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Preparation method of benzyl salicylate

A technology of benzyl salicylate and salicylic acid, which is applied in the field of preparation of benzyl salicylate, can solve the problems of pungent aroma, high production cost and low purity of benzyl salicylate, so as to improve production efficiency, The effect of shortening the reaction time and increasing the specific surface area

Pending Publication Date: 2021-09-21
宁夏万香源生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of this, it is necessary to provide a kind of preparation method of benzyl salicylate to solve the high production cost of benzyl salicylate, low purity, the problem of pungent aroma

Method used

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Examples

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preparation example Construction

[0022] The embodiment of the present invention provides a high-efficiency synthesis method of salicylic acid, comprising the following steps:

[0023] (S 1 ) High-efficiency dehydration of sodium phenate solution: put sodium phenate solution into a medium pressure kettle, remove part of the water under reduced pressure, and then add phenol, in which part of phenol and water form a binary azeotrope, and the binary azeotrope is dehydrated under negative pressure conditions Separating to obtain dry bulky compound, said bulky compound is made up of phenol and sodium phenate;

[0024] (S 2 ) Carboxylation reaction: CO is introduced into the dry bulky compound above 2 , Sodium phenate and CO in the bulky compound 2 The reaction generates sodium salicylate, and after the reaction is over, the phenol that does not participate in the reaction is separated under negative pressure conditions to obtain sodium salicylate;

[0025] (S 3 ) Preparation of benzyl salicylate: react sodium ...

Embodiment 1

[0038] (S 0 ) Preparation of sodium phenoxide solution: take by weighing 90kg of sodium hydroxide, prepare a 40% solution with distilled water, weigh 200kg of phenol, prepare a 54% solution with distilled water, add the phenol solution into the sodium hydroxide solution to react, control The reaction temperature is 80° C., and the reaction time is 10 to 15 minutes to obtain a sodium phenoxide solution.

[0039] (S 1 ) High-efficiency dehydration of sodium phenate solution: put 590kg of the above-mentioned sodium phenate solution into a medium pressure kettle, vacuumize, start decompression distilling, and when the solution becomes thick, check the water content, and stop decompression distilling when the water content is about 45% , the distilled water is reused (S 0 ) step to prepare sodium hydroxide lye, add 200kg of phenol to the obtained sodium phenate fluid, vacuumize, heat up to 90°C, evaporate and collect the binary azeotrope formed by water and part of phenol, and th...

Embodiment 2

[0053] (S 0 ) Preparation of sodium phenoxide solution: take by weighing 90kg of sodium hydroxide, prepare a 40% solution with distilled water, weigh 200kg of phenol, prepare a 54% solution with distilled water, add the phenol solution into the sodium hydroxide solution to react, control The reaction temperature is 80° C., and the reaction time is 10 to 15 minutes to obtain a sodium phenoxide solution.

[0054] (S 1 ) High-efficiency dehydration of sodium phenate solution: put 590kg of the above-mentioned sodium phenate solution into a medium pressure kettle, vacuumize, start decompression distilling, and when the solution becomes thick, check the water content, and stop decompression distilling when the water content is about 45% , the distilled water is reused (S 0 ) step to prepare sodium hydroxide lye, add 210kg of phenol to the obtained sodium phenate fluid, vacuumize, heat up to 90°C, evaporate and collect the binary azeotrope formed by water and part of phenol, and th...

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Abstract

A preparation method of benzyl salicylate belongs to the technical field of preparation of perfume compounds, and comprises the following steps: by taking cheap phenol and sodium phenolate as raw materials, firstly vacuumizing a sodium phenolate solution for partial dehydration, then adding phenol into the sodium phenolate solution, forming a binary azeotrope by part of phenol and water, and separating the binary azeotrope under a negative pressure condition to achieve the purpose of bringing out water by phenol. Meanwhile, the residual phenol and sodium phenate form a bulky compound under vacuum, and due to the fact that the specific surface area of the bulky compound is large, when CO2 is introduced for carboxylation reaction, the reaction rate is increased, the reaction time is greatly shortened, the production efficiency is improved, and the production cost is reduced. The prepared benzyl salicylate is subjected to steam impact steaming under the high vacuum condition, impurity gas is removed, the purity of the benzyl salicylate is effectively improved, and the fragrance of the product is fresh and quietly elegant.

Description

technical field [0001] The invention belongs to the technical field of preparation of perfume compounds, and in particular relates to a preparation method of benzyl salicylate. Background technique [0002] Benzyl salicylate, also known as benzyl o-hydroxybenzoate, has ambergris-like and amber-like aromas. It is often used as a diluent, blending agent, and fixative for floral and non-floral flavors. It is widely used in fragrances industry; and it is an additive of cosmetics, used in sunscreen cosmetics, which can protect the skin from ultraviolet rays; at the same time, it can also be used as a modifier of pesticides and plastics or an intermediate of pharmaceutical products, which has a wide range of applications . [0003] At present, the synthetic method of benzyl salicylate mainly contains esterification method and condensation method, and esterification method is traditional synthetic method, but cost is higher, and productive rate is low; The condensation reaction o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/84C07C67/10C07C67/48
CPCC07C67/10C07C67/48C07C51/41C07C69/84C07C65/10
Inventor 宋公龙沈华杨育清李向前
Owner 宁夏万香源生物科技有限公司
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