Purification process for o-phenylenediamine

A technology of o-phenylenediamine and process, which is applied in the field of purification process of o-phenylenediamine, can solve the problems that the content and color number are difficult to meet high-quality requirements, and achieve the effects of reduced energy consumption, stable and reliable operation, and stable product quality

Active Publication Date: 2013-12-11
NANTONG BOTAO CHEM
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  • Description
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  • Application Information

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Problems solved by technology

[0003] In the production process of benzotriazole with o-phenylenediamine as raw material, conventional crude o-phenylenediamine is usually used for production, and the generated benzotriazole needs to be pickled, washed with water, rectified, decolorized and recrystallized, etc. More process steps can meet the requirements, otherw

Method used

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  • Purification process for o-phenylenediamine
  • Purification process for o-phenylenediamine
  • Purification process for o-phenylenediamine

Examples

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Embodiment 1

[0017] Raw material: crude o-phenylenediamine, o-phenylenediamine content of 90%, tan crystalline appearance; more than 80% of protective agent, it is an industrial product.

[0018] Pilot equipment:

[0019] 1) Rectification equipment: 3600L distillation kettle, made of 304 stainless steel; Φ600×195000mm rectification tower, packing height of 9000mm, made of 304 stainless steel;

[0020] 2) Crystallization equipment: vacuum or nitrogen protection flake machine.

[0021] The purification process of o-phenylenediamine is as follows:

[0022] 4 tons of crude o-phenylenediamine with a content of 90% pre-dissolved in the storage tank V1 are transported to the distillation column still at 120±2°C through the pump P1, and the ingredients are circulated in the thin-film evaporator E1 by the circulating pump P2 for heating. , produce gas, rise to the tower for exchange and separation through packing, the gas phase is cooled by the condenser E2 at the top of the tower to form a liqui...

Embodiment 2

[0026] The degree of vacuum in this example is 6 mmHg, the temperature of the tower still is 130° C., the protective agent is 1 g, and the rest are the same as in Example 1.

Embodiment 3

[0028] The vacuum degree in this embodiment is 10mmHg, the temperature of the tower still is 145 DEG C, and the protective agent is 0.5g, and the rest are the same as in Example 1.

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Abstract

The invention discloses a purification process for o-phenylenediamine. An o-phenylenediamine crude product is used as a raw material and an ammonolysis and reduction process of o-chloronitrobenzene is employed by the synthesis of o-phenylenediamine. The purification process comprises the steps of transporting a crude product of o-phenylenediamine to a rectification tower kettle to carry out distillation and purification. During the whole rectification process, a vacuum degree is controlled at 6-10 mmHg; and a temperature of the tower kettle is controlled at about 145 +/-3 DEG C. Finally, a proper amount of a protective agent is added in materials of a product; and the materials are flaked under the vacuum or nitrogen protection to obtain a white o-phenylenediamine finished product. The purification process is advantageous in that process is simple; operation is stable and reliable; energy consumption is low; product quality is stable; and product yield is increased.

Description

technical field [0001] The invention relates to a purification process of o-phenylenediamine and belongs to the field of fine chemical preparation. Background technique [0002] O-phenylenediamine is an important organic chemical, often used as an intermediate for dyes, pesticides, auxiliaries, photosensitive materials, etc., for the manufacture of polyamide, polyurethane, carbendazim and thiophanate, vat red GG, leveling agent, Antiaging agent MB is also used in the preparation of developers, surfactants, etc. At present, with the development of technology, the demand for high-quality o-phenylenediamine in the international and domestic markets is increasing year by year. [0003] In the production process of benzotriazole with o-phenylenediamine as raw material, conventional crude o-phenylenediamine is usually used for production, and the generated benzotriazole needs to be pickled, washed with water, rectified, decolorized and recrystallized, etc. More process steps can...

Claims

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Application Information

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IPC IPC(8): C07C211/51C07C209/84
Inventor 黄海波黄奎生王宏黄雪平
Owner NANTONG BOTAO CHEM
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