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A modified montmorillonite catalyst that catalyzes the preparation of 5-hydroxymethylfurfural from biomass sugar and its preparation method and application

A technology of hydroxymethyl furfural and biomass sugar, which is applied in the field of organic catalysis synthesis, can solve the problems of non-reusability, influence the recycling use of catalysts, etc., and achieves improved catalytic activity, improved conversion rate and product yield, and improved recycling use. effect of times

Active Publication Date: 2021-08-31
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this document, with glucose as raw material, although the productive rate of 5-hydroxymethylfurfural is higher (80.4%), it is mentioned in the text that a large amount of by-products (humin) are produced in the reaction process, which affects the performance of the catalyst. Recycled use, although washed with water, washed with alcohol, and ultrasonically treated, after 6 cycles, the conversion rate of glucose and the yield of 5-hydroxymethylfurfural dropped rapidly to 71.4% and 50.4%, basically no longer use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The 100g Ca-mont, AlCl 3 Content of 0.5mmol / L Al 0.1g of 3+ (AlCl 3 · 6h 2 O) was added to a three neck round bottom flask and stirred at 99 ℃ 6 hours to obtain a mixed solution, the mixed solution was cooled to room temperature, filtered off with suction washing and drying, to obtain an intermediate product leaving the sample stand. The intermediate product, AlCl 3Content of 0.5mmol / L Al 0.1g of 3+ (AlCl 3 · 6h 2 O) was added to a three neck round bottom flask and stirred at 99 ℃ 6 hours to obtain a mixed solution, the mixed solution was cooled to room temperature, filtered off with suction washing and drying. Named Al-mont-0.5-1, leaving aside like. Then Al-mont-0.5-1, AlCl 3 Content of 0.5mmol / L Al 0.1g of 3+ (AlCl 3 · 6h 2 O) was added to a three neck round bottom flask and stirred at 99 ℃ 6 hours to obtain a mixed solution, the mixed solution was cooled to room temperature, filtered off with suction washing and drying. Named Al-mont-0.5-2. So, the catalyst synthe...

Embodiment 2

[0037] The 100g Ca-mont, AlCl 3 Content of 1.5mmol / L Al 0.6g of 3+ (AlCl 3 · 6h 2 O) was added to a three neck round bottom flask, stirred at 40 ℃ 24 hours to obtain a mixed solution, the mixed solution was cooled to room temperature, washed by suction filtration and drying to give an intermediate product, leaving the sample stand. The intermediate product, AlCl 3 Content of 1.5mmol / L Al 0.6g of 3+ (AlCl 3 · 6h 2 O) was added to a three neck round bottom flask, stirred at 40 ℃ 24 hours to obtain a mixed solution, the mixed solution was cooled to room temperature, filtered off with suction washing and drying. Named Al-mont-1.5-1, leaving aside like. Then Al-mont-1.5-1, AlCl 3 Content of 1.5mmol / L Al 0.6g of 3+ (AlCl 3 · 6h 2 O) was added to a three neck round bottom flask, stirred at 40 ℃ 24 hours to obtain a mixed solution, the mixed solution was cooled to room temperature, filtered off with suction washing and drying. Named Al-mont-1.5-2. So, the catalyst synthesized Al-mon...

Embodiment 3

[0040] The 100g Ca-mont, AlCl 3 An amount of 1mmol / L Al 0.5g of 3+ (AlCl 3 · 6h 2 O) was added to a three neck round bottom flask, stirred at 80 ℃ 12 hours to obtain a mixed solution, the mixed solution was cooled to room temperature, washed by suction filtration and drying to give an intermediate product, leaving the sample stand. The intermediate product, AlCl 3 An amount of 1mmol / L Al 0.5g of 3+ (AlCl 3 · 6h 2 O) was added to a three neck round bottom flask, stirred at 80 ℃ 12 hours to obtain a mixed solution, the mixed solution was cooled to room temperature, filtered off with suction washing and drying. Named Al-mont-1-1, leaving aside like. Then Al-mont-1-1, AlCl 3 Content of 0.5g of 1mmol / LAl 3+ (AlCl 3 · 6h 2 O) was added to a three neck round bottom flask, stirred at 80 ℃ 12 hours to obtain a mixed solution, the mixed solution was cooled to room temperature, filtered off with suction washing and drying. Named Al-mont-1-2. (2 cycles).

[0041] The 1g glucose, 4g Al-m...

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PUM

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Abstract

The invention relates to a synthesis method of an inorganic modified montmorillonite catalyst, which is applied to the synthesis of 5-hydroxymethylfurfural prepared from biomass sugar, and belongs to the field of organic catalytic synthesis. A certain amount of calcium-based montmorillonite was mixed with a low-concentration aluminum ion solution and stirred overnight. After cooling, it is filtered, washed and dried, and then mixed with a low-concentration aluminum ion solution, stirred overnight, cooled, filtered, washed and dried, and repeated several times to obtain a catalyst. And the catalyst was applied to the synthesis of 5-hydroxymethylfurfural prepared from biomass sugar, and a good catalytic effect was obtained within 2 hours. The use of low-concentration aluminum ions maximizes the reactivity, and the synthesis process is easy to operate and low in cost, and has good industrial application prospects.

Description

Technical field [0001] The present invention belongs to the field of organic synthesis catalyst, relates to a method for synthesizing the inorganic modified montmorillonite catalyst, and applied to the synthetic preparation of 5-hydroxymethylfurfural biomass sugars. Background technique [0002] Montmorillonite clay known as montmorillonite (MMT), is a readily available and inexpensive inorganic nanomaterials. Montmorillonite is an aqueous layered silicate material, mainly composed of alumina and silica, i.e., each unit cell 2 by the intermediate wafer entrained silica tetrahedron a wafer composed of an aluminum octahedral sheet structure , connected by the sharing of oxygen atoms therebetween. This special crystalline structure gives MMT many properties, such as swelling, adsorption, ion exchange, dispersion, suspension and the like, and bonding. [0003] Montmorillonite has a strong ion-exchange capacity, adsorption cycle is short, good biological stability, easy intercalation ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/16B01J37/30C07D307/46
CPCB01J21/16B01J37/30C07D307/46
Inventor 田戈曹靖劼杨永权徐兴良刘辉
Owner JILIN UNIV