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A Cooling Crystallization Method for Membrane Assisted Nucleation

A technology of cooling crystallization and nucleation, which is applied in the selection of crystallization auxiliary conditions, crystallization separation, solution crystallization, etc., can solve the problems of difficult expansion of production, fluctuation of crystal product quality, etc. control effect

Active Publication Date: 2019-04-05
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the Chinese patents CN1736970A and CN102070625A, it is mentioned that a crystal product that meets the requirements is obtained by putting in crystal seeds, but in order to obtain a crystal product that meets the requirements, there are strict requirements on the time of putting in the crystal seeds and the quality and particle size of the crystal seeds in the control conditions , once the operating conditions deviate, the crystal product quality will fluctuate
Therefore, the use of this method to produce different crystals with different particle sizes is very limited, and it is difficult to expand production.

Method used

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  • A Cooling Crystallization Method for Membrane Assisted Nucleation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take the PP hollow fiber membrane to make the membrane module 3. Prepare 300g of KNO at 50°C 3 Saturated aqueous solution, and it was added to the crystallization kettle 1, and the stirring device 2 was turned on. Turn on the computer, set the first-stage temperature to 50°C and the time to 1h in the computer, and set the second-stage temperature to 10°C and the time to 4h. Turn on the temperature control device 6, turn on the circulating water, and maintain the running state for 1h. Add an appropriate amount of water to the coolant tank 5, turn on the second temperature control device 7, set the temperature to 15°C, and adjust the first peristaltic pump 8 to 30rpm to maintain a stable circulation. After running for 55 minutes, open the first valve 14, open the a and b ports of the first three-way regulating valve 12, close the c port, open the b and c ports of the second three-way regulating valve 13, close the a port, and open the second peristaltic pump 9, and adj...

Embodiment 2

[0031] Take the PVDF flat membrane to make the membrane module 3. Prepare 200g of CoSO at 50°C 4 Saturated aqueous solution, and it was added to the crystallization kettle 1, and the stirring device 2 was turned on. Turn on the computer 11, and in the computer 11, the first stage temperature is set to 50° C., and the time is set to 40 minutes; the second stage temperature is set to 20° C., and the time is set to 3 hours. Turn on the first temperature control device 6, turn on the circulating water, and maintain the running state for 50 minutes. Add an appropriate amount of water to the coolant tank 5, turn on the second temperature control device 7, set the temperature to 15° C., and adjust the second peristaltic pump 2 to 70 rpm to keep the coolant flowing rapidly and stably. After running for 30 minutes, open the first valve 14, open ports a and b of the first three-way regulating valve 12, close port c, open ports b and c of the second three-way regulating valve 13, close...

Embodiment 3

[0033] Take the PTFE hollow fiber membrane to make the membrane module 3. Prepare 150g of NaNO at 40°C 3Saturated aqueous solution, and it was added to the crystallization kettle 1, and the stirring device 2 was turned on. Turn on the computer 11, set the temperature of the first stage to 40°C and the time to 50min in the computer 11, and set the temperature of the second stage to 10°C and the time to 3h. Turn on the first temperature control device 6, turn on the circulating water, and maintain the running state for 50 minutes. Add an appropriate amount of water into the coolant tank 5, turn on the second temperature control device 7, set the temperature to 14° C., and adjust the peristaltic pump to 50 rpm to keep the coolant circulating and flowing stably. After running for 50 minutes, open the first valve 14, open the a and b ports of the first three-way regulating valve 12, close the c port, open the b and c ports of the second three-way regulating valve 13, close the a ...

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Abstract

The invention provides a membrane-assisted nucleation cooling crystallization method, and belongs to the technical field of crystallization engineering. Solution to be crystallized is added into a crystallizing kettle, a computer and a stirring and temperature control device is started, and a cooling liquid loop is started. After a system is stabilized, a peristaltic pump is started, and the solution to be crystallized is conveyed to a membrane component. When crystal nucleuses appear in the membrane component, mother solution with the crystal nucleuses is conveyed to the crystallizing kettle and subjected to crystal growth. By controlling cooling liquid and operation conditions, generation of the crystal nucleuses and crystal growth are systematically regulated, so that an ideal crystal product is obtained.

Description

technical field [0001] The invention belongs to the technical field of crystallization engineering, and is especially suitable for the preparation of substances whose solubility decreases significantly with the decrease of temperature. Background technique [0002] Cooling crystallization relies on lowering the temperature to produce supersaturation and precipitate crystallization. In order to shorten the crystallization period, prevent explosive nucleation, effectively control the growth of crystals, and obtain crystal products with a relatively uniform particle size, an appropriate number and particle size of seeds are usually added to the solution so that the crystallized solute is only on the surface of the seeds. grow. Choose proper stirring so that the seeds can be suspended in the whole solution evenly without coalescence, and try to avoid the secondary nucleation phenomenon. The temperature or concentration of the solution must be carefully controlled throughout th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D9/02C01G51/10C01D9/18
CPCB01D9/005B01D9/0059B01D2009/0086C01D9/18C01G51/10
Inventor 姜晓滨李冠男卢大鹏贺高红肖武李祥村吴雪梅
Owner DALIAN UNIV OF TECH
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