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Hydrogenation catalyst for 2, 5-furandicarboxylic acid and reaction process

A technology of furandicarboxylic acid and tetrahydrofurandicarboxylic acid, which is applied in the field of 2,5-furandicarboxylic acid hydrogenation catalyst and its reaction process, can solve the problems of less research, achieve strong acid corrosion resistance, good stability, and simplify production The effect of process operations

Pending Publication Date: 2022-08-05
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are few related studies on the preparation of THFDCA by hydrogenation of FDCA

Method used

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  • Hydrogenation catalyst for 2, 5-furandicarboxylic acid and reaction process

Examples

Experimental program
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Effect test

Embodiment 1

[0022] By dipping method, 0.65g RuCl 3 ·3H 2 O was added to 5 mL of aqueous solution, and 5 g of TiO was added 2 The carrier was mixed, then stirred at 25°C until it became a paste, left standing at room temperature for 24h to make the ruthenium salt evenly dispersed in the carrier, and then dried in an oven at 110°C for 12h. Final catalyst precursor at 500 °C H 2 Reduction in atmosphere for 4h, H 2 The flow rate was 40 mL / min.

[0023] Catalyst performance test: In a 75mL autoclave, add 0.2g of the 5% Ru / TiO prepared above 2 Catalyst, 1g FDCA, 20mL water, after the reactor is airtight, fill with 1MPa hydrogen to replace the residual air in the reactor, after repeating 6-8 times, fill the reactor with hydrogen, the reaction pressure is 2MPa, and the reaction temperature is 120°C , stirred at 700rpm, and reacted for 1h. After the reaction, the liquid-solid mixture was taken out for suction filtration separation, the obtained liquid was filtered with a 0.22um membrane, the...

Embodiment 2

[0025] By dipping method, 0.78g RuCl 3 ·3H 2 O was added to 10 mL aqueous solution, and 10 g SiO was added 2 The carrier was mixed, then stirred at 25°C until it became a paste, left at room temperature for 24h to make the ruthenium salt evenly dispersed in the carrier, and then dried in an oven at 100°C for 12h. Final catalyst precursor at 550 °C H 2 Reduction in atmosphere for 4h, H 2 The flow rate was 50 mL / min.

[0026] Catalyst performance test: In a 75mL autoclave, add 0.5g of the 3% Ru / SiO prepared above 2 Catalyst, 2g FDCA, 20mL tetrahydrofuran, after the reactor is sealed, fill with 1MPa hydrogen to replace the residual air in the reactor, after repeating 6-8 times, fill the reactor with hydrogen, the reaction pressure is 2MPa, and the reaction temperature is 100°C , stirred at 700rpm, and reacted for 2h. After the reaction, the liquid-solid mixture was taken out for suction filtration separation, the obtained liquid was filtered with a 0.22um membrane, the obta...

Embodiment 3

[0028] Using the impregnation method, 1.3 g RuCl 3 ·3H 2 O was added to 10 mL of aqueous solution, and 10 g of diatomaceous earth carrier was added to mix, then stirred at 50 °C until it became a paste, stood at room temperature for 24 h to make the ruthenium salt evenly dispersed in the carrier, and then dried in an oven at 110 °C Dry for 12h. Final catalyst precursor at 400 °C H 2 Reduction in atmosphere for 4h, H 2 The flow rate was 100 mL / min.

[0029] Catalyst performance test: In a 75mL autoclave, add 0.2g of the 5% ruthenium / diatomite catalyst prepared above, 2g of FDCA, and 20mL of methanol. After the reactor is sealed, fill it with 1MPa hydrogen to replace the residual air in the reactor. After repeating 6-8 times, the reaction kettle was filled with hydrogen, the reaction pressure was 3MPa, the reaction temperature was 120°C, and the reaction was carried out for 2h under stirring at a speed of 700rpm. After the reaction, the liquid-solid mixture was taken out fo...

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Abstract

The invention discloses a hydrogenation catalyst for 2, 5-furandicarboxylic acid and a reaction process. The catalyst takes one of palladium, ruthenium or rhodium as an active component; the oxide is used as a carrier, and the carrier is one of aluminum oxide, silicon oxide, titanium oxide, zirconium oxide, attapulgite, diatomite and hydrotalcite; the catalyst is used for a reaction for preparing 2, 5-tetrahydrofurandicarboxylic acid through catalytic hydrogenation of 2, 5-furandicarboxylic acid. Due to the synergistic catalysis effect of the active metal and the oxide and the high-temperature heat treatment reduction process, the catalyst has high reaction activity and good stability. Under mild reaction conditions, 2, 5-furandicarboxylic acid can be converted into 2, 5-tetrahydrofurandicarboxylic acid with high selectivity by the catalyst, and the catalyst can be recycled.

Description

technical field [0001] The invention belongs to the technical field of preparation of nano metal catalysts, in particular to a 2,5-furandicarboxylic acid hydrogenation catalyst and a reaction process thereof. Background technique [0002] 2,5-Furandicarboxylic acid (FDCA) is considered as a platform molecule for the conversion of biomass cellulose, hemicellulose and starch into fuels and downstream chemicals. As early as 2004, the U.S. Department of Energy has listed FDCA as one of the most important "Twelve Platform Molecules" for biomass conversion and utilization in the future. FDCA can be used to produce degradable plastics, semi-aromatic nylons, unsaturated resins, etc. It can be used as a modifier for petroleum-based polymers in the short term. The market potential is huge. FDCA has been included in the top 10 bio-refined carbohydrates produced by bio-based industrial products. derivative. [0003] 2,5-Tetrahydrofurandicarboxylic acid (THFDCA) is a downstream derivat...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J23/44C07D307/24
CPCB01J23/462B01J23/464B01J23/44C07D307/24B01J35/23Y02P20/584
Inventor 荣泽明王梓旭任小红杜雪霏王梅王越
Owner DALIAN UNIV OF TECH
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