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ZSM-5 structure zeolite, preparation and use thereof

A ZSM-5 and zeolite technology, applied in the field of ZSM-5 structure zeolite, can solve the problems of difficulty in filtration/separation, increased difficulty in industrial production and application, etc., to solve the difficulty of filtration, solve the difficulty of separation between catalyst and liquid phase, and achieve good conversion. rate effect

Inactive Publication Date: 2004-09-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in actual operation, no matter in the synthesis process or in the separation of cyclohexene hydration reaction, the fine-grained zeolite is difficult to filter / separate due to the fine grain of zeolite, which is an increase for industrial production and application. Difficulty

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] This example illustrates the preparation of the zeolites provided by the invention.

[0022] Get 50 grams of commercially available ZSM-5 zeolite (commercial brand is ZRP-5, SiO 2 / Al 2 o 3 =60, primary particle diameter is 3μm, mesopore surface area is 8m 2 / g), put into 2 liters of concentration and be in the sodium hydroxide aqueous solution of 0.5 mole (record pH=11). Stir at a constant temperature of 80°C for 3 hours under reflux, filter, rinse with 100 ml of deionized water, exchange with 500 ml of 1 molar ammonium nitrate solution at a constant temperature of 90°C for 1 hour, filter, repeat the ammonium exchange once, filter, and The filter cake was dried at 110°C for 5 hours and calcined at 500°C for 3 hours.

[0023] The resulting zeolite product is designated as T1. Its SiO 2 / Al 2 o 3 = 41, the primary particle diameter measured by the electron microscope is 2.7 μm, and the mesopore surface area measured by the BET low-temperature nitrogen adsorption ...

Embodiment 2

[0032] This example illustrates the preparation of the zeolites provided by the invention.

[0033] Get 40 grams of commercially available ZSM-5 zeolite (commercial brand is ZRP-5, SiO 2 / Al 2 o 3 =60, primary particle diameter is 3μm, mesopore surface area is 8m 2 / g), put into 2 liters of concentration and be 0.5 mole sodium hydroxide aqueous solution (recording PH=11), under reflux at 85 ℃ of constant temperature stirring 2 hours, filter, rinse with 100 milliliters of deionized water, then use 500 ml of 1 molar ammonium nitrate solution was exchanged at 90°C for 1 hour at a constant temperature, filtered, repeated ammonium exchange once, filtered, and the filter cake was dried at 110°C for 5 hours and then roasted at 500°C for 3 hours.

[0034] The resulting zeolite product is designated as T2. Its SiO 2 / Al 2 o 3 =37, the primary particle diameter measured by the electron microscope is 2.5 μm, and the mesopore surface area measured by the BET low-temperature nitroge...

Embodiment 3

[0036] This example illustrates the preparation of the zeolites provided by the invention.

[0037] Get 20 grams of commercially available ZSM-5 zeolite (commercial brand is ZRP-5, SiO 2 / Al 2 o 3 =60, primary particle diameter is 3μm, mesopore surface area is 8m 2 / g), put into 3 liters of concentration and be 0.8 moles of sodium hydroxide aqueous solution (record pH=11.8), under reflux at 80 ℃ of constant temperature and stir for 1.5 hours, filter, rinse with 100 milliliters of deionized water, then use 500 ml of 1 molar ammonium nitrate solution was exchanged at 90°C for 1 hour at a constant temperature, filtered, repeated ammonium exchange once, filtered, the filter cake was dried at 110°C for 5 hours, and then roasted at 500°C for 3 hours.

[0038] The resulting zeolite product is designated as T3. Its SiO 2 / Al 2 o 3 =30, the primary particle diameter measured by the electron microscope is 2.1 μm, and the mesopore surface area measured by the BET low-temperature ni...

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Abstract

A ZSM-5 zeolite with 15-200 for the mole ration of silicon oxide to aluminium oxide, 0.5-10 microns for diameter, and 25-250 sq.m / g for mesopore surface area is prepared from the large-grain zeolite through treating in alkaline aqueous solution, ammonium ion exchanging, drying, and calcining. Said zeolite can be used to prepare cyclohexanol from cyclohexene by hydrating with high conversion rate, easy separation from liquid phase and easy filter.

Description

technical field [0001] The invention relates to a ZSM-5 structure zeolite, its preparation and application. More specifically, the present invention relates to a ZSM-5 zeolite with a specific physicochemical structure, its preparation method, and its application in the reaction of cyclohexene hydration 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 m...

Claims

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Application Information

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IPC IPC(8): B01J29/40C01B39/38
Inventor 王殿中舒兴田何鸣元
Owner CHINA PETROLEUM & CHEM CORP
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