Levoglucosenone preparation method
A technology of L-glucosone and carbon sulfonic acid is applied in the preparation of sugar derivatives, chemical instruments and methods, dehydrated sugars, etc., to avoid environmental pollution, simplify the pretreatment process of raw materials, and facilitate recovery.
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Embodiment 1
[0022] Using 200 g of dry poplar wood (average particle size 0.1 mm) as raw material, the temperature was raised from room temperature to 350 ℃ at a rate of 20 ℃ / min under a vacuum of 50 Pa and kept for 1 h for pyrolysis to obtain Poplar charcoal: Mix the above poplar charcoal and concentrated sulfuric acid (98%) at a mass ratio of 1:10, then sulfonate at a constant temperature of 150 °C for 12 h under a nitrogen atmosphere, and wash with deionized water until no sulfuric acid is removed after cooling Root ions were obtained after drying to obtain 40 g of charcoal sulfonic acid.
[0023] Take 10 g of the above charcoal sulfonic acid and grind it to an average particle size of 0.2 mm. Poplar wood is used as a raw material (average particle size is 0.1 mm), and the two are mechanically mixed. The mass ratio of poplar wood and charcoal sulfonic acid is 1:2 , and then the mixture was pyrolyzed at 330 °C for 25 s under a nitrogen atmosphere, and the yield of liquid product was 47%....
Embodiment 2
[0025] Measure 30 g of FeCl respectively 2 4H 2 O and 6 g FeCl 3 ·6H 2 O, add water to prepare a 200 mL mixed solution and add it to a three-necked flask, place it in a constant temperature water bath at 65 °C, and slowly add NaOH solution with a concentration of 0.1 mol / L dropwise while stirring until the pH value of the solution reaches 12, continue Stir and age at constant temperature for 30 min; then remove the three-neck flask from the constant temperature water bath and cool to room temperature, use a magnetic field to separate the magnetic matrix and the supernatant, then wash the magnetic matrix repeatedly with water until it is neutral, and dry it at 110 °C for 12 h. The black solid magnetic matrix Fe can be obtained 3 o 4 .
[0026] Take 2 g of magnetic matrix Fe 3 o 4 Carry out mechanical mixing with 10 g charcoal sulfonic acid (prepared according to embodiment 1), add the water of 2.5 g again and stir, obtain the cylindrical magnetic charcoal sulfonic acid c...
Embodiment 3
[0029] Get 10 g of charcoal sulfonic acid prepared in Example 1, grind to an average particle size of 0.2 mm, use commercial microcrystalline cellulose as raw material (average particle size is 0.05 mm), the two are mechanically mixed, cellulose and carbon The mass ratio of sulfonic acid is 1:1, and then the mixed material is pyrolyzed at 340 °C under nitrogen atmosphere for 20 s, and the yield of liquid product is 52%. The yield of L-glucosone was 21.9%.
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