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A modification method of all-silicon beta molecular sieve containing three-membered ring

A technology of molecular sieves and three-membered rings, applied in molecular sieve catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problems of harsh synthesis conditions, non-green synthesis process, unfavorable environmental protection, etc., and achieve simple and feasible process and regular structure Effect

Active Publication Date: 2022-01-04
CHINA UNIV OF MINING & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] All-silicon Beta molecular sieves are not easy to obtain through in-situ synthesis. In-situ synthesis generally requires hydrofluoric acid as a mineralizer. The synthesis process is not green and is not conducive to environmental protection.
CN111333082A and CN105800624A disclose the synthesis method of all-silicon Beta molecular sieves. They all used fluorine-containing mineralizers in the process of in-situ synthesis of all-silicon Beta molecular sieves. The synthesis conditions are relatively harsh, and the requirements of green environmental protection cannot be realized.

Method used

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  • A modification method of all-silicon beta molecular sieve containing three-membered ring
  • A modification method of all-silicon beta molecular sieve containing three-membered ring
  • A modification method of all-silicon beta molecular sieve containing three-membered ring

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Experimental program
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Effect test

Embodiment 1

[0046] Such as figure 2 As shown, take 630 grams of nitric acid (mass fraction 65%-68%) and place it in a 500ml volumetric flask, then use deionized water to make up to 500ml to obtain a nitric acid solution, which is designated as A solution. Weigh 25g of Beta molecular sieve powder (Si / Al=10.6) and mix it with A solution evenly and transfer it to a round bottom flask. Place the round bottom flask in an oil bath and heat it through the oil bath at a temperature of 100°C. The heating rate is 1°C / min, the heating time is 12 hours, the magnet is placed at the bottom of the round bottom flask for stirring, and the outlet of the top of the round bottom flask is equipped with a serpentine condenser for condensation and reflux, and the dealuminated modified all-silicon Beta molecular sieve Si- Beta. The Si-Beta was washed several times with deionized water until the supernatant obtained after centrifugation had pH ≈ 7. The washed Si-Beta molecular sieves were placed in an oven an...

Embodiment 2

[0048] Such as image 3 As shown, take 630 grams of nitric acid (mass fraction 65%-68%) and place it in a 500ml volumetric flask, then use deionized water to make up to 500ml to obtain a nitric acid solution, which is designated as A solution. Weigh 25g of Beta molecular sieve raw powder (Si / Al=10.6) and mix it evenly with solution A, then transfer it to a round bottom flask, place the round bottom flask in an oil bath, and heat it through the oil bath at a temperature of 100°C , the heating rate is 1°C / min, the heating time is 12 hours, the magnet is placed at the bottom of the round bottom flask for stirring, and the outlet of the top of the round bottom flask is equipped with a serpentine condenser for condensing and reflux, that is, the dealuminated modified all-silicon Beta molecular sieve Si -Beta. The Si-Beta was washed several times with deionized water until the supernatant obtained after centrifugation had pH ≈ 7. The washed Si-Beta molecular sieves were placed in ...

Embodiment 3

[0050] if Figure 4 As shown, take 630 grams of nitric acid (mass fraction 65%-68%) and place it in a 500ml volumetric flask, then use deionized water to make up to 500ml to obtain a nitric acid solution, which is designated as A solution. Weigh 25g of Beta molecular sieve raw powder (Si / Al=10.6) and mix it evenly with solution A, then transfer it to a round bottom flask, place the round bottom flask in an oil bath, and heat it through the oil bath at a temperature of 100°C , the heating rate is 1°C / min, the heating time is 12 hours, the magnet is placed at the bottom of the round bottom flask for stirring, and the outlet of the top of the round bottom flask is equipped with a serpentine condenser for condensing and reflux, that is, the dealuminated modified all-silicon Beta molecular sieve Si -Beta. The Si-Beta was washed several times with deionized water until the supernatant obtained after centrifugation had pH ≈ 7. The washed Si-Beta molecular sieves were placed in an o...

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Abstract

The invention provides a method for modifying an all-silicon Beta molecular sieve containing a three-membered ring and a Lewis acid, belonging to the field of petrochemical industry. Firstly, the Beta molecular sieve with a Si / Al ratio higher than 10 is used as the raw powder, and then it is completely dealuminated by a nitric acid solution, and then deionized water is used to balance the acid-base of the dealuminated thick Beta molecular sieve to obtain a full-silicon The Beta molecular sieve is then dried, and then put into a muffle furnace for roasting to obtain an all-silicon Beta molecular sieve containing a three-membered ring and a Lewis acid. This method avoids the use of fluorine-containing mineralizers in in-situ synthesis, and is environmentally friendly; the obtained all-silicon Si-Beta molecular sieve contains a three-membered ring structure and effective Lewis acid sites, and can be used for the isomerization of olefins. The steps are simple, the preparation is quick and environmentally friendly.

Description

technical field [0001] The invention relates to a method for modifying a three-membered ring-containing all-silicon Beta molecular sieve, which belongs to the field of petrochemical industry. Background technique [0002] Molecular sieves are widely used in the petrochemical industry due to their adjustable acid properties and unique pore structure. The acid properties of molecular sieves essentially determine the application and catalytic performance of molecular sieves. The acidic modulation of molecular sieves is difficult to control, and it is difficult to obtain molecular sieves with only Lewis acid. The Lewis acid in molecular sieves is mainly derived from non-framework aluminum species, and it is impossible to only exist in non-framework aluminum species in molecular sieves, generally there will be both framework aluminum and non-framework aluminum species, so in general molecular sieves there will be both acid and Lewis acid. Molecular sieves exist only Acids or...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08B01J29/70C07C5/25C07C11/09C07C11/08C07C11/02
CPCC01B39/08B01J29/7007C07C5/25C01P2002/82C01P2002/72C01P2004/03C07C11/09C07C11/08C07C11/02
Inventor 伊凤娇杨勇曹景沛何育荣
Owner CHINA UNIV OF MINING & TECH
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