Method for preparing levorodextrone based on pyrolytic carbon-catalyzed cellulose
A technology of levoglucosone and pyrolysis carbon, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, dehydrated sugars, etc., can solve problems such as environmental pollution, complex preparation process, and complex process, and achieve easy separation and extraction, production The effect of high rate and easy preparation
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Embodiment 1
[0025] Self-pyrolysis carbon modified catalyst, the specific preparation steps are:
[0026] (1) Preparation of pyrolytic carbon:
[0027] With 6g of microcrystalline cellulose purchased from Sinopharm Group Chemical Reagent Co., Ltd., the particle size of 0.05-0.1mm was taken as raw material after sieving, and N 2 As a protective atmosphere, the fixed bed reactor was first heated to 350°C, and then the cellulose raw material was continuously and uniformly added to the reactor to realize rapid pyrolysis, and the cellulose carbon was collected, and the experiment was repeated many times to obtain a certain amount of activated carbon.
[0028] (2) Preparation of self-pyrolysis carbon modified catalyst:
[0029] Take by weighing about 10g of the cellulose charcoal powder prepared in step (1), 2 Under the protection of the atmosphere, put it into 100mL of concentrated sulfuric acid (98%) purchased from Sinopharm Chemical Reagent Co., Ltd. at 140°C for sulfonation for 12h, and af...
Embodiment 2
[0032] Adopt self-pyrolysis carbon modified catalyst prepared in Example 1, and grind to about 0.2-0.3mm particle diameter, get wherein 1g is put into fixed-bed reactor, adopt N 2 As a protective atmosphere, and N 2 The gas velocity is 150mL / min, and then the reactor is heated to 350°C at a heating rate of 23°C / min, and then 2 g of the above-mentioned cellulose is added to the fixed-bed reactor at a continuous and uniform rate to achieve rapid pyrolysis After the reaction, the pyrolytic carbon and the catalyst do not need to be separated. After collection, repeat the above step (2), and more self-pyrolytic carbon modified catalysts can be obtained. The yield of the liquid product is 68.6%. The content of levoglucosone was analyzed by chromatography, and the output of levoglucosone was calculated to be 4.9%.
Embodiment 3
[0034] Adopt self-pyrolysis carbon modified catalyst prepared in Example 1, and grind to about 0.2-0.3mm particle diameter, get wherein 1g is put into fixed-bed reactor, adopt N 2 As a protective atmosphere, and N 2 The gas velocity is 150mL / min, and then the reactor is heated to 400°C at a heating rate of 23°C / min, and then 2g of the above-mentioned cellulose is added to the fixed-bed reactor at a continuous and uniform rate to achieve rapid pyrolysis After the reaction, the pyrolytic carbon and the catalyst do not need to be separated. After collection, repeat the above step (2), and more self-pyrolytic carbon modified catalysts can be obtained. The yield of the liquid product is 67.0%. The content of levoglucosone was analyzed by chromatography, and the yield of levoglucosone was calculated to be 3.0%.
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