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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 the amplification effect of the preparation reaction is serious.
First of all, local over-temperature deterioration or insufficient reaction are common in industrial production, and the control of product quality is facing great challenges; secondly, with the expansion of the reaction scale, the reaction time extended by multiples also greatly limits the production capacity of the product
The capacity of the existing process is gradually difficult to meet the increasing market demand

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 recovers s...

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 viscou...

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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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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