Method for catalyzing glucose by using magnetic solid acid to produce methyl glucoside

A technology of methyl glucoside and magnetic solid acid, applied in the field of chemical conversion of biomass, can solve the problems of strong corrosion, high pollution, high price, etc., and achieve the effects of less equipment corrosion, abundant sources and less environmental pollution

Inactive Publication Date: 2014-03-12
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the present invention is to provide a kind of method that catalyzes glucose to prepare methyl glucoside by simple, low pol...

Method used

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  • Method for catalyzing glucose by using magnetic solid acid to produce methyl glucoside
  • Method for catalyzing glucose by using magnetic solid acid to produce methyl glucoside
  • Method for catalyzing glucose by using magnetic solid acid to produce methyl glucoside

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preparation example Construction

[0015] Preparation of nano-magnetic solid acid SZT: refer to the literature Jun Wang, Piaoping Yang, Meiqing Fan, et al.Materials Letters, 2007, 61, 2235-2238. Prepared a magnetic solid superacid for the glucose glycoside involved in the present invention reaction.

[0016] The implementation process of producing methyl glucoside from glucose: use glucose as raw material, magnetic solid acid as catalyst, and react under subcritical methanol conditions at a temperature of 130-170°C for 1.5-7 hours to obtain methyl glucoside in high yield . After the reaction, the magnetic technology separates the nano-magnetic solid acid, and the methanol is removed by rotary evaporation to obtain methyl glucoside. The yield of the methyl glucoside obtained by the present invention is as high as 84.6%.

Embodiment 1

[0018] Take anhydrous glucose (0.6g), magnetic solid acid (0.3g) and methanol (12mL) in a 25mL hydrothermal kettle, stir magnetically, react at 140°C for 1.5 hours, and stop the reaction. Magnetic technology is used to separate nano-magnetic solid acid, and the reaction solution is concentrated using a rotary evaporator; the concentrated solution is subjected to column chromatography (silica gel is used as a filler, and the eluent is methanol to ethyl acetate at a ratio of 1:6), and methylglucose is separated to obtain Glycosides.

[0019] The nuclear magnetic spectrum data of product methyl glucoside is: 1 HNMR (D 2 O, 400Hz, TMS) δ (ppm): 3.39 (m, 1H), 3.43 (s, 1H), 3.57 (m, 1H), 3.65 (m, 1H), 3.68 (m, 1H), 3.77 (m, 1H), 3.88(m, 1H), 4.8(s, 1H). The infrared spectrum data is: IR(KBr, cm -1 ):-OH(3542,3296);-CH 3 (2913); -CH 2 -(1464); C-O-C(1145).

Embodiment 2～8

[0021] Other process conditions and reaction steps are the same as Example 1, but the temperature of magnetic solid acid activation is different (100~700 DEG C), react at 140 DEG C for 1.5 hours, stop reaction. Magnetic technology is used to separate nano-magnetic solid acid, and the reaction solution is concentrated using a rotary evaporator; the concentrated solution is subjected to column chromatography (silica gel is used as a filler, and the eluent is methanol to ethyl acetate at a ratio of 1:6), and methylglucose is separated to obtain Glycosides.

[0022]

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Abstract

The invention discloses a method for producing methyl glucoside by using reproducible raw material glucose. The method comprises the following step: by using glucose as a raw material and magnetic solid acid as a catalyst, reacting for 1.5-7 hours under the condition of subcritical methanol at the temperature of 100-170 DEG C to obtain methyl glucoside at the high yield rate. According to the method, the raw material of the catalyst is bulk commodity, nanometer magnetic solid superacid is prepared in a chemical coprecipitation method, so that nanometer magnetic solid superacid can be quickly separated from the product to be recycled; the obtained methyl glucoside is an important platform chemical compound and can be used as an intermediate or a monomer to be used in the fields of food, living beings, oil extraction and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical transformation of biomass, and relates to a method for catalyzing glucose to synthesize methyl glucoside in subcritical methanol with nano-metal magnetic solid acid. technical background [0002] Because solid acid has the advantages of good chemical and thermal stability, uniform distribution of active centers and easy access, super acidity, non-toxicity, easy recovery, and high catalytic activity at lower temperatures, it has been widely used. focus on. Many solid acid materials, such as metal oxides and their modified products, exhibit super acidic properties, especially the metal oxide ZrO with the acid center on its surface. 2 , is considered to be a green and versatile catalyst and catalyst carrier, and is widely used in many organic synthesis reactions in industry. Methyl glucoside is widely used in food additives, drilling fluids, initiators and resin regulators in the synthesis of poly...

Claims

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Application Information

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IPC IPC(8): C07H15/04C07H1/00
CPCY02P20/584
Inventor 李炜范乐明刘凯鸿夏咏梅方云
Owner JIANGNAN UNIV
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