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Method for preparing catalyst containing molecular sieve of MFI structure

A molecular sieve and catalyst technology, applied in the field of catalyst preparation, can solve the problems of insufficient caprolactam selectivity and insufficient crushing strength, and achieve the effects of high crushing strength and high selectivity

Active Publication Date: 2009-07-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to overcome the insufficient crushing strength of the molecular sieve catalyst containing the MFI structure in the prior art, the conversion rate of cyclohexanone oxime and the selection of caprolactam when it is used for the gas phase Beckmann rearrangement of cyclohexanone oxime to prepare caprolactam In order to solve the disadvantages of not being high enough, to provide a molecular sieve catalyst containing MFI structure with high crushing strength, the conversion rate of cyclohexanone oxime and the high selectivity of caprolactam when it is used in the gas-phase Beckmann rearrangement of cyclohexanone oxime to prepare caprolactam Preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] This example illustrates the preparation method of the catalyst containing molecular sieve with MFI structure of the present invention.

[0028] With 90 gram all-silicon molecular sieves (by the all-silicon molecular sieve that the embodiment 1 in CN1338427A makes), 44 gram alkaline silica sols (SIGAM-ALDRICH reagent, model is Ludox AS-40, SiO 2 content of 40% by weight, pH=9.4), 25 grams of ammonia water with a concentration of 26% by weight, 4.5 grams of turnip powder, and 5.6 grams of water were mixed and ground for 30 minutes to obtain a mixture. In this mixture, SiO in basic silica gel 2The weight ratio to all silicon molecular sieve is 1:5.1.

[0029] Then the mixture was extruded into a mold with a volume of 300 ml and a diameter of 1.5 mm, dried, and calcined at 580° C. for 8 hours to obtain a calcined product.

[0030] The above-mentioned roasted product after 95 grams is mixed with the alkaline buffer solution of 950 grams of nitrogenous compounds (the alkal...

Embodiment 2

[0035] Prepare the catalyst according to the method of Example 1, the difference is that the alkaline buffer solution of the nitrogen-containing compound is obtained by mixing ammonia water and ammonium acetate aqueous solution, the concentration of the ammonia water is 20% by weight, and the concentration of the ammonium acetate aqueous solution is 20% by weight %, the weight ratio of ammonia water to ammonium acetate aqueous solution is 2:3, and the pH value of the alkaline buffer solution of the nitrogen-containing compound is 10.65. Catalyst A2 containing molecular sieve with MFI structure was finally obtained.

Embodiment 3

[0037] The catalyst is prepared according to the method of Example 1, and the difference is that the alkaline buffer solution of the nitrogen-containing compound is obtained by mixing ammonia and ammonium carbonate solution, the concentration of the ammonia solution is 25% by weight, and the concentration of the ammonium carbonate solution is 7.5% by weight, the weight ratio of ammonia water to ammonium carbonate aqueous solution is 3:2, and the pH value of the alkaline buffer solution of the nitrogen-containing compound is 10.88. Catalyst A3 containing molecular sieve with MFI structure was finally obtained.

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Abstract

The invention provides a method for preparing a catalyst containing MFI-structure molecular sieves. The method comprises the steps of molding, drying and roasting a mixture containing the MFI-structure molecular sieves and a SiO2 carrier, wherein the method also comprises the step of allowing a product obtained after roasting to be in contact with an alkaline buffer solution of nitrogen-containing compounds. The catalyst containing MFI-structure molecular sieves, which is prepared by the method has high crushing strength, and can be used for a fixed bed process for preparing caprolactam by cyclohexanone-oxime gas phase Beckmann rearrangement. In addition, when the catalyst prepared by the method is used to perform the gas-phase Beckmann rearrangement reaction of cyclohexanone-oxime, both the conversion rate of cyclohexanone-oxime and the selectivity of caprolactam are high.

Description

technical field [0001] The invention relates to a preparation method of a catalyst containing molecular sieve with MFI structure. Background technique [0002] Caprolactam is the main raw material for the production of three series of products including nylon, industrial cord and nylon engineering plastics, and its demand has been relatively strong. The caprolactam is generally obtained by Beckmann rearrangement of cyclohexanone oxime. At present, the liquid phase rearrangement process using concentrated sulfuric acid or oleum as a catalyst is usually used in industry. The caprolactam produced by this process accounts for about 90% of the world's total production of caprolactam, but this process needs to consume a large amount of sulfuric acid and ammonia water. Generally, 1.3-1.8 tons of ammonium sulfate will be produced as a by-product for every ton of caprolactam produced, and the production cost is relatively high. In addition, the use of sulfuric acid will cause probl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40C07D201/04
CPCY02P20/52
Inventor 程时标张树忠慕旭宏闵恩泽
Owner CHINA PETROLEUM & CHEM CORP
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