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Electrolytic synthesis method of 2-pyridinecarboxylic acid

A picolinic acid, electrolytic synthesis technology, applied in electrolytic process, electrolytic components, electrolytic organic production and other directions, can solve the problems of large environmental pollution, poor economic benefits, low product yield, etc., and achieves less generation of three wastes and low raw material cost. , the effect of high purity

Inactive Publication Date: 2012-04-11
ZHEJIANG AVILIVE CHEM CO LTD
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  • Abstract
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Problems solved by technology

[0004] The purpose of this invention is to provide a kind of polychloride with 2-pyridine carboxylic acid or the polychloride salt of 2-pyridine carboxylic acid as the production method of raw material electrolytic synthesis 2-pyridine carboxylic acid, to solve the product collection problem that exists in the existing production method Low production rate, large environmental pollution, poor economic benefits and other problems, so as to realize the improvement of product yield, reduce the discharge of three wastes, easy industrial production, and environmentally friendly green synthesis process

Method used

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  • Electrolytic synthesis method of 2-pyridinecarboxylic acid
  • Electrolytic synthesis method of 2-pyridinecarboxylic acid
  • Electrolytic synthesis method of 2-pyridinecarboxylic acid

Examples

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Embodiment 1

[0039] 1. Ingredients

[0040] (1) Alkali preparation: put 1125L pure water into the preparation kettle; turn on the stirring paddle, then add 375 kg of sodium hydroxide at a uniform speed, dissolve completely, and prepare 25% lye; turn on the cooling circulating water to make the lye temperature When the temperature is lowered to 25-30°C, turn on the preparation liquid pump and send the lye to the lye metering tank for standby.

[0041](2) Initial electrolytic material preparation: put 3600L pure water into the preparation kettle, start stirring, then add 400 kg of 25% lye from the lye metering tank, and stir evenly; then add 103 kg of 2-pyridinecarboxylic acid at a uniform speed Chlorides (6-chloro-2-pyridinecarboxylic acid 18 wt%, 3,6-dichloro-2-pyridinecarboxylic acid 70 wt%, 3,5,6-trichloro-2-pyridinecarboxylic acid 9 wt%, 3,4, 5,6-tetrachloro-2-pyridinecarboxylic acid 3 wt %), stop stirring after completely dissolving, turn on the preparation solution pump, and send it ...

Embodiment 2-5

[0053] The operation process is the same as in Example 1, and the polychloride component (wt%) of 2-pyridinecarboxylic acid is changed into:

[0054]

Embodiment 6-7

[0056] Operation process is identical with embodiment 1, and extraction solvent changes into:

[0057]

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Abstract

The invention relates to the field of compound synthesis, in particular to an electrolytic synthesis method of 2-pyridinecarboxylic acid. The method comprises the following steps: taking a polychloride or polychloride salt of 2-pyridinecarboxylic acid as the raw material to carry out electroreduction at 20-80 DEG C in an alkaline solution with pH value being 8.5-13.4, then adding acid in the electrolyte to neutralize until the pH value is 3-4, vaporizing to remove moisture, then extracting the obtained solid with a solvent and vaporizing out the solvent to obtain an 2-pyridinecarboxylic acid crystal product. The method has the following advantages: the method has the characteristics of low raw material cost, simple and practicable production process control, low yield of three wastes and environment friendliness; and the HPLC (high performance liquid chromatography) purity of the 2-pyridinecarboxylic acid product is not less than 99.5% and the total yield is not less than 85%.

Description

technical field [0001] The invention relates to the field of compound synthesis, in particular to an electrolytic synthesis method for intermediate 2-picolinic acid used for preparing carbocaine medicine and neurological medicine. Background technique [0002] 2-Pyridinecarboxylic acid is an important intermediate in organic synthesis. It is used in the pharmaceutical industry to prepare carbocaine drugs and neurological drugs. It is widely used in nerve suppression and local anesthesia; An essential raw material for formate, among which chromium 2-picolinate is an important health care medicine for human beings, widely used in chromium supplements for human body, feed additives, treatment of diabetes, etc.; 2-picolinate can also be used for the preparation of herbicides. [0003] The existing methods for synthesizing 2-pyridinecarboxylic acid mainly include chemical oxidation, air catalytic oxidation and 2-cyanopyridine hydrolysis. The chemical oxidation method uses 2-pico...

Claims

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Application Information

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IPC IPC(8): C25B3/04C07D213/79C25B3/25
Inventor 金克强李惠跃孙云雷吴洪星徐庄委
Owner ZHEJIANG AVILIVE CHEM CO LTD
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