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Non-catalytic acetylation reaction in supercritical CO2 and online detection method thereof

A non-catalytic acetylation and detection method technology, which is applied in the application of supercritical fluid CO2 analysis technology and the field of green synthetic chemistry, can solve the problems of poor accuracy and reproducibility, and achieve high accuracy, moderate reaction temperature and good reproducibility Effect

Pending Publication Date: 2021-01-12
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the invention is to provide a supercritical CO 2 Non-catalyzed acetylation reaction and its online detection method, the method can carry out the acetylation reaction at a lower temperature and without the use of a catalyst, and track the dissolution equilibrium process of the reactant, the acetylation reaction process and the product dissolution equilibrium online The process and product distribution solve the problems of the existing acetylation reaction technology that requires a catalyst, and the accuracy and reproducibility of the online tracking test results are poor.

Method used

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  • Non-catalytic acetylation reaction in supercritical CO2 and online detection method thereof
  • Non-catalytic acetylation reaction in supercritical CO2 and online detection method thereof
  • Non-catalytic acetylation reaction in supercritical CO2 and online detection method thereof

Examples

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Embodiment 1

[0046] [Example 1] in supercritical CO 2 Acetylation of 2-aminophenol in medium and its on-line detection

[0047] 10-20mg of 2-aminophenol is operated according to the operation steps (1)-(5). The specific operating conditions are that the reaction kettle and the external circulation loop are both at 50°C, the magnetic stirring speed of the reaction kettle is 1800rpm, the speed of the gear pump is 2400rpm; the constant temperature is 20min , during which the reactor was pressurized to 20MPa, CO 2 Pump pressurization rate 10mL / min, CO 2 Density 785 kg / m 3 . Before each acetylation reaction starts, earlier the reactant 2-aminophenol in the reactor is continuously sampled and analyzed on-line, and the numerical change (peak area and retention time) of each sampling analysis is compared, such as Figure 4 Shown in 1# and 2# peaks. After 2-aminophenol reaches the dissolution equilibrium, add 0.5-1.5mL of acetic anhydride acetonitrile solution into the reactor to initiate the ...

Embodiment 2

[0053] [Example 2] in supercritical CO 2 Acetylation of 4-aminophenol in medium and its on-line detection

[0054] 10-20mg of 4-aminophenol is operated according to the operation steps (1)-(5). The specific operating conditions are that the reaction kettle and the external circulation loop are both at 50°C, the magnetic stirring speed of the reaction kettle is 1800rpm, the speed of the gear pump is 2400rpm; the constant temperature is 20min , during which the reactor was pressurized to 20MPa, CO 2 Pump pressurization rate 10mL / min, CO 2 Density 785 kg / m 3 . Before each acetylation reaction starts, earlier the reactant 4-aminophenol in the reactor is continuously sampled and analyzed on-line, and the numerical change (peak area and retention time) of each sampling analysis is compared, such as Figure 4 Shown in 1# and 2# peaks. After 4-aminophenol reaches the dissolution equilibrium, add 0.5-1.5mL of acetic anhydride acetonitrile solution into the reactor to initiate the ...

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Abstract

The invention discloses a non-catalytic acetylation reaction in supercritical CO2 and an online detection method thereof. According to the method, dissolving aniline or aminophenol or methylaniline ormethoxyaniline in the supercritical CO2 to reach solubility equilibrium, then adding an acetic anhydride acetonitrile solution according to a molar ratio of aniline or aminophenol or methylaniline ormethoxyaniline to acetic anhydride of 1.1-1.5 to initiate an acetylation reaction; in the supercritical CO2 acetylation reaction process, the reaction kettle and the supercritical CO2 chromatographyare connected through the outer circulation loop, online sampling analysis and detection of the acetylation reaction are achieved, and the acetylation reaction process is monitored. The invention develops a green and efficient acetylation reaction and a method for quickly and accurately monitoring the reaction process, and solves the technical problems that the existing acetylation reaction technology needs a catalyst, the accuracy of an online tracking detection result is poor, the reproducibility is poor and the like.

Description

technical field [0001] A supercritical CO 2 Non-catalytic acetylation reaction and its online detection method, belonging to supercritical fluid CO 2 Analytical technology application and green synthetic chemistry. Background technique [0002] With the expansion of the application fields of acetaminophen acetylation reaction products and the increasingly stringent environmental protection policies, the original synthesis and analysis detection methods can no longer meet the needs of industry development. The development of green and efficient acetylation reaction methods and the rapid and accurate monitoring of the acetylation reaction process are key issues that need to be solved urgently. [0003] Supercritical CO 2 It is a cheap, easy-to-obtain and environment-friendly solvent with mild critical conditions, low viscosity and high diffusivity. 2 Carrying out chemical synthesis reactions in the medium can increase the chemical reaction rate, significantly reduce the te...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/74G01N30/54C07C231/02C07C233/25
CPCG01N30/02G01N30/06G01N30/74G01N30/54C07C231/02C07C233/25Y02P20/54
Inventor 李犇郭威
Owner UNIV OF SCI & TECH LIAONING
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