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Method for preparing levoglucose ketone through catalyzing and pyrolyzing cellulose by utilizing solid phosphoric acid

A technology catalyzed by levoglucosone and phosphoric acid, applied in chemical instruments and methods, preparation of sugar derivatives, dehydrated sugars, etc., can solve the problems of inability to separate and recover phosphoric acid, environmental pollution, etc., simplify the pretreatment process of raw materials, and avoid environmental pollution , highly selective effect

Inactive Publication Date: 2012-07-04
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the impregnation process, factors such as the concentration of phosphoric acid solution, the material ratio of cellulose and phosphoric acid solution, and the impregnation time must be strictly controlled to obtain a suitable impregnation amount of phosphoric acid; in addition, certain environmental pollution may be caused during the impregnation process
In addition, phosphoric acid-loaded cellulose raw materials cannot be separated and recovered after pyrolysis.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Preparation of solid phosphoric acid catalyst: use diatomaceous earth as a carrier, measure 50g of diatomite, place it in 200mL of orthophosphoric acid solution with a concentration of 80%, soak it for 12h under stirring, then filter it, place it in a normal blast Dry at 140°C for 10 hours in a drying oven, and bake at 500°C in a muffle furnace (programmed temperature increase rate is 3°C / min, holding time is 3 hours), and 60g of solid phosphoric acid is obtained.

[0020] Take 5g of the above-mentioned solid phosphoric acid catalyst and grind it until the particle size is about 0.5mm, use commercial microcrystalline cellulose as raw material (average particle size is 0.05mm), and mix the two mechanically, the ratio of cellulose and catalyst is 1:1 , and then the mixed material was pyrolyzed at 340° C. under a nitrogen atmosphere for 15 s to obtain a liquid product with a yield of 53%. The content of levoglucosone was analyzed by gas chromatography, and the yield of levo...

Embodiment 2

[0022] Adopt the solid phosphoric acid catalyst 10g that prepares in implementing 1, and grind to particle diameter about 0.5mm, take absorbent cotton as raw material (average particle diameter is 0.05mm), the two are mechanically mixed, the ratio of cellulose and catalyst is 1 : 2, then the mixed material is pyrolyzed for 20s at 320° C. under a nitrogen atmosphere, and the yield of liquid product obtained is 49%, and the content of levoglucosone is analyzed by gas chromatography, and the output of levoglucosone is calculated to be 20.2%. .

Embodiment 3

[0024] Preparation of solid phosphoric acid catalyst: Take SBA-15 as the carrier, measure 20g of SBA-15, put it in 200mL of 70% orthophosphoric acid solution, soak it for 12h under stirring, then filter it, put it in a normal blast Dry in a drying oven at 160°C for 8 hours, and bake in a muffle furnace at 500°C (programmed temperature increase rate is 3°C / min, holding time is 3h), and 28g of solid phosphoric acid is obtained.

[0025] Get 1.7g of the above-mentioned solid phosphoric acid catalyst and grind it to a particle size of about 0.5mm, use commercial microcrystalline cellulose as a raw material (average particle size is 0.05mm), and mix the two mechanically, the ratio of cellulose and catalyst is 3: 1. Then the mixed material was pyrolyzed at 350°C under nitrogen atmosphere for 15s, and the yield of liquid product was 55%. The content of levoglucosone was analyzed by gas chromatography, and the yield of levoglucosone was calculated to be 20.6%.

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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 method for preparing levoglucose ketone through catalyzing and pyrolyzing cellulose by utilizing solid phosphoric acid. The method comprises the steps of taking the solid phosphoric acid as catalyst, mechanically mixing with the cellulose, carrying out fast pyrolysis at a temperature of 280-450 DEG C under an oxygen-free condition, condensing the pyrolysis gas and obtaining a liquid product rich in the levoglucose ketone. In the liquid product obtained through catalyzing and pyrolyzing the cellulose by utilizing the solid phosphoric acid, the yield and the purity of the levoglucose ketone are both high; in addition, the solid phosphoric acid catalyst is stable in performance and can be repeatedly and cyclically utilized.

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 solid phosphoric acid catalyst to catalyze pyrolysis of cellulose. Background technique [0002] Levoglucosone (LGO, 1,6-anhydro-3,4-dideoxy-β-D-pyranosen-2-one) is a dehydrated sugar product formed by pyrolysis of cellulose, due to its 6,8 - Dioxobicyclo[3.2.1]octane enone system, highly active ketone group and acetal center, LGO can be widely used in a variety of synthetic reactions for the preparation of various sugar and non-sugar derivatives , as well as drugs to treat cancer, immune diseases and heart disease, among others. A suitable method for producing LGO on a large scale has not yet been found, making it extremely expensive. [0003] In the liquid products of conventional pyrolysis of cellulose, the yield of LGO is extremely low, generally difficult to exceed 1%. Moreover, the separation and recove...

Claims

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Application Information

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