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Titanium-based magnetic solid super-acid catalyst and preparation thereof and method for preparing laevoglucose ketone by means of catalytic pyrolysis of cellulose or biomass

A technology of levoglucosone and solid superacid, applied in chemical instruments and methods, physical/chemical process catalysts, sugar derivatives, etc., can solve the difficulty of separation and purification of levoglucosone, the low level of levoglucosone, and the difficulty of catalyst recovery and other problems, to achieve the effect of easy separation and extraction, high yield and convenient recovery

Inactive Publication Date: 2012-03-21
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most catalysts are not very selective to L-glucosone, the pyrolysis products are still complex, and the separation and purification of L-glucosone is still difficult
Zhi Wang et al. reported in the Catalytic fast pyrolysis of cellulose to prepare levoglucosenone using sulfated zirconia literature that the conventional solid superacid was used to catalyze pyrolysis of cellulose, and a higher yield of levoglucosone was obtained, but the recovery of the catalyst in the process more difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] SO 4 2- / TiO 2 -Fe 3 o 4 Magnetic solid superacid catalyst, the specific preparation steps are:

[0029] (1) Preparation of magnetic matrix: Measure 30g of FeCl respectively 2 4H 2 O and 6g FeCl 3 ·6H 2 O was prepared into a 200mL mixed solution and added to a three-necked flask, placed in a constant temperature water bath at 65°C, and slowly dripped a NaOH solution with a concentration of 0.1mol / L while stirring until the pH value of the solution reached 12, and continued to stir at a constant temperature. Aging for 30min; then the three-neck flask was removed from the constant temperature water bath and cooled to room temperature, the magnetic matrix and the supernatant were separated by a magnetic field, and then the magnetic matrix was washed repeatedly until neutral, and then the magnetic matrix was repeatedly washed until neutral, at 110 After drying at ℃ for 12 hours, the black solid magnetic matrix Fe can be obtained 3 o 4 .

[0030] (2) Nano-SO 4 2...

Embodiment 2

[0034] Using the SO prepared in Implementation 1 4 2- / TiO 2 -Fe 3 o 4 Magnetic solid superacid catalyst, and ground to a particle diameter of about 0.5mm, with poplar as raw material (average particle diameter is 0.1mm), the two are mechanically mixed, the ratio of poplar and catalyst is 1:2, and then The mixed material was pyrolyzed at 330° C. for 30 seconds under a nitrogen atmosphere, and the yield of liquid product was 46%. The content of levoglucosone was analyzed by gas chromatography, and the yield of levoglucosone was calculated to be 7.8%.

Embodiment 3

[0036] SO 4 2- / TiO 2 -Fe 3 o 4 Magnetic solid superacid catalyst, the specific preparation steps are:

[0037] (1) Preparation of magnetic matrix: Measure 30g of FeCl respectively 2 4H 2 O and 6g FeCl 3 ·6H 2 O was prepared into a 200mL mixed solution and added to a three-necked flask, placed in a constant temperature water bath at 65°C, and slowly dripped a NaOH solution with a concentration of 0.1mol / L while stirring until the pH value of the solution reached 12, and continued to stir at a constant temperature. Aging for 60min; then the three-neck flask was removed from the constant temperature water bath and cooled to room temperature, the magnetic matrix and the supernatant were separated by a magnetic field, and then the magnetic matrix was washed repeatedly until neutral, and then the magnetic matrix was repeatedly washed until neutral, and then the magnetic matrix was washed repeatedly until neutral, at 105 After drying at ℃ for 15 hours, the black solid magnet...

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Abstract

The invention belongs to the field of utilization of biomass energy, and particularly relates to a titanium-based magnetic solid super-acid catalyst and a preparation method thereof and a method for preparing laevoglucose ketone by means of catalytic pyrolysis of cellulose or biomass through the catalyst. The titanium-based magnetic solid super-acid catalyst is a composite catalyst utilizing SO42- / TiO2 which is accelerated by sulfate radical as a catalytic active component and utilizing Fe3O4 as a magnetic matrix. The preparation method includes steps of mechanical mixing of cellulose or biomass, quick pyrolysis on anaerobic condition at the temperature of 280 DEG C to 450 DEG C and condensation of pyrolysis gas, and finally liquid product rich in laevoglucose ketone can be obtained. The laevoglucose ketone in the liquid product which is generated by utilizing the magnetic solid super acid catalyst to realize pyrolysis of cellulose or biomass is high in productivity and purity. In addition, the catalyst can be separated and recycled from solid residues by the aid of an external magnetic field directly.

Description

technical field [0001] The invention belongs to the field of utilization of biomass energy, and in particular relates to a titanium-based magnetic solid superacid catalyst and a preparation method thereof, and a method for preparing levoglucosone by using the catalyst to catalyze pyrolysis of cellulose or biomass. Background technique [0002] Levoglucosone (LGO, 1,6-anhydro-3,4-dideoxy-β-D-pyranosen-2-one) is one of the anhydrosugar products formed by pyrolysis of cellulose. As early as 1973, scientists discovered L-glucosone in the product of acid-catalyzed pyrolysis of cellulose and confirmed its chemical structure for the first time. After that, different research institutions at home and abroad have carried out more applied research on it. Since L-glucosone is very active, it can participate in various synthetic reactions, such as chiral raw materials for the synthesis of various sugars and non-sugar derivatives. Therefore, it can be used to synthesize various products...

Claims

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Application Information

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IPC IPC(8): B01J27/053C07H3/10C07H1/00
Inventor 陆强张旭明董长青杨勇平张俊姣
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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