Method for preparing laevoglucose ketone and special reaction equipment thereof
Inactive Publication Date: 2010-06-16
UNIV OF SCI & TECH OF CHINA
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The above phosphoric acid impregnation and drying process will greatly increase the production cost of levoglucosone, and the treatment of the impregnation solution will bring certain pollution
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[0013] The method for preparing L-glucosone provided by the present invention, the specific preparation process is as follows:
[0014] Crush the cellulose or biomass raw material to less than 1mm, send the material into the pyrolysis reactor 4 through the feeder 2, control the pyrolysis reaction temperature to 400-500°C, and the heating rate to 10 3 -10 5 ℃ / s, the residence time of the pyrolysis gas in the reactor 4 is not more than 1s; then the pyrolysis gas is quickly introduced into the fixed-bed catalytic reactor 7 equipped with a chromium chloride catalyst, and the reaction temperature is controlled at 250-400°C, and the mass air The speed is 10-1000h -1 ; Finally, the pyrolysis gas is rapidly condensed in the spray condenser 8 by means of spray condensation to obtain a liquid product, which is discharged from the discharge port.
[0015] The following determination methods are conventional methods unless otherwise specified.
Embodiment 1
[0017] Using microcrystalline cellulose as raw material, it is prepared in the fluidized bed biomass fast pyrolysis equipment with a processing capacity of 10kg / h shown in Fig. 1 . In this equipment, the inner diameter of the pyrolysis reactor is 70mm, and the bed height is 2m; the inner diameter of the fixed bed catalytic reactor is 70mm, and the bed thickness of chromium chloride is 2cm.
[0018] The cellulose was fed into the fluidized bed pyrolysis reactor through a two-stage screw feeder, nitrogen was used as the fluidized carrier gas, the pyrolysis reaction temperature was controlled at 420 °C, and the heating rate was 10 4 ℃ / s, after rapid pyrolysis of the raw material, the gas-solid separation is first realized by the cyclone separator, and then the pyrolysis gas enters the fixed-bed catalytic reactor, the catalytic reaction temperature is 380°C, and finally the pyrolysis gas is rapidly condensed to obtain A mixture of water and organic matter. Experiment is carried o...
Embodiment 2
[0020] In the same reaction conditions and reaction environment as in Example 1, only the pyrolysis reaction temperature was changed to 460°C, the experiment was carried out according to the method of Example 1 for 6 minutes, the amount of cellulose was 1 kg, and the collected organic product was 0.22 kg, the calculated organic liquid yield is 46% (percentage by weight), the organic product is analyzed by GC / MS, and the content of L-glucosone determined by GC is 48% (percentage by weight).
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Abstract
The invention discloses a method for preparing laevoglucose ketone and special reaction equipment thereof. The reaction equipment comprises a fluidized bed pyrolysis reactor(4), wherein an opening on the bottom part of the side wall of the fluidized bed pyrolysis reactor(4) is connected with a feeder(2) by a tube, an opening at the top end of the reactor(4) is connected with a separator(6) by a tube, an opening at the top end of the separator(6) is connected with an opening at the top end of a catalytic reactor(7) by a tube, an opening on the bottom part of the catalytic reactor(7) is connected with a condenser(8) by a tube, and the bottom part of the condenser is provided with a liquid outlet. The preparation method comprises the following steps of: in the reaction equipment, feeding cellulose or biomass materials to the pyrolysis reactor for pyrolysis, performing gas-solid separation by the separator, performing a catalytic cracking reaction of the pyrolyzed gas generated in the pyrolysis reaction in a reactor filled with a catalyst of chromic chloride, and after reaction, condensing the gas by the condenser to obtain the finished product. Because the celluloses or biomass are used as raw materials and the yields of the organic liquid products all reach over 15 percent, wherein the laevoglucose ketone content reaches over 30 percent.
Description
technical field [0001] The invention belongs to the field of utilization of biomass energy, and relates to a method for preparing L-glucosone and special reaction equipment thereof. Background technique [0002] As a cellulose-derived α, β-unsaturated cyclic ketone, L-glucosone can be used as a chiral raw material for the synthesis of sugar and non-sugar derivatives. In addition, L-glucosone can also be used in the synthesis of various drugs for the treatment of cancer, immune diseases and heart diseases. At present, there is no large-scale production of levoglucosone. [0003] Cellulose will depolymerize under the condition of rapid heating at medium temperature to form a large number of anhydrosugar products, mainly levoglucosan. Under the action of a suitable catalyst, levoglucosan will undergo dehydration reaction to form levoglucosone. Debele et al reported in the literature of Pretreatment of biomass with phosphoric acid prior to fastpyrolysis-A promising method for...
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