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Method for preparing direct yellow G

A freezing and direct technology, applied in etherification preparation and other directions, can solve the problems of lack of competitiveness, difficult governance, and increased production costs, and achieve the effect of reducing production costs, large market competitiveness, and achieving zero emissions.

Active Publication Date: 2011-05-04
平顶山市铭源化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Adopt said method to have following shortcoming: 1, every ton of directly frozen yellow G will produce 15 tons of industrial waste water, these industrial waste waters are difficult to manage, and can take away a part of direct frozen yellow G finished product, thereby increased the cost of production; 2. The dissolution, salting-out and acid-out of DSD acid in the process will use a large amount of auxiliary materials such as industrial salt and sulfuric acid. These auxiliary materials will not only increase the cost of production, but also increase the difficulty of industrial wastewater treatment; 3. The final direct production Frozen yellow G has high salt content, low color strength, low color brightness, low solubility, low color fastness and color rate, and the product lacks competitiveness in the market

Method used

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  • Method for preparing direct yellow G
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Effect test

Embodiment 1

[0030] The preparation method of the direct frozen yellow G of the present embodiment, the steps are as follows:

[0031] 1) Add 2400L of ethanol, 400kg of DSD acid, and 500kg of hydrochloric acid to the diazo reaction tank at one time to maintain the acidic environment of the diazo reaction, stir and beat for 2 hours, control the temperature at 20°C, and add dropwise a solution containing 152kg of sodium nitrite Alcohol solution can also be used, the purpose is to allow sodium nitrite to be better mixed with the beating liquid, the present embodiment adopts 190kg of water and 165kg of ethanol to prepare the above-mentioned sodium nitrite solution, and the total time of dropping is 40 minutes , control the temperature at 20°C and continue the reaction for 0.5 hours. During the diazotization process, the appearance of the solution will change from light yellow to yellow-brown, and the material will also change from thick to thin; at the end of the reaction, there is a slight exc...

Embodiment 2

[0037] The preparation method of the direct frozen yellow G of the present embodiment, the steps are as follows:

[0038] 1) Add 3000L of ethanol, 400kg of DSD acid, and 500kg of hydrochloric acid to the diazo reaction tank at one time to maintain the acidic environment of the diazo reaction, stir and beat for 2 hours, control the temperature at 25°C, and add dropwise a solution containing 152kg of sodium nitrite Alcohol solution can also be used, and the purpose is to allow sodium nitrite to be better mixed with the beating liquid. In this embodiment, 190kg of water and 165kg of ethanol are used to prepare the above-mentioned sodium nitrite solution, and the total time for dropping is 50 minutes. , control the temperature at 25°C and continue the reaction for 0.8 hours. During the diazotization process, the appearance of the solution will change from light yellow to yellowish brown. Destroy excess sodium nitrite to obtain a diazonium salt solution containing intermediate 1 of...

Embodiment 3

[0044] The preparation method of the direct frozen yellow G of the present embodiment, the steps are as follows:

[0045]1) Add 3600L of ethanol, 400kg of DSD acid, and 500kg of hydrochloric acid to the diazo reaction tank at one time to maintain the acidic environment of the diazo reaction, stir and beat for 2 hours, control the temperature at 30°C, and add dropwise a solution containing 152kg of sodium nitrite Alcohol solution can also be used, the purpose is to allow sodium nitrite to better mix evenly with the beating liquid, the present embodiment adopts 190kg of water and 165kg of ethanol to prepare the above-mentioned sodium nitrite solution, and the total time of dropping is 60 minutes , control the temperature at 30°C and continue the reaction for 1 hour. During the diazotization process, the appearance of the solution will change from light yellow to yellow-brown. Destroy excess sodium nitrite to obtain a diazonium salt solution containing intermediate 1 of formula 1...

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Abstract

The invention discloses a method for preparing direct yellow G. DSD acid is taken as an initial raw material, and the method comprises the following steps of: reacting with sodium nitrite, phenol and chloroethane in turn, and respectively performing diazotization, coupling and chloroethane etherification to obtain the direct yellow G, wherein a solvent in diazotization, coupling and chloroethane etherification is ethanol. The DSD acid is taken as the initial raw material and is subjected to diazotization, coupling and chloroethane etherification respectively to form a dye of the direct yellow G, the ethanol is adopted as a reaction solvent in the diazotization, coupling and chloroethane etherification and can be recycled after reaction, a large amount of water is prevented from serving as the reaction solvent, the problem that a large amount of industrial wastewater is difficult to treat is radically solved and the zero emission of the industrial wastewater is achieved.

Description

technical field [0001] The invention relates to an anhydrous preparation method of directly frozen yellow G, which belongs to the technical field of chemical synthesis. Background technique [0002] Direct Frozen Yellow G is a kind of direct dye, which can be directly dissolved in water and has high directness to cellulose fiber. It does not need to use dyes related to chemical methods to color fibers and other materials. Direct dyes can be used in weak acid or neutral It can be used to color protein fibers (such as wool and silk) in the solution, and it can also be used for dyeing cotton, linen, rayon and rayon. The chromatogram is complete, the price is low, and the operation is convenient. [0003] At present, the process flow of the usual preparation method of direct frozen yellow G is as follows: [0004] 1. DSD acid diazotization: [0005] Add water to the diazo tank, add DSD acid with stirring, heat up to 60°C and mix with soda ash to dissolve it completely (pH=8),...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B43/28
Inventor 刘晨义员海峡师阿丽
Owner 平顶山市铭源化工有限公司
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