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Solution concentration on-line detection method in solventing-out crystallization process and special device thereof

A technology of solution concentration and dissolution crystallization, applied in the measurement of color/spectral characteristics, etc., can solve the problems of long detection time, poor repeatability and accuracy, and achieve short detection time, good accuracy and reproducibility, and the influence of external factors. small effect

Active Publication Date: 2010-07-28
STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem solved by the present invention is to solve the shortcomings of the prior art such as long detection time, poor stability, repeatability and accuracy, and provide a fast and effective online detection method and special device for solution concentration in the process of dissolution and crystallization

Method used

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  • Solution concentration on-line detection method in solventing-out crystallization process and special device thereof
  • Solution concentration on-line detection method in solventing-out crystallization process and special device thereof
  • Solution concentration on-line detection method in solventing-out crystallization process and special device thereof

Examples

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Effect test

Embodiment 1

[0026] On-line concentration detection of artemether dissolution and crystallization process, the solvent is ethanol, and the anti-solvent is water. In this example, according to the method and steps of the present invention, the absorbance R at the wavelength of 283nm in the ultraviolet region is taken, and according to the Lambert-beer law, the relational expression of the system is established as follows:

[0027] R=(-6.95W+8.15)x+(-0.25W-0.82)

[0028] The specific implementation process: put 250ml of artemether ethanol solution with a concentration of 0.15g / g solvent in a 500ml crystallization kettle, start stirring and keep it at 200rpm, turn on the temperature control and keep it at 25°C. Turn on the feed pump, add anti-solvent water at a rate of 5ml / min, and carry out elution and crystallization, and the crystallization time is 30min. During the crystallization process, the sampling pump is turned on to send the sample into the detection pool, and the ultraviolet fibe...

Embodiment 2

[0030] Online concentration detection of inosinic acid IMP dissolution and crystallization process, the solvent is water, and the anti-solvent is ethanol. In this example, according to the method and steps of the present invention, the absorbance R at the wavelength of 280nm in the ultraviolet region is taken, and according to the Lambert-beer law, the relational expression of the system is established as follows:

[0031] R=(3.88W+1.44)x+(-0.03W+2.01)

[0032]The specific implementation process: put 200ml of IMP aqueous solution with a concentration of 0.10g / g solvent in a 500ml crystallization kettle, start stirring and keep it at 200rpm, turn on the temperature control and keep it at 25°C. Turn on the feed pump, add anti-solvent ethanol at a rate of 10ml / min, and carry out elution and crystallization, and the crystallization time is 30min. During the crystallization process, the sampling pump is turned on to send the sample into the detection pool, and the ultraviolet fibe...

Embodiment 3

[0034] On-line concentration detection of guanylic acid GMP dissolution and crystallization process, the solvent is water, and the anti-solvent is ethanol. In this example, according to the method and steps of the present invention, the absorbance R at the wavelength of 275nm in the ultraviolet region is taken, and according to the Lambert-beer law, the relational expression of the system is established as follows:

[0035] R=(6.03W+0.96)x+(-0.02W+2.11)

[0036] The specific implementation process: put 200ml of GMP aqueous solution with a concentration of 0.10g / g solvent in a 500ml crystallization kettle, start stirring and keep it at 200rpm, turn on the temperature control and keep it at 25°C. Turn on the feed pump, add anti-solvent ethanol at a rate of 10ml / min, and carry out elution and crystallization, and the crystallization time is 30min. During the crystallization process, the sampling pump is turned on to send the sample into the detection pool, and the ultraviolet fi...

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Abstract

The invention relates to a solution concentration on-line detection method in the solventing-out crystallization process and a special device thereof. The method comprises the following steps: A. filtering samples through a sampling tube with a microfilter arranged at the front end for filtering and removing crystal grains in solution, and then, using a sampling pump for continuously pumping the samples from a crystallization kettle and conveying the samples to a detection tank; B. adopting a ultraviolet optical fiber spectrometer for continuously recording the ultraviolet absorption spectrum of the solution in the detection tank and transferring the ultraviolet absorption spectrum to a computer to be recorded in real time, and making the tested solution flow back to the crystallization kettle; and C. after correcting the continuously recorded ultraviolet detection spectrum in the computer by an orthogonal signal correction OSC method, taking the light absorbance value R under any wave length within 200nm to 400nm from the ultraviolet region, using a least square method to obtain a calculation factor in a Lambert-beer law calculation method, and further working out the solute concentration x of the solution to be tested in certain time. The method has the advantages of short detection time, capability of realizing on-line detection, small temperature influence, high precision, good reproducibility, simple detection device and low cost.

Description

technical field [0001] The invention belongs to the technical field of on-line detection, and in particular relates to an on-line detection method and a special device for solution concentration in a dissolution and crystallization process. Background technique [0002] Crystallization is a widely used chemical separation and purification unit operation, widely used in the production process of pharmaceuticals, food, fertilizers, soda ash, chemical reagents, rubber, plastics, polymers, vitamins, building materials, explosives and other products. Dissolution crystallization belongs to the category of solution crystallization, with low operating temperature and low energy consumption. It is especially suitable for the preparation of heat-sensitive organic substances such as nucleotides, amino acids, drugs, explosives, etc., and has been more and more widely used in recent years. In the dissolution and crystallization process, the degree of supersaturation is the driving force ...

Claims

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Application Information

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IPC IPC(8): G01N21/33
Inventor 江燕斌张扬张端科郑明英李凯霞钱宇
Owner STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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