Preparation method and application of hierarchical pore molecular sieve

A molecular sieve and multi-stage pore technology, applied in the field of molecular sieves, can solve the problems of high price, inability to carry out large-scale application, and low yield of furan ether compounds, and achieve low cost, good application prospects, and high conversion activity of furan compounds Effect

Active Publication Date: 2021-01-29
ZHEJIANG SUGAR ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the above literature reports, it can be seen that when the etherification reaction of furan compounds is catalyzed by molecular sieves, the yield of furan ether compounds is generally low, which is mainly due to the difficulty in effectively suppressing side reactions such as ring opening, hydration, transition etherification, and polymerization.
At the same time, at present, the preparation of multi-stage molecular sieves is mostly prepared by the double-template method, which is expensive and cannot be used in large-scale applications.

Method used

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  • Preparation method and application of hierarchical pore molecular sieve
  • Preparation method and application of hierarchical pore molecular sieve
  • Preparation method and application of hierarchical pore molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] Example 1 Sample 1 # preparation

[0100] Mix 0.54g of ammonium chloride and 100mL of deionized water in a 250mL three-necked flask, heat and reflux to 80°C under stirring, then add 2g of microporous ZSM-5 molecular sieve (silicon-aluminum atomic ratio is 12), continue stirring for 1h and use Wash with deionized water, filter, and dry at 100°C for 2 hours; repeat the above ammonium ion exchange operation twice, and the obtained sample is calcined at 550°C for 7 hours to obtain an acidic microporous ZSM-5 molecular sieve, which is designated as sample 1 # .

Embodiment 2

[0101] Example 2 Sample 2 # preparation

[0102] Mix 2g of sodium hydroxide, 1.8g of cetyltrimethylammonium bromide and 100mL of deionized water in a 250mL three-neck flask, heat and reflux to 80°C under stirring, then add 2g of microporous ZSM-5 molecular sieve (silicon The molar ratio of aluminum atoms is 12.5), continued stirring for 24 hours, washed with deionized water, filtered, dried at 100°C for 2 hours, and calcined at 550°C for 7 hours to obtain ZSM-5 molecular sieve after alkali treatment.

[0103] Mix 0.54g of ammonium chloride and 100mL of deionized water in a 250mL three-necked flask, heat and reflux to 80°C under stirring, then add ZSM-5 molecular sieve after alkali treatment, continue stirring for 1 hour, wash with deionized water, and filter. Dry at 100° C. for 2 hours; repeat the ammonium ion exchange operation twice, and roast the obtained sample at 550° C. for 6 hours to obtain acidic ZSM-5 molecular sieve after alkali treatment.

[0104] Mix 0.18g of oxa...

Embodiment 3

[0105] Example 3 Sample 3 # preparation of

[0106] Mix 2g of sodium hydroxide, 1.8g of cetyltrimethylammonium bromide and 100mL of deionized water in a 250mL three-neck flask, heat and reflux to 80°C under stirring, then add 2g of microporous ZSM-5 molecular sieve (silicon The molar ratio of aluminum atoms is 25), continue to stir for 24h, wash with deionized water, filter, dry at 110°C for 2h, and roast at 550°C for 6h to obtain ZSM-5 molecular sieve after alkali treatment.

[0107] Mix 0.54g of ammonium chloride and 100mL of deionized water in a 250mL three-necked flask, heat and reflux to 80°C under stirring, then add ZSM-5 molecular sieve after alkali treatment, continue stirring for 1 hour, wash with deionized water, and filter. Dry at 100°C for 2h; repeat the above ammonium ion exchange operation twice, and the obtained sample is calcined at 550°C for 7h to obtain an acidic ZSM-5 molecular sieve after alkali treatment, which is designated as sample 3 # .

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Abstract

The invention discloses a preparation method of a hierarchical pore molecular sieve, and the method comprises the following steps of: treating a to-be-treated molecular sieve in a solution containingalkali and a surfactant, and performing roasting to obtain an alkali-treated molecular sieve; carrying out ammonium exchange on the molecular sieve subjected to alkali treatment, and performing roasting to obtain an acidic molecular sieve subjected to alkali treatment; and putting the acidic molecular sieve subjected to alkali treatment into an acid-containing solution for treatment, and conducting roasting to obtain the hierarchical pore molecular sieve. According to the preparation method of the hierarchical pore molecular sieve, a commercial microporous molecular sieve is taken as a treatment object, and the hierarchical pore molecular sieve is prepared by adopting a simple acid-base post-treatment method. The hierarchical pore molecular sieve is used as a catalyst, and can efficientlycatalyze the etherification reaction of furan compounds to obtain high yield of furan ether compounds.

Description

technical field [0001] The application relates to a multi-level porous molecular sieve and its preparation method and application, belonging to the field of molecular sieves. Background technique [0002] With the continuous increase of global energy demand, the depletion of fossil energy and the increasingly serious environmental pollution, the development of processes for preparing fuels and chemicals from renewable biomass energy has attracted widespread attention. Biomass-based furan ether compounds are considered to be a class of biofuel additives with great development potential due to their high energy density, octane number and good fuel mixability. Molecular sieve catalysts have the advantages of easy separation, good thermal stability, renewability, and adjustable acidity, and are widely used in petrochemical and fine chemical industries. At present, there have been many reports on the preparation of furan ether compounds by using molecular sieves as catalysts to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40B01J29/70B01J35/10B01J37/30C07D307/46C07D307/44
CPCB01J29/40B01J29/7007B01J35/1061B01J35/1038B01J35/1042B01J35/1019B01J35/1023B01J37/30C07D307/46C07D307/44B01J2229/37B01J2229/38Y02P20/584
Inventor 王磊胡华雷张建金海涛杨勇胡丹鑫
Owner ZHEJIANG SUGAR ENERGY TECH CO LTD
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