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Preparation method of dimethyl furan-2, 5-dicarboxylate

A technology of dimethyl furandicarboxylate and hydroxymethyl furfural, applied in directions such as organic chemistry, to achieve the effects of excellent performance, efficient catalyst and low cost

Inactive Publication Date: 2018-05-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

If the selectivity of the product is not high, it exists in the form of a mixture of acids and esters, and its subsequent different polymerization processes will inevitably cause further product purification problems

Method used

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  • Preparation method of dimethyl furan-2, 5-dicarboxylate
  • Preparation method of dimethyl furan-2, 5-dicarboxylate

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Experimental program
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Effect test

Embodiment 1

[0015] CoO x -N / C-phen (Co 3.0wt%) catalyst, 0.5mmol 5-hydroxymethylfurfural, and 10ml of methanol are added to a stainless steel high-pressure reaction kettle, which is lined with polytetrafluoroethylene, and the metal: 5-hydroxymethylfurfural =0.13:1 (mol:mol). The temperature was raised to a reaction temperature of 100° C. using an automatic temperature controller, and 0.6 MPa oxygen was added to react for 12 hours, keeping the pressure constant during the reaction. The reaction products were analyzed by GC, and the reaction results are shown in Table 1.

Embodiment 2

[0017] 40mg MnO 2 , 0.5 mmol of 5-hydroxymethylfurfural and 10 ml of methanol were added to a stainless steel autoclave with a polytetrafluoroethylene lining inside. The temperature was raised to a reaction temperature of 100° C. using an automatic temperature controller, and 0.6 MPa oxygen was added to react for 12 hours, keeping the pressure constant during the reaction. The reaction products were analyzed by GC, and the reaction results are shown in Table 1.

Embodiment 3

[0019] 40mg Mn 3 o 4 , 0.5 mmol of 5-hydroxymethylfurfural and 10 ml of methanol were added to a stainless steel autoclave with a polytetrafluoroethylene lining inside. The temperature was raised to a reaction temperature of 100° C. using an automatic temperature controller, and 0.6 MPa oxygen was added to react for 12 hours, keeping the pressure constant during the reaction. The reaction products were analyzed by GC, and the reaction results are shown in Table 1.

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Abstract

The invention relates to a method for synthesis of dimethyl furan-2, 5-dicarboxylate from 5-hydroxymethylfurfural by means of catalytic oxidation. The method adopts oxygen or air as the oxidant and uses a cheap metal catalyst for efficient and highly selective catalysis of 5-hydroxymethylfurfural oxidation esterification, thus synthesizing dimethyl furan-2, 5-dicarboxylate. The catalytic reactionof the method has simple operation and mild conditions, the reaction system has no need for adding alkali additive, the 5-hydroxymethylfurfural conversion rate reaches 99% or more, and the yield of the product dimethyl furan-2, 5-dicarboxylate can reach 99%.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to a method for synthesizing dimethyl 2,5-furandicarboxylate. Background technique [0002] Dimethyl 2,5-furandicarboxylate is an important biomass-derived chemical and has attracted attention in the field of biomass conversion. In recent years, with the development of biomass-based synthetic chemicals, researchers have begun to focus on the synthesis of dimethyl 2,5-furandicarboxylate. It and 2,5-furandicarboxylic acid in the form of carboxylic acid can be used as a monomer to prepare a new generation of bio-based polyester PEF. The polyester is not only similar to the important petroleum-based polyester PET (polyethylene terephthalate) in terms of monomer structure, but also has the advantage of biodegradability. It has passed the EU food safety certification and has important application development value. Therefore, the development of a simple, efficient, and ...

Claims

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Application Information

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IPC IPC(8): C07D307/68
CPCC07D307/68
Inventor 徐杰孙玉霞马红罗杨张树静高进马继平贾秀全
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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