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Process for preparing small crystal ZSM-5 zeolite

A ZSM-5, small-grain technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the difficulty of industrial production and application, the decrease of product yield, and the filtration process. Difficulties and other problems, to achieve the effect of simplifying the production process, improving the yield and improving the conversion rate

Active Publication Date: 2006-01-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the preparation process, because the crystal grains of zeolite are too fine, the filtration process of separating zeolite and water phase becomes the most difficult step in industrial production, and it will also cause a decrease in product yield, which increases the difficulty for industrial production and application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] This example illustrates the preparation process of the small-grain ZSM-5 zeolite provided by the present invention.

[0029] (1) Preparation of silica-alumina gel

[0030] Get 100 grams of water glass (containing 28.8% SiO 2 and 8.9% Na 2 O) add 10 grams of sodium aluminate solution (containing 7.9% Al 2 o 3 and 12.3% Na 2 (0), stir evenly, and then dropwise add 25% sulfuric acid solution under stirring until the pH value of the solution is 6. The obtained gel is washed with water, dried, and then ion-exchanged with ammonium nitrate according to the weight ratio of silica gel: ammonium nitrate: water = 1:0.5:10, and the gel after exchange is washed with water, dried, and calcined at 500°C to obtain Silica-alumina gel required for zeolite.

[0031] The analytical result of the silica-alumina gel is: Na 2 O4 ＝ 2 / Al 2 o 3 =60; the pore volume is 0.8 ml / g.

[0032] (2) Preparation process of small grain ZSM-5 zeolite

[0033] Mix 40 grams of the 80-120 mesh si...

Embodiment 2

[0037] This example illustrates the preparation process of the small-grain ZSM-5 zeolite provided by the present invention.

[0038] (1) Preparation of silica-alumina gel

[0039] Get 100 grams of water glass (containing 28.8% SiO 2 and 8.9% Na 2 O) add 10 grams of sodium aluminate solution (containing 7.9% Al 2 o 3 and 12.3% Na 2(0), stir evenly, and then dropwise add 25% sulfuric acid solution under stirring until the pH value of the solution is 9, and heat up to 80° C. for 1 hour at a constant temperature. The obtained gel is washed with water, dried, and then ion-exchanged with ammonium nitrate according to the weight ratio of silica gel: ammonium nitrate: water = 1:0.5:10, and the gel after exchange is washed with water, dried, and roasted at 500°C to obtain the synthesis Silica-alumina gel required for zeolite.

[0040] The analytical result of the silica-alumina gel is: Na 2 O4 ＝ 2 / Al 2 o 3 =60; the pore volume is 0.52 ml / g.

[0041] (2) Preparation process ...

Embodiment 3

[0054] This example illustrates the preparation process of the small-grain ZSM-5 zeolite provided by the present invention.

[0055] (2) Preparation of silica-alumina gel

[0056] Get 100 grams of water glass (containing 28.8% SiO 2 and 8.9% Na 2 O) add 4.7 grams of sodium aluminate solution (containing 7.9% Al 2 o 3 and 12.3% Na 2 (0), stir evenly, and then dropwise add 25% sulfuric acid solution under stirring until the pH value of the solution is 8. The obtained gel is washed with water, dried, and then ion-exchanged with ammonium nitrate according to the weight ratio of silica gel: ammonium nitrate: water = 1:0.5:10, and the gel after exchange is washed with water, dried, and roasted at 500°C to obtain the synthesis Silica-alumina gel required for zeolite.

[0057] The analytical result of the silica-alumina gel is: Na 2 O4 ＝ 2 / Al 2 o 3 =120; the pore volume is 0.68 ml / g.

[0058] (2) Preparation process of small grain ZSM-5 zeolite

[0059] 40 grams of the ab...

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Abstract

The preparation process of small crystal grain ZSM-5 zeolite includes the following steps: mixing alumino sillica gel grain in SiO2 / Al2O3 molar ratio of 20-600 and granularity of 20-300 mesh and water solution of organic template agent, and hydrothermal crystallization of the mixture with or without ZSM-5 zeolite crystal seed; and once filtering, drying and roasting. The said process can preparing ZSM-5 zeolite product with Si / Al molar ratio of 15-200 and initial crystal granularity of 0.1-0.5 micron. The process uses no sodium ion material, needs no ammonium exchange, filtering and roasting process, and thus has high zeolite product yield and simplified production process. The zeolite product is used in the catalyst for hydrolyzing cyclohexene to prepare cyclohexanol and has high cyclohexanol converting rate.

Description

technical field [0001] The invention relates to a preparation method of ZSM-5 zeolite. More specifically, the present invention relates to a method for preparing small-grain ZSM-5 zeolite used in the hydration of cyclohexene to prepare cyclohexanol. Background technique [0002] Cyclohexanol is an important chemical product and chemical raw material, which is currently produced by the hydration method of cyclohexene. The catalyst used in it was an inorganic acid such as sulfuric acid in the early stage, but the product and the catalyst were mixed together and it was difficult to separate and recover; there were a large number of side reactions in the reaction, which made it difficult to purify the product; once the catalyst was deactivated, it was difficult to regenerate. For this reason, it is proposed to use solid catalysts, such as ion exchange resins. However, ion exchange resins have poor mechanical strength and poor heat resistance, resulting in low catalyst activity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38
Inventor 王殿中冯强舒兴田何鸣元
Owner CHINA PETROLEUM & CHEM CORP
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