How long does the crystallization process of sodium abietate take and optimization methods?
Time:
Nov 09,2021
1、 Crystallization time of sodium abietate
The time required for the crystallization process of sodium abietate is not fixed, but is influenced by various factors. The following are the main influencing factors and their effects on the crystallization time:
Main influencing factors
Supersaturation: The supersaturation of the slurry is mainly controlled by temperature, and the lower the temperature, the lower the supersaturation. The higher the supersaturation, the more crystal nuclei are generated, and the smaller the crystal particle size, but it may shorten the crystallization time.
Retention time: The longer the retention time, the larger the particle size of the resulting crystals. The higher the liquid level, the longer the residence time, and the crystallization process may be more complete.
Impurities: When there are many impurities, it is easy to form crystal nuclei, which may lead to a shortened crystallization time.
Temperature: Crystallization is usually carried out at low temperatures, which can reduce solubility, prevent denaturation, and bacterial growth. The cooling rate also affects the size of crystal particles, with faster cooling resulting in smaller crystal particles and slower cooling resulting in larger crystal particles.
Seed crystals: For biochemical drugs that are difficult to crystallize (similar situations can be referred to), seed crystals are often added to promote crystallization, which may significantly shorten the crystallization time.
Crystallization time range
Generally, the formation and growth of crystals take several hours to complete, but the specific time needs to be adjusted according to the above conditions.
For example, in the experiment of rosin crystallization, the start time of crystallization can be shortened from 2 hours (such as wetland pine rosin) to 15 minutes (when a specific resin acid is added).
The crystallization time of sodium abietate needs to be determined through experiments, and it is recommended to optimize it according to actual process conditions (such as temperature, impurities, seed crystals, etc.), which can usually be completed within a few hours
2、 Optimization Method for Crystallization Time of Sodium Rosinate
Optimizing the crystallization time of sodium rosin requires comprehensive control of key factors such as supersaturation, temperature, impurity management, and seed crystal addition. The specific methods are as follows:
Supersaturation control
Supersaturation is the core driving force for crystallization and requires precise control through temperature regulation. Lowering the temperature can reduce supersaturation, thereby suppressing the rapid formation of crystal nuclei, prolonging the crystal growth period, and optimizing the crystallization time.
For example, in evaporative crystallization, maintaining supersaturation in the metastable region (such as 1.05-1.15) can balance the crystal growth rate and quantity.
Temperature and residence time
Temperature directly affects the rate of molecular motion and crystallization kinetics. Appropriately increasing the temperature can accelerate solute diffusion, but it is necessary to avoid excessive supersaturation caused by high temperature, which can lead to fine crystals.
Meanwhile, extending the residence time (by adjusting the liquid level) can promote sufficient crystal growth, but it needs to be optimized in conjunction with supersaturation.
Impurity management
Impurities can easily become crystal nuclei, leading to shortened crystallization time and smaller crystals. Chemical impurity removal (such as adding disodium EDTA) or process optimization (such as controlling evaporation temperature<80 ℃) is required to reduce impurity interference.
Low purity rosin may inhibit excessive crystallization due to its high impurities.
Seed addition
Introducing seed crystals can guide ordered nucleation and avoid fluctuations in crystallization time caused by spontaneous nucleation. By controlling the number and timing of seed crystals, the crystallization process can be stabilized and the overall time can be shortened
For example, maintaining a solid-liquid ratio of 15-25% in a DTB crystallizer with a stirring speed of 200-400rpm can optimize crystal growth efficiency.
Optimization of mixing intensity
The stirring intensity needs to match the crystallization target. Excessive stirring will break the crystals and prolong the crystallization time; Moderate stirring can promote mass transfer, but it is necessary to avoid excessive local supersaturation.
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