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Y/silicate compound molecular sieve and method for preparing same

A technology of composite molecular sieve and pure silicon molecular sieve, applied in the field of new composite catalytic materials and their preparation, to achieve the effect of increasing straight chain alkanes

Active Publication Date: 2010-01-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] No compound molecular sieve with Y molecular sieve as core and pure silicon molecular sieve as shell and its preparation method have been found in the published patent technology

Method used

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  • Y/silicate compound molecular sieve and method for preparing same
  • Y/silicate compound molecular sieve and method for preparing same
  • Y/silicate compound molecular sieve and method for preparing same

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preparation example Construction

[0021] (1) Preparation of reaction mixture gel

[0022] Mix Y-type molecular sieve, sodium hydroxide, distilled water, templating agent and silicon source evenly under stirring to make a reaction mixture gel, and the molar ratio of each component is as follows:

[0023] (0~1.3)Na 2 O:(34.4~110)H 2 O:(0.75~11.3)SiO 2 : (0.046~0.7)R, SiO 2 / Y (mass ratio) = 0.1 ~ 7; the preferred ratio is: (0 ~ 1.2) Na 2 O:(42~97)H 2 O:(1~8)SiO 2 : (0.072~0.6)R, SiO 2 / Y (mass ratio) = 0.2 ~ 5; in the formula, R represents the template agent, and Y represents the Y-type molecular sieve;

[0024] (2) Crystallization

[0025] The reaction mixture gel prepared in (1) is crystallized at 80-180°C for 12-70h, the optimum temperature is 100-160°C, and the optimum crystallization time is 14-48h.

[0026] (3) After the crystallization is completed, a core-shell composite molecular sieve is obtained by suction filtration and washing.

[0027] The preparation method of the reaction mixture gel de...

Embodiment 1

[0038] Add 1.0g of sodium hydroxide, 45ml of distilled water, and 12g of NaY to the beaker successively, stir well, then add 15ml of tetrapropylammonium hydroxide aqueous solution (the content of tetrapropylammonium hydroxide is 25wt%), stir for 10min, and finally add 32ml of silicon Sol (SiO 2 content is 30wt%), stirred for 3 hours, loaded into synthetic bombs, and crystallized in an oven at 120°C for 32 hours. Then the obtained product is washed with distilled water until it becomes neutral to obtain a Y / Silicalite-I composite molecular sieve.

[0039] The XRD spectrum and scanning electron microscope photos of the composite molecular sieve are as follows: figure 1 , 2 shown. As can be seen from the XRD spectrum, in the spectrum, the diffraction peaks at 2θ=7.90°, 8.80°, (23.11±0.42)° are the main characteristic peaks of Silicalite-I, and 2θ=6.1°, 10.1°, 11.8°, The diffraction peaks at 15.6°, 18.6°, and 20.2° are characteristic peaks of Y-type molecular sieves. It shows...

Embodiment 2

[0041] Add 1.8g sodium hydroxide, 55ml distilled water, 9g USY molecular sieve to the beaker successively, stir evenly, then add 11ml tetrapropyl ammonium hydroxide, stir for 10min, finally add 32ml silica sol, stir for 3h, put into synthetic bomb, Crystallize in an oven at 160°C for 20h. Then the obtained product was washed with distilled water to neutrality to obtain USY / Silicalite-I composite molecular sieve.

[0042] The XRD spectrum and scanning electron microscope photos of the composite molecular sieve are shown in image 3 , 4 . It can be seen from the XRD spectrum that there are main characteristic peaks of Silicalite-I and USY molecular sieves in the spectrum. It shows that the synthetic sample contains both Silicalite-I molecular sieve and Y-type molecular sieve. The content of Y molecular sieve in the compound molecular sieve is 33wt%. From the SEM photos, it can be clearly seen that the Y / Silicalite-I composite molecular sieve has a core-shell structure, the ...

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Abstract

The invention discloses a Y / silicate compound molecular sieve and a method for preparing the same. The compound material has XRD characteristic diffraction peaks of the Y molecular sieve and a pure silicon molecular sieve. The structure of the compound molecular sieve is a closely combined nucleus-shell type structure taking the Y molecular sieve as the nucleus and the pure silicon molecular sieve as the shell. The compound molecular sieve is prepared by a one-step hydrothermal crystallization method, and the Y molecular sieve is used as the nucleus molecular sieve and buried in the gel of the pure silicon molecular sieve, so that the synthetic process is not related to the complicated preparation steps, and the preparation method is simple. In the compound molecular sieve, the Y molecular sieve used as the nucleus can provide the acid catalysis property, and the pure silicon molecular sieve used as the shell can provide the shape selecting function, so that the Y / silicate compound molecular sieve can be used for all kinds of shape-selective reaction.

Description

technical field [0001] The invention relates to a novel composite catalytic material and a preparation method thereof, in particular to a preparation method of a composite molecular sieve with Y as the core and pure silicon molecular sieve as the shell. Background technique [0002] Molecular sieves are named for their shape selectivity, which is mainly due to the shape-selective effect of molecular sieve channels on reactants, intermediates and products. However, the outer surface of the molecular sieve does not have such shape selectivity, and the acidity of the outer surface of the molecular sieve has an opposite effect on the shape selectivity of the molecular sieve. For this reason, there have been many inventions about eliminating the acidity of the outer surface of molecular sieves to improve the selectivity of molecular sieves. Hydrothermal crystallization method, that is, a layer of inert pure silicon molecular sieve is grown on the outer surface of the acidic mole...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/08
Inventor 张志智张喜文凌凤香孙万付范峰
Owner CHINA PETROLEUM & CHEM CORP
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