Distillation and purification device for N-propyl carbazole

Abstract

The utility model relates to the technical field of purification of N-propyl carbazole, in particular to a distillation purification device of N-propyl carbazole. Comprising a generator used for accommodating an N-propyl carbazole raw material; the recoverer is used for collecting an N-propyl carbazole product, and a vacuum gas pipe is arranged on the recoverer; the distillation gas pipe is used for connecting an outlet of the generator and an inlet of the recoverer to form a distillation loop; the generator heating tank is arranged outside the generator and is used for heating the generator; the recoverer heating tank is arranged outside the recoverer and is used for heating the recoverer; and the vacuum pump is connected with the vacuum air pipe so as to vacuumize the distillation loop. The device disclosed by the utility model is low in cost and can be used as a distillation system for research.

Description

Technical Field

[0001] The utility model relates to the technical field of N-propylcarbazole purification, in particular to a distillation purification device for N-propylcarbazole. Background Art

[0002] Hydrogen is a readily available, green, low-carbon, and widely used secondary energy source. It can facilitate the large-scale absorption of renewable energy and accelerate the decarbonization of industries, construction, transportation, and other sectors. Liquid organic hydrogen carriers (LOHCs), as a key element in hydrogen storage and transportation, offer advantages such as safe and convenient transportation, making them a promising approach for achieving large-scale hydrogen storage and transportation in the future. N-propylcarbazole, a commonly used LOHC, can achieve a theoretical maximum hydrogen storage capacity of 5.4 wt% when used as a hydrogenation catalyst. It is also inexpensive and easy to store.

[0003] Most of the existing industrially produced N-propylcarbazole raw materials are primarily carbazole, supplemented with additives such as potassium chloroacetate. After a series of reactions, the resulting product often contains small amounts of impurities and byproducts, such as carbazole, phenanthrene, and other carbazole derivatives. These impurities can affect hydrogen storage performance. Therefore, N-propylcarbazole, as a hydrogen carrier for organic liquid hydrogen storage, requires purification when necessary. However, N-propylcarbazole has a melting point of 52°C-54°C and readily solidifies at room temperature. Furthermore, existing distillation equipment, mostly used in large-scale applications such as petroleum and water purification, is expensive, bulky, and lacks specificity, making it unsuitable for the distillation and purification of N-propylcarbazole, which is still under research. Furthermore, since no research has yet been conducted on its boiling point, its boiling point range remains undefined. Utility Model Content

[0004] The embodiment of the utility model provides a distillation purification device for N-propylcarbazole, which effectively purifies N-propylcarbazole.

[0005] The embodiment of the present utility model provides a distillation purification device for N-propylcarbazole, comprising:

[0006] a generator for containing an N-propylcarbazole raw material;

[0007] A recovery device for collecting the N-propylcarbazole product, wherein the recovery device is provided with a vacuum air pipe;

[0008] A distillation gas pipe, used to connect the outlet of the generator and the inlet of the recovery device to form a distillation loop;

[0009] A generator heating tank is provided outside the generator and is used to heat the generator;

[0010] A recovery device heating tank is provided outside the recovery device and is used to heat the recovery device;

[0011] A vacuum pump is connected to the vacuum air pipe to evacuate the distillation loop.

[0012] In the embodiments of the present application, a generator and a reclaimer are connected via a distillation gas pipe to form a distillation loop. N-propylcarbazole is extracted from the N-propylcarbazole raw material into the reclaimer. The generator and reclaimer are heated by a generator heating tank and a reclaimer heating tank, respectively, to control the reaction temperature. A vacuum pump evacuates the distillation loop to control the vacuum level of the reaction. This device is low-cost and can be used as a distillation system for research.

[0013] In one embodiment, a heating device is provided on the distillation gas pipe.

[0014] In the embodiment of the present application, the distillation gas pipe is heated by a heating device on the distillation gas pipe, so that the temperature of the distillation gas pipe can be controlled, thereby preventing volatiles flowing through the distillation gas pipe from solidifying on the pipe wall of the distillation gas pipe and causing blockage.

