Synthesis process of DL-panthenol
Through vacuum dehydration treatment and control of reaction conditions, the problems of low yield and high impurities in the traditional DL-panthenol synthesis process are solved, the yield and purity of the product are improved, and more efficient DL-panthenol synthesis is achieved.
Patent Information
- Application Number
- CN202411474359.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-22
- Publication Date
- 2025-01-14
AI Technical Summary
The traditional DL-panthenol synthesis process has low yield and high impurity content of the product, resulting in incomplete reactions and affecting subsequent processing and use.
DL-pantothenic acid lipid was treated by vacuum dehydration, and then the liquid triaminopropantool was heated in the reactor and the DL-pantothenic acid lipid raw material was added, and ethyl acetate solvent was added for crystallization. The reaction temperature and reagent ratio were controlled to ensure the thorough reaction. sex.
It improves the yield of DL-panthenol, reduces the impurity content, and ensures the purity and quality of the product.
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Figure SMS_1
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of wastewater treatment, in particular to a synthesis process of DL-panthenol. Background Art
[0002] DL-Panthenol is a deep penetrating moisturizer that can stimulate the growth of epidermal cells, easily absorb, penetrate and penetrate the stratum corneum on the surface of the skin, give the skin luster, prevent roughness and aging, and at the same time, it can also enter the inside of the hair to improve hair luster, reduce hair split ends, repair damaged hair and continuously moisturize the hair. Therefore, it is often added to shampoo, hair conditioner and skin care products.
[0003] The yield of the traditional DL-panthenol synthesis process is mostly only about 70%, with obvious incomplete reaction and too high impurity content in the product, which is not conducive to subsequent processing and use. Summary of the invention
[0004] The purpose of the present invention is to provide a synthesis process of DL-panthenol to solve the deficiencies in the prior art.
[0005] The technical solution adopted by the present invention is as follows: The synthesis process of DL-panthenol comprises the following steps: (1) Dehydration of DL-pantothenic acid lactone: The water content of DL-pantothenic acid lactone is treated to ≤ 0.08% under a vacuum environment to obtain the required DL-pantothenic acid lactone raw material, wherein the vacuum degree of the vacuum environment is -0.09 to -0.096 MPa, the temperature during the dehydration treatment is 105 to 115°C, and the treatment time is 2.5 hours.
[0006] (2) Synthesis reaction of DL-panthenol: firstly, liquid triaminopropanol is placed in a reaction kettle, and then the DL-pantothenic acid lactone raw material prepared in step (1) is added into the reaction kettle, the temperature is raised, then kept warm and then cooled, and ethyl acetate solvent is added to react, and after cooling, crystallization is carried out in a low temperature environment to synthesize DL-panthenol.
[0007] Preferably, the insulation temperature in step (2) is 90-98°C.
[0008] Preferably, the time of keeping warm after heating in step (2) is 4.5 to 5.5 hours.
[0009] Preferably, the temperature range of cooling before adding ethyl acetate in step (2) is 55-65°C.
[0010] Preferably, the low temperature environment described in step (2) has a temperature range of -20 to -5°C.
[0011] Preferably, the molar ratio of the DL-pantothenic acid lactone raw material to triaminopropanol in step (2) is 1-1.04:1-1.02, and the ratio of the mass of the ethyl acetate solvent to the total mass of the DL-pantothenic acid lactone raw material and triaminopropanol in step (2) is 1.1:1.3-1.0.
[0012] The beneficial effects of the present invention are as follows: during the treatment process of the crystallization process of the present invention, liquid triaminopropanol is used as a reaction base, DL-pantothenic acid lactone raw material is added thereto, the temperature is first raised to about 90 degrees Celsius for heat preservation, the activities of the two are fully activated before adding the reaction medium, the temperature is lowered to about 60 degrees Celsius, the reaction temperature is controlled and then ethyl acetate solvent is added, the content ratio of each reagent is fully controlled, impurities caused by incomplete reaction of raw materials due to excessive raw materials on one side can be effectively avoided, and the final cooling and crystallization can precipitate crystals from the solvent to the maximum extent, thereby improving the yield of the product and being worthy of promotion. DETAILED DESCRIPTION Example 1
[0013] The synthesis process of DL-panthenol comprises the following steps: (1) Dehydration of DL-pantothenic acid lactone: The water content of DL-pantothenic acid lactone is treated to ≤ 0.08% under a vacuum environment to obtain the required DL-pantothenic acid lactone raw material, wherein the vacuum degree of the vacuum environment is -0.09 to -0.096 MPa, the temperature during the dehydration treatment is 105 to 115°C, and the treatment time is 2.5 hours.
[0014] (2) Synthesis reaction of DL-panthenol: firstly, liquid triaminopropanol is placed in a reaction kettle, and then the DL-pantothenic acid lactone raw material prepared in step (1) is added into the reaction kettle, the temperature is raised, then kept warm and then cooled, and ethyl acetate solvent is added to react, and after cooling, crystallization is carried out in a low temperature environment to synthesize DL-panthenol.
[0015] The insulation temperature in step (2) is 90°C.
[0016] The time of keeping warm after heating in step (2) is 4.5 hours.
[0017] The temperature range of cooling before adding ethyl acetate in step (2) is 55°C.
[0018] The low temperature environment described in step (2) has a temperature range of -20°C.
