Efficient o-phenylenediamine recovery method

A technology of o-phenylenediamine and recovery method, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, chemical industry, etc., can solve problems such as high cost and high labor intensity, improve quality and yield, improve efficiency, The effect of reducing distillation bottoms

Inactive Publication Date: 2017-01-11
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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Problems solved by technology

After the material is reduced, it is crystallized and t

Method used

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Embodiment

[0016] A high-efficiency recovery method for o-phenylenediamine, which mainly includes the steps as follows: (1) add 1 weight part of o-nitroaniline and 4 weight parts of ethanol to the reactor, stir to fully dissolve the o-nitroaniline, and then add 2 parts by weight of sodium sulfide solution makes the reduction reaction of o-nitroaniline, and the temperature of the system is lowered to 80° C. after the reaction is finished; The coil is cooled, and the liquid flows into the collection tank through a U-shaped bend from the bottom of the stratified tank; (3) transfer the hydrate of o-phenylenediamine and salt at the top of the stratified tank to the heating kettle, and the material is heated to 110 °C in the heating kettle. ℃, remove the moisture therein, and collect the salt after separating out from o-phenylenediamine; (4) after collecting the salt, transfer the mixture of o-phenylenediamine and salt to the layered tank again, repeat the operation of steps 2 and 3, Until the...

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Abstract

The invention discloses an efficient o-phenylenediamine recovery method. The efficient o-phenylenediamine recovery method mainly comprises the steps that 1, an ortho-nitroaniline and sodium sulfide solution makes ortho-nitroaniline produce reduction reaction; 2, after system cooling, all the materials in the step 1 are pressed into a layering tank for primary layering; 3, an o-phenylenediamine and salt hydrate at the top of the layering tank is transferred to a heating kettle, the materials in the heating kettle are heated to remove moisture in the materials and make the salt precipitate from the o-phenylenediamine, and then collection is performed; 4, the o-phenylenediamine solution obtained after layering is collected; 5, filtration and rectification are performed, and pure o-phenylenediamine is collected and recovered for standby application. By the adoption of the method, the process including cooling, crystallization, centrifugation and heating during rectification is omitted, energy consumption is reduced, the working time is shortened, the phenomenon that a large amount of salt and water is brought to a rectification process is avoided, rectification residues are decreased, and the follow-up o-phenylenediamine rectification quality and yield are improved.

Description

technical field [0001] The invention relates to the field of environmental protection engineering, in particular to a high-efficiency recovery method of o-phenylenediamine. Background technique [0002] O-phenylenediamine is also called 1,2-diaminobenzene and 1,2-phenylenediamine. Those separated from water are white to light yellow leaf-shaped crystals, those separated from chloroform are prismatic crystals. It is easy to change color when exposed to the air, from white to yellow, brown, purple, and finally black. The relative density is 1.2698. The melting point is 103-104°C. The boiling point is 256-258°C. Slightly soluble in cold water, easily soluble in hot water, ethanol, ether, chloroform and benzene. It reacts with inorganic acid to generate water-soluble salt; reacts with carbon disulfide in aqueous solution to generate 2-mercaptobenzimidazole; reacts with carbon dioxide under pressure to generate benzimidazolone. This product is poisonous. After inhalation, i...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C209/86C07C211/51B01D3/14
CPCB01D3/14C07C209/36C07C209/86C07C211/51Y02P20/50
Inventor 朱礼华刘心龙余玉好马军
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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