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Hierarchical porous molecular sieve and preparation method thereof

A molecular sieve and multi-level pore technology, which is applied in the directions of fauhhedral crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc. The operation process is complicated, the template agent is expensive, etc., to achieve good environmental and economic benefits, high yield, and effective utilization.

Active Publication Date: 2019-03-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above methods can obtain molecular sieves containing both mesopore and micropore structures, the templates used are expensive, the synthesis operation process is complicated, and all involve the use of a large number of micropore directing agents, so the cost is high and the environmental pollution is serious. , not suitable for large-scale industrial applications

Method used

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  • Hierarchical porous molecular sieve and preparation method thereof
  • Hierarchical porous molecular sieve and preparation method thereof
  • Hierarchical porous molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The enzymolysis residue used is enzymolysis corn stalk residue. The specific process is: after the corn stalk is pretreated by steam explosion, it is enzymatically hydrolyzed by cellulase to convert most of the cellulose and hemicellulose in the straw into hydrolyzed sugar. The enzymolysis residue was obtained after liquid separation. On a dry basis, the lignin content in the dry basis is 60wt%, the cellulose content is 8wt%, the hemicellulose content is 2wt%, the ash content is 18wt%, and the soluble component is 12wt%. After testing, the main components and contents in the ash are: C 7wt%, O37wt%, Si 32wt%, Fe, Ca, Na and other metal ions 22%, other 2%.

[0034] Concrete preparation process is as follows:

[0035] (1) Crush the residue of enzymatically hydrolyzed corn stalks to 100-200 mesh, and vacuum-dry at 80°C for 24 hours.

[0036](2) Take 1L of deionized water, 1L of ethanol, and 10g of NaOH to prepare a mixed solution, add 100g of pretreated corn stalk residu...

Embodiment 2

[0042] The same enzymatic hydrolysis of corn stalk residue as in Example 1 was used.

[0043] (1) Crush the residue of enzymatically hydrolyzed corn stalks to 100-200 mesh, and dry in vacuum at 50°C for 24 hours.

[0044] (2) Take 0.5L deionized water, 0.5L ethanol, and 1g NaOH to prepare a mixed solution, add 100g of pretreated corn stalk residue, heat up to 180°C, stir for 3 hours, and filter after the reaction is completed. The filtrate was rotary evaporated to obtain 35 g of earth brown enzymatic lignin.

[0045] (3) Wash the filter residue with water until neutral, dry at 80°C for 5 hours, add 7mL of 7wt% NaOH lye per gram of filter residue, treat at 100°C for 12 hours, and filter to obtain solution A.

[0046] Step (4) is the same as in Example 1. The characteristics of the prepared hierarchical porous ZSM-5 molecular sieve are shown in Table 1.

Embodiment 3

[0048] The same enzymatic hydrolysis of corn stalk residue as in Example 1 was used.

[0049] (1) Crush the enzymatically hydrolyzed corn stalk residue to 100-200 mesh, and vacuum-dry at 100°C for 12 hours.

[0050] (2) Take 1.2L of deionized water, 1.8L of ethanol, and 27g of NaOH to prepare a mixed solution, add 100g of the residue of enzymatically hydrolyzed corn stalks after pretreatment, mix well, heat up to 220°C, stir for 1 hour, and filter after the reaction is completed. The filtrate was rotary evaporated to obtain 55 g of earth brown enzymatic lignin.

[0051] (3) Wash the filter residue with water until neutral, dry at 120°C for 2 hours, add 3 mL of 10wt% NaOH lye per gram of filter residue, treat at 120°C for 8 hours, and filter to obtain solution A.

[0052] Step (4) is the same as in Example 1. The characteristics of the prepared hierarchical porous ZSM-5 molecular sieve are shown in Table 1.

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Abstract

The invention relates to a hierarchical porous molecular sieve and a preparation method thereof. The preparation method includes crushing enzymolysis residue, and drying; mixing the treated enzymolysis residue with a mixed liquid containing ethanol and a base, allowing reacting at 180-220 DEG C for certain time, filtering, and evaporating moisture from filtrate to obtain enzymatically hydrolyzed lignin; washing produced filter residue with water, drying, adding an alkaline liquid to treat for certain time, and filtering to obtain solution A; preparing a molecule sieve by a hydrothermal synthetic process, adding a certain amount of the solution A into molecular sieve mother liquor, centrifuging the product, washing, drying, and calcining to obtain the hierarchical porous molecular sieve. The enzymolysis residue is used herein to prepare the hierarchical porous molecular sieve; the hierarchical molecular sieve with high yield and rich mesopores can be attained; waste is effectively utilized, and economy is evidently improved.

Description

technical field [0001] The invention belongs to the field of biomass energy, and in particular relates to a multi-stage molecular sieve and a preparation method thereof. Background technique [0002] Hierarchical molecular sieves contain pore structures of different scales. At the same time, they combine the excellent hydrothermal stability of microporous molecular sieve crystals and the excellent diffusion and transport properties of mesoporous and macroporous materials. They show more excellent performance than traditional microporous molecular sieves in the field of catalysis. performance. [0003] At present, the synthesis methods of hierarchical porous molecular sieves mainly include post-treatment method and template method. Post-treatment methods mainly include high temperature heat treatment, steam heat treatment, acid treatment, alkali treatment, etc. However, the mesopores obtained by the post-processing method are irregular and often accompanied by the collapse ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38C01B39/36C01B39/24C01B39/22C01B39/02
CPCC01B39/02C01B39/22C01B39/24C01B39/36C01B39/38C01P2002/72C01P2002/82C01P2004/03C01P2004/61
Inventor 张通白富栋李政王领民乔凯
Owner CHINA PETROLEUM & CHEM CORP
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