Method for efficiently converting furfural to gamma-valerolactone by using POMOF catalyst synthesis and one-pot method

A catalyst, valerolactone technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the complex composition method, difficult operation and low safety and other problems, to achieve the effect of strong operability, simple reaction system and stable catalytic performance

Active Publication Date: 2019-05-03
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007]Therefore, there is an urgent need for a method for POMOF catalyst synthesis and one-pot efficient conversion of furfural to gamma-valerolactone, which solves the complex composition method existing in the prior art , high cost, difficult operation and low safety

Method used

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  • Method for efficiently converting furfural to gamma-valerolactone by using POMOF catalyst synthesis and one-pot method
  • Method for efficiently converting furfural to gamma-valerolactone by using POMOF catalyst synthesis and one-pot method
  • Method for efficiently converting furfural to gamma-valerolactone by using POMOF catalyst synthesis and one-pot method

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Effect test

preparation example Construction

[0039] The preparation method of POMOF catalyst comprises the following steps:

[0040] Step (1), 0.9624g ZrOCl 2 ·8H 2 O and 0.6996g of terephthalic acid were dissolved in 50mL of dimethylformamide solution; then transferred to a 100mL capacity reactor, heated at 120°C for 12 hours and then cooled;

[0041] Step (2), centrifuge the product obtained in step (1) with an 8000rpm centrifuge, remove the liquid, then add dimethylformamide to wash and continue centrifuging, remove the liquid; then add water to wash and then centrifuge again, remove liquid; finally add ethanol to wash and continue to centrifuge, remove the liquid;

[0042] Step (3), cycle step (2) once, after removing the liquid for the last time, place the centrifuge tube containing the solid in an oven at 100°C for 12 hours to obtain UiO-66;

[0043] Step (4), get 1g UiO-66 and 0.1-1g H 3 [P(W 3 o 10 ) 4](PW) was dispersed in 100mL of water, put into a reflux device containing a 250mL round bottom flask, ref...

Embodiment 1

[0050] Put 0.67mmol of furfural, 0.1g of POMOF-PW-0.5, and 20ml of isopropanol into a 35mL autoclave. After sealing the autoclave, stir and react at 160°C for 23h. After the autoclave is cooled, it is ready to be tested.

[0051] The preparation method of the POMOF catalyst is as follows: dissolve 0.9624g ZrOCl2 8H2O and 0.6996g terephthalic acid in 50mL dimethylformamide (DMF); then move it into a 100mL capacity reactor, heat it in water at 120°C for 12h and then cool it down . Then centrifuge with 8000rpm centrifuge to remove the liquid, then add dimethylformamide to wash and continue to centrifuge to remove the liquid; then add water to wash and then centrifuge again to remove the liquid; finally add ethanol to wash and continue to centrifuge to remove the liquid ; The aforementioned steps of washing and centrifugation were cycled once, and after the liquid was removed for the last time, the centrifuge tube containing the solid was dried in an oven at 100°C for 12 hours, an...

Embodiment 2

[0058] Put 0.67mmol of furfural, 0.1g of POMOF-PW-0.1, and 20ml of isopropanol into a 35mL autoclave. After sealing the autoclave, stir and react at 160°C for 23h. After the autoclave is cooled, it is ready to be tested.

[0059] The preparation method of the POMOF catalyst is as follows: dissolve 0.9624g ZrOCl2 8H2O and 0.6996g terephthalic acid in 50mL dimethylformamide (DMF); then move it into a 100mL capacity reactor, heat it in water at 120°C for 12h and then cool it down . Then centrifuge with 8000rpm centrifuge to remove the liquid, then add dimethylformamide to wash and continue to centrifuge to remove the liquid; then add water to wash and then centrifuge again to remove the liquid; finally add ethanol to wash and continue to centrifuge to remove the liquid ; The aforementioned steps of washing and centrifugation were cycled once, and after the liquid was removed for the last time, the centrifuge tube containing the solid was dried in an oven at 100°C for 12 hours, an...

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Abstract

The invention discloses a method for efficiently converting furfural to gamma-valerolactone by using POMOF catalyst synthesis and a one-pot method. In an isopropanol solvent, the one-pot method is used for converting the furfural into the gamma-valerolactone. The reaction process comprises the following steps: putting furfural, isopropanol and POMOF into a high-pressure reaction kettle, uniformlycarrying out mixing, carrying out sealing, then carrying out stirring for 1-48 hours at a temperature of 120-180 DEG C, and carrying out cooling to obtain a gamma-valerolactone solution. The catalystused in the method is cheap, is easily available, and has stable catalytic performance and good reusability. In addition, a hydrogen environment is not needed in the whole reaction, inorganic acid isnot used, and high operation safety and very good industrial application potential are achieved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a POMOF catalyst synthesis and a one-pot method for efficiently converting furfural into gamma-valerolactone. Background technique [0002] γ-valerolactone (γ-GVL), as a multifunctional biomass-derived platform chemical, has been widely used in the field of It has developed rapidly in the past ten years. The existing production strategy of γ-GVL is synthesized by hydrogenolysis of levulinic acid or its esters. However, such raw materials are usually expensive, and commonly used catalysts are hydrogenation catalysts containing precious metals such as Pt, Pd, and Au, which are expensive and easy to deactivate. High catalyst has great significance. [0003] Levulinic acid and its esters can be prepared by hydrolysis of furfural or its intermediates (furfural is an important derivative of hemicellulose). If starting from furfural, design a catalyst to prepare γ-GVL in one ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33B01J31/22B01J27/188B01J27/19B01J31/34
Inventor 田戈马明伟侯攀曹靖劼刘辉徐兴良鄢歆雨
Owner JILIN UNIV
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