Dimethylamine gas generating device for laboratory

Abstract

The utility model discloses a dimethylamine gas generating device for a laboratory, which comprises a constant-pressure dropping funnel, a gas making bottle, a first gas extraction head, a bubbler, a drying tower, a snakelike condenser pipe, a reaction bottle, a second gas extraction head, a U-shaped bubbler, a first magnetic stirrer and a second magnetic stirrer, the other opening of the gas making bottle is connected with a first gas extraction head, the gas making bottle is arranged above the first magnetic stirrer, the first gas extraction head is sleeved with a first rubber pipe, the other end of the first rubber pipe is connected to a gas inlet of the bubbler, and a gas outlet of the bubbler is connected with a gas inlet of the drying tower through a second rubber pipe. A gas outlet of the drying tower is connected with a gas inlet of the snakelike condensation pipe through a rubber pipe III, a gas outlet of the snakelike condensation pipe is connected to the reaction bottle, and the reaction bottle is arranged above the magnetic stirrer II; the technical problem that in the prior art, when dimethylamine gas is prepared through an existing method, a dimethylamine aqueous solution which is difficult to store needs to be used is solved.

Description

Technical Field

[0001] This utility model relates to the field of experimental equipment technology, and more specifically, to a dimethylamine gas generator for laboratory use. Background Technology

[0002] In existing technologies, dimethylamine gas is a colorless gas with a pungent odor, highly soluble in water, and is an important intermediate in the production of various chemical products. For example, in pesticide production, dimethylamine can be used to prepare fungicides (such as thiram and thiram), insecticides (such as imidacloprid and chlorpyrifos), and herbicides (such as chlormequat and isoproturon). In the pharmaceutical industry, dimethylamine is an intermediate for many drugs, such as antidepressants and anticancer drugs. In the semiconductor field, dimethylamine is an important raw material for the High-K metal precursors tetratetra(dimethylamino)zirconium and tetratetra(dimethylamