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Zeolite molecular sieve with multi-stage pore structure and preparation method and application of zeolite molecular sieve

A technology of zeolite molecular sieve and pore structure, applied in molecular sieves and base exchange compounds, molecular sieve catalysts, crystalline aluminosilicate zeolites, etc., can solve the problem of reducing the wear resistance of catalysts in fluidized beds, destroying the crystallinity and strength of molecular sieves, Time-consuming and labor-intensive problems, to achieve the effects of rich pore structure, improved anti-carbon deposition ability, and reduced production costs

Inactive Publication Date: 2020-11-24
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to prepare molecular sieves with mesoporous and macroporous structures, the existing technical methods often use acid-base treatment, recrystallization and other modifications and secondary synthesis to increase the specific surface area and pore volume of zeolite molecular sieves. However, the above processes are often cumbersome and need to be repeated. The modification of molecular sieves destroys the crystallinity and strength of molecular sieves to a certain extent, which is time-consuming and laborious; and the synthesis of hollow type HZSM-5, nano-sized HZSM-5, and core-shell type MCM-22 also requires the addition of expensive soft and hard templates. Pore ​​formation, not only harsh conditions, but also reduces the wear resistance of the catalyst in the fluidized bed

Method used

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  • Zeolite molecular sieve with multi-stage pore structure and preparation method and application of zeolite molecular sieve
  • Zeolite molecular sieve with multi-stage pore structure and preparation method and application of zeolite molecular sieve
  • Zeolite molecular sieve with multi-stage pore structure and preparation method and application of zeolite molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Take a clean 100ml beaker, add 47.96ml of deionized water and 1g of PDDA, place in a water bath at 30°C and stir for 3 hours. Accurately weigh 0.4896g of sodium aluminate and 0.2025g of sodium hydroxide, pour into a beaker, mix and stir until the solution is clear. Add 4.5ml of hexamethyleneimine at a rate of 1 drop per second, and mix and stir for 30 minutes. Add 24.848g of silica sol at a rate of 2 drops per second, and stir vigorously for 30 minutes. Pour the above mixture into a polytetrafluoroethylene-lined hydrothermal kettle, and place it in a rotary oven for dynamic crystallization at a rotation rate of 60r / min. First crystallized at 50℃ for 2h, then heated to 140℃ for 5d. After the crystallization, wash and centrifuge and dry, and then place it in a muffle furnace and bake at 550°C for 10 hours to obtain Na-MCM-22. Mix Na-MCM-22 and 1mol / L ammonium nitrate solution with 80 at a ratio of 1:30 °C ammonium exchange in a water bath for 3 times, and then calcined ...

Embodiment 2

[0055] Take a clean 100ml beaker, add 47.96ml of deionized water and 1.5g of PDDA, place in a water bath at 30°C and stir for 3 hours. Accurately weigh 0.4896g of sodium aluminate and 0.2025g of sodium hydroxide, pour into a beaker, mix and stir until the solution is clear. Add 4.5ml of hexamethyleneimine at a rate of 1 drop per second, and mix and stir for 30 minutes. Add 24.848g of silica sol at a rate of 2 drops per second, and stir vigorously for 30 minutes. Pour the above mixture into a polytetrafluoroethylene-lined hydrothermal kettle, and place it in a rotary oven for dynamic crystallization at a rotation rate of 60r / min. The crystallization is carried out step by step. Firstly, it is crystallized at 50°C for 4h, and then it is heated to 140°C for 5d. After the crystallization is completed, it is washed and centrifuged and dried, and then placed in a muffle furnace and roasted at 550°C for 10h to obtain Na-MCM-22. Na-MCM-22 and 1 mol / L ammonium nitrate solution were ex...

Embodiment 3

[0057] Take a clean 100ml beaker, add 47.96ml of deionized water and 2.5g of PDDA, place in a water bath at 30°C and stir for 3 hours. Accurately weigh 0.4896g of sodium aluminate and 0.2025g of sodium hydroxide, pour into a beaker, mix and stir until the solution is clear. Add 4.5ml of hexamethyleneimine at a rate of 1 drop per second, and mix and stir for 30 minutes. Add 24.848g of silica sol at a rate of 2 drops per second, and stir vigorously for 30 minutes. Pour the above mixture into a polytetrafluoroethylene-lined hydrothermal kettle, and place it in a rotary oven for dynamic crystallization at a rotation rate of 60r / min. The crystallization is carried out step by step. Firstly, it is crystallized at 50°C for 6h, and then it is heated to 140°C for 5d. After the crystallization is completed, it is washed and centrifuged and dried, and then placed in a muffle furnace and roasted at 550°C for 10h to obtain Na-MCM-22. Na-MCM-22 and 1 mol / L ammonium nitrate solution were ex...

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Abstract

The present invention discloses a zeolite molecular sieve with a multi-stage pore structure and a preparation method and an application of the zeolite molecular sieve. The zeolite molecular sieve withthe multi-stage pore structure is prepared by adding a small amount of a cationic polymer structure directing agent in a one-step manner. Compared with conventional molecular sieves, the zeolite molecular sieve has a relatively high specific surface area and pore volume, and a rich pore structure, solves problems of cumbersome post-processing operations or use of expensive organic templates whenthe conventional preparation of the molecular sieve with the multi-stage pore structure is conducted. At the same time, after active metal components are loaded, carbon holding capacity of a catalystis enhanced, reaction stability of the molecular sieve is effectively improved, and the molecular sieve shows good reaction performance when applied in anaerobic aromatization reaction of methane.

Description

technical field [0001] The invention belongs to the technical field of energy and chemical catalysts, and in particular relates to a multi-stage pore structure zeolite molecular sieve and its preparation method and application. Background technique [0002] Since the discovery of zeolite molecular sieve, it has been widely used in petrochemical industry due to its rich specific surface area and pore structure. The characteristics of zeolites have also been discovered more and more thoroughly. Although some zeolite molecular sieves have been industrialized, with the conditions of various experimental reaction conditions, there are more stringent requirements for molecular sieves, such as modification by different methods to improve catalytic activity. Researchers have been exploring new techniques and methods for the synthesis of zeolite molecular sieves by modifying the molecular sieve itself to improve catalytic stability, and have prepared various forms of molecular sieves...

Claims

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Application Information

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IPC IPC(8): C01B39/04C01B39/02B01J29/78B01J37/10B01J37/02
CPCB01J29/7876B01J37/0201B01J37/10B01J2229/186C01B39/026C01B39/04C01P2002/72C01P2004/03C01P2006/12C01P2006/14C01P2006/16C01P2006/17
Inventor 马晓迅韩运达黄帆张浩
Owner NORTHWEST UNIV
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