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Method and catalyst for preparing ethyl furfuryl ether by liquid-phase hydrogenation of furfural and preparation method of catalyst

A technology of furfuryl ether and catalyst, which is applied in the field of furfural liquid-phase hydrogenation to produce ethyl furfuryl ether, can solve the problems of difficult industrial synthesis production, difficult reaction control, high catalyst cost, etc., achieve high conversion rate, easy scale-up, The effect of low production cost

Active Publication Date: 2019-07-09
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, due to the difficulty of controlling the reaction and the high cost of the catalyst, it is difficult to realize industrial synthesis production

Method used

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  • Method and catalyst for preparing ethyl furfuryl ether by liquid-phase hydrogenation of furfural and preparation method of catalyst
  • Method and catalyst for preparing ethyl furfuryl ether by liquid-phase hydrogenation of furfural and preparation method of catalyst
  • Method and catalyst for preparing ethyl furfuryl ether by liquid-phase hydrogenation of furfural and preparation method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Preparation of Cu / SiO by Ammonia Distillation 2 . Will accurately weigh 3.09g of Cu(NO 3 ) 2 ·3H 2 O was placed in a three-neck round bottom flask and dissolved in 100ml of deionized water, and ammonia water (14%) was added dropwise at room temperature at 1mL / min until the pH of the solution was >9.0 to form a cuproammonia solution. After the solution was stirred for 10 min, 4.9 g of mesoporous SiO was added 2 , continue to stir for 2 hours, and then move to a 90°C water bath until the pH of the solution is 5. Take out the three-neck round bottom flask, and observe the color change of the solution. The catalyst precursor was obtained by filtration, washed with deionized water for 3 times, dried in an oven at 120°C overnight, and calcined at 250°C in an air atmosphere for 2 hours; after that, the catalyst was ground and sieved to 40-60 mesh particles for future use. in H 2 Reduction at 150°C for 1 h in the atmosphere; after the reduction, cool to room temperature, ...

Embodiment 2

[0038] Preparation of Cu / SiO by Ammonia Distillation 2 . Will accurately weigh 6.17g of Cu(NO 3 ) 2 ·3H 2 O was placed in a three-neck round bottom flask and dissolved in 100ml of deionized water, and ammonia water (14%) was added dropwise at room temperature at 1mL / min until the pH of the solution was >9.0 to form a cuproammonia solution. After the solution was stirred for 20 min, 4.9 g of mesoporous SiO was added 2 , continue to stir for 2 hours, and then move to a 90°C water bath until the pH of the solution is 6. Take out the three-neck round bottom flask, and observe the color change of the solution. The catalyst precursor was obtained by filtration, washed with deionized water for 3 times, dried in an oven at 120°C overnight, and calcined at 450°C in an air atmosphere for 4 hours; after that, the catalyst was ground and sieved to 40-60 mesh particles for future use. in H 2 Restore at 350°C for 2 hours in the atmosphere; after the reduction, cool to room temperature...

Embodiment 3

[0040] Preparation of Cu / SiO by Ammonia Distillation 2 . Will accurately weigh 8.23g of Cu(NO 3 ) 2 ·3H 2 O was placed in a three-neck round bottom flask and dissolved in 100ml of deionized water, and ammonia water (14%) was added dropwise at room temperature at 1mL / min until the pH of the solution was >9.0 to form a cuproammonia solution. After the solution was stirred for 30 min, 4.9 g of mesoporous SiO was added 2, continue to stir for 2 hours, and then move to a 90°C water bath until the pH of the solution is 7. Take out the three-neck round bottom flask, and observe the color change of the solution. The catalyst precursor was obtained by filtration, washed with deionized water for 3 times, dried in an oven at 120°C overnight, and calcined at 650°C in an air atmosphere for 6 hours; after that, the catalyst was ground and sieved to 40-60 mesh particles for future use. in H 2 Reduction at 550°C for 4 hours in the atmosphere; after the reduction, cool to room temperatur...

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Abstract

The invention relates to a method and catalyst for preparing ethyl furfuryl ether by liquid-phase hydrogenation of furfural and a preparation method of the catalyst. Active metal Cu is supported on asilica-containing carrier by adopting an ammonia distillation method, and the catalyst is the metal Cu supported by the silica-containing carrier, wherein the supporting capacity of the copper is 5-45wt%. The silica-containing carrier is one or more selected from mesoporous SiO2, MCM-41, SBA-15 and silica sol. Absolute ethyl alcohol is taken as a solvent, and furfural and the catalyst are added,wherein the mass ratio of the furfural to the absolute ethyl alcohol is (0.1-1):1, and the mass ratio of the catalyst to the furfural is (0.02-0.1):1; and a reaction is carried out for 0.5-24 hours under the condition that the hydrogen pressure is 0.5-15 MPa and the reaction temperature is 80-250 DEG C to obtain the ethyl furfuryl ether. The catalyst disclosed by the invention has relatively highcatalytic activity. When furfural is used as a raw material to synthesize ethyl furfuryl ether in one step, the reaction conditions are mild, and requirements of large-scale industrial production aremet.

Description

technical field [0001] The present invention relates to the method for preparing ethyl furfuryl ether by furfural liquid-phase hydrogenation, using Cu / SiO 2 The catalyst is used in the method of furfural liquid-phase hydrogenation to produce ethyl furfuryl ether. Specifically, it relates to a method for preparing ethyl furfuryl ether by furfural liquid-phase hydrogenation, a catalyst and a preparation method of the catalyst. Background technique [0002] Ethyl furfuryl ether is a biomass ether compound that can be directly added to fuels such as gasoline and diesel to reduce the generation of particulate matter and smoke emissions after fuel combustion. It can also be used as an additive for medicine and food. At present, the synthesis of ethyl furfuryl ether has not been industrialized. According to the existing literature, there are two ways to prepare ethyl furfuryl ether with furfural as raw material: one is to hydrogenate furfural to obtain furfuryl alcohol, and then...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J29/03B01J29/46B01J35/00B01J37/00C07D307/42C07D307/44
CPCB01J23/72B01J29/0333B01J29/46B01J37/0018C07D307/42C07D307/44B01J2229/18B01J35/394
Inventor 纪娜刘云冲郑明远赵宇张涛刁新勇贾志超
Owner TIANJIN UNIV
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