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Preparation method of organic cobalt complex

A technology of complexes and organic cobalt, which is applied in the direction of organic dyes, chemical instruments and methods, azo dyes, etc., can solve the problems of high labor intensity, complicated process, dust pollution, etc., and achieve the effect of reducing energy consumption

Active Publication Date: 2018-12-14
JINHUA SHUANGHONG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] 2) Diazotization and coupling reactions require a temperature of 0-5°C, which needs to be controlled by adding ice, which not only increases energy consumption but also increases the amount of wastewater generated
[0019] In this method, if it is carried out at a room temperature of 10-30°C, the speed of the diazonium salt decomposition reaction will increase and more impurities will be produced.
[0020] 3) During the manufacturing process, salting out once and filtering twice are required. For each ton of product produced, about 10-15 tons of high-salt, high-COD wastewater is produced, which is very difficult to treat and has extremely high environmental risks
[0021] 4) In the manufacturing process, the process is complicated, the number of material transfers is high, the energy consumption is high, the labor intensity is high, the material loss is serious, and the production site management is difficult
[0022] 5) In the process of product standardization, it is necessary to carry out crushing, blending additives, and unloading packaging of blending machines, resulting in serious dust pollution

Method used

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  • Preparation method of organic cobalt complex
  • Preparation method of organic cobalt complex
  • Preparation method of organic cobalt complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] Embodiment 1, a kind of preparation method of organic cobalt complex compound, carry out following steps successively:

[0090] 1), add 3000L water to the reaction kettle, then add 30% (mass%) hydrochloric acid 3.5kmol (about 426kg); slowly add 3.0kmol (564kg) of compound II under stirring, and the feeding time is 1 hour (to ensure that compound II is dissolved) , and then add 30% (mass%) sodium nitrite aqueous solution 715kg (containing sodium nitrite 3.12kmol) within 10 minutes, after adding, stir and react for 1 hour under the condition of 20~30°C, and add an appropriate amount of sulfamic acid , destroy excess sodium nitrite (the addition is based on the iodine-starch test paper no longer showing blue); obtain the acidic solution of compound III;

[0091] Compound II is 3-amino-4-hydroxybenzenesulfonamide, and its chemical structural formula is:

[0092]

[0093] Compound III is benzoxazole-5-sulfonamide, and its chemical structural formula is:

[0094]

[0...

Embodiment 2

[0107] Embodiment 2, a kind of preparation method of organic cobalt complex, carries out following steps successively:

[0108] 1), add 3000L water in the reactor, then add 401.5kg (3.3kmol) of 30% hydrochloric acid; slowly drop in 925kg (3.0kmol) compound II under stirring, and the feeding time is about 1 hour; then add 30% hydrochloric acid in 10 minutes Sodium nitrate aqueous solution 715kg (containing sodium nitrite 3.12kmol), after adding, stir and react at 20-30°C for 1 hour, add an appropriate amount of sulfamic acid to destroy excess sodium nitrite (the amount added is based on iodine-starch test paper Show blue again); Obtain the acidic solution of compound III;

[0109] Compound II is 2-(3-amino-4-hydroxyphenylsulfonamido)benzoic acid, the chemical structural formula is:

[0110]

[0111] Compound III is 2-(benzoxazole-5-sulfonamido)benzoic acid, the chemical structural formula is:

[0112]

[0113] 2), in the dissolution kettle, add 2000L of water, then add ...

Embodiment 3

[0123] Embodiment 3, a kind of preparation method of organic cobalt complex, carries out following steps successively:

[0124] 1) Add 3000L of water to the reactor, then add 3.53kmol (about 430kg) of 30% hydrochloric acid; slowly add 3.0kmol (606.1kg) of compound II under stirring, and the feeding time is about 1 hour, and then add 30% hydrochloric acid within 10 minutes Sodium nitrite aqueous solution 715kg (containing 3.12kmol sodium nitrite), after adding, stir and react at 20-30°C for 1 hour, then add appropriate amount of sulfamic acid to destroy excess sodium nitrite Show blue prevail); Obtain the acidic solution of compound III;

[0125] Compound II is 3-amino-4-hydroxyl-N-methylbenzenesulfonamide, the chemical structural formula is:

[0126]

[0127] Compound III is N-methylbenzoxazole-5-sulfonamide, and its chemical structural formula is:

[0128]

[0129] 2), in the dissolution kettle, add 2000L of water, then add 400kg of 30% sodium hydroxide aqueous soluti...

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Abstract

The invention discloses a preparation method of an organic cobalt complex. The preparation method comprises the following steps: 1) in an acidic aqueous solution, mixing and then reacting a compound II and sodium nitrite, and adding sulfamic acid until the rest sodium nitrite is reacted completely; 2) adding a compound IV into an alkaline aqueous solution to prepare a compound IV aqueous solution,slowly adding the compound IV aqueous solution into the product obtained in step 1), and performing coupling reaction at 10-40 DEG C for 2-3 hours; and 3) heating the obtained product, adding a cobalt salt, and performing complexation reaction at 50-95 DEG C for 2.5-4 hours, wherein the obtained reaction solution contains an organic cobalt complex. The organic cobalt complex prepared by the method provided by the invention has the technical advantages of reducing material consumption, shortening process flow and having a remarkable environmental protection effect.

Description

technical field [0001] The invention relates to a method for producing an organic cobalt complex. Background technique [0002] The organic cobalt complex according to the present invention can be used as a dye. The dye is a cobalt complex with an azo structure. Existing this type of azo dye synthesis will go through the following steps: [0003] 1), the diazonium component is subjected to diazotization reaction with sodium nitrite under acidic conditions to make a diazonium salt solution or suspension; [0004] 2), in addition, the coupling component is made into a solution under alkaline conditions; then the diazonium salt solution is added to the alkaline solution of the coupling component to perform a coupling reaction to obtain an azo compound, and the filter cake of the azo compound is obtained by filtration ; [0005] 3), the obtained azo compound filter cake is made into slurry with water, and cobalt complexation is carried out with cobalt sulfate or cobalt chlor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B57/10
CPCC09B57/10C09B68/28
Inventor 徐建成肖刚
Owner JINHUA SHUANGHONG CHEM CO LTD
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