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Preparation method of catalyst for preparation of FDCA through catalytic oxidation of HMF, and application of catalyst

A catalytic oxidation and catalyst technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve problems such as poor selectivity and low catalytic activity, and achieve low cost , good catalytic activity and high selectivity

Inactive Publication Date: 2018-05-18
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Non-precious metal catalysts have problems such as low catalytic activity and poor selectivity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Place the round bottom flask in a constant temperature magnetic stirring water bath, weigh 1mmol HMF and 15mmol potassium ferrate into the round bottom flask, measure 10mL deionized water into the beaker, stir evenly, weigh a certain amount of NaOH, and make Its molar concentration in the reaction system is 1.6mol / L, and a certain amount of K 2 HPO 4 , so that the molar concentration in the reaction system is 0.2mol / L, after reacting at 25°C for 15 minutes, the solution is in the form of a slurry, and the slurry is filtered to obtain a filtrate, and concentrated hydrochloric acid is added dropwise to the filtrate until there is a large amount of white Precipitation was formed, the obtained turbid liquid was filtered, and the substance was baked in an oven at 50° C. for 24 hours to obtain a dry white product FDCA with a yield of 80%.

Embodiment 2

[0032]Place the round bottom flask in a constant temperature magnetic stirring water bath, weigh 1mmol HMF and 15mmol potassium ferrate into the round bottom flask, measure 10mL deionized water into the beaker, stir evenly, weigh a certain amount of NaOH, and make Its molar concentration in the reaction system is 1.6mol / L, and a certain amount of K 2 HPO 4 , so that the molar concentration in the reaction system is 0.4mol / L. After reacting at 25°C for 15 minutes, the solution is in the form of slurry. The slurry is filtered to obtain the filtrate, and concentrated hydrochloric acid is added dropwise to the filtrate until there is a large amount of white Precipitation was formed, the obtained turbid solution was filtered, and the substance was baked in an oven at 50° C. for 24 hours to obtain a dry white product FDCA with a yield of 86.1%.

Embodiment 3

[0034] Place the round bottom flask in a constant temperature magnetic stirring water bath, weigh 1mmol HMF and 15mmol potassium ferrate into the round bottom flask, measure 10mL deionized water into the beaker, stir evenly, weigh a certain amount of NaOH, and make Its molar concentration in the reaction system is 1.6mol / L, and a certain amount of K 2 HPO 4 , so that the molar concentration in the reaction system is 0.6mol / L. After reacting at 25°C for 15 minutes, the solution is in the form of slurry. The slurry is filtered to obtain the filtrate, and concentrated hydrochloric acid is added dropwise to the filtrate until there is a large amount of white Precipitation was formed, the obtained turbid solution was filtered, and the substance was baked in an oven at 50° C. for 24 hours to obtain a dry white product FDCA with a yield of 80.6%.

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Abstract

The invention relates to a catalyst preparation technology, and aims to provide a preparation method of a catalyst for preparation of FDCA (2,5-furandicarboxylic acid) through catalytic oxidation of HMF (5-hydroxymethylfurfural), and application of the catalyst. The application method comprises the following steps: adding HMF and potassium ferrate into a reaction container; adding deionized water,NaOH and K2HPO4 into a flask, and reacting under the condition of 25 DEG C for 15 minutes, wherein after the reaction, the solution is pasty; filtering to obtain filtrate, and adding concentrated hydrochloric acid into the filtrate dropwise until a large amount of white precipitate is generated; and filtering, putting solid substances into a drying box at the temperature of 50 DEG C and drying for 24 hours to obtain a white product, namely the 2,5-furandicarboxylic acid. The catalytic cost of the potassium ferrate is lower relative to that of noble metal, and the reduction product of the potassium ferrate after reaction is ferric oxide hydrate which is environmentally friendly, is a green product and avoids pollution. Through control of the alkaline condition of the system and the use amount of the buffer solution K2HPO4, the stability of the potassium ferrate can be improved and efficient preparation is realized.

Description

technical field [0001] The invention relates to catalyst preparation technology, in particular to a catalyst used for catalytic oxidation of HMF to prepare FDCA and an application method thereof. Background technique [0002] Since the industrial revolution, countries around the world have used petroleum resources in large quantities. With the gradual depletion of non-renewable petroleum resources and the increasing price of the world, the traditional petroleum-based polyester industry is facing great challenges. Therefore, it is extremely important to research and develop renewable polyester materials to gradually replace traditional petroleum-based polyesters. In recent years, a kind of 2,5-furandicarboxylic acid (FDCA) prepared from woody biomass-based platform compound——5-hydroxymethylfurfural (5-hydroxymethylfurfural, HMF) has With a structure similar to terephthalic acid, it is considered to be a very promising biomass-based polyester monomer, which has attracted much...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/78B01J23/889C07D307/68
CPCB01J23/002B01J23/78B01J23/8892B01J2523/00C07D307/68B01J2523/13B01J2523/72B01J2523/842B01J2523/17
Inventor 张俊华谢文兴梁启迪
Owner ZHEJIANG SCI-TECH UNIV
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