Solventing-out crystallization device and method through auxiliary control of films

Abstract

The invention provides a solventing-out crystallization technique device and method through auxiliary control of films, and belongs to the technical field of crystallization engineering. When a crystallization solution is added to a raw material pot, a solventing-out agent is added to a material-liquid pot, electronic scales, a computer, a stirring device and temperature controlling devices are started, and after a system is stable, squirm pumps of the material-liquid pot are started, so that solventing-out agents can circulate between the material-liquid pot and a film assembly; and after the solventing-out agent is stable in circulation, the squirm pump connected to the raw material pot is started so that the crystallization solution enters the film assembly. The solventing-out agent and the crystallization solution which are in sufficient contact in the film assembly can perform nucleation growth in the film assembly, and then the solventing-out agent and the crystallization solution, after the nucleation growth, can flow into an external storing pot for filtration and post-treatment; and the solventing-out agent and the crystallization solution can also perform nucleation growth outside the film assembly, and after solutes are wholly dissolved, filtration is performed. The electronic scales record the addition quantity of the solventing-out agent in a real-time manner, and the addition quantity of the solventing-out agent is systematically controlled through controlling films and operation conditions, so that ideal crystal products are obtained.

Description

technical field [0001] The invention belongs to the technical field of crystallization engineering, is especially suitable for the preparation of some special crystals and the production process with strict requirements on crystallization products, and provides a broader space for the development of dissolution crystallization technology. Background technique [0002] Solvent crystallization is a common separation method. It is a process in which the solubility of the solute in the original solvent is reduced by adding a solvent to the solution, thereby generating supersaturation, causing the solute to crystallize and precipitate from the solution. The solvent added can be gas or liquid. Compared with other crystallization processes, dissolution crystallization has no temperature change in the system, which can greatly increase the yield of crystal products, and plays an important role in the field of crystallization. In recent years, elution crystallization has been widely...

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Problems solved by technology

However, the dissolution and crystallization mentioned in the patent is a drop-stirring production process, which has poor control over operating conditions, difficulty in expanding production, and limitations in the types of crystals produced.

Moreover, the optimization of the elution crystallization in the patent is mostly an improvement in the pretreatment of the crystallization solution, and there is no improvement in the main production link of the elution crystallization, so the improvement of the crystal product quality is very limited, and it is difficult to Promote the use of different dissolution and crystallization systems

[0005] In the pharmaceutical and chemical industries, some new coupling processes and mixing equipment can improve the defects of elution crystallization to a certain extent, but they still cannot solve the problems of uneven supersaturation distribution, explosive nucleation and crystal agglomeration

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