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Method for separating and purifying vitamin C palmitate from reaction liquid of direct esterification method

A separation and purification technology of palmitic acid ester, applied in the direction of organic chemistry, can solve the problems of cumbersome separation steps and high toxicity, and achieve the effect of simple operation, low toxicity and mild conditions

Active Publication Date: 2013-08-21
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the subsequent separation and purification process of this method, a variety of organic solvents are required, and many solvents are highly toxic. The separation steps are cumbersome, and the separation cost can be close to about half of the total cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Add 100ml (about 184g) of 99-99.5% sulfuric acid into a 250ml four-necked bottle, add 35g of palmitic acid under stirring, stir and dissolve at 30-35°C, it takes about 0.5-1 hour; To 20-25°C, under nitrogen protection, add 17.6 grams of vitamin C under stirring, stop stirring after it is completely dissolved, keep warm at 18-20°C for 48 hours, and obtain vitamin C palmitate reaction solution.

[0019] (2) Control the temperature below 40°C, slowly pour the reaction solution into a 2000ml four-necked bottle filled with 200ml of ice cooling water; then add 700ml of toluene for extraction, heat to 60°C and then naturally stir to cool down. When the temperature of the system drops to about 40°C, the layers are still separated, the lower layer of waste acid is separated, and the toluene layer is retained;

[0020] (3) Add 200 ml of water at 30-35°C to the toluene layer, heat and stir at 30-35°C for 3 hours to crystallize; cool to 10-15°C with ice water, stir and crystall...

Embodiment 2

[0024] (1) Add 17.6 grams of vitamin C to 100 ml (about 184 grams) of 99-99.5% sulfuric acid and add it to a 250 ml four-necked bottle, let it stand for 24 hours, then add 35 grams of palmitic acid while stirring, and stir at about 30°C for 2 -3 hours, to obtain vitamin C palmitate reaction solution.

[0025] (2) Control the temperature below 50°C, slowly pour the reaction solution into a 2000ml four-necked bottle filled with 200ml of ice cooling water; then add 700ml of toluene for extraction, heat to 50°C and then naturally stir to cool down. When the temperature of the system drops to about 35°C, the layers are still separated, the lower layer of waste acid is separated, and the toluene layer is retained;

[0026] (3) Add 200ml of water at 30-35°C to the toluene layer, heat and stir at 25-30°C for 1 hour to crystallize; cool to 5-10°C with ice water, stir and crystallize for 0.5 hour; filter, wash the filter cake with 50ml of toluene, Then wash with 500 ml of 30-35°C water...

Embodiment 3

[0030](1) Under nitrogen protection, add 17.6 grams of vitamin C to 100 milliliters (about 184 grams) of 99-99.5% sulfuric acid into a 250 milliliter four-neck bottle, let it stand for 24 hours, then add 35 grams of palmitic acid while stirring, Stir at about 30°C for 2-3 hours to obtain a vitamin C palmitate reaction liquid.

[0031] (2) Control the temperature below 40°C, slowly pour the reaction solution into a 2000ml four-necked bottle filled with 200ml of ice cooling water; then add 700ml of toluene for extraction, heat to 60°C and then naturally stir to cool down. When the temperature of the system drops to about 40°C, the layers are still separated, the lower layer of waste acid is separated, and the toluene layer is retained;

[0032] (3) Add 200 ml of water at 30-35°C to the toluene layer, heat and stir at 30-35°C for 3 hours to crystallize; cool to 10-15°C with ice water, stir and crystallize for 1.5 hours; filter, wash the filter cake with 50 ml of toluene, Then wa...

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Abstract

The invention relates to a method for separating and purifying vitamin C palmitate from reaction liquid of a direct esterification method, and the method applied to separation and purification fields of the reaction liquid. The separating and purifying method comprises the following steps of: reacting vitamin C with palmitic acid under catalysis of concentrated sulfuric acid, so as to obtain the reaction liquid of the vitamin C palmitate; slowly pouring the reaction liquid into ice-bath cooling water or trash ice, adding methylbenzene to carry out extraction, and carrying out standing and layering to separate out a lower-layer waste acid layer and leave a methylbenzene layer; adding water into the methylbenzene layer, carrying out crystallization and filtering so as to obtain a filter cake, and respectively washing the filter cake by utilizing proper amount of methylbenzene and water; adding the filter cake into the water and stirring for 0.5-3 hours, filtering, and carrying out water washing until the pH of the effluent water is 6-7, so as to obtain crude products of the vitamin C palmitate; and carrying out recrystallization on the crude products of the vitamin C palmitate by utilizing ethanol so as to obtain finished products of the vitamin C palmitate. The method for separating and purifying the vitamin C palmitate from the reaction liquid of the direct esterification method has the advantages that solvents are simply separated and purified, are low in toxin and can be recycled, the separation and purification cost is low, the product purity is high, the condition is mild and the operation is simple and convenient.

Description

technical field [0001] The invention belongs to the field of separation and purification of reaction mixtures, in particular to a method for separating and purifying vitamin C palmitate from a direct esterification reaction liquid. 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; molecular formula is C 22 h 38 o 7 , molecular weight 414.54; specific rotation +22~+24°; insoluble in water, slightly soluble in vegetable oil (300mg / L), soluble in ethanol (100,000mg / L); melting point 107-117℃. [0003] 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 vitamin C fatty acid ester...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/62
Inventor 杨渐飞刘丹周联波郑静
Owner NORTHEAST PHARMA GRP
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