An improved ultra-high liquid chromatography-mass spectrometer purification method using acetonitrile

A purification method and an improved technology, applied in the direction of instruments, scientific instruments, measuring devices, etc., can solve problems such as waste water, high personnel operation intensity, and environmental impact

Active Publication Date: 2022-04-19
FTSCI HUBEI BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, in the process of acetonitrile purification, the adsorption column is generally used for adsorption operation. In order to reduce the cost, the adsorption column needs to be regenerated. have a certain amount of impact

Method used

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  • An improved ultra-high liquid chromatography-mass spectrometer purification method using acetonitrile
  • An improved ultra-high liquid chromatography-mass spectrometer purification method using acetonitrile
  • An improved ultra-high liquid chromatography-mass spectrometer purification method using acetonitrile

Examples

Experimental program
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Effect test

Embodiment 1

[0105] This example provides an improved acetonitrile purification process, including the following steps:

[0106] (1) Add industrial acetonitrile containing impurities, water and acetonitrile to the oxidant, the weight percentage of the oxidant industrial acetonitrile is 0.01wt%, and the oxidant is a mixture of potassium superoxide, potassium hydroxide and sodium hydroxide, and the weight ratio is 1:5:8, after oxidation reaction at 80°C and 10KPa pressure for 1 hour, it is sent to the adsorption rectification tower for adsorption, and the obtained top product of the adsorption rectification tower is condensed to obtain a crude product; the adsorption essence The height of the distillation tower is 7m, and the pressure difference between the top and the bottom of the tower is 30kPa, and the number of the adsorption rectification towers is 2, connected in parallel, and 2 adsorption rectification towers are connected with the controller respectively; The rectifying tower is fil...

Embodiment 2

[0114] This example provides an improved acetonitrile purification process, including the following steps:

[0115] (1) Add industrial acetonitrile containing impurities, water and acetonitrile to the oxidant, the weight percentage of the oxidant industrial acetonitrile is 1wt%, and the oxidant is a mixture of potassium superoxide, potassium hydroxide and sodium hydroxide, and the weight ratio is 1 : 5:8, after oxidation reaction at 90°C and 90KPa pressure for 6 hours, it is sent to the adsorption rectification tower for adsorption, and the obtained top product of the adsorption rectification tower is condensed to obtain a crude product; the adsorption rectification The height of the tower is 30m, and the pressure difference between the tower top and the bottom of the tower is 40kPa, and the number of the adsorption rectification towers is 2, connected in parallel, and 2 adsorption rectification towers are connected with the controller respectively; Packing adsorbent in the di...

Embodiment 3

[0123] This example provides an improved acetonitrile purification process, including the following steps:

[0124] (1) Add the industrial acetonitrile containing impurity, water and acetonitrile to oxidant, the weight percent of described oxidant industrial acetonitrile is 0.1wt%, and described oxidant is the mixture of potassium superoxide, potassium hydroxide and sodium hydroxide, and the weight ratio is 1:5:8, after oxidation reaction at 90°C and 60KPa pressure for 4 hours, it is sent to the adsorption rectification tower for adsorption, and the obtained top product of the adsorption rectification tower is condensed to obtain a crude product; the adsorption essence The height of the distillation tower is 20m, and the pressure difference between the tower top and the bottom of the tower is 40kPa, and the number of the adsorption rectification towers is 2, connected in parallel, and 2 adsorption rectification towers are connected with the controller respectively; The rectify...

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Abstract

The invention relates to the technical field of acetonitrile purification, more specifically, the invention relates to an improved acetonitrile purification process for ultra-high liquid chromatography-mass spectrometry. The invention provides an acetonitrile purification process, through the operation of oxidation, rectification and adsorption, drying, reflux rectification and filtration of industrial acetonitrile, and related parameters such as temperature and flow are controlled, high-purity finished products can be obtained to ensure continuous production, Its transmittance of ultraviolet light at 200-260nm is greater than or equal to 95%, removes water and impurities in industrial acetonitrile, and meets the requirements of ultra-high liquid chromatography-mass spectrometry; and by controlling process parameters and equipment, the finished product can be improved. The yield reaches more than 95%, and the purification efficiency is improved; in addition, the present invention replaces the adsorption column by using an adsorption rectification tower, which can increase the regeneration efficiency and reduce environmental pollution while improving the purity.

Description

technical field [0001] The invention relates to the technical field of acetonitrile purification, more specifically, the invention relates to an improved acetonitrile purification process for ultra-high liquid chromatography-mass spectrometry. Background technique [0002] UPLC-MS reagents, also known as ultra-high performance liquid chromatography-mass spectrometry reagents, generally refer to special solvents or reagents for chromatography. The UV transmittance at low wavelengths is relatively good. The indicators have strict and demanding requirements. Some indicators require to reach the ppb level, and some even require to reach the ppt level. UPLC-MS reagent refers to the standard reagent used in ultra-high performance liquid chromatography-mass spectrometry. Under chromatographic conditions, only the peak of the specified compound appears, and impurity peaks cannot appear, or the background noise peak is required to be lower than the sensitivity of the instrument. UPLC...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72C07C253/34C07C255/03C07C255/07
Inventor 文胜赵正崇龚春丽程凡刘海胡富强
Owner FTSCI HUBEI BIOTECH CO LTD
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