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Method for online ultraviolet monitoring of 1H-Benzotriazole continuous crystallization process

A benzotriazole and ultraviolet technology, applied in the field of online analysis, can solve the problems of complex time-consuming, unsuitable needle-shaped crystal benzotriazole, etc., and achieve the effect of high accuracy and simple operation

Inactive Publication Date: 2021-02-12
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is not suitable for the special needle-like crystal benzotriazole, and there are few related studies on the continuous crystallization of needle-like crystals. There is no mention in the literature of trying to use other online monitoring equipment to monitor the crystal concentration in real time, but The method of static sampling and analysis of filtrate concentration or suspension density is too complicated and time-consuming. Therefore, the method of the present invention monitors the concentration change of needle-like crystal benzotriazole in the continuous crystallization process in real time through online ultraviolet light, and quickly judges that the continuous crystallization process is stable. State point, laying the foundation for subsequent experiments

Method used

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  • Method for online ultraviolet monitoring of 1H-Benzotriazole continuous crystallization process
  • Method for online ultraviolet monitoring of 1H-Benzotriazole continuous crystallization process
  • Method for online ultraviolet monitoring of 1H-Benzotriazole continuous crystallization process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] On-line UV monitoring of the continuous crystallization process of benzotriazole, the specific steps are as follows:

[0035] Spectral conditions: the wavelength range of the online ultraviolet spectrometer is 200-380nm; the online ultraviolet spectrometer is equipped with an attenuated total reflection ultraviolet probe, the number of scans is 119 times, the average number of times is 20 times, and the acquisition time is 2s / sheet.

[0036] Specific steps are as follows:

[0037] (1) Place the attenuated total reflection ultraviolet probe in the air, adjust the count value to 55000 by changing the integration time, open the light shield to turn off the light source, record and deduct the dark current; close the light shield to turn on the light source, and the attenuated total reflection ultraviolet Insert the probe into the pure water solvent, record and subtract the solvent background peak;

[0038] (2) Prepare a series of benzotriazole solutions with a concentratio...

Embodiment 2

[0044] On-line UV monitoring of the continuous crystallization process of benzotriazole, the specific steps are as follows:

[0045] Spectral conditions: the wavelength range of the online ultraviolet spectrometer is 200-380nm; the online ultraviolet spectrometer is equipped with an attenuated total reflection ultraviolet probe, the number of scans is 119 times, the average number of times is 20 times, and the spectrum acquisition time is 4s / sheet.

[0046] Specific steps are as follows:

[0047] (1) Place the attenuated total reflection ultraviolet probe in the air, adjust the count value to 55000 by changing the integration time, open the light shield to turn off the light source, record and deduct the dark current; close the light shield to turn on the light source, and the attenuated total reflection ultraviolet Insert the probe into the pure water solvent, record and subtract the solvent background peak;

[0048] (2) Prepare a series of benzotriazole solutions with a con...

Embodiment 3

[0054] On-line UV monitoring of the continuous crystallization process of benzotriazole, the specific steps are as follows:

[0055] Spectral conditions: the wavelength range of the online ultraviolet spectrometer is 200-380nm; the online ultraviolet spectrometer is equipped with an attenuated total reflection ultraviolet probe, the number of scans is 119 times, the average number of times is 20 times, and the acquisition time is 10s / sheet.

[0056] Specific steps are as follows:

[0057] (1) Place the attenuated total reflection ultraviolet probe in the air, adjust the count value to 55000 by changing the integration time, open the light shield to turn off the light source, record and deduct the dark current; close the light shield to turn on the light source, and the attenuated total reflection ultraviolet Insert the probe into the pure water solvent, record and subtract the solvent background peak;

[0058] (2) Prepare a series of benzotriazole solutions with a concentrati...

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Abstract

The invention discloses a method for online ultraviolet monitoring of a 1H-benzotriazole continuous crystallization process. The method mainly comprises the following steps: monitoring the concentration of 1H-benzotriazole in a system in real time through an attenuated total reflection ultraviolet spectrometer in the 1H-benzotriazole continuous crystallization process, and judging the degree of the continuous crystallization process by utilizing the ultraviolet characteristic peak position of 1H-benzotriazole and different absorbances at different moments. According to the method, the concentration change of 1H-benzotriazole in the continuous crystallization process can be monitored in real time, and a plurality of staying time needed for achieving the steady state in the 1H-benzotriazolecontinuous crystallization process is determined. For special acicular crystals, under the condition that equipment such as an FBRM and a Malvern laser particle size analyzer is not suitable, a staticmethod is not needed for sampling and analyzing the filtrate concentration or the suspension density, the operation is simple, the accuracy is high, and the steady-state point of the continuous crystallization process is judged at the second level.

Description

technical field [0001] The invention belongs to the technical field of on-line analysis, in particular to an on-line monitoring and analysis method for a continuous crystallization process, in particular to an on-line monitoring method for a continuous crystallization process of benzotriazole. Background technique [0002] Benzotriazole (Benzotriazole), also known as benzotriazole, benzotriazole, referred to as BTA; is an important fine chemical product, mainly used as corrosion inhibitor for copper and copper alloy, metal rust inhibitor, photographic Antifogging agent and organic synthesis intermediate; benzotriazole derivatives have strong biological activity and can be used in antibacterial, anticancer, anti-anxiety and other aspects. [0003] The crystallization process in the traditional pharmaceutical industry is mostly batch operation, however, the problems of batch-to-batch variation and low process efficiency still exist. As a method that can solve the above-mentio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/33G01N21/552
CPCG01N21/33G01N21/552G01N2201/129
Inventor 王学重张露张扬
Owner SOUTH CHINA UNIV OF TECH
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