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Preparation and applications of heterogeneous catalyst containing MCM-41 mesoporous material

A technology of MCM-41 and catalyst, applied in the field of solid acid catalysis, can solve the problems of high price, low yield, unfavorable promotion and use, etc., and achieve the effects of large specific surface area, easy separation and simple preparation

Active Publication Date: 2017-06-30
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the use of metal salts and metal oxides to catalyze fructose can still obtain high HMF yields, its application is limited due to the difficulty of recycling homogeneous catalysts; ionic liquids have made great progress in fructose catalysis, but due to the preparation of ionic liquids The process is complex and expensive, which is not conducive to large-scale promotion and use; H-type zeolites or molecular sieves have attracted widespread attention, and unmodified zeolites or molecular sieves still have disadvantages such as low yields in catalyzing the conversion of fructose

Method used

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  • Preparation and applications of heterogeneous catalyst containing MCM-41 mesoporous material
  • Preparation and applications of heterogeneous catalyst containing MCM-41 mesoporous material
  • Preparation and applications of heterogeneous catalyst containing MCM-41 mesoporous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Take by weighing 100mg fructose, the Zr-salen-MCM-41 catalyst of 50mg joins in the 25mL reactor that fills 2mLDMSO;

[0033] (2) Replace DMSO in (1) with other solvents, such as NMP, DMA, DMF, THF, DMSO-H 2 O mixture (wherein DMSO and H 2 The volume ratio of O is 1.5:0.5, 1:1, 0.5:1.5), DMSO-[AMIM]Cl (the volume ratio of DMSO to [AMIM]Cl is 1.5:0.5, 1:1, 0.5:1.5) ;

[0034] (3) The above reactor was placed in an oil bath at 140°C and stirred for 4-5 hours. After the reaction was cooled, 50 μL of the reacted solution was diluted to 10 mL with deionized water, and the yield of 5-HMF was determined by HPLC. The results are shown in Table 1.

[0035] Table 1 Solid acid catalyst catalyzes the 5-HMF yield of fructose reaction in different solvents

[0036]

Embodiment 2

[0038] (1) Take by weighing 100mg fructose, the Zr-salen-MCM-41 catalyst of 50mg joins in the 25mL reactor that fills 2mLDMSO;

[0039] (2) Replace 50 mg of Zr-salen-MCM-41 in (1) with 30, 40, 60 mg;

[0040] (3) Cool after the above reaction is completed, place the above reactor in an oil bath at 140°C and stir for 4 hours, after the reaction is cooled, take 50 μL of the reacted solution and dilute it to 10 mL with deionized water, and measure the 5-HMF yield by HPLC , the result is as figure 1 shown. The results showed that the yields of 5-HMF obtained by using 30, 40, 50, and 60 mg of catalysts were 74.0%, 76.8%, 92.0%, and 89.9%, respectively.

Embodiment 3

[0042] (1) Weigh 100 mg of fructose, add 50 mg of Zr-salen-MCM-41 catalyst into a 25 mL reactor containing 2 mL of DMSO, place the reactor in an oil bath at 140° C. and stir for 4 h;

[0043] (2) Set the temperature of the oil bath in (1) to 120, 130, 150°C and stir for 4 hours;

[0044] (3) After the above reaction is completed, cool down, take 50 μL of the reacted solution and dilute it into 10 mL with deionized water, and measure the 5-HMF productive rate with HPLC, the results are as follows figure 2 shown. The results showed that with the increase of time, the yield of HMF gradually increased, and at 140°C, the maximum yield of HMF was 92.0%. °C is the optimum reaction temperature.

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Abstract

The invention discloses preparation and applications of a heterogeneous catalyst containing a MCM-41 mesoporous material, and belongs to the technical field of solid acid catalysis, wherein the chemical formula of the heterogeneous catalyst is Zr-Salen-MCM-41. According to the present invention, the synthesis step is simple, the raw material is inexpensive and easily-available, and the prepared catalyst simultaneously contains the Lewis acid site and the bronsted site, and can efficiently catalyze the dehydration of fructose to produce 5-HMF; and the catalyst after the reaction is easy to separate and can be recycled a plurality of times so as to meet the green sustainable development requirement.

Description

technical field [0001] The invention relates to the preparation and application of a heterogeneous catalyst containing MCM-41 mesoporous material, belonging to the technical field of solid acid catalysis. Background technique [0002] With the development of the world economy, the global demand for fossil raw materials such as oil and natural gas is rising sharply, and due to the excessive development and consumption of these precious resources, they are facing a crisis of depletion; at the same time, the impact of fossil energy on environmental pollution is also becoming more and more serious. The sustainable development of human beings is seriously threatened. Therefore, it is imminent to make full use of renewable and degradable resources to alleviate the energy crisis, and it is also a hot spot of current research. Biomass resources are considered as a promising resource because of their large reserves, renewable and low cost. At present, the hot spot of biomass energy...

Claims

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Application Information

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IPC IPC(8): C07D307/46B01J31/22
CPCB01J31/22B01J2531/48C07D307/46
Inventor 王海军袁文文吴春炎黄义
Owner JIANGNAN UNIV
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