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Synthetic method of 2,3-pentanedione

A synthesis method and pentanedione technology are applied in chemical instruments and methods, condensation preparation of carbonyl compounds, organic chemistry, etc., and can solve the problems of complicated catalyst preparation, difficult operation control, industrial application limitations, etc., and achieve high selectivity and Conversion rate, simple production operation, yield reduction effect

Pending Publication Date: 2018-10-16
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthesis method of 2,3-pentanedione reported in the above documents and patents has the disadvantages of cumbersome catalyst preparation, difficult operation control, and low reaction yield, and its industrial application is limited.

Method used

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  • Synthetic method of 2,3-pentanedione

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Preparation of solid base

[0023] Weigh 2.9g KF, add it to the beaker, add 20ml water, stir, then weigh 6.2g Al 2 o 3 Added to the above solution (KF and Al 2 o 3 The molar ratio is 1:1.2), heated to 60°C and stirred for 1 hour to obtain a mixture, and put the obtained mixture into a vacuum drying oven at 50-60°C for 12 hours to obtain an unactivated solid superbase catalyst. The above-mentioned solid is activated for 4 hours at 350-550° C. under a nitrogen atmosphere to obtain an activated solid superbase catalyst.

[0024] (2) Catalytic synthesis of 2,3-pentanedione

[0025] Mix 75g of lactic acid solution (90% content) with 5g of the above-prepared solid base catalyst, and slowly heat the reaction mixture. When the reaction temperature reaches 200°C, the lactic acid undergoes condensation dehydration and decarboxylation to generate 2,3-pentanedione. At the same time, the generated 2,3-pentanedione and water are vaporized from the reaction mixture system, an...

Embodiment 2

[0027] (1) Preparation of solid base

[0028] Weigh 2.9g KF, add it into the beaker, add 20ml water, stir, then weigh 10.2gAl 2 o 3 Added to the above solution (KF and Al 2 o 3 The molar ratio is 1:2), heated to 60°C and stirred for 2h to obtain a mixture, and put the obtained mixture into a vacuum drying oven at 50-60°C for 12h to obtain an unactivated solid superbase catalyst. The above-mentioned solid is activated for 5 hours at 350-550° C. under a nitrogen atmosphere to obtain an activated solid superbase catalyst.

[0029] (2) Catalytic synthesis of 2,3-pentanedione

[0030] Mix 75g of lactic acid solution (90% content) with 5g of the above-prepared solid base catalyst, and slowly heat the reaction mixture. When the reaction temperature reaches 200°C, the lactic acid undergoes condensation dehydration and decarboxylation to generate 2,3-pentanedione. At the same time, the generated 2,3-pentanedione and water are vaporized from the reaction mixture system, and after b...

Embodiment 3

[0032] (1) Preparation of solid base

[0033] Weigh 6.9gK 2 CO 3 , into the beaker, add 20ml of water, stir, and weigh 6.2g of Al 2 o 3 Added to the above solution (K 2 CO 3 and Al 2 o 3 The molar ratio is 1:1.2), heated to 60°C and stirred for 1.5h to obtain a mixture, and put the obtained mixture into a vacuum drying oven at 50-60°C for 12h to obtain an unactivated solid superbase catalyst. The above-mentioned solid is activated for 4.5 hours at 350-550° C. under a nitrogen atmosphere to obtain an activated solid superbase catalyst.

[0034] (2) Catalytic synthesis of 2,3-pentanedione

[0035] Mix 75g of lactic acid solution (90% content) with 5g of the above-prepared solid base catalyst, and slowly heat the reaction mixture. When the reaction temperature reaches 200°C, the lactic acid undergoes condensation dehydration and decarboxylation to generate 2,3-pentanedione. At the same time, the generated 2,3-pentanedione and water are vaporized from the reaction mixture s...

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Abstract

The invention relates to a synthetic method of 2,3-pentanedione. The synthetic method of the 2,3-pentanedione comprises the following steps: mixing a lactic acid solution with a solid alkali catalystM / N and carrying out catalytic reaction for 2-10 hours at the temperature being 100-400 DEG C to obtain 2,3-pentanedione. M is an active load and is any one of K2CO3, KHCO3, KNO3, KPO4 and KF, N is acarrier and is any one of Al2O3, a zeolite molecular sieve and ZrO2, and the mole ratio of the active load to the carrier is 1: (0.1-10); and the mass ratio of the solid alkali catalyst M / N to lacticacid is 1: (5-100). Load type superbase is a catalyst, the 2,3-pentanedione is synthesized by catalyzing the lactic acid, the selectivity and the conversion ratio can be high, and the yield of directly synthesized 2,3-pentanedione reaches 60-80%.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a synthesis method of 2,3-pentanedione. Background technique [0002] 2,3-Pentanedione, also known as levulinyl, is an important intermediate raw material, which can be used in the synthesis of drugs, preservatives, fungicides, hardeners for epoxy resins and dyeing aids for acrylic fibers. At the same time, the most important use of 2,3-pentanedione is as a fragrance product, which can replace diacetyl. Therefore, the study of low-cost, high-efficiency 2,3-pentanedione production technology will have important application prospects and market value. [0003] The current industrial production method of 2,3-pentanedione is to use 2-pentanone as a raw material, react with nitrous acid to generate pentanone oxime, and then decompose it with sulfuric acid to prepare 2,3-pentanedione. However, the pollution of this method is large and does not meet the principle of green pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/48B01J27/12B01J27/18B01J27/232B01J27/25C07C49/12
CPCB01J27/12B01J27/18B01J27/232B01J27/25C07C45/48C07C49/12
Inventor 冯乙巳刘文强陶婷婷王旭东徐卓玮贾涛
Owner HEFEI UNIV OF TECH
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