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Industrialized preparation method of copper 2-picolinate

A technology of copper picolinate and picolinic acid, which is applied in the direction of organic chemistry, can solve the problem of no copper 2-picolinate, etc., and achieve the effects of good product quality, high yield, and short reaction cycle

Inactive Publication Date: 2015-11-04
SICHUAN BIOTECH FORCE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, there is no copper 2-picolinate product on the market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 123.5kg of 2-pyridinecarboxylic acid into a 1000L reactor, add 175kg of water, heat up to 90°C and stir to dissolve; after the 2-pyridinecarboxylic acid is fully dissolved, the temperature drops to 72°C, adjust to PH=6.4 with liquid caustic soda, and then stir 1.5h; Add 125kg of copper sulfate pentahydrate in batches, once every 15 minutes, 25kg each time. After the addition, react at 94°C for 2.5h; cool down to room temperature, centrifuge, and dry at 90°C to obtain 144.61kg of copper 2-picolinate, which is a blue crystalline powder, the content of copper 2-picolinate is ≧99.27%, and the yield is 94.11%.

Embodiment 2

[0025] Add 247kg of 2-pyridinecarboxylic acid into a 2000L reactor, add 350kg of water, heat up to 90°C and stir to dissolve; after the 2-pyridinecarboxylic acid is fully dissolved, the temperature drops to 78°C, adjust to PH = 6 with liquid caustic, and then stir for 1.5 h; Add 250kg of copper sulfate pentahydrate in batches, once every 15 minutes, 50kg each time. After the addition, react at 98°C for 1.7h; cool down to room temperature, centrifuge, and dry at 90°C to obtain 288.73kg of copper 2-picolinate, which is a blue crystalline powder, the content of copper 2-picolinate is ≧99.64%, and the yield is 94.31%.

Embodiment 3

[0027] Add 494kg of 2-pyridinecarboxylic acid into a 4000L reactor, add 600kg of water, heat up to 90°C and stir to dissolve; after the 2-pyridinecarboxylic acid is fully dissolved, the temperature drops to 76°C, adjust to PH=6.5 with liquid caustic soda, and then stir for 2 hours ;Add 500kg of copper sulfate pentahydrate in batches, once every 15 minutes, 100kg each time. After the addition, react at 96°C for 3h; cool down to room temperature, centrifuge, and dry at 90°C to obtain 577.24kg of copper 2-picolinate, which is a blue crystalline powder, the content of copper 2-picolinate is ≧99.28%, and the yield is 94.07 %.

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Abstract

The invention discloses an industrialized preparation method of 2-copper picolinate. The method comprises the following steps: (1) charging and warming: adding 123.5-494kg of 2-picolinic acid into a 2000L reaction kettle, adding 175-600kg of water, and warming to 90 DEG C to stir and dissolve; (2) dissolving, cooling, adjusting pH and stirring: after fully dissolving 2-picolinic acid, cooling to 70-78 DEG C, adjusting the pH to 6-7 by liquid caustic soda, and then stirring for 1-2 hours; (3) a reaction step: adding 125-500kg of copper sulfate pentahydrate, and reacting for 1.7-3 hours at 90-98 DEG C; and (4) product separation: cooling to room temperature, centrifugalizing and drying at 90 DEG C to obtain 2-copper picolinate blue powder. Compared with the prior art, the industrialized preparation method of 2-copper picolinate protected by the invention is simple in synthetic line, safe and reliable in process, short in reaction period, high in yield, good in product quality and free from pollutants.

Description

technical field [0001] The invention relates to an industrialized preparation method of copper 2-picolinate. Background technique [0002] 2-Pyridinecarboxylic acid has special physiological activity, belongs to organic formic acid, and is also a very important biological ligand. The molecule contains carboxyl and heterocycle groups that can coordinate with different metals. 2-Pyridinecarboxylic acid and its derivatives It is an intermediate of many kinds of drugs, and is widely used in medicine, agriculture and daily chemicals. Copper is an essential trace element for life, which is ubiquitous in animals and plants and plays an important role in the process of life. Copper ions have always been an important ion for the synthesis of complexes due to their good coordination ability and structural diversity. Selecting ligands with biological functions to synthesize new copper complexes is of great importance to biology, inorganic chemistry, medicine, feed industry and applica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/803
CPCC07D213/803
Inventor 竹文坤
Owner SICHUAN BIOTECH FORCE TECH