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Process for synthesizing ZSM-5 molecular sieve

A ZSM-5 and seed crystal technology, applied in the field of synthesizing ZSM-5 molecular sieve, can solve the problems of reducing the production efficiency per unit kettle volume, increasing the production cost of molecular sieve, expensive silica gel, etc. Yield effect

Inactive Publication Date: 2004-06-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When water glass is used as raw material, due to the gelation process, the amount of water must be increased to ensure heat and mass transfer, which reduces the production efficiency per unit volume of the kettle; while using solid silica gel as raw material can reduce the ratio of water to silicon, but the price of silica gel More expensive, increasing the production cost of molecular sieves

Method used

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  • Process for synthesizing ZSM-5 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The diatomite raw soil is produced in Changbai, Jilin, and it is crushed to a finer than 40 meshes, and its reduction on ignition is 16.6%. The weight percentage composition is shown in Table 1.

[0021] SiO 2

[0022] NaOH, perbasic sodium metaaluminate (composed of Al 2 o 3 =44.4g / l, Na 2 O=291.8g / l), NaY (produced by the Catalyst Factory of Qilu Petrochemical Company) was added into water, and stirred evenly. Add the above-mentioned diatomite raw soil, and configure the mole fraction to be SiO 2 / Al 2 o 3 =40,Na 2 O / SiO 2 =0.1,H 2 O / SiO 2 =10, NaY / diatomaceous earth=0.05 (weight fraction) system, continue stirring. Stir and crystallize in a pressure vessel and raise the temperature to 120°C, keep the temperature constant for 4 hours, then raise the temperature to 180°C, and keep the temperature constant for 16 hours. After cooling, filter, wash, and dry, the X-ray diffraction spectrum of the obtained sample is shown in the accompanying drawing, ...

Embodiment 2

[0024] The raw diatomite in Example 1 was treated with 30% sulfuric acid at 90°C for 6 hours, filtered, washed, and dried. This diatomite is hereinafter referred to as refined soil, and its calcined reduction is 8.2%. The weight percentage composition is shown in the table 2:

[0025] SiO 2

[0026] Other conditions are the same as in Example 1, and the X-ray diffraction spectrum of the obtained sample has the characteristics of the accompanying drawings, which is a ZSM-5 molecular sieve with a crystallinity of 94%.

Embodiment 3

[0028] Add NaOH and perbasic sodium metaaluminate into water and stir well. Add fine soil and configure the mole fraction as SiO 2 / Al 2 o 3 =40,Na 2 O / SiO 2 =0.1,H 2 O / SiO 2 =10 system, continue to stir. Stir and crystallize in a pressure vessel and raise the temperature to 120°C, keep the temperature constant for 4 hours, then raise the temperature to 180°C, and keep the temperature constant for 16 hours. After cooling, filter, wash, and dry, the X-ray diffraction pattern of the obtained sample has the characteristics of the accompanying drawings, which is a ZSM-5 molecular sieve with a crystallinity of 54%.

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Abstract

The invention provides a process for synthesizing ZSM-5, characterized in that, diatomaceous soil is used as a silicon source, and total or part of aluminum source to be mixed with other aluminum source, NaOH and water, 0-10 wt.% molecular sieve is added in as seed crystal to prepare slurry of reaction mixture, performing water thermal crystallization in normal condition. The process can reduce gelatification, increase solid content and reduce the cost.

Description

technical field [0001] The invention relates to a method for synthesizing ZSM-5 molecular sieve. Background technique [0002] ZSM-5 molecular sieve is a high-silicon five-membered ring (Pentasil) zeolite, which was first successfully developed by Mobil Company (USP3702886). Because of its high silicon-aluminum ratio, unique pore structure and excellent thermal and hydrothermal stability, it is widely used in many chemical processes and other fields. The synthesis method of ZSM-5 molecular sieve has also been developed from the classic organic method using organic ammonium as a template to the synthesis method without ammonium. The silicon sources mainly used in the synthesis are mainly water glass and solid silica gel. When water glass is used as raw material, due to the gelation process, the amount of water must be increased to ensure heat and mass transfer, which reduces the production efficiency per unit volume of the kettle; while using solid silica gel as raw materia...

Claims

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Application Information

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IPC IPC(8): C01B39/38
Inventor 朱斌舒兴田汝迎春林民
Owner CHINA PETROLEUM & CHEM CORP
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