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Preparation method of chromium picolinate

A technology of chromium picolinate and picolinate, which is applied in the field of chromium picolinate, can solve the problems of high melting point, ammonia-containing waste pollution, long reaction time, etc., and achieve the effects of shortening the process flow, high product yield and simple steps

Inactive Publication Date: 2019-01-18
SICHUAN SINYIML BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, because 2-cyanopyridine has a high melting point and is insoluble in water, the hydrolysis reaction is carried out in a heterogeneous phase, and the reaction time is long. At the same time, a large amount of ammonia gas needs to be absorbed and treated after hydrolysis, and the ammonia-containing waste generated will have a negative impact on the environment. Pollution has brought enormous pressure to the environment

Method used

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  • Preparation method of chromium picolinate
  • Preparation method of chromium picolinate

Examples

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Effect test

Embodiment 1

[0020] Such as figure 1 Shown, the preparation method of the chromium picolinate provided by the present embodiment comprises the steps:

[0021] (1) Put 80kg of 2-picoline, 246kg of sodium dichromate and 400kg of water into the reactor, add sulfuric acid to adjust the pH value to 4.5-5.0, and then heat to make the temperature in the reactor 200-210 ℃, pressure 2.5 ~ 3.2MPa, heat preservation and pressure oxidation reaction for 1h;

[0022] (2) The temperature in the reaction kettle is reduced to 85-90° C., distilled under reduced pressure, and the distillate is a 2-picoline aqueous solution, which can be used as a raw material for the next production;

[0023] (3) Add sulfuric acid to the reaction kettle that has been distilled under reduced pressure, adjust the pH value to 2.0-2.5, and keep the temperature at 85-90°C, perform complexation reaction under normal pressure for 5h, and then lower the temperature to 20-30°C Crystallize, finally centrifuge, wash with 50kg of wate...

Embodiment 2

[0025] The preparation method of the chromium picolinate provided by the present embodiment may further comprise the steps:

[0026] (1) Put 100kg of 2-picoline, 246kg of potassium dichromate and 400kg of water into the reactor, add hydrochloric acid to adjust the pH value to 5.0-5.5, and then heat to make the temperature in the reactor 210-230 ℃, pressure 2.2 ~ 3.2MPa, heat preservation and pressure oxidation reaction for 10h;

[0027] (2) The temperature in the reaction kettle is reduced to 85-90° C., distilled under reduced pressure, and the distillate is a 2-picoline aqueous solution, which can be used as a raw material for the next production;

[0028] (3) Add hydrochloric acid to the reaction kettle that has been distilled under reduced pressure, adjust the pH value to 2.5-3.0, and keep the temperature at 85-90°C, perform complexation reaction under normal pressure for 1h, and then lower the temperature to 20-30°C Crystallize, finally centrifuge, wash with 50kg of water...

Embodiment 3

[0030] The preparation method of the chromium picolinate provided by the present embodiment may further comprise the steps:

[0031] (1) Put 100kg of 2-picoline, 246kg of ammonium dichromate and 400kg of water into the reactor, add phosphoric acid to adjust the pH value to 5.0-5.5, and then heat to make the temperature in the reactor 230-240 ℃, pressure 3.2 ~ 3.5MPa, heat preservation and pressure oxidation reaction for 6 hours;

[0032] (2) The temperature in the reaction kettle is reduced to 85-90° C., distilled under reduced pressure, and the distillate is a 2-picoline aqueous solution, which can be used as a raw material for the next production;

[0033] (3) Add phosphoric acid to the reaction kettle that has been distilled under reduced pressure, adjust the pH value to 2.0-3.0, and keep the temperature at 85-90°C, perform complexation reaction under normal pressure for 1h, and then lower the temperature to 20-30°C Crystallize, finally centrifuge, wash with 50kg of water,...

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Abstract

The invention discloses a preparation method of chromium picolinate. The preparation method comprises the following steps: mixing methylpyridine, an oxidant and water in a mass ratio of 1.1-1.3 to 3.0to 3.0-5.0, and adjusting the pH value to 4.5-6.0 for an oxidizing reaction, wherein the oxidizing reaction temperature is 200-240 DEG C, the oxidizing reaction pressure is 2.5-4.2 MPa, and the oxidizing reaction time is 1-10 hours; then cooling and recovering 2-methylpyridine, then adjusting the pH value to 2.0-3.0, and carrying out a complexing reaction at a constant temperature, wherein the complexing reaction temperature is 85-90 DEG C and the complexing reaction time is 1-5 hours; and finally, carrying out cooling crystallization, centrifugalization, washing and drying to obtain chromiumpicolinate. The preparation method which comprises the steps of oxidizing 2-methylpyridine into 2-picolinic acid through an oxidant aqueous solution at a high pressure and a high temperature in an acidic condition by taking 2-methylpyridine as an initial raw material, reducing the oxidant into chromium sulfate basic and then complexing 2-picolinic acid and chromium sulfate basic into chromium picolinate at a constant temperature, and the preparation method is simple in structure and high in product yield, and has the advantages of being green, environment-friendly, low in cost and the like.

Description

technical field [0001] The invention relates to the technical field of chromium picolinate, in particular to a preparation method of chromium picolinate. Background technique [0002] With the development of chromium research, humans have realized that chromium is an essential trace element for the human body. The current valence states of chromium include Cr 2+ 、Cr 3+ and Cr 6+ , Cr 3+ It is a stable form of chromium in the human body. Its compounds participate in the biochemical process of bone formation, protein, fat, sugar metabolism and insulin, and promote the synthesis of hemoglobin and hematopoiesis. But Cr 6+ In the human body, it affects the metabolism of the three major substances of sugar, fat and protein, inhibits the activity of glutathione reductase, forms chromium oxide with oxygen, and takes part of the oxygen in the blood, resulting in hypoxia in the body and metabolic disorders. [0003] Chromium sources are divided into inorganic chromium and organi...

Claims

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Application Information

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IPC IPC(8): C07D213/79C07D213/807
CPCC07D213/79C07D213/807
Inventor 王斐英
Owner SICHUAN SINYIML BIOTECH CO LTD
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