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A preparation process and device system for continuous cooling and recrystallization of ethyl carbazole

A technology of ethylcarbazole and a preparation process, which is applied in the field of preparation technology and device system of continuous cooling and recrystallization of ethylcarbazole, can solve the problems of improper control of process parameters, deterioration of ethylcarbazole, small crystal size and the like, and achieves Guaranteed crystal size, improved crystal growth, and reduced moisture content

Active Publication Date: 2022-04-19
CHENGDU CHENGDE CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] (1) The process parameters of the crystallization process are not properly controlled, resulting in small crystal particle size, and crystals with smaller particle size are easy to float;
[0010] (2) The polar growth of ethyl carbazole crystals in ethanol solvent is easy to form long needle-like crystals. With the continuous crystallization process, the growth interface becomes smaller and smaller, and more crystals are mainly spontaneous nucleation. Lead to the deterioration of ethyl carbazole, resulting in floating phenomenon

Method used

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  • A preparation process and device system for continuous cooling and recrystallization of ethyl carbazole
  • A preparation process and device system for continuous cooling and recrystallization of ethyl carbazole
  • A preparation process and device system for continuous cooling and recrystallization of ethyl carbazole

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Embodiment 1

[0039] The present embodiment provides a preparation process for continuous cooling and crystallization of ethylcarbazole, comprising the following steps:

[0040] Step 1: Mix the crude ethylcarbazole and the ethanol solvent in a mass ratio of 25:100, add it to the continuous cooling crystallizer, until the solution reaches the specified liquid level, where the temperature is about 60 °C, turn on the external circulation pump And the refrigeration unit, adjust the freezing settings, and conduct the first cooling, and the cooling rate is 3 °C / h;

[0041] Step 2: When the temperature of the solution reaches 52°C, add ethylcarbazole seed crystals with a particle size of 0.05mm to 0.1mm in an amount of 10‰, and after 45min of heat preservation, conduct a second cooling, and the cooling rate is 4°C / h , until the temperature drops to 10°C to obtain the mother liquor of continuous crystallization;

[0042] Step 3: Add the pre-configured raw material liquid with a temperature of 60 °C ...

Embodiment 2

[0045] The present embodiment provides a preparation process for continuous cooling and crystallization of ethylcarbazole, comprising the following steps:

[0046] Step 1: Mix the crude ethylcarbazole and ethanol solvent in a mass ratio of 22:100 and add it to the continuous cooling crystallizer until the solution reaches the specified liquid level, where the temperature is about 55°C, and the external circulation pump is turned on. And the refrigeration unit, adjust the freezing settings, and conduct the first cooling, and the cooling rate is 3.5 °C / h;

[0047] Step 2: When the temperature of the solution reaches 51°C, add ethylcarbazole seed crystals with a particle size of 0.05mm to 0.1mm, and the addition amount is 10‰, and after 30min of heat preservation, the second cooling is performed, and the cooling rate is 4°C / h , until the temperature drops to 10°C to obtain the mother liquor of continuous crystallization;

[0048] Step 3: Add the pre-configured raw material liqui...

Embodiment 3

[0051] The present embodiment provides a preparation process for continuous cooling and crystallization of ethylcarbazole, comprising the following steps:

[0052] Step 1: Mix the crude ethylcarbazole and ethanol solvent in a mass ratio of 30:100, and add it to the continuous cooling crystallizer until the solution reaches the specified liquid level, where the temperature is about 53 °C, and the external circulation pump is turned on. And the refrigeration unit, adjust the freezing settings, and conduct the first cooling, and the cooling rate is 4 °C / h;

[0053] Step 2: When the temperature of the solution reaches 53°C, add ethylcarbazole seed crystals with a particle size of 0.05mm to 0.1mm, and the addition amount is 10‰, and after 60min of heat preservation, the second cooling is performed, and the cooling rate is 4°C / h , until the temperature drops to 10°C to obtain the mother liquor of continuous crystallization;

[0054] Step 3: Add the pre-configured raw material liqui...

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Abstract

The invention discloses a preparation process and device system for continuous cooling and crystallization of ethyl carbazole, which solves the problem that floating crystals are prone to appear in the process of preparing ethyl carbazole in the traditional process, resulting in high moisture content of crystals and easy preparation of powdery crystals. question. The invention includes a preparation process of continuous cooling and recrystallization of ethyl carbazole. The ethyl carbazole crude product and ethanol solvent are mixed according to the mass ratio, and after heating and dissolving, the temperature is lowered for the first time, and the solution temperature is reduced to a supercooling degree of 1 ℃~4℃, add ethyl carbazole seed crystals with a particle size of 0.05mm~0.1mm, keep warm, and then lower the temperature to the crystallization temperature for the second time to obtain the mother liquor of continuous crystallization. Ultrasonic treatment is carried out on the pre-configured raw material solution, and the crystallization time is controlled, followed by centrifugation, washing and drying to obtain ethyl carbazole granule products; the above-mentioned preparation process is used to provide the device system. The invention has the advantages of being able to continuously cool and recrystallize to prepare short rod-shaped ethyl carbazole, and at the same time completely avoid the generation of floating crystals.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation process and a device system for continuous cooling and recrystallization of ethylcarbazole. Background technique [0002] In 2004, after researchers such as Pez proposed the ethylcarbazole hydrogen storage system, it has become a new research hotspot of organic liquid hydrides in recent years. The melting point of ethylcarbazole is 68°C, and the dehydrogenation reaction enthalpy is about 50KJ / molH 2 , the dehydrogenation temperature is less than 200 ℃, it can be completely hydrogenated / dehydrogenated, and its theoretical hydrogen storage density can reach 5.8%, which has reached the technical indicators of the US Department of Energy (DOE). CO, NH 3 It is a new type of organic liquid hydrogen storage medium. The ethylcarbazole hydrogenation / dehydrogenation process is as follows: [0003] [0004] As a new organic liquid hydrogen storage medium, the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/84C07D209/86
CPCC07D209/84C07D209/86
Inventor 徐程浩杨德建
Owner CHENGDU CHENGDE CHEM TECH
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