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Method for preparing Ti-MWW molecular sieve film

A technology of molecular sieves and supports, which is applied to the preparation of molecular sieve catalysts, molecular sieves and base exchange compounds, oximes, etc., can solve the problems of high production costs, large demand for titanium-silicon molecular sieves, difficulties in separation and recovery, etc., and achieve simple operation, membrane Preparation of highly reproducible, good catalytic activity effect

Inactive Publication Date: 2016-11-09
JIANGXI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing Ti-MWW molecular sieve membrane. In view of the problems of large demand, high preparation cost, and difficulty in separation and recovery of existing titanium-silicon molecular sieves, a secondary hydrothermal growth method is used to develop a porous tubular support. A method for preparing Ti-MWW molecular sieve membranes with continuous growth and high catalytic activity. The Ti-MWW molecular sieve membranes prepared by this method have the advantages of compact growth, high catalytic activity and good repeatability. The application in the catalytic oxidation of the

Method used

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  • Method for preparing Ti-MWW molecular sieve film
  • Method for preparing Ti-MWW molecular sieve film
  • Method for preparing Ti-MWW molecular sieve film

Examples

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Embodiment 1

[0028]Preparation of Ti-MWW molecular sieve crystal seeds: Mix tetraethylorthosilicate and template agent hexamethyleneimine (HMI) into a pp bottle of water and hydrolyze in an ice-water bath at 0ºC, while tetrabutyl titanate, boric acid Add water and water to hydrolyze in an ice-water bath at 0ºC. After the titanium source and silicon source are completely hydrolyzed, mix them to obtain a molar ratio of 1.0 SiO 2 : 0.03TiO 2 : 0.67B 2 o 3 : 1.4HMI: 19H 2 The light yellow synthetic sol of O, and then transfer the synthetic sol to a stainless steel reactor with a polytetrafluoroethylene liner and crystallize it in an oven at 170 ºC for 8 days. The crystallized material is washed in boiling water until neutral and dried Ti-MWW molecular sieve precursor with 2 M HNO 3 The solution was refluxed at 100ºC to treat the dried molecular sieve precursor, wherein the mass ratio of the molecular sieve precursor to the volume of the nitric acid solution was 1:20, the acid treatment tim...

Embodiment 2

[0031] The synthesis ratio of the Ti-MWW molecular sieve membrane is the same as that of the preparation step Example 1, except that the secondary hydrothermal time is extended to 6 d, Figure 5 SEM photographs of the surface and cross-section of the prepared Ti-MWW molecular sieve membrane. The electron microscope photographs show that the surface of the support is covered by dense flaky Ti-MWW molecular sieve crystals, and the crystals on the upper layer grow perpendicular to the direction of the support. The thickness of the crystal layer is about 4 μm, the crystals in the lower layer grow parallel to the direction of the support, and the thickness of the crystal layer is about 7 μm.

Embodiment 3

[0033] The synthesis ratio of the Ti-MWW molecular sieve membrane is the same as that of the preparation step Example 1, except that the secondary hydrothermal time is extended to 8 d, Figure 6 SEM photos of the surface and cross-section of the prepared Ti-MWW molecular sieve membrane. The SEM photos show that the surface of the support is covered by two layers of dense sheet-like Ti-MWW molecular sieve crystals. The crystals on the upper layer grow perpendicular to the direction of the support. The thickness of the crystal layer is about The thickness of the crystal layer is 3 μm; the crystals in the lower layer grow parallel to the direction of the support, and the thickness of the crystal layer is 9 μm.

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Abstract

The present invention discloses a method for preparing Ti-MWW molecular sieve film; the high-catalytic-activity Ti-MWW molecular sieve film is prepared on a porous tubular ceramic support by: applying pure-phase Ti-MWW molecular sieve crystal as seed crystal to the outer surface of a tubular support, carrying out double hydrothermal growth, using tetrabutyl titanate and hexamethyleneimine as a titanium source and a template agent respectively, and carrying out acid treatment and calcining. The double hydrothermal growth is used herein, the Ti-MWW molecular sieve film that grows continuous and dense is prepared on a porous mullite support for the first time, the problems that it is difficult to separate and recycle Ti-MWW molecular sieve and the sieve is low in reuse rate are solved, and theoretical and technic basis is laid for the industrial application of titanium-silicon molecular sieve film in catalytic oxidative reaction systems for hydrogen peroxide.

Description

technical field [0001] The invention relates to the field of inorganic membrane materials, in particular to a method for preparing Ti-MWW molecular sieve membranes. Background technique [0002] Due to the shape-selective effect of the channel and the controllability of the catalytic activity, molecular sieve materials have been widely used in oil refining, chemical and environmental protection industries. Titanium silicon molecular sieve is a molecular sieve material containing titanium (IV). Taramaso et al. successfully synthesized TS-1 molecular sieve with MFI topology for the first time in 1983. for H 2 o 2 Composed of a catalytic oxidation reaction system (such as olefin epoxidation and aromatic hydrocarbon hydroxylation), TS-1 molecular sieve has excellent catalytic performance, and the reaction system has mild reaction conditions, process safety, and the by-product is only water, which is in line with green chemistry and Therefore, TS-1 molecular sieve has a good a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B41/85C01B39/08C01B39/04B01J29/89C07D301/03C07D303/06C07C249/04C07C251/32
CPCB01J29/89C01B39/04C01B39/085C01P2002/72C01P2004/03C04B41/009C04B41/5024C04B41/85C07C249/04C07D301/03C07D303/06C04B35/10C04B35/185C04B41/4552C04B41/4535C04B41/0072C07C251/32
Inventor 朱美华刘永生李羚姚永康卢章辉陈祥树
Owner JIANGXI NORMAL UNIV
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