Method for producing anisidine by mixed nitrochlorobenzene reacting in aqueous solvent

A technology of aminoanisole and nitrochlorobenzene, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., can solve the problems of increasing difficulty in environmental protection, increasing processing requirements, and increasing production costs, etc. problems, to achieve the effect of reducing equipment investment, simplifying production processes, and reducing labor intensity

Inactive Publication Date: 2012-04-25
扬州铭睿达化工科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This will inevitably lead to higher requirements for solvent recovery equipment, safety level, wastewater treatment, nitrochlorophenyl etherification reaction or raw material pretreatment, higher production costs, and greater difficulty in environmental protection

Method used

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  • Method for producing anisidine by mixed nitrochlorobenzene reacting in aqueous solvent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) etherification reaction: at 2M 3 Add mixed nitrochlorobenzene (o-nitrochlorobenzene content 36.8%, p-nitrochlorobenzene content 61.6%, m-nitrochlorobenzene 1.6%) 600kg, methyl alcohol 120kg, sodium hydroxide 200kg in the reaction kettle. Heating to 70°C, and then adding 700kg of water. Heat to 120°C, control the reaction pressure to 0.6MPa, and keep the reaction time for 4 hours. Sampling analysis showed that the total etherification conversion rate of o- and p-nitrochlorobenzene was 98.3%.

[0019] (2) Liquid-liquid separation: the reaction liquid in the previous step was cooled to room temperature (27° C.), and the water phase was separated to obtain 580 kg of etherified oil. After the water phase is filtered to remove impurities, it can be recycled for secondary batching.

[0020] (3) Hydrogenation reduction: Add 580kg of etherified oil obtained in the previous step, 1.5kg of Ce-modified Pd-C catalyst, and 50kg of water to 1M 3 In the reaction kettle, the rea...

Embodiment 2

[0025] (1) etherification reaction: at 2M 3 Add mixed nitrochlorobenzene (44.7% o-nitrochlorobenzene content, 54.1% p-nitrochlorobenzene content, 1.2% m-nitrochlorobenzene) 600kg, methanol 200kg, and sodium hydroxide 300kg in the reactor. Heat to 70°C, and then add 200kg of water. Heat to 80°C, control the reaction pressure to 0.2MPa, and keep the reaction time for 8 hours. Sampling analysis showed that the total etherification conversion rate of o- and p-nitrochlorobenzene was 97.7%.

[0026] (2) Liquid-liquid separation: the reaction liquid in the previous step was cooled to room temperature (25° C.), and the water phase was separated to obtain 586 kg of etherified oil. After the water phase is filtered to remove impurities, it can be recycled for secondary batching.

[0027] (3) Hydrogenation reduction: 583kg of etherified oil obtained in the previous step, 2.0kg of La modified Pd-C catalyst, and 250kg of water were added to 1M 3 In the reaction kettle, the reaction tem...

Embodiment 3

[0032] (1) etherification reaction: at 2M 3 Add mixed nitrochlorobenzene (65.7% o-nitrochlorobenzene content, 32.4% p-nitrochlorobenzene content, 1.9% m-nitrochlorobenzene) 600kg, methyl alcohol 120kg, sodium hydroxide 300kg in the reaction kettle. Heat to 70°C, and then add 500kg of water. Heat to 150°C, control the reaction pressure to 1.6MPa, and keep the reaction time for 4 hours. Sampling and analysis showed that the total etherification conversion rate of o- and p-nitrochlorobenzene was 99.4%.

[0033] (2) Liquid-liquid separation: the reaction liquid in the previous step was cooled to room temperature (24° C.), and the water phase was separated to obtain 586 kg of etherified oil. After the water phase is filtered to remove impurities, it can be recycled for secondary batching.

[0034] (3) Hydrogenation reduction: Add 586kg of etherified oil obtained in the previous step, 12kg of skeleton nickel catalyst, and 100kg of water to 1M 3 In the reaction kettle, the reaction...

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Abstract

The invention relates to a method for producing anisidine by mixed nitrochlorobenzene (comprising o-nitrochlorobenzene, p-nitrochlorobenzene and m-nitrochlorobenzene) in an aqueous solvent through steps of etherification, hydrogenation, distillation separation, and the like. The method comprises the technical processes: (1) enabling the mixed nitrochlorobenzene and methanol to react, using water as a solvent and sodium hydroxide as a catalyst; (2) separating an aqueous phase; (3) catalyzing and hydrogenating etherified oil, and directly hydrogenating and reducing the etherified oil by using water as the solvent without washing to remove alkaline by water; (4) filtering the catalyst; (5) separating crude products, cooling and precipitating an organic phase, and separating and removing the water phrase; and (6) rectifying and separating an organic phase, and rectifying the organic phase obtained by separating water to obtain pure p-anisidine and pure o-anisidine with the purity over 99 percent. The method for producing anisidine by mixed nitrochlorobenzene reacting in an aqueous solvent has simple technology, low cost and energy consumption, high product purity, environmental protection and low toxicity.

Description

technical field [0001] The invention relates to a process for producing aminoanisole by reacting mixed nitrochlorobenzenes in a water solvent, belonging to the technical field of chemical industry. technical background [0002] Aminoanisole (o-aminoanisole, p-aminoanisole) is an intermediate for synthetic dyes, spices and medicines, and can be used to manufacture azo dyes, ice dyes, naphthol, guaiacol and vanillin, There are more than 100 kinds of fine chemicals such as artificial musk, and the domestic and foreign market demand continues to grow. Therefore, in recent years, aminoanisole has developed rapidly in China. According to statistics, in 2008, the global production capacity has reached 120,000 tons, while the domestic annual production capacity has reached more than 80,000 tons, which also plays a pivotal role in the international arena. [0003] The traditional production process of o-aminoanisole or p-aminoanisole is to use o-nitrochlorobenzene or p-nitrochlorobe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/84C07C213/02
Inventor 段睿菅盘铭范以宁赵红坤菅睿琪宋桂芳
Owner 扬州铭睿达化工科技有限公司
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