Hierarchical porous ZSM-5 zeolite catalyst for preparing acrolein through glycerin dehydration as well as preparation method and application of hierarchical porous ZSM-5 zeolite catalyst

A ZSM-5 and zeolite catalyst technology, which is applied in the direction of molecular sieve catalysts, carbon-based compound preparation, chemical instruments and methods, etc., can solve the problems of fast deactivation and achieve low cost, simple synthesis, and high selectivity.

Inactive Publication Date: 2014-03-19
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The catalyst has high selectivity to acrolein and is relatively s

Method used

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  • Hierarchical porous ZSM-5 zeolite catalyst for preparing acrolein through glycerin dehydration as well as preparation method and application of hierarchical porous ZSM-5 zeolite catalyst
  • Hierarchical porous ZSM-5 zeolite catalyst for preparing acrolein through glycerin dehydration as well as preparation method and application of hierarchical porous ZSM-5 zeolite catalyst
  • Hierarchical porous ZSM-5 zeolite catalyst for preparing acrolein through glycerin dehydration as well as preparation method and application of hierarchical porous ZSM-5 zeolite catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Prepare the initial gel in the following molar ratios: 1SiO 2 : 0.004Al 2 o 3 : 0.14Na 2 O : 0.3KCl : 0.1TPABr : 30H 2 O, silica sol, aluminum sulfate, and sodium hydroxide were dissolved in deionized water respectively, and potassium chloride, tetrapropylammonium bromide, and 5wt% 200nm-sized MFI seed crystals were added under constant stirring. The above mixture was stirred and aged at room temperature for 2 hours, then put into a stainless steel static crystallization kettle with a polytetrafluoroethylene liner, and reacted at 140° C. for 12 hours.

[0031] After crystallization, cool, filter and wash with deionized water for 3-4 times, and then dry the obtained sample at 80-120°C. The product is calcined in a muffle furnace or a tube furnace to remove the template agent, generally in an air atmosphere at 550 ° C for 4 to 6 hours. Then use ammonium nitrate solution with a concentration of 5wt% at 80°C for three consecutive ion exchanges (solution volume / produc...

Embodiment 2

[0033] Prepare the initial gel in the following molar ratios: 1SiO 2 : 0.004Al 2 o 3 : 0.15Na 2 O : 0.3KCl : 0.1TPABr : 60H 2 O, silica sol, aluminum sulfate, and sodium hydroxide were dissolved in deionized water respectively, and potassium chloride, tetrapropylammonium bromide, and 5 wt % MFI seed crystals of 200 nm in size were added under constant stirring. The above mixture was stirred and aged at room temperature for 2 hours, then put into a stainless steel static crystallization kettle with a polytetrafluoroethylene liner, and reacted at 120° C. for 12 hours.

[0034] After crystallization, cool, filter and wash with deionized water for 3-4 times, and then dry the obtained sample at 80-120°C. The product is calcined in a muffle furnace or a tube furnace to remove the template agent, generally in an air atmosphere at 550 ° C for 4 to 6 hours. Then use ammonium nitrate solution with a concentration of 5wt% at 80°C for three consecutive ion exchanges (solution volum...

Embodiment 3-6

[0036] The steps in this embodiment are exactly the same as those in Embodiment 1 above. The difference is that during the preparation of the reaction mixture, the Na used 2 O / Si 2 O changed from 0.14 to 0.10, 0.12, 0.16, 0.18.

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Abstract

The invention belongs to the technical field of chemical catalysts, particularly relates to a hierarchical porous ZSM-5 zeolite catalyst for preparing acrolein through glycerin dehydration as well as a preparation method and application of the hierarchical porous ZSM-5 zeolite catalyst and also provides a method for synthesizing hierarchical porous ZSM-5 zeolite with high crystallinity, controllable particle size, controllable Si/Al ratio and controllable appearance at high yield, low time consumption and low (no) template agent dosage, wherein the hierarchical porous ZSM-5 zeolite is synthesized by introducing a small amount of MFI zeolite crystal seeds and parts of inorganic salt additives to a general synthesis system (a silicon source, an aluminum source, an alkaline source and water) and regulating the synthesis ratio and reaction conditions. The prepared catalyst has the characteristics such as controllable quantity of acid sites, large special surface area, short mass transfer path and the like, can be used for the catalytic reaction for preparing acrolein through the glycerin dehydration and has favorable catalytic activity, selectivity and stability.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, and in particular relates to a multi-level porous ZSM-5 zeolite catalyst and its preparation method and application. Background technique [0002] The high-value conversion and utilization technology of glycerol is an important part of biodiesel technology. The full utilization of by-product glycerol is one of the urgent problems to be solved to reduce the cost of biodiesel and promote the industrialization of biodiesel technology. It is of great significance to alleviate the energy crisis. [0003] The technology of dehydration of glycerol to produce acrolein is one of the options for high-value conversion of glycerol. The key to this reaction is to improve the stability of the catalyst and the selectivity of the product. During the dehydration process of glycerol, reactions such as cracking, condensation, and oxidation occur simultaneously, and macromolecular aromatic compounds and p...

Claims

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Application Information

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IPC IPC(8): B01J29/40C07C47/22C07C45/52
Inventor 唐颐张宏斌胡志洁秦枫徐华龙沈伟张红霞张亚红
Owner FUDAN UNIV
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