Acid-base bifunctional metal organic skeletal catalyst and preparation method and application thereof

A metal-organic framework and acid-base bifunctional technology, which is applied in the field of acid-base bifunctional metal-organic framework catalysts and their preparation, can solve problems such as poor catalytic performance, restrictions on the large-scale synthesis and use of acid-base bifunctional catalysts, and complicated preparation processes. question

Inactive Publication Date: 2017-09-29
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the shortcomings of the acid-base bifunctional solid catalysts that have appeared are mainly manifested in: (1) the preparation process is complicated, and the modifiers used are relatively expensive, which limits the large-scale synthesis and use of acid-base bifunctional catalysts in this field
(2) The

Method used

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  • Acid-base bifunctional metal organic skeletal catalyst and preparation method and application thereof
  • Acid-base bifunctional metal organic skeletal catalyst and preparation method and application thereof
  • Acid-base bifunctional metal organic skeletal catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. UiO-66-NH 2 -SO 3 The preparation method of H is characterized in that it is carried out according to the following steps:

[0026] (1) Dissolve 1.8g of zirconium chloride and 1.2g of 2-aminoterephthalic acid in 150mL of weakly acidic 4 / 1 water and acid mixed solvent, disperse the mixed system evenly under ultrasonic conditions, and then put it in a 250mL In the flask, react in a water bath at 90°C for 24h. The reacted product was collected by filtration and washed 3 times with deionized water. The washed product was soaked in methanol for two days, filtered, and then dried under vacuum at 100 °C to obtain UiO-66-NH 2 Material.

[0027] (2) Prepare a mixed solution containing 575 μL of 1,3-propane sultone and 250 mL of chloroform in a flask, and prepare 0.67 g of UiO-66-NH 2 The crystals were placed in a flask, heated in a water bath at 45° C. for 3 h, and then the obtained solid product was centrifuged and washed by Soxhlet extraction (first with acetonitrile f...

Embodiment 2

[0045] 1. UiO-66-NH 2 -SO 3 The preparation method of H is characterized in that it is carried out according to the following steps:

[0046] (1) Dissolve 0.06g of zirconium chloride and 0.04g of 2-aminoterephthalic acid in 5mL of weakly acidic 3 / 2 water and acid mixed solvent, disperse the mixed system evenly under ultrasonic conditions, and then put it in 25mL In a flask, react in a water bath at 80°C for 12h. The reacted product was collected by filtration and washed 3 times with deionized water. The washed product was soaked in methanol for two days, filtered, and then dried under vacuum at 100 °C to obtain UiO-66-NH 2 Material.

[0047] (2) Prepare a mixed solution containing 11.5 μL of 1,3-propane sultone and 5 mL of chloroform in a flask, and prepare 0.01 g of UiO-66-NH 2 The crystals were placed in a flask, heated in a water bath at 30° C. for 1 h, and then the obtained solid product was centrifuged and washed by Soxhlet extraction (first with acetonitrile for 12 ...

Embodiment 3

[0055] 1. UiO-66-NH 2 -SO 3 The preparation method of H is characterized in that it is carried out according to the following steps:

[0056] (1) 3.6g of zirconium chloride and 2.6g of 2-aminoterephthalic acid were dissolved in 300mL of weakly acidic 6.5 / 1 water and acid mixed solvent, and the mixed system was dispersed evenly under ultrasonic conditions, and then placed in a 500mL In the flask, react in a bath at 100°C for 36h. The reacted product was collected by filtration and washed 3 times with deionized water. The washed product was soaked in methanol for two days, filtered, and then dried under vacuum at 100 °C to obtain UiO-66-NH 2 Material.

[0057] (2) Prepare a mixed solution containing 1150 μL of 1,3-propane sultone and 500 mL of chloroform in a flask, and prepare 1.33 g of UiO-66-NH 2 The crystals were placed in a flask, heated in a water bath at 50°C for 12 hours, and then the obtained solid product was centrifuged and washed by Soxhlet extraction (first was...

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Abstract

The invention provides an acid-base bifunctional metal organic skeletal catalyst and a preparation method and an application thereof. The preparation steps are as follows: zirconium salt and 2-aminaterephthalic acid are dissolved in weakly acidic solution, and the obtained mixed solution is uniformly dispersed under an ultrasonic condition, and reacts in water bath; after reaction, the product is filtered, collected and washed; after the washed product is immersed in low-boiling point solvent, filtration is carried out, vacuum drying is then carried out, and thereby a UiO-66-NH2 material is obtained; trichloromethane solution which contains 1,3-propane sultone is prepared, added with the prepared UiO-66-NH2 material and heated in water bath to react, and the prepared solid product is then centrifugally separated and washed by using Soxhlet extraction; the obtained solid material is put into a vacuum drying oven, and thereby the acid-base bifunctional metal organic skeletal catalyst is obtained. The process of preparing the product is simple, the preparation cost is low, the acid-base bifunctional metal organic skeletal catalyst is used in the preparation of 5-hydroxymethylfurfural by one-step catalysis of dextrose, the reaction progress is accelerated, and the reaction process is simplified.

Description

technical field [0001] The invention belongs to the field of solid catalysts, in particular to an acid-base bifunctional metal-organic framework catalyst and a preparation method thereof. Background technique [0002] With the increasing energy crisis and environmental pollution, seeking a sustainable green energy has become an urgent problem to be solved. Biomass energy has become an ideal energy source to replace non-renewable energy sources such as coal, oil, and natural gas because of its wide range of sources, low price, and abundant reserves. 5-Hydroxymethylfurfural (5-HMF) is a biomass-based platform compound that contains active aldehyde groups, hydroxyl groups and furan rings in its structural formula derived from biomass conversion. It can be derived from many downstream products through further reactions. Products are key intermediates connecting biomass chemistry and petrochemistry. Biomass preparation of 5-HMF is one of the hotspots in the comprehensive utiliz...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J35/10C07D307/46
CPCB01J31/1691B01J31/0225B01J31/2217B01J35/0013B01J35/10B01J2531/0238B01J2531/48C07D307/46
Inventor 金佩张云雷李春香闫永胜戴江栋
Owner JIANGSU UNIV
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