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Novel preparation method of o-phenylenediamine

A technology of o-phenylenediamine and o-nitroaniline, which is applied in the chemical industry, can solve the problems of complicated preparation process, poor product quality, and complicated components, and achieve the effect of convenient and simple preparation, easy operation, and simple components

Inactive Publication Date: 2014-10-08
ANHUI HUARUN PAINTS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The three wastes in this method are serious, the product quality is poor, and the yield is low. At the same time, the traditional p-aminophenol has complex components and complicated preparation process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] An o-phenylenediamine consisting of starting materials by weight of,

[0021] o-nitroaniline 70g

[0022] 150ml ethanol or methanol

[0023] Raney Nickel 1 g.

[0024] A preparation method of o-phenylenediamine, comprising the following processing steps,

[0025] a. Add 70g of o-nitroaniline, 150ml of methanol or ethanol, and 1g of Raney nickel into the reaction kettle;

[0026] b. Close the reactor and check the airtightness.

[0027] c. Replace the air in the autoclave with 0.3MP nitrogen for 3 times, and then replace the nitrogen in the autoclave with 0.3MP hydrogen for 3 times;

[0028] d. Pressurize the hydrogen in the autoclave to 1.5MP, start stirring and heating, and raise the temperature to 65°C to keep the autoclave at a constant temperature for 120 minutes.

[0029] e. When the hydrogen pressure in the autoclave no longer drops, stop the reaction, cool down to 85°C and start discharging, depressurizing, and filtering to obtain the finished product.

Embodiment 2

[0031] An o-phenylenediamine consisting of starting materials by weight of,

[0032] o-Nitroaniline 80g

[0033] 170ml ethanol or methanol

[0034] Raney Nickel 2 g.

[0035] A preparation method of o-phenylenediamine, comprising the following processing steps,

[0036] a. Add 80g of o-nitroaniline, 170ml of methanol or ethanol, and 2g of Raney nickel into the autoclave;

[0037] b. Close the autoclave and check the airtightness.

[0038] c. Replace the air in the autoclave with 0.3MP nitrogen for 3 times, and then replace the nitrogen in the autoclave with 0.3MP hydrogen for 3 times;

[0039] d. Pressurize the hydrogen in the autoclave to 1.5MP, start stirring and heating, and the temperature rises to 65°C to keep the constant temperature in the autoclave for 120 minutes.

[0040] e. When the hydrogen pressure in the autoclave no longer drops, stop the reaction, cool down to 85°C and start discharging, depressurizing, and filtering to obtain the finished product.

Embodiment 3

[0042] An o-phenylenediamine consisting of starting materials by weight of,

[0043] o-Nitroaniline 75g

[0044] 160ml ethanol or methanol

[0045] Raney nickel 1.5 g.

[0046] A preparation method of o-phenylenediamine, comprising the following processing steps,

[0047] a. Add 75g of o-nitroaniline, 160ml of methanol or ethanol, and 1.5g of Raney nickel into the autoclave;

[0048] b. Close the autoclave and check the airtightness.

[0049] c. Replace the air in the autoclave with 0.3MP nitrogen for 3 times, and then replace the nitrogen in the autoclave with 0.3MP hydrogen for 3 times;

[0050] d. Pressurize the hydrogen in the autoclave to 1.5MP, start stirring and heating, and raise the temperature to 65°C to keep the autoclave at a constant temperature for 120 minutes.

[0051] e. When the hydrogen pressure in the autoclave no longer drops, stop the reaction, cool down to 85°C and start discharging, depressurizing, and filtering to obtain the finished product.

[0...

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PUM

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Abstract

A preparation method of o-phenylenediamine. The invention relates to the technical field of chemical engineering. The method includes following steps: employing 70-80g of o-nitroaniline, 150-170ml of alcohol or methanol and 1-2g of a catalyst as raw materials; feeding the raw materials into a reaction kettle; closing the reaction kettle and inspecting an air-tightness of the reaction kettle; replacing air in the reaction kettle by nitrogen under 0.3 MPa for three times; replacing the nitrogen in the reaction kettle by hydrogen under 0.3 MPa for three times; increasing the pressure of the hydrogen in the reaction kettle to 1.5 MPa; carrying out a stirring process with a heating process; increasing the temperature in the reaction kettle to 65 DEG C; maintaining the temperature to be constant for 120 min; stopping the reaction when the pressure of the hydrogen in the reaction is not decreased anymore; decreasing the temperature to 85 DEG C; carrying out a material-discharging process, a pressure-decreasing process and a filtering process to obtain a finish product. The method is simple in components of the raw materials, is cheap in raw materials, is convenient and easy to carry out and is convenient to operate. The prepared o-phenylenediamine is good in usage effects and is safe and reliable.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a novel preparation method of o-phenylenediamine. Background technique [0002] O-phenylenediamine is an intermediate of dyes, pesticides, auxiliaries, photosensitive materials, etc. It is a dye fur yellow brown M, which is used to manufacture polyamide, polyurethane, fungicides carbendazim and thiophanate, reduced red GG, homogeneous Dyeing agent and anti-aging agent MB are also used in the preparation of developer, surfactant, etc., and the preparation process of o-nitroaniline by reduction of iron powder or alkali sulfide is currently the main process in China. The three wastes in this method are serious, the product quality is poor, and the yield is on the low side. Meanwhile, the traditional p-aminophenol has complex components and complicated preparation process. Contents of the invention [0003] The technical problem to be solved by the present invention i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/51C07C209/36
Inventor 张学永陆建新靳民张广生
Owner ANHUI HUARUN PAINTS
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