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Heteropoly ionic liquid catalyst with Br*nsted-Lewis dual acidity

An ionic liquid, dual-acid technology, which is applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, organic chemistry, etc., can solve problems such as low acid strength, and achieve low cost and simple preparation method. , the effect of rich varieties

Active Publication Date: 2013-11-20
山东星际石化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The purpose of the present invention is to provide a novel strong-acid heteropolyionic liquid catalyst with Brönsted-Lewis biacidity in order to solve the problem of low acid strength existing in the existing acid functionalized ionic liquids, and to provide this ion liquid preparation method

Method used

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  • Heteropoly ionic liquid catalyst with Br*nsted-Lewis dual acidity
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  • Heteropoly ionic liquid catalyst with Br*nsted-Lewis dual acidity

Examples

Experimental program
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Effect test

Embodiment 1

[0037] [Example 1] Synthesis of Ionic Liquid 1:

[0038] (1) Weigh 12.21 g (0.10 mol) of 1,3-propane sultone into a three-necked flask (250 mL), add 100 mL of toluene to dissolve it, then add 9.02 g (0.10 mol) of N-methylimidazole, Under magnetic stirring at 50°C, react with nitrogen for 24 h, filter the reaction solution with suction, wash the obtained white precipitate with ethyl acetate three times, and dry it in vacuum at 60°C for 4 h, the obtained white powdery solid is 1-formazol 3-(3-sulfopropyl) imidazolidine sulfonate (MIMPS).

[0039] (2) Weigh Al(NO 3 ) 3 ?9H 2 Add 1.00 g (2.67 mmol) of O and 0.82 g (4 mmol) of MIMPS into a three-neck flask (100 mL), weigh 11.52 g (4 mmol) of phosphotungstic acid, add 40 mL of deionized water to the beaker to dissolve it, and dissolve the phosphorus Add tungstic acid aqueous solution into a three-necked flask, react at room temperature (25 °C) for 24 h under magnetic stirring, distill under reduced pressure, and dry in vacuum at...

Embodiment 2

[0042] [Example 2] Synthesis of ionic liquid 2:

[0043] (1) Weigh 12.21 g (0.10 mol) of 1,3-propane sultone into a three-necked flask (250 mL), add 100 mL of toluene to dissolve it, then add 9.02 g (0.10 mol) of N-methylimidazole, Under magnetic stirring at 50 °C and nitrogen gas for 24 h, the reaction liquid was filtered with suction, the obtained white precipitate was washed three times with ethyl acetate, and vacuum-dried at 60 °C for 4 h, the obtained white powdery solid was MIMPS.

[0044] (2) Weigh Al(NO 3 ) 3 ?9H 2 Add 0.50 g (1.33 mmol) of O and 1.64 g (4 mmol) of MIMPS into a three-necked flask (100 mL), weigh 11.52 g (4 mmol) of phosphotungstic acid, add 40 mL of deionized water to the beaker to dissolve it, and dissolve the phosphorus Add tungstic acid aqueous solution into a three-necked flask, react at room temperature (25 °C) for 24 h under magnetic stirring, distill under reduced pressure, and dry under vacuum at 80 °C for 6 h. The obtained white solid is de...

Embodiment 3

[0047] [Example 3] Synthesis of ionic liquid 3:

[0048] (1) Weigh 12.21 g (0.10 mol) of 1,3-propane sultone into a three-necked flask (250 mL), add 100 mL of toluene to dissolve it, then add 9.02 g (0.10 mol) of N-methylimidazole, Under magnetic stirring at 50 °C and nitrogen gas for 24 h, the reaction liquid was filtered with suction, the obtained white precipitate was washed three times with ethyl acetate, and vacuum-dried at 60 °C for 4 h, the obtained white powdery solid was MIMPS.

[0049] (2) Weigh Al(NO 3 ) 3 ?9H 2 Add 0.50 g (1.33 mmol) of O and 1.64 g (8 mmol) of MIMPS into a three-necked flask (100 mL), weigh 11.52 g (4 mmol) of phosphotungstic acid and add 40 mL of deionized water to the beaker to dissolve it. Add tungstic acid aqueous solution into a three-necked flask, react at room temperature (25 °C) for 24 h under magnetic stirring, distill under reduced pressure, and dry under vacuum at 80 °C for 6 h. The obtained white solid is designated as ionic liquid ...

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Abstract

The invention relates to a heteropoly ionic liquid catalyst with Br*nsted-Lewis dual acidity and a preparation method thereof, belonging to the technical field of novel chemical materials and preparation thereof. The synthesis method comprises the following steps: (1) reacting 1,3-propane sultone with N-methylimidazole in toluene in a nitrogen protective atmosphere to obtain an intermediate 1-methyl-3-(3-sulfopropyl)imidazolyl sulfonate (MIMPS); and (2) by using the intermediate MIMPS and Al(NO3)3.9H2O as counter cation sources and phosphotungstate as an anion source, reacting in a water solution under certain conditions by regulating the anion-cation ratio to obtain the heteropoly ionic liquid catalytic material with Br*nsted-Lewis dual acidity. The organic cation with sulfo-group, metal aluminum ion and proton are simultaneously used as the counter cations to prepare the heteropoly salt strong-acid functional ionic liquid with Br*nsted-Lewis dual acidity at the cation part; and the preparation process is simple and easy to implement, and can be used as a benzylation reaction high efficiency catalyst for benzalcohol route.

Description

technical field [0001] The invention relates to an acid-functionalized ionic liquid catalyst and a preparation method thereof, in particular to a strong-acid-functionalized heteropolyionic liquid catalyst with Brönsted-Lewis double acidity in the cationic part and a preparation method thereof, which belongs to a novel Materials and their preparation technologies. [0002] Background technique [0003] Functionalized ionic liquids refer to ionic liquids that introduce functional groups into ions (anions or cations), and the presence of such functional groups has a great impact on ionic liquids, making the ionic liquids have some unique properties or can meet specific requirements. Requirements, including functionalization for physical properties (such as mobility, conductivity, liquid range, solubility) and functionalization for chemical properties (polarity, acidity, chirality, coordination ability). The design of specific functionalization of ionic liquids can be achieved...

Claims

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Application Information

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IPC IPC(8): B01J31/18C07C41/30C07C43/205
Inventor 袁冰解从霞于凤丽赵雯生刘宗群于世涛
Owner 山东星际石化科技有限公司
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