Continuous preparation method of benzil or derivative of benzil

A technology of derivatives and benzil, which is applied in the field of continuous preparation of benzil or its derivatives, can solve the problems of high risk factor and large environmental pollution, and achieve the effects of high safety, environmental protection and short process flow

Active Publication Date: 2018-11-06
维思普新材料(苏州)有限公司
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  • Description
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Problems solved by technology

[0010] The present invention aims to solve the problems of large environmental pollution and high risk factor in the existing production method of synthesizing benzil or its derivatives from benzoin or its derivatives, thereby providing a kind of product that is beneficial to the environment and has a high product conversion rate and Preparation method of benzil or its derivatives with excellent product quality

Method used

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  • Continuous preparation method of benzil or derivative of benzil
  • Continuous preparation method of benzil or derivative of benzil
  • Continuous preparation method of benzil or derivative of benzil

Examples

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preparation example Construction

[0030] The invention provides a continuous preparation method of benzil or derivatives thereof, characterized in that:

[0031] In a microchannel reactor, benzoin or benzoin derivatives are reacted with nitric acid according to the following reaction formula to obtain benzil or derivatives thereof,

[0032]

[0033] Among them, R 1 and R 2 same or different, each H, halogen, substituted or unsubstituted C 1 -C 8 Alkyl, substituted or unsubstituted C 1 -C 8 Alkoxy, or nitro; wherein said C 1 -C 8 Alkyl or C 1 -C 8Alkoxy is optionally replaced by C 1 -C 8 Alkyl, C 1 -C 8 Alkoxy or halogen substitution.

[0034] Specific examples of halogen include fluorine, chlorine, bromine, and iodine.

[0035] as substituted or unsubstituted C 1 -C 8 Specific examples of the alkyl group include, for example, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl, n-pentyl, 1-methyl-n-butyl Base, 2-methyl-n-butyl, 3-methyl-n-butyl, 1,1-dimethyl-n-propy...

Embodiment 1

[0055] The molar flow ratio of benzoin and nitric acid in the microchannel reactor is 1:1, and the reaction raw materials benzoin and nitric acid are both fed in the form of solution. According to 100g benzoin, add 200g toluene to prepare the toluene solution of benzoin, the concentration is 2.05mol / L, the mass percent concentration of nitric acid is 40%, and the concentration is 7.91mol / L. The volume flow of benzoin solution is 50mL / min, and the volume flow of nitric acid is 12.9mL / min. Microchannel reactor 1 is a mixing preheating module with a controlled temperature of 130°C. The microchannel reactor 2 is a reaction module, and the reaction is carried out at normal pressure and 130° C., and the residence time is 20 s. The microchannel reactor 3 is a cooling module, and the temperature is controlled at 25°C. According to HPLC analysis, the conversion rate of the product benzil was 98.2%.

Embodiment 2

[0057] The molar flow ratio of benzoin and nitric acid in the microchannel reactor is 1:1.1, and the reaction raw materials benzoin and nitric acid are both fed in the form of solution. According to 100g benzoin, add 200g toluene to prepare the toluene solution of benzoin, the concentration is 2.05mol / L, the mass percent concentration of nitric acid is 40%, and the concentration is 7.91mol / L. The volume flow of benzoin solution is 50mL / min, and the volume flow of nitric acid is 14.2mL / min. Microchannel reactor 1 is a mixing preheating module with a controlled temperature of 130°C. The microchannel reactor 2 is a reaction module, and the reaction is carried out at normal pressure and 130° C., with a residence time of 10 s. The microchannel reactor 3 is a cooling module, and the temperature is controlled at 25°C. According to HPLC analysis, the conversion rate of the product benzil was 98.3%.

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Abstract

The invention relates to a continuous preparation method of benzil or a derivative of the benzil. The preparation method comprises the following steps: performing a reaction on benzoin or a derivativeof the benzoin and nitric acid in a microchannel reactor to obtain the benzil or the derivative of the benzil, and optionally introducing oxygen or air during the reaction. After the completion of the reaction, the conversion rate of the product benzil is 98% or higher by a HPLC analysis. The reacted nitric acid solution can be recycled and reused.

Description

technical field [0001] The invention relates to a continuous preparation method of benzil or derivatives thereof, belonging to the technical field of functional materials. Background technique [0002] Benzil, also known as diphenyl ethylene dione, is a yellow diamond-shaped crystalline powder, which exhibits special reactivity due to its non-conjugated aromatic α-dicarbonyl structure. It is used in the production of biomedicine, pesticides and daily chemicals It has a wide range of applications and is an important class of organic synthesis intermediates. Benzoin is also known as benzoin, and its chemical name is 1,2-diphenylethanolone, which can also be called 2-hydroxy-1,2-diphenylethanone, diphenylethanolone, 2-hydroxy- 2-Phenylacetophenone is an important raw material for the synthesis of benzil. The method of oxidative synthesis of benzil from benzoin is currently the most mature, the highest reaction yield, and the most widely used synthetic route. [0003] At pres...

Claims

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Application Information

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IPC IPC(8): C07C45/29C07C49/784C07C49/84
CPCC07C45/29C07C49/784C07C49/84
Inventor 袁晓冬刘海丰陈潇陈华
Owner 维思普新材料(苏州)有限公司
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