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Method for preparing o-nitro anisole by using micro-channel reaction apparatus

A technology of o-nitroanisole and microchannel reaction, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of high energy consumption, short time, and no reaction platform for rectification, and achieve Precisely control the reaction conditions, improve the reaction efficiency and shorten the reaction time

Inactive Publication Date: 2016-04-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the present invention solves the technical problems of rectification tower equipment investment in the existing production process of o-nitroanisole and p-nitroanisole, high rectification energy consumption and high cost, but because it is an atmospheric pressure method, the reaction It takes a long time, which affects the product production cycle and its output
[0007] (2) Changzhou Jiasen Chemical Co., Ltd. also disclosed a process for producing o-nitroanisole, p-nitroanisole and m-nitrochlorobenzene from chlorobenzene (Chinese patent CN200610085488.8). Chlorobenzene is used as raw material, nitrochlorobenzene mixture is obtained through nitration reaction, and the nitrochlorobenzene mixture directly undergoes etherification reaction in etherification agent, and the etherification product is separated and refined to obtain o-nitroanisole, p- Nitroanisole and m-nitrochlorobenzene products, the etherification reaction is characterized in that the etherification agent can be methanol, or a mixture or compound of an acid-binding agent and methanol, and the acid-binding agent can be sodium hydroxide, carbonic acid Sodium, magnesium oxide, calcium oxide, ammonium carbonate, magnesium carbonate, calcium carbonate, ammonium bicarbonate, sodium bicarbonate, etc. The etherification reactor can be a continuous tubular reactor, a continuous stirred tank reactor with multiple tanks connected in series, a batch Stirred tank reactors, static mixers, dynamic mixers, etc., the raw material used in this invention is mixed nitrochlorobenzene, although it solves the problems of rectification tower equipment investment and rectification energy consumption, there is no reaction of the present invention Advantages such as short time
[0011] To sum up, some of the existing production methods of o-nitroanisole have high cost of raw materials, some have long production cycle, some have high energy consumption, some have many three wastes, and there are more or less problems of one kind or another.

Method used

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  • Method for preparing o-nitro anisole by using micro-channel reaction apparatus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Mix 500 grams of o-nitrochlorobenzene, 200 grams of methanol, 25 grams of sodium hydroxide, and 500 grams of water, and adjust the temperature of the constant temperature system to a reaction temperature of 60°C. In the reaction system, after the reaction was finished, sampling and analysis showed that the conversion rate of o-nitrochlorobenzene was 62%.

Embodiment 2

[0039] Mix 500 grams of o-nitrochlorobenzene, 200 grams of methanol, 25 grams of sodium hydroxide, and 500 grams of water, and adjust the temperature of the constant temperature system to a reaction temperature of 80°C. In the reaction system, after the reaction was finished, sampling and analysis showed that the conversion rate of o-nitrochlorobenzene was 75%.

Embodiment 3

[0041] Mix 500 grams of o-nitrochlorobenzene, 200 grams of methanol, 25 grams of sodium hydroxide, and 500 grams of water, and adjust the temperature of the constant temperature system to the reaction temperature of 100°C. The reaction system, after the reaction, was sampled and analyzed, and the conversion rate of o-nitrochlorobenzene was 85%.

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Abstract

The present invention provides a new method for preparing o-nitro anisole by using a micro-channel reactor, particularly application of a micro-channel reactor with an enhanced mass transfer unit structure to carry out a continuous flow o-nitro chloro benzene etherification reaction. According to the present invention, the mass transfer and the heat transfer can be completed dependent on the kinetic energy of the fluid without the mechanical stirring process under the reactor operation condition higher than the normal temperature, the space time reaction rate of the micro-channel reactor can be substantially improved, the temperature fluctuation and the concentration fluctuation during the reaction process can be avoided, the phenomena such as temperature runaway and overheating do not exist, and the reaction process is safe.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for preparing o-nitroanisole by using a microchannel reaction device. Background technique [0002] o-Nitroanisole is an important intermediate for the synthesis of dyes, spices and medicines, and an important raw material for the synthesis of o-aminoanisole. As we all know, anthranil can produce more than 100 kinds of fine chemicals such as azo dyes, ice dyes, naphthol, guaiacol, vanillin, and artificial musk. The traditional production process of anthranil is It is prepared by taking o-nitrochlorobenzene as raw material through etherification, hydrogenation, separation, rectification and other processes. Domestic and foreign market demand is constantly increasing, so it is extremely urgent to invent a method for producing anthranil with low cost, low energy consumption and less waste. [0003] Liaoning Shixing Pharmaceutical Co., Ltd. discloses a p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C205/37
Inventor 张萍郁铭付春
Owner CHINA PETROLEUM & CHEM CORP
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