Method for preparing benzaldehyde by continuously oxidizing methylbenzene through tubular reactor

A tubular reactor and benzaldehyde technology, applied in the direction of oxidation to prepare carbonyl compounds, etc., can solve the problems of target product selectivity, low yield, low oxidant utilization rate, poor mass transfer and heat transfer effect, etc., to improve the reaction rate And the utilization rate of raw materials, avoiding the use of co-catalysts, and expanding the effect of production scale

Inactive Publication Date: 2017-04-26
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the Chinese patent with patent number CN101607867 in 2009, the method of connecting multi-stage oxidation reactors and gas-liquid separators in series was adopted, the conversion rate of toluene reached more than 95%, and the total selectivity of benzaldehyde and benzyl alcohol reached more than 50% , but the conversion rate of the single-stage reactor is low and the energy consumption is high
In summary, the existing technology has many disadvantages such as high cost, high energy consumption, complicated process, and low selectivity of benzaldehyde.
[0007] The above-mentioned methods optimize and improve the preparation of benzaldehyde by oxidation of toluene from different angles, but there are still some problems to be solved: firstly, batch production in batch still is mainly used in large-scale production; secondly, in the above-mentioned method, there are still traditional The mass heat transfer effect is poor, the utilization rate of the oxidant is low, and the phenomenon of "flying temperature" easily occurs due to local overheating, which also causes the use of a large amount of oxidant in the above process, increased side reactions, and low selectivity and yield of the target product. In addition, in the above-mentioned intermittent production method, the decomposition rate of hydrogen peroxide is relatively fast, which is likely to cause safety accidents, which is also the reason why hydrogen peroxide oxidation has no large-scale application.

Method used

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  • Method for preparing benzaldehyde by continuously oxidizing methylbenzene through tubular reactor
  • Method for preparing benzaldehyde by continuously oxidizing methylbenzene through tubular reactor
  • Method for preparing benzaldehyde by continuously oxidizing methylbenzene through tubular reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) Device: refer to figure 2 Determine the connection mode of the tubular reactor. The pipeline type is: (3a+3b) direct flow channel + round cake pulse variable diameter rectangular flat pipeline. The inner diameter and volume of the pipeline are determined according to the flow rate and reaction residence time. The heat exchange medium is heat conduction Oil.

[0033] (2) Dissolve 6.06g of cobalt acetate and 6.06g of sodium molybdate in 200ml of toluene and 200ml of acetic acid to form a mixed solution. At this time, n (cobalt acetate): n (toluene) = 0.015:1, and dissolve 6.06g of sodium bromide at 15%H 2 o 2 form H 2 o 2 -Acetic acid solution, at this time n (sodium bromide):n (toluene)=0.015:1, toluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by constant flow pump respectively with the flow velocity of 8.33ml / min and 16.67ml / min, at this moment n (H 2 o 2 ): n (toluene) = 2:1, usin...

Embodiment 2

[0035] (1) Device: refer to figure 2 Determine the connection mode of the tubular reactor. The pipeline type is: (3a+3c) direct flow channel + oblique square cake pulse variable diameter rectangular flat pipeline. The inner diameter and volume of the pipeline are determined according to the flow rate and reaction residence time. The heat exchange medium is heat transfer oil.

[0036] (2) Dissolve 12.12g of cobalt acetate and 12.12g of sodium molybdate in 200ml of toluene and 200ml of acetic acid to form a mixed solution. At this time, n (cobalt acetate): n (toluene) = 0.03:1, and dissolve 12.12g of sodium bromide at 15%H 2 o 2 form H 2 o 2 -Acetic acid solution, at this time n (sodium bromide):n (toluene)=0.03:1, toluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by constant flow pump respectively with the flow velocity of 8.33ml / min and 16.67ml / min, at this moment n (H 2 o 2 ): n (toluene) = 2...

Embodiment 3

[0038] (1) Device: refer to figure 2 Determine the connection mode of the tubular reactor. The pipeline type is: (3a+3d) straight-through channel + enhanced mixing circular cake type rectangular flat pipeline. The inner diameter and volume of the pipeline are determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil. .

[0039] (2) Dissolve 6.06g of cobalt acetate and 6.06g of sodium molybdate in 200ml of toluene and 200ml of acetic acid to form a mixed solution. At this time, n (cobalt acetate): n (toluene) = 0.015:1, and dissolve 6.06g of sodium bromide at 15%H 2 o 2 form H 2 o 2 -Acetic acid solution, at this time n (sodium bromide):n (toluene)=0.015:1, toluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by constant flow pump respectively with the flow velocity of 8.33ml / min and 16.67ml / min, at this moment n (H 2 o 2 ): n (toluene) = ...

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Abstract

The invention discloses a method for preparing benzaldehyde by continuously oxidizing methylbenzene through a tubular reactor, and belongs to the technical field of organic synthesis processes. The method is a process technology that a methylbenzene compound is adopted as a raw material, a metal ion complex of one or more of cobalt, molybdenum and bromine is adopted as a catalyst, hydrogen peroxide is adopted as an oxidizing agent, acetic acid is adopted as a solvent, and methylbenzene is continuously oxidized in the tubular reactor to prepare benzaldehyde. The method is mild in condition, short in reaction time, high in raw material utilization rate, capable of achieving effective control in the reaction process, safe, stable and high in production efficiency and achieves continuous operation.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and relates to a method for preparing benzaldehyde by continuous oxidation of toluene under liquid-phase reaction conditions, more specifically, using toluene as a substrate, hydrogen peroxide as an oxidant, and a compound of cobalt, molybdenum and bromine Or several metal ion complexes are used as catalysts, monocarboxylic acid is used as solvent, and benzaldehyde products are prepared continuously in tubular reactors with different microstructures. Background technique [0002] Benzaldehyde is an important fine chemical product, which is widely used in industrial fields such as medicine, dyestuff, fragrance, pesticide and materials. [0003] The traditional industrial production methods of benzaldehyde mainly include the following three methods: toluene chlorination and hydrolysis, benzoic acid (fat) reduction method and toluene direct oxidation method, wherein the toluene ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/28C07C47/54
CPCC07C45/28C07C47/54
Inventor 严生虎蒋鑫张跃刘建武沈介发马晓明陈代祥辜顺林倪风超李彦飞王秋红陈明珠魏进吴飞张勇超
Owner CHANGZHOU UNIV
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