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A method for preparing glycolic acid esters from carbohydrates

A carbohydrate and glycolic acid ester technology, applied in the preparation of organic compounds, chemical instruments and methods, and carboxylate preparation, etc., to achieve high-yield preparation, high selectivity, and convenient separation

Active Publication Date: 2018-01-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to the research results of the current literature, there is no report on the efficient and selective catalytic degradation of carbohydrates as raw materials to prepare glycolic acid esters.

Method used

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  • A method for preparing glycolic acid esters from carbohydrates
  • A method for preparing glycolic acid esters from carbohydrates
  • A method for preparing glycolic acid esters from carbohydrates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Cs 2.5 h 0.5 PW 12 o 40 Catalyst preparation

[0017] 2.5g CS 2 CO 3 and 18.12g of pretreated H 3 PW 12 o 40 6H20 formulated into 0.1mol L -1 and 0.08mol L -1 solution, 0.1mol.L -1 Cs 2 CO 3 Solution at 1mL·min -1 The rate is added dropwise to 0.08mol L at room temperature -1 h 3 PW 12 0 40 in solution. After the dropwise addition, continue to stir for 0.5h, then let it stand at room temperature for 20h. Then slowly evaporate the water at 323K to obtain a white solid, which is then dried at about 110°C and roasted at 300°C for 2 hours before use, with a specific surface area of ​​108m 2 g-1.

Embodiment 2

[0019] W 2 Preparation of C / AC: weigh 50g activated carbon (AC), 250mL 33wt% HNO 3 , placed in a 500mL three-neck flask, treated in a water bath at 80°C for 24h, washed until neutral, and dried at 120°C for 24h. Pour 1g of pretreated AC into an aqueous solution containing 0.588g of ammonium metatungstate, and after drying in an oven at 120°C, the catalyst precursor is subjected to temperature-programmed reduction in hydrogen. The specific reaction process is: from room temperature to 8.8°C The temperature was raised to 550 °C at a heating rate of 1 °C / min, and then to 900 °C at a heating rate of 1 °C / min and maintained for 1 h, with a hydrogen flow rate of 120 mL / min. The theoretical loading of W in the prepared catalyst is 30wt%.

Embodiment 3

[0021] W 2 Preparation of C / CMK-3: The preparation process was similar to Example 2, except that the AC carrier was replaced by CMK-3. The preparation process of CMK-3 is as follows: dissolve 1.25g sucrose in 5g deionized water, add 0.14g concentrated sulfuric acid, add 1g SBA-15 to the obtained mixed solution, soak at room temperature for 6h, and then dry at 100°C and 160°C for 6h respectively . The obtained beige powder was dipped again in a solution consisting of 0.8 g of sucrose, 0.09 g of concentrated sulfuric acid and 5 g of deionized water, and the drying step was repeated. Transfer to a tube furnace at a constant temperature of 900°C for 6 hours under a nitrogen atmosphere to completely carbonize the sucrose. Add 50ml of 4wt% hydrofluoric acid to the obtained black powder, stir at room temperature for 2h, filter / wash, repeat this process three times to completely remove silica, and finally dry overnight in an oven at 120°C to obtain ordered mesoporous carbon CMK -3....

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Abstract

The present invention provides a carbohydrate, including cellulose, starch, hemicellulose, sucrose, glucose, fructose, fructan, xylose, soluble xylooligosaccharides, and natural wood fiber raw materials containing the above carbohydrate components Glycolate method. The method uses carbohydrates or natural wood fiber raw materials containing carbohydrate components as reaction raw materials, and uses tungsten oxides, tungsten sulfides, tungsten chlorides, tungsten carbides, tungsten hydroxides, tungsten bronze, tungsten Acid, containing tungstate, metatungstic acid, metatungstate, paratungstic acid, paratungstate, peroxytungstic acid, peroxytungstate, containing tungstic heteropolyacid, containing tungsten heteropolyacid One or more than two are used as catalysts, and undergo a one-step catalytic conversion process in an alcohol solvent at 100-400°C to achieve high selectivity for carbohydrates and high yield for the preparation of glycolic acid esters. The reaction provided by the invention has the remarkable advantages that the raw materials are renewable resources and the atom economy is high.

Description

technical field [0001] The invention relates to a preparation method of glycolic acid ester, in particular to a method for preparing glycolic acid ester by one-step catalysis of carbohydrate in alcohol solution through a tungsten-containing catalyst. Background technique [0002] Glycolic acid esters are widely used in many fields such as chemical industry, medicine, pesticide, feed, spices and dyestuffs, and are important intermediates in organic synthesis and drug synthesis, as well as important chemical intermediates. As a chemical intermediate, glycolic acid ester has the following uses: hydrogenation reduction to produce ethylene glycol, hydrolysis to produce glycolic acid, which can be used to produce polyester fiber and used as a cleaning agent; carbonylation to produce malonate; aminolysis to produce glycine; oxidation Glyoxylate is dehydrogenated to produce glyoxylic acid, which can be used to produce vanillin, oral penicillin and allantoin, etc., thus forming a bra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/675C07C67/08B01J27/188B01J27/22
CPCB01J27/188B01J27/22C07C67/08C07C69/675
Inventor 王爱琴徐刚张涛郑明远庞纪峰王华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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