Method and device for preparing 1-aminoanthraquinone

A technology of aminoanthraquinone and nitroanthraquinone, applied in chemical instruments and methods, preparation of organic compounds, chemical/physical/physicochemical fixed reactors, etc. Increased investment and other issues to achieve the effect of reduced equipment investment, stable product quality, and investment savings

Inactive Publication Date: 2009-02-25
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] 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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  • Method and device for preparing 1-aminoanthraquinone
  • Method and device for preparing 1-aminoanthraquinone

Examples

Experimental program
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Embodiment 1

[0024] See attached figure 1 , the reaction device of the present invention comprises a metering tank 1 of 1-nitroanthraquinone, a metering tank 2 of a catalyst, a metering tank 3 of liquefied ammonia, a pipeline reactor 17 with a coil 18, a premixer 13, and a heater 16 is connected with pipeline reactor 17, and this heater 16 can select oil bath heater; Premixer 13 is connected with booster pump 24, and 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 premixer 13 through pipeline 7; S...

Embodiment 2

[0028] The reaction device is as in Example 1. In metering tank 1, be the n-hexane solution (mass percentage concentration 40%) of 1-nitroanthraquinone, in metering tank 2, be the triethylamine solution (mass percentage concentration 1%) of ammonium bromide, in metering tank 3, be liquid ammonia. Adjust the flow ratio in the three metering tanks = 3.7:1:0.37 into the pipeline, control the reaction temperature at 150°C, the pressure at 10MPa, and maintain a material flow rate of about 0.3ml / s. The residence time of the ammonolysis reaction is about 20 minutes, and the rest of the operations are the same Example 1, the 1-aminoanthraquinone product was obtained with a yield of about 52%.

Embodiment 3

[0030]The reaction device is as in Example 1. In metering tank 1, be the xylene solution (mass percentage concentration 40%) of 1-nitroanthraquinone, be the n-octanol solution (mass percentage concentration 1%) of trimethylammonium bromide in metering tank 2, metering tank 3 Inside is liquid ammonia. Adjust the flow ratio in the three metering tanks = 5:1:0.6 into the pipeline, control the reaction temperature at 175°C, the pressure at 12MPa, and maintain a material flow rate of about 0.1ml / s. The ammonolysis reaction residence time is about 60 minutes, and the rest of the operations are the same Example 1. The 1-aminoanthraquinone product was obtained with a yield of 72%.

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Abstract

The invention discloses a manufacturing method of 1-amino anthraquinone, which comprises the following steps: premixing 1-nitro anthraquinone, liquid ammonia and 0.25-0.5% catalyst corresponding to the weight of 1-nitro anthraquinone into premixer; loading into pipe-typed reactor with coiler to do ammonolytic reaction; setting the weight rate of liquid ammonia and 1-nitro anthraquinone at 0.27-0.67:1; selecting catalyst from halogenated inorganic amino salt or halogenated alkyl organic amino salt; setting ammonolytic temperature at 150-200 deg.c under 10-15Mpa.

Description

technical field [0001] The invention relates to a method and device for synthesizing aromatic organic amines, in particular to a high-pressure pipeline synthesis method and device for chemical intermediate 1-aminoanthraquinone. Background technique [0002] Anthraquinone dyes are the second largest category of dyes next to azo dyes, and 1-aminoanthraquinone is an important intermediate for the synthesis of anthraquinone dyes. , The main raw material of pyrazole anthraquinone occupies an extremely important position in the dye industry. With the increasing demand for 1-aminoanthraquinone, it is said that the output of 1-aminoanthraquinone reached 2,500 tons in 1991, and the current domestic demand alone has exceeded 4,000 tons. The output of low-quality 1-aminoanthraquinone in the domestic market has exceeded the demand, while the output of high-quality is far from meeting the needs of export. In recent years, due to the "three wastes", the production of anthraquinone-based...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C221/00C07C225/34B01J19/24
Inventor 陈新志高建荣钱超毛筱媛
Owner ZHEJIANG UNIV OF TECH
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