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ZSM-5 and ZSM-11 eutectic molecular sieve as well as preparation method and application thereof

A technology of ZSM-11 and ZSM-5, which is applied in the field of molecular sieve synthesis, ZSM-5 and ZSM-11 eutectic molecular sieves and their preparation, to achieve the effects of facilitating industrialization, improving stability, and easily obtaining raw materials

Active Publication Date: 2020-08-04
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] ZSM-5 and ZSM-11 are very similar, so the eutectic structure of the two will often appear in the process of synthesizing one of the molecular sieves, but the preparation of ZSM-5 / 11 eutectic molecular sieve by steam-assisted crystallization has not been reported so far. The application of ZSM-5 / 11 eutectic molecular sieve in the reaction of methanol to aromatics has not been reported yet

Method used

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  • ZSM-5 and ZSM-11 eutectic molecular sieve as well as preparation method and application thereof
  • ZSM-5 and ZSM-11 eutectic molecular sieve as well as preparation method and application thereof
  • ZSM-5 and ZSM-11 eutectic molecular sieve as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The preparation method of ZSM-5 and ZSM-11 eutectic molecular sieve of the present embodiment comprises the following steps:

[0054] 1) Add 36ml of deionized water to a beaker, add 0.246g tetrapropylammonium bromide (TPABr, 99wt%), 7.442g tetrabutylammonium bromide (TBABr, 99wt%), 15.2g silicon Sol (40wt% SiO 2 meter), 0.487g sodium metaaluminate (41wt%, as Al 2 o 3 ) and 0.584g of sodium hydroxide, and kept stirring at room temperature for 12 hours until uniformly mixed to obtain a mixed gel;

[0055] Among them, the molar ratio of each substance in the raw material is 1SiO 2 : 0.02Al 2 o 3 : 0.07Na 2 O: 0.01TPA + : 0.23TBA + : 20H 2 O.

[0056] 2) Transfer the mixed gel in step 1) to a petri dish, perform drying treatment, and then perform grinding treatment to obtain gel powder;

[0057] Wherein, the temperature of the drying treatment is 25° C., and the time of the drying treatment is 36 hours.

[0058] 3) Put the gel powder obtained in step 2) in a sma...

Embodiment 2

[0069] The preparation method of ZSM-5 and ZSM-11 eutectic molecular sieve of the present embodiment comprises the following steps:

[0070] 1) Add 27ml of deionized water into the beaker, and add 0.469g of tetrapropylammonium hydroxide (TPA + , 40wt%), 14.9694g tetrabutylammonium hydroxide (TBA + , 40wt%), 14.93g silica sol (40wt% with SiO 2 meter), 0.487g sodium metaaluminate (41wt%, as Al 2 o 3 ) and 0.584g of sodium hydroxide, and kept stirring at room temperature for 12 hours until uniformly mixed to obtain a mixed gel;

[0071] Among them, the molar ratio of each substance in the raw material is 1SiO 2 : 0.02Al 2 o 3 : 0.07Na 2 O: 0.01TPA + : 0.23TBA + : 20H 2 O.

[0072] 2) Transfer the mixed gel in step 1) to a petri dish, perform drying treatment, and then perform grinding treatment to obtain gel powder;

[0073] Wherein, the temperature of the drying treatment is 25° C., and the time of the drying treatment is 36 hours.

[0074] 3) Put the gel powder obt...

Embodiment 3

[0086] The preparation method of ZSM-5 and ZSM-11 eutectic molecular sieve of the present embodiment comprises the following steps:

[0087] 1) Add 36ml of absolute ethanol to a beaker, add 0.738g tetrapropylammonium bromide (TPABr, 99wt%), 7.442g tetrabutylammonium hydroxide (TBABr, 40wt% aqueous solution), 21.458g orthosilicon Ethyl acetate (TEOS, 28wt% as SiO 2 ), 1.651g aluminum isopropoxide (24.7wt%, as Al 2 o 3 Meter) and 0.584g sodium hydroxide; Continue stirring at room temperature for 12 hours to mix evenly, obtain mixed gel;

[0088] Among them, the molar ratio of each substance in the raw material is 1SiO 2 : 0.04Al 2 o 3 : 0.07Na 2 O: 0.03TPA + : 0.226TBA + : 10EtOH.

[0089] 2) Transfer the mixed gel in step 1) to a petri dish, perform drying treatment, and then perform grinding treatment to obtain gel powder;

[0090] Wherein, the temperature of the drying treatment is 40° C., and the time of the drying treatment is 28 hours.

[0091] 3) Put the gel po...

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Abstract

The invention provides a ZSM-5 and ZSM-11 eutectic molecular sieve as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) mixing and stirring a silicon source, an aluminum source, a first organic template agent, a second organic template agent, sodium hydroxide and a solvent to obtain mixed gel; (2) carrying out drying treatment and grinding treatment on the mixed gel to obtain gel powder; (3) performing crystallization treatment on the gel powder in a hydrothermal kettle to obtain an intermediate product, wherein in the crystallization treatment, the pressure is 0.7-1.3 Mpa, the temperature is 160-180 DEG C, the time is 24-48 hours, and the mass ratio of the water to the gel powder in the hydrothermal kettle is (1-10): 1; and (4)washing, drying and roasting the intermediate product to obtain the ZSM-5 and ZSM-11 eutectic molecular sieve. According to the preparation method disclosed by the invention, the eutectic molecular sieve with a controllable ratio of ZSM-5 to ZSM-11 is innovatively prepared by virtue of a water vapor assisted crystallization method.

Description

technical field [0001] The invention relates to a molecular sieve, in particular to a ZSM-5 and ZSM-11 eutectic molecular sieve and its preparation method and application, belonging to the technical field of molecular sieve synthesis. Background technique [0002] On the one hand, the development of the global economy has led to increased global energy demand and dwindling oil resources, so the development of non-traditional fuel and chemical supplies is crucial. On the other hand, the aromatics produced by traditional pyrolysis of petroleum cannot satisfy the rapidly developing polyester industry. Therefore, under the background of increasing consumption of petrochemical products and high dependence on foreign oil, the development of methanol-to-aromatics technology is conducive to my country's energy security and economic development. [0003] ZSM-5 molecular sieve is a kind of aluminosilicate zeolite material developed by Mobil in the 1970s. ZSM-5 molecular sieve is due ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/36C01B39/40B01J29/40C07C1/20C07C15/02
CPCC01B39/365C01B39/40B01J29/005B01J29/40C07C1/20C01P2004/82C01P2006/14C01P2006/12C01P2004/61C07C15/02
Inventor 冯丽梅徐亚荣张力许磊
Owner PETROCHINA CO LTD
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