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Method for treating and reclaiming waste water of 2-aminopyridine production

An aminopyridine, a technology for producing wastewater, which is applied in water/sewage treatment, natural water treatment, chemical instruments and methods, etc., and can solve the problems of waste of resources, strong corrosiveness and high toxicity of wastewater

Inactive Publication Date: 2008-08-06
YANCHENG TEACHERS UNIV
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Problems solved by technology

The wastewater is highly corrosive and toxic. In addition to 2-aminopyridine and other organic substances that are not easy to decompose, there are remaining reactants and some by-products. If it is directly discharged, it will not only waste resources, but also cause serious pollution to the environment.

Method used

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  • Method for treating and reclaiming waste water of 2-aminopyridine production
  • Method for treating and reclaiming waste water of 2-aminopyridine production
  • Method for treating and reclaiming waste water of 2-aminopyridine production

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Embodiment Construction

[0019] 1. Oil separation: The waste water produced by the hydrolysis reaction is separated from the organic layer through the oil separation tank, and the 2-aminopyridine is recovered by vacuum distillation, and the residue is incinerated.

[0020] 2. Neutralization: the water layer was adjusted to a pH close to neutral with dilute sulfuric acid, crystallized by cooling, and filtered under reduced pressure. The obtained crude product is purified by recrystallization method, and the inorganic salt is recovered. The filtrate is light yellow, pH 7-8, density 1.26, color 50 times, COD Cr About 3600mg / L.

[0021] 3. Resin pretreatment: Accurately weigh 2.000g of NDA-150 ultra-high cross-linked adsorption resin, place it in a small measuring cylinder, soak it in methanol for 2 hours, read the volume (BV) of the wet resin, pour out the methanol, and wash it with pure water until No alcohol smell, transfer the resin to the exchange column to drive away the air bubbles in the resin l...

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Abstract

The invention provides a treatment and recovery method of 2-aminopyridine production waste water, comprising separating organic layer from waste water via an oil separation pool, depressurizing, distilling and recovering 2-aminopyridine, adjusting pH of aqueous layer via a diluted acid until neutral, cooling, crystallizing, depressurizing, extracting and filtering to obtain crude salt, purifying and recovering inorganic salt via recrystallization, using adsorption column stuffed with high-crosslinked adsorption resin to absorb and remove organics, collecting effluent to be used for hydrolysis or be discharged via biochemical treatment, eluting the adsorption resin via sodium-hydroxide-alcohol solution to be regenerated via methanol to be repeatedly used, neutralizing and combining the desorption solution and organic layer, distilling to recover 2-aminopyridine. The treatment and recovery method of 2-aminopyridine production waste water has the advantages of improved waste water treatment effect and recovered useful material in waste water, thereby reducing pollution, saving cost and combining waste water treatment and resource recovery.

Description

Technical field [0001] The invention relates to a method for treating and recovering waste water from the production of 2-aminopyridine, the main intermediate of synthetic antipyretic and analgesic and non-steroidal anti-inflammatory and analgesic piroxicam (alias: piroxicam). Background technique [0002] At present, the synthesis process route of 2-aminopyridine is usually: take pyridine as raw material, and prepare 2-aminopyridine through nucleophilic substitution reaction-amination method. Specifically, sodium amide is prepared by reacting metal sodium with liquid ammonia, and pyridine and sodium amide are refluxed in toluene or xylene for amination reaction, and the main product is 2-aminopyridine. The specific production process is as follows: [0003] The first step: production of sodium amide [0004] <chemistry num="0001"> <chem file="200710199586_CML001.XML" / > < / chemistry> [0005] Step 2: Amination [0006] [0007] Step 3: Hydrolysis ...

Claims

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Application Information

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IPC IPC(8): C07D213/73C07C31/04C02F1/28C02F1/58C02F103/36
Inventor 唐树和吕文林王京平王兴隆陈香许海燕
Owner YANCHENG TEACHERS UNIV
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