Method for producing hydroxymethylfurfural by using two-phase method
A technology of hydroxymethyl furfural and biomass raw materials, applied in the direction of organic chemistry and the like, can solve the problems of high cost, high boiling point, large heat of vaporization, etc., and achieve the effects of fast reaction speed, low temperature, and green process.
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Embodiment 1
[0028] (1) 40g zinc chloride, 5g concentrated hydrochloric acid and 55g water mix evenly, prepare zinc chloride reaction solution 72ml;
[0029] (2) Mix 0.5 g of dried cellulose microcrystals with 100 g of the above-mentioned zinc chloride reaction solution, use 36 ml of 2,5-dimethylpentanone as the extractant, and react at 100° C. for 160 min;
[0030] (3) The 2,5-dimethylpentanone phase obtained after the reaction was concentrated and evaporated to dryness, and crystallized with ethanol to obtain a hydroxymethylfurfural product, and the molar yield of the reaction was 43%.
Embodiment 2
[0032] (1) 45g zinc chloride, 0.1g vitriol oil and 54.9g water are mixed, prepare zinc chloride reaction solution 70ml;
[0033] (2) 10 g of dried wheat straw was mixed with 100 g of zinc chloride reaction solution, and 70 ml of 1-butanol was used as an extractant, and reacted at 110° C. for 15 h;
[0034] (3) The 1-butanol phase obtained after the reaction was concentrated and evaporated to dryness, crystallized with acetone to obtain a hydroxymethylfurfural product, and the molar yield of the reaction was 50%.
Embodiment 3
[0036] (1) 50g zinc chloride, 3g phosphoric acid and 47g water mix evenly, prepare zinc chloride reaction solution 66ml;
[0037] (2) Mix 5 g of dried rice straw with 100 g of zinc chloride reaction solution, use 180 ml of ethyl butyrate as the extractant, and react at 115° C. for 10 h;
[0038] (3) The ethyl butyrate phase obtained after the reaction was concentrated and evaporated to dryness, and the hydroxymethylfurfural product was obtained by crystallization with ethyl acetate, and the molar yield of the reaction was 36%.
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