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Nanocrystalline catalyst and preparation method thereof, and preparation method of propylene oxide

A technology of propylene oxide and nanocrystals, applied in the field of nanomaterials, can solve problems such as long synthesis steps, large investment, and environmental pollution

Inactive Publication Date: 2018-08-28
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the methods for industrial production of propylene oxide are mainly the chlorohydrin method and the Halcon process; the chlorohydrin method is a traditional synthesis method for the indirect production of epoxy compounds from olefins. Many, equipment corrosion is serious, because chlorine gas is used in the production process, a large amount of organic chlorides are produced, which causes serious pollution to the environment; the Halcon process uses alkyl hydrogen peroxide as the oxygen source, and produces a large number of co-products after the reaction, which requires a large one-time investment
Therefore, the reaction process of the above-mentioned method is complicated, and the environment is unfriendly.
The gas-phase one-step synthesis of alkylene oxides from olefins using oxygen as an oxidant is an ideal reaction with environmental friendliness and low energy consumption, which has important research value, but the traditional Au / TiO 2 (P25) in H 2 and O 2 The conversion rate of catalytic propylene epoxidation to propylene oxide under atmosphere is too low, and the rate of generating propylene oxide per unit mass of gold is relatively small. Therefore, seeking a simple and efficient catalyst for propylene epoxidation is a major challenge in this field. technical problems

Method used

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  • Nanocrystalline catalyst and preparation method thereof, and preparation method of propylene oxide
  • Nanocrystalline catalyst and preparation method thereof, and preparation method of propylene oxide
  • Nanocrystalline catalyst and preparation method thereof, and preparation method of propylene oxide

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preparation example Construction

[0039] The application also provides the preparation method of above-mentioned four kinds of nanocrystalline catalysts, for Au / TiO 2 The preparation method of {001}-1 nanocrystal specifically comprises the following steps:

[0040] TiO 2 {001} nanocrystal, water and containing Au and TiO 2 The precursor solution is mixed, the pH is adjusted to 7-10 with ammonia water, and the reaction product is obtained after the reaction;

[0041] The resulting reaction product was filtered and dried, then in H 2 / Ar atmosphere to obtain Au / TiO 2 {001}-1 nanocrystalline catalyst.

[0042] For Au / H-TiO 2 The preparation method of {001}-1 nanocrystal specifically comprises the following steps:

[0043] H-TiO 2 {001} nanocrystal, water and containing Au and TiO 2 The precursor solution is mixed, the pH is adjusted to 7-10 with ammonia water, and the reaction product is obtained after the reaction;

[0044] The resulting reaction product was filtered and dried, then in H 2 / Ar atmosphe...

Embodiment 1

[0068] Example 1TiO 2 Preparation of {001} Nanocrystals

[0069] Take 25ml of tetra-n-butyl titanate and 3ml of hydrofluoric acid in a 50ml polytetrafluoroethylene inner kettle and stir at room temperature for half an hour, then put it into a stainless steel jacket, keep it at 180°C for 24h, and centrifuge the obtained product after the reaction Separated and washed repeatedly with ethanol and ultrapure water to obtain white TiO 2 {001} solid powder, and dried at 70°C for 12 hours, then dispersed the obtained powder in 700ml 0.1M NaOH solution, stirred at room temperature for 24h, centrifuged and washed with ultrapure water for several times until the pH of the solution was between 7-8, Finally and dried at 70 °C for 12 hours, a clean white TiO 2 {001} Solid powder.

[0070] Preparation of TiO as above 2 The method of (001) nanocrystal refers to the method provided by Xie Zhaoxiong et al. Materials such as tetra-n-butyl titanate, hydrofluoric acid, absolute ethanol and ul...

Embodiment 2

[0072] Example 2H-TiO 2 Preparation of {001} Nanocrystals

[0073] The TiO prepared according to the method provided in Example 1 will be prepared under atmospheric pressure 2 {001} nanocrystals placed in a quartz tube at 5%-H 2 / Reduction treatment at 200-800°C under Ar atmosphere for no more than 4 hours to obtain H-TiO 2 {001} nanocrystals.

[0074] image 3 The H-TiO prepared for this example 2 TEM photo of {001} nanocrystals, Figure 4 The H-TiO prepared for this example 2 HR-TEM photograph of {001} nanocrystals.

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Abstract

The invention provides a nanocrystalline catalyst selected from Au / TiO2(001) or Au / H-TiO2(001). In Au / TiO2(001), Au is supported on TiO2(001) nanocrystals and has a size of 1.4-3.8nm or 0.62-1.28nm; in Au / H-TiO2(001), Au is supported on H-TiO2(001) nanocrystals and has a size of 1.4-3.8nm or 0.62-1.28nm. The application also provides a preparation method of the nanocrystalline catalyst and application of the nanocrystalline catalyst in preparation of propylene oxide. The nanocrystalline catalyst provided by the application exhibits excellent activity and selectivity in the catalytic reaction of propylene epoxidation to prepare propylene oxide.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular to a nanocrystalline catalyst, a preparation method thereof and a preparation method of propylene oxide. Background technique [0002] Gold is an environmentally friendly noble metal. Since Haruta reported in 1989 that Au particles smaller than 5 nm supported on metal oxides have high catalytic activity in low-temperature CO oxidation reactions, gold catalysis has become a hot research field. , has developed greatly in the following decades. At the same time, Au has comprehensive excellent characteristics such as high temperature resistance, oxidation resistance and corrosion resistance, and has become the most important catalyst material. It is currently widely used in CO oxidation, CO-PROX reaction, WGS reaction and some hydrogenation reactions. The vast majority of heterogeneous reaction catalysts are supported by noble metals, such as Au / Al 2 o 3 , Au / TS-1, Au / TiO 2 , ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/52B01J35/02C07D301/10C07D303/04B01J35/00
CPCC07D301/10C07D303/04B01J23/52B01J35/393B01J35/396B01J35/40Y02P20/52
Inventor 黄伟新李丹
Owner UNIV OF SCI & TECH OF CHINA