A kind of preparation method of L-glucosone

A technology of L-glucosone and cellulose, which is applied in the field of preparation of high-yield L-glucosone, can solve the problems of waste of concentrated sulfuric acid, unfavorable environmental protection, pollution, etc., achieves significant economic and social benefits, is beneficial to environmental protection, and has large applications. Foreground effect

Inactive Publication Date: 2019-10-29
HENAN UNIV OF URBAN CONSTR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using charcoal sulfonic acid or magnetic charcoal sulfonic acid as a catalyst can obtain about 20% LGO yield, but the preparation of charcoal sulfonic acid or magnetic charcoal sulfonic acid requires a large amount of concentrated sulfuric acid, resulting in waste of concentrated sulfuric acid and environmental pollution, which is not conducive to Environmental friendly

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  • A kind of preparation method of L-glucosone
  • A kind of preparation method of L-glucosone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation method of L-glucosone of the present invention, the detailed steps of this preparation method are as follows:

[0031] a. First, dissolve phosphoric acid in water to form 100mL of 2.0mol / L phosphoric acid solution, then add 10g of microcrystalline cellulose to the obtained phosphoric acid solution, mix thoroughly after adding, and soak for 10min;

[0032] b. Filter the material after soaking (by filtering to remove most of the liquid absorbed in the microcrystalline cellulose after soaking), and then put the obtained filter cake in a pyrolysis furnace under vacuum (5mmHg) and 200°C. Pyrolysis pretreatment for 10 minutes to obtain a dehydrated intermediate product;

[0033] c. Cool the obtained dehydrated intermediate product to room temperature, place it in 100 mL, 0.05 mol / L sodium hydroxide aqueous solution after cooling, mix well, and soak for 10 min;

[0034] d. Filter the product obtained in step c (remove most of the liquid adsorbed in the product...

Embodiment 2

[0038] The preparation method of L-glucosone of the present invention, the detailed steps of this preparation method are as follows:

[0039] a. First, dissolve phosphoric acid in water to form 100 mL of 1.5 mol / L phosphoric acid solution, then add 10 g of microcrystalline cellulose to the obtained phosphoric acid solution, mix thoroughly after adding, and soak for 20 minutes;

[0040] b. Filter the material after soaking (by filtering to remove most of the liquid absorbed in the microcrystalline cellulose after soaking), and then put the obtained filter cake in a pyrolysis furnace under vacuum (5mmHg) and 150°C. Pyrolysis pretreatment for 30 minutes to obtain the dehydrated intermediate product;

[0041] c. Cool the obtained dehydrated intermediate product to room temperature, place it in 100 mL, 0.03 mol / L sodium hydroxide aqueous solution and mix thoroughly after cooling, and soak for 20 min;

[0042] d. Filter the product obtained in step c (remove most of the liquid adso...

Embodiment 3

[0045] The preparation method of L-glucosone of the present invention, the detailed steps of this preparation method are as follows:

[0046] a. First, dissolve phosphoric acid in water to form 100mL of 2.2mol / L phosphoric acid solution, then add 10g of microcrystalline cellulose to the obtained phosphoric acid solution, mix thoroughly after adding, and soak for 10min;

[0047] b. Filter the material after soaking (by filtering to remove most of the liquid absorbed in the microcrystalline cellulose after soaking), and then put the obtained filter cake in a pyrolysis furnace, in a vacuum (vacuum degree of 5mmHg), 220 ℃ Perform pyrolysis pretreatment for 10 minutes under the same conditions to obtain a dehydrated intermediate product;

[0048] c. Cool the obtained dehydrated intermediate product to room temperature, place it in 100mL, 0.08mol / L sodium hydroxide aqueous solution and mix thoroughly after cooling, and soak for 10min;

[0049] d. Filter the product obtained in step...

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Abstract

The invention discloses a preparation method of levoglucosenone. The preparation method comprises the following steps of firstly, dissolving phosphoric acid in water to form a phosphoric acid solution; adding cellulose or cellulose-contained biomass, mixing and soaking; filtering the soaked cellulose or cellulose-contained biomass, pressing and extruding or centrifuging, and performing pyrolysis pretreatment on the treated matter, so as to obtain a dewatered intermediate product; cooling the obtained dewatered intermediate product to room temperature, cooling, putting into a sodium hydroxide or potassium hydroxide water solution, and fully mixing and soaking; filtering the mixed and soaked product, pressing and extruding or centrifuging, performing non-oxygen pyrolysis on the treated product, and collecting condensate in the pyrolysis process, so as to obtain a pyrolysate containing the levoglucosenone. The preparation method of the levoglucosenone has the advantages that by adopting two-step reaction, the yield rate is greatly increased and reaches about 40%; compared with the prior art, the cost is greatly reduced; by adopting the technical scheme, the large application prospect is realized.

Description

technical field [0001] The invention belongs to the technical field of utilization of biomass energy, and in particular relates to a preparation method of high-yield L-glucosone. Background technique [0002] Levoglucosone (LGO, 1,6-anhydro-3,4-dideoxy-β-D-pyranose-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. At present, no suitable method has been found to produce LGO on a large scale, making it extremely expensive. [0003] In the pyrolysis of cellulose, if there is an acidic catalyst, a high-value compound can be obtained: Levoglucosenone (LGO). L-glucosone is an important chiral synthon and a new platform for the development and utilization ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H1/00C07H3/10
CPCC07B2200/07C07H1/00C07H3/10
Inventor 杨治广刘雪平刘小珍宋丰明郭一飞康海彦张岩
Owner HENAN UNIV OF URBAN CONSTR
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