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A kind of titanium-containing molecular sieve composite material and preparation method thereof

A composite material and molecular sieve technology, applied in the field of titanium-containing molecular sieve composite materials and preparation, can solve the problems of increasing difficulty of diffusion and decreasing utilization rate of titanium active centers.

Active Publication Date: 2011-11-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One of the purposes of the present invention is to provide a titanium-containing molecular sieve composite material for the problems existing in the prior art. will significantly reduce the problem

Method used

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  • A kind of titanium-containing molecular sieve composite material and preparation method thereof
  • A kind of titanium-containing molecular sieve composite material and preparation method thereof
  • A kind of titanium-containing molecular sieve composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] According to tetraethyl silicate: tetrabutyl titanate: TPAOH: IPA: H 2 O = 25: 1: 4.7: 10: 450 molar ratio Weigh the raw materials, mix the raw materials at 30°C, heat up to 90°C, heat and hydrolyze the alcohol to obtain a uniform clear solution. Add Silicalite-1 (produced by Hunan Jianchang Petrochemical Company, crystallinity > 90%, SiO 2 >99.5%) fully stirred to obtain a mixture in which the total SiO 2 with TiO 2 The mass ratio is 50:1. Put the mixture into a closed autoclave, raise the temperature to 165°C, and keep it for 24 hours, then cool, filter, and wash the obtained product until the pH of the filtrate is <8, dry the solid part at 110°C for 4 hours, and then dry it at 550°C Calcined for 3 hours to obtain a sample.

[0041] The composite material sample contains Si, Ti and O elements, and the ratio of Si to Ti is 1:0.03 in terms of oxides. The XRD spectrum pattern of this sample is attached figure 1 , showing that strong diffraction peaks appear at 2θ=7...

Embodiment 2

[0043] According to tetraethyl silicate: tetrabutyl titanate: TPAOH: H 2 The molar ratio of O=15:1:5:250 weighs the raw materials, mixes the raw materials at 50°C, heats up to 90°C, heats and hydrolyzes the alcohol to obtain a uniform clear solution. Add unbaked Silicalite-1 and stir well to obtain a mixture, so that the total SiO in the mixture 2 with TiO 2 =100:1, put the mixture into a closed autoclave, raise the temperature to 175°C, and keep it for 36 hours. The obtained product was cooled, filtered and washed until the pH of the filtrate was 2 with SiO 2 The molar ratio is the TiO with the target at the center 2 with SiO 2 450% of the molar ratio (Table 1). Tested by BET method, its specific surface area is 420m 2 / g.

Embodiment 3

[0045] According to tetrabutyl titanate:TPAOH:IPA:H 2 The molar ratio of O=1:2.5:20:200 weighs the raw materials, mixes the raw materials at 30°C, heats up to 100°C, heats and hydrolyzes the alcohol to obtain a uniform clear solution. Add Silicalite-1 that has been roasted at 550°C for 3 hours and stir well to obtain a mixture. The total SiO in the mixture 2 : with TiO 2 The mass ratio of the mixture was 75:1, the mixture was put into a closed autoclave, the temperature was raised to 170° C., and kept for 48 hours. The obtained product was cooled, filtered and washed until the pH of the filtrate was 2 with SiO 2 The molar ratio is the TiO with the target at the center 2 with SiO 2 250% of the molar ratio (Table 1). Tested by BET method, its specific surface area is 405m 2 / g.

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Abstract

The invention discloses a titanium-containing molecular sieve composite material which is characterized in that: the composite material contains Silicalite-1 used as a matrix and also contains silicon, titanium and oxygen elements; based on oxides, the molar ratio of silicon to titanium is 1:>(0-0.05); the X-ray diffraction spectra of the composite material shows the characteristic diffraction peaks of an MFI (Mobil Five) structure; and in the TEM (Transmission Electron Microscopy)-spectrum microscopic composition of the composite material, the molar ratio of TiO2 to SiO2 of the composite material at the edge of which a target is located is more than 150% that of the composite material in the center of which a target is located. The invention also discloses a preparation method of the titanium-containing molecular sieve composite material.

Description

technical field [0001] The invention relates to a titanium-containing molecular sieve composite material and a preparation method. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. At present, TS-1 with MFI structure, TS-2 with MEL structure, and TS-48 with larger pore structure have been synthesized. Especially TS-1 molecular sieve, since it was first reported by Taramasso et al. (US 4,410,501) in 1983, has attracted widespread attention due to its excellent catalytic oxidation performance. TS-1 molecular sieve is a new type of molecular sieve with excellent oxidation catalytic performance formed by introducing transition metal element titanium into the molecular sieve framework with ZSM-5 structure. TS-1 not only has the catalytic oxidation effect of titanium active center, but also has the shape-selective effect and excellent stability of ZSM-5 molecular sieve. At present, using TS-1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J37/00C07C37/60C07C39/02
Inventor 朱斌龙立华林民舒兴田史春风汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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