New tower type oxidation technology for indigo blue

A kind of indigo and tower technology, applied in the field of high-efficiency synthesis of indigo, can solve the problems of uneven gas distribution, easy foaming reaction time, large washing loss, etc.

Active Publication Date: 2014-11-26
JIANGSU TAIFENG CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing kettle reaction model has the problems of uneven gas distribution, low air utilization rate, easy foaming, long reaction time, incomplete reaction, large adsorption and wrapping of raw materials and alkali by the product, resulting in large washing loss, and the concentration of oxidized dilute alkali It can only reach about 12%. Concentrating into solid alkali needs to consume a lot of heat and configure evaporation equipment with a large processing capacity. Increasing the concentration of alkali will lead to more incomplete reaction and worse product yield and purity. It is necessary to solve the indigo oxidation process The above-mentioned engineering problems must consider new high-efficiency mass transfer equipment. We have successfully developed a high-efficiency and energy-saving tower loop reactor (patent number: 200810173635.6). It has shown very good results in chemical reactions, and this kind of reactor combined with high-efficiency mass transfer tower equipment on a macro level and enhanced intermolecular dispersion on a micro level is the biggest highlight of the present invention

Method used

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  • New tower type oxidation technology for indigo blue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The ultrasonic generator used in this experiment has a frequency of 25KHz and a power of 100W.

[0018] After adding 200g of alkali melt into 800g of water to dissolve (the temperature is 71.6°C), transfer the material to an airlift reactor, turn on the ultrasonic wave, and feed air into the reactor to keep the temperature of the material in the reactor at 68-72 ℃, reacted for 3 hours, reached the end of the reaction, filtered and washed the reaction material, and obtained the indigo product. In the filtrate, the filter value of indigo is 3.0g / L, the content of carbonate is 13.2g / L, the alkalinity is 15%, the content of indigo after drying is 95.6%, the moisture is 0.40%, and the iron ion is 86ppm.

Embodiment 2

[0020] The ultrasonic generator used in this experiment has a frequency of 25KHz and a power of 100W.

[0021] After adding 200g of alkali melt into 800g of experiment 1's alkali water (alkali concentration is 15%) and dissolving (alkali concentration is 25%, temperature is 75.6°C), the material is transferred to the air-lift reactor, and the ultrasound is turned on. Air is introduced into the reactor, the temperature of the materials in the reactor is kept at 68-72° C., and the pressure is 0.15 Mp. The reaction is carried out for 5 hours until the end of the reaction is reached. After the reaction materials are filtered and washed, the indigo product is obtained. In the filtrate, the filter value of indigo is 5.4g / L, the content of carbonate is 21.3g / L, the alkalinity is 36%, the content of indigo after drying is 95.1%, the moisture is 0.38%, and the iron ion is 114ppm.

Embodiment 3

[0023] The ultrasonic generator used in this experiment has a frequency of 25KHz and a power of 100W.

[0024] After adding 400g of alkali melt into 800g of water for dissolution (the alkali concentration is 25%, and the temperature is 80.6°C), the material is transferred to the air-lift reactor, the ultrasonic is turned on, and air is introduced into the reactor to keep the reactor inside The temperature of the material is 68-72° C., the pressure is 0.15 Mp, and the reaction is carried out for 6 hours until the end of the reaction is reached. After the reaction material is filtered and washed, the indigo product is obtained. In the filtrate, the filter value of indigo is 4.8g / L, the content of carbonate is 18.2g / L, the alkalinity is 38%, the content of indigo after drying is 95.3%, the moisture is 0.42%, and the iron ion is 109ppm.

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Abstract

The present invention relates to a new technology for direct oxidation of a 3-indoxyl salt into indigo blue in a novel efficient ultrasonic circulation type reactor by using air or oxygen-containing gas. According to the present invention, the new technology and the new equipment are combined, such that concentration of the existing oxide material can be substantially increased, yield and purity of the reaction can be ensured well, significant effects of energy saving and consumption reduction are provided, and indigo production with characteristics of large scale, continuality and automation can be achieved.

Description

technical field [0001] The invention relates to a new technology for high-efficiency synthesis of indigo under the condition of high alkali concentration by using a new tower reactor instead of the traditional tank reactor for indigo. Scale-up, serialization and automation. Background technique [0002] Indigo is a vat dye that is widely used in the coloring of cellulose textiles such as cotton and linen, especially in the light yarn dyeing of indigo denim products. [0003] At present, most factories prepare indigo through the oxidation of 3-indoxyl salt, which includes the reaction of aniline acetate, sodium amide, and a mixed alkali of sodium hydroxide and potassium hydroxide at 220-250°C to obtain 24-30% of indigo The alkali melt of 3-indoxyl salt, put the alkali melt into water to form a solution containing 5% of 3-indoxyl salt and about 12% of mixed alkali, at 30m 3 Air bubbling in the oxidation kettle oxidizes for 2 hours, and then undergoes pressure filtration, wat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B7/02
Inventor 尹应武张正西喻宏贵吴德生栾敏红赖永华朱建董泽高
Owner JIANGSU TAIFENG CHEM
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