that after the 2% Pd/UiO-66 prepared by the method is subjected to sodium borohydride reduction treatment, formic acid is used as a hydrogen source to reduce Cr (VI) to Cr (III) within 60 min, the conversion rate is 82.30%, and the structure of the catalyst is not changed after the catalyst is used.
Example 8
The preparation process according to the invention of example 1 was followed, the catalyst amount being 6 mg. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 2% Pd/UiO-66 prepared by the method reduces Cr (VI) into Cr (III) in 30 min after reduction treatment by sodium borohydride, the conversion rate is 100%, and the structure of the catalyst is not changed after use.
Example 9
The preparation process according to the invention of example 1 was followed, the catalyst amount being 8 mg. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 2 percent Pd/UiO-66 prepared by the method is reduced by sodium borohydride
After the original treatment, Cr (VI) can be completely reduced into Cr (III) within 20 min, the Cr (VI) catalytic reduction effect is good, the conversion rate is 100%, and the structure of the catalyst is not changed after the catalyst is used.
Example 10
The preparation process of example 1 was followed, with varying amounts of Pd supported. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 1% Pd/UiO-66 prepared by the method reduces Cr (VI) into Cr (III) within 60 min after reduction treatment by sodium borohydride, the conversion rate is 74.53%, and the structure of the catalyst is not changed after use.
Example 11
The preparation process of example 1 was followed, with varying amounts of Pd supported. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 3% Pd/UiO-66 prepared by the method can completely reduce Cr (VI) into Cr (III) within 40 min after reduction treatment by sodium borohydride, has good Cr (VI) catalytic reduction effect, the conversion rate is 100%, and the structure of the catalyst is not changed after use.
Example 12
According to the preparation method of the invention in example 1, the molar concentration of the contaminant is 0.79 mM. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 2% Pd/UiO-66 prepared by the method can completely reduce Cr (VI) into Cr (III) within 30 min after reduction treatment by sodium borohydride, has good Cr (VI) catalytic reduction effect, the conversion rate is 100%, and the structure of the catalyst is not changed after use.
Example 13
According to the preparation method of the invention in example 1, the molar concentration of the contaminant is 1.56 mM. The catalyst was evaluated in the same manner as in example 1. The activity test shows that the 2% Pd/UiO-66 prepared by the method can completely reduce Cr (VI) into Cr (III) within 40 min after reduction treatment by sodium borohydride, has good Cr (VI) catalytic reduction effect, the conversion rate is 100%, and the structure of the catalyst is not changed after use.
Example 14
According to the preparation process of the invention of example 1, the molar concentration of the contaminant is 2.43 mM. Evaluation of catalyst
The procedure is as in example 1. The activity test shows that the 2% Pd/UiO-66 prepared by the method can completely reduce Cr (VI) into Cr (III) within 50 min after reduction treatment by sodium borohydride, has good Cr (VI) catalytic reduction effect, the conversion rate is 100%, and the structure of the catalyst is not changed after use.
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 ofDissolving terephthalic acid in N, N-dimethylformamide solution, dissolving a zirconium source in the solution, and then adding micromolecular acid into the mixed solution;transferring the obtained mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining for reaction to obtain a reactant;centrifuging, washing and drying the obtained reactant to obtain a zirconium-based metal organic framework UiO-66;dissolving a palladium source, loading the palladium source on a zirconium-based metal organic framework UiO-66 by an impregnation 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 and potassium borohydride.
- 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 sodium borohydride as a reducing agent to reduce metal Pd to Pd atoms after loading, and is used for catalysis of hexavalent chromium catalytic reduction, selective catalytic reduction of nitrogen oxides, catalytic oxidation of toluene, phenol hydrogenation reaction, and the like.
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Cited By (5)
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| CN113663736A (en) * | 2021-09-27 | 2021-11-19 | 长春工业大学 | Preparation and application of Pd/UiO-66 by strong electrostatic adsorption method |
| CN113694968A (en) * | 2021-09-27 | 2021-11-26 | 常州大学 | Palladium-loaded magnetic UiO-66 ternary composite catalytic material and preparation method and application thereof |
| CN115007210A (en) * | 2022-04-28 | 2022-09-06 | 华南理工大学 | Hollow UiO-66-NH 2 (MZr) packaging metal particle and preparation method and application thereof |
| CN115845843A (en) * | 2022-12-02 | 2023-03-28 | 桂林理工大学 | VOCs (volatile organic compounds) low-temperature oxidation catalyst with highly dispersed Pd component on cerium-zirconium-carbon porous composite carrier and preparation method thereof |
| CN116328833A (en) * | 2023-03-30 | 2023-06-27 | 南京工业大学 | Two-dimensional MOF supported nano palladium catalyst and preparation method and application thereof |
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| CN113694968A (en) * | 2021-09-27 | 2021-11-26 | 常州大学 | Palladium-loaded magnetic UiO-66 ternary composite catalytic material and preparation method and application thereof |
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| CN115007210A (en) * | 2022-04-28 | 2022-09-06 | 华南理工大学 | Hollow UiO-66-NH 2 (MZr) packaging metal particle and preparation method and application thereof |
| CN115007210B (en) * | 2022-04-28 | 2023-11-24 | 华南理工大学 | Hollow UiO-66-NH 2 (MZr) encapsulated metal particles, and preparation method and application thereof |
| CN115845843A (en) * | 2022-12-02 | 2023-03-28 | 桂林理工大学 | VOCs (volatile organic compounds) low-temperature oxidation catalyst with highly dispersed Pd component on cerium-zirconium-carbon porous composite carrier and preparation method thereof |
| CN116328833A (en) * | 2023-03-30 | 2023-06-27 | 南京工业大学 | Two-dimensional MOF supported nano palladium catalyst and preparation method and application thereof |
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