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Load-type ion liquid catalyst and preparation method and application thereof

A technology of ionic liquid and acidic ionic liquid, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., to achieve high conversion rate and selectivity, simple preparation method and long service life

Inactive Publication Date: 2010-03-10
WENZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report on the application of supported ionic liquid catalysts in the preparation of diethylene glycol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Get 79g of pyridine in the reactor, add 152.6g of bromoethane, under the effect of 40kHz, 500W ultrasonic waves, react for 3h, distill off the unreacted reactant under reduced pressure, obtain 188g of [EPy]Br solid, the product [EPy] Dissolve Br in dichloromethane to make a 0.5mol / L solution. Under the condition of 40kHz and 500W ultrasonic power, the reaction temperature is 0°C, add 130g of 98wt% concentrated sulfuric acid dropwise, and then reflux for 3 hours, then remove the ice bath , the reaction solution was returned to room temperature, and the solvent dichloromethane was distilled off under reduced pressure to obtain the pyridine acidic ionic liquid [EPy]HSO 4 (N-Ethylpyridinium bisulfate).

[0023] Take the above-mentioned pyridine acidic ionic liquid 92.5g and add 47g γ-Al 2 o 3 Soak for 24h to obtain a supported ionic liquid catalyst, which can be expressed as [EPy]HSO 4 / γ-Al 2 o 3 .

Embodiment 2

[0025] Get 80g of pyridine in the reactor, add 153g of bromoethane, under the effect of 28kHz, 100W ultrasonic waves, react for 1h, distill off the unreacted reactant under reduced pressure, obtain 75g of [EPy]Br solid, the product [EPy]Br Dissolved in dichloromethane, made into a 0.5mol / L solution, under the conditions of 28kHz, 100W ultrasonic power, the reaction temperature is 0°C, 50g of 98wt% concentrated sulfuric acid was added dropwise, and then refluxed for 3h, and the ice bath was removed. The reaction solution was returned to room temperature, and the solvent dichloromethane was distilled off under reduced pressure to obtain the pyridine acidic ionic liquid [EPy]HSO 4 (N-Ethylpyridinium bisulfate).

[0026] Take the above-mentioned pyridine acidic ionic liquid 50g and add 27g γ-Al 2 o 3 Soak for 24h to obtain a supported ionic liquid catalyst, which can be expressed as [EPy]HSO 4 / γ-Al 2 o 3 .

Embodiment 3

[0028]Take 79g (1mol) of pyridine in the reactor, add 68.5g (0.5mol) of n-bromobutane, under the action of 45kHz, 600W ultrasonic waves, react for 4h, distill off the unreacted reactants under reduced pressure, and obtain 108g [BPy ]Br solid, product [BPy]Br is dissolved in carbon tetrachloride, is made into the solution of 0.5mol / L, under 45kHz, power is 600W ultrasonic conditions, reaction temperature is 0 ℃, drips 50g of 98wt% concentrated sulfuric acid , then after reflux reaction for 8h, the ice bath was removed, the reaction solution was returned to room temperature, and the solvent carbon tetrachloride was distilled off under reduced pressure to obtain the pyridine acidic ionic liquid [BPy]HSO 4 (N-n-Butylpyridinium bisulfate).

[0029] Get the above-mentioned pyridine acidic ionic liquid 58g and add 58g SiO 2 Soak for 24h to obtain a supported ionic liquid catalyst, which can be expressed as [BPy]HSO 4 / SiO 2 .

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PUM

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Abstract

The invention discloses a load-type ion liquid catalyst and a preparation method and an application thereof. The load-type ion liquid catalyst is characterized in that a carrier is loaded with pyridine acidic ionic liquid [XPy]HSO4, wherein X is ethyl, propyl, isopropyl, normal-butyl, 3-methylbutyl or 3-amyl; the carrier is gamma-Al2O3, SiO2, mesoporous molecular sieve SBA-15 and carbon fiber; themass ratio of the carrier to the pyridine acidic ionic liquid is 0.5-1.5:1. The invention also discloses the preparation method of the load-type ion liquid catalyst and the application thereof in enzymatic synthesis of diglycol. The invention has the beneficial effects that the invention provides a novel load-type ion liquid catalyst, has simple catalyst preparing method, high catalyst activity and long service life, is applied to enzymatic synthesis of diglycol, has moderate reaction condition, simple production technology, higher diglycol percent conversion and selectivity and is suitable for industrialization.

Description

technical field [0001] The invention relates to a supported ionic liquid catalyst and a preparation method thereof, and also relates to a method for catalytically synthesizing diethylene glycol by using a supported ionic liquid as a catalyst. Background technique [0002] Diethylene glycol is an important chemical product. Its molecular structure contains two functional groups of ether bond and hydroxyl group, which make it have unique physical and chemical properties. Mainly used in solvents, aromatics separation and extraction agents, natural gas dehydration desiccants, textile lubricants, brake fluids, antifreeze agents in compressor lubricating oils, cleaning agents, etc. In addition, diethylene glycol is also an important chemical intermediate. Diethylene glycol can be used as raw material to produce ethers, acids, esters, amines and other chemical products. At present, the main products that can be produced with diethylene glycol as raw materials are morpholine and i...

Claims

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Application Information

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IPC IPC(8): B01J31/26B01J31/02B01J37/34C07C43/11C07C41/09
Inventor 赵亚娟余卫芳司朗诵金雪华
Owner WENZHOU UNIVERSITY
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