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Technique for separating disperse blue 2BLN mother liquor

A separation technology and a technology for dispersing blue, applied in the field of multi-stage separation and treatment, can solve the problems of low quality, poor quality of bis-nitrophenol, low purity of by-product bis-nitrophenol, etc., so as to improve yield, reduce production cost, improve quality effect

Inactive Publication Date: 2012-10-24
ZHEJIANG QICAI ECO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method of synthesizing disperse blue 2BLN is mainly phenoxylation method and methoxylation method. No matter which method, the target product must be obtained through secondary nitration and hydrolysis reaction. Analysis by TLC plate and liquid chromatography shows that after hydrolysis Still contain the hydrolyzate of 2-3wt% in the mother liquor, and by-products such as bisnitrophenol, and hydrolyzate can not be separated completely, mix and reclaim together with the by-product in the mother liquor, cause the purity of by-product bisnitrophenol etc. High, low quality, poor quality of dinitrophenol recovery; at the same time, the hydrolyzate can not be well utilized, reducing the yield of the target product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 1000mL of the mother liquor, adjust the pH value to 5 with sulfuric acid, and control the temperature to ≤60 degrees. During the acid adjustment process, the temperature rises, and the temperature is lowered with cooling water to ensure that the hydrolysis target product is completely precipitated as much as possible. During the stirring process, the rhythm of acid addition is strictly controlled. Use filter paper to detect whether there is a precipitate, filter the precipitate, and dry to obtain 25g of hydrolyzate, accounting for 2.5wt% of the total amount, and the product purity is 93.5%; the remaining mother liquor is adjusted to PH=1 with acid, stirred and filtered to obtain the by-product bismuth The dry product of nitrophenol is 50g, and the purity is 93%.

Embodiment 2

[0015] Take 1000mL of the same hydrolysis mother liquor, the rest are the same as in Example 1, adjust the pH value to 4 with sulfuric acid, control the temperature ≤ 60 degrees, increase the temperature during the acid adjustment process, and lower the temperature with cooling water to ensure that the hydrolysis target product is completely separated out as much as possible. In the process, strictly control the rhythm of acid addition, filter the precipitate, and dry to obtain 27g of hydrolyzate, accounting for 2.7wt% of the total, with a product purity of 92%. The mother liquor is collected and adjusted to PH=2 with acid, stirred and filtered to obtain the by-product bisnitrate The dry product of base phenol is 53g, the purity is 93.5%.

Embodiment 3

[0016] Example 3: Take 1000 mL of the same hydrolysis mother liquor, the rest are the same as in Example 1, adjust the pH value to 5.5 with sulfuric acid, control the temperature ≤ 60 degrees, increase the temperature during the acid adjustment process, and use cooling water to lower the temperature to ensure that the hydrolysis target product is as complete as possible Precipitate, during the stirring process, strictly control the rhythm of adding acid, filter the precipitate, and get 29g of hydrolyzate after drying, accounting for 2.9wt% of the total, the product purity is 92.5%, the collected mother liquor is adjusted to PH=1.5 with acid, stirred and filtered, 52 g of the by-product bis-nitrophenol was obtained in dry form, with a purity of 93.7%.

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Abstract

The invention discloses a technique for separating a disperse blue 2BLN mother liquor, belonging to the technical field of a multi-stage separation process of organic compound production. The technique comprises the following steps: controlling the pH value of the mother liquor between 10-14; regulating the pH value of the mother liquor between 4-6 by using H2SO4, controlling the temperature between 10-60 DEG C, stirring and filtering, and collecting precipitates as a target product; when no precipitate generates in the mother liquor, regulating the pH value of the mother liquor between 1-3 by using H2SO4, and stirring to obtain a byproduct. According to the invention, by carrying out secondary purification on the mother liquor, the purity of the target product can reach more than 80-92%, the recovery rate is 2-5wt%; and the purity of the byproduct dinitrophenol can reach more than 90%, thus the yield of the target product is raised, the quality of the hydrolyzed byproduct is raised, and the production cost is reduced.

Description

technical field [0001] The invention relates to a disperse blue 2BLN mother liquid separation technology, which belongs to the technical field of multistage separation and treatment of organic compound production. Background technique [0002] Disperse Blue 2BLN is a main color dye with a wide range of uses. It has excellent light fastness, sublimation fastness, good covering and level dyeing properties, and good compatibility. The traditional method of synthesizing disperse blue 2BLN is mainly phenoxylation method and methoxylation method. No matter which method, the target product must be obtained through secondary nitration and hydrolysis reaction. Analysis by TLC plate and liquid chromatography shows that after hydrolysis Still contain the hydrolyzate of 2-3wt% in the mother liquor, and by-products such as bisnitrophenol, and hydrolyzate can not be separated completely, mix and reclaim together with the by-product in the mother liquor, cause the purity of by-product bisn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/50C07C201/16C07C205/23
Inventor 胡启木李学坤
Owner ZHEJIANG QICAI ECO TECH CO LTD
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