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Method for preparing acrolein by catalyzing glycerin dehydration with solid-supported acidic ionic liquid

A technology of acidic ionic liquid and catalyzed glycerin, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of harsh reaction conditions, high cost, and no one has tried it, and achieve low raw material cost, The effect of fast speed and low raw material price

Active Publication Date: 2011-12-07
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN 101735195A discloses a method for catalytically synthesizing cyclic carbonates with acidic ionic liquids. This invention solves the problems of harsh reaction conditions and high costs
[0007] Due to the advantages of high catalytic activity, mild reaction conditions, and no pollution, acidic ionic liquids can be used in various reactions so far, but in the reaction of glycerol dehydration to acrolein no one tried

Method used

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  • Method for preparing acrolein by catalyzing glycerin dehydration with solid-supported acidic ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Take 16.41g of 1-methylimidazole in a four-necked flask, then add toluene, add 32.88g of bromo-n-butane in a constant pressure dropping funnel, then heat to 80°C and react for 12 hours to obtain a pale yellow liquid and Colorless liquid, a light yellow liquid was separated, washed with ethyl acetate, and dried in a vacuum drying oven for 8 hours to obtain a light yellow liquid [BMIM]Br. Take 28.55g [BMIM]Br in a four-necked flask and add HBF dropwise 4 , Heated in a water bath to 65°C, reacted for 6 hours to obtain a viscous liquid, washed 3 times with ether, and dried in vacuum to obtain an ionic liquid [BMIM]BF 4 .

[0027] The activated carbon (AC) is crushed to 18-30 mesh, the catalyst is prepared by the impregnation method, and the amount of acidic ionic liquid [BMIM] BF4 used is calculated according to the loading amount of 10% (based on the weight of the carrier as 10g), and anhydrous Ethanol is used as a solvent, the acidic ionic liquid is weighed to prepare a solu...

Embodiment 2

[0030] Ionic liquid [BMIM]BF 4 The synthesis is as in Example 1. The activated carbon (AC) is crushed to 18-30 mesh, the catalyst is prepared by the impregnation method, and the acidic ionic liquid [BMIM]BF is calculated according to the load of 15%. 4 Use absolute ethanol as the solvent, weigh the acidic ionic liquid to prepare a solution, then pour the broken carrier into the prepared acidic ionic liquid solution, and immerse it for 24 hours. After drying and calcining, the catalyst is obtained.

[0031] Put 5ml 18~30 mesh with 15% [BMIM]BF 4 The / AC catalyst is charged into the middle section of a fixed-bed reactor with continuous flow at normal pressure, and the upper and lower sections are filled with 10ml quartz sand. After the system is checked and sealed, slowly increase the temperature of the catalyst bed to 260°C, and then drive a 15% aqueous bioglycerin solution containing 3% polymerization inhibitor hydroquinone into the fixed bed reactor through a micro pump. The li...

Embodiment 3

[0033] Ionic liquid [BMIM]BF 4 The synthesis is as in Example 1, the SiO 2 Crush to 18-30 mesh, prepare the catalyst by impregnation method, calculate the acidic ionic liquid [BMIM]BF according to the load of 20% 4 Use absolute ethanol as the solvent, weigh the acidic ionic liquid to prepare a solution, then pour the broken carrier into the prepared acidic ionic liquid solution, and immerse it for 24 hours. After drying and calcining, the catalyst is obtained.

[0034] Load 5ml 18~30 mesh with 20% [BMIM]BF 4 / SiO 2 The catalyst is charged into the middle section of a fixed-bed reactor with continuous flow at normal pressure, and the upper and lower sections are filled with 10 ml of quartz sand. After the system is checked and sealed, slowly increase the temperature of the catalyst bed to 280°C, and then drive a 25% aqueous bioglycerin solution with 4% polymerization inhibitor hydroquinone added into the fixed bed reactor through a micro pump. The liquid hourly space velocity is ...

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Abstract

The invention discloses a preparation method of acrolein, and relates to the field of acrolein preparation by catalyzing dehydration of glycerol. The preparation method is characterized in that: glycerol is used as a raw material, an immobilized ionic liquid is used as a catalyst, and acrolein is prepared by dehydration; the used ionic liquid is acidic ionic liquid [BMIM]BF4 (1-butyl-3-methylimidazolium terafluoroborate) or [BMIM]H2PO4, and the acidic ionic liquid is immobilized by impregnation; the molar selectivity of the acrolein prepared by adding 1-8% of hydroquinone used as a polymerization inhibitor to 10-60% of glycerol aqueous solution used as a reaction solution and reacting under the conditions of atmospheric pressure, reaction temperature of 240-360 DEG C and volume space velocity of 5-15 / h can reach 90.4%; and the conversion rate of glycerol can reach 100%. The preparation method has the advantages that the immobilized acidic ionic liquid has higher selectivity in the dehydration reaction of glycerol, the acrolein yield is higher, the reaction stability is good, and the life of the catalyst is long.

Description

technical field [0001] The invention relates to the field of catalyzing the dehydration of glycerin to produce acrolein. The specific method is to continuously prepare the product acrolein through a fixed-bed reactor by using glycerin as a raw material and under the action of a solid-supported acidic ionic liquid as a catalyst. Background technique [0002] The traditional production processes of acrolein mainly include: formaldehyde-acetaldehyde gas-phase condensation method, propylene or propane oxidation method, propylene ether pyrolysis method, etc. These traditional production processes mainly rely on the development of the petroleum industry. Now that petroleum resources are exhausted, it is particularly important to develop new acrolein production processes. The production process of glycerol dehydration to acrolein has high economic benefits and meets the needs. [0003] The catalytic system of acrolein is mainly divided into homogeneous and heterogeneous systems. Th...

Claims

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Application Information

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IPC IPC(8): C07C47/22C07C45/52B01J31/26B01J31/02
Inventor 张跃卢乐严生虎刘建武沈介发
Owner CHANGZHOU UNIV
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