Crystallization method of sodium ascorbate

A vitamin and crystallization technology, applied in the direction of organic chemistry, organic chemistry, etc., can solve the problems of poor color of vitamin C sodium products, affecting the color of vitamin C sodium, low yield of vitamin C sodium, etc., to promote stable growth and uniform particle size , the effect of high purity

Active Publication Date: 2017-05-10
自然资源部天津海水淡化与综合利用研究所
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  • Description
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Problems solved by technology

In the first preparation method, the temperature of the esterification reaction is relatively high, and because vitamin C sodium is heat-sensitive, high temperature greatly damages its quality, making the vitamin C sodium solution system appear reddish-brown, which seriously affects the color of vitamin C sodium, and Using concentrated sulfuric acid as a catalyst will produce sodium sulfate by-products to be mixed in the sodium vitamin C product. The sodium vitamin C product obtained by this method has poor color and low purity; the second method has a lower preparation temperature than the first method, and the produced vitamin C The color and quality of sodium C have been improved, but there are still many problems in the crystallization process. The yield of vitamin C sodium obtained by cooling crystallization is low, while the crystals obtained by dissolution crystallization have small main particle size, uneven particles, and high impurity content.

Method used

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  • Crystallization method of sodium ascorbate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Neutralization reaction (S1): Add 300mL of distilled water into the reactor, then add 300g of vitamin C and 255g of sodium bicarbonate into the reactor, heat to 50°C, stir, and carry out the neutralization reaction for 30min, and control the terminal pH of the neutralization reaction The value is 4.5, and the reaction complete liquid is obtained, and the reaction complete liquid is filtered with a 0.22 μm organic filter membrane, and the filtration temperature is 50° C., to obtain the reaction clear liquid;

[0050] Constant temperature crystal growth (S2): Add 0.35 g of 200-mesh sodium vitamin C seed crystals to the reaction clarified liquid to obtain a seed crystal suspension, and grow the crystal seed suspension at 50° C. for 1.5 hours to obtain a crystal growth complete liquid;

[0051] Cooling-dissolution coupled crystallization (S3): Cool the crystal growth complete solution to 25°C at a uniform speed, and the cooling time is 2 hours, and cool and crystallize to ob...

Embodiment 2

[0055] Neutralization reaction (S1): Add 360mL of distilled water into the reactor, then add 300g of vitamin C and 270g of sodium bicarbonate into the reactor, heat to 50°C, stir, and carry out the neutralization reaction for 40min, and control the terminal pH of the neutralization reaction The value is 5, and the reaction complete liquid is obtained, and the reaction complete liquid is filtered with a 0.22 μm organic filter membrane, and the filtration temperature is 50° C., to obtain the reaction clear liquid;

[0056] Constant temperature crystal growth (S2): Add 0.4 g of 180-mesh sodium vitamin C seed crystal to the reaction clarified liquid to obtain a seed crystal suspension, and grow the seed crystal suspension at 50° C. for 1 hour to obtain a crystal growth complete liquid;

[0057] Cooling-dissolution coupling crystallization (S3): Cool down the crystal growth complete liquid to 25°C at a uniform speed, and the cooling time is 2.5 hours, and cool and crystallize to obt...

Embodiment 3

[0061] Neutralization reaction (S1): Add 270mL of distilled water into the reactor, then add 300g of vitamin C and 240g of sodium bicarbonate into the reactor, heat to 55°C, stir, and carry out the neutralization reaction for 35min, and control the terminal pH of the neutralization reaction The value is 5.5, and the reaction complete liquid is obtained, and the reaction complete liquid is filtered with a 0.22 μm organic filter membrane, and the filtration temperature is 55° C., to obtain the reaction clear liquid;

[0062] Constant temperature crystal growth (S2): Add 0.43 g of 190-mesh sodium vitamin C seed crystals to the reaction clarified liquid to obtain a seed crystal suspension, and grow the seed crystal suspension at 55° C. for 1 hour to obtain a crystal growth complete liquid;

[0063] Cooling-dissolution coupled crystallization (S3): Cool down the crystal-growing liquid to 25°C at a uniform speed, and the cooling time is 2.5 hours, and cool and crystallize to obtain a...

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Abstract

The invention discloses a crystallization method of sodium ascorbate. A high-purity and large-granularity sodium ascorbate crystal product is prepared by a cooling crystallization and dilution crystallization coupling method through regulation and control of crystallization conditions. The method comprises the following specific technical steps: adding vitamin C and sodium bicarbonate into water; heating to 50 to 60 DEG C to carry out a neutralization reaction; filtering reaction completion liquid through an organic filter membrane, and adding a sodium ascorbate seed crystal; growing the crystal for 1 to 1.5 hours; lowering the temperature by 20 to 30 DEG C to perform first-stage cooling crystallization; raising the temperature by 20 to 30 DEG C, and adding methanol to perform first-stage heating dilution crystallization; performing second-stage cooling crystallization, second-stage heating dilution crystallization and third-stage cooling crystallization; performing centrifugal separation; washing a sodium ascorbate crystal filter cake; performing vacuum drying to obtain a sodium ascorbate crystal product. The crystallization method has high yield, and the obtained sodium ascorbate crystal product has high purity, homogeneous granularity and large crystal main granularity.

Description

technical field [0001] The invention relates to chemical technology, in particular to a crystallization method of vitamin C sodium. Background technique [0002] Vitamin C, also known as L-ascorbic acid, plays an important role in medicine and is an indispensable substance for maintaining human health. It is a catalyst for redox reactions in living cells, participates in various metabolisms in the body, and has the ability to promote various hormones in the body. Synthetic Physiological Effects. The lack of vitamin C in the body will lead to scurvy, which can cause death in severe cases. Vitamin C is both a medicine and a nutritional agent, and has been widely used in the food and cosmetic industries in recent years. With the continuous improvement of people's living standards in our country and the increasing awareness of vitamin C to increase the body's resistance and prolong life, the demand for vitamin C in my country is expected to have a relatively large increase. H...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/62
CPCC07B2200/13C07D307/62
Inventor 张辉张琦路绍琰骆碧君宋达
Owner 自然资源部天津海水淡化与综合利用研究所
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