Method for synthesizing TS-1 molecular sieve

A technology of TS-1 and molecular sieve, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low oxidation activity and high content of non-skeletal titanium, achieve low dosage, overcome activity decline, and operate simple effect

Active Publication Date: 2011-04-20
CHINA PETROLEUM & CHEM CORP +1
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved in the present invention is to provide a new method for synthesizing titanium-silicon molecular sieve (TS-1) aiming at the shortcomings of high non-skeleton titanium content and low oxidation activity in the TS-1 molecular sieve synthesized by the prior art

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for synthesizing TS-1 molecular sieve
  • Method for synthesizing TS-1 molecular sieve
  • Method for synthesizing TS-1 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Mix tetraethyl orthosilicate, 10-20 mesh silica gel particles and tetrabutyl titanate evenly, then add it to the aqueous solution of tetrapropyl ammonium hydroxide and stir well, wherein tetraethyl orthosilicate (as SiO 2 In terms of), silica gel particles (in terms of SiO 2 In terms of), tetrabutyl titanate (as TiO 2 The molar ratio of tetrapropylammonium hydroxide and water is 1:1:0.04:0.1:15, and then transferred to a stainless steel sealed reaction kettle for crystallization at a temperature of 170°C and autogenous pressure for 24 hours, and the obtained crystal The compounded product was filtered, washed with water, dried at 110°C for 120 minutes, and then calcined at 550°C for 3 hours to obtain TS-1 molecular sieve. The particle size of the sample was 10-40 mesh as measured by sieving. Its XRD crystal phase diagram is shown in Figure 1 (C), similar to the comparative example, with MFI topology; the Fourier transform infrared spectrum is shown in Figure 2 (C), sim...

Embodiment 2

[0037] Mix tetraethyl orthosilicate, 20-40 mesh silica gel particles and tetraethyl titanate evenly, then add it to the aqueous solution of tetrapropyl ammonium hydroxide and stir well, wherein tetraethyl orthosilicate (use SiO 2 In terms of), silica gel particles (in terms of SiO 2 In terms of), tetraethyl titanate (as TiO 2 The molar ratio of tetrapropylammonium hydroxide and water is 1:0.5:0.1:0.25:75, and then transferred to a stainless steel sealed reaction kettle for crystallization at a temperature of 150°C and autogenous pressure for 96 hours, and the obtained crystal The product was filtered, washed with water, dried at 110°C for 120 minutes, and then calcined at 550°C for 3 hours to obtain TS-1 molecular sieve. The particle size of the sample was 40-80 mesh as measured by sieving. Its XRD crystal phase diagram, Fourier transform infrared spectrogram and ultraviolet-visible spectrogram are similar to the sample of Example 1. X-ray diffraction (XRD) and infrared spec...

Embodiment 3

[0039] Mix the silica sol, 40-80 mesh silica gel particles and tetrabutyl titanate evenly, then add them to the aqueous solution of tetrapropyl ammonium hydroxide and triethanolamine and stir well, wherein the silica sol (use SiO 2 In terms of), silica gel particles (in terms of SiO 2 In terms of), tetrabutyl titanate (as TiO 2 The molar ratio of tetrapropylammonium hydroxide, triethanolamine and water is 1: 2: 0.01: 0.15: 0.15: 35, and then transferred to a stainless steel sealed reaction kettle for crystallization at a temperature of 170°C and autogenous pressure for 48 After 1 hour, the obtained crystallized product was filtered, washed with water, dried at 110°C for 120 minutes, and then roasted at 550°C for 3 hours to obtain the product. The particle size of the sample was 80-120 mesh as measured by sieving. Its XRD crystal phase diagram, Fourier transform infrared spectrogram and ultraviolet-visible spectrogram are similar to those of the sample in Example 1.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
particle sizeaaaaaaaaaa
particle sizeaaaaaaaaaa
particle sizeaaaaaaaaaa
Login to view more

Abstract

A method for synthesizing a TS-1 molecular sieve comprises the steps of mixing the aqueous solution of silicon source, titanium source, solid silica gel particles and organo-alkali compound and carrying out hydrothermal crystallization; wherein, the molar ratio of the silicon source: the titanium source: the solid silica gel particles: the organic alkali: water is 1: 0.001-2.5: 0.1-10: 0.001-0.8:5-150; the silicon source and the silica gel particles are counted by SiO2 and the titanium source is counted by TiO2, wherein, the silicon source is silica sol or organic silicate ester. The TS-1 molecular sieve synthesized by the method has low content of non-skeleton titanium and has high activity, stability and selectivity when being used in oxidation reaction.

Description

technical field [0001] The invention relates to a method for synthesizing titanium-silicon molecular sieve (TS-1) with MFI structure. Background technique [0002] Titanium silicate molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. TS-1 with MFI structure, TS-2 with MEL structure and TS-48 with larger pore structure have been synthesized so far. Among them, TS-1 molecular sieve is a molecular sieve with ZSM-5 structure containing transition metal element titanium in the framework, which has excellent catalytic selective oxidation performance, shape selection and excellent stability. TS-1 molecular sieve is used in the oxidation reaction of organic matter. It can use non-polluting low-concentration hydrogen peroxide as the oxidant, thereby simplifying the oxidation process and reducing environmental pollution. It has the incomparable advantages of energy saving, economy and environmental friendliness in tradition...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/06B01J29/89
Inventor 林民史春风朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap