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Preparation method for catalyst containing MFI structure zeolite

A molecular sieve and catalyst technology, applied in the field of catalyst preparation, can solve the problems of low conversion rate of cyclohexanone oxime, complex fluidized bed process, high requirements on catalyst performance, etc., and achieve high conversion rate, good selectivity and good regeneration performance Effect

Inactive Publication Date: 2011-11-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The fluidized bed process is complicated, the equipment investment cost and operating cost are all high, and the conversion rate of cyclohexanone oxime is on the low side in the reaction process, only about 98%; while the fixed bed process is simple, the equipment investment is low, and the operation is simple, but the catalyst is relatively low. Higher performance requirements, for example, the catalyst is required to have a good cyclohexanone oxime conversion rate (above 99.5%) and caprolactam selectivity (about 96%), as well as high mechanical properties, and the crushing strength (σ) is required to reach 60N / cm
But so far there is no relevant report on the preparation method of non-microspherical catalysts applied to fixed bed technology

Method used

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  • Preparation method for catalyst containing MFI structure zeolite
  • Preparation method for catalyst containing MFI structure zeolite
  • Preparation method for catalyst containing MFI structure zeolite

Examples

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example 1

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

[0028] The preparation process of all-silicon molecular sieve: Pour ethyl orthosilicate (abbreviated as TEOS) into a beaker at room temperature, stir for 30 minutes, add 22.5% tetrapropylammonium hydroxide (abbreviated as TPAOH) solution In ethyl silicate, stir and hydrolyze at room temperature for 3 to 5 hours, add water to form a sol, stir evenly to obtain a molar concentration of TPAOH / SiO 2 =0.22, EtOH / SiO 2 = 4, H 2 O / SiO 2 =18 mixture, transfer the above mixture into a stainless steel reactor lined with polytetrafluoroethylene, crystallize at 100°C for 3 days, filter, wash, dry at 120°C for 24 hours, and calcinate at 550°C for 5 hours to obtain a silicon molecular sieve. The BET specific surface area of ​​the silica molecular sieve product is 439 meters 2 / G, the outer surface is 58 meters 2 / G, the particle size is 0.1~0.2μm, the si...

example 2

[0042] The preparation process of silicon molecular sieve: Pour ethyl orthosilicate into a beaker at room temperature, stir for 30 minutes, add 22.5% tetrapropylammonium hydroxide solution to ethyl orthosilicate, stir and hydrolyze 3~5 at room temperature After hours, add water to form a sol, stir evenly, and get the molar concentration of TPAOH / SiO 2 =0.15, EtOH / SiO 2 = 4, H 2 O / SiO 2 = 25, transfer the above mixture into a stainless steel reactor lined with polytetrafluoroethylene, crystallize at 100°C for 3 days, filter, wash, dry at 120°C for 24 hours, and calcinate at 550°C for 5 hours to obtain silicon molecular sieve. The BET specific surface area of ​​the silica molecular sieve product is 435 meters 2 / G, the outer surface is 42 meters 2 / G, the particle size is 0.1-0.2μm, and the silicon / aluminum ratio reaches more than 50,000. X-ray diffraction spectrum has figure 1 Features; TEM photos have figure 2 Characteristics.

[0043] 170 grams of silica molecular sieve dry ba...

example 3

[0048] The preparation process of silicon molecular sieve: Pour ethyl orthosilicate into a 1000 ml beaker at room temperature, stir for 30 minutes, add 22.5% tetrapropylammonium hydroxide aqueous solution, stir and hydrolyze at room temperature for 3 hours, add water, stir evenly, and make The chemical composition of the mixed clear liquid is H 2 O / SiO 2 =10, EtOH / SiO 2 =4, TPAOH / SiO 2 =0.18, crystallization at 110°C for 2 days, filtration, washing, drying at 120°C for 24 hours, and baking at 550°C for 5 hours.

[0049] The BET specific surface area of ​​the silica molecular sieve product is 435 meters 2 / G, the outer specific surface is 52 meters 2 / G, the particle size is 0.1-0.2μm, and the silicon / aluminum ratio reaches more than 50,000. X-ray diffraction spectrum has figure 1 Features; TEM photos have figure 2 Characteristics.

[0050] 46.2 grams of silica molecular sieve dry basis, 30 grams of alkaline silica sol (produced by Yueyang, Hunan, SiO 2 The content is 30%, pH=9.0)...

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Abstract

The invention relates to a preparation method for a catalyst containing a MFI structure zeolite. The method is characterized in that: raw materials comprising the MFI structure zeolite and alkaline silica sol are subjected to mixing, forming, drying and baking to obtain a baked product, then the baked product contacts a alkaline buffer solution of a nitrogen compound, wherein a pH value of the alkaline silica sol is 9-11, a weight ratio of the MFI structure zeolite to the alkaline silica sol (according to a SiO2 content) is 1-50:1.

Description

Technical field [0001] The present invention relates to a preparation method of a catalyst containing MFI structure molecular sieve, and more specifically, the present invention relates to a preparation method of a catalyst containing MFI structure molecular sieve for preparing caprolactam by gas-phase Beckman rearrangement of cyclohexanone oxime method. Background technique [0002] Caprolactam, the product of the Beckmann rearrangement reaction of cyclohexanone oxime, is the main raw material for the production of three series of nylon, industrial cord and nylon engineering plastics. Its demand has been strong. It is expected that the world's caprolactam demand will exceed 4 million in 2004 Ton. The domestic caprolactam gap has always been large, and the annual import volume is generally above 300,000 tons. With the increase in consumption in the future, the caprolactam gap will be even greater. [0003] Industrially, the Beckmann rearrangement reaction of cyclohexanone oxime a...

Claims

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Application Information

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IPC IPC(8): B01J29/89B01J29/40B01J29/035C07D223/10C07D201/04
CPCY02P20/52
Inventor 程时标涂椿滟张树忠谢丽闵恩泽
Owner CHINA PETROLEUM & CHEM CORP
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