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Synthetic method of 2-heptanone

A synthesis method and technology of acetone, applied in the field of synthesizing 2-heptanone, can solve the problems of many by-products, high production cost, and high equipment requirements, and achieve the effects of reducing the probability of side reactions, reducing equipment investment, and shortening the technological process.

Active Publication Date: 2015-04-01
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2-Heptanone can be extracted from clove oil or cinnamon oil, but due to limited natural resources, it is difficult to realize industrial production; under certain pH conditions, short-chain fatty acids such as caprylic acid or fatty acid salts such as sodium caprylate can also be produced after biological fermentation 2-heptanone is obtained, but the yield of MAK prepared by the biological fermentation method is low, and there are many by-products, the separation and purification are difficult, and the production cost is high; 2-heptanol can be dehydrogenated and oxidized under the action of a catalyst to obtain 2-heptanol Ketone, but the price of raw material 2-heptanol is relatively high, and it is difficult to obtain; n-butyl ethyl acetoacetate can produce MAK through steps such as saponification, neutralization, and decarboxylation, and the operation is safe, but the raw material n-butyl acetoacetate ethyl Ester is not easy to get, and the production cost is higher, so the above methods are not suitable for industrial production
However, since the process is dehydrated under acidic conditions, it is still necessary to add a certain amount of acid solution to produce a certain amount of acid-containing waste liquid, and the addition of acid will lead to an increase in by-products. higher requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] According to attached figure 1 As shown in the process flow, in a single-tube reactor with a jacket (inner diameter of 10 mm), SiC pellets, 250 g of hydrogen-oxygen type macroporous strongly basic type I anion exchange resin and SiC pellets were respectively loaded, and the jacket Condensed water was added to control the reaction temperature. Acetone, butyraldehyde and water were fed into the reactor with a metering pump. The reaction products were analyzed by gas chromatography. Reaction conditions and results are shown in Table 1

[0033]

[0034]

[0035] Note: C6 is acetone self-condensation product and its partial dehydration product

[0036]C7 is the condensation product of acetone and butyraldehyde and its partial dehydration product

[0037] C8 is the self-condensation product of butyraldehyde and its partial dehydration product

Embodiment 2

[0039] The technical process identical with embodiment 1, in the there-necked flask that has stirrer, thermometer and dropping funnel, add 30ml massfraction and be 10% sodium hydroxide solution, add 350g acetone butyl mixed in a certain proportion through dropping funnel For the aldehyde mixture, control the dropwise addition time for about 2 hours. After the dropwise addition, continue to stir and react for 15 minutes, and then add a small amount of sulfuric acid to neutralize the reaction solution to make it neutral. The product was analyzed by gas chromatography, and the results are shown in Table 2.

[0040] Table 2

[0041]

Embodiment 3

[0043] The same technological process as embodiment 1, in the there-necked flask with stirrer, thermometer, dropping funnel, add 100ml concentration and be the sulfuric acid solution of 1mol / L, and adorn on the there-necked flask with the condensing tube of receiving bottle, condense Put condensed water into the tube, then add the three-necked flask to 100-120°C, then add 150g diacetone alcohol and 150g 4-hydroxy 2-heptanone dropwise through the dropping funnel within about 3 hours, and receive the dehydration product isopropyl through the condenser tube Acetone, 3-hepten-2-one and the water taken out by azeotropy continued to react for about 5 hours after the dropwise addition was completed. During the reaction, the water phase collected in the receiving bottle was intermittently added back to the three-necked flask to continue the reaction, and the oil phase was the products mesityl oxide and 3-hepten-2-one. After the reaction, the aqueous phase was extracted with ether, and...

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Abstract

The invention discloses a chemical synthetic method, specifically a method for synthesizing 2-heptanone by using acetone and butyraldehyde as raw materials. According to the invention, acetone and butyraldehyde which used as raw materials undergo a cross aldol condensation reaction under catalysis of solid base, and reaction products further undergo dehydration and catalytic hydrogenation so as to prepare 2-heptanone. The invention has advantages as follows: technological process is shortened by the technology; generation of an acid-containing waste liquid is avoided; generation of by-products is minimized; investment in equipment is reduced; and production costs of the product are decreased.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a method for synthesizing 2-heptanone by using acetone and butyraldehyde as raw materials. Background technique [0002] 2-Heptanone (2-Heptanone) chemical name Methyl Amyl Ketone (MethylAmylKetone), referred to as MAK, is a colorless liquid, slightly soluble in water, soluble in alcohol, ether and other organic solvents. MAK has high solubility to resins, polymers, etc., and is a green and environmentally friendly oxygen-containing solvent with very promising market prospects. [0003] The synthesis methods of 2-heptanone mainly include extraction method, biological fermentation method, 2-heptanol dehydrogenation oxidation method, n-butyl acetoacetate ethyl ester method and acetone butyraldehyde condensation method. 2-Heptanone can be extracted from clove oil or cinnamon oil, but due to limited natural resources, it is difficult to realize industrial production; under certain pH c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/04C07C45/62
CPCC07C45/62C07C45/74C07C49/04C07C49/203
Inventor 刘承伟王卫明应思斌谢自强祝航应兰兰
Owner ZHEJIANG XINHUA CHEM
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