A kind of method preparing nitroanisole with nitrochlorobenzene meta-position oil

Abstract

The purpose of the present invention is to provide a method for producing nitroanisole with low cost, low energy consumption, short production cycle, and less waste, that is, using nitrochlorobenzene meta-oil under anhydrous system to prepare meta Methods for nitrochlorobenzene, p-nitroanisole, and o-nitroanisole. In order to achieve the above object, the technical scheme adopted in the present invention is as follows: nitrochlorobenzene meta-oil is added in the autoclave, and methanol and sodium hydroxide are added respectively, wherein the molar ratio of sodium hydroxide and meta-oil is 0.01 ~ 2.00 : 1, the molar ratio of methanol to meta-oil is 1~20:1, the reaction temperature is 10~200°C, the reaction time is 1~20 hours, the pressure is 0.1~4.0MPa, and the reaction product is analyzed by gas chromatography. Its content varies with the composition of the reaction raw material meta-oil. Compared with the traditional technology, the invention has the advantages of low production cost, short process, low energy consumption and little pollution.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, in particular to a method for producing o-nitroanisole, p-nitroanisole and m-nitrochlorobenzene with meta-oil. Background technique [0002] Nitroanisole (o-nitroanisole, p-nitroanisole) is an important intermediate for the synthesis of dyes, spices and medicines. ) is an important raw material. As we all know, aminoanisole (o-aminoanisole, p-aminoanisole) is an intermediate in the synthesis of dyes, spices and medicines, and can be used to manufacture azo dyes, ice dyes, naphthol, guaiacol and pandan More than 100 kinds of fine chemicals such as element, artificial musk, domestic and foreign market demands are constantly increasing, so inventing a kind of method of producing aminoanisole with low cost, low energy consumption, and three wastes is extremely urgent. [0003] The traditional production process of o-aminoanisole or p-aminoanisole is made from o-nitrochlorobenzene or p-nitroc...

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

[0009] (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 materials used in this invention are mixed nitrochlorobenzene, although the problems of rectification tower equipment investment and rectification energy consumption are solved, there is no raw material used in the present invention The cost of meta oil is low because meta oil is the distillation residue of nitrochlorobenzene

[0014] To sum up, some of the existing nitroanisole production methods 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.

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