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Preparation method of modified copper-based catalyst for furfural hydrogenation to furfuryl alcohol

A copper-based catalyst, a technology for preparing furfuryl alcohol, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve problems such as no copper-based catalyst, and achieve good hydrogenation effect, simple operation and good catalytic activity. Effect

Active Publication Date: 2020-07-10
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In summary, there is currently no method for preparing copper-based catalysts by in-situ reduction of formic acid, which is used for the hydrogenation of furfural to prepare furfuryl alcohol; especially, there is no hydrogenation of furfural with doped barium salt or barium salt as the carrier and copper as the active ingredient. Modification Catalyst of Furfuryl Alcohol
In addition, there is no report on the process conditions for the production of furfuryl alcohol by using the above-mentioned catalyst

Method used

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  • Preparation method of modified copper-based catalyst for furfural hydrogenation to furfuryl alcohol
  • Preparation method of modified copper-based catalyst for furfural hydrogenation to furfuryl alcohol
  • Preparation method of modified copper-based catalyst for furfural hydrogenation to furfuryl alcohol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Accurately weigh 0.2g MgCO 3 , 1g of anhydrous formic acid and 20mL of 1,4-dioxane were added to a 50mL autoclave, sealed, and stirred at 170°C for 30min. After cooling, add 1g Cu(NO 3 ) 2 4H 2 O, sealed reactor, N 2 Replace 3 to 5 times to empty, and react at 170°C for 30 minutes. After cooling, centrifuge, wash, and dry under vacuum at 60°C to obtain 57% Cu-MgCO 3 Composite catalyst. In a similar manner, change the additive to CaCO 3 、BaCO 3 or Ba(CH 3 COO) 2 ·H 2 O, copper salt precursor is Cu(HCOO) 2 4H 2 O, Cu(CH 3 COO) 2 ·H 2 O or CuSO 4 ·5H 2 O, modified Cu-based catalysts supported by different metals or additives can be prepared.

[0025] The above Cu-MgCO 3 Add 0.3g of catalyst, 0.6g of furfural and 20mL of 1,4-dioxane into the reaction kettle, then add 1.15g of anhydrous formic acid, after mixing and sealing, use N 2 The air was replaced 3 to 5 times, and the reaction was carried out at 170° C. for 2 hours. The conversion rate of furfuryl ...

Embodiment 2

[0027] Accurately weigh 0.08g BaCO 3 , 1g of anhydrous formic acid and 20mL of 1,4-dioxane were added to a 50mL autoclave, sealed, and stirred at 200°C for 30min. After cooling, add 0.43g Cu(HCOO) to the above reaction solution 2 4H 2 O, sealed reactor, N 2 Replace 3 to 5 times to evacuate, and react at 170°C for 30 minutes. After cooling, centrifuge, wash, and dry under vacuum at 60°C to obtain 60% Cu-BaCO 3 Composite catalyst. In a similar way, changing Cu(HCOO) 2 4H 2 O and BaCO 3 The amount of addition, the preparation of different mass fractions of Cu-BaCO 3 Composite catalyst.

[0028] The above Cu-BaCO 3 Add 0.3g of catalyst, 0.6g of furfural and 20mL of 1,4-dioxane into the reaction kettle, then add 1.15g of anhydrous formic acid, after mixing and sealing, use N2 Replace the air 3 to 5 times to discharge the air, react at 170°C for 2 hours, the conversion rate of furfuryl alcohol is 100%, and the selectivity is 99%. Under the same conditions, use 2MPa H 2 I...

Embodiment 3

[0030] Accurately weigh 0.08g BaCO 3 , 0.02g of anhydrous formic acid and 20mL of 1,4-dioxane were added to a 50mL autoclave, sealed, and stirred at 170°C for 30min. After cooling, add 0.43g Cu(HCOO) to the above reaction solution 2 4H 2 O, sealed reactor, N 2 Replace 3-5 times to empty, and react at 170°C for 60min. After cooling, centrifuge, wash, and dry under vacuum at 60°C to obtain 60% Cu-BaCO 3 Composite catalyst.

[0031] The above Cu-BaCO 3 Add 0.3g of catalyst, 0.6g of furfural and 20mL of 1,4-dioxane into the reaction kettle, then add 1.15g of anhydrous formic acid, after mixing and sealing, use N 2 The air was replaced 3 to 5 times, and the reaction was carried out at 170° C. for 2 hours. The conversion rate of furfuryl alcohol was 58%, and the selectivity was 97%. Under the same conditions, use 2MPa H 2 Instead of formic acid, the conversion rate of furfural is 41%, and the selectivity is 96%.

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Abstract

The invention discloses a furfural hydrogenation furfuryl alcohol modified copper-based catalyst preparation method, and relates to furfuryl alcohol. The method includes the steps: firstly, performingreaction on alkali metal salt modified agents and formic acid to form solution; secondly, regenerating a compound of copper salt and modified agent salt through hydrogen and carbon dioxide generatedby the formic acid in the decomposing process to form alkali carbonate modified copper-based catalyst. The prepared modified copper-based catalyst has high furfural conversion rate and furfuryl alcohol selectivity, and the yield of furfuryl alcohol can reach 80%-99% under suitable reaction conditions. Low-cost carbonate serves as a carrier or is doped into the catalyst, copper salt serves as a precursor, the copper-based catalyst with high activity is prepared by a simple in-situ reduction method, and furfural is catalyzed to prepare the furfuryl alcohol in a hydrogenation manner under the suitable process conditions. According to the furfural hydrogenation furfuryl alcohol modified copper-based catalyst, a preparation process is simple to operate, consumed time is short, cost is low, catalytic reaction activity is high, furfural selectivity is good, cycle performance is stable, and the catalyst has wide application prospects.

Description

technical field [0001] The present invention relates to furfuryl alcohol, in particular to the preparation of a modified copper-based catalyst for hydrogenation of furfural to furfuryl alcohol, which can be prepared by regenerating organic copper salt and alkali metal modifier salt complex with formic acid as a dissolving agent and regeneration agent method. Background technique [0002] Furfuryl alcohol is an important fine chemical widely used in synthetic fiber, rubber, resin, fragrance, pharmaceutical and pesticide intermediates and other industries. Furfuryl alcohol is the product of selective hydrogenation of furfural carbonyl. Cu-Cr catalysts are mainly used in industry, but the catalysts have high toxicity, short service life and unstable activity. The noble metal-supported catalysts developed in recent years are not conducive to large-scale production due to their high cost. As a common catalyst, non-noble metal or metal oxide supported catalyst is widely used in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/232C07D307/44
Inventor 孙勇杜鹃林鹿唐兴曾宪海雷廷宙
Owner XIAMEN UNIV
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