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Organic heteropoly acid hybrid catalyst for alcohol oxidation reaction and preparation method thereof

A solid acid catalyst and heteropoly acid salt technology, which is applied in the direction of organic compound/hydride/coordination complex catalyst, oxidation to carbonyl compound, physical/chemical process catalyst, etc., can solve the problem of low alcohol oxidation activity and unstable stability Ideal and other problems, to achieve the effect of simple synthesis process, high selectivity and high yield

Inactive Publication Date: 2012-09-19
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of ionic liquid macromolecule-heteropolyacid hybrid catalyst for the low alcohol oxidation activity of the existing small molecule modified heteropolyacid hybrid catalyst and the unsatisfactory repeated use stability. The preparation method, the present invention also provides the application of the catalyst in the solvent-free alcohol oxidation reaction, the catalyst has the characteristics of high activity and selectivity, easy recovery, stable reuse, etc.

Method used

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  • Organic heteropoly acid hybrid catalyst for alcohol oxidation reaction and preparation method thereof
  • Organic heteropoly acid hybrid catalyst for alcohol oxidation reaction and preparation method thereof
  • Organic heteropoly acid hybrid catalyst for alcohol oxidation reaction and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1) In a 100mL three-necked flask equipped with a magnetic stirrer, a constant pressure dropping funnel and a spherical condenser, add 9.4g N-vinylimidazole, 20.5g 2-bromoethylamine hydrobromide and 50mL ethanol, 70 Stir at °C for 48 h, cool and filter, wash repeatedly with ethanol, and dry at 80 °C for 12 h to obtain an amine functionalized ionic liquid [VmimAM]Br·HBr with a yield of 90%. 1 H NMR (300MHz, D 2 O, TMS) characterization results are ( figure 1 ) δ (ppm) = 2.00 (m, 2H, -CH 2 ), 4.34 (s, 2H, -CH 2 ), 5.44 (d, 1H, -CH), 5.86 (d, 1H, -CH), 7.18 (m, 1H, -CH), 7.63 (s, 1H, -CH), 7.81 (s, 1H, -CH ), 9.11(s, 1H, -CH).

[0021] 2) Add 1g of amine-functionalized ionic liquid [VmimAM]Br·HBr, 2g of divinylbenzene and 10mL of methanol into a 100mL round-bottomed flask, protect it with nitrogen, stir and dissolve at 60°C, then add 0.05g of azobis Isobutyronitrile (AIBN), continue stirring at 60°C for 10-24h. Centrifuge, wash repeatedly with ethanol, adjust the pH v...

Embodiment 2

[0025] 1) In a 100mL three-necked flask equipped with a magnetic stirrer, a constant pressure dropping funnel and a spherical condenser, add 9.4g of N-vinylimidazole, 18.5g of N-chloroethylpiperidine hydrochloride and 50mL of acetonitrile , stirred at 80°C for 48h, cooled and filtered, washed repeatedly with ethanol, and dried at 80°C for 12h to obtain piperidine functionalized ionic liquid [VmimPD]Cl·HCl with a yield of 85%.

[0026] 2) Add 1g of piperidine functionalized ionic liquid [VmimPD]Cl·HCl, 2g of divinylbenzene and 10mL of methanol into a 100mL round-bottomed flask, pass through nitrogen protection, stir and dissolve at 60°C, add 0.05g of AIBN, continue Stir at 60°C for 10-24h. Centrifuge, wash repeatedly with ethanol, adjust the pH value to neutral with NaOH aqueous solution, centrifuge, and dry at 100°C for 12 hours to obtain 2.0 g of cross-linked ionic liquid polymer (PD-DVB).

[0027] 3) Disperse the above-mentioned ionic liquid polymer PD-DVB in the aqueous so...

Embodiment 3

[0030] 1) In a 100mL three-necked flask equipped with a magnetic stirrer, a constant pressure dropping funnel and a spherical condenser, add 9.4g N-vinylimidazole, 20.5g 2-bromoethylamine hydrobromide and 50mL ethanol, Stir at 70°C for 48h, cool and filter, wash repeatedly with ethanol, and dry at 80°C for 12h to obtain amine-functionalized ionic liquid [VmimAM]Br·HBr with a yield of 90%.

[0031]2) Add 1g of amine-functionalized ionic liquid [VmimAM]Br HBr, 2g of styrene and 10mL of a mixed solvent of ethanol and water (v:v=1:1) into a 100mL round-bottomed flask, nitrogen protection, 60°C After stirring and dissolving under the condition, add 0.05g AIBN, and continue stirring at 60°C for 10-24h. The solvent was removed by rotary evaporation, washed repeatedly with ethanol, adjusted to neutral pH with NaOH aqueous solution, filtered, and dried at 100°C for 12 hours to obtain 2.4g of ionic liquid polymer (AM-St).

[0032] 3) Disperse the above-mentioned ionic liquid polymer AM...

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Abstract

An organic heteropoly acid hybrid catalyst is prepared with ionic liquid polymer and heteropoly acid. A preparation method for the organic heteropoly acid hybrid catalyst is divided into the following three steps: firstly, ionic liquid is amino-functionalized; the unsaturated functional ionic liquid and unsaturated aromatic compound are initiated by initiator to polymerize, so that the ionic liquid polymer is produced; and finally, after the anion exchange between the ionic liquid polymer and the heteropoly acid, the ionic liquid polymer-heteropoly acid hybrid catalyst is produced. The catalyst is applicable to a variety of alcohol oxidation reactions with H2O2 as oxidizer, solvent is not used in the process of alcohol oxidation, the environment cannot be polluted, and the catalyst also has the characteristics of high activity and selectivity and stable reusability, and is a environment-friendly novel organic heteropoly acid hybrid catalyst.

Description

technical field [0001] The invention relates to the preparation and application of an organic heteropolyacid hybrid catalyst, in particular to a preparation method of an ionic liquid polymer-heteropolyacid hybrid catalyst and the application of the catalyst in alcohol oxidation. Background technique [0002] Aldehydes and ketones are common organic intermediates, and the liquid-phase catalytic oxidation of alcohols to aldehydes or ketones is an important reaction in fine organic chemicals. Chromium salts, permanganates, Ru(VI) oxides, etc. are traditional catalysts for this reaction, which require one or more relatively expensive oxidants, produce a large amount of heavy metal waste, and are often carried out in organic halide solvents, Not desirable from an environmental point of view. In order to meet the requirements of green chemical industry, using environmentally friendly H 2 o 2 Instead of other oxidants, the development of green catalysts with mild reaction condit...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J31/16C07C45/29
Inventor 冷炎吴江浩蒋平平
Owner JIANGNAN UNIV
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