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

A technology of dissolution crystallization and auxiliary control, which is applied in the general layout of the crystallization device, solution crystallization, selection of auxiliary crystallization conditions, etc. limited and other problems, to achieve the effect of controlling the morphology and particle size distribution, easy to scale up and down, and high quality of crystalline products

Active Publication Date: 2016-11-30
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 crysta

Method used

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

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Effect test

Embodiment 1

[0033] Take the PES hollow fiber membrane to make a membrane module, and the packing ratio is 0.6. Take 80g of NaCl and add it into deionized water to prepare a saturated solution at 25°C. Add the prepared crystallization solution into the raw material tank, and turn on the stirring device. Adjust the temperature control device to 25°C, turn on the circulating water, and maintain the running state for 30 minutes. Add an appropriate amount of ethanol to the feed liquid tank, turn on the temperature control device, adjust to 25°C, turn on the circulating water, electronic balance and computer, and maintain the running state for 30 minutes. After the temperature is stable, open ports a and b of three-way valves A and B, close port c, open the valve of the ethanol feed liquid tank, and adjust the peristaltic pump to 50rpm to allow ethanol to flow through the membrane module. After the ethanol runs stably, open the valve of the raw material tank and adjust the peristaltic pump so...

Embodiment 2

[0035] Take the PES flat membrane to make a membrane module. Take 80g of NaCl and add it into deionized water to prepare a saturated solution at 25°C. Slowly add ethanol dropwise to the solution and stir fully to make the solution close to supersaturated, but not supersaturated. Add the prepared crystallization solution into the raw material tank, and turn on the stirring device. Adjust the temperature control device to 25°C, turn on the circulating water, and maintain the running state for 30 minutes. Add an appropriate amount of ethanol to the feed liquid tank, turn on the temperature control device, adjust to 25°C, turn on the circulating water, electronic balance and computer, and maintain the running state for 30 minutes. After the temperature is stable, open ports a and c of three-way valves A and B, close port b, open the valve of the ethanol feed liquid tank, and adjust the peristaltic pump to 200rpm to allow ethanol to pass through the membrane module at high speed. ...

Embodiment 3

[0037] Take the PTFE hollow fiber membrane to make the membrane module, and the packing ratio is 0.1. Take 25g of L-asparagine and add it into deionized water to prepare a saturated solution at 25°C. Slowly add isopropanol dropwise to the solution, and stir well, so that the solution is close to supersaturated, but not supersaturated. Add the prepared crystallization solution into the raw material tank, and turn on the stirring device. Adjust the temperature control device to 25°C, turn on the circulating water, and maintain the running state for 30 minutes. Add an appropriate amount of isopropanol to the feed liquid tank, turn on the temperature control device, adjust it to 25°C, turn on the circulating water, electronic balance and computer, and keep it running for 30 minutes. After the temperature is stable, open ports a and c of the three-way valves A and B, close port b, open the valve of the isopropanol feed liquid tank, and adjust the peristalsis to 200rpm to allow iso...

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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...

Claims

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Application Information

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IPC IPC(8): B01D9/02B01D61/00
CPCB01D9/005B01D9/0059B01D9/0063B01D61/00B01D2009/0086
Inventor 姜晓滨贺高红脱凌晗肖武李祥村吴雪梅
Owner DALIAN UNIV OF TECH
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