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Process for preparing ortho-aminophenol by virtue of continuous catalytic hydrogenation

An o-aminophenol, catalytic hydrogenation technology, applied in the preparation of organic compounds, preparation of aminohydroxy compounds, catalysts for physical/chemical processes, etc., can solve the problems of harsh reaction conditions, poor product quality, large labor, etc. The effect of less investment, higher production costs, and less labor

Active Publication Date: 2014-04-23
宁夏德昊科技产业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the deficiencies of the prior art, the present invention provides a process for preparing o-aminophenol by continuous catalytic hydrogenation, which solves the problems of cumbersome operation, heavy labor, harsh reaction conditions, and low yield of the batch hydrogenation reduction reaction process in the prior art. Low, poor product quality, and a large amount of waste water, difficult to handle, serious environmental pollution and other issues

Method used

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  • Process for preparing ortho-aminophenol by virtue of continuous catalytic hydrogenation
  • Process for preparing ortho-aminophenol by virtue of continuous catalytic hydrogenation
  • Process for preparing ortho-aminophenol by virtue of continuous catalytic hydrogenation

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Embodiment 1

[0027] A process for preparing o-aminophenol by continuous catalytic hydrogenation, using o-nitrophenol as raw material, using Pd / Al 2 o 3 The catalyst is used for continuous catalytic hydrogenation in a fixed-bed reactor, and the target product o-aminophenol is obtained after separation and purification. Its reaction equation is:

[0028]

[0029] Specific steps include:

[0030] (1) Dissolve 1.0Kg of o-nitrophenol in 3L of ethanol-water solution with a volume fraction of 50%, preheat to 70°C, and feed continuously with a metering pump. 3 / h flow rate into the Pd / Al 2 o 3 In the fixed bed reactor of the catalyst, hydrogen gas is introduced at the same time to carry out continuous catalytic hydrogenation reduction reaction. The reaction temperature is 120°C and the reaction pressure is 1.0MPa. The reaction feed liquid enters the cooling tank and is cooled to 35°C by circulating water;

[0031] The Pd / Al 2 o 3 The mass fraction that Pd accounts for catalyst is 15% in ...

Embodiment 2

[0035] A process for preparing o-aminophenol by continuous catalytic hydrogenation, using o-nitrophenol as raw material, using Pd / Al 2 o 3 The catalyst is used for continuous catalytic hydrogenation in a fixed-bed reactor, and the target product o-aminophenol is obtained after separation and purification. Its reaction equation is:

[0036]

[0037] Specific steps include:

[0038] (1) Dissolve 1.0Kg of o-nitrophenol in 4.5L of ethanol-water solution with a volume fraction of 70%, preheat to 75°C, and feed continuously with a metering pump to 0.23m 3 / h flow rate into the Pd / Al 2 o 3 In the fixed bed reactor of the catalyst, hydrogen gas is fed at the same time to carry out continuous catalytic hydrogenation reduction reaction. The reaction temperature is 95°C and the reaction pressure is 1.5MPa. The reaction feed liquid enters the cooling tank and is cooled to 45°C by circulating water;

[0039] The Pd / Al 2 o 3 In the catalyst, the mass fraction of Pd in ​​the cataly...

Embodiment 3

[0043] A process for preparing o-aminophenol by continuous catalytic hydrogenation, using o-nitrophenol as raw material, using Pd / Al 2 o 3 The catalyst is used for continuous catalytic hydrogenation in a fixed-bed reactor, and the target product o-aminophenol is obtained after separation and purification. Its reaction equation is:

[0044]

[0045] Specific steps include:

[0046] (1) Dissolve 1Kg of o-nitrophenol in 4.5L of ethanol-water solution with a volume fraction of 85%, preheat to 80°C, and feed continuously with a metering pump. 3 / h flow rate into the Pd / Al 2 o 3 In the fixed bed reactor of the catalyst, hydrogen gas is introduced at the same time to carry out continuous catalytic hydrogenation reduction reaction. The reaction temperature is 70°C and the reaction pressure is 2.0MPa. The reaction feed liquid enters the cooling tank and is cooled to 38°C by circulating water;

[0047] The Pd / Al 2 o 3 The mass fraction that Pd accounts for catalyst is 20% in t...

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Abstract

The invention discloses a process for preparing ortho-aminophenol by virtue of continuous catalytic hydrogenation, and the process is implemented by taking o-nitrophenol as a raw material through carrying out a continuous catalytic hydrogenation reaction in a fixed bed reactor by using a Pd / Al2O3 catalyst, and then separating and purifying the obtained product so as to obtain a target product ortho-aminophenol. The process disclosed by the invention can be used for realizing a continuous catalytic hydrogenation reaction, and is short in technological process, high in degree of automation, low in labor strength, less in equipment investment, and large in production capacity; the Pd / Al2O3 catalyst is good in selectivity and high in activity, and can be used for improving the yield and purity of products, the yield reaches up to 97%, and the purity reaches up to over 99%; no material is discharged and spills over in the whole reaction process, so that the consumption is minimized, therefore, the process is beneficial to resource conservation and environmental conservation, and has good economic and social benefits; both the labor intensity of workers is reduced, and the whole site environment is clean and tidy, so that the intrinsic competitiveness and extrinsic appearance of products are promoted, and therefore, the process is suitable for being widely applied to industrial production.

Description

technical field [0001] The invention relates to a preparation process of o-aminophenol, in particular to a method using a supported catalyst Pd / Al 2 o 3 Process for preparing o-aminophenol by continuous catalytic hydrogenation. Background technique [0002] At present, Raney nickel is used as a catalyst in the industrial production of o-aminophenol to carry out batch-type hydrogenation reduction reaction to obtain o-aminophenol products. However, Raney nickel has its own shortcomings as a catalyst. The conditions for Raney nickel to act are relatively harsh, and it can only exert higher catalytic activity in an alkaline reaction system, which requires a high pH value of the solution. Otherwise, the catalyst activity will decrease. Soon, the proper catalytic effect will not be achieved, resulting in high catalyst consumption; at the same time, during the reaction process, side reactions will increase, a certain amount of solid by-products will be produced, and a large amoun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/76C07C213/02B01J23/44
Inventor 袁胜群马洪云张永猛高花杨杰赵仁花
Owner 宁夏德昊科技产业有限公司
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