A kind of method of refining furandicarboxylic acid
A technology of furandicarboxylic acid and furandicarboxylic acid, which is applied in the direction of organic chemistry, can solve the problem of difficult separation of impurities, and achieve the effect of high decolorization rate and remarkable effect of impurity removal
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Embodiment 1
[0040] The FDCA solid processed in this embodiment is crude FDCA, the color is dark yellow, and the main components are: FDCA (91.54wt%), 5-hydroxymethylfurfural (0.86%), 2,5-diformylfuran (DFF, 1.35 wt%), 5-formaldehyde furan-2-carboxylic acid (FCA, 2.01 wt%), other impurities (4.24 wt%).
[0041] Mix 35g of DMAC and 10g of crude FDCA solid powder (mass ratio 2:1), stir in a 40°C water bath for 10min, after FDCA dissolves, cool down at a rate of 0.5°C / min to 20°C, then keep the temperature in a 20°C water bath for 60min , after crystallization and solid-liquid separation, washed with 6 mL of new DMAC solvent to obtain 10.52 g of FDCA adduct crystals. Take a small amount of crystals for thermogravimetric analysis, the results are as follows figure 1 As shown, the adduct crystallization solvent decomposes and volatilizes from the adduct crystallization as the temperature rises, and the weight loss is 53.224%, that is, the molecular ratio of FDCA to DMAC is about 1:2.04, which ...
Embodiment 2
[0046] Carry out the refining of FDCA in the mode similar to Example 1 in the present embodiment. Only the FDCA adopted in this embodiment is 10g of the product to be refined, the color is off-white, and the main components are: FDCA (97.22wt%), 5-hydroxymethyl-2-furanoic acid (HFCA, 2.13wt%), other Impurities (0.65 wt%). The solid mass ratio of DMAC to FDCA was 7:1, the dissolution temperature was 80°C, and the cooling rate was 0.1°C / min to 8°C. After solid-liquid separation, 10.86 g of FDCA adduct crystals were obtained. The mass fraction of solvent DMAC in the FDCA adduct crystallization was analyzed by gas chromatography to be 50.10%, that is, one FDCA molecule in the FDCA adduct crystallization was combined with about 2 DMAC molecules. The DMAC solvent was blown dry at 125° C. with a dry nitrogen blower to obtain 5.43 g of FDCA as a white solid. The same method as in Example 1 was analyzed by high pressure liquid chromatography. The purity of FDCA was 99.91 wt %, and the...
Embodiment 3
[0048] Carry out the refining of FDCA in the mode similar to Example 1 in the present embodiment. Just the raw material that adopts in the present embodiment is 10g FDCA solid waste, and color is tan, mainly consists of: FDCA (72.52wt%), DFF (6.33wt%), FCA (10.17wt%), other impurity (10.98wt%) %). Because the purity of FDCA is less than 90wt%, it needs to be pre-purified first: the mass ratio of DMAC to FDCA solid is 12:1, the dissolution temperature is 55°C, and the cooling rate is 55°C / min. 9.12 g of FDCA adduct crystals. The mass fraction of solvent DMAC in the FDCA-DMAC adducted crystals was analyzed by gas chromatography to be 51.22%, that is, one FDCA molecule in the FDCA adducted crystals was bound to about 2 DMAC molecules. Add the adducted crystals obtained after filtration to 2 times the mass of DMAC solvent, dissolve at 30°C and crystallize at 0°C for 4 hours, filter to obtain the repurified FDCA adducted crystals, dry in vacuum at 30°C for 6 hours to evaporate th...
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