Method for preparing 2,5-furandicarboxylic acid by supported bifunctional catalyst by catalyzing fructose

A bifunctional catalyst, furandicarboxylic acid technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as inconsistency of catalysts, easy generation of waste water, strong corrosion, etc.

Active Publication Date: 2016-03-23
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, the current methods for preparing FDCA mostly use strong acid as a catalyst in the fructose dehydration step, which is highly corrosive and easy to generate waste water; and the generated HMF basically needs to be extracted and separated before the next oxidation reaction, the process is relatively cumbersome, or although In situ oxidation of HMF using a one-pot method, but the catalysts used in the dehydration and oxidation stages are inconsistent

Method used

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  • Method for preparing 2,5-furandicarboxylic acid by supported bifunctional catalyst by catalyzing fructose
  • Method for preparing 2,5-furandicarboxylic acid by supported bifunctional catalyst by catalyzing fructose
  • Method for preparing 2,5-furandicarboxylic acid by supported bifunctional catalyst by catalyzing fructose

Examples

Experimental program
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Effect test

Embodiment 1

[0045] K 6 [CoW 12 o 40 ]·16H 2 The preparation of O solid heteropolyacid:

[0046] (A1) 19.8gNa 2 WO 4 2H 2 O was dissolved in 40mL deionized water and adjusted to pH5.0-7.0 with glacial acetic acid to obtain solution A, 2.5g (CH 3 CO 2 ) 2 Co 4H 2 O was dissolved in 12mL deionized water, adjusted to pH 5.0-7.0 with glacial acetic acid to obtain solution B; both solution A and solution B were heated to close to the boiling point, and solution B was slowly dropped into solution A while hot to produce a dark green solution , the mixture was boiled for 10-20 minutes and then filtered while it was hot;

[0047] (A2) Reheat the filtrate obtained in step (A1), and dissolve 20 mL of saturated CH with a pH of 6.0-7.0 3 Slowly add COOK solution to the heated filtrate, stir to produce a green solid, cool to room temperature and filter, wash the solid twice with the filtrate, dissolve the solid in 40mL of 2M sulfuric acid solution, stir at 50°C for 15min, the solution turns d...

Embodiment 2

[0049] Solid catalyst heteropoly acid salt K 5 [Co III W 12 o 40 ]·20H 2 Preparation of O:

[0050] On the basis of Example 1, the filtrate C was heated to boiling, and 10 g K 2 S 2 o 8 , after the solution turns from blue to yellow, stop heating, cool in an ice bath to obtain yellow needle-like crystals, filter to obtain K 5 [Co III W 12 o 40 ]·20H 2 O solid heteropolyacids.

Embodiment 3

[0052] Dawson type Co 2 h 6+n P 2 Mo 18-n V n o 62 (n=3) preparation of heteropolyacid catalyst:

[0053] (A1) Dissolve 0.015mol of ammonium metavanadate in 75ml of distilled water, dissolve 0.01mol of sodium dihydrogen phosphate in 12.5ml of distilled water, stir to make it fully dissolved and mix, add dropwise 49wt% sulfuric acid aqueous solution to adjust pH4.0-6.0, add 0.075mol Sodium molybdate aqueous solution 37.5ml, add 49wt% sulfuric acid aqueous solution dropwise again to adjust pH 4.0-6.0, reflux at 100-120°C for 8h, cool, extract with ether, add a small amount of 49wt% sulfuric acid aqueous solution in batches, shake until red oil appears , standing for stratification, separating the lower layer, standing in the fume hood for 1-2 days, until the crystalline particles are precipitated, adding a small amount of distilled water to recrystallize, and vacuum drying to obtain phosphomolybdovanadate heteropolyacid H 9 P 2 Mo 15 V 3 o 62 ;

[0054] (A2) 2mmol of ...

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Abstract

The invention provides a method for preparing 2,5-furandicarboxylic acid by catalyzing fructose with a supported bifunctional catalyst. According to the method, a supported heteropolyacid salt is taken as a catalyst; and the catalyst disclosed by the invention is the bifunctional catalyst, and has acidity and catalytic oxidation performance. The fructose and biomass materials rich in the fructose can be efficiently catalyzed to dewater and prepare HMF; and meanwhile, 2,5-furandicarboxylic acid can be prepared by in-situ catalytic oxidation of the HMF at high selectivity. The catalyst is convenient to recycle and good in reusability, so that a foundation is laid for efficient preparation of the 2,5-furandicarboxylic acid.

Description

technical field [0001] The invention provides a method for preparing 2,5-furandicarboxylic acid by catalyzing fructose with a supported bifunctional catalyst, which belongs to the technical field of chemical synthesis. Background technique [0002] Petroleum, as an energy source and a raw material for the production of petrochemicals, has abundant downstream products and is widely used in various industries with increasing demand. However, due to its non-renewability, under the dual pressure of energy crisis and environmental protection, the development of new renewable Alternative energy has become a major strategic issue of global concern. Glucose, fructose, sucrose, cellulose, hemicellulose, lignin and other biomass raw materials are abundant in nature and low in price. They are important biomass resources. They can be synthesized into high value-added chemical intermediates through chemical methods. It has become an important way to rationally utilize biomass resources....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/68B01J23/882B01J23/888B01J27/188B01J27/19B01J27/199B01J29/16B01J29/48B01J29/78
CPCY02P20/584C07D307/68B01J23/882B01J23/888B01J27/188B01J27/19B01J27/199B01J29/166B01J29/48B01J29/7815B01J2229/186
Inventor 应汉杰刘铖朱晨杰汤晶晶吴菁岚陈勇陈晓春
Owner NANJING UNIV OF TECH
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