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Preparation of a polyionic liquid functionalized mofs material and its application in the synthesis of isopulegol

A polyionic liquid, functionalized technology, applied in the reduction preparation of oxygen-containing functional groups, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problem of excessive catalyst dosage, slow reaction rate and harsh reaction conditions. and other problems, to achieve the effect of excellent catalytic performance

Active Publication Date: 2021-11-30
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been reported that such as diatomaceous earth, SiO 2 , sulfuric acid, acetic anhydride, zinc bromide, acidic oxides, rhodium complexes, etc. can all be used for the cyclization catalysis of citronellal, and these catalyzers all have isopulegol selectivity not high, catalyst consumption is too large, reaction Problems such as slow rate, difficult recovery, and harsh reaction conditions

Method used

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  • Preparation of a polyionic liquid functionalized mofs material and its application in the synthesis of isopulegol
  • Preparation of a polyionic liquid functionalized mofs material and its application in the synthesis of isopulegol
  • Preparation of a polyionic liquid functionalized mofs material and its application in the synthesis of isopulegol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of UiO material

[0031] Uniformly disperse 0.6 mmol of imidazole-4,5-dicarboxylic acid, 1.2 mmol of terephthalic acid, and 1.2 mmol of zirconium chloride in 42 mL of DMF, then add 3 mL of glacial acetic acid and sonicate, then pour into 100 mL of polytetrafluoroethylene Crystallization was carried out at 130 °C for 24 h in an ethylene-lined hydrothermal synthesis kettle. After cooling down to room temperature, it was centrifuged, washed twice with DMF and five times with methanol, and the solid powder obtained by drying was the UiO material.

[0032] (2) Preparation of UiO-prePIL material

[0033] Disperse 0.12 mmol of UiO material in ethanol, add 0.06 mmol of epichlorohydrin, and polymerize at 80°C for 72h. After cooling down to room temperature, it was centrifuged, washed five times with ethanol, and the solid powder obtained after drying was UiO-prePIL.

[0034] (3) Preparation of UiO-PIL materials

[0035] Disperse 0.06mmol UiO-prePIL in ethanol...

Embodiment 2

[0042] Application: Take 0.05g of the synthetic material in Example 1, disperse it in 3ml of ethanol solution, add 0.5g of citronellal, and react at 30°C for 2h. After determination, under the above-mentioned reaction conditions, the yield of isopulegol is 92.67%.

Embodiment 3

[0044] (1) Preparation of UiO material

[0045] Uniformly disperse 0.6 mmol of imidazole-4,5-dicarboxylic acid, 1.2 mmol of terephthalic acid, and 1.2 mmol of zirconium chloride in 42 mL of DMF, then add 3 mL of glacial acetic acid and sonicate, then pour into 100 mL of polytetrafluoroethylene Crystallization was carried out at 130 °C for 24 h in an ethylene-lined hydrothermal synthesis kettle. After cooling down to room temperature, it was centrifuged, washed twice with DMF and five times with methanol, and the solid powder obtained by drying was the UiO material.

[0046] (2) Preparation of UiO-prePIL material

[0047] Disperse 0.12 mmol of UiO material in ethanol, add 0.06 mmol of epichlorohydrin, and polymerize at 80°C for 72h. After cooling down to room temperature, it was centrifuged, washed five times with ethanol, and the solid powder obtained after drying was UiO-prePIL.

[0048] (3) Preparation of UiO-PIL materials

[0049] Disperse 0.06mmol UiO-prePIL in ethanol, ...

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Abstract

The invention relates to the preparation of a polyionic liquid functionalized MOFs material (UiO‑66) and its application in synthesizing isopulegol, belonging to the technical field of composite materials. The present invention utilizes imidazole containing carboxylic acid groups as a polyionic liquid monomer, combines it with UiO-66 by a thermal solvent method, polymerizes and performs ion exchange, and successfully synthesizes a polyimidazole ionic liquid functionalized MOFs material (UiO-PIL) . The material exhibits excellent catalytic performance in the synthesis of isopulegol from citronellal under green and mild conditions, and its catalytic performance is greatly improved compared with UiO-66.

Description

technical field [0001] The invention belongs to the technical field of composite material synthesis, and in particular relates to a preparation method of a polyionic liquid functionalized MOFs material and its application in the reaction of synthesizing isopulegol from citronellal. Background technique [0002] Menthol is an important aroma chemical, which can be used in food, medicine, daily necessities and other industries, and its demand has been increasing in recent years. The menthol currently on the market mainly comes from natural purification and separation. Due to limitations such as climate and geography, the output of natural purified menthol is unstable. Compared with this, artificially synthesized menthol has higher economy, better stability, and can better meet market demand, and has great advantages. And isopulegol is an important intermediate for the artificial synthesis of menthol, so the cyclization of citronellal to prepare isopulegol is a key step in the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J31/22C07C29/14C07C35/17
CPCB01J31/1691B01J31/1815B01J2531/48C07C29/14C08G83/008C07C35/17
Inventor 李玲卢佳尧邱挺叶长燊陈杰葛雪惠
Owner FUZHOU UNIV
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