Trimethylsilyl azide rectification device

Abstract

The utility model provides a trimethyl silicon azide rectification device, which belongs to the technical field of organic compound purification and comprises a rack, a controller, a placement frame, a magnetic stirring electric jacket, an electric heating rectification column, a first bracket, a rectification head, a second bracket, a collection bottle, a third bracket, a primary water cooling pipe, a secondary water cooling pipe, a gas guide connecting pipe and a water drainage pipe, by arranging a double condensation structure, steam introduced from the rectification head flows through the inner pipe of the first-stage water-cooling pipe to be condensed, the first-stage water-cooling pipe is a snake-shaped condensation pipe, the lower opening of the outer pipe of the first-stage water-cooling pipe is connected to the faucet, condensation of the steam occurs on the inner wall of the inner pipe, and a space defined by the inner pipe and the outer pipe provides steam heat absorption for a water flowing area. And steam condensed by the first-stage water-cooling pipe is introduced into the second-stage water-cooling pipe for continuous condensation, and cooling water of an outer pipe of the first-stage water-cooling pipe enters the second-stage water-cooling pipe through the water drainage pipe for continuous condensation of steam entering the second-stage water-cooling pipe, so that the safety of trimethylsilyl azide distillation can be improved.

Description

Technical Field

[0001] This utility model relates to the field of organic compound purification technology, and in particular to a trimethylsilyl azide distillation apparatus. Background Technology

[0002] Trimethylsilyl azide is a commonly used organosilicon compound, usually a colorless liquid, readily soluble in organic solvents such as alcohols and ethers. As an azide reagent, it is mainly used in organic synthesis and materials science, and is widely used in various chemical reactions, especially showing unique advantages in the preparation of nitrogen-containing compounds.

[0003] In actual use, the following shortcomings were found in this device:

[0004] Trimethylsilane azide is sensitive to heat, mechanical shock, and electrostatics. In the distillation and purification process of trimethylsilane azide (TMSN3), the condensation system is the core link to ensure safety and purification efficiency. Due to the high volatility, thermal instability, and potential explosion risk of TMSN3, uncondensed azide vapor may accumulate in the pipeline and decompose and explode when heated or rubbed (such as generating highly reactive HN3). In addition, TMSN3 has a low boiling point (95–98℃) and needs to be condensed quickly to avoid loss, especially under high vacuum conditions.

[0005] Therefore, this application provides a trimethylsilane azide distillation apparatus to meet the requirements. Utility Model Content

[0006] The purpose of this invention is to solve the problems existing in the above-mentioned background technology by proposing a trimethylsilane azide distillation apparatus.

[0007] To solve the above-mentioned technical problems, this utility model provides the following technical solution:

[0008] A trimethylsilane azide distillation apparatus includes: a frame, a controller, a mounting rack, a magnetic stirring heating mantle, an electrically heated distillation column, a first support, a distillation head, a second support, a collection flask, a third support, a primary water-cooling pipe, a secondary water-cooling pipe, a gas inlet pipe, and a drain pipe. The controller is mounted on the upper left side of the frame, and the mounting rack is welded to the lower right side of the frame. The magnetic stirring heating mantle is mounted on the mounting rack, and the electrically heated distillation column is mounted on the upper inner part of the magnetic stirring heating mantle. The side of the electrically heated distillation column... A first support is installed at the outer end, a distillation head is installed at the top of the electrically heated distillation column, a second support is installed at the upper right end of the frame, a collection bottle is fixedly installed inside the tube sleeve of the second support, a third support is installed at the top right side of the frame, a primary water-cooling pipe is installed inside the tube sleeve of the third support, a secondary water-cooling pipe is installed inside the tube sleeve of the third support located on the side of the primary water-cooling pipe, a gas guide pipe is installed at the bottom of the primary water-cooling pipe, and a drain pipe is installed at the outlet of the upper end of the primary water-cooling pipe.

