Method for producing aminoanisole by solvent-free catalytic hydrogenation

A technology for the catalytic hydrogenation of aminoanisole, which is applied in chemical instruments and methods, the preparation of organic compounds, and the preparation of aminohydroxyl compounds, etc., to achieve the effects of saving equipment investment, production safety, and reducing catalyst consumption

Inactive Publication Date: 2017-03-15
连云港泰盛化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for producing aminoanisole by solvent-free catalytic hydrogenation that is relatively safe, environmentally friendly and low in production cost, in view of the shortcomings of the existing process technology, so as to solve the problem of existing aminoanisole reduction methods. technical issues

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  • Method for producing aminoanisole by solvent-free catalytic hydrogenation
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Experimental program
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Effect test

Embodiment 1

[0022] like figure 1 , the method steps of producing aminoanisole by solvent-free catalytic hydrogenation are as follows:

[0023] Put the measured o-nitroanisole and palladium / carbon catalyst into a 10m³ hydrogenation reactor, the catalyst dosage is 0.20% of the o-nitroanisole, fill it with nitrogen for 3 to 4 times, and take gas samples Analyze the oxygen content ≤ 0.1%, then replace it with hydrogen, take a gas sample to analyze the hydrogen content ≥ 99.0%, start stirring, raise the temperature to 70°C, feed hydrogen, control the reaction pressure at 0.6-1.0Mpa, and the reaction temperature at 80-100°C Catalytic hydrogenation reaction.

[0024] After the catalytic hydrogenation reaction is over, the reducing solution is pumped to the catalyst filter for catalyst recovery. The filtered catalyst is carried by a small part of the reducing solution back to the hydrogenation reactor for recycling, and most of the reducing solution after filtering the catalyst is removed. Redu...

Embodiment 2

[0029] like figure 1 , the method steps of producing aminoanisole by solvent-free catalytic hydrogenation are as follows:

[0030] Put metered p-nitroanisole and palladium / carbon catalyst into two series-connected 10m³ hydrogenation reactors, the amount of catalyst is 0.25% of p-nitroanisole, fill with nitrogen replacement 3 to 4 times, take The oxygen content of the gas sample analysis is ≤0.1%, and then replaced with hydrogen, the gas sample is taken to analyze the hydrogen content ≥99.0%, the stirring is started, the temperature is raised to 70°C, the hydrogen gas is introduced, the reaction pressure is controlled at 0.6-1.0Mpa, and the reaction temperature is 80- Batch or continuous catalytic hydrogenation reaction at 100°C.

[0031] After the catalytic hydrogenation reaction is over, the reducing solution is pumped to the catalyst filter for catalyst recovery. The filtered catalyst is carried by a small part of the reducing solution back to the hydrogenation reactor for ...

Embodiment 3

[0036] like figure 1 , the method steps of producing aminoanisole by solvent-free catalytic hydrogenation are as follows:

[0037] In two 10m³ hydrogenation reactors connected in series, put into the mixture of o-nitroanisole and p-nitroanisole and palladium / carbon catalyst, the amount of catalyst is o-nitroanisole, p-nitrobenzene 0.30% of the total amount of the mixture of methyl ether, filled with nitrogen to replace 3 to 4 times, take a gas sample to analyze the oxygen content ≤ 0.1%, and then replace it with hydrogen, take a gas sample to analyze the hydrogen content ≥ 99.0%, start stirring, and heat up to 70 °C, feed hydrogen, control the reaction pressure at 0.6-1.0Mpa, and the reaction temperature at 80-100 °C for intermittent or continuous catalytic hydrogenation reaction.

[0038] After the catalytic hydrogenation reaction is over, the reducing solution is pumped to the catalyst filter for catalyst recovery. The filtered catalyst is carried by a small part of the red...

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Abstract

The invention discloses a method for producing aminoanisole by solvent-free catalytic hydrogenation. The method includes the steps: adding nitroanisole and catalysts into a hydrogenation reaction kettle; replacing oxygen with nitrogen in the hydrogenation reaction kettle until oxygen content is lower than or equal to 0.1%, replacing the oxygen with hydrogen until hydrogen content is higher than or equal to 99.0%, starting stirring, increasing temperature to 70+ / -10 DEG C, leading in hydrogen, controlling reaction pressure to be 0.6-1.0Mpa and performing catalytic hydrogenation reaction at the reaction temperature of 80-100 DEG C; finishing reaction, cooling filtered reduction liquid and then conveying the reduction liquid to a reduction liquid separator for automatic layering; conveying layered materials to a dewatering device for normal-pressure or negative-pressure dewatering, and conveying wastewater to a wastewater treatment device; performing negative-pressure distillation separation for the dewatered materials with water content lower than or equal to 0.1% to obtain a target product. Solvents are omitted, a solvent recovery device is omitted, the problems of environmental protection and solvent recovery of methanol solvents are fundamentally solved, equipment investment is saved, production cost is reduced, and equipment capacity is improved.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a method for producing aminoanisole by catalytic hydrogenation of nitroanisole, in particular to a method for producing aminoanisole by non-solvent catalytic hydrogenation. Background technique [0002] Aminoanisole is an important dye, spice and pharmaceutical intermediate. At present, the domestic production of o-aminoanisole and p-aminoanisole is mainly based on o-nitroanisole and p-nitroanisole as raw materials, through three production methods of sodium sulfide, sodium hydrosulfide or solvent catalytic hydrogenation reduction . Using sodium sulfide or sodium hydrosulfide to reduce, the amount of waste water is more; using solvent catalytic hydrogenation reduction process needs to add methanol as a solvent, the disadvantage of this method is that the use of solvents brings environmental pollution and solvent recovery problems, which increases the Solvent recovery costs...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C217/84B01J23/44
CPCC07C213/02B01J23/44
Inventor 于建民姚春红王苏广
Owner 连云港泰盛化工有限公司
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