Process and apparatus for producing o-phenylenediamine

A technology of o-phenylenediamine and o-dichlorobenzene, which is applied in the field of synthesis of aromatic organic amines, can solve problems such as small equipment production capacity, hidden safety hazards, and increased equipment investment, and achieve stable product quality, easy control of reaction conditions, The effect of saving investment

Active Publication Date: 2005-03-16
江西扬帆新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The kettle-type ammonolysis process is relatively mature, but the defects are: first, intermittent reaction, long operation time, and small equipment production capacity; The corrosion of the equipment is extremely serious, the investment in the equipment increases, and there are potential safety hazards; third, the long-term high-temperature reaction has an adverse effect on the color of the product, especially the color of the dye intermediate, which has a more serious impact on the color

Method used

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  • Process and apparatus for producing o-phenylenediamine
  • Process and apparatus for producing o-phenylenediamine
  • Process and apparatus for producing o-phenylenediamine

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0025] Embodiment 1: A kind of reaction device, comprises the metering tank 1 that provides o-dichlorobenzene, the metering tank 2 that mainly provides catalyst, the metering tank 3 that provides liquefied ammonia, the pipeline reactor 17 that sets coil 18 inside, premixer Device 13, heater 16 links to each other with pipeline reactor 17, this heater 16 can select oil bath heater; Premixer 13 links to each other with booster pump 24, booster pump 24 can keep the pressure in the premixer 13 as required pressure. In order to facilitate the observation of the raw materials in the tank, the measuring tank 1 and the measuring tank 2 are designed as measuring tanks made of glass; the measuring tank 3 containing liquid ammonia is made of stainless steel, and the surface of the measuring tank 3 is provided with a glass liquid level gauge. The outlet of metering tank 1 is provided with high-pressure metering pump 4, and high-pressure metering pump 4 is connected to the inlet end of pre...

Embodiment 2

[0028] Embodiment 2: The reaction device is the same as in Embodiment 1. Adding concentration is 15% dilute ammonia water in metering tank 2, and this dilute ammonia water contains 0.979% cuprous chloride and 0.979% tetrabutylammonium bromide. Adjust the flow ratio of o-dichlorobenzene:dilute ammonia water:liquid ammonia=1.5:1:3.3 into the pipeline, and the outlet pressures of high-pressure metering pumps 4, 5, and 6 are all set to 15Mpa. (the weight ratio of actual cuprous chloride and liquefied ammonia is 0.5%: 1 now; The weight ratio of liquefied ammonia and o-dichlorobenzene is 1.076: 1.) Control the ammonolysis reaction temperature 150 ℃ in coil pipe 18, the pressure 15Mpa, keep the material flow rate of about 0.3ml / second, the calculated value of the ammonolysis reaction residence time is 19.625 minutes, all the other production methods are the same as in Example 1, and the o-phenylenediamine product with similar properties is obtained, and the yield is about 56%.

Embodiment 3

[0029]Embodiment 3: The reaction device is the same as in Embodiment 1. Adding concentration is 5% dilute ammonia water in metering tank 2, and this dilute ammonia water contains 1% cuprous chloride and 1% tetrabutylammonium bromide. Adjust the flow ratio of dichlorobenzene:dilute ammonia water:liquid ammonia=2:1:5 to enter the pipeline, and the outlet pressure of high-pressure metering pumps 4, 5, and 6 are all set to 16Mpa. (At this moment, the weight ratio of actual cuprous chloride and liquid ammonia is 0.38%: 1, and the weight ratio of liquid ammonia and o-dichlorobenzene is 1.223: 1.) Control reaction temperature 175 ℃, pressure 16Mpa, keep about 0.1ml / Second material flow rate, the ammonolysis reaction residence time calculated value is 58.88 minutes, and all the other production methods are with embodiment 1. The o-phenylenediamine product with similar properties was obtained with a yield of 68%.

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Abstract

The invention provides a process for producing o-phenylendiamine comprising the steps of, charging ortho dichlorobenzene, ammonia into high temperature, high pressure container, proceeding ammonolysis reaction at the presence of catalyst, analyzing and separating the obtained reactant, charging ortho dichlorobenzene, liquid ammonia, copper catalyst, phase shift catalyst into pipe type reactor continuously for ammonolysis reaction. The invention also discloses a production apparatus for realizing the method.

Description

Technical field: [0001] The invention relates to a synthesis method and device of an aromatic organic amine, in particular to a high-pressure pipeline synthesis method and device of a chemical intermediate - o-phenylenediamine. 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, phenoxyl, and (methyl) thiophanate. At present, there are many routes for the synthesis of o-dichlorobenzene, and three of the more important routes are as follows: [0003] 1. Literature Rev.Chim., 1976, 27(5): 394~401, using o-nitrochlorobenzene as starting material, through ammoniation and reduction to obtain o-phenylenediamine product, the reaction formula is as follows: [0004] [0005] The process route is mature, and the total yield of the two steps is about 64%. The ammoniation reaction of the first step...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/10C07C211/51
Inventor 陈新志钱超
Owner 江西扬帆新材料有限公司
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