Catalyst for benzene hydroxylation for preparation of phenol and preparation method thereof

Patent metadata

Field	Value
Publication number	US-11033884-B2
Application number	US-201415028438-A
Country	US
Kind code	B2
Filing date	Sep 12, 2014
Priority date	Oct 11, 2013
Publication date	Jun 15, 2021
Grant date	Jun 15, 2021

Abstract

The invention relates to a catalyst for benzene hydroxylation for preparation of phenol and a preparation method thereof, wherein said catalyst uses a mesoporous material as carrier, and the catalyst is prepared by first modifying the surface of the carrier using aminosilane, then immersing with acetylacetonate salt of metal, and finally washing and drying. Advantage of the invention is that a reactive metal is loaded on the silane-modified mesoporous material to form a homogeneous-heterogeneous composite catalyst, wherein, the reactive metal component is present in a reaction system in a homogeneous form, which ensures high catalytic performance of the catalyst component, and it is loaded on the carrier through bridging action of aminosilane, which improves the acting force between the metal component and the carrier, enhances stability of the catalyst, and facilitates separation of the catalyst from the product. The catalyst has a simple preparation process, has excellent catalytic performance, and can be applied to the reaction system of benzene hydroxylation for preparation of phenol.

First claim

What is claimed is:

1. A method for preparing a catalyst for benzene hydroxylation for preparation of phenol, wherein the catalyst comprises a carrier being a mesoporous material SBA-16, SBA-16 or MC M-41 with its channel surface functionally modified using aminosilane, and a reactive component being palladium, platinum, copper, vanadium, iron or zinc; wherein the catalyst is a homogeneous-heterogeneous composite catalyst; and wherein the reactive component is loaded onto the carrier through bridging action of the aminosilane, the method comprising the following steps:
A. carrier surface modification process: immersing the carrier into an aminosilane solution with a concentration of 0.1-2 g/L, performing surface modification at a temperature of 20-40° C. taking out, washing and air drying;
B. immersion process: immersing the modified carrier obtained from the step A into acetylacetonate solution containing the reactive component at a temperature of 20-40° C. for 6-36 hours; wherein the acetylacetonate solution has a concentration of 0.1-0.25 mol/L; and
C. washing and drying process: washing the catalyst obtained from the step B with absolute ethanol or dichloromethane and drying
wherein the temperature used in both the method steps A and B does not exceed 40° C.

2. The preparation method according to claim 1 , wherein in the step A the aminosilane is γ-aminopropyltriethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, or N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane;
the solvent is dichloromethane, toluene or absolute ethanol; and
the modification time is 1-32 hours.

Assignees

• Nanjing University Of Technology

Inventors

• Chen Rizhi
• Bao Yaohui
• Jiang Hong
• Fan Yiqun
• Xing Weihong

Classifications

• B01J29/0341 Primary

  containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium · CPC title

• B01J2229/32

  Reaction with silicon compounds, e.g. TEOS, siliconfluoride · CPC title

• Y02P20/52

  using catalysts, e.g. selective catalysts · CPC title

• B01J29/0325

  Noble metals · CPC title

• B01J29/0333

  Iron group metals or copper · CPC title