Method and system for continuously synthesizing furandicarboxylic acid

A technology of furandicarboxylic acid and solid acid, which is applied in the direction of organic chemistry, can solve the problem of low yield of target products, achieve the effects of inhibiting side reactions, shortening reaction time, and promoting oxidation

Active Publication Date: 2018-09-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In summary, the target product yield of the current one-pot method is low, and it mainly focuses on the design of the catalyst

Method used

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  • Method and system for continuously synthesizing furandicarboxylic acid
  • Method and system for continuously synthesizing furandicarboxylic acid
  • Method and system for continuously synthesizing furandicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-4

[0048] Preparation of HMF by Dehydration of Sugars

[0049] Add 4g fructose, 16g DMSO and 1g Amberlyst-15 catalyst into a 50mL three-necked flask, pass N 2 Evacuate, heat up to the temperature shown in Table 1, fully stir, and react for 90 minutes to obtain HMF solution. The HMF content in the product liquid was analyzed by high performance liquid chromatography to obtain the HMF yield, as shown in Table 1.

[0050] The productive rate of fructose dehydration preparation HMF under table 1 different temperatures

[0051]

[0052] Wherein, the calculation method of HMF productive rate is as follows:

[0053]

Embodiment 5-7

[0055] Other process conditions and experimental steps are the same as in Example 4, but different reaction times are used in the stage of fructose dehydration reaction to prepare HMF. The reaction conditions and results are shown in Table 2.

[0056] The productive rate of fructose dehydration preparation HMF under table 2 different reaction times

[0057]

[0058]

[0059] It can be seen from Table 2 that in the early stage, as the reaction time increases, the yield of HMF basically shows an increasing trend. When the reaction time reaches 90 minutes, the yield of HMF reaches the maximum value. As the reaction time continues to increase, side reactions occur in HMF, and the yield begins reduce.

Embodiment 8-9

[0061] Other process conditions and experimental steps are the same as in Example 4, but different solvents are used in the stage of fructose dehydration reaction to prepare HMF, and the reaction results are shown in Table 3 below.

[0062] The productive rate that fructose dehydration prepares HMF in the different solvents of table 3

[0063]

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Abstract

The invention discloses a method for continuously synthesizing furandicarboxylic acid. The method comprises the following steps: (1) dissolving sugars into an organic solvent to prepare a sugar solution with the mass concentration of 5 percent to 50 percent; reacting at 60 to 140 DEG C for 0.5 to 12h under the action of a solid acid dehydration catalyst; (2) adding an alkaline water solution and an oxidant into effluent liquid of step (1); reacting for 2 to 12h under the action of a loading type oxidization catalyst and under the conditions of 60 to 110 DEG C and 0.1 to 1MPa; (3) evaporating the effluent liquid of step (2) to remove a solvent; then adding an acidifying agent and adjusting the pH (Potential of Hydrogen) to be less than 2; precipitating to obtain a furandicarboxylic acid crude product; filtering, washing and recrystallizing to obtain the furandicarboxylic acid. The invention further discloses a system for continuously synthesizing the furandicarboxylic acid. According tothe method disclosed by the invention, an intermediate 5-hydroxymethylfurfural does not need to be separated and purified and the furandicarboxylic acid is synthesized in a high-yield manner under moderate conditions; the method can be continuously operated and has an important application prospect.

Description

technical field [0001] The invention relates to the field of synthesis of furandicarboxylic acid, in particular to a method and system for continuously synthesizing furandicarboxylic acid. Background technique [0002] Due to the non-renewability of fossil resources such as oil and coal, the chemical industry based on fossil resources is not sustainable. Starting from renewable biomass resources, through efficient biological and chemical transformation, bio-based chemicals and energy sources with important application prospects can be obtained, which can find a reasonable and effective way to replace petrochemical products, and is the solution to the current unsustainable fossil resources. effective measures for the problem. [0003] 2,5-Furandicarboxylic acid (2,5-Furandicarboxylic acid, FDCA) is an important new type of bio-based monomer with broad application prospects. It is different from the traditional petroleum-based monomer terephthalic acid in terms of structure a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/68
CPCC07D307/68
Inventor 吴林波陈光宇
Owner ZHEJIANG UNIV
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