Coordination zirconium phosphotungstate catalyst and its application in catalytic hydrogenation of furfural

Patent metadata

Field	Value
Publication number	US-11938465-B2
Application number	US-201916971775-A
Country	US
Kind code	B2
Filing date	Mar 18, 2019
Priority date	Mar 18, 2019
Publication date	Mar 26, 2024
Grant date	Mar 26, 2024

Abstract

The invention discloses a coordination type zirconium phosphotungstate catalyst and its application in catalytic hydrogenation of furfural, belonging to the field of heterogeneous catalysis. The zirconium phosphotungstate catalyst prepared by the invention not only has good catalytic effect on the conversion of furfural to furfuryl alcohol, but also has mild reaction conditions. The yield of solid line furfuryl alcohol can be 98% if it can be reacted for 1 h at 120 ° C., and the amount of catalyst is less, which greatly reduces the energy consumption in the prior art. In addition, the zirconium phosphotungstate prepared by the invention is easy to separate, has good stability for catalyzing the hydrogenation of furfural to furfuryl alcohol, and is a new, efficient and green catalyst.

First claim

What is claimed is:

1. A method for preparing furfuryl alcohol by catalytic hydrogenation of furfural comprising hydrogenating the furfural in presence of the coordination zirconium phosphotungstate as a catalyst, wherein the method of making the coordination type zirconium phosphotungstate catalyst comprising: dissolving phosphotungstic acid and ZrCl 4 in DMF respectively to obtain phosphotungstic acid solution and ZrCl 4 solution; after ultrasonic treatment, adding phosphotungstic acid solution drop by drop into ZrCl 4 solution within 5-30 min;
after uniform mixing, adding triethylamine; then reacting at room temperature for 3-6 hours; aging more than 4 hours; washing for 1-3 times with DMF, methanol, and anhydrous ether respectively;
and drying in vacuum at 70-100° C. for more than 8 hours.

2. The method according to claim 1 wherein the hydrogenating is conducted in presence of isopropanol in an amount of 5-10 ml/mmol furfural as a hydrogen source.

3. The method according to claim 2 wherein the amount of isopropane is 5 ml/mmol furfural.

4. The method of claim 1 wherein the hydrogenating is conducted at a temperature of 120° C.

5. The method of claim 1 wherein the hydrogenating is conducted for 1 hour.

6. The method of claim 1 further comprising converting the furfuryl alcohol to resin, fuel, synthetic fiber, rubber, plastic, or pesticide.

7. The method of claim 1 wherein the hydrogenating is conducted in presence of 0.01-0.03 g coordination zirconium phosphotungstate/mmol furfural as the catalyst at 110-150° C. for 0.5-4 hours.

8. The method according to claim 1 wherein the molar ratio of the phosphotungstate and ZrCl 4 is 3:1˜1:3.

9. The method according to claim 1 wherein the concentration of the phosphotungstate solution is (0.05-0.15) mol/L, and the concentration of the ZrCl 4 solution is (0.05-0.15) mol/L.

10. The method according to claim 1 wherein the ultrasonic treatment time is 5 to 30 minutes.

Assignees

• Univ Jiangnan

Inventors

• Zhang Liping
• Wang Haijun
• Xu Guangzhi
• Liu Chen

Classifications

• B01J2235/30

  Scanning electron microscopy; Transmission electron microscopy · CPC title

• B01J2235/15

  X-ray diffraction · CPC title

• B01J27/188 Primary

  with chromium, molybdenum, tungsten or polonium · CPC title

• B01J37/04

  Mixing {(B01J37/0009, B01J37/0018 take precedence)} · CPC title

• B01J37/06

  Washing {(B01J37/0009, B01J37/0018 take precedence)} · CPC title