Preparation method of Dexpanthenol

A technology of panthenol and aminopropanol, which is applied in the field of D-panthenol preparation, can solve the problems of low purification yield of D-pantothenolactone, difficult production capacity to meet market demand, serious reaction amplification effect, etc. Stable and controllable, convenient for transportation and measurement, and reduce the effect of crystallization operation

Active Publication Date: 2020-12-08
SHANDONG NHU FINE CHEM SCI & TECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, it is necessary to carry out multiple recrystallization, purification and thorough drying of the D-pantoolactone obtained after the split (CN 101851171), but the purification yield of D-pantoolactone is low, and a large amount of waste gas is produced simultaneously, which is harmful to the environment. unfriendly
[0009] In addition, due to the extremely high viscosity and poor fluidity of D-panthenol, its mass transfer effect in the reactor is very poor, and t...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 100 kg of D-pantolactone crude product and add it to the reactor, then add 100 kg of methanol, stir and dissolve, add 1 kg of activated carbon, decolorize under reflux conditions for 1 hour, then filter, the obtained filtrate is colorless and transparent, and the mass percentage concentration is 50% D-pantolactone methanol solution, set aside.

[0032] The methanol solution of D-pantolactone and 3-aminopropanol were pumped into the three reactors in series at a rate of 2 kg / h and 0.58 kg / h, respectively. The volume of each tank was 2 L, and the reaction temperature was 50°C. After 4 hours of pumping, samples were taken from the outlet of the reactor to detect that the residual D-pantolactone was 0.3%, indicating that the reaction system had reached a steady state. Start to connect the reaction liquid to the solvent recovery device, stop the reaction after receiving for 10 hours, and receive a total of 25.7 kg of the reaction liquid. Then recovery device recove...

Embodiment 2

[0048] According to the method of Example 1, ethyl acetate was used as a solvent to prepare a solution with a mass percent concentration of 50% D-pantolactone. The D-pantolactone solution and 3-aminopropanol were pumped into the 3-tank series reactor at a rate of 2 kg / h and 0.58 kg / h, respectively. The volume of each kettle is 2L, and the reaction temperature is 60°C. After reacting for 3 hours, a sample was taken from the outlet of the reactor to detect that the residual D-pantolactone was 0.5%. Start to connect the reaction solution into the solvent recovery device, stop the reaction after 10 hours of receiving, and receive a total of 25.8kg. The recovering device then reclaims the solvent under reduced pressure at 10kPa. When the recovery rate of ethyl acetate reaches 90%, 1kg of distilled water is added to increase the vacuum until the pressure is 1kPa and the temperature is 80°C. Continue to recover until no solvent is evaporated. 15.6 kg of colorless transparent vi...

Embodiment 3

[0050] According to the method of Example 1, a solution with a mass percent concentration of 50% D-pantolactone was prepared using water as a solvent. The D-pantolactone solution and 3-aminopropanol were pumped into the 3-tank series reactor at the speed of 2kg / h and 0.58kg / h respectively, the volume of each kettle was 2L, and the reaction temperature was 60°C. After 4 hours of reaction, a sample was taken from the outlet of the reactor to detect that the residual D-pantolactone was 0.2%. Start to connect the reaction solution into the solvent recovery device, stop the reaction after 10 hours of receiving, and receive a total of 25.8kg. Then the recovery device recovers the solvent under reduced pressure at 1kPa. After the recovery, 15.8 kg of D-panthenol, a light yellow transparent viscous liquid, is obtained, with a yield of 100%, and a residual amount of 3-aminopropanol of 0.2%. The water content is detected to be 0.9%, and the specific rotation is [α] D 20 =+29.9°. ...

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PUM

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Abstract

The invention discloses a preparation method of Dexpanthenol. The method comprises the following steps: dissolving a D-pantolactone rude product with a solvent, performing decolorizing and filtering to obtain a D-pantolactone solution, and continuously introducing the D-pantolactone solution and 3aminopropanol into a continuous reactor to carry out continuous reaction. And carrying out post-treatment on the obtained reaction solution to obtain the Dexpanthenol. According to the preparation method, the amplification effect in large-scale production can be eliminated, and the problem of solventresidue can be solved.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a preparation method of D-panthenol. Background technique [0002] Panthenol, also known as 2,4-dihydroxy-N-(3-hydroxypropyl)-3,3-dimethylbutanamide or N-panthenyl-3-propanolamine, is the alcohol corresponding to pantothenic acid. Panthenol, commonly known as provitamin B5, belongs to the category of B vitamins. Ubiquinol can be divided into three forms: DL-form, D-form, and L-form. Only the dextrorotary form has biological activity, and the L-form has no biological activity. [0003] D-panthenol, also known as dexpanthenol, is a very viscous liquid, and its viscosity is above 10,000 centipoise at 40°C. D-panthenol is the equivalent of D-pantothenic acid, widely used in medical, food and cosmetic industries, specific preparations such as oral liquids, eye drops, multivitamin injections, shampoos, mousses, moisturizers, etc. [0004] Panthenol can be prepared by ch...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C231/24C07C235/08C07D307/33
CPCC07C231/02C07C231/24C07D307/33C07B2200/07C07C235/08
Inventor 王玉岗李博彭志国张伟王钰孙勇李守垒
Owner SHANDONG NHU FINE CHEM SCI & TECH CO LTD
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