[0015] In one embodiment, the generator and the recycler are both provided with inner containers; and / or

[0016] The generator and the recoverer each include a trough body and a cover, and the trough body is sealed and connected to the cover.

[0017] In the embodiments of the present application, an inner container is provided in the generator and the recovery vessel to hold the raw materials and collect the products for easy access. By separating the generator and the recovery vessel into a tank and a lid, the distillation circuit can be sealed and the operation can be facilitated.

[0018] In one embodiment, the distillation purification device further comprises a magnetic stirrer for stirring the N-propylcarbazole raw material in the generator; and / or

[0019] The distillation purification device also includes a temperature sensor, which is arranged on the generator and the recoverer and is used to monitor the temperature inside the generator and the recoverer.

[0020] In the embodiments of the present application, a magnetic stirrer can be used to maintain a sealed loop formed by the generator and the reclaimer while stirring the raw materials in the generator. A temperature sensor can effectively monitor the temperature in the generator and the reclaimer, thereby controlling the temperature in the generator and the reclaimer, and thus controlling the temperature of the distillation purification.

[0021] In one embodiment, the distillation purification device further comprises a control panel, which is communicatively connected to the temperature sensor, the magnetic stirrer, the generator heating tank, the recovery heating tank and the heating device.

[0022] In an embodiment of the present application, by setting up a control panel, the heating temperatures of the generator heating tank, the recovery heating tank and the heating device can be adjusted according to the measurement values ​​of the temperature sensor, and the stirring speed of the magnetic stirrer can be controlled.

[0023] In one embodiment, the distillation purification device further comprises a bracket, and the magnetic stirrer, the generator heating tank, the recovery heating tank and the control panel are arranged on the bracket. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative work.

[0025] Figure 1 This is a schematic structural diagram of a distillation and purification device for N-propylcarbazole of the present invention;

[0026] Figure 2 This is a chromatogram of the distillation product S1 of N-propylcarbazole provided in an embodiment of the present utility model.

[0027] Description of the drawings: generator-1; recovery device-2; distillation gas pipe-3; control panel-4; bracket-5; vacuum gas pipe-6; heating device-7; inner container-8; magnetic stirrer-9; temperature sensor-10. DETAILED DESCRIPTION

[0028] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without making creative efforts shall fall within the scope of protection of the present invention.

[0029] like Figure 1 As shown, the utility model provides a distillation purification device for N-propylcarbazole, comprising:

[0030] Generator 1, for containing N-propylcarbazole raw material;

[0031] A recovery device 2 is used to collect the N-propylcarbazole product, and a vacuum air pipe 6 is provided on the recovery device 2;

[0032] A distillation gas pipe 3 is used to connect the outlet of the generator 1 and the inlet of the recovery device 2 to form a distillation loop;

[0033] A generator heating tank is provided outside the generator 1 and is used to heat the generator 1;

[0034] A recovery device heating tank is provided outside the recovery device 2 and is used to heat the recovery device 2;

[0035] A vacuum pump is connected to the vacuum air pipe 6 to evacuate the distillation loop.

[0036] The generator 1 and the recycler 2 are connected via a distillation gas pipe 3, forming a distillation loop. N-propylcarbazole is extracted from the N-propylcarbazole raw material into the recycler 2. The generator and recycler 2 are heated by the generator heating tank and the recycler heating tank, respectively, to control the reaction temperature. A vacuum pump evacuates the distillation loop to control the vacuum level of the reaction. This device is low-cost and can be used as a distillation system for research.

[0037] Preferably, a heating device 7 is provided on the distillation gas pipe 3. The heating device 7 on the distillation gas pipe 3 heats the distillation gas pipe 3 to control the temperature of the distillation gas pipe 3, thereby preventing volatiles flowing through the distillation gas pipe 3 from solidifying on the pipe wall of the distillation gas pipe 3 and causing blockage.

[0038] Preferably, the generator 1 and the recycler 2 are both provided with an inner container 8; and / or

[0039] The generator 1 and the recoverer 2 each include a trough body and a cover, and the trough body and the cover are sealed and connected.

