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Uio-66 in-situ immobilized carboxyl functionalized ionic liquid composite material as well as preparation and application thereof

A technology of carboxyl functionalization and uio-66, which is applied in the preparation of organic compounds, carboxylic acid ester preparation, catalytic reactions, etc., can solve the problems of macromolecular substance adsorption and poor catalytic effect, and achieve good physical and chemical stability properties, fast mass transfer rate, and obvious adsorption effect

Inactive Publication Date: 2018-11-16
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the "boat-in-a-bottle method" has strict requirements on the cage diameter of MOF materials, and has poor adsorption and catalytic effects on macromolecular substances.

Method used

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  • Uio-66 in-situ immobilized carboxyl functionalized ionic liquid composite material as well as preparation and application thereof
  • Uio-66 in-situ immobilized carboxyl functionalized ionic liquid composite material as well as preparation and application thereof
  • Uio-66 in-situ immobilized carboxyl functionalized ionic liquid composite material as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Preparation of monocarboxyl functionalized ionic liquid

[0023] Accurately weigh 0.1mol of chloroacetic acid and add it to a 100ml round-bottomed flask, add 0.1mol of 1-methylimidazole dropwise under mechanical stirring, react at 70°C for 8 hours, wash with ethanol and dry in vacuum to obtain a white solid Dissolve this white solid in a small amount of deionized water, add sulfuric acid of the same amount, stir magnetically at 70°C for 8 hours, wash with ethyl acetate, and dry in vacuo to obtain 1-carboxymethyl-3-methyl Imidazolium bisulfate;

[0024] (2) Preparation of in situ immobilized monocarboxyl functionalized IL@Uio-66

[0025] Accurately weigh 0.0603g of terephthalic acid in 42ml of DMF, then quickly add 0.0848g of zirconium chloride, ultrasonicate for 30min, add 0.15g of the 1-carboxymethyl-3-methylimidazolium bisulfate synthesized above, and ultrasonicate for 30min , placed in 100ml polytetrafluoroethylene liner, reacted at 120°C for 24h, centrifuged a...

Embodiment 2

[0027] (1) Preparation of dicarboxyl functionalized ionic liquid

[0028] Accurately weigh 0.1mol of 1-methylimidazole and add it to a 100ml round-bottomed flask, add an appropriate amount of bromosuccinic acid dissolved in methanol drop by drop under the condition of mechanical stirring, react at 80°C for 8 hours, and distill under reduced pressure , ethyl acetate, and vacuum-dried to obtain an orange-yellow viscous liquid; dissolve the orange-yellow viscous liquid in a small amount of deionized water, add the same amount of sulfuric acid, and stir magnetically at 70°C for 8 hours. After washing with ethyl ester and vacuum drying, 1-bromo-1,2-dicarboxyethyl-3-methylimidazolium bisulfate was obtained;

[0029] (2) Preparation of in situ immobilized dicarboxyl functionalized IL@Uio-66

[0030] Accurately weigh 0.0603g of terephthalic acid into 42ml of DMF, then quickly add 0.0848g of zirconium chloride, sonicate for 30min, add 0.15g of 1-bromo-1,2-dicarboxyethyl-3-methylimidaz...

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Abstract

The invention belongs to the technical fields of light-industry and chemical materials, and provides a Uio-66 in-situ immobilized carboxyl functionalized ionic liquid composite material as well as preparation and an application thereof. The composite material uses a metal organic skeleton material Uio-66 as a carrier and a carboxyl functionalized ionic liquid as an active component, carboxyl of the carboxyl functionalized ionic liquid and a zirconium metal cluster are subjected to coordination bonding while the Uio-66 is synthesized, the carboxyl functionalized ionic liquid is immobilized in aUio-66 pore cage in situ, and therefore the composite material is prepared. The composite material provided by the invention has the characteristics of high catalytic activity, a quick mass transferspeed, good selectivity, easy recovery and separation, environmental friendliness, and broad industrialized application prospects in addition to good physical stability and chemical stability; the composite material prepared by the method has a very good effect as a catalyst of an esterification reaction and transesterification reaction of various acids and alcohols; and the composite material hasan obvious adsorption effect on heavy metal ions contained in a liquid as an adsorbent.

Description

technical field [0001] The invention relates to the technical field of composite material synthesis, in particular to a Uio-66 in-situ immobilized carboxyl functionalized ionic liquid composite material and its preparation and application. Background technique [0002] Ionic Liquid (Ionic Liquid) is a compound composed of organic cations and organic or inorganic anions that is liquid at room temperature or near room temperature. It has the advantages of designability, strong thermal stability, wide liquid temperature range, and strong conductivity. It is used in various fields of chemical research. At present, liquid ionic liquids are widely used in green organic synthesis, separation and purification, electrochemistry and other fields, and good results have been achieved. However, in the actual application process, there are problems such as large amount of ionic liquid used, difficulty in product separation and catalyst recovery, resulting in high cost and difficulty in i...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C67/08C07C69/24C11C3/04B01J20/22B01J20/30C02F1/28C02F101/20
CPCB01J20/22B01J20/226B01J31/0292B01J31/1691B01J31/2239B01J2231/49B01J2531/48C02F1/285C02F2101/20C07C67/08C11C3/04C07C69/24
Inventor 叶长燊齐兆洋邱挺李玲王红星黄智贤杨臣王晓达陈锦溢林小城杨金杯王清莲
Owner FUZHOU UNIV
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