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Preparation method of organophosphorus compound modified ZSM-5 zeolite

A ZSM-5 and compound technology, applied in the field of ZSM-5 zeolite, can solve the problems of poor zeolite pores and poor hydrothermal stability of ZSM-5 zeolite, and achieve the effect of protecting zeolite

Inactive Publication Date: 2018-11-16
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above modification using inorganic phosphorus results in poor hydrothermal stability of ZSM-5 zeolite, and relatively poor zeolite channels.

Method used

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  • Preparation method of organophosphorus compound modified ZSM-5 zeolite
  • Preparation method of organophosphorus compound modified ZSM-5 zeolite
  • Preparation method of organophosphorus compound modified ZSM-5 zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Referring to patent CN102502696B to synthesize nano ZSM-5 zeolite raw powder, and obtain nano H-type ZSM-5 zeolite through ammonium exchange and acid pore expansion. Before modification, the nano ZSM-5 zeolite is calcined to remove water. The calcination temperature is 540°C; the calcination time is 6 hours.

[0046] (2) Perform phosphorus impregnation modification on the calcined nanometer ZSM-5 zeolite obtained in (1). Specific process: at room temperature, stir and impregnate 30 g of calcined nano H-type ZSM-5 zeolite in a cyclohexane solution of trimethyl phosphate prepared in advance for 12 hours. The amount of trimethyl phosphate is 1.36g, and it is configured as a 150ml solution with cyclohexane, and the concentration of trimethyl phosphate is 0.065mol / L. The volume ratio of the calcined nano H-type ZSM-5 zeolite to the cyclohexane solution of trimethyl phosphate is 6:1.

[0047] (3) The solvent used for impregnation is removed by distillation. The distilla...

Embodiment 2

[0052] Repeat Example 1, but change the amount of trimethyl phosphate to 2.72g and add cyclohexane to configure 150ml solution, the concentration of trimethyl phosphate is 0.13mol / L, and the mass percentage of P obtained is 2% trimethyl phosphate Ester-modified ZSM-5 zeolite.

Embodiment 3

[0054] Repeat Example 1, but change the amount of trimethyl phosphate to 4.08g, add cyclohexane to configure a 150ml solution, the concentration of trimethyl phosphate is 0.195mol / L, and the mass percentage of P obtained is 3% triphosphate Methyl ester modified ZSM-5 zeolite.

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Abstract

The invention discloses a preparation method of organophosphorus compound modified ZSM-5 zeolite. The method comprises the following steps: the roasted nano H-type ZSM-5 zeolite is stirred and impregnated in a pre-prepared organophosphorus compound solution, the concentration of the organophosphorus compound in the organophosphorus compound solution is 0.01-2 mol / L, and the organophosphorus compound solution and the roasted nano ZSM-5 zeolite are in a volume ratio of 1:1-20:1; the solvent is removed by distillation, and the organophosphorus compound modified ZSM-5 zeolite is obtained by dryingand roasting. According to the nano ZSM-5 zeolite modified with the organophosphorus compound, crystallinity, pore structure, acidity, catalytic reaction performance and retention after high temperature hydrothermal treatment are obviously better than those of nano ZSM-5 zeolite which are not modified or modified with an inorganic phosphorus compound as a phosphorus source.

Description

technical field [0001] The invention belongs to the technical field of ZSM-5 zeolite, and in particular relates to a preparation method of modifying ZSM-5 zeolite with an organic phosphorus compound, so as to improve the hydrothermal stability of nanometer ZSM-5 zeolite. Background technique [0002] ZSM-5 zeolite was successfully synthesized by the American Mobil Company in the 1960s. Because ZSM-5 zeolite has unique properties in terms of chemical composition, crystal structure, acidity, etc., it has been widely used in the field of petrochemical industry. Part or all of ZSM-5 zeolite is used as catalyst in reactions such as catalytic cracking, toluene disproportionation, selective synthesis of p-diethylbenzene, MTO or MTG. As a catalyst, ZSM-5 zeolite should not only have good catalytic performance, but also have good hydrothermal stability. This is because some reactions, such as catalytic cracking reactions, are carried out in a high-temperature hydrothermal environme...

Claims

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Application Information

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IPC IPC(8): C01B39/38B01J29/40C10G11/05
CPCB01J29/40B01J2229/183C01B39/026C01B39/38C01P2004/64C01P2006/14C01P2006/37C10G11/05
Inventor 郭洪臣赵云刘家旭刘春燕
Owner DALIAN UNIV OF TECH
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