[0009] Preferably, the third support extends vertically upward to the upper end of the distillation head, and the primary water cooling pipe and the secondary water cooling pipe are located on the upper side of the distillation head through the third support.

[0010] Preferably, both the primary and secondary water-cooling pipes are inclined at 15°.

[0011] Preferably, the gas guide pipe at the bottom of the primary water-cooling pipe is connected to the top of the distillation head, and the gas guide pipe is made of PTFE material. The bottom of the distillation head is connected to the collection bottle through a PTFE connector.

[0012] Preferably, the other end of the drain pipe is connected downward to the water inlet at the lower end of the side of the secondary water-cooling pipe, and the water outlet at the upper end of the side of the secondary water-cooling pipe is connected to an external connecting pipe.

[0013] Preferably, the primary water-cooling tube is a serpentine condenser tube, and the inner core tube of the primary water-cooling tube is spiral.

[0014] Preferably, the secondary water-cooling tube is a spherical condenser tube, and the inner core tube of the secondary water-cooling tube has a spherical structure.

[0015] Compared with the prior art, this utility model has at least the following beneficial effects:

[0016] In the above scheme, by setting up a dual condensation structure, the steam introduced from the distillation head flows through the inner tube of the first-stage water-cooled pipe and is condensed. The lower opening of the outer tube of the first-stage water-cooled pipe is connected to a water tap. The condensation of the steam occurs on the inner wall of the inner tube. The space enclosed by the inner and outer tubes provides the water flow zone with the ability to absorb the heat of the steam and remove the heat. The steam condensed in the first-stage water-cooled pipe is introduced into the second-stage water-cooled pipe for further condensation. The cooling water from the outer tube of the first-stage water-cooled pipe enters the second-stage water-cooled pipe through the drain pipe to further condense the steam entering the second-stage water-cooled pipe. This can improve the safety of trimethylsilane distillation.

[0017] In the above scheme, by setting the first-stage water-cooling tube as a serpentine condenser tube with a spiral inner core tube, the length of the glass tube and the cooling area are significantly increased, allowing for more sufficient contact between the steam and the cooling medium and achieving a higher heat exchange effect. The second-stage water-cooling tube is a spherical condenser tube, and the spherical inner core tube makes it easier for the condensate to collect, ensuring that low-boiling-point components are completely condensed during reflux and reducing exhaust emissions. Attached Figure Description

[0018] The accompanying drawings, which are incorporated herein and form part of the specification, illustrate embodiments of the present disclosure and, together with the specification, further serve to explain the principles of the present disclosure and enable those skilled in the art to implement and use the present disclosure.

[0019] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0020] Figure 2 This is a schematic diagram of the specific connection structure of the condensation structure of this utility model;

[0021] Figure 3 This is a schematic diagram of the specific structure of the primary water-cooling pipe of this utility model;

[0022] Figure 4 This is a schematic diagram of the specific structure of the secondary water-cooled pipe of this utility model.

[0023] [Figure Labels]

[0024] 1-Frame; 2-Controller; 3-Placement rack; 4-Magnetic stirring heating mantle; 5-Electric heating distillation column; 6-First support; 7-Distillation head; 8-Second support; 9-Collection bottle; 10-Third support; 11-First-stage water cooling pipe; 12-Second-stage water cooling pipe; 13-Gas delivery pipe; 14-Drain pipe.

[0025] As shown in the figure, specific structures and devices are marked in the figure to clearly illustrate the structure of the embodiments of this utility model. However, this is only for illustrative purposes and is not intended to limit this utility model to the specific structure, device and environment. According to specific needs, those skilled in the art can adjust or modify these devices and environments, and such adjustments or modifications are still included in the scope of the appended claims. Detailed Implementation

[0026] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0027] In the description of this utility model, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc., indicating the orientation or positional relationship are based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this utility model and simplifying the description, and are not intended to indicate or imply that the device or component referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model.

