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Preparation method of vitamin C palmitate

A technology of palmitate and vitamin, applied in organic chemistry and other directions, can solve the technical difficulties of extraction, separation and purification, and achieve the effects of fewer types of solvents, fewer reaction steps, and faster extraction and separation

Inactive Publication Date: 2017-06-13
安徽泰格生物技术股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are certain technical difficulties in the extraction, separation and purification technology.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In a three-necked flask equipped with a stirrer and a thermometer, add 50-58 mL of 95-96% concentrated sulfuric acid. After nitrogen replacement, quickly add 15 grams of vitamin C under stirring, nitrogen protection, 3 grams of cyclohexanehexanol, and seal. Dissolve for 3.5 to 4 hours. The temperature is controlled at 15°C to 20°C. After the VC insulation reaction is complete, under the protection of nitrogen, quickly add 29.8 grams of palmitic acid, and the reaction is closed and stirred for 1 to 2 hours, and the static reaction is 10 to 15 hours, and then the reaction is stirred for 36 to 40 hours. . Pour the reacted feed liquid into a 1000-2000mL beaker with a thermometer and magnetic stirring, and hydrolyze it in a mixture of ice and water at 0-5°C to obtain crude ester. After the hydrolyzed crude ester is vacuum filtered, 800-1200 mL of toluene and 400 mL of pure water are added for extraction. When extracting, heat with a water bath, the temperature is controll...

Embodiment 2

[0040] In a three-necked flask equipped with a stirrer and a thermometer, add 50-58 mL of 96-96.5% concentrated sulfuric acid. After nitrogen replacement, quickly add 15 grams of vitamin C under stirring, nitrogen protection, 3 grams of cyclohexanehexanol, and seal. Dissolve for 3.5 to 4 hours. The temperature is controlled at 15°C to 20°C. After the VC heat preservation reaction is complete, under the protection of nitrogen, quickly add 29.8 g of palmitic acid, and react for 1 to 2 hours with closed stirring, and react for 10 to 15 hours at rest, and then stir for 36 to 40 hours. Pour the reacted feed liquid into a 1000-2000mL beaker with a thermometer and magnetic stirring, and hydrolyze it in a mixture of ice and water at 0-5°C to obtain crude ester. After the hydrolyzed crude ester is vacuum filtered, 800-1200 mL of toluene and 400-600 mL of pure water are added for extraction. When extracting, heat with a water bath, the temperature is controlled at 40-50°C, the holdin...

Embodiment 3

[0042]In a three-necked flask equipped with a stirrer and a thermometer, add 50-58 mL of 97-98% concentrated sulfuric acid. After nitrogen replacement, quickly add 15 grams of vitamin C under stirring, nitrogen protection, 3 grams of cyclohexanehexanol, and seal. Dissolve for 3.5 to 4 hours. The temperature is controlled at 15°C to 20°C. After the VC heat preservation reaction is complete, under the protection of nitrogen, quickly add 29.8 g of palmitic acid, and react for 1 to 2 hours with closed stirring, and react for 10 to 15 hours at rest, and then stir for 36 to 40 hours. Pour the reacted feed liquid into a 1000-2000mL beaker with a thermometer and magnetic stirring, and hydrolyze it in a mixture of ice and water at 0-5°C to obtain crude ester. After the hydrolyzed crude ester is vacuum filtered, 800-1200 mL of toluene and 400-600 mL of pure water are added for extraction. During extraction, heat with a water bath, control the temperature at 40-50°C, and keep warm for...

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PUM

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Abstract

The invention relates to the technical field of production of vitamin C palmitate, and more specifically discloses a preparation method of vitamin C palmitate. Using vitamin C and palmitic acid as raw materials, using concentrated sulfuric acid as a catalyst and solvent, and using cyclohexyl alcohol or citric acid as an antioxidant, the crude ester of vitamin C palmitic acid is synthesized by direct esterification, and the crude ester is further washed and separated, Crystallization and recrystallization. The method has few reaction steps, few types of solvents, fast extraction and separation, low toxicity, recyclable solvents for repeated application, low cost, simple operation and easy industrial production.

Description

technical field [0001] The invention relates to the technical field of production of vitamin C palmitate, more specifically, relates to a preparation method of vitamin C palmitate. Background technique [0002] Vitamin C palmitate, also known as L-ascorbic acid palmitate, English name L ~ Ascorbic Acid Palmitate, is the esterification product of vitamin C and palmitic acid. Vitamin C palmitate is white to light yellow powder; specific rotation +22°~+24°; insoluble in water, slightly soluble in vegetable oil, soluble in ethanol; melting point 107~117℃. [0003] Structural formula: [0004] Molecular formula: C 22 h 38 o 7 , molecular weight: 414.54. [0005] Vitamin C palmitate not only maintains the antioxidant properties of vitamin C, but also has considerable solubility in animal oil and vegetable oil, and is widely used in food, cosmetics, medicine and health and other fields. Vitamin C palmitate belongs to the group of vitamin C fatty acid esters. [0006] At pr...

Claims

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Application Information

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IPC IPC(8): C07D307/62
CPCC07D307/62
Inventor 伏传久
Owner 安徽泰格生物技术股份有限公司
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