Method for preparing VC (Vitamin C) crystal in one step by using aqueous solution of 2-keto-L-gulonic acid

A technology of aqueous solution and gulonic acid, applied in the direction of organic chemistry, can solve problems such as endangering the health of production personnel, production environment pollution, production safety hazards, etc., and achieve the effects of saving treatment costs, reducing environmental pollution, and reducing procedures

Pending Publication Date: 2022-04-19
河北乐开节能科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In summary, although the prior art discloses the direct catalytic preparation of VC using 2-KLG as a raw material, it is necessary to use an inert solvent to provide a reaction environment.
However, inert solvents are usually highly volatile, toxic and even flammable, which no

Method used

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  • Method for preparing VC (Vitamin C) crystal in one step by using aqueous solution of 2-keto-L-gulonic acid

Examples

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Effect test

Embodiment 1

[0029] 200mL of 2-KLG saturated solution in a 1000mL three-necked flask, add 1‰ ammonium molybdate to the solution, shake to dissolve; Keep it at 22-25Kpa. Quickly put the flask into a 50°C constant temperature water tank with ultrasonic waves while shaking, so that the saturated 2-KLG aqueous solution is all below the hot water, and turn on the ultrasonic waves with a frequency of 20khz. It was observed that there was crystallization at the bottom of the flask. When the volume of the solution became 100mL, the reaction was stopped and filtered to obtain crystals, which were detected as VC. After subtracting 0.4g of VC seeds, the calculated yield was 78%. The ammonium molybdate remains in the solution and can be used as a catalyst after adding a new saturated solution of 2-KLG.

Embodiment 2

[0031] 200mL of 2-KLG saturated solution in a 1000mL three-neck flask, add 0.9‰ ammonium molybdate to the solution, shake to dissolve; Keep it at 25-26Kpa. Quickly put the flask into a 55°C constant-temperature water tank with ultrasonic waves while shaking, so that the saturated 2-KLG aqueous solution is all below the hot water, and turn on the ultrasonic waves with a frequency of 30khz. It was observed that there was crystallization at the bottom of the flask. When the volume of the solution became about 100mL, the reaction was stopped and filtered to obtain crystals, which were detected as VC. After subtracting 0.4g of VC seeds, the calculated yield was 74%.

Embodiment 3

[0033] 200mL of 2-KLG saturated solution in a 1000mL three-necked flask, add 0.9‰ ammonium molybdate to the solution, shake to dissolve; Keep it at 22-25Kpa. Put the flask into a 60°C constant-temperature water bath with ultrasonic waves while shaking, so that the saturated 2-KLG aqueous solution is all below the hot water, and turn on the ultrasonic waves with a frequency of 30khz. It was observed that crystals were produced at the bottom of the flask. When the volume of the solution became about 100 mL, the reaction was stopped and filtered to obtain crystals, which were detected as VC. After subtracting 0.2 g of VC seeds, the calculated yield was 70.1%.

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Abstract

The invention relates to a method for preparing VC (Vitamin C) crystals in one step by using an aqueous solution of 2-keto-L-gulonic acid, which comprises the following steps: S1, adjusting the concentration of the aqueous solution of 2-keto-L-gulonic acid to enable the aqueous solution to reach or approach to a saturated state at normal temperature; s2, adding soluble molybdate into the aqueous solution of the 2-keto-L-gulonic acid, and uniformly stirring to enable the concentration of the soluble molybdate in the aqueous solution to be 0.85-0.12% o; and S3, adding a certain amount of VC seed crystals into the aqueous solution to induce graining, keeping the temperature of 50-60 DEG C to evaporate water in a low-pressure air environment to provide a driving force for crystallization, loading ultrasonic waves on the aqueous solution to intensify crystallization, separating VC crystals from the bottom of the aqueous solution, and drying to obtain the product. According to the method, the technological process is shortened, inorganic acid/alkali is not used in the production process, an inert solvent does not need to be used for providing a reaction environment, VC crystals can be directly obtained through conversion in the gulonic acid aqueous solution, and the method has the advantages of being simple in follow-up treatment, low in production cost, environmentally friendly and the like.

Description

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Claims

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Application Information

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Owner 河北乐开节能科技股份有限公司
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