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Production method of acidic blue dye containing active groups

A technology of blue dyes and reactive groups, applied in the production field of acid blue dyes containing reactive groups, can solve the problems of easy deterioration and loss of products, high cost of sewage treatment, high labor intensity, etc., and can reduce the content of wastewater. Generate, simplify the production process, reduce the effect of labor

Active Publication Date: 2013-09-04
杭州下沙恒升化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process has a long operation process, relatively high operation requirements, high labor intensity, and the product is easy to deteriorate and lose
At the same time, the process will produce two-step wastewater. According to statistics, for every 1 ton of standard product produced, 7 tons of diluted filtrate wastewater will be produced; 5 tons of condensation neutralization wastewater will contain 20% NaCl and a large number of organic compounds in the wastewater, with an average COD=5500mg / L or so, the cost of sewage treatment is relatively high
At the same time, in the drying standardization process, dust pollution is also a serious environmental problem

Method used

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  • Production method of acidic blue dye containing active groups
  • Production method of acidic blue dye containing active groups
  • Production method of acidic blue dye containing active groups

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A method for producing an acid blue dye containing active groups, the structure of the compound is shown in the following formula (I): , where R is -CH 3 ,

[0025] Including the following process steps: a condensation reaction step and a neutralization reaction step,

[0026] Condensation reaction steps: put 900kg of sulfuric acid with a concentration of 98% into the condensation reactor, add 250kg of the original powder of formula (Ⅴ) and keep stirring for 1 hour, cool down to 20~25°C, add 116kg of compound of formula (Ⅲ), keep stirring for 5 hours , to obtain the compound of formula (Ⅳ), after the end point is reached, dilute it into 3500kg of ice water, the dilution temperature will be less than 10°C, after dilution, stir it evenly and press filter to obtain a filter cake, and the filtrate is recycled to the treatment kettle;

[0027] Neutralization reaction steps: put 2000kg of ice water into the neutralization reaction kettle, add the filter cake, adjust the te...

Embodiment 2

[0029] A method for producing an acid blue dye containing active groups, the structure of the compound is shown in the following formula (I): , where R is -CH 2 Br,

[0030] Including the following process steps: a condensation reaction step and a neutralization reaction step,

[0031] Condensation reaction steps: put 1200kg of sulfuric acid with a concentration of 95% into the condensation reactor, add 250kg of the original powder of formula (Ⅴ) and keep stirring for 1 hour, cool down to 20~25°C, add 125kg of compound of formula (Ⅲ), keep stirring for 4 hours , to obtain the compound of formula (Ⅳ), after the end point is reached, dilute it into 4000kg of ice water, the dilution temperature will be less than 8°C, after dilution, stir it evenly for a while and press filter to obtain a filter cake, and the filtrate is recycled to the treatment kettle;

[0032] Neutralization reaction steps: put 2000kg of ice water into the neutralization reaction kettle, add the filter cake,...

Embodiment 3

[0034] A method for producing an acid blue dye containing active groups, the structure of the compound is shown in the following formula (I): , where R is -C 6 h 5 ,

[0035] Including the following process steps: a condensation reaction step and a neutralization reaction step,

[0036] Condensation reaction steps: put 1600kg of sulfuric acid with a concentration of 90% into the condensation reactor, add 250kg of the original powder of formula (Ⅴ) and keep stirring for 1 hour, cool down to 20~25°C, add 135kg of compound of formula (Ⅲ), keep stirring for 3 hours , to obtain the compound of formula (Ⅳ), after the end point is reached, dilute it into 4500kg of ice water, the dilution temperature will be less than 5°C, after dilution, stir evenly for a while and press filter to obtain a filter cake, and the filtrate is recycled to the treatment kettle;

[0037] Neutralization reaction steps: put 2000kg of ice water into the neutralization reaction kettle, add the filter cake, ...

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Abstract

The invention discloses a production method of an acidic blue dye containing active groups. The production method is characterized by comprising the following technological steps: a condensation reaction step and a neutralization step, wherein the condensation reaction step contains the following steps: pouring sulfuric acid into a condensation reaction vessel, adding Formula (II) and Formula (III) into sulfuric acid, cooling to 20-25 DEG C, carrying out thermal insulation and stirring for 3-5h so as to obtain a compound as shown in the formula (IV), diluting in ice water at the dilution temperature of less than 10 DEG C, uniformly stirring after dilution, carrying out press filtration to obtain a filter cake, recovering a filtrate into a processing kettle; and the neutralization step contains the following steps: pouring ice water into a neutralization reaction vessel, adding the filter cake obtained from the above condensation reaction step, adjusting the temperature to 5-30 DEG C, adjusting pH to 3.5-9 by adding alkali lye, transferring to a transfer kettle, carrying out wet product standardization, and carrying out spray drying so as to obtain a finished product as shown in the formula (I). The production method provided by the invention has the following advantages: one filtering process is omitted; production of wastewater with high salinity is minimized; production technology is simplified; and production cost is reduced.

Description

technical field [0001] The invention relates to a production method of acid blue dye containing active groups. Background technique [0002] In the prior art, the following process is used for the production of Chinese formula (I) in dyes: Formula (Ⅴ) is dissolved in sulfuric acid and undergoes condensation reaction with formula (Ⅲ). After the end point of condensation is reached, it is diluted into ice water, filtered, washed and filtered The filter cake is beaten, neutralized with mixed lye to obtain the target compound, and then subjected to salting-out filtration, oven-dried, crushed and standardized to obtain the corresponding dye product. The technological process has long operating procedures, relatively high operating requirements, high labor intensity, and easy deterioration and loss of products. At the same time, the process will produce two-step wastewater. According to statistics, for every 1 ton of standard product produced, 7 tons of diluted filtrate wastewate...

Claims

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Application Information

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IPC IPC(8): C09B1/34
Inventor 邢国章吴志彤刘世刚唐安定
Owner 杭州下沙恒升化工有限公司
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