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ZSM-5 type molecular sieve and method for preparing the same

A ZSM-5, molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of no aluminum source found, no aluminum source found, and achieve the effect of reducing the cost of raw materials

Active Publication Date: 2006-07-19
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The inventor has gone through a large amount of literature research, has not seen the report that utilizes perlite, medical stone, montmorillonite, bentonite to synthesize ZSM-5 molecular sieve, also does not find to utilize cheap clay (kaolin) and utilize clay (kaolin) to remove and other mineral raw materials other than diatomaceous earth as raw materials for the synthesis of ZSM-5 molecular sieves, and the research reports on the preparation of ZSM-5 molecular sieves by the cheap seed crystal method have not been found to use natural minerals (or processed natural minerals) The raw material is used as the aluminum source for the synthesis of ZSM-5 molecular sieve, and the report on the preparation of ZSM-5 molecular sieve by the cheap seed crystal method

Method used

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  • ZSM-5 type molecular sieve and method for preparing the same
  • ZSM-5 type molecular sieve and method for preparing the same

Examples

Experimental program
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Effect test

Embodiment 1

[0059] Using commercially available 400-mesh perlite (product of Dalian Zhongde Perlite Factory, see attached table 1 for composition) as raw material, 15 g was roasted in a muffle furnace at 700°C for 5 hours. Water glass (containing SiO 2 20.9 wt%, Na 2 O 6.9wt%) 200g, 1.5g ZSM-5 seed crystal (Nankai University Catalyst Factory, silicon-aluminum ratio 38), distilled water 350g, concentration is that the about 55g of 3M sulfuric acid aqueous solution and the perlite after roasting process drop into stainless steel reactor, stir The mixture was formulated into a gel (pH about 11.0) in 40 minutes. The molar ratio of each component in the gel according to its oxide is: SiO 2 / Al 2 o 3 =49; (Na 2 O+K 2 O) / SiO 2 =0.26;H 2 O / SiO 2 =33. After sealing, heat up to 180°C and crystallize at a constant temperature for 24 hours under stirring. After the crystallization is completed, cool and filter to remove the mother liquor, wash and dry the filter cake to obtain a crystalli...

Embodiment 2

[0062] Using fine-grained commercially available kaolin as raw material (50% of the particle size is not greater than 3.1 μm, see attached table 2 for the composition), 15 g was roasted in a muffle furnace at 950° C. for 6 hours. Water glass (containing SiO 2 20.9 wt%, Na 2 (06.9wt%) 200g, 2g ZSM-5 crystal seed (commercially available commodity of Nankai University Catalyst Factory, silicon-aluminum ratio 38), water 250g, concentration is that the kaolin after the about 55g of 3M sulfuric acid and the above-mentioned roasting process drops into the stainless steel reactor, Stir for 30 minutes to form a mixture gel (pH about 10.6). The molar ratio of each component in the gel according to its oxide is: SiO 2 / Al 2 o 3 =14; (Na 2 O+K 2 O) / SiO 2 =0.26;H 2 O / SiO 2 =28. After the stainless steel reactor was sealed, the temperature was raised to 180°C for crystallization for 20 hours. After the crystallization is completed, the temperature is lowered, the mother liquor i...

Embodiment 3

[0065] All reaction raw materials are with example 2, and wherein kaolin roasting condition is 930 ℃ of roasting 7 hours, with water glass 250g, 1g ZSM-5 crystal seed (Nankai University Catalyst Factory, silicon-aluminum ratio 38), deionized water 300g, and roasting treatment The last 18g of kaolin is dropped into the stainless steel reactor, and the molar ratio of the oxide in the gel is: SiO 2 / Al 2 o 3 =14; (Na 2 O+K 2 O) / SiO 2 = 0.26. Under stirring, add 1M nitric acid aqueous solution to adjust the pH value of the system to about 10.5, and stir for 30 minutes. After the stainless steel reactor was sealed, the temperature was raised to 150°C for crystallization for 10 hours, and then the temperature was raised to 180°C for 10 hours for crystallization. After the crystallization is completed, the mother liquor is removed by filtration, and the filter cake is washed and dried to obtain a crystallized product. As determined by X-ray diffraction, the phase is ZSM-5 mole...

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Abstract

The invention provides a preparation method for small-size ZSM-5 molecular sieve. Wherein, using pearlite and montmorillonite as material for aluminum, adding crystal seed for crystallization reaction on hydrothermal condition, and obtaining a small-size product with 5~95% ZSM-5 that can be used to prepare modified ZSM-5 molecular sieve by different post-treatment method or as the active intergradient or carrier for catalyst. This invention cuts the cost more.

Description

technical field [0001] The invention belongs to molecular sieve and its preparation technology. Specifically, it involves the process of using natural minerals to provide all or part of the aluminum source needed for the synthesis of ZSM-5, and at the same time using the seed crystal method to synthesize small particle ZSM-5 molecular sieves. Background technique [0002] Since ZSM-5 molecular sieve was first reported by Mobil Corporation of the United States in 1972 (USP3702886), it has been applied in many oil refining and chemical processes due to its unique pore structure and shape-selective catalysis. Its preparation method is also constantly improved, from the initial synthesis using organic amine templates to the later synthesis without amines, which significantly reduces the manufacturing cost of ZSM-5, and then through post-modification of the synthesized ZSM-5 molecular sieve product The progress of treatment and other technologies has continuously expanded the ap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38B01J29/40
Inventor 申宝剑王萍何丽瑞刘佳刘涛高金森郭巧霞
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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