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Synthesis method of 2-chromium picolinate

A kind of technology of chromium picolinate and synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of high price of potassium permanganate, low yield per pass, many side reactions, etc., and achieves good product quality, high reaction yield, synthesis Simple route effect

Active Publication Date: 2009-12-16
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Potassium permanganate is more expensive
Product one-way yield is also low, and side reactions are many

Method used

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  • Synthesis method of 2-chromium picolinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Synthetic aqueous solution of 2-pyridinecarboxylic acid:

[0019] In a 200ml three-necked flask, add 40g of deionized water, then add 20g of 2-cyanopyridine, start stirring, heat up to 70°C, add 26g of 30% sodium hydroxide in the flask, after the addition, Continue to raise the temperature, keep the reaction at 70°C for 6 hours, then cool to 30°C, add 30% hydrochloric acid, adjust the pH value of the reaction solution at 5.5, and maintain the temperature of the reaction solution at 50°C for use;

[0020] (2) Complexation reaction:

[0021] Add the prepared 20% chromium trichloride aqueous solution dropwise in the above 200ml three-necked flask, the amount of dropwise addition is 51.8g, after the addition, stir the complexation reaction for 1 hour, then cool to 20°C, and discharge, After draining, the filter cake was washed with 100 g of ion-free water for 4 times, then filtered and dried to obtain about 26.53 g of chromium 2-picolinate, with a yield of 99.0%. The q...

Embodiment 2

[0023] (1) Synthetic aqueous solution of 2-pyridinecarboxylic acid:

[0024] In a 200ml three-necked flask, add 40g of deionized water, then add 20g of 2-cyanopyridine, start stirring, heat up to 70°C, add 26g of 30% sodium hydroxide in the flask, after the addition, Continue to heat up, keep the temperature at 70°C for 6 hours, then cool to 30°C, add 30% hydrochloric acid, adjust the pH value of the reaction solution to 4.5, and maintain the temperature of the reaction solution at 50°C for use;

[0025] (2) Complexation reaction:

[0026] Add the prepared 20% chromium trichloride aqueous solution dropwise in the above 200ml three-necked flask, the amount of dropwise addition is 51.8g, after the addition, stir the complexation reaction for 1 hour, then cool to 20°C, and discharge, After draining, the filter cake was washed with 200g of ion-free water for 4 times, then filtered and dried to obtain about 26.20g of chromium 2-picolinate, with a yield of 97.8%. The quality index ...

Embodiment 3

[0028] (1) Synthetic aqueous solution of 2-pyridinecarboxylic acid:

[0029] In a 200ml three-necked flask, add 40g of deionized water, then add 20g of 2-cyanopyridine, start stirring, heat up to 50°C, add 30g of 30% sodium hydroxide in the flask, after the addition, Continue to heat up, keep the temperature at 60°C for 10 hours, then cool to 30°C, add 30% hydrochloric acid, adjust the pH value of the reaction solution to 5.5, and wait for the temperature of the reaction solution to drop to 45°C before use;

[0030] (2) Complexation reaction:

[0031] Add the prepared 20% chromium trichloride aqueous solution dropwise in the above 200ml three-necked flask, the amount of dropwise addition is 53.8g, and then stir the complexation reaction for 1 hour after adding, then cool to 20°C, and discharge, After draining, the filter cake was washed with 200 g of ion-free water for 4 times, then filtered and dried to obtain about 26.40 g of chromium 2-picolinate, with a yield of 98.5%. Th...

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Abstract

The invention discloses a synthesis method of 2-chromium picolinate, which is implemented by hydrolyzing 2-cyanopyridine to obtain sodium salt solution of 2-chromium picolinate, adding chromium trichloride for complexation to obtain 2-chromium picolinate product. Compared with traditional method for synthesizing 2-chromium picolinate with 2-methylpyridine as raw material, the invention is simple in synthesis route, sate and reliable in process procedure, strong in maneuverability, high in reaction yield and good in product quality.

Description

Technical field: [0001] The invention relates to a method for synthesizing chromium 2-picolinate. Background technique: [0002] The synthetic route of 2-chromium picolinate in the prior art: [0003] 1. Patent CN1408708A uses 2-vinylpyridine as raw material to synthesize 2-pyridinecarboxylic acid by potassium permanganate oxidation method and then complexes with chromium trichloride. The 2-pyridinecarboxylic acid obtained by this method has low purity and requires multiple crystallizations to obtain qualified 2-pyridinecarboxylic acid, and the process also produces a large amount of by-product manganese dioxide to be processed. Potassium permanganate is also more expensive. [0004] 2. Patent CN1772737A uses 2-picoline as raw material, oxidizes it with sulfuric acid to 2-pyridinecarboxylic acid, and then complexes it with chromium trichloride to get the product. Due to the use of sulfuric acid for oxidation in this process, a large amount of waste acid is produced, which...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/803C07D213/79
Inventor 丁彩峰朱小刚刘芳周新建薛建锋
Owner NANTONG ACETIC ACID CHEM
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