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A kind of synthesis technique of ethyl maltol

A technology of ethyl maltol and ethyl, which is applied in the field of synthesis process of ethyl maltol, can solve the problems of catalyst loss, small preparation cost, cumbersome process, etc., and achieve less time-consuming reaction, easy process control, and stable combination Effect

Active Publication Date: 2022-04-01
广东省肇庆华格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the small particle size of the catalyst TS-1 and the high cost of preparation, the process of recovery and reuse through filtration, chloroform washing and drying is cumbersome, and the loss of the catalyst is inevitable.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Disperse 50 g of carbon nanotubes modified by oxygen plasma in 500 ml of ethanol solution under ultrasonic conditions, adjust the pH value of the mixed solution to 8, then add 20 ml of n-butyl titanate solution, heat to 120 ° C for water Heat reaction for 4h, filter, wash and dry to obtain TiO 2 Anatase nano-TiO supported by carbon nanotubes with a mass content of 4% 2 .

[0028] (2) get the anatase nano-TiO prepared by step (1) 2 / Carbon nanotubes 10g mixed with 0.2g polyethylene glycol aqueous solution evenly, then impregnated with 3mm porous glass bead carrier, taken out and sintered at 300°C for 0.5h to obtain nano TiO loaded on porous glass bead carrier 2 / carbon nanotube catalyst.

[0029] (3) Get the nano-TiO loaded on the porous glass bead carrier prepared by step (2) 2The carbon nanotube catalyst is filled on the multi-section bed in the fixed-bed photocatalytic reactor, 200mL acetonitrile is added in the reactor, and then 3g α-furan propanol is added ...

Embodiment 2

[0032] (1) Prepare TiO according to the step (1) of Example 1 2 Anatase nano-TiO supported by carbon nanotubes with a mass content of 10% 2 ;

[0033] (2) according to the step (2) of embodiment 1, prepare the nano-TiO loaded on the 20mm porous glass bead carrier 2 / Carbon nanotube catalyst

[0034] (3) Get the nano-TiO loaded on the porous glass bead carrier prepared by step (2) 2 / The carbon nanotube catalyst is filled on the multi-stage bed of the fixed bed photocatalytic reactor, 200mL of acetonitrile is added to the reactor, and then 3g of α-furan propanol is added under the condition of constant stirring, the temperature of the reactor is controlled at 50°C, and the Ultraviolet light source, control the output power to 200W, and pass 30% hydrogen peroxide into the mixed solution of α-furan propanol, control the molar ratio of hydrogen peroxide to α-furan propanol to be 2:1, under the irradiation of ultraviolet light with a wavelength of 254nm React for 4 hours to ge...

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Abstract

The invention belongs to the technical field of maltol, and in particular relates to a synthesis process of ethyl maltol. The process involves nano-TiO 2 / Carbon nanotubes are loaded on the porous glass bead carrier, then fill on the bed layer in the fixed-bed photocatalytic reactor, add acetonitrile solution in this reactor, then add α-furan propanol under constant stirring condition, control The temperature of the reactor is 20-50°C, turn on the ultraviolet light source, control the output power of 200W-500W, and pass 10-30% hydrogen peroxide into the mixed solution of α-furan propanol, and react under ultraviolet light for 0.5-4h, Generate 6-hydroxy-2-ethyl-2H-pyrone-[3] ​​intermediate product mixed solution, and then prepare ethyl maltol through acetalization, oxidation and hydrolysis. The process of the invention is environmentally friendly, easy to control, high in catalytic efficiency, less time-consuming in reaction, and the yield of intermediate products is as high as 94%.

Description

technical field [0001] The invention belongs to the technical field of maltol, and in particular relates to a synthesis process of ethyl maltol. Background technique [0002] Ethyl maltol, English name: ethylmaltol, chemical name: 2-ethyl-3-hydroxy-4H-pyrone (2-ethyl-3-hydroxy-4H-pyrone), molecular formula: C 7 h 8 0 3 , is a white acicular or white crystalline powder with a fragrant aroma. It is used more and more widely as a flavor improver and flavor enhancer. It is recognized as a safe, reliable, less dosage and effective food additive. Ethyl maltol is a derivative of γ-pyrone, which is white or slightly yellow crystal, and turns yellow when it meets alkali. Melting point 89-92℃, easily soluble in hot water, ethanol, chloroform and glycerin, with caramel and fruit flavor. [0003] The preparation methods of ethyl maltol mainly include fermentation method / kojic acid method, pyrofuric acid method, closed-loop method, furfuryl alcohol method, condensation method, furfu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D309/40B01J21/18B01J37/02B01J37/08
CPCC07D309/40B01J21/185B01J37/0201B01J37/08B01J35/39
Inventor 彭志强李俊召温细坤覃伟华
Owner 广东省肇庆华格生物科技有限公司
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