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Method for synthesizing chromium picolinate with direct reduction process

A technology of chromium picolinate and reduction method, which is applied in organic chemistry and other fields, can solve problems such as safety hazards, unstable product yield, unsuitable control of intermediate pH value, etc., and achieve the effect of no by-products and low cost

Active Publication Date: 2016-05-04
四川尚元惠生生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many ways to synthesize chromium 2-picolinate, which mainly include the following forms: 2-cyanopyridine is used as the main raw material, and 2-picolinic acid or sodium picolinate is synthesized by acid or alkali hydrolysis and other raw materials The synthesized 2-picolinic acid or sodium picolinate is chelated with trivalent chromium salt directly or indirectly through alkaline solution titration to generate chromium 2-picolinate. The color of chromium picolinate synthesized by this type of process is not uniform, and it is not suitable to control the intermediate pH value. The product The yield is also unstable, which is not conducive to industrial standard operation
[0004] Put 2-cyanopyridine, one or more of sulfuric acid, hydrochloric acid or nitric acid, and trivalent chromium salt in a high-pressure reactor to synthesize chromium 2-picolinate. This type of process requires high production equipment and is a pressure Containers, there are certain hidden dangers in the production process
Decompose 2-picoline or 2-vinylpyridine with potassium permanganate, remove manganese dioxide and synthesize chromium 2-picolinate with trivalent chromium salt. In this type of process, potassium permanganate is expensive and produces a large amount of Manganese dioxide, a by-product, has certain environmental risks

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 100L of water into the reaction tank, add 10kg of sodium carbonate while stirring, raise the temperature to 50°C, slowly drop in 20kg of 2-cyanopyridine, after the hydrolysis is complete, adjust the pH value to 0.5 with sulfuric acid, and add 5kg of potassium dichromate , after titrating with 5% methanol solution to no hexavalent chromium, keep warm at 50°C for 2h, cool down to 40°C, centrifugally dehydrate and filter, and dry the filtrate to obtain chromium 2-picolinate. Wherein the yield of 2-chromium picolinate is 97.5%, and the main content of chromium picolinate measured by high performance liquid chromatography is 99.59%.

Embodiment 2

[0023] Add 300L of water into the reaction tank, add 20kg of sodium hydroxide while stirring, raise the temperature to 70°C, slowly drop in 40kg of 2-cyanopyridine, after the hydrolysis is complete, adjust the pH value to 4.5 with sulfuric acid, add 15kg of chromic anhydride, After titrating with 5% glucose solution to no hexavalent chromium, keep warm at 70°C for 2h, cool down to 25°C, centrifugal dehydration and filter, and dry the filtrate to obtain chromium 2-picolinate. Wherein the yield of 2-chromium picolinate is 95%, and the main content of chromium picolinate recorded by high performance liquid chromatography is 99.85%.

Embodiment 3

[0025] Add 350L of water into the reaction tank, add 20kg of potassium hydroxide while stirring, raise the temperature to 105°C, slowly drop in 35kg of 2-cyanopyridine, after the hydrolysis is complete, adjust the pH value to 3.5 with sulfuric acid, add 12kg of chromic anhydride, and use 10 % white sugar solution was titrated to free of hexavalent chromium, kept at 110°C for 1.5h, cooled to 25°C, centrifugally dehydrated and filtered, and dried to obtain chromium 2-picolinate. Wherein the yield of 2-chromium picolinate is 96%, and the main content of chromium picolinate recorded by high performance liquid chromatography is 99.77%.

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Abstract

The invention relates to a method for synthesizing chromium picolinate with a direct reduction process. The method comprises the following steps: (1) taking 10kg to 40kg of alkali and dissolving the alkalis into 100L to 450L of water; stirring and heating; heating until the temperature is 50 DEG C to 150 DEG C; (2) slowly dropping 20kg to 80kg of 2-cyanopyridine; after the 2-cyanopyridine is completely hydrolyzed, dripping an acid to adjust the pH value to be 0.5 to 6.5; (3) adding 5kg to 50kg of chromium salt into a 2-picolinic acid solution prepared in the step (2) and stirring and raising the temperature to be 50 DEG C to 150 DEG C; (4) adding a reducing agent water solution with the concentration of 0.5 percent to 50 percent into the solution prepared in the step (3) until the solution has no hexavalent chromium; preserving heat and curing for 0.5 hour to 5 hours; (5) cooling to be 50 DEG C or lower than 50 DEG C, and dehydrating and filtering; drying a filtered matter to obtain 2-chromium picolinate.

Description

technical field [0001] The invention relates to a method for synthesizing chromium picolinate by a direct reduction method. Background technique [0002] Chromium picolinate is a mineral, an essential trace element for the human body. The latest research by authoritative institutions such as the Nutrition Center of the United States Department of Agriculture has once again confirmed that trivalent inorganic chromium has little effect on enhancing insulin activity, but when converted into organic chromium, it has a significant effect on enhancing insulin activity. As an important part of glucose tolerance factor, chromium picolinate is an indispensable trace element for diabetics. Studies have shown that chromium picolinate has strong stability. As a fat-soluble non-electrolyte, it can pass through the cell membrane and directly act on tissue cells, enhance insulin activity, improve human glucose metabolism, and play an important role in the treatment of diabetes. New resea...

Claims

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Application Information

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IPC IPC(8): C07D213/803
CPCC07D213/803
Inventor 谭光坤
Owner 四川尚元惠生生物科技有限公司