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A blue dye, cation technology, applied in the field of preparation of cation blue dye, can solve the problems of high COD, high chroma, environmental threats and so on
Active Publication Date: 2020-01-24
HENAN CHEM IND RES INST +1
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During the production of conventional cationic blue series dyes, a large amount of wastewater with h
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Embodiment 1
[0141] (1) Preparation of 4-(dimethylamino)benzenediazonium chloride
[0142] Add 1mol of N,N-dimethylaniline and 400mL of 37% concentrated hydrochloric acid into a 1L three-necked flask, drop 200mL of aqueous solution of 1.04mol of sodium nitrite into the reaction solution, and keep the dropping temperature at (- 5°C)-0°C, react at 0°C-5°C for 2 hours, after the reaction, filter with suction and dry to obtain N,N-dimethyl-4-nitrosoaniline.
[0143] Add 1mol of N,N-dimethyl-4-nitrosoaniline, 600mL of water and 600mL of 37% concentrated hydrochloric acid into a 2L three-necked flask, add 2.6mol of zinc powder into the reaction solution, and keep the reaction The temperature was 20°C-25°C for 4 hours. After the reaction, 4 mol of sodium hydroxide was added to adjust the pH to 7-8, filtered by suction, and dried to obtain N,N-dimethyl-p-phenylenediamine.
[0144] Add 1mol of N,N-dimethyl-p-phenylenediamine and 400mL of 37% concentrated hydrochloric acid into a 1L three-neck flas...
Embodiment 2
[0152] (1) Preparation of 4-(diethylamino)benzenediazonium chloride
[0153] Add 1mol of N,N-diethylaniline and 400mL of 37% concentrated hydrochloric acid into a 1L three-necked flask, add 1.04mol of sodium nitrite in 200mL of aqueous solution dropwise into the reaction solution, and keep the dropping temperature at (- 5°C)-0°C, react at 0°C-5°C for 2 hours, after the reaction, filter with suction and dry to obtain N,N-diethyl-4-nitrosoaniline.
[0154] Add 1mol of N,N-diethyl-4-nitrosoaniline, 600mL of water and 600mL of 37% concentrated hydrochloric acid into a 2L three-necked flask, add 2.6mol of zinc powder into the reaction solution, and keep the reaction The temperature was 20°C-25°C for 4 hours. After the reaction, 4 mol of sodium hydroxide was added to adjust the pH to 7-8, suction filtered, and dried to obtain N,N-diethyl-p-phenylenediamine.
[0155]
[0156]Add 1mol of N,N-diethyl-p-phenylenediamine and 400mL of 37% concentrated hydrochloric acid into a 1L three...
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Abstract
The invention belongs to the technical field of dyes, and particularly relates to a preparation method of a cationic blue dye. According to the invention, a compound II is used as a diazonium component and a compound I is used as a coupling component for synthesizing the cationic blue dye for the first time; and the method has the advantages of simple process, environmental friendliness, high product purity, high yield and the like. The results of multiple production experiments with scales not below pilot tests show that mother liquor (such as mother liquor in steps 2, 3 and 4) in the reaction process can be cyclically used 6-8 times without treatment, so the amount of high-salt, high-COD and high-chroma wastewater is greatly reduced, a working environment is effectively improved while product yield is further increased and reaction reagent cost is saved, and the product still keeps high purity; and thus, product quality is guaranteed, production cost is reduced, and obvious economicbenefits, social benefits and environmental benefits are produced.
Description
technical field [0001] The invention belongs to the technical field of dyes, and in particular relates to a preparation method of cationic blue dyes. Background technique [0002] Cationic blue is a typical representative of conjugated cationic dyes. It has the advantages of strong tinting strength and high light fastness. Its chromophore conjugate has azo bonds, aromatic rings and nitrogen-containing heterocycles. During the production of conventional cationic blue dyes, a large amount of waste water with high COD, high chroma and high salt will be produced, which poses a serious threat to the environment. In order to solve these common key technical problems, it is necessary to develop a new preparation process for cationic blue dyes, which can greatly reduce the amount of wastewater generated, realize energy-saving and environmentally friendly innovative production processes for cationic blue dyes, and promote the technological upgrading and sustainable development of the...
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