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Method for preparing nitroanisole from m-nitrochlorobenzene oil

A technology for nitrochlorobenzene meta oil and nitroanisole, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc. Distillation energy consumption and other problems, to achieve the effect of short reaction time, reduce production costs, reduce process steps

Active Publication Date: 2015-04-29
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
[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.

Method used

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  • Method for preparing nitroanisole from m-nitrochlorobenzene oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 157.5 g (1 mol) of nitrochlorobenzene meta-oil, 240 ml (6 mol) of methanol, and 20 g (0.5 mol) of sodium hydroxide into the reaction kettle. Heat to 120°C, control the reaction pressure to 0.3MPa, and keep the reaction time for 3 hours. Sampling analysis showed that the total etherification conversion rate of o- and p-nitrochlorobenzene was 99.5%.

Embodiment 2

[0036] Embodiment 2 (comparative example)

[0037] Add 157.5 g (1 mol) of nitrochlorobenzene meta-oil, 240 ml (6 mol) of methanol, and 20 g (0.5 mol) of sodium hydroxide into the reaction kettle. Heating to methanol reflux temperature of 70°C, reflux reaction, keeping the reaction time for 10 hours. Sampling analysis showed that the total etherification conversion rate of o- and p-nitrochlorobenzene was 85.0%.

Embodiment 3

[0039] Add 157.5 g (1 mol) of meta-nitrochlorobenzene oil, 240 ml (6 mol) of methanol (recovered methanol) and 20 g (0.5 mol) of sodium hydroxide in the reaction kettle. Heat to 120°C, control the reaction pressure to 0.3MPa, and keep the reaction time for 3 hours. Sampling analysis showed that the total etherification conversion rate of o- and p-nitrochlorobenzene was 99.5%.

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Abstract

The invention aims to provide a nitroanisole production method with low cost, low energy consumption, short production cycle and few three wastes (waste gas, wastewater and industrial residue), namely a method for preparing m-nitrochlorobenzene, p-nitroanisole and o-nitroanisole from m-nitrochlorobenzene oil under an anhydrous system by a high pressure method. To achieve the above purpose, the technical scheme of the invention is as follows: m-nitrochlorobenzene oil is added into an autoclave, and methanol and sodium hydroxide are respectively added, wherein the mole ratio of sodium hydroxide to m-nitrochlorobenzene oil is 0.01-2.00:1, the mole ratio of methanol to m-nitrochlorobenzene oil is 1-20:1, reaction temperature is 10-200 DEG C, reaction time is 1-20 h, and pressure is 0.1-4.0 MPa; and products obtained after the reaction undergo gas chromatography, and content changes with the composition change of the reaction raw material m-nitrochlorobenzene oil. In comparison with traditional technologies, the method provided by the invention has advantages of low production cost, short process, low energy consumption and little pollution.

Description

Technical field [0001] The present invention is a fine chemical technology field. Specifically, it involves a method of producing tunnels, nitrogenzol ether, and spinning nitrate chloride. Background technique [0002] Nitro -nitrogen ether (tangentopenzoethyl, to nitrophenyl ether) is an important intermediate of synthetic dyes, spices and medicine.) Important raw materials.As we all know, amino benzo ether (adjacent aminozoethyl ether, aminozozoethyl) is an intermediate of synthetic dyes, spices and medicines.There are more than 100 fine chemicals such as vegetarian and artificial musk, and the demand for markets at home and abroad is growing. Therefore, it is even more imminent to invent a method of low -cost, low -energy consumption, and three wastes. [0003] The traditional neighboring amino benzoethe or the production process of aminozyl ether is based on tunnel nitrochloride or nitrochloride as raw materials.EssenceThis traditional preparation process has the disadvantage...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/37C07C201/12
Inventor 郁铭付春张萍孙阿沁高留冕
Owner CHINA PETROLEUM & CHEM CORP
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