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Method for preparing levoglucosenone with magnetic solid phosphoric acid catalyst

A technology of levoglucosone and phosphoric acid catalysts, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as inability to separate and recover, environmental pollution, and complicated pretreatment process, so as to avoid environmental pollution, The effect of high yield and simplified raw material pretreatment process

Active Publication Date: 2012-06-27
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest problem with this method is that the pretreatment process of raw materials is relatively complicated, and many factors must be strictly controlled in the impregnation process to obtain raw materials with suitable phosphoric acid loading, and the use of liquid acid may also cause certain environmental pollution.
In addition, during the pyrolysis process of phosphoric acid, a series of reactions will occur. After pyrolysis, it cannot be separated and recovered.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Preparation of magnetic matrix:

[0026] 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 .

[0027] (2) Preparation of solid phosphoric acid:

[0028] Take diatomaceous earth as a carrier, measure 50g of diatomite, pu...

Embodiment 2

[0033] Adopt the magnetic solid phosphoric acid catalyst 10g that prepares in implementing 1, and grind to particle diameter about 0.5mm, take poplar as raw material (average particle diameter is 0.1mm), the two are mechanically mixed, the ratio of poplar and catalyzer 1: 2, then the mixed material is pyrolyzed for 25s at 330° C. under a nitrogen atmosphere, and the yield of the liquid product obtained is 46%, and the content of levoglucosone is analyzed by gas chromatography, and the output of levoglucosone is calculated as 7.4%.

Embodiment 3

[0035] (1) Preparation of magnetic matrix:

[0036] 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 magnetic matrix Fe can be obtained 3 o 4 .

[0037] (2) Preparation of solid phosphoric acid:

[0038] ...

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Abstract

Belonging to the utilization field of biomass energies, the invention specifically relates to a method for preparing levoglucosenone by utilizing a magnetic solid phosphoric acid catalyst for catalytic pyrolysis of cellulose / biomasses. The method comprises: taking magnetic solid phosphoric acid as the catalyst, which is then mechanically mixed with cellulose / biomasses, then conducting rapid pyrolysis under an anaerobic condition at a temperature of 280-450DEG C, and carrying out condensation on pyrolysis gas, thus obtaining a liquid product rich in levoglucosenone. In the liquid product of magnetic solid phosphoric acid catalyzed pyrolysis of cellulose, the yield and purity of levoglucosenone are both high. In addition, being stable in performance, the catalyst can be separated and recovered from solid residue by directly utilizing an external magnetic field and can be recycled repeatedly.

Description

technical field [0001] The invention belongs to the field of utilization of biomass energy, and in particular relates to a method for preparing L-glucosone by using a magnetic solid phosphoric acid catalyst to catalyze pyrolysis of cellulose / biomass. Background technique [0002] Levoglucosone (LGO, 1,6-anhydro-3,4-dideoxy-β-D-pyranose-2-one) is one of the many anhydrosugar products formed by pyrolysis of cellulose. Due to its high reactivity, it can be widely used in various synthetic reactions, so it has extremely high added value in chemical industry or medicine. However, the liquid products formed by conventional pyrolysis of cellulose or biomass have extremely complex compositions, and the content of LGO is extremely low, which makes it difficult to separate LGO from conventional pyrolysis liquid products. In order to obtain LGO, appropriate means must be introduced to control the pyrolysis reaction process in a directional way to achieve selective pyrolysis to obtain ...

Claims

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Application Information

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IPC IPC(8): C07H3/10C07H1/00B01J27/185B01J29/035
Inventor 陆强田慧云董长青杨勇平
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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