Production process for o-aminoanisole and preparation method thereof

Abstract

The invention discloses a production process for o-aminoanisole. The production process for the o-aminoanisole comprises the following steps: carrying out etherification by using methanol and sodium hydroxide as methoxyl reagents to obtain o-nitroanisole; and reducing the o-nitroanisole by sodium sulphide under the effect of a catalyst to synthesize the o-aminoanisole. According to specific reaction, main reaction is as shown in specification. In the production process for the o-aminoanisole, production raw materials are easily obtained; the production process is simple and easy; the problemsof difficulty in recycling of the catalyst and serious fire in hydrogenation reduction are solved, a certain amount of waste water is generated by reduction through sodium sulfide, and the productionprocess for the o-aminoanisole has the advantages of good product quality and high safety factors.

Description

technical field

[0001] The invention relates to the technical field of heavy metal polluted soil treatment, in particular to a production process of anthranil. Background technique

[0002] Anthranil is an important dye and pharmaceutical intermediate, which is used to produce dyes such as azo dyes, ice dyes, naphthol ASOL and other drugs, such as guaiacol and anitropium, and can also be used to prepare vanillin, etc. product.

[0003] At present, the commonly used synthesis route of o-aminoanisole in domestic industry is: take o-nitrochlorobenzene as raw material, carry out methoxylation reaction with methanol and sodium hydroxide to generate o-nitroanisole, and then reduce, and the reaction product undergoes Separation and distillation under reduced pressure give the product anthranil. The reduction methods of o-nitroanisole include: iron powder reduction, alkali sulfide reduction, hydrogenation reduction, etc. Iron powder reduction is an obsolete process ordered by the...

Examples

Embodiment 1

[0021] Add 40g of flaky caustic soda and 120ml of methanol with a mass percentage concentration of 99% in the methanol preparation pot, stir evenly, the temperature of the preparation pot rises naturally, stir when the temperature no longer rises, take a sample for analysis, and when the NaOH content reaches the set standard , cooling, the material is compressed into the sodium methoxide storage tank with air pressure; the methanol from the methanol tank is pumped into the metering tank and then added to the etherification kettle; 1000ml of water is added from the water metering tank; the o-nitrochlorobenzene is pumped Enter the kettle after entering the metering tank; pump sodium methoxide from the sodium methoxide storage tank to the metering tank, then use an air compressor to add compressed air to the sodium methoxide metering tank and etherification reaction kettle, raise the temperature and add sodium methoxide dropwise to control the dropping speed , temperature; after t...

Embodiment 2

[0023] Add 30g of flaky caustic soda and 100ml of methanol with a mass percentage concentration of 99% in the methanol preparation pot, stir evenly, the temperature of the preparation pot rises naturally, stir when the temperature no longer rises, take a sample for analysis, and when the NaOH content reaches the set standard , cooling, the material is air-compressed to the sodium methoxide storage tank; the methanol from the methanol tank is pumped into the metering tank and then added to the etherification kettle; 800ml of water is added from the water metering tank; the o-nitrochlorobenzene is pumped Enter the kettle after entering the metering tank; pump sodium methoxide from the sodium methoxide storage tank to the metering tank, then use an air compressor to add compressed air to the sodium methoxide metering tank and etherification reaction kettle, raise the temperature and add sodium methoxide dropwise to control the dropping speed , temperature; after the dropwise addit...

Embodiment 3

[0025] Add 20g of flaky caustic soda and 80ml of methanol with a mass percentage concentration of 98% in the methanol preparation pot, stir evenly, the temperature of the preparation pot rises naturally, stir when the temperature no longer rises, take a sample for analysis, when the NaOH content reaches the set standard , cooling, the material is air-compressed to the sodium methoxide storage tank; the methanol from the methanol tank is pumped into the metering tank and then added to the etherification kettle; 150ml of water is added from the water metering tank; the o-nitrochlorobenzene is pumped Enter the kettle after entering the metering tank; pump sodium methoxide from the sodium methoxide storage tank to the metering tank, then use an air compressor to add compressed air to the sodium methoxide metering tank and etherification reaction kettle, raise the temperature and add sodium methoxide dropwise to control the dropping speed , temperature; after the dropwise addition, ...

technical field

[0001] The invention relates to the technical field of heavy metal polluted soil treatment, in particular to a production process of anthranil. Background technique

[0002] Anthranil is an important dye and pharmaceutical intermediate, which is used to produce dyes such as azo dyes, ice dyes, naphthol ASOL and other drugs, such as guaiacol and anitropium, and can also be used to prepare vanillin, etc. product.

[0003] At present, the commonly used synthesis route of o-aminoanisole in domestic industry is: take o-nitrochlorobenzene as raw material, carry out methoxylation reaction with methanol and sodium hydroxide to generate o-nitroanisole, and then reduce, and the reaction product undergoes Separation and distillation under reduced pressure give the product anthranil. The reduction methods of o-nitroanisole include: iron powder reduction, alkali sulfide reduction, hydrogenation reduction, etc. Iron powder reduction is an obsolete process ordered by the...

Examples

Embodiment 1

[0021] Add 40g of flaky caustic soda and 120ml of methanol with a mass percentage concentration of 99% in the methanol preparation pot, stir evenly, the temperature of the preparation pot rises naturally, stir when the temperature no longer rises, take a sample for analysis, and when the NaOH content reaches the set standard , cooling, the material is compressed into the sodium methoxide storage tank with air pressure; the methanol from the methanol tank is pumped into the metering tank and then added to the etherification kettle; 1000ml of water is added from the water metering tank; the o-nitrochlorobenzene is pumped Enter the kettle after entering the metering tank; pump sodium methoxide from the sodium methoxide storage tank to the metering tank, then use an air compressor to add compressed air to the sodium methoxide metering tank and etherification reaction kettle, raise the temperature and add sodium methoxide dropwise to control the dropping speed , temperature; after t...

Embodiment 2

[0023] Add 30g of flaky caustic soda and 100ml of methanol with a mass percentage concentration of 99% in the methanol preparation pot, stir evenly, the temperature of the preparation pot rises naturally, stir when the temperature no longer rises, take a sample for analysis, and when the NaOH content reaches the set standard , cooling, the material is air-compressed to the sodium methoxide storage tank; the methanol from the methanol tank is pumped into the metering tank and then added to the etherification kettle; 800ml of water is added from the water metering tank; the o-nitrochlorobenzene is pumped Enter the kettle after entering the metering tank; pump sodium methoxide from the sodium methoxide storage tank to the metering tank, then use an air compressor to add compressed air to the sodium methoxide metering tank and etherification reaction kettle, raise the temperature and add sodium methoxide dropwise to control the dropping speed , temperature; after the dropwise addit...

Embodiment 3

[0025] Add 20g of flaky caustic soda and 80ml of methanol with a mass percentage concentration of 98% in the methanol preparation pot, stir evenly, the temperature of the preparation pot rises naturally, stir when the temperature no longer rises, take a sample for analysis, when the NaOH content reaches the set standard , cooling, the material is air-compressed to the sodium methoxide storage tank; the methanol from the methanol tank is pumped into the metering tank and then added to the etherification kettle; 150ml of water is added from the water metering tank; the o-nitrochlorobenzene is pumped Enter the kettle after entering the metering tank; pump sodium methoxide from the sodium methoxide storage tank to the metering tank, then use an air compressor to add compressed air to the sodium methoxide metering tank and etherification reaction kettle, raise the temperature and add sodium methoxide dropwise to control the dropping speed , temperature; after the dropwise addition, ...

Images