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Synthesis process of chronium 2-picolinate

A technology of chromium picolinate and synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of low conversion rate of raw materials and high reaction pressure, and achieve the effects of simple process operation, mild reaction conditions and cheap raw materials

Inactive Publication Date: 2006-05-17
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction pressure of this method is relatively high, and the conversion rate of raw materials is also relatively low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: in 500ml there-necked flask, add 2 gram chromic anhydrides, 45 gram sodium dichromate, 70ml sulfuric acid (65wt%), stir and be heated to 100 ℃, dropwise add 10ml2-picoline and 20ml (65wt%) sulfuric acid The mixed solution was reacted for 6 hours. After the reaction is completed, add 10ml of ethanol dropwise to the reaction solution, adjust the pH value of the reaction mixture solution to 10 with sodium hydroxide solution, heat to reflux, filter to remove the chromium salt, adjust the pH to 8 after the filtrate is concentrated, and start dripping the chromium nitrate solution to the reaction solution The pH value was 6, and 10.5 grams of purple-red precipitated chromium picolinate was obtained.

Embodiment 2

[0022] Embodiment 2: in 500ml there-necked flask, add 24 grams of chromic anhydride, 70ml sulfuric acid (65wt%), stir and be heated to 110 ℃, add dropwise the mixed solution of 10ml2-picoline and 40ml (65wt%) sulfuric acid to react for 8 hours. After the reaction is completed, add 10ml of ethanol dropwise to the reaction solution, then adjust the pH value of the reaction mixture solution to 9 with sodium hydroxide solution, heat to reflux, filter to remove the chromium salt, adjust the pH to 7 after the filtrate is concentrated, and add dropwise chromium nitrate solution to the reaction solution pH The value is 5.5, and 10 grams of chromium picolinate is obtained.

Embodiment 3

[0023] Embodiment 3: in 500ml there-necked flask, add 45 grams of sodium dichromate, 60ml sulfuric acid (70wt%), stir and heat to 90 ℃, dropwise add the mixed solution of 10ml2-picoline and 30ml sulfuric acid (70wt%) to react for 7 hours . After the reaction is completed, add 10ml of ethanol dropwise to the reaction solution and adjust the pH value of the reaction mixture solution to 11 with sodium hydroxide solution, heat to reflux, filter to remove the chromium salt, adjust the pH to 8 after the filtrate is concentrated, and add dropwise chromium nitrate solution to the reaction solution pH The value was 7, and 9.8 grams of chromium picolinate was obtained.

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Abstract

The synthesis process of chromium 2-picolinate includes oxidizing 2-picoline into 2-picolinic acid, separating side product chromium oxide and mirabilite, and complexing with trivalent chromium salt to produce chromium 2-picolinate. The synthesis process of the present invention has simple operate, cheap material, high additional value of the side product, mild reaction condition, short reaction time, low power consumption, low cost, high yield and easy application in production.

Description

technical field [0001] The invention belongs to a method for synthesizing chromium 2-picolinate. Background technique [0002] 2-Pyridinecarboxylic acid and its derivatives exhibit remarkable physiological activity and are widely used in medicine, agriculture and daily chemicals. Chromium 2-picolinate is not only an effective and potential feed additive, but also can be used as an auxiliary drug for treating diabetes and a weight-loss drug. [0003] At present, the synthesis of chromium 2-pyridinecarboxylate generally uses 2-picoline as a raw material, prepares 2-pyridinecarboxylic acid through oxidation and acidification, and then complexes with chromium trichloride under alkaline conditions to prepare, but The handling of 2-pyridinecarboxylic acid is cumbersome, and product loss affects yield. The reaction takes a long time, consumes a lot of energy, the yield is low, and the cost is high. [0004] Industrially, 2-pyridinecarboxylic acid can be prepared by liquid-phase ...

Claims

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Application Information

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IPC IPC(8): C07D213/79
Inventor 田艳青李德宝李文怀
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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