Acetonitrile Purification Process for UPLC-MS
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Solution Overview
Problem
Current acetonitrile purification processes for ultrahigh performance liquid chromatography-mass spectrometry (UPLC-MS) are inefficient, resulting in low yield and high costs, and fail to meet stringent purity requirements for water, evaporation residues, and metal ions, while also generating environmental pollution during adsorption column regeneration.
Innovation Solution
An improved acetonitrile purification process involving oxidation, adsorption, rectification, and filtration steps, using an oxidizing agent and adsorbents in a tower system with controlled parameters to achieve high-purity acetonitrile, replacing the adsorption column with an adsorption and rectification tower to enhance regeneration efficiency and reduce environmental impact.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If conventional purification methods (oxidation, dehydrogenation, heavy component removal, adsorption, rectification) are used, then some purification is achieved, but the yield is low and the cost is high
Solution Approach 1:
The patent combines multiple purification operations (oxidation, adsorption, rectification) into an integrated continuous process system where the oxidized acetonitrile is directly fed into the adsorption and rectification tower without intermediate separation steps, improving yield while maintaining purity
Solution Approach 2:
The patent implements continuous production through a continuous oxidation process followed by continuous adsorption and rectification, eliminating batch processing interruptions and improving overall yield while maintaining consistent purity standards
2Productivity
If conventional purification methods are used, then some purification is achieved, but the purity is insufficient to meet UPLC-MS requirements
Solution Approach 1:
The patent controls specific parameters including tower height (7-30m), pressure difference (30-40kPa), temperature (80-90°C), and reaction time (1-6h) to optimize both purification effectiveness and production efficiency, achieving UPLC-MS grade purity at lower cost
Solution Approach 2:
The patent replaces manual adsorption column regeneration with an automated continuous adsorption and rectification tower system that uses controlled pressure differences and temperature gradients to achieve purification, reducing operational costs while maintaining high purity
3Ease of operation
If an adsorption column is used for adsorption operation, then adsorption is achieved, but the regeneration process is tedious and produces waste water
Solution Approach 1:
The adsorption and rectification tower system automatically regenerates the adsorbent in-situ through the continuous flow process and pressure differential, eliminating the need for manual regeneration operations and waste water discharge
Solution Approach 2:
The patent extracts the harmful regeneration step from the conventional adsorption process by integrating it into the continuous rectification tower operation, where the adsorbent is regenerated in-place without producing waste water
Applied Scientific Principles
This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.
Function Achieved in This Case
The process achieves a high-purity acetonitrile product with a yield greater than 95%, meeting UPLC-MS standards, while reducing waste and operational intensity, and minimizing environmental pollution through continuous production and efficient regeneration.
Implementation Method 1
adding an oxidizing agent into industrial acetonitrile containing impurities, water and acetonitrile to perform oxidation reaction
Implementation Method 2
feeding the product into an adsorption and rectification tower for adsorption
Implementation Method 3
condensing the obtained tower top product of the adsorption and rectification tower
Implementation Method 4
adding a drying agent into the crude product for drying
Implementation Method 5
heating and entering a reflux rectifying tower for total reflux after removing water, removing heavy component impurities at the tower bottom
Implementation Method 6
extracting and condensing light component impurities and acetonitrile at the tower top
Implementation Method 7
filtering, the semi-finished product extracted later to obtain a finished product
Data Source
AI summary
The present invention relates to the technical field of acetonitrile refining, and in particular, to an improved acetonitrile purification process for an ultrahigh performance liquid chromatography-mass spectrometer. The present invention provides an acetonitrile purification process. A high-purity finished product may be obtained by performing operations of oxidation, rectification adsorption, drying, reflux rectification and filtration on industrial acetonitrile and controlling related parameters such as temperature, flow and the like, continuous production is ensured, a light transmittance of the finished product in ultraviolet rays of 200 to 260 nm is greater than or equal to 95%, water and impurities in the industrial acetonitrile are removed, and the requirements of the ultrahigh performance liquid chromatography-mass spectrometer are met; moreover, by controlling process parameters and equipment.