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Method for synthesizing 1-chloroanthraquinone through direct chlorination of chlorine gas

A technology of chloranthraquinone and chlorine gas, applied in chemical instruments and methods, preparation of organic compounds, preparation of quinones, etc., can solve the problems of high reaction temperature, simplify the operation process, reduce waste water discharge, and improve the level of green dye production technology Effect

Inactive Publication Date: 2010-10-20
HEFEI UNIV OF TECH
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Problems solved by technology

[0004] The present invention aims at the defect of high reaction temperature for synthesizing 1-chloroanthraquinone by the existing direct chlorination method, and aims to provide a new synthesis method for generating 1-chloroanthraquinone by direct chlorination of chlorine gas, and the technical problem to be solved is to reduce the reaction temperature And realize continuous safe production

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  • Method for synthesizing 1-chloroanthraquinone through direct chlorination of chlorine gas

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Embodiment Construction

[0027] Now taking the sieve tray tower as an example, non-limiting examples are described as follows:

[0028] Add the composite chlorination initiator (azoisobutyronitrile: triphenylphosphine=1: 1w / w) of 0.2% azoisobutyrocyanide and triphenylphosphine to the 1- In nitroanthraquinone, heating to 170°C makes it melt into a light brown liquid with low viscosity. Add dropwise from the upper part of the sieve plate type chlorination reaction tower to a reaction tower with a length of 2000mm and a diameter of 100mm, which is provided with ten layers of sieve plates, and the rate of dropping is 3kg / h. The sieve plate acts as a distributor to fully disperse the liquid 1-nitroanthraquinone. At the same time, the chlorination reagent composed of chlorine and nitrogen (chlorine: nitrogen = 70:30v / v) is introduced from the bottom of the tower and distributed through the sieve plate. After fully dispersed, the rate of feeding is 120L / h, chlorine gas and 1-nitroanthraquinone are chlorinat...

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Abstract

The invention relates to a method for synthesizing 1-chloroanthraquinone through direct chlorination of chlorine gas, which uses 1-chloroanthraquinone as raw materials and comprises the steps of chlorination and separation. The invention is characterized in that the chlorination is carried out in a reverse flow type in a reaction tower with a built-in distributor, i.e. fused materials are added into the tower from the top of the tower, chlorination reagents are introduced from the bottom of the tower, two phases of the reverse flow are mutually and uniformly dispersed under the effect of the distributor, and the chlorination process is completed at 150 to 170 DEG C. The materials are prepared from adding fluxing agents accounting for 8 to 12 mass percent of the raw materials and composite triggering agents accounting for 0.1 to 0.3 mass percent of the raw materials into the raw materials of 1-chloroanthraquinone, wherein the composite triggering agents are prepared from free radical triggering agents and organic phosphine compounds through being mixed according to a mass ratio of 1 / 1. In the method, the free radical chloro reaction is stably carried out at a temperature lower than 170 DEG C under the effect of the fluxing agents and the composite triggering agents, the content of coarse products is about 90 percent, and high-purity 1-chloroanthraquinone with the content higher than or equal to 99 percent can be obtained through two-step purification of sulfogroup conversation and recrystallization.

Description

1. Technical field [0001] The invention relates to a synthesis method of a dye intermediate, in particular to a method for directly chlorinating and synthesizing 1-chloroanthraquinone with chlorine gas. 2. Background technology [0002] Dyestuffs are indispensable fine chemicals in modern society, but their production and use have always been accompanied by major environmental pollution problems for a long time. Research and development of green technologies in the dye production process, design, manufacture and application of new production equipment and It is of great economic and social significance to carry out industrial production and application, reduce the consumption of raw materials and energy, reduce the discharge of three wastes and the difficulty of treatment, realize the production of clean technology, and achieve the goal of energy saving and emission reduction, and it is also a very urgent task. Halogenated anthraquinone is an important and key intermediate o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/24C07C46/00C07C46/10
Inventor 冯乙巳杨春燕张博叶加久许华建
Owner HEFEI UNIV OF TECH
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