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ZSM-35 molecular sieve in the form of hollow aggregation and preparation method thereof

A technology of ZSM-35 and molecular sieve, which is applied to iron conglomerate crystalline aluminum silicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems of high dispersion of molecular sieves and the inability to form aggregated forms, and achieve uniform particle size and discharge The effect of less material and favorable structure

Active Publication Date: 2016-05-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At this time, the conventional dosage of sodium lignosulfonate only plays a role in dispersing, and the obtained molecular sieve has high dispersibility, and cannot form any cavity or hollow aggregation form.

Method used

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  • ZSM-35 molecular sieve in the form of hollow aggregation and preparation method thereof
  • ZSM-35 molecular sieve in the form of hollow aggregation and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Under mechanical stirring and ultrasonic conditions, dissolve sodium lignosulfonate into water, and then add sodium hydroxide, sodium aluminate, cyclohexylamine, and silica sol in sequence. The final material ratio satisfies: Al 2 o 3 / SiO 2 =33,OH - / SiO 2 =0.12, cyclohexylamine / SiO 2 =0.25,H 2 O / SiO 2 =50, sodium lignosulfonate content 2.7wt%. Firstly, the above mixture was ultrasonically (1KW / L) and stirred for 40 minutes at room temperature of 25°C to make the materials evenly mixed, and then aged for 3 hours under the same stirring and ultrasonic conditions. Finally, the aged mixture was put into a reactor for crystallization at 170° C. for 80 hours. The obtained product was washed with distilled water until neutral, dried at 120°C for 12 hours, and then calcined at 550°C for 5 hours to obtain a ZSM-35 molecular sieve hollow aggregate. Observed by a transmission electron microscope, it has a hollow structure with a size of 6.8 μm. The hollow wall is compos...

Embodiment 2

[0036] Under mechanical stirring and ultrasonic conditions, dissolve sodium lignosulfonate into water, and then add sodium hydroxide, sodium aluminate, cyclohexylamine, and silica sol in sequence. The final material ratio satisfies: Al 2 o 3 / SiO 2 =45,OH - / SiO 2 =0.17, ethylenediamine / SiO 2 =0.35,H 2 O / SiO 2 =50, sodium lignosulfonate content 3.5wt%. First, the above mixture is ultrasonically (2KW / L) and stirred for 40 minutes at room temperature of 25°C to make the materials evenly mixed, and then aged for 4 hours under the same stirring and ultrasonic conditions. Finally, the aged mixture was put into a reactor for crystallization at 175° C. for 72 hours. The obtained product was washed with distilled water until neutral, dried at 120°C for 12 hours, and then calcined at 550°C for 5 hours to obtain a ZSM-35 molecular sieve hollow aggregate. Observed by a transmission electron microscope, it has a hollow structure with a size of 10 μm. The hollow cavity wall is com...

Embodiment 3

[0038] Under mechanical stirring and ultrasonic conditions, dissolve sodium lignosulfonate into water, and then add sodium hydroxide, sodium aluminate, cyclohexylamine, and silica sol in sequence. The final material ratio satisfies: Al 2 o 3 / SiO 2 =36,OH- / SiO 2 =0.12, Ethylenediamine / SiO 2 =0.35,H 2 O / SiO 2 =67, sodium lignosulfonate content 4.2wt%. Firstly, the above mixture was ultrasonically (4KW / L) and stirred at room temperature of 25°C for 40 minutes to make the materials evenly mixed, and then aged for 4 hours under the same stirring and ultrasonic conditions. Finally, the aged mixture was put into a reactor for crystallization at 175° C. for 72 hours. The obtained product was washed with distilled water until neutral, dried at 120°C for 12 hours, and then calcined at 550°C for 5 hours to obtain a ZSM-35 molecular sieve hollow aggregate. Observed by a transmission electron microscope, it has a hollow structure with a size of 13 μm. The hollow cavity wall is co...

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Abstract

The invention discloses a ZSM-35 molecular sieve in the form of hollow aggregation and a preparation method thereof. The ZSM-35 molecular sieve is 2-20 [mu]m, preferably 5-15 [mu]m, in size. A hollow wall is composed of ZSM-35 micro-crystal grains being 50-2000 nm, preferably 100-1000 nm. The thickness of the hollow wall is 0.5-3.0 [mu]m, preferably 0.5-2.0 [mu]m. The preparation method includes the following steps: 1) uniformly mixing an aluminum source, a silicon source, alkali, water, sodium lignin sulfonate and a template agent under the combined effect of ultrasound dispersion and physical mixing; 2) continuously aging the mixture under the combined effect of the ultrasound dispersion and the physical mixing; and 3) crystallizing the material in the step 2), and washing, drying and roasting a product to prepare the ZSM-35 molecular sieve in the form of hollow aggregation. The ZSM-35 molecular sieve has uniform particle and is strong in controllability. The structure is beneficial to mass transmission of materials. The template agent is low in cost and easy to obtain and is easy to burn away, so that the molecular sieve is less in generated emission and is low in environment pollution, and has unique application prospect in the field of butene isomerization reaction.

Description

technical field [0001] The invention relates to a method for preparing a hollow-structure ZSM-35 molecular sieve, belonging to the technical field of molecular sieve synthesis. Background technique [0002] Microporous molecular sieve ZSM-35 can be widely used in the conversion process of hydrocarbons, such as isomerization, polymerization, aromatization and cracking, etc., and has a good application prospect. Molecular sieve materials have shapes such as rods, strips, blocks, or spheres. At present, the preparation of molecular sieves with hollow structures or their aggregates has aroused great interest. Because this special hollow structure often leads to some special properties of materials, especially in the fields of catalysis, adsorption, and controlled release of drugs. [0003] At present, molecular sieves in hollow form are mainly prepared by polystyrene microspheres as templates, combined with layer-by-layer self-assembly and hydrothermal or gas-phase conversion c...

Claims

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Application Information

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IPC IPC(8): C01B39/44
Inventor 杨卫亚凌凤香王少军沈智奇郭长友季洪海
Owner CHINA PETROLEUM & CHEM CORP
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