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Preparation method of furanone

A technology for furanone and glyoxal, which is applied to the preparation field of furanone, can solve problems such as low purity and low total yield of furanone, and achieve the effects of improving purity, improving total yield and improving extraction efficiency.

Active Publication Date: 2019-10-25
安徽金轩科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problem of low total yield and low purity of the intermediate product 3,4-dihydroxy-2,5-hexanedione intermediate product and furanone in the preparation of furanone by the existing acetone aldehyde method , a preparation method of furanone with high yield and purity is now provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Preparation of methylglyoxal solution: Add 4g of silver catalyst into the oxidizer, then add 1,2-propanediol into the oxidizer, pass in air, heat to 370°C, carry out catalytic oxidation reaction to generate methylglyoxal, and then Absorbed in water to obtain a solution of methylglyoxal with a mass concentration of 25%, for subsequent use.

[0027] (2) Preparation of 3,4-dihydroxy-2,5-hexanedione solution: Add 50mL pure water, 15g Sodium acetate and 1g of tetrabutylammonium iodide were stirred and dissolved, then 3g of zinc powder, 3g of iron powder and 2g of manganese powder were added, and 40mL of aceglyoxal aqueous solution with a mass concentration of 25% and 15mL of dilute sulfuric acid with a concentration of 50% were added dropwise. Control the temperature at 20°C, then add 3g of zinc powder, 3g of iron powder and 2g of manganese powder, and then dropwise add 40mL of 25% aqueous solution of methylglyoxal and 15mL of 50% dilute sulfuric acid, and then raise the...

Embodiment 2

[0032](1) Preparation of methylglyoxal solution: Add 3g of silver catalyst into the oxidizer, then add 1,2-propanediol into the oxidizer, pass in air, heat to 360°C, carry out catalytic oxidation reaction to generate methylglyoxal, and then Absorbed in water to obtain a solution of methylglyoxal with a mass concentration of 25%, for subsequent use.

[0033] (2) Preparation of 3,4-dihydroxy-2,5-hexanedione solution: Add 50mL pure water, 15g Potassium acetate and 1g of tetrabutylammonium iodide are stirred and dissolved, then 4g of zinc powder, 2g of iron powder and 3g of manganese powder are added, and 40mL of aceglyoxal aqueous solution with a mass concentration of 25% and 15mL of dilute sulfuric acid with a concentration of 50% are added dropwise. Control the temperature at 20°C, then add 4g of zinc powder, 2g of iron powder and 3g of manganese powder, and then dropwise add 40mL of 25% aqueous solution of aceglyoxal and 15mL of 50% dilute sulfuric acid, and then raise the tem...

Embodiment 3

[0038] (1) Preparation of methylglyoxal solution: Add 5g of silver catalyst into the oxidizer, then add 1,2-propanediol into the oxidizer, pass in air, heat to 380°C, carry out catalytic oxidation reaction to generate methylglyoxal, and then Absorbed in water to obtain a solution of methylglyoxal with a mass concentration of 25%, for subsequent use.

[0039] (2) Preparation of 3,4-dihydroxy-2,5-hexanedione solution: Add 50mL pure water, 15g Calcium acetate and 1g of tetrabutylammonium iodide are stirred and dissolved, then 5g of zinc powder, 2g of iron powder and 1g of manganese powder are added, and 40mL of aceglyoxal aqueous solution with a mass concentration of 25% and 15mL of dilute sulfuric acid with a concentration of 50% are added dropwise. Control the temperature at 20°C, then add 5g of zinc powder, 2g of iron powder and 1g of manganese powder, and then dropwise add 40mL of 25% aqueous solution of aceglyoxal and 15mL of 50% dilute sulfuric acid, and then raise the temp...

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PUM

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Abstract

The invention discloses a preparation method of furanone. The preparation method includes the steps that an acetone aldehyde solution is prepared, a 3,4-dihydroxy-2,5-hexanedione solution is prepared,3,4-dihydroxy-2,5-hexanedione is purified, semi-finished furanone is prepared, and finished furanone is prepared. The preparation method has the advantages that 1, the yield of the intermediate 3,4-dihydroxy-2,5-hexanedione and the total yield of the furanone can be increased through composite catalyst zinc powder, iron powder and manganese powder, 2, purity of the intermediate 3,4-dihydroxy-2,5-hexanedione is obviously increased by adding anhydrous sodium sulphate and sodium chloride composite powder, and 3, purity of the furanone can be obviously improved by combining extractant ethanol andethyl acetate.

Description

technical field [0001] The invention belongs to the technical field of chemical production and relates to a preparation method of furanone. Background technique [0002] Furanone natural products exist in strawberry, oats, cheese, boiled beef, beer, cocoa, coffee, tea, mango, lychee, malt, gooseberry, grape, heated beef, pineapple, etc., in 1965, in the ether extraction of pineapple juice For the first time, furanone was isolated from the solution, and its molecular structure was determined. The furanone synthesized by it has simple process, low cost and pure aroma. At present, in the actual production process, it is more common to use aceglyoxal and zinc powder to react and couple to obtain 3 , 4-dihydroxy-2, 5-hexanedione, and then to obtain furanone through cyclization. [0003] The aceglyoxal process generally has problems such as difficult reaction control, high safety hazards due to the generation of hydrogen, low yield, and serious pollution of three wastes (mainly ...

Claims

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Application Information

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IPC IPC(8): C07D307/60
CPCC07D307/60
Inventor 孙多龙程光锦姜维强沙里峰万顺张浩
Owner 安徽金轩科技有限公司
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