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Novel method for preparing acetylsalicylic acid

A technology of acetylsalicylic acid and a new method, which is applied in the field of preparation of acetylsalicylic acid, can solve problems such as the inability to strengthen the reaction process safely and effectively, and achieve the effects of shortening the reaction time, geochemical reaction process, and efficient reaction

Inactive Publication Date: 2018-06-08
浙江省衢州第二中学
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional batch reactor preparation process is limited by the temperature and pressure of the equipment, and cannot safely and effectively strengthen the reaction process. The continuous flow reaction device has the advantages of high pressure resistance, high temperature, and high heat exchange capacity, which can strengthen the traditional batch reactor process. , while the process is safe and reliable

Method used

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  • Novel method for preparing acetylsalicylic acid
  • Novel method for preparing acetylsalicylic acid

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0032] Example 1: Reaction of salicylic acid and acetic acid to prepare acetanilide

[0033] 10m of stainless steel tube with an inner diameter of 5mm and an outer diameter of 6mm is divided into a reaction part of 5m and a cooling part of 5m. The stainless steel tube of the reaction part is immersed in a high-temperature methyl silicone oil bath, and the cooling part of 5m is cooled by a low-temperature constant temperature water bath. Stir and mix 13.8g (0.1mol) of o-hydroxybenzoic acid and 51.8g (0.5mol) of acetic anhydride, and slowly add 1g (98%wt, 0.01mol) of concentrated sulfuric acid, the reaction mixture is light yellow and clear, with a total volume of 50ml. Set the oil bath temperature to 160°C, the water bath temperature to 45°C, the feed pump pressure to 1.5MPa, and the flow rate to 20ml / min. After the temperature and pressure of each part of the continuous flow tubular reactor are stabilized, start feeding. It takes 4.9 minutes for the reaction material to flow t...

example 2

[0034] Example 2: Reaction of salicylic acid and acetic acid to prepare acetanilide

[0035] 10m of stainless steel tube with an inner diameter of 5mm and an outer diameter of 6mm is divided into a reaction part of 5m and a cooling part of 5m. The stainless steel tube of the reaction part is immersed in a high-temperature methyl silicone oil bath, and the cooling part of 5m is cooled by a low-temperature constant temperature water bath. Stir and mix 69 g (0.5 mol) of o-hydroxybenzoic acid and 259 g (2.5 mol) of acetic anhydride, and slowly add 5 g (98% wt, 0.05 mol) of concentrated sulfuric acid. The reaction mixture is light yellow and clear, with a total volume of 240 ml. Set the temperature of the oil bath to 180°C, the temperature of the water bath to 45°C, the pressure of the feed pump to 1.6MPa, and the flow rate to 50ml / min. After the temperature and pressure of each part of the continuous flow tube reactor are stabilized, start to feed the material. It takes 2 minutes ...

example 3

[0036] Example 3: Reaction of salicylic acid and acetic acid to prepare acetanilide

[0037] 8m copper tube with an inner diameter of 8mm and an outer diameter of 10mm is divided into a reaction part of 4m and a cooling part of 4m. The reaction part of the copper tube is immersed in a high temperature methyl silicone oil bath, and the cooling part of 5m is cooled by a low temperature constant temperature water bath. Stir and mix 138g (1mol) of o-hydroxybenzoic acid and 460g (4.5mol) of acetic anhydride evenly, slowly add 10g (98%wt, 0.1mol) of concentrated sulfuric acid, the reaction mixture is light yellow and clear, with a total volume of 425ml. Set the temperature of the oil bath to 180°C, the temperature of the water bath to 60°C, the pressure of the feed pump to 1.6MPa, and the flow rate to 200ml / min. After the temperature and pressure of each part of the continuous flow tube reactor are stabilized, start feeding. The reaction material needs 2 minutes to flow through the ...

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Abstract

The invention discloses a novel method for preparing acetylsalicylic acid. The method comprises the following steps: adding reaction materials into a continuous flow tubular reactor for reaction, discharging a product, and carrying out cooling, extraction, concentration and purification. The temperature of a reaction part of the reactor is set at 150-250 DEG C, the residence time is 3-20min, the temperature of a cooling part is set at 0-80 DEG C, the residence time is 3-20min, the pressure of a feed pump is set to be 1.5-2.5MPa, and the feed speed is 20-200ml / min. The continuous flow reactor is adopted by the method provided by the invention, so that the method is more efficient and safe, can effectively strengthen the reaction process, shorten the reaction time and improve the reaction efficiency.

Description

technical field [0001] The invention belongs to the technical field of chemical products, and in particular relates to a preparation method of acetylsalicylic acid. Background technique [0002] Acetylsalicylic acid is the traditional antipyretic and analgesic drug aspirin. In recent years, it has been widely used in the field of medicine. In addition to the traditional anticoagulant, antipyretic, anti-inflammatory and anti-rheumatic effects, it also has good anti-cancer effects , so its market demand is gradually picking up. [0003] Esterification of salicylic acid and acetic anhydride is a classic synthesis method of acetylsalicylic acid. Common catalysts include sulfuric acid, phosphoric acid, vitamin C, oxalic acid and some inorganic bases. [0004] The traditional batch reactor preparation process is limited by the temperature and pressure of the equipment, and cannot safely and effectively strengthen the reaction process. The continuous flow reaction device has the a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/157
CPCC07C67/08C07C69/157
Inventor 廖恒一吕孜涵张玉林
Owner 浙江省衢州第二中学