[0028] like Figure 1 , Figure 2 , Figure 3 and Figure 4The trimethylsilane azide distillation apparatus shown in this embodiment includes: a frame 1, a controller 2, a mounting rack 3, a magnetic stirring heating mantle 4, an electrically heated distillation column 5, a first support 6, a distillation head 7, a second support 8, a collection bottle 9, a third support 10, a primary water-cooling pipe 11, a secondary water-cooling pipe 12, a gas guide pipe 13, and a drain pipe 14. The controller 2 is mounted on the upper left side of the frame 1, and the mounting rack 3 is welded to the lower right side of the frame 1. The magnetic stirring heating mantle 4 is mounted on the mounting rack 3, and the electrically heated distillation column 5 is mounted on the upper inner part of the magnetic stirring heating mantle 4. A first support 6 is installed at the outer side of the electrically heated distillation column 5, a distillation head 7 is installed at the top of the electrically heated distillation column 5, a second support 8 is installed at the upper right side of the frame 1, a collection bottle 9 is fixedly installed inside the tube sleeve of the second support 8, a third support 10 is installed at the top right side of the frame 1, a primary water-cooling pipe 11 is installed inside the tube sleeve of the third support 10, a secondary water-cooling pipe 12 is installed inside the tube sleeve of the third support 10 located on the side of the primary water-cooling pipe 11, a gas guide pipe 13 is installed at the bottom of the primary water-cooling pipe 11, and a drain pipe 14 is installed at the outlet of the upper end of the primary water-cooling pipe 11.

[0029] In this embodiment, the third support 10 extends vertically upward to the upper end of the distillation head 7, and the primary water cooling pipe 11 and the secondary water cooling pipe 12 are located at the upper end of the side of the distillation head 7 through the third support 10. The primary water cooling pipe 11 and the secondary water cooling pipe 12 are used to condense vapor, ensuring that the vapor generated during distillation of the distillation head 7 can smoothly flow upward into the primary water cooling pipe 11.

[0030] In this embodiment, both the primary water-cooling pipe 11 and the secondary water-cooling pipe 12 are inclined at 15° to better collect condensate.

[0031] In this embodiment, the gas guide pipe 13 at the bottom of the primary water cooling pipe 11 is connected to the top of the distillation head 7, and the gas guide pipe 13 is made of PTFE material. The bottom of the distillation head 7 is connected to the collection bottle 9 through a PTFE connector. Compared with the traditional ground joint connector, this can avoid leakage caused by TMSN3 corrosion and reduce the dangerous side reactions that may be caused by TMSN3 coming into contact with air or moisture. The main fraction is collected in the collection bottle 9 at 95–98°C.

[0032] In this embodiment, the other end of the drain pipe 14 is connected downward to the inlet at the lower end of the side of the secondary water-cooling pipe 12, and the outlet at the upper end of the side of the secondary water-cooling pipe 12 is connected to an external connecting pipe. The steam introduced from the distillation head 7 flows through the inner tube of the primary water-cooling pipe 11 and is condensed. The lower opening of the outer tube of the primary water-cooling pipe 11 is connected to a faucet. The condensation of the steam occurs on the inner wall of the inner tube. The space enclosed by the inner and outer tubes provides the water flow area with the ability to absorb the heat of the steam and remove the heat. The steam condensed in the primary water-cooling pipe 11 is introduced into the secondary water-cooling pipe 12 for further condensation. The cooling water in the outer tube of the primary water-cooling pipe 11 enters the secondary water-cooling pipe 12 through the drain pipe 14 to further condense the steam entering the secondary water-cooling pipe 12.

[0033] In this embodiment, the primary water-cooling tube 11 is a serpentine condenser tube, and the inner core tube of the primary water-cooling tube 11 is spiral, which significantly increases the length of the glass tube and the cooling area, making the contact between the steam and the cooling medium more sufficient and achieving a higher heat exchange effect.

