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

Inactive Publication Date: 2017-05-10
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most catalysts are not very selective for the formation of L-glucosone
Debele et al. reported in Application of catalysts forobtaining 1,6-anhydrosaccharides from cellulose and wood by fast pyrolysis that pyrolysis of cellulose was catalyzed by phosphoric acid on pyrolysis-chromatography / mass spectrometry (Py-GC / MS). LGO, up to 30% selectivity, impregnated with Fe 3+ It can increase the output of LG and LGO, but the process is more complicated and will bring certain environmental pollution problems; Lu et al. in "Catalytic fast pyrolysis of cellulose and biomass to produce levoglucosenone using magnetic SO 4 2- / TiO 2 -Fe 3 o 4 " and "Using solid superacid to catalyze the pyrolysis of cellulose to prepare L-glucosone" reported that the use of solid superacid, TiO 2 , ZrO 2 , SO 4 2- / ZrO 2 , SO 4 2- / TiO 2 and SO 4 2- / TiO 2 -Fe 3 o 4 The experimental study on the preparation of LGO by catalytic pyrolysis of cellulose on Py-GC / MS found that they all can promote the formation of LGO, among which SO 4 2- / TiO 2 Under catalysis, the selectivity of LGO reaches 60% at 350 °C, and the yield reaches the highest at 400 °C
However, the vast majority of current research is carried out on Py-GC / MS, and the biomass feed is basically less than 1 mg, and the pyrolysis characteristics obtained are comparable to those obtained in practice in commercial devices such as fixed-bed and fluidized-bed reactors. A big difference
In addition, these catalysts are all inorganic materials, the preparation process is complicated, the price is relatively expensive, and they need to be separated from the generated pyrolytic carbon.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention belongs to the field of biomass energy utilization and particularly relates to a preparation method of a pyrolytic carbon-modified catalyst, and a method for preparing levorodextrone by catalyzing pyrolytic cellulose by using the catalyst. The pyrolytic carbon-modified catalyst is a composite catalyst formed by activating activated carbon generated by pyrolyzation of the cellulose as a carrier by using a sulfuric acid; and the pyrolytic carbon-modified catalyst and the cellulose are quickly catalyzed and pyrolyzed at 300-400 DEG C in an oxygen-free environment in a fixed bed reactor to obtain a liquid product containing levorodextrone. Levorodextrone is high in yield and high in purity. In addition, the catalyst is cheap and easy to prepare, does not need to be separated from a pyrolytic residue of the cellulose, and can be further processed for further use.

Description

technical field [0001] The invention belongs to the field of utilization of biomass energy, and in particular relates to a self-pyrolysis carbon modification catalyst and a preparation method thereof, and a method for preparing levoglucosone by using the catalyst to catalyze pyrolysis of cellulose. Background technique [0002] Levoglucosone (LGO, 1,6-anhydro-3,4-dideoxy-β-D-pyranose-2-one) is an anhydrosugar product formed by pyrolysis of cellulose, and its structure was established in 1973 It is determined. Due to the enone system of 6,8-dioxobicyclo[3.2.1]octane, highly active ketone group and acetal center, L-glucosone can participate in a variety of synthetic reactions, such as the synthesis of various sugars and non- Chiral raw materials for carbohydrate 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 levoglucoso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/18C07H3/10C07H1/00
CPCB01J21/18C07H1/00C07H3/10
Inventor 张会岩肖睿祝敏敏孟鑫
Owner SOUTHEAST UNIV
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