Method for preparing palmitoyl chloride

A technology of palmitoyl chloride and palmitic acid, which is applied in the field of palmitoyl chloride preparation, can solve the problems of high energy consumption and high recovery cost of distilling thionyl chloride, difficulty in separating palmitoyl chloride, and high reaction yield, so as to achieve easy industrial production and avoid The effect of a large amount of use and easy-to-obtain raw materials

Active Publication Date: 2013-03-06
GUANGDONG GUANGYI TECH IND
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Problems solved by technology

Although the reaction conversion rate of phosphorus trichloride or phosphorus pentachloride reaction method is high, a large amount of solid phosphorus trichloride or phosphorus pentachloride and related phosphides remain after the reaction, which makes it difficult to separate palmitoyl chloride; solvent reaction method conversion The rate is about 85%, and the use of solvent and residual thionyl chloride to distill the energy consumption and recovery cost are higher; the palmitic acid melting reaction method avoids the use of solvents, and uses excess thionyl chloride as solvent, the reaction yield is higher, and two Thionyl chloride can be distilled and recycled for reuse
However, the palmitic acid melting reaction method also has its disadvantages. The reaction time of this method is relatively long, and a catalyst is needed to improve its reaction rate, otherwise it is difficult to industrialize

Method used

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  • Method for preparing palmitoyl chloride

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Effect test

Embodiment 1

[0022] The preparation method of palmitoyl chloride: add palmitic acid (10mol, 2564g) and thionyl chloride (20mol, 2379g) into a magnetic stirring reaction kettle, then add 5ml N, N-dimethylformamide, heat to 60°C and stir for 1.5 hour; after the reaction finished, the reactant in the magnetic stirring reactor was poured into the distiller, 65 ℃ vacuum rotary evaporation, the pressure control in the distiller was 0.08Mpa in vacuum degree, and reclaimed thionyl chloride condensate, finally 2692g of colorless palmitoyl chloride liquid was obtained, the content of palmitoyl chloride was 97.0%, and the yield was 95%.

Embodiment 2

[0024] The preparation method of palmitoyl chloride: add palmitic acid (10mol, 2564g) and thionyl chloride (20mol, 2379g) into a magnetic stirring reaction kettle, then add 5ml N,N-dimethylformamide, heat to 75°C and stir to react 2 hours; after the reaction, the reactant in the magnetic stirring reactor was poured into the distiller, 80 DEG C vacuum rotary evaporation, the pressure in the distiller was controlled at a vacuum degree of 0.08Mpa, and the thionyl chloride condensate was recovered, Finally, 2692g of colorless palmitoyl chloride liquid was obtained, the content of palmitoyl chloride was 97.0%, and the yield was 95%.

Embodiment 3

[0026] The preparation method of palmitoyl chloride: add palmitic acid (10mol, 2564g) and thionyl chloride (30mol, 3569g) into a magnetic stirring reaction kettle, then add 5ml N,N-dimethylformamide, heat to 75°C and stir to react 2 hours; after the reaction, pour the reactant in the magnetic stirring reactor into the distiller, 90 DEG C vacuum rotary evaporation, the pressure in the distiller is controlled at a vacuum degree of 0.08Mpa, and the thionyl chloride condensate is recovered, Finally, 2693g of colorless palmitoyl chloride liquid was obtained, the content of palmitoyl chloride was 98.2%, and the yield was 96%.

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Abstract

The invention relates to the technical field of preparation of palmitoyl chloride, in particular to a method for preparing the palmitoyl chloride from palmitic acid and thionyl chloride. In the method, the palmitic acid and the thionyl chloride are reacted at the temperature of between 60 and 75 DEG C for 0.5 to 2 hours in a magnetic stirring reaction kettle in the presence of organic amine to form the palmitoyl chloride. The method has the advantages of readily available raw materials, simple process equipment, low energy consumption, low cost, particularly quick reaction in the whole process, and easy industrial production.

Description

technical field [0001] The invention relates to the technical field of palmitoyl chloride preparation, in particular to a method for preparing palmitoyl chloride by using palmitic acid and thionyl chloride. Background technique [0002] Palmitoyl chloride is an important raw material of ascorbyl palmitate, and its quality directly affects the purity and yield of ascorbyl palmitate products. At present, regarding the preparation of palmitoyl chloride, there are three methods reported in the data: phosphorus trichloride or phosphorus pentachloride reaction method, solvent reaction method and palmitic acid melting reaction method. Although the reaction conversion rate of phosphorus trichloride or phosphorus pentachloride reaction method is high, a large amount of solid phosphorus trichloride or phosphorus pentachloride and related phosphides remain after the reaction, which makes it difficult to separate palmitoyl chloride; solvent reaction method conversion The rate is about ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/42C07C51/60
Inventor 梁嘉臻王力林跃先
Owner GUANGDONG GUANGYI TECH IND
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