Method for preparing fine-grain low silica/alumina ratio X zeolite

A technology of zeolite and grain size, which is applied in the field of preparation of small-grain X zeolite, can solve the problems that are not conducive to improving the adsorption efficiency and reducing the effective cage structure, so as to reduce the subsequent processing steps, reduce the synthesis cost, and simplify the operation steps. Effect

Active Publication Date: 2010-06-23
CHINA PETROLEUM & CHEM CORP +1
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The use of small grain X zeolite as the active component of the adsorbent is beneficial to increase the diffusion rate in the grain and improve the utilization rate of the zeolite, but the grain size of the zeolite should not be too low. The cage structure will be reduced, which is not conducive to improving the adsorption efficiency

Method used

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  • Method for preparing fine-grain low silica/alumina ratio X zeolite
  • Method for preparing fine-grain low silica/alumina ratio X zeolite
  • Method for preparing fine-grain low silica/alumina ratio X zeolite

Examples

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example 1

[0031] Small crystal X zeolites are prepared according to the process of the present invention.

[0032] (1) Preparation of directing agent

[0033] Add 10.3 grams of sodium metaaluminate solution (which contains Al 2 o 3 17.3% by mass, Na 2 (21.0 mass%), 55.9 gram deionized water and 13.3 gram sodium hydroxide, stir to make solid alkali dissolve completely, then add 55.3 gram sodium silicate solution (wherein contain SiO 2 28.3% by mass, Na 2 (08.8% by mass), stirred until uniformly mixed, 25 ℃ static aging 20 hours made the directing agent, and its molar composition was 16Na 2 O: Al 2 o 3 : 14.93SiO2 2 :318H 2 O.

[0034] (2) Preparation of X zeolite

[0035] At 25°C, add 214.2 grams of sodium silicate solution, 526 grams of deionized water, 42 grams of sodium hydroxide and 210 milliliters of sulfuric acid solution with a concentration of 2.5 mol / liter into a 2-liter stainless steel synthesis kettle, stir to make it fully mixed, and Add 213.2 grams of sodium metaa...

example 2

[0037] In the synthesis kettle, add 214.2 grams of sodium silicate solution, 715.4 grams of deionized water, 30 grams of sodium hydroxide and 33 grams of anhydrous sodium sulfate at 25 ° C, stir to dissolve them fully and mix them evenly, then add 206 grams of gram of sodium metaaluminate solution, then add the directing agent prepared by 24 gram examples 1, continue to stir until mixing evenly, the molar composition of the mixture that obtains is 4.7Na 2 O: Al 2 o 3 : 3.0 SiO 2 : 0.65SO 4 2- : 157.9H 2 O, and then heated to 98 ° C, static crystallization for 2 hours. The product was washed with water until the pH value of the washing solution was less than 10, filtered, and dried at 80°C for 12 hours to obtain the X zeolite product. The property data are shown in Table 1.

example 3

[0039] Get 102 grams of aluminum sulfate octadecahydrate and add it to 407 grams of deionized water, and stir until completely dissolved to make an aluminum sulfate solution. Add 214.2 grams of sodium silicate solution, 323 grams of deionized water and 62 grams of sodium hydroxide in the synthesis kettle, mix well, add 115 grams of sodium metaaluminate solution and the above-mentioned aluminum sulfate solution successively under stirring, and then add 24 grams of For the directing agent prepared in Example 1, continue stirring at 25°C until it is evenly mixed, and the molar composition of the obtained mixture is 4.32Na 2 O: Al 2 o 3 : 3.0 SiO 2 : 1.3SO 4 2- : 161H 2 O, and then heated up to 102°C for static crystallization for 2 hours. The product was washed with water until the pH value of the washing solution was less than 10, filtered, and dried at 80°C for 12 hours to obtain the X zeolite product. The property data are shown in Table 1.

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Abstract

A preparation method of small-grain low-silica-content X zeolite includes mixing silicon-containing compound, sodium hydroxide, water and sulfuric acid solution or water soluble sulfate, stirring and adding aluminum-containing compound to obtain gel, adding the directing agent to the gel to obtain the mixture with the molar composition of (2.5-5.0)Na2O:Al2O3:(2.4-3.0) SiO2:(0.5-2.0)SO4<2->:(80-200)H2O, standing and crystallizing at 80-120 DEG C for 0.5-3.0 hours, water washing, filtering and drying. The obtained X zeolite has a crystal grain of 0.2-1.2 Mum, the molar ratio of silica / alumina is 2.07-2.3, and the crystallinity is more than 95%.

Description

technical field [0001] The invention is a preparation method of X zeolite, in particular, a preparation method of small grain X zeolite. Background technique [0002] X zeolite is a kind of faujasite, its theoretical silicon / aluminum ratio (SiO 2 / Al 2 o 3 Molar ratio) is 2.0 to 3.0. Water glass, sodium metaaluminate, and sodium hydroxide are generally used as raw materials in industry, and prepared by aging and hydrothermal crystallization. The silicon / aluminum ratio of X zeolite obtained by conventional methods is generally about 2.5, and the grain size is 2-6 microns. [0003] In the application of zeolite, the performance of zeolite is usually closely related to physical indicators such as its grain size and structural silicon / aluminum ratio. By reducing the grain size of zeolite, the specific surface area can be increased and the pores can be shortened, thereby increasing the effective active sites and improving Diffusion rate within grains; lower structural Si / Al r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/22
Inventor 王辉国王德华马剑锋郁灼
Owner CHINA PETROLEUM & CHEM CORP
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