Preparation method of aluminum-enriched beta zeolite

A beta zeolite and aluminum-rich technology, which is applied in the field of preparation of aluminum-rich beta zeolite, can solve the problems of long crystallization time and achieve the effects of shortened crystallization time, high crystallinity and high yield

Active Publication Date: 2008-01-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, ethyl silicate and metal aluminum powder are used as raw materials, tetraethylammonium hydroxide is used as a template, and hydrofluoric acid is added at the same time, the gel

Method used

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  • Preparation method of aluminum-enriched beta zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～5

[0027] The raw materials and proportioning of Examples 1-5 are shown in Table 1. First prepare the silica-alumina co-gel, age the prepared silica-alumina co-gel at 20°C-220°C for 12-48 hours, then grind it into particles smaller than 20 mesh, and continue to heat it at 400°C, 500°C, 600°C, and 800°C respectively. ℃, 1200 ℃ for treatment. Control the appropriate ratio of raw materials, add tetraethylammonium hydroxide (TEAOH), water and hydrofluoric acid, after ultrasonic dispersion or mechanical stirring, and then put in the reactor for crystallization reaction. After crystallization for the required time, take out the water to cool, filter and wash the reacted material, and dry at 120°C to obtain aluminum-rich beta zeolite. The silicon-aluminum ratio and crystallinity of the product are shown in Table 1.

[0028] In Table 1, the standard method for testing the silicon-aluminum molar ratio data of the product beta zeolite is ICP analysis (referring to Zamechek W. Determinati...

example 6～10

[0032] The raw materials and proportioning of Examples 6-10 are shown in Table 2. First prepare the silica-alumina co-gel, age the prepared silica-alumina co-gel at 20°C-220°C for 12-48 hours, then grind it into particles smaller than 20 mesh, and continue to heat it at 450°C, 550°C, 650°C, and 860°C respectively. ℃, 1150 ℃ for 24h. Control the appropriate ratio of raw materials, add a certain amount of tetraethylammonium hydroxide, water and hydrofluoric acid, and disperse evenly through ultrasonic dispersion or mechanical stirring. Then put it in a reaction kettle for crystallization reaction, and the reacted material is filtered and washed, and dried at 120°C to obtain aluminum-rich beta zeolite.

[0033] The XRD spectrogram features of the samples of Examples 6-10 are the same as those in accompanying drawing 2.

[0034] Table 2

[0035] Example

[0036] Compared with the standard industrial agent β30, the XRD pattern of the aluminum-rich beta zeolite prepared...

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Abstract

The invention discloses a making method of allitic beta-zeolite, which comprises the following steps: making silica-alumina gel through silicon source and aluminium source under hydrolytic reagent; aging at 20-220 deg. c; roasting at 300-1400 deg. c; grinding the gel into silica-alumina source; adding the solution with ammonium tetraethyl cation, ammonium ion, fluorine ion and water; crystallizing; recycling the crystallized product as zeolite.

Description

technical field [0001] The present invention relates to a preparation method of crystalline silicate zeolite, more specifically to a preparation method of aluminum-rich beta zeolite. Background technique [0002] Beta zeolite was synthesized by the classic hydrothermal crystallization method for the first time in 1967 by the Mobile Company of the United States (Wadlinger R.L, Kerr G.T, Rosinski E.J.US 3308069). The zeolite has a unique three-dimensional pore structure and high catalytic activity for hydrocracking and hydroisomerization. After modification or loading of certain metal components, it can be used for hydrocracking, hydroisomerization, hydrofinishing and Petroleum refining and petrochemical processes such as hydrodewaxing and diesel decondensation. Said beta zeolite is synthesized in such a way that it will contain Na 2 O, Al 2 o 3 , TEAOH, SiO 2 The mixture with water is made into a slurry, and the crystallization reaction is carried out in an autoclave at ...

Claims

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Application Information

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IPC IPC(8): C01B39/04B01J20/18B01J29/06
Inventor 宋家庆宋守强曾光乐
Owner CHINA PETROLEUM & CHEM CORP
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