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A kind of preparation method of aluminum-free MFI structure spherical molecular sieve catalyst

A spherical molecular sieve, molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of difficult molding content, low crushing strength, etc.

Active Publication Date: 2015-12-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to solve the problems that aluminum-free molecular sieves are difficult to form, have low content and low crushing strength, and provide a method for preparing a spherical molecular sieve catalyst with an aluminum-free MFI structure on the basis of the existing rolling forming technology. The molecular sieve content High crushing strength can meet the requirements of fixed bed and moving bed reactors

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0029] The preparation process of all-silicon-1 molecular sieve: Pour ethyl orthosilicate (abbreviated as TEOS) into a beaker at room temperature, stir for 30 minutes, and use 22.5% tetrapropylammonium hydroxide (abbreviated as TPAOH) solution Add it to tetraethyl orthosilicate, stir and hydrolyze for 3 to 5 hours at room temperature, add water to form a sol, stir evenly, and obtain a molar concentration of TPAOH / SiO 2 =0.2,EtOH / SiO 2 =4,H 2 O / SiO 2 =20 mixture, move the above mixture into a stainless steel reactor lined with polytetrafluoroethylene, crystallize at 100°C for 3 days, filter, wash, and dry at 120°C for 24 hours to obtain a full silicon- 1 molecular sieve (referred to as RBS-1).

[0030] (1) Put 2kg of 200-500 mesh RBS-1 in the turntable molding machine. The diameter of the turntable used in the turntable molding machine is 1.2m, the depth of the turntable is 450mm, the inclination angle of the turntable is determined to be 50°, and the speed of the turntable ...

example 2

[0035] (1) Crush 2kg of HTS-1 (aluminum-free TS-1 molecular sieve with MFI structure, produced by Hunan Jianchang Petrochemical Co., Ltd., a commercial brand, with a molecular sieve solid content of about 85%) into 200-500 meshes, and place in In the turntable forming machine, the turntable diameter of the turntable rotary forming machine used is 1.2m, the depth of the turntable is 450mm, the inclination angle of the turntable is determined to be 46°, and the rotation speed of the turntable is set at 28rpm. Spray about 1.5 kg of deionized water therein to obtain spherical particles with a diameter of about 0.2 to 0.6 mm.

[0036] (2) Separately crush the HTS-1 molecular sieve into 200-600 mesh, mix it with 30% alkaline silica sol (pH value 9-10) at a weight ratio of 2.0:1 and re-pulverize it, and take the particles smaller than 20 mesh Add 120kg to the turntable molding machine at a constant speed, finish adding within 180min, and sieve through 13 mesh and 10 mesh sieves to ob...

example 3

[0042] (1) Put 2kg of 200-500 mesh RS-1 (MFI structure all-silicon-1 molecular sieve, produced by Hunan Jianchang Petrochemical Co., Ltd., commercial brand, molecular sieve solid content 85%) in the rotary forming machine, which uses a rotary The diameter of the turntable of the rotary molding machine is 1.2m, the depth of the turntable is 450mm, the inclination angle of the turntable is determined to be 50°, and the rotation speed of the turntable is set at 30rpm. Spray about 1.5 kg of deionized water therein to obtain spherical particles with a diameter of about 0.2-0.8 mm.

[0043] (2) In addition, crush RS-1 molecular sieve into 200-800 mesh, mix it with 30% alkaline silica sol at a weight ratio of 2.2:1 and crush it again, take particles smaller than 30 mesh and add 120kg to the turntable molding machine at a constant speed, Finish adding within 240min. Sieve through 12-mesh and 9-mesh sieves to obtain spherical catalysts with a diameter of 1.7 to 2.2 mm and about 90 kg ...

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Abstract

The invention relates to a preparation method of an aluminum-free MFI structure spherical molecular sieve catalyst. The method includes the steps of: molding an aluminum-free MFI structure molecular sieve, then contacting the molded molecular sieve with an alkaline buffer solution of a nitrogen-containing compound. Specifically, the molding process of the aluminum-free MFI structure molecular sieve consists of: under the rotating operation conditions of a turntable molding machine, (1) placing a molecular sieve raw material of 200-500 meshes in the turnable molding machine to undergo mixing contact with water and / or a binder, thus obtaining spherical particles with a diameter of 0.1-1mm; (2) then adding a molecular sieve raw material of 100-1000 meshes and the binder to obtain a spherical catalyst with a diameter of 1.5-2.5mm; and (3) drying and roasting the spherical catalyst. The spherical molecular sieve catalyst prepared by the method has a high molecular sieve content, crushing strength of 1.5-5.0kg / particle, and can satisfy the technological requirements of fixed-bed and moving-bed reactors.

Description

technical field [0001] The invention relates to a method for preparing a catalyst containing a molecular sieve with an MFI structure, more specifically, the invention relates to a method for preparing a spherical molecular sieve catalyst with an aluminum-free MFI structure. Background technique [0002] All-silicon Silicalite-1 molecular sieve was successfully synthesized for the first time in 1978 by E.M.Flanigen of UCC, etc., and belongs to the last member of the "Pentasil" family. All-silicon Silicalite-1 is an aluminum-free all-silicon-1 molecular sieve with MFI topological structure. It is the simplest molecular sieve in the ZSM-5 structural molecular sieve family. Its skeleton only contains silicon atoms and oxygen atoms. The structural unit is SiO 4 tetrahedron. Silicalite-1 has a rich microporous structure and regular and uniform three-dimensional fine channels. It has a definite crystal structure of ZSM-5 molecular sieve, high internal specific surface area, good ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/035B01J35/08
Inventor 程时标涂椿滟张树忠谢丽凌云
Owner CHINA PETROLEUM & CHEM CORP
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