[0034] In this embodiment, the secondary water-cooling tube 12 is a spherical condenser tube, and the inner core tube of the secondary water-cooling tube 12 has a spherical structure. The spherical structure of the inner core tube makes it easier for condensate to collect, ensuring that low-boiling-point components are completely condensed during reflux and reducing exhaust emissions.

[0035] This utility model encompasses any substitutions, modifications, equivalent methods, and solutions made within the spirit and scope of this utility model. To provide the public with a thorough understanding of this utility model, specific details are described in detail in the following preferred embodiments; however, those skilled in the art will fully understand this utility model even without these detailed descriptions. Furthermore, to avoid unnecessary confusion regarding the essence of this utility model, well-known methods, processes, procedures, components, and circuits are not described in detail.

[0036] The above description is only a preferred embodiment of the present utility model. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present utility model, and these improvements and modifications should also be considered within the protection scope of the present utility model.

Claims

1. A trimethylsilane azide distillation apparatus, characterized in that, include: The machine includes a frame (1), a controller (2), a mounting rack (3), a magnetic stirring heating mantle (4), an electrically heated distillation column (5), a first support (6), a distillation head (7), a second support (8), a collection bottle (9), a third support (10), a primary water cooling pipe (11), a secondary water cooling pipe (12), a gas guide pipe (13), and a drain pipe (14). The controller (2) is installed on the upper left side of the frame (1), and the mounting rack (3) is welded to the lower right side of the frame (1). The magnetic stirring heating mantle (4) is installed on the mounting rack (3), and the electrically heated distillation column (5) is installed at the upper inner part of the magnetic stirring heating mantle (4). The electrically heated distillation column (5) is installed at the outer side of the side of the electrically heated distillation column (5). A first support (6) is installed, a distillation head (7) is installed on the top of the electrically heated distillation column (5), a second support (8) is installed at the upper right side of the frame (1), a collection bottle (9) is fixedly installed inside the tube sleeve of the second support (8), a third support (10) is installed at the top right side of the frame (1), a primary water-cooling pipe (11) is installed inside the tube sleeve of the third support (10), a secondary water-cooling pipe (12) is installed inside the tube sleeve of the third support (10) on the side of the primary water-cooling pipe (11), a gas guide pipe (13) is installed at the bottom of the primary water-cooling pipe (11), and a drain pipe (14) is installed at the outlet of the upper end of the primary water-cooling pipe (11).

2. The trimethylsilane azide distillation apparatus according to claim 1, characterized in that: The third support (10) extends vertically upward to the upper end of the distillation head (7), and the primary water cooling pipe (11) and the secondary water cooling pipe (12) are located on the upper side of the distillation head (7) through the third support (10).

3. The trimethylsilane azide distillation apparatus according to claim 1, characterized in that: Both the primary water-cooling pipe (11) and the secondary water-cooling pipe (12) are set at an inclination of 15°.

4. The trimethylsilane azide distillation apparatus according to claim 1, characterized in that: The gas guide pipe (13) at the bottom of the primary water cooling pipe (11) is connected to the top of the distillation head (7), and the gas guide pipe (13) is made of PTFE material. The bottom of the distillation head (7) is connected to the collection bottle (9) through a PTFE connector.

5. The trimethylsilane azide distillation apparatus according to claim 1, characterized in that: The other end of the drain pipe (14) is connected downward to the inlet at the lower end of the side of the secondary water cooling pipe (12), and the outlet at the upper end of the side of the secondary water cooling pipe (12) is connected to the external connecting pipe.

6. The trimethylsilane azide distillation apparatus according to claim 1, characterized in that: The primary water-cooling tube (11) is a serpentine condenser tube, and the inner core tube of the primary water-cooling tube (11) is spiral.

7. The trimethylsilane azide distillation apparatus according to claim 1, characterized in that: The secondary water-cooling tube (12) is a spherical condenser tube, and the inner core tube of the secondary water-cooling tube (12) has a spherical structure.

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