CN110227455B - Preparation method of two-dimensional layered glycerol oxidation nano catalyst - Google Patents
Preparation method of two-dimensional layered glycerol oxidation nano catalyst Download PDFInfo
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- CN110227455B CN110227455B CN201910558073.5A CN201910558073A CN110227455B CN 110227455 B CN110227455 B CN 110227455B CN 201910558073 A CN201910558073 A CN 201910558073A CN 110227455 B CN110227455 B CN 110227455B
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/23—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of oxygen-containing groups to carboxyl groups
- C07C51/235—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of oxygen-containing groups to carboxyl groups of —CHO groups or primary alcohol groups
Abstract
The invention relates to a preparation method of a novel two-dimensional layered glycerol oxidation nano-catalyst. The two-dimensional layered glycerol oxidation nano-catalyst is prepared by preparing two-dimensional cerium dioxide from graphene oxide and then loading gold nanoparticles, and has the advantages of high product selectivity and catalytic activity, novel structure, simple preparation process, greenness, safety, wide application prospect and great significance in deep research.
Description
Technical Field
The invention relates to a preparation method of a two-dimensional layered glycerol oxidation nano catalyst.
Background
The contradiction between energy crisis and economic development is increasingly prominent, the current biomass diesel is an ideal substitute of fossil fuel, and the biomass diesel has wide sources, high combustion heat value and small environmental pollution and can be produced in large scale, so the biomass diesel has wide application prospect and economic market. However, a large amount of glycerin byproducts are inevitably generated in the production process of the biodiesel, and the accumulation of the byproducts not only causes energy waste, but also limits the popularization and use of the biodiesel. Glycerol is an important basic raw material in the chemical industry, and a product with higher economic benefit can be obtained through a series of different catalytic reactions, wherein the selective oxidation of glycerol has important research significance, and the search for a novel efficient catalyst is important. The current selective oxidation catalyst for glycerin mainly uses activated carbon, carbon nano tubes, alumina and partial non-metallic mineral materials as carriers, and the overall catalytic effect is poor due to the fact that the reaction process is variable and complex and the reaction products are various. Therefore, the search for a novel catalyst with high efficiency, stronger universality and higher selectivity becomes the key point for determining the development of selective oxidation of the glycerol.
Disclosure of Invention
The invention provides a preparation method of a two-dimensional layered glycerol oxidation nano-catalyst aiming at the defects of various glycerol selective oxidation products, low conversion rate and the like.
A preparation method of a two-dimensional layered glycerol oxidation nano-catalyst comprises the following steps:
s1: and (3) fully and violently mixing the cerium nitrate ethanol solution with the KIT-6/G template, and drying, calcining and the like to obtain the cerium dioxide and KIT-6/G composite material.
S2: and mixing and heating the prepared cerium dioxide and KIT-6/G composite material and a certain amount of strong alkali solution to prepare the graphene-supported two-dimensional ordered layered cerium dioxide carrier.
S3: gold nanoparticles are loaded on the surface of a graphene-supported two-dimensional layered ordered cerium dioxide carrier by a sol method, so that the gold-supported two-dimensional cerium dioxide glycerol selective oxidation catalyst is obtained.
The mass ratio of the active metal to the composite cerium dioxide carrier can be 1-5%.
Compared with the prior preparation technology of the glycerol selective oxidation catalyst, the gold nanoparticle-loaded two-dimensional layered ordered cerium dioxide catalyst is a catalyst with novel structure and good product selectivity.
Drawings
Figure 1 is a TEM image of a two-dimensional layered ordered ceria support according to the invention.
FIG. 2 is an X-ray powder diffraction pattern of gold nanoparticles of the present invention supported on two-dimensional layered ordered ceria for use in a selective oxidation catalyst for glycerol.
Fig. 3 is a TEM image of gold nanoparticles of the present invention supported on two-dimensional layered ordered ceria for a glycerol selective oxidation catalyst.
Fig. 4 is a product distribution diagram of gold nanoparticles of the present invention supported on two-dimensional layered ordered ceria for selective oxidation of glycerol.
Detailed Description
Example 1 graphene oxide was prepared using an oxidation process.
Compounding graphene oxide and mesoporous silicon to construct a two-dimensional layered graphene-mesoporous silicon precursor.
Dissolving 0.5 g of cerium nitrate in 3 mL of ethanol solution, mixing with 0.2 g of graphene-mesoporous silicon composite, drying, calcining and the like to obtain the cerium dioxide and graphene-mesoporous silicon composite.
Mixing and heating the prepared cerium dioxide and graphene-mesoporous silicon composite material with a strong alkali solution, and carrying out a series of basic treatment processes such as washing, filtering and drying to obtain the graphene-supported two-dimensional ordered layered cerium dioxide carrier.
Fully mixing 0.2 g of graphene-supported two-dimensional ordered layered cerium dioxide carrier with 1 g/100 mL of chloroauric acid and 2.25 mL of 1 g/100 mL of polyvinyl alcohol, and finally adding 4.5 mL of 0.38 g/100 mL of sodium borohydride and stirring for 90 minutes to obtain the gold-supported two-dimensional cerium dioxide glycerol selective oxidation catalyst.
50 mg of the catalyst, 2 g of NaOH and 20 mL of 0.5 mol/L glycerol solution were mixed and reacted in an oil bath at 80 ℃ for 12 hours.
Claims (2)
1. A preparation method of a two-dimensional layered glycerol oxidation nano-catalyst comprises the following steps:
(1) dissolving cerium nitrate in an ethanol solution, mixing the solution with the graphene-mesoporous silicon composite, and drying and calcining the mixture to obtain a cerium dioxide and graphene-mesoporous silicon composite material;
(2) mixing and heating the prepared cerium dioxide and graphene-mesoporous silicon composite material with a strong alkaline solution, and washing, filtering and drying to obtain a graphene-supported two-dimensional ordered layered cerium dioxide carrier;
(3) uniformly and fully mixing the graphene-supported two-dimensional ordered layered cerium dioxide carrier with the sol-gel dispersed with the gold nanoparticles to obtain the gold-supported two-dimensional cerium dioxide glycerol selective oxidation catalyst.
2. The preparation method of the two-dimensional layered glycerol oxidation nano-catalyst according to claim 1, wherein the mass ratio of the active metal gold to the graphene-supported two-dimensional ordered layered cerium dioxide carrier is 1-5%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910558073.5A CN110227455B (en) | 2019-06-26 | 2019-06-26 | Preparation method of two-dimensional layered glycerol oxidation nano catalyst |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910558073.5A CN110227455B (en) | 2019-06-26 | 2019-06-26 | Preparation method of two-dimensional layered glycerol oxidation nano catalyst |
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| Publication Number | Publication Date |
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| CN110227455A CN110227455A (en) | 2019-09-13 |
| CN110227455B true CN110227455B (en) | 2022-02-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104016825B (en) * | 2014-06-05 | 2017-02-22 | 天津大学 | Technology for preparing organic fuel through directly converting carbon dioxide by using sunlight and photothermal catalyst |
| CN107573213A (en) * | 2017-08-11 | 2018-01-12 | 厦门大学 | A kind of chemical method of biomass ethanol and ethylene glycol |
| CN109336755A (en) * | 2018-11-27 | 2019-02-15 | 嘉兴市秀洲区洪合镇中学 | A kind of preparation method of medicine intermediate succinic acid |
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