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Method for monitoring solubility, metastable zone and solution concentration on line in crystallization process of organic salt system

A solution concentration and solubility technology, applied in the field of process analysis, can solve the problems of patents and literature reports without online control, and achieve the effects of short measurement response time, wide measurement concentration range and simultaneous measurement

Active Publication Date: 2014-02-12
阜新达得利化工股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN101788464A proposes that the conductivity method is not suitable for monitoring the concentration of the organic system, and there is no literature using the conductivity method to monitor the crystallization process of organic salts in the organic solution system
[0008] In the previous research on the monitoring equipment and measurement methods of the organic system crystallization process of organic salts, there were no patents and literature reports on the online control of the crystallization process based on the measurement of the conductivity of the solution.

Method used

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  • Method for monitoring solubility, metastable zone and solution concentration on line in crystallization process of organic salt system
  • Method for monitoring solubility, metastable zone and solution concentration on line in crystallization process of organic salt system
  • Method for monitoring solubility, metastable zone and solution concentration on line in crystallization process of organic salt system

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Embodiment 1

[0044] In this embodiment, the experimental device is as attached figure 1 , crystallizer diameter D = 70mm, height H = 100mm, the impeller is a push-type double-bladed impeller. By controlling the temperature of the crystallizer, the concentrations of 1g / 100g, 5g / 100, 10g / 100g, 15g / 100g, 20g / 100g, 25g / 100g, 30g / 100g, 35g / 100g and 40g / 100% of the ethanol solution of flunixin meglumine was heated slowly from 5°C at a rate of 0.05K / min until the solids were completely dissolved, and the conductivity data during this process was recorded, and the conductivity data was plotted against the temperature. attached figure 2 In the middle is a curve diagram of the change of conductivity with the temperature rising process of 200mL 25g flunixin meglumine / 100g ethanol solution system. The circle point in the figure, that is, 1 point represents the sudden change point of the conductivity during the heating process, that is, the clarification point of the solution, indicating that the 2...

Embodiment 2

[0063] The present embodiment is the same as the device of the above-mentioned embodiment 1, and the solubility of donepezil hydrochloride in methanol has been measured by the same method in embodiment 1, and the solubility curve is as attached Figure 11 shown. When measuring the cooling rate and being 0.2K / min, the supersolubility curve of donepezil hydrochloride in methanol, as attached Figure 12 As shown, the range between the supersolubility curve and the solubility curve is the metastable region of the system.

[0064] On-line supersaturation monitoring in the crystallization process of donepezil hydrochloride was carried out by the same method as in Example 1, and the solvent was methanol. In this example, according to the method and steps of the present invention, according to the relational expression between conductivity and concentration, the relational expression of the system is established as follows:

[0065] V=0.033exp (0.029t N ) + (t-t N ) (-288.101+0.95...

Embodiment 3

[0068] The present embodiment is identical with the device of above-mentioned embodiment 1, has measured the solubility of ampicillin sodium in isopropanol with the same method in embodiment 1, and solubility curve is as attached Figure 14 shown. When measuring the cooling rate and being 0.2K / min, the supersolubility curve of ampicillin sodium in isopropanol, as attached Figure 15 As shown, the range between the supersolubility curve and the solubility curve is the metastable region of the system.

[0069] The online supersaturation monitoring of the ampicillin sodium crystallization process was carried out with the same method in Example 1, and the solvent was isopropanol. In this example, according to the method and steps of the present invention, according to the relational expression between conductivity and concentration, the relational expression of the system is established as follows:

[0070] V=0.2328exp (0.0791t N ) + (t-t N ) (-143.179+0.486t N )

[0071] Th...

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Abstract

The invention relates to a method for monitoring solubility, a metastable zone and solution concentration on line in a crystallization process of an organic salt system. The solution temperature of the system can be determined according to the mutational point in an electrical conductivity and temperature relation curve in a heating process, so that the solubility curve of a solute in the solvent is determined. The crystallization temperature of the system can be determined according to the mutational point in an electrical conductivity and temperature relation curve in a cooling process, so that the metastable zone of the solution system at the cooling rate is acquired. Coefficients of recorded electrical conductivity and temperature are calculated by using a least square method according to a relational expression of the electrical conductivity and the solution saturation temperature, so that the relation between the electrical conductivity and the solution concentration is acquired, and the super-saturation degree of the solution to be detected is calculated. The method is applied to measurement of various organic salts in polar organic solvents in the industrial crystallization process under different operating conditions. The method is practical, simple and convenient, can realize on-line measurement, and has the advantages of wide measurement temperature range, wide solution concentration range, simple operating instruments, low cost and strong practicability.

Description

technical field [0001] The invention belongs to the technical field of process analysis, in particular to an online monitoring method for measuring the supersaturation of a solution in the crystallization process of an organic system of an organic salt, which can also measure the solubility and metastable region of a solute in a solvent, and can be applied to fine chemical industry, Analysis of industrial crystallization process in liquid-solid system in biochemical pharmaceutical and other fields. Background technique [0002] In the pharmaceutical and chemical industries, crystallization is a commonly used separation technique, and is often used as the last separation process for the purification of raw materials (P. Wang, et al. Fluid Phase Equilibrium, 2011, 306:171-174). Supersaturation is the driving force for crystal nucleation and crystal growth during crystallization, and has a significant impact on the quality of crystal products. The so-called supersaturation is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N25/12G01N27/00
Inventor 龚俊波吴送姑王静康尹秋响张美景王永莉侯宝红郝红勋鲍颖陈巍董伟兵
Owner 阜新达得利化工股份有限公司
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