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

A technology of zeolite and crystal grain size, applied in the field of preparation of small crystal X zeolite, can solve problems such as unfavorable improvement of adsorption efficiency, reduction of effective cage structure, etc., and achieve the advantages of reducing subsequent processing steps, reducing synthesis cost and simplifying operation steps. Effect

Active Publication Date: 2008-09-03
CHINA PETROLEUM & CHEM CORP +1
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  • Description
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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

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

Experimental program
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Example Embodiment

[0030] Example 1

[0031] According to the method of the present invention, small-crystalline X zeolite is prepared.

[0032] (1) Preparation of directing agent

[0033] Add 10.3 g of sodium metaaluminate solution (which contains Al 2 O 3 17.3% by mass, Na 2 O 21.0% by mass), 55.9 grams of deionized water and 13.3 grams of sodium hydroxide, stir to completely dissolve the solid alkali, and then add 55.3 grams of sodium silicate solution (which contains SiO 2 28.3% by mass, Na 2 O 8.8% by mass), stir until the mixture is uniform, and statically aged at 25°C for 20 hours to prepare a directing agent, the molar composition of which is 16Na 2 O: Al 2 O 3 : 14.93SiO 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 / L to a 2 liter stainless steel synthesis kettle, stir to mix them thorough...

Example Embodiment

[0036] Example 2

[0037] In the synthesis kettle, add 214.2g of sodium silicate solution, 715.4g of deionized water, 30g of sodium hydroxide and 33g of anhydrous sodium sulfate at 25℃, stir to make it fully dissolved and mix well, then add 206 under stirring Gram of sodium metaaluminate solution, then add 24 grams of the directing agent prepared in Example 1, continue to stir until the mixture is uniform, the molar composition of the obtained mixture is 4.7Na 2 O: Al 2 O 3 : 3.0SiO 2 : 0.65SO 4 2- : 157.9H 2 O, then heated to 98°C, static crystallization for 2 hours. The product was washed with water until the pH value of the washing liquid 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 Embodiment

[0038] Example 3

[0039] Add 102 g of aluminum sulfate octahydrate to 407 g of deionized water, and stir until it is completely dissolved to prepare an aluminum sulfate solution. Add 214.2 grams of sodium silicate solution, 323 grams of deionized water and 62 grams of sodium hydroxide to the synthesis kettle, mix well, add 115 grams of sodium metaaluminate solution and the above-prepared aluminum sulfate solution under stirring, and then add 24 grams For the directing agent prepared in Example 1, continue to stir at 25°C until the mixture is uniform, and the molar composition of the obtained mixture is 4.32Na 2 O: Al 2 O 3 : 3.0SiO 2 : 1.3SO 4 2- : 161H 2 O, then heated to 102°C, static crystallization for 2 hours. The product was washed with water until the pH value of the washing liquid 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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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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