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Catalyst for producing levoglucosenone, and preparation method thereof

A technology of L-glucosone and catalyst, which is applied in the preparation of sugar derivatives, chemical instruments and methods, catalysts for physical/chemical processes, etc., can solve the problems of increased preparation cost, high price of ionic liquid catalysts, impossible recycling, etc. Good catalytic effect, promoting activity and improving selectivity

Active Publication Date: 2019-04-30
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, H 3 PO 4 and H 2 SO 4 Thermal condensation reactions occur during pyrolysis, making recycling impossible
The ionic liquid catalyst is expensive, which increases the preparation cost to a certain extent

Method used

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  • Catalyst for producing levoglucosenone, and preparation method thereof
  • Catalyst for producing levoglucosenone, and preparation method thereof
  • Catalyst for producing levoglucosenone, and preparation method thereof

Examples

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Comparison scheme
Effect test

preparation example Construction

[0037] figure 1 It is a flow chart of the catalyst preparation method for producing levoglucosone according to the embodiment of the present invention. like figure 1 Shown, the present invention provides a kind of catalyst preparation method for producing L-glucosone, comprises the steps:

[0038] S1: The biomass raw material is pulverized and fully mixed with KOH activator at a mass ratio of 4:1 to 1:4, then placed in a reactor, pyrolyzed under the protection of nitrogen, and reacted to obtain biochar, which is pyrolyzed from biomass raw material The temperature is 300°C-600°C, and the pyrolysis time of biomass raw materials is 20min-60min;

[0039]S2: After mixing biochar and concentrated sulfuric acid in S1 at a mass ratio of 1:8 to 1:90, sulfonate in a hydrothermal kettle at 100°C to 180°C for 3h to 15h, and rinse with deionized water to medium after cooling. After curing, use a drying box to dry at 65°C to 120°C for 6h to 12h to obtain sulfonated carbon; the concentrat...

Embodiment 1

[0047] A method for preparing a catalyst for the production of glucosone, comprising the steps of:

[0048] S1: Crush the coconut shell to less than 120 mesh, take 2g sample and mix it with 1g KOH activator, send it into the electric heating reactor, the pyrolysis temperature is 600°C, the pyrolysis time is 30min, and N 2 As shielding gas, N 2 The flow rate is 200ml / min, and the biochar is obtained by cooling. And repeat the experiment to get enough biochar.

[0049] S2: Mix 6g of biochar with concentrated sulfuric acid (98wt%) at a mass ratio of 1:90, sulfonate in a hydrothermal kettle at a constant temperature of 150°C for 12h under a nitrogen atmosphere, cool and filter, and rinse with deionized water to medium properties, placed in a drying oven at 105°C for 6 hours to obtain sulfonated carbon.

[0050] S3: Take 0.5g sulfonated carbon, press Cu 2+ A certain amount of Cu(NO 3 ) 2 ·3H 2 O, configure 10mlCu(NO 3 ) 2 · 3 h 2 O solution.

[0051] S4: Soak sulfonated...

Embodiment 2

[0055] S1: Get 0.5g sulfonated carbon prepared in Example 1, press Ca 2+ A certain amount of Ca(NO 3 ) 2 , configure 10mlCa(NO 3 ) 2 solution.

[0056] S2: Soak sulfonated carbon in the solution for 30min, filter to get Ca 2+ Supported metal sulfonated carbon catalysts.

[0057] S3: Rinse with deionized water, and dry in a drying oven at 105°C for 6 hours.

[0058] Further, the method for preparing levoglucosone using a metal sulfonated carbon catalyst comprises the following steps: taking 0.3 mg of the above-mentioned Ca 2+ Loaded metal sulfonated carbon catalyst, using glucopyranose as raw material, mechanically mixing the two, the mass ratio of glucopyranose and catalyst is 1:1, and the mixture is subjected to rapid pyrolysis reaction in PY-GC / MS, 400 ℃ under the atmosphere of helium pyrolysis for 10ms. The content of glucosone was analyzed by gas chromatography-mass spectrometry. Figure 4 As shown, the calculated content of L-glucosone is 53.5%.

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Abstract

The invention discloses a preparation method of a catalyst for producing levoglucosenone. The preparation method comprises the following steps: S1, crushing a biomass raw material, fully mixing the crushed biomass raw material with a KOH activator according to a mass ratio of 4:1 to 1:4, adding the obtained mixture into a reactor, and carrying out a pyrolysis reaction under the protection of nitrogen to obtain biochar; S2, mixing the biochar obtained in S1 with concentrated sulfuric acid, sulfonating the biochar in a hydrothermal kettle, cooling the hydrothermal kettle, washing the obtained reaction product with deionized water to be neutral, and drying the washed reaction product in a drying oven to obtain sulfonated carbon; and S3, impregnating the sulfonated carbon to load metal ions, and performing washing and drying to obtain the metal sulfonated carbon catalyst. The invention also discloses the catalyst for producing levoglucosenone. The catalyst loaded with metal ions can effectively promote the conversion of the biomass raw material to a dehydration intermediate in the pyrolysis process, and also enhances the activity of strong acidic sites of the sulfonated carbon in orderto dehydrate the intermediate into the levoglucosenone.

Description

technical field [0001] The invention belongs to the technical field of biomass energy utilization, and more specifically relates to a catalyst and a preparation method for producing L-glucosone. Background technique [0002] With the development of the world's industrialization process, the consumption of fossil energy has brought enormous pressure to the environment and caused a certain degree of pollution. In order to protect the natural environment on which human beings live and realize the sustainable use of energy, countries all over the world are actively developing various green, efficient and clean energy sources to replace traditional fossil energy sources. The use of biomass energy can effectively reduce the consumption of fossil energy. Biomass pyrolysis, which can convert solid biomass into bio-oil, is one of the most promising technologies for biomass utilization. Bio-oils contain many high-value oxygenated chemicals, a property that allows the production of a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/02B01J35/10C07H1/00C07H3/10
CPCC07H1/00C07H3/10B01J27/02B01J35/61
Inventor 杨海平徐坤方阳陈应泉陈伟邵敬爱杨晴曾阔王贤华张世红陈汉平
Owner HUAZHONG UNIV OF SCI & TECH
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