Nano-sheet-like ZSM-5 molecular sieve preparation method

A technology of ZSM-5 and nano flakes, which is applied in the field of preparation of nano flake ZSM-5 molecular sieves, can solve the problems of high synthesis cost and unfavorable industrial production, achieve large industrial application potential, reduce synthesis cost, and simplify synthesis steps Effect

Active Publication Date: 2020-03-10
WISON ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above-mentioned shortcomings of the prior art, the object of the present invention is to provide a method for preparing nanosheet ZSM-5 molecu

Method used

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  • Nano-sheet-like ZSM-5 molecular sieve preparation method
  • Nano-sheet-like ZSM-5 molecular sieve preparation method
  • Nano-sheet-like ZSM-5 molecular sieve preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Na in this example 2 O, Al 2 o 3 , SiO 2 , n-butylamine and H 2 The molar ratio of O is 0.08:0.01:1:0.15:30, and the seed crystal addition amount does not exceed SiO 2 10wt% of the content.

[0037] 1) According to SiO 2 with Na 2 O molar ratio is 3.2, 30wt% silica sol is pretreated with sodium hydroxide, and pretreated at 80°C for 24 hours. Add 0.15 g of sodium metaaluminate, 0.34 g of sodium hydroxide, and 0.66 g of n-butylamine to 24 g of water, stir and dissolve at room temperature, add 13.6 g of alkali-pretreated silica sol, and add concentrated sulfuric acid dropwise to adjust the pH value to 10.0 , and finally add 0.36 grams of ZSM-5 seed crystals;

[0038] 2) Stir and age at 100°C 200 rpm for 24 hours

[0039] 3) Raise the temperature to 170° C., react at 200 rpm for 72 hours, wash and dry to prepare ZSM-5 molecular sieve crystals.

[0040] figure 1 Scanning electron micrograph of the ZSM-5 molecular sieve obtained by the preparation method. It can b...

Embodiment 2

[0048] Na in this example 2 O, Al 2 o 3 , SiO 2 , n-butylamine and H 2 The molar ratio of O is 0.08:0.01:1:0.15:30, and the seed crystal addition amount does not exceed SiO 2 30% of the content.

[0049] The difference with Example 1 is that step 1) joins 0.43 gram of aluminum sulfate octadecahydrate, 14.9 gram of water glass (modulus is 3), 0.7 gram of n-butylamine in 24 gram of water, stirring and dissolving at room temperature, then Concentrated sulfuric acid was added dropwise to adjust the pH to 9.5, and 1.08 g of ZSM-5 seed crystals were added. All the other steps are the same as in Example 1.

[0050] image 3 The SEM spectrum of the ZSM-5 molecular sieve obtained by the preparation method is a pure phase ZSM-5 molecular sieve with good crystallization. It can be seen that the crystal grains of the molecular sieve are well crystallized and the thickness is 50-100 nanometers.

Embodiment 3

[0052] Na in this example 2 O, Al 2 o 3 , SiO 2 , isopropylamine and H 2 The molar ratio of O is 0.15:0.05:1:0.2:100, and the seed crystal addition amount is 0.1%.

[0053] The difference from Example 1 is that step 1) add 0.75 grams of sodium metaaluminate and 0.72 grams of isopropylamine to 100 grams of water, stir and dissolve at room temperature, then add 13.6 grams of alkali to treat the silica sol dropwise, and add concentrated sulfuric acid dropwise Adjust the pH to 11.5 and add 0.004 g of ZSM-5 seed crystals. All the other steps are the same as in Example 1.

[0054] Figure 4 The SEM spectrum of the ZSM-5 molecular sieve obtained by the preparation method is a pure phase ZSM-5 molecular sieve with good crystallization. It can be seen that the crystal grains of the molecular sieve are well crystallized and the thickness is 50-100 nanometers.

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Abstract

The invention provides a nano-sheet-like ZSM-5 molecular sieve preparation method, which comprises the following steps: 1) uniformly mixing and stirring an aluminum source, a silicon source, a seed crystal, water and a template agent, and regulating the alkalinity to form a molecular sieve synthesis mother liquor; 2) aging under a stirring condition; and 3) after aging, carrying out crystallization to obtain the nano-sheet-like ZSM-5 molecular sieve. The preparation method is simple in process and low in cost, and can synthesize nano-sheet-like ZSM-5 without a special template agent and an expensive quaternary ammonium salt template agent, and the synthesized product has obvious advantages in catalytic reactions prone to carbon deposition, and particularly has great industrial applicationpotential in the catalytic fields of benzene/ethylene alkylation, benzene alkylation, toluene alkylation and the like.

Description

technical field [0001] The invention relates to a preparation method of a molecular sieve, in particular to a preparation method of a nanosheet ZSM-5 molecular sieve. Background technique [0002] ZSM-5 molecular sieve is widely used in catalytic fields such as petrochemical, coal chemical and fine chemical industries. It has two-dimensional ten-membered ring channels, one of which is a ten-membered ring straight channel, and the other is a ten-membered ring channel with a Zigzag shape: channel structure It is 0.51 nanometers × 0.55 nanometers ([100] direction) and 0.53 nanometers × 0.56 nanometers ([010] direction), belonging to the orthorhombic crystal system. [0003] The morphology of the molecular sieve has a significant impact on the performance of the catalyst. Because of its thin c-axis, the sheet-shaped ZSM-5 has a short diffusion path in the straight channel of the catalytic reaction and strong anti-coking ability, which can greatly improve the stability of the cat...

Claims

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Application Information

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IPC IPC(8): C01B39/44B01J29/40
CPCB01J29/40C01B39/445C01P2004/20C01P2004/62C01P2004/64
Inventor 李猛卓佐西杨文书
Owner WISON ENG
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