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Preparation method of methyl glucoside

A technology of methyl glucoside and methanol, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve problems such as yield not exceeding, and achieve high molar yield, abundant sources and simple process. Effect

Inactive Publication Date: 2010-03-03
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2001, Ishikawa (Ishikawa.Cellulose 2001, 8, (3), 189-195) reported that methanol can convert cellulose to methyl glucoside under supercritical conditions, but the yield did not exceed 35wt%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The catalytic reaction is carried out in a stainless steel autoclave (the volume of the reactor is 75ml), and 0.025g of concentrated sulfuric acid catalyst and 0.2g of cellulose are weighed in a polytetrafluoroethylene liner, and 20ml of methanol and a magneton are added. Put the liner into the stainless steel autoclave, use N 2 Exhaust the air in the kettle, repeat 3 times, and fill with 3MPa N 2 . The reaction temperature was 195° C., and the reaction time was 1 h. The product was analyzed by high performance liquid chromatography (HPLC) after centrifugal separation. The catalytic reaction results are listed in Table 1.

[0021] Table 1 Sulfuric acid catalytic conversion of cellulose to produce methyl glucoside

[0022] catalyst

Embodiment 2

[0024] The catalytic reaction is carried out in a stainless steel autoclave (the volume of the reactor is 75ml), and 0.05g of concentrated sulfuric acid catalyst and 0.2g of cellulose are weighed in a polytetrafluoroethylene liner, and 20ml of methanol and a magneton are added. Put the liner into the stainless steel autoclave, use N 2 Exhaust the air in the kettle, repeat 3 times, and fill with 3MPa N 2 . The reaction temperature was 195° C., and the reaction time was 1 h. The product was analyzed by high performance liquid chromatography (HPLC) after centrifugal separation. The catalytic reaction results are listed in Table 2.

[0025] Table 2 Sulfuric acid catalytic conversion of cellulose to produce methyl glucoside

[0026] catalyst

Embodiment 3

[0028] The catalytic reaction is carried out in a stainless steel autoclave (the volume of the reactor is 75ml), and 0.01g of concentrated sulfuric acid catalyst and 0.6g of cellulose are weighed in a polytetrafluoroethylene liner, and 30ml of methanol and a magneton are added. Put the liner into the stainless steel autoclave, use N 2 Exhaust the air in the kettle, repeat 3 times, and fill with 3MPa N 2 . The reaction temperature was 140° C., and the reaction time was 10 h. The product was analyzed by high performance liquid chromatography (HPLC) after centrifugal separation. The results of the catalytic reactions are listed in Table 3.

[0029] Table 3 Sulfuric acid catalytic conversion of cellulose to produce methyl glucoside

[0030] catalyst

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Abstract

A preparation method of methyl glucoside relates to preparation of methyl glucoside, in particular to a new way for directly preparing the methyl glucoside by taking cellulose as raw material, then combing the cellulose in a methanol medium, and then conducting catalyzed reaction between the cellulose and the methanol under the existence of an acid catalyst, and a related acid catalyst. The invention provides the preparation method of methyl glucoside, which has rich resource of adopted reactants, does not compete with grain such as starch, and has simple technological process and the highestmolar yield of the methyl glucoside of 65 percent. The cellulose, the methanol and the acid catalyst are mixed and added in a high pressure autoclave, then nitrogen is led in for evacuation, and afterreaction, cooling is conducted to obtain the methyl glucoside. The molar yield of the methyl glucoside is higher, which is 40 percent generally, and can reach 65 percent maximally.

Description

technical field [0001] The present invention relates to the preparation of methyl glucoside, especially relates to the new way of directly preparing methyl glucoside and related acid catalyst by using cellulose as raw material, then combining it in methanol medium, under the presence of acidic catalyst, catalyzing reaction of cellulose and methanol to directly prepare methyl glucoside . Background technique [0002] The methyl glucoside in the present invention refers to α- and β-methyl glucoside (MEG). Methyl glucoside is a non-reducing glucose derivative, a tetrahydric polyol with a unique ring structure, and has excellent chemical properties. It is mainly used in rigid polyurethane foam, melamine and phenolic resin, fabric finishing, Industries such as adhesives, cosmetics, coatings and surfactants. Used as the starting material in the synthesis of polyols such as polyether and polyester, it can improve the compatibility with the blowing agent, so that the compressive s...

Claims

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Application Information

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IPC IPC(8): C07H15/04C07H1/00B01J27/02B01J27/188B01J23/04B01J31/02
Inventor 张庆红邓卫平刘密王野
Owner XIAMEN UNIV
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