[0019] The molar ratio of the DL-pantothenic acid lactone raw material to triaminopropanol in step (2) is 1:1, and the ratio of the mass of the ethyl acetate solvent to the total mass of the DL-pantothenic acid lactone raw material and triaminopropanol in step (2) is 1.1:1. Example 2
[0020] The synthesis process of DL-panthenol is characterized by comprising the following steps: (1) Dehydration of DL-pantothenic acid lactone: The water content of DL-pantothenic acid lactone is treated to ≤ 0.08% under a vacuum environment to obtain the required DL-pantothenic acid lactone raw material, wherein the vacuum degree of the vacuum environment is -0.09 to -0.096 MPa, the temperature during the dehydration treatment is 105 to 115°C, and the treatment time is 2.5 hours.
[0021] (2) Synthesis reaction of DL-panthenol: firstly, liquid triaminopropanol is placed in a reaction kettle, and then the DL-pantothenic acid lactone raw material prepared in step (1) is added into the reaction kettle, the temperature is raised, then kept warm and then cooled, and ethyl acetate solvent is added to react, and after cooling, crystallization is carried out in a low temperature environment to synthesize DL-panthenol.
[0022] The insulation temperature in step (2) is 95°C.
[0023] The heat preservation time after heating in step (2) is 5 hours.
[0024] The temperature range of cooling before adding ethyl acetate in step (2) is 60°C.
[0025] The low temperature environment described in step (2) has a temperature range of -10°C.
[0026] The molar ratio of the DL-pantothenic acid lactone raw material to triaminopropanol in step (2) is 1:1 to 1.02, and the ratio of the mass of the ethyl acetate solvent to the total mass of the DL-pantothenic acid lactone raw material and triaminopropanol in step (2) is 1.1:1.2. Example 3
[0027] The synthesis process of DL-panthenol is characterized by comprising the following steps: (1) Dehydration of DL-pantothenic acid lactone: The water content of DL-pantothenic acid lactone is treated to ≤ 0.08% under a vacuum environment to obtain the required DL-pantothenic acid lactone raw material, wherein the vacuum degree of the vacuum environment is -0.09 to -0.096 MPa, the temperature during the dehydration treatment is 105 to 115°C, and the treatment time is 2.5 hours.
[0028] (2) Synthesis reaction of DL-panthenol: firstly, liquid triaminopropanol is placed in a reaction kettle, and then the DL-pantothenic acid lactone raw material prepared in step (1) is added into the reaction kettle, the temperature is raised, then kept warm and then cooled, and ethyl acetate solvent is added to react, and after cooling, crystallization is carried out in a low temperature environment to synthesize DL-panthenol.
[0029] The insulation temperature in step (2) is 98°C.
[0030] The time of keeping warm after heating in step (2) is 5.5h.
[0031] The temperature range of cooling before adding ethyl acetate in step (2) is 65°C.
[0032] The low temperature environment described in step (2) has a temperature range of -5°C.
[0033] The molar ratio of the DL-pantothenic acid lactone raw material to triaminopropanol in step (2) is 1.04:1.02, and the ratio of the mass of the ethyl acetate solvent to the total mass of the DL-pantothenic acid lactone raw material and triaminopropanol in step (2) is 1.1:1.3.
[0034] Comparative Example 1 DL-panthenol is synthesized using traditional technology.
[0035] The specific indicators for comparison are:
[0036] It can be seen from the above table that the yield of the crystal of DL-panthenol prepared by the present invention is not only greatly improved, but also the content of impurities is reduced, indicating that the components are fully reacted during the reaction.
[0037] The above description is only a preferred embodiment of the present invention, but the present invention does not limit the scope of implementation. Any changes made in accordance with the concept of the present invention, or modifications to equivalent embodiments with equivalent changes, which still do not exceed the spirit covered by the description and embodiments, should be within the protection scope of the present invention.
Claims
1. A process for synthesizing DL-panthenol, characterized in that: The following steps are involved: (1) Dehydration of DL-pantolactone: The water content of DL-pantolactone is reduced to ≤0.08% under vacuum to obtain the required DL-pantolactone raw material, wherein the vacuum degree of the vacuum environment is -0.09 to -0.096 MPa, the temperature during the dehydration treatment is 105 to 115°C, and the treatment time is 2.5 hours; (2) Synthesis reaction of DL-panthenol: firstly, liquid triaminopropanol is placed in a reaction kettle, and then the DL-pantothenic acid lactone raw material prepared in step (1) is added into the reaction kettle, the temperature is raised, then kept warm and then cooled, and ethyl acetate solvent is added to react, and after cooling, crystallization is carried out in a low temperature environment to synthesize DL-panthenol.
2. The synthesis process of DL-panthenol according to claim 1, characterized in that: The insulation temperature in step (2) is 90-98°C.
3. The synthesis process of DL-panthenol according to claim 1, characterized in that: The time of keeping warm after heating in step (2) is 4.5 to 5.5 hours.
4. The process for synthesizing DL-panthenol according to claim 1, characterized in that: The temperature range of cooling before adding ethyl acetate in step (2) is 55-65°C.
5. The process for synthesizing DL-panthenol according to claim 1, characterized in that: The low temperature environment described in step (2) has a temperature range of -20 to -5°C.
6. The process for synthesizing DL-panthenol according to claim 1, characterized in that: The molar ratio of the DL-pantothenic acid lactone raw material to triaminopropanol in step (2) is 1-1.04:1-1.02, and the ratio of the mass of the ethyl acetate solvent to the total mass of the DL-pantothenic acid lactone raw material and triaminopropanol in step (2) is 1.1:1.3-1.0.