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Sublimating crystallizing device

A technology of crystallization device and crystallization tube, which is applied in the field of chemical equipment, can solve the problems of changing the crystallization matrix, the inability to introduce target impurity molecules, and the inconvenient removal of crystallization products, so as to avoid the effect of shape damage

Inactive Publication Date: 2015-07-08
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a sublimation crystallization device with fine temperature control, convenient product transfer and scientific experiment, so as to solve the existing problems in the existing crystallization device, such as imprecise temperature control in the crystallization area, inconvenient transfer of crystallized products, and inability to introduce Target impurity molecules and deficiencies in changing the crystallization matrix

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Vacuum sublimation crystallization

[0029] Such as figure 1 As shown, put about 1g of β-succinic acid crystal powder into the loading tube 7, weigh the total weight as m0, put the thermocouple into the temperature measuring tube 5, and move the loading tube 7 to the sublimation zone of the thermostatic tube 14 The middle part of the middle part, cover the rubber stopper 13, place the glass sheet above the crystallization tube 15, adjust the temperature controller 4, set the heating temperature to 180°C, turn on the vacuum pump connected to the air release pipe 9, turn on the circulation constant temperature tank 10, and keep it until the set temperature Set the temperature at 95°C, and the material in the loading tube 7 is heated and sublimated into a gas under reduced pressure. When the hot air flow passes through the glass sheet above the crystallization tube 15, the temperature of the hot air flow drops, and the formed supersaturated steam slowly flows on...

Embodiment 2

[0030] Example 2: Carrier gas flow sublimation crystallization

[0031] Such as figure 2 As shown, about 1g of pyrene crystal powder is loaded into the loading tube 7, and the total weight is called m0. The thermocouple is placed in the temperature measuring tube 5, and the loading tube 7 is moved to the middle part of the sublimation zone of the thermostatic tube 14. Cover the rubber stopper 13, connect the carrier gas cylinder 8 (nitrogen), and fix the nitrogen flow rate at 20 ml / min. Place the glass flake or aluminum foil above the crystallization tube 15, adjust the temperature controller 4, set the heating temperature to 140°C, connect the air release pipe 9 to the atmosphere, open the circulation constant temperature tank 10, keep the set temperature at 35°C, and adjust the flow regulator The material in the loading tube 7 is heated and sublimated into a gas under a nitrogen flow, and when the steam flows through the glass sheet or aluminum foil above the crystallizati...

Embodiment 3

[0032] Example 3: Sublimation crystallization intervened by target impurities

[0033] Such as image 3 As shown, put about 1g of β-succinic acid crystal powder into the loading tube 7, weigh the total weight as m0, put the thermocouple into the temperature measuring tube 5, and move the loading tube 7 to the sublimation zone of the thermostatic tube 14 The middle part of the middle part, cover the rubber stopper 13, connect the material storage 2 (the target impurity is isopropanol solvent), open the constant temperature tank 1 to maintain a certain temperature to ensure that the evaporation pressure of isopropanol remains constant, and place the glass sheet in the crystallization Above the pipe 15, adjust the temperature controller 4, set the heating temperature to 180° C., turn on the vacuum pump connected to the air release pipe 9, maintain a certain degree of vacuum, and ensure that the flow rate of the flow regulator is fixed. Open the circulating constant temperature t...

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Abstract

The invention discloses a sublimating crystallizing device. The sublimating crystallizing device comprises a constant warm tube, a heating layer, a temperature controller and a discharging air pipe; a movable material loading tube is placed in a sublimating area of the constant warm tube; a temperature measuring tube is fixedly arranged on the inner wall of the material loading tube; a thermocouple connected with the temperature controller is placed into the temperature measuring tube; a crystallizing tube is arranged in a crystallizing area of the constant warm tube; the upper part of the crystallizing pipe is of a plane structure; and constant-temperature circulating liquid medium is fed into the crystallizing pipe and is used for controlling the temperature of the outer surface of the crystallizing pipe. By adopting the sublimating crystallizing device, three processes of sublimating crystallizing, namely, the process of carrier-gas-stream sublimating crystallizing, the process of vacuum sublimating crystallizing, and the process of target impurity interfering, can be realized; the sublimating crystallizing device is simple and convenient to operate, and accurate in temperature measuring and control, and can precisely adjust the degree of supersaturation in crystallizing; the obtained product is easy to move and take, and convenient to analyze; and the sublimating crystallizing device is beneficial to developing new polymorphism products, and studying a nucleation and growth mechanism.

Description

technical field [0001] The invention relates to a sublimation crystallization device, belonging to the technical field of chemical equipment. Background technique [0002] Sublimation crystallization is different from solution crystallization. The crystallization process is less affected by other molecules, and can directly change from gaseous state to solid crystal. Some substances can be purified by sublimation crystallization or converted into polymorphic products that cannot be obtained by other crystallization methods. [0003] The sublimation device in the current experiment has the following deficiencies: (1) The design of the device is simple, only the temperature of the sublimation zone is properly controlled, and the fine temperature adjustment of the crystallization zone is lacking; (2) The effect of supersaturation on the sublimation crystal morphology and (3) It is inconvenient to pipette the crystalline product, and the pipetting process can easily cause damag...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D7/02
Inventor 于秋硕马晓迅徐龙
Owner NORTHWEST UNIV
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