[0040] By arranging an inner container 8 in the generator 1 and the recovery vessel 2, it can be used to hold raw materials and collect products for easy access. By dividing the generator 1 and the recovery vessel 2 into a tank body and a lid, the distillation circuit can be sealed and easy to operate.

[0041] Preferably, the distillation purification device further comprises a magnetic stirrer 9 for stirring the N-propylcarbazole raw material in the generator 1; and / or

[0042] The distillation purification device further includes a temperature sensor 10 , which is disposed on the generator 1 and the recoverer 2 and is used to monitor the temperature inside the generator 1 and the recoverer 2 .

[0043] The magnetic stirrer 9 can keep the loop formed by the generator 1 and the recycler 2 sealed while achieving stirring of the raw materials in the generator 1. The temperature sensor 10 can effectively monitor the temperature in the generator 1 and the recycler 2, thereby controlling the temperature in the generator 1 and the recycler 2, and thus controlling the temperature of the distillation purification.

[0044] Preferably, the distillation purification device further includes a control panel 4, which is communicatively connected to the temperature sensor 10, the magnetic stirrer 9, the generator heating tank, the recovery heating tank and the heating device 7.

[0045] By setting up the control panel 4, the heating temperatures of the generator heating tank, the recovery heating tank and the heating device 7 can be adjusted according to the measurement value of the temperature sensor 10, and the stirring speed of the magnetic stirrer 9 can be controlled.

[0046] Preferably, the distillation purification device further comprises a bracket 5 , and the magnetic stirrer 9 , the generator heating tank, the recovery heating tank and the control panel 4 are arranged on the bracket 5 . Example 1

[0047] (1) Installation of distillation purification device: put 200g of N-propylcarbazole raw material and the magnet of magnetic stirrer 9 into the inner container 8 of generator 1, put the inner container 8 of generator 1 into the tank body of generator 1, cover the lid to achieve fixed sealing between the tank body and the lid, and put generator 1 into the generator heating tank; put the inner container 8 of recovery device 2 into the tank body of recovery device 2, cover the lid to achieve fixed sealing, and then put recovery device 2 into the recovery heating tank, and then connect the outlet of generator 1 to the inlet of recovery device 2 through distillation gas pipe 3. At the same time, connect the wires of the heating device 7 (heating wire) in the distillation gas pipe 3 to the circuit, and connect the temperature sensor 10 on the generator 1 and the recovery device 2 to the circuit. Then, connect the vacuum air pipe 6 on the cover of the recovery device 2 to the vacuum pump exhaust pipe port through the air pipe, and the device installation is completed; wherein, the temperature sensor 10, the magnetic stirrer 9, the generator heating tank, the recovery device heating tank and the heating device 7 are communicatively connected with the control panel 4, and the magnetic stirrer 9, the generator heating tank, the recovery device heating tank and the control panel 4 are fixedly arranged on the bracket 5;

[0048] (2) Start the vacuum pump, control the temperature in generator 1 to 100°C, the magnetic speed to 300 r / min, and evacuate for 1 hour until the vacuum degree is -0.05 MPa;

[0049] (3) Turn off the vacuum pump, adjust the temperature in the generator 1 to 120°C, control the temperature in the recovery device 2 to 60°C, turn on the heating device 7 in the distillation gas pipe 3, control the temperature in the distillation gas pipe 3 to 70°C, and distill under this condition for 12 hours;

[0050] (4) After the distillation process is completed, the inner container 8 of the recovery device 2 is taken out to obtain the distilled product, which is named S1. Its chromatogram is as follows Figure 2 shown. Example 2

[0051] This example is basically the same as Example 1, except that after the vacuum pump is turned off, the temperature in the generator 1 is adjusted to 150° C. and the distillation time is 15 hours. The product is named S2. Example 3

[0052] This example is basically the same as Example 1, except that after the vacuum pump is turned off, the temperature in the generator 1 is adjusted to 200° C. and the distillation time is 12 hours. The product is named S3. Example 4

[0053] This example is basically the same as Example 1, except that after the vacuum pump is turned off, the temperature in the generator 1 is adjusted to 250° C. and the distillation time is 15 hours. The product is named S4. Example 5

[0054] This example is substantially the same as Example 1, except that after the vacuum pump is turned off, the temperature in the generator 1 is adjusted to 300° C., and the distillation time is 12 hours. The product is named S5.

