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Method for separating and purifying nicotinic acid from 3-cyanopyridine wastewater

A technology of cyanopyridine and nicotinic acid, which is applied in the field of chemical intermediate waste treatment, to achieve the effects of environmental protection, simple process and short process flow

Pending Publication Date: 2020-12-25
ANHUI RUIBANG BIOLOGICAL SCI & TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses biotransformation method to prepare nicotinic acid, obtains high-purity nicotinic acid mother liquor for extraction and separation, and is not suitable for treating multi-impurity wastewater

Method used

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  • Method for separating and purifying nicotinic acid from 3-cyanopyridine wastewater
  • Method for separating and purifying nicotinic acid from 3-cyanopyridine wastewater
  • Method for separating and purifying nicotinic acid from 3-cyanopyridine wastewater

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Resin activation: Soak in analytical pure methanol for 4 to 12 hours, treat with 4% (g / 100mL) NaOH solution, and wash with water;

[0033] (2) Waste water pretreatment: get 4kg waste water and add the active carbon decolorization filtration of waste water quality 3%;

[0034] (3) Adsorption on the column: the waste water in step (2) is adsorbed on the column with macroporous ion exchange resin Haipu HP334, and the flow rate is controlled at 1BV / hr;

[0035] (4) Analysis: use hot water at a temperature of 70°C for analysis, with a flow rate of 2BV / hr, to obtain a niacin analysis solution, and sample T0;

[0036] (5) Resin regeneration: After the analysis is finished, feed 3 times of column volume methanol, control flow rate 0.5BV / hr; Wash with water to pH7.0±0.5, control flow rate 1BV / hr;

[0037] (6) Concentrated crystallization: Concentrate the niacin analysis solution in step (4) by 20 times, add 3% activated carbon of the concentrated solution for decolorizatio...

Embodiment 2

[0042] (1) Resin activation: Soak in methanol for 4 to 12 hours, treat with 4% (g / 100mL) NaOH solution, and wash with water;

[0043] (2) Waste water pretreatment: get 4.0kg waste water and add activated carbon decolorization filtration of waste water quality 4%;

[0044] (3) Adsorption on the column: the waste water in step (2) is adsorbed on the column with macroporous ion exchange resin Haipu HP334, and the flow rate is controlled at 1BV / hr;

[0045] (4) Analysis: use hot water at a temperature of 75°C for analysis, with a flow rate of 2BV / hr, to obtain a niacin analysis solution, and sample T0;

[0046] (5) Resin regeneration: After the analysis is finished, feed 3 times column volume methanol solution, control flow rate 1BV / hr; Wash with water to pH7.0±0.5, control flow rate 2BV / hr;

[0047] (6) Concentrated crystallization: Concentrate the niacin analysis solution in step (4) by 15 times, add 4% activated carbon to the concentrated solution for decolorization, and then...

Embodiment 3

[0052] (1) Resin activation: Soak in methanol for 4 to 12 hours, treat with 4% (g / 100mL) NaOH solution, and wash with water;

[0053] (2) Wastewater pretreatment: get 4.0kg waste water and add 5% activated carbon of waste water quality to decolorize and filter;

[0054] (3) Adsorption on the column: the waste water in step (2) is adsorbed on the column with macroporous ion exchange resin Haipu HP334, and the flow rate is controlled at 1BV / hr;

[0055] (4) Analysis: use hot water at a temperature of 80°C for analysis, with a flow rate of 2BV / hr, to obtain a niacin analysis solution, and sample T0;

[0056] (5) Resin regeneration: after the analysis is finished, feed 3 times column volume methanol solution, control flow rate 1BV / hr; Wash with water to pH7.0±0.5, control flow rate 1BV / hr;

[0057] (6) Concentrated crystallization: Concentrate the niacin analysis solution in step (4) by 10 times, add 5% activated carbon of the concentrated solution for decolorization, and then p...

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Abstract

The invention discloses a method for separating and purifying nicotinic acid from 3-cyanopyridine wastewater, which comprises the steps of (1) soaking resin in methanol for 4-12h, treating with a 4% NaOH solution, and cleaning with water; (2) adding activated carbon accounting for 3-5% of the mass of the wastewater to decolorize and filter; (3) adsorbing the wastewater in the step (2) on a column;(4) after the adsorption is finished, desorbing by using hot water with the temperature of 7080 DEG C to obtain a nicotinic acid analytic solution ; (5) introducing a methanol solution of which the volume is 3 times that of the column, introducing a NaOH solution of which the volume is 3 times that of the column, and washing with pure water until the pH value is 7.0+ / -0.5; (6) concentrating the nicotinic acid analytic solution obtained in the step (4) by 10-20 times, adding activated carbon accounting for 3--5% of the mass of the concentrated solution for decoloration, and performing acidification crystallization to obtain a crude product, recovering crystallization mother liquor, and performing column chromatography crystallization according to the step (3) to obtain a crude product; and(7) adding the nicotinic acid crude product obtained in the step (6) into absolute ethyl alcohol, heating for dissolving, adding activated carbon accounting for 3-5% of the mass of the nicotinic acidethanol solution for decoloration, cooling the filtrate to the temperature of 15-25 DEG C, controlling the temperature for crystallization, and drying to obtain a nicotinic acid finished product.

Description

technical field [0001] The invention relates to the technical field of three-waste treatment of chemical intermediates, in particular to a method for separating and purifying nicotinic acid from 3-cyanopyridine wastewater. Background technique [0002] 3-cyanopyridine, also known as nicotinonitrile, has a molecular formula of C6H4N2 and a molecular weight of 104.11. It is a white crystal. Can be sublimated, soluble in ethanol, ether, chloroform, benzene and petroleum ether, slightly soluble in water. The main use is as an intermediate for medicine, food additives, feed additives, pesticides, etc. The wastewater from 3-cyanopyridine production often contains nicotinic acid, nicotinamide, etc. How to improve the recovery rate and purity of extracting nicotinic acid from 3-cyanopyridine wastewater has been studied by those skilled in the art. [0003] The Chinese patent application with application number CN2011101226069 discloses a method for treating waste water produced in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/80
CPCC07D213/80
Inventor 董亢谷顺明袁晓路李玉山
Owner ANHUI RUIBANG BIOLOGICAL SCI & TECH CO LTD
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