Method for synthesizing o-phenylenediamine through continuous ammoniation

A technology for o-phenylenediamine and chemical synthesis, which is applied in the field of continuous ammoniated synthesis of o-phenylenediamine, can solve the problems of poor product quality and low yield of o-phenylenediamine, and achieves increased energy consumption, improved catalytic activity, excellent The effect of catalytic performance

Active Publication Date: 2022-03-08
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The synthesis of o-phenylenediamine mainly includes the following methods. Patent CN102633653 reports a method for preparing o-phenylenediamine by catalytic hydrogenation of o-nitroaniline, using o-nitroaniline as a raw material, alcohol as a solvent, and nickel as a catalyst. 1-6MPa hydrogen pressure, 40-80°C temperature, reduction reaction for 2-10 hours, rectification to obtain white o-phenylenediamine, the reaction formula is as follows, but the yield of this method is low, and Poor product quality with certain safety risks

Method used

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  • Method for synthesizing o-phenylenediamine through continuous ammoniation

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Effect test

Embodiment 1

[0022] A method for continuous ammoniation synthesis of o-phenylenediamine, comprising the steps of:

[0023] Add o-dichlorobenzene into the continuous reaction kettle disclosed in the invention patent CN201710645689.7, add liquid ammonia while stirring, raise the temperature to 85°C, control the reaction pressure to 5MPa, add the catalyst, react for 6h, after the reaction is completed, at 100°C Separate the oil phase, vacuum distill to obtain o-phenylenediamine, control the mol ratio of o-dichlorobenzene and liquefied ammonia to be 1:5, the consumption of catalyst is 1% of o-dichlorobenzene weight, the yield of o-phenylenediamine is 92.5%, with a purity of 99.1%;

[0024] The catalyst is formed by mixing cuprous chloride and a synergistic body according to a weight ratio of 3:1, and the synergistic body comprises the following steps to make:

[0025] Step S1, add benzene into a three-necked flask, add phosphorus trichloride and aluminum trichloride in turn, feed nitrogen gas...

Embodiment 2

[0029] A method for continuous ammoniation synthesis of o-phenylenediamine, comprising the steps of:

[0030] Add o-dichlorobenzene into the continuous reaction kettle disclosed in the invention patent CN201710645689.7, add liquid ammonia while stirring, raise the temperature to 85°C, control the reaction pressure to 5MPa, add the catalyst, react for 6h, after the reaction is completed, at 100°C Separate the oil phase, vacuum distill to obtain o-phenylenediamine, control the mol ratio of o-dichlorobenzene and liquefied ammonia to be 1: 6, the consumption of catalyst is 1.2% of o-dichlorobenzene weight, the yield of o-phenylenediamine is 92.8%, with a purity of 99.1%;

[0031] Described catalyst is that cuprous chloride and synergistic body are mixed according to the weight ratio of 3.5: 1, and described synergistic body comprises the following steps to make:

[0032] Step S1, add benzene into a three-necked flask, add phosphorus trichloride and aluminum trichloride in turn, f...

Embodiment 3

[0036] A method for continuous ammoniation synthesis of o-phenylenediamine, comprising the steps of:

[0037] Add o-dichlorobenzene into the continuous reaction kettle disclosed in the invention patent CN201710645689.7, add liquid ammonia while stirring, raise the temperature to 90°C, control the reaction pressure to 5.5MPa, add the catalyst, react for 6h, and after the reaction is completed, the reaction temperature is 100°C The oily phase is separated under vacuum distillation to obtain o-phenylenediamine, the mol ratio of controlling o-dichlorobenzene and liquefied ammonia is 1: 8, the consumption of catalyst is 1.4% of the weight of o-dichlorobenzene, and the yield of o-phenylenediamine 92.3% and a purity of 99.5%;

[0038] Described catalyst is that cuprous chloride and synergistic body are mixed according to the weight ratio of 4.5: 1, and described synergistic body comprises the following steps to make:

[0039] Step S1, add benzene into a three-necked flask, add phosp...

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Abstract

The invention relates to a method for synthesizing o-phenylenediamine by continuous ammoniation, which comprises the following steps: adding o-dichlorobenzene into a continuous reaction kettle, adding liquid ammonia while stirring, heating to 85-100 DEG C, controlling the reaction pressure at 5-6 MPa, adding a catalyst, reacting for 6 hours, separating out an oil phase at 100 DEG C after the reaction is finished, and carrying out vacuum distillation to obtain o-phenylenediamine, the molar ratio of the orthodichlorobenzene to the liquid ammonia is controlled to be 1: (5-10), and the dosage of the catalyst is 1-1.5% of the weight of the orthodichlorobenzene; the catalyst comprises cuprous chloride and a synergy body, the synergy body is structurally a phosphorus ligand skeleton structure and can serve as a strong power supply ligand, when the synergy body is combined with cuprous chloride, the space structure and the electronic effect of a metal center can be influenced, the catalytic activity of a catalytic system is improved, and the catalytic activity of the catalyst is improved. Therefore, the prepared catalyst has excellent catalytic performance on synthesis of o-phenylenediamine.

Description

technical field [0001] The invention belongs to the technical field of o-phenylenediamine synthesis, and in particular relates to a method for synthesizing o-phenylenediamine through continuous ammoniation. Background technique [0002] O-phenylenediamine is an important organic chemical intermediate. In addition to being used in the production of dyes, it is also the main raw material for systemic fungicides such as pesticides carbendazim, benomyl, and (methyl) thiophanate. It is also a developer , Leveling agent and surfactant, etc. are important raw materials. [0003] The synthesis of o-phenylenediamine mainly includes the following methods. Patent CN102633653 reports a method for preparing o-phenylenediamine by catalytic hydrogenation of o-nitroaniline, using o-nitroaniline as a raw material, alcohol as a solvent, and nickel as a catalyst. 1-6MPa hydrogen pressure, 40-80°C temperature, reduction reaction for 2-10 hours, rectification to obtain white o-phenylenediamine,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/10C07C211/51B01J31/18
CPCC07C209/10B01J31/188B01J2231/4283B01J2531/16C07C211/51Y02P20/584
Inventor 齐德发高彬吴双旺谢君齐永福倪盛兰
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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