Study On The Characterization Of 5-hydroxymethylfurfural And Its Derivatives

With the increasing attention paid to environmental protection and fossil resource issues,it is particularly important to develop bio-based compounds using renewable biomass resources.5-hydroxymethylfurfural（HMF）is an important bio-based platform compound,as a key bridge linking biomass and petroleum chemicals,it can prepare a variety of high value-added chemicals through oxidation,hydrogenation,esterification and other reactions,and then it is widely used in polymer materials,chemical industry and energy fields.2,5-Furanedicarboxylic acid（FDCA）is an oxidized derivative of HMF and a green substitute for terephthalic acid.Tetrahydrofuran dimethanol（THFDM）is a chemical intermediate derived from deep hydrogenation of HMF,which has higher stability than unsaturated furan compounds and can be used as a stabilizer,dispersant and decolorizer.Due to the lack of corresponding standards and reference materials,the market for HMF,FDCA and THFDM products is chaotic.The research goal of this paper is to develop three biological based chemical reference materials.Firstly,qualitative analysis of HMF,FDCA and THFDM was performed using UV,NMR,IR,and MS methods.Secondly,the mass balance method was used to conduct a calibration study on the sample,the optimum conditions for the determination of principal component content were determined.At the same time,the content of moisture,ash and volatile solvent were determined accurately.Thirdly,by optimizing the deuterium reagent,internal standard,quantitative peak and experimental parameters,the optimum conditions for determining the purity of HMF by quantitative nuclear magnetic method were established:ethyl paraben was used as internal standard and DMSO-d₆ as deuterium solventδ7.42 andδ7.83 were selected as quantitative peaks.The optimized instrument conditions were SW 13 ppm,O1P 7.65 ppm,D1 30 s,DS 16 times,NS 32 times,AQ 6.30 s,Te 298 K and HMF determination result was 99.54%.At the same time,the optimum determination conditions of FDCA and THFDM were determined.The fixed values of FDCA and THFDM were 99.70%and 99.53%.Finally,the uniformity and stability of the samples were investigated in the experiment,and the results of the two methods were statistically processed.The purity of HMF was 99.53%,the expanded uncertainty was 0.136%（k=2）,the purity of FDCA was 99.72%,the expanded uncertainty was 0.628%（k=2）,the purity of THFDM was 99.55%and the expanded uncertainty was 0.195%（k=2）.