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Method for continuous preparation of C.I. acid orange 10 in micro-channel

An acid orange, micro-channel technology, applied in chemical instruments and methods, azo dyes, organic dyes, etc., to achieve the effects of strong corrosiveness, simple production process and short production cycle

Inactive Publication Date: 2015-09-09
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Therefore, on the basis of the basic coupling of traditional aniline diazonium salt and G salt as raw materials, with the help of the advantages of micro-reaction technology, the production technology of C.I. acid orange 10 prepared by continuous coupling in the microchannel reactor can be effectively improved. The quality includes the stability of intensity and color, simplification of process, improvement of selectivity, reduction of cost and reduction of pollutant emissions, but no similar reports have been seen so far

Method used

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  • Method for continuous preparation of C.I. acid orange 10 in micro-channel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 0.005 mol of aniline and 0.29 mol of 37.5% hydrochloric acid in water to prepare 10 mL of a mixed solution with a final aniline concentration of 0.5 mol / L, as feed solution A; dissolve 0.005 mol of sodium nitrite in water to form a final concentration of 0.5 mol of sodium nitrite / L mixed solution 10 mL, as the feed liquid B; slowly add the feed liquid B to the feed liquid A, and control the temperature of the reaction liquid at 0-5°C during the feeding process to prevent the temperature from rising suddenly. Stir and react in a conventional reactor for 30 minutes under normal conditions to obtain 20 mL of aniline diazonium salt feed solution C; take 1.75 g (0.005 mol) of G salt and dissolve it in baking soda solution to prepare a 20 mL feed solution with a final concentration of 0.25 mol / L D; Feed liquid C and feed liquid D are sent to the microchannel reactor 4 by the calibrated syringe pump (model LSP01-1A, manufacturer: Baoding Lange Constant Flow Pump Co., ...

Embodiment 2

[0032] Feed liquid A, feed liquid B are the same as embodiment 1; Feed liquid C and feed liquid D are injected into the microchannel reactor by a certain flow rate and reacted respectively, and process parameters such as flow rate, reaction temperature, residence time, internal diameter are shown in Table 2, Collect the effluent liquid E to obtain C.I. Acid Orange 10. Use a UV ultraviolet detector to detect the absorbance Abs value at the position of the maximum absorption peak wavelength 475nm, and compare it with the standard working curve of C.I. Acid Orange 10 c=(12.42*Abs+0.158)*10 -5 The one-way yield measured by mol / L was 87.5-94.0%, as shown in Table 2 for details.

[0033] The impact of each process condition of table 2 on reaction

[0034]

[0035] It can be concluded from the data in Table 2 that the process conditions set in Example 1 are optimal process conditions.

[0036] Comparative example 1 (preparation of C.I. acid orange 10 by conventional batch reactio...

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Abstract

The invention relates to a method for continuous preparation of C.I. acid orange 10 in a micro-channel. The method comprises the steps: a material liquid A prepared by dissolving phenylamine and concentrated hydrochloric acid in water is subjected to a diazotization reaction with a sodium nitrite aqueous solution, and a material liquid C containing phenylamine diazonium salt is obtained; the material liquid C and a sodium bicarbonate aqueous solution of G salt are sent into a micro-channel reactor by an injection pump and are subjected to a coupling reaction, and after posttreatment, the C.I. acid orange 10 is obtained. With adopting of the micro-channel reactor, the reaction time is shortened, the reaction efficiency and the product quality are improved, and the product selectivity is greatly improved; the reaction system has no amplifying effect, and can be amplified by multiple times through parallel connection; moreover, the method has the advantages of stability of the continuous reaction, simple and convenient operation, short production cycle, cheap and easily obtained raw materials, simple production process and the like, and is suitable for industrialized production; and the micro-channel reactor is made of a polytetrafluoroethylene material, thereby having the advantages of simple preparation, good solvent resistance, strong corrosion resistance and the like, and being conducive to industrial application.

Description

technical field [0001] The invention relates to a method for continuously preparing C.I. acid orange 10 in a microchannel. Background technique [0002] C.I. Acid Orange 10 is a monoazoic acid dye with low directness and good level dyeing property. It is mainly used for dyeing and printing of wool, silk and nylon blended fabrics. The diazo coupling process developed so far is all batch production, which has the disadvantages of poor product quality stability (differences in intensity and color between different batches), low yield, and many wastes. Therefore, by optimizing the synthesis process of C.I. Acid Orange 10, increasing the yield, obtaining products with stable quality and reducing the three wastes in the production process of the product will greatly promote the production and application of the product. [0003] As a new enhanced reaction technology, micro-reaction technology is to replace the traditional batch reactor with a micro-channel reactor based on contin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/16
Inventor 高建荣朱博也孙岩峰许萌叶青余武斌郑明明陈文忠
Owner ZHEJIANG UNIV OF TECH
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