Method for preparing 2,5-furandicarboxylic acid (FDCA) from 5-hydroxymethylfurfural (5-HMF)
A technology of hydroxymethyl furfural and furandicarboxylic acid, applied in the field of chemical preparation, can solve the problems of high reaction conditions and poor product selectivity, and achieve the effects of simple process, high selectivity and yield, and increased solubility
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Embodiment 1
[0041] In a 10 mL Shrek tube, charge 126 mg 5-hydroxymethylfurfural (5-HMF), 11 mg Catalyst 1, and 24 mg NaNO 2 , then add 60mg H 3 PO 4 , 0.2mL of water and 2mL of tert-butanol, and heated to 55°C in a water bath for 48h in an oxygen atmosphere at normal pressure with magnetic stirring (stirring rate: 800r / min). After the reaction was completed, samples were sent to high-performance liquid chromatography (HPLC) under agitation for detection, wherein the detection conditions were as follows: Hitachi L2000 HPLC System, Alltech C18 column, mobile phase CH 3 OH:H 2 O=20:80; flow rate: 1.0 mL / min, column temperature: 30° C., detector: DAD, detection wavelength: 264 nm. As detected by HPLC, the yield of the product 2,5-furandicarboxylic acid (FDCA) was 92.17%, the selectivity was 95%, and its purity was 99%.
Embodiment 2
[0043] Concrete reaction process and detection method are identical with embodiment 1, only change tert-butanol into 3-methyl-pentan-3-alcohol, as a result gained main product is 2,5-furandicarboxylic acid (FDCA), and receive The yield was 85.76%, the selectivity was 96%, and its purity was 99.3%.
Embodiment 3
[0045] Concrete reaction process and detection method are identical with embodiment 1, just change tert-butanol into tert-amyl alcohol, as a result gained main product is 2,5-furandicarboxylic acid (FDCA), and yield is 80.33%, selectivity is 98%, and its purity is 98.6%.
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