Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of ZSM-5 molecular sieve nanosphere with multi-level pore hollow structure

A technology of ZSM-5 and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of harsh treatment conditions, long lye treatment time, small mesopore diameter, etc. , to achieve the effect of simple and quick preparation, saving reaction time and energy consumption

Active Publication Date: 2012-09-26
PETROCHINA CO LTD +1
View PDF4 Cites 34 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, there are certain shortcomings in the synthesis of ZSM-5 micro-mesoporous materials in the prior art. First, the mesoporous aperture of the ZSM-5 micro-mesoporous materials synthesized by the template method is relatively small, and there are no reports of macropores; two, the processing conditions are relatively harsh. , generally processed at a higher temperature; 3. The use of lye for a long time and high energy consumption

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
  • Preparation method of ZSM-5 molecular sieve nanosphere with multi-level pore hollow structure
  • Preparation method of ZSM-5 molecular sieve nanosphere with multi-level pore hollow structure
  • Preparation method of ZSM-5 molecular sieve nanosphere with multi-level pore hollow structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Synthesis of nano-ZSM-5: add 100g15.7% TPAOH aqueous solution to 32g deionized water, then add 2.24g NaOH (1mol / L), stir for 10min, add 0.54g aluminum isopropoxide, continue stirring for 5h until the solution is clear, then add 64mlTEOS, stirred for 12h until the solution was clear. Put the above solution into a stainless steel reaction kettle lined with polytetrafluoroethylene, crystallize at 100°C for 12h, then transfer to 180°C for 12h to continue crystallization. After the reaction solution is cooled, centrifuge at 8000rpm for 10min, pour off the supernatant, add deionized water, and then ultrasonicate for 10min to disperse the solids in the lower layer evenly into the water, then centrifuge again. After repeating twice, disperse the solids in the lower layer with ethanol. After centrifugation for 10 min, the white solid in the lower layer was dried at 100° C. for 2 h. Calcined at 550°C for 6h to remove the template agent. A nano ZSM-5 molecular sieve with an aver...

Embodiment 2

[0027] The experimental method is the same as in Example 1, and the microwave treatment time is changed to 15s. The result obtained is a hierarchically porous ZSM-5 molecular sieve nanosphere with meso-micropores, and the average size of the hollow pores is about 50nm. Figure 5 It is a spectrum obtained by X-ray diffraction. It can be seen from the figure that the sample still shows a high crystallinity ZSM-5 molecular sieve after microwave treatment. Figure 6 The scanning electron microscope photos of the sample are given, and the average size of the pores in the ZSM-5 grains decreases, and the average size of the hollow pores is about 50nm. The results show that the hollow nano ZSM-5 molecular sieves can still be prepared by shortening the microwave treatment time, but the pore size of the hollow pores decreases.

Embodiment 3

[0029] The experimental method was the same as in Example 1, but the microwave treatment time was changed to 18s, and the obtained result was macropore-micropore hierarchically porous ZSM-5 molecular sieve nanospheres, and the average size of the hollow pores was about 80nm. The spectrogram that X-ray diffraction obtains shows that sample is the ZSM-5 molecular sieve of high crystallinity ( Figure 7 ).

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
pore sizeaaaaaaaaaa
sizeaaaaaaaaaa
Login to View More

Abstract

The invention relates to a preparation method of a ZSM-5 molecular sieve nanosphere with a multi-level pore hollow structure. The method comprises: taking 64ml of tetraethyl orthosilicate, 0.54g of aluminum isopropoxide and 2.24g of sodium hydroxide (1mol / L) as starting raw materials, adopting 100g of a 15.7% tetrapropylammonium hydroxide aqueous solution as a template agent, controlling the crystallization temperature at 100DEG C-200DEG C, and subjecting the obtained product to drying and roasting so as to obtain a nano-ZSM-5 molecular sieve; adding a nano-ZSM-5 molecular sieve crystal into an alkaline solution, carrying out microwave treatment and centrifugal drying, thus obtaining multi-level pore ZSM-5 molecular sieve nanosphere with a macropore-micropore or mesopore-micropore structure, with the microwave treatment time controlled at 1-25s, the microwave output power controlled at 400-900w, and the concentration of the alkaline solution maintained at 0.1-2 mol / L. By changing the microwave treatment time, the aperture of a ZSM-5 molecular sieve nanosphere hollow pore can be adjusted in the range of 30-150nm.

Description

technical field [0001] The invention relates to a preparation method of a ZSM-5 molecular sieve nanosphere with a multi-level hole hollow structure. Background technique [0002] Since the synthesis of ZSM-5 molecular sieve was first reported by Mobil Corporation of the United States in 1972 (USP3702886), ZSM-5 molecular sieve has been obtained in industrial catalysts due to its unique three-dimensional pore structure, high selectivity, high activity, and high stability. widely used. [0003] A series of microporous materials such as ZSM-5 molecular sieves have been the main active components in cracking catalytic reactions. Their strong acidity and good hydrothermal stability have obvious advantages for the cracking of small and medium molecules, but the pore size of microporous materials is limited The heavy oil molecules are restricted from entering the pores, thus limiting its wide application in cracking reactions. Therefore, mesoporous or macroporous hierarchical por...

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 Applications(China)
IPC IPC(8): C01B39/38
Inventor 张宗弢高晓慧许迪欧阎立军王润伟周志远沈宜泓朴佳锐庞新梅
Owner PETROCHINA CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products