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A kind of preparation method of isovaleraldehyde

A technology of isovaleraldehyde and isoamyl alcohol, applied in the chemical industry, can solve the problems of many side reactions, easy carbon deposition and deactivation of catalysts, and low production efficiency.

Active Publication Date: 2022-08-05
WANHUA CHEM GRP CO LTD
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Problems solved by technology

[0002] Isovaleraldehyde is an important chemical raw material, which is mainly used in the fields of synthetic spices, nutraceuticals, and medicines. Currently, the industrialized liquid-phase oxidation method uses catalysts such as sulfuric acid, dichromate, and manganese oxide. Unfavorable factors such as severe corrosion, large environmental pollution, and many side reactions
[0003] Chinese patent CN1261399C mentions the method of using brass catalysts to catalyze the oxidation of isoamyl alcohol to prepare isovaleraldehyde. The brass catalysts are copper-zinc or copper-nickel-copper-tin alloys, and the reaction temperature is 400-500°C. The catalyst is prone to carbon deposition and deactivation at high temperature, and the production energy consumption is high
[0004] It is mentioned in Chinese patent CN106117024 that at 800°C, the space velocity is 0.8h -1 Isovaleraldehyde is prepared by dehydrogenation and oxidation of isoamyl alcohol under certain conditions. The catalyst used is a mixture of amorphous silica-alumina, molecular sieve, alumina, boron oxide, iron oxide, zinc oxide, and zirconia. The isovaleraldehyde semi-finished product obtained by gas phase reaction It also needs to be treated with sodium hydroxide, alumina adsorption treatment, refining and other means, which has the disadvantages of high energy consumption and complicated process. At the same time, there is also the risk of aldehyde gasification and deterioration under alkali catalysis when isovaleraldehyde is treated with sodium hydroxide.
[0005] Chinese patent CN205868243U mentions the method of producing isovaleraldehyde from isoamyl alcohol using a reactor, but there are problems such as complex operation and low production efficiency in the reactor, which is not suitable for industrialized large-scale continuous production
[0006] In view of the deficiencies in the above-mentioned processes, it is urgent to develop a novel method for producing isovaleraldehyde from isoamyl alcohol, which overcomes the serious liquid phase oxidation corrosion, large environmental pollution, high temperature of the gas phase method, easy carbon deposition, and low production capacity in the current production. high consumption

Method used

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  • A kind of preparation method of isovaleraldehyde
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  • A kind of preparation method of isovaleraldehyde

Examples

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Effect test

Embodiment 1

[0034]Dissolve 125.5g cuprous nitrate and 18.9g zinc nitrate in 1000g distilled water to obtain a mixed salt solution, heat up to 60°C, add 82.1g of methylglycine diacetic acid under the stirring state of the mixed salt solution, and maintain after the dropwise addition is completed. The temperature continued to stir for 5 hours, the obtained solid precipitate was suction filtered, and dried at 100 ° C for 3 hours to obtain 152.1 g of metal organic framework material, 152.1 g of metal organic framework material and 80 g of molecular sieve were mixed uniformly and then kneaded with 220 g of 5% citric acid aqueous solution to form 2.5 -3.5mm spherical particles, the spherical particles were calcined at 300° C. for 5 h to obtain catalyst 1. Through ICP analysis, it is determined that in catalyst 1, by mass, (the above-mentioned metal salt raw material crystal water is not counted, there is no loss of organic matter and carrier, and the decomposition of citric acid is not counted, ...

Embodiment 2

[0036] Dissolve 188.3g cuprous nitrate and 8.9g manganese nitrate in 1000g distilled water to obtain a mixed salt solution, heat up to 80°C, add 125.9g of diethylenetriaminepentaacetic acid under the stirring state of the mixed salt solution, and after the dropwise addition is completed Maintain the temperature and continue to stir for 3 hours, filter the obtained solid precipitate with suction, and dry it at 100 ° C for 3 hours to obtain 223.9 g of metal organic framework material. Mix 223.9 g of metal organic framework material with 50 g of molecular sieves and knead with 240 g of 5% citric acid aqueous solution. The spherical particles of 2.5-3.5 mm were synthesized, and the spherical particles were calcined at 320° C. for 5 h to obtain catalyst 2. It was determined by ICP analysis that in catalyst 2, by mass, the following components accounted for the percentage of the total mass of catalyst 2: Cu34.8%, Mn1.0%, diethylenetriaminepentaacetic acid 46.0%, carrier 18.2%, the ca...

Embodiment 3

[0038] Dissolve 125.5g cuprous nitrate and 35.3g molybdenum nitrate in 1000g distilled water to obtain a mixed salt solution, heat up to 70°C, add 120.6g of hydroxyethylethylenediamine triacetic acid under the stirring state of the mixed salt solution, and add dropwise. After the end, the temperature was maintained and stirring was continued for 5 hours, the obtained solid precipitate was suction filtered, and dried at 100 ° C for 3 hours to obtain 193.6 g of metal-organic framework material, 193.6 g of metal-organic framework material and 60 g of molecular sieve were mixed uniformly, and then 120 g of 8% citric acid was used. The aqueous solution was kneaded into spherical particles of 2.5-3.5 mm, and the spherical particles were calcined at 300° C. for 5 hours to obtain catalyst 3. It is determined by ICP analysis that in catalyst 3, the following components account for the percentage of the total mass of catalyst 3 in terms of mass: Cu25.0%, Mo3.7%, hydroxyethylethylenediami...

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Abstract

The invention discloses a method for preparing isovaleraldehyde. Under the action of a porous metal organic Cu catalyst, isoamyl alcohol undergoes a gas phase dehydrogenation reaction to generate isovaleraldehyde. The isovaleraldehyde product is separated and produced, and the unreacted isoamyl alcohol is recovered to continue the oxidation reaction. The catalyst is used in the process of isoamyl alcohol dehydrogenation to prepare isovaleraldehyde, the conversion rate of dehydrogenation is > 90%, the selectivity is > 95.0%, the catalyst is stable during the dehydrogenation process, not easy to be lost, and the stability of the catalyst has a life span of 1500h There was no significant decrease in the experiment. The method of the invention has simple operation and good economic benefit.

Description

technical field [0001] The invention relates to a method for producing isovaleraldehyde, in particular to a method for preparing isovaleraldehyde by oxidation of isoamyl alcohol, and belongs to the technical field of chemical industry. technical background [0002] Isovaleraldehyde is an important chemical raw material, mainly used in the synthesis of fragrances, nutritional chemicals, medicine and other fields. The industrialized liquid-phase oxidation method uses sulfuric acid, dichromate, manganese oxide and other catalysts. Unfavorable factors such as serious corrosion, large environmental pollution, and many side reactions. [0003] Chinese patent CN1261399C mentions a method for preparing isovaleraldehyde by catalyzing isoamyl alcohol oxidation with a brass catalyst, the brass catalyst is an alloy of copper-zinc or copper-nickel, copper-tin, and the reaction temperature is 400-500 ℃, At high temperature, the catalyst is prone to carbon deposition and deactivation, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/00C07C45/78C07C47/02B01J31/22B01J35/10
CPCC07C45/002C07C45/783B01J35/1028B01J35/1042B01J31/1691B01J31/2243B01J2531/16C07C47/02
Inventor 王中华张永振张德旸刘英俊黎源
Owner WANHUA CHEM GRP CO LTD
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