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Preparation method of europium oxide (EUO) type molecular sieve

A molecular sieve and seed crystal technology, which is applied in the field of EUO molecular sieve preparation, can solve the problem of too long crystallization time, and achieve the effects of reducing particle size, increasing supersaturation and improving crystallization speed.

Active Publication Date: 2011-05-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although adding seeds and inorganic salts shortens the crystallization time, the crystallization time is still too long

Method used

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  • Preparation method of europium oxide (EUO) type molecular sieve
  • Preparation method of europium oxide (EUO) type molecular sieve
  • Preparation method of europium oxide (EUO) type molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Add 1.83g of sodium hydroxide, 0.85g of sodium aluminate, and 87.7ml of distilled water to the beaker successively, stir well, then add 40ml of ethanol, 18.3ml of trimethylamine, 6.48ml of 1,6-dibromohexane, stir for 10min, and finally add 10.14g of white carbon black and 0.4g of unroasted EU-1 molecular sieve seed crystals were stirred for 1 hour and then charged into a synthesis kettle. Heated in an oven at 80°C for 3h, then heated to 180°C for 96h to crystallize. When reaching 180°C, the pressure of the synthesis tank is 1.2MPa. The obtained product was filtered, washed with distilled water until neutral, dried, and calcined at 550° C. for 5 hours to obtain EU-1 molecular sieve.

[0051] The XRD spectrum and scanning electron microscope photo of EU-1 molecular sieve are as figure 1 , 2 shown. It can be seen from the XRD spectrum that in the spectrum, the diffraction peaks at 2θ=7.90°, 8.80°, (23.11±4.2)° are the main characteristic peaks of EU-1 molecular sieve. ...

Embodiment 2

[0053] Add 1.83g sodium hydroxide, 0.80g sodium aluminate, 87.7ml distilled water to the beaker successively, stir well, then add 14ml ethanol, 20ml acetone, 18.3ml trimethylamine, 6.48ml 1,6-dibromohexane, stir for 10min , and finally add 10.14g white carbon black and 0.4g unroasted EU-1 molecular sieve seed crystals, stir for 1 hour and then put into the synthesis kettle. After sealing, fill the synthesis kettle with high-pressure nitrogen to 0.1 MPa. Heated in an oven at 70°C for 4h, then heated to 170°C for 120h of crystallization. When reaching 170°C, the pressure of the synthesis kettle is 0.9MPa. The obtained product was filtered, washed with distilled water until neutral, dried, and calcined at 550° C. for 5 hours to obtain EU-1 molecular sieve.

[0054] The XRD spectrum and scanning electron microscope photo of EU-1 molecular sieve are as image 3 , 4 shown. It can be seen from the XRD spectrum that in the spectrum, the diffraction peaks at 2θ=7.90°, 8.80°, (23.1...

Embodiment 3

[0056] Add 5.93g of sodium hydroxide, 3.81g of sodium aluminate, and 257ml of distilled water to the beaker successively, stir evenly, then add 85ml of ethanol, 38.26ml of benzyldimethylamine, and 29.18ml of benzyl chloride, stir for 10 minutes, and finally add 84.3g of white Carbon black and 3.37g uncalcined EU-1 molecular sieve seed crystals were stirred for 1 hour and then charged into the synthesis kettle. Heated in an oven at 60°C for 3h, then heated to 180°C for 96h of crystallization. When reaching 180°C, the pressure of the synthesis tank is 0.91MPa. The obtained product was filtered, washed with distilled water until neutral, dried, and calcined at 550°C for 5 hours to obtain ZSM-50 molecular sieve.

[0057] The XRD spectrogram and scanning electron microscope photo of ZSM-50 molecular sieve are as Figure 5 , 6 shown. It can be seen from the XRD spectrum that in the spectrum, the diffraction peaks at 2θ=7.90°, 8.80°, (23.11±4.2)° are the main characteristic peaks...

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Abstract

The invention provides a preparation method of a europium oxide (EUO) type molecular sieve. The preparation process comprises the steps: adding one or more of ethanol, propylene glycol, methyl alcohol and acetone with a proper amount to be taken as an organic solvent; filling a high-pressure inert gas into a high-pressure kettle, and carrying out sectional type crystallization under a certain condition; filtering and washing the product to be neutral; and drying, roasting to obtain the EUO molecular sieve. The organic solvent is added, so that a template agent precursor is promoted to be dissolved in an aqueous phase, and the generation of a template agent is accelerated; and therefore, the crystallization speed of the molecular sieve is accelerated, and the crystallization time of the molecular sieve is remarkably shortened.

Description

technical field [0001] The invention relates to a molecular sieve and a preparation method thereof, in particular to a preparation method of an EUO type molecular sieve. Background technique [0002] EUO structure molecular sieve is a medium-porous high-silicon molecular sieve with a one-dimensional network microporous channel structure, including a ten-membered ring straight-through channel (the diameter of the hole is 0.58×0.41nm) and a twelve-membered ring side pocket vertically connected to it. (0.68×0.58×0.81 nm in size) structure. Due to the particularity of the channel, EUO molecular sieves exhibit excellent catalytic performance in reactions such as xylene isomerization, linear alkane isomerization, and hydrodewaxing, and have good industrial application prospects. [0003] EUO structure molecular sieves include EU-1, TPZ-3 and ZSM-50 molecular sieves, which generally have the following anhydrous chemical formula: 1~100XO 2 : 0~10T 2 o 3 : 0-20R, X represents sil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 张志智刘全杰张喜文秦波
Owner CHINA PETROLEUM & CHEM CORP
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