ZSM-5-based hierarchical porous molecular sieve material and preparation method thereof

A ZSM-5, molecular sieve technology, applied in the directions of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of increasing the synthesis cost, increasing the complexity of the synthesis process, and being unfavorable for large-scale production, etc. Achieve the effect of reducing dosage, good micro-mesoporous distribution, and good mesoporous distribution

Inactive Publication Date: 2014-09-10
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, there are many synthetic approaches for hierarchically porous molecular sieve materials based on ZSM-5, but these methods have certain shortcomings.
For example, the use of raw materials and templates with special properties to induce the simultaneous generation of micropores and mesopores (macropores) usually requires pretreatment of raw materials or complex preparation processes or adding additional raw materials during the preparation of gels And need post-processing to remove, these processes not only increase the cost of synthesis, but also increase the complexity of the synthesis process, which is not conducive to large-scale industrial production

Method used

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  • ZSM-5-based hierarchical porous molecular sieve material and preparation method thereof
  • ZSM-5-based hierarchical porous molecular sieve material and preparation method thereof
  • ZSM-5-based hierarchical porous molecular sieve material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0045] Under stirring conditions, prepare the following two working solutions respectively:

[0046] Mixture I: a homogeneous solution prepared with 1.39g of aluminum sulfate, 1.57g of sodium hydroxide and 10g of deionized water;

[0047] Mixture II: 17.27g silica sol (40% SiO 2 , 60%H 2 O, hereinafter the same), 0.92g tetrapropylammonium bromide (99%), 10g deionized into the beaker and mix well.

[0048] Under constant stirring, the two mixtures are mixed, and continue to be strongly stirred until uniform, and the mass ratio of the obtained reaction mixture is Na 2 O: Al 2 o 3 : SiO 2 : (TPA) 2 O: H 2 O=9.0:1.0:55:0.82:825, transfer the obtained initial gel to a reaction kettle with a polytetrafluoroethylene liner, seal it and place it in a hydrothermal synthesis oven, and keep the temperature at 80°C for 24h. Then be warming up to 175 DEG C and continue constant temperature 24h. After the reaction kettle was cooled, the solid was separated from the mother liquor, th...

Embodiment 2

[0051] Under stirring conditions, prepare the following two working solutions respectively:

[0052] Solution I: a uniform solution prepared with 1.27g of aluminum sulfate, 1.91g of sodium hydroxide and 10g of deionized water;

[0053] Solution II: Put 8.61g of silica sol, 0.23g of tetrapropylammonium bromide, and 10g of deionized into a beaker and mix well.

[0054] With constant stirring, combine the two mixtures and continue stirring vigorously until homogeneous. The molar ratio of the initial gel is Na 2 O: Al 2 o 3 : SiO 2 : (TPA) 2 O: H 2 O=12.0:1.0:30:0.23:750. The obtained initial gel was transferred to a reaction kettle with a polytetrafluoroethylene liner, sealed and placed in a hydrothermal synthesis oven. The temperature was first kept at 80°C for 24h, and then the temperature was raised to 175°C for 30h. After the reaction kettle was cooled, the solid was separated from the mother liquor, the solid was washed with deionized water until neutral, dried at 12...

Embodiment 3

[0056] Under stirring conditions, prepare the following two working solutions respectively:

[0057] Solution I: a uniform solution prepared by 0.25g aluminum sulfate, 0.25g sodium hydroxide and 10g deionized water;

[0058] Solution II: Add 11.20g silica sol, 0.40g tetrapropylammonium bromide, and 10g deionized into a beaker and mix well.

[0059] With constant stirring, combine the two mixtures and continue stirring vigorously until homogeneous. The molar ratio of the initial gel is Na 2 O: Al 2 o 3 : SiO2 : (TPA) 2 O: H 2 O=8.2:1.0:200:2.0:4000. The obtained initial gel was transferred to a reaction kettle with a polytetrafluoroethylene liner, sealed and placed in a hydrothermal synthesis oven. The temperature was first kept at 80°C for 12h, and then the temperature was raised to 170°C for 16h. After the reaction kettle was cooled, the solid was separated from the mother liquor, the solid was washed with deionized water until neutral, dried at 120°C in air, and then ...

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Abstract

The invention discloses a ZSM-5-based hierarchical porous molecular sieve. The dimension of the ZSM-5-based hierarchical porous molecular sieve material prepared in the invention is 100nm-20[mu]m; when the dimension of the ZSM-5 molecular sieve is greater than 1[mu]m, the ZSM-5 molecular sieve has a cruciate flower morphology, every individual is formed by accumulating nanometer crystals, and a gap among the nanometer crystals forms a mesopore; or when the dimension of the ZSM-5 molecular sieve is not greater than 1mum, the ZSM-5 molecular sieve has a nanometer rod plug self-assembling morphology characteristic, and a gap among nanometer rods forms a mesopore. The ZSM-5-based hierarchical porous molecular sieve is prepared by adopting cheap raw materials through a one step method with tetrapropyl ammonium bromide as a template. The method has the advantages of low cost and simple operation, and the obtained hierarchical porous molecular sieve material has good physical and chemical properties and a catalysis characteristic, and is suitable for the industrial production.

Description

technical field [0001] The invention relates to a hierarchical porous molecular sieve material, in particular to a hierarchical porous molecular sieve material with controllable size and shape based on ZSM-5 nanocrystal stacking or plugging and a preparation method thereof. Background technique [0002] ZSM-5 molecular sieve belongs to the "pentaisl" family of high-silica shape-selective molecular sieves. It has a three-dimensional channel system, which is composed of sinusoidal channels parallel to the a-axis direction (the corner is 150°) and straight channels parallel to the b-axis. The pore diameter is about 0.54nm. Due to the high silicon-aluminum ratio of the skeleton, the molecular sieve has high thermal and hydrothermal stability, strong acidity and hydrophobicity, and because of its unique pore structure and high carbon deposition resistance, it can be used in shape selective The field of catalysis plays an important role. Especially in terms of increasing propyle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38C01B39/40
Inventor 李春义于庆君
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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