[0055] The distilled N-propylcarbazole product obtained in the example was subjected to chromatographic analysis. The results are shown in Table 1.

[0056] Table 1 is a comparison of the purity of N-propylcarbazole after distillation in each embodiment

[0057] Product Name Distillation temperature Distillation time purity impurities Example 1 S1 120℃ 12h 99.97% 0.03% Example 2 S2 150℃ 15h 99.97% 0.03% Example 3 S3 200℃ 12h 99.98% 0.02% Example 4 S4 250℃ 15h 99.98% 0.02% Example 5 S5 300℃ 12h 99.97% 0.03%

[0058] As can be seen from Table 1, after the distillation process of Examples 1-5 at 120°C-300°C for 12h-15h, the purity of the products obtained also reached above 99.97%.

[0059] Table 2 is the test data of the product S1 obtained by distillation purification of N-propylcarbazole provided in Example 1 of the present application after chromatograph detection. In Table 2, retention time refers to the time from injection of the substance to reaching the peak. Peak area is the peak area of ​​the substance, which can represent the relative content of the substance. Peak height indicates the peak height. There are 3 peaks shown in the chromatogram, representing 3 substances respectively. Among them, the second peak has the highest height, which is N-propylcarbazole, and the other 2 are impurities. Area percentage refers to the area ratio of the 3 peaks. It can be seen that the proportion of N-propylcarbazole in the 3 substances is the purity of N-propylcarbazole. As can be seen from Table 2, the present application has increased the purity of N-propylcarbazole from 87.6721% to 99.9681% through distillation purification.

[0060] Table 2

[0061] Serial number Retention time (min) Peak area Peak height Area percentage 1 23.1158 0.1353 0.0794 0.0205 2 23.3450 659.9686 204.0992 99.9681 3 23.5800 0.0751 0.0729 0.0114

[0062] The above is a detailed introduction to the embodiments of the present invention. Specific examples are used in this article to illustrate the principles and implementation methods of the present invention. The description of the above embodiments is only used to help understand the method and core idea of ​​the present invention. At the same time, for those skilled in the art, based on the idea of ​​the present invention, there will be changes in the specific implementation methods and application scope. In summary, the contents of this specification should not be understood as limiting the present invention.

Claims

1. A distillation purification device for N-propylcarbazole, characterized in that, include: a generator for containing an N-propylcarbazole raw material; A recovery device for collecting the N-propylcarbazole product, wherein the recovery device is provided with a vacuum air pipe; A distillation gas pipe, used to connect the outlet of the generator and the inlet of the recovery device to form a distillation loop; A generator heating tank is provided outside the generator and is used to heat the generator; A recovery device heating tank is provided outside the recovery device and is used to heat the recovery device; A vacuum pump is connected to the vacuum air pipe to evacuate the distillation loop.

2. The distillation purification device for N-propylcarbazole according to claim 1, characterized in that: The distillation gas pipe is provided with a heating device.

3. The distillation purification device for N-propylcarbazole according to claim 1, characterized in that: The generator and the recycler are both provided with inner containers; and / or The generator and the recoverer each include a trough body and a cover, and the trough body is sealed and connected to the cover.

4. The distillation purification device for N-propylcarbazole according to claim 1, characterized in that: The distillation purification device further comprises a magnetic stirrer for stirring the N-propylcarbazole raw material in the generator; and / or The distillation purification device also includes a temperature sensor, which is arranged on the generator and the recoverer and is used to monitor the temperature inside the generator and the recoverer.

5. The distillation purification device for N-propylcarbazole according to claim 4, characterized in that: The distillation purification device also includes a control panel, which is communicatively connected with the temperature sensor, the magnetic stirrer, the generator heating tank, the recovery heating tank and the heating device.

6. The distillation purification device for N-propylcarbazole according to claim 5, characterized in that: The distillation purification device also includes a bracket, and the magnetic stirrer, the generator heating tank, the recovery heating tank and the control panel are arranged on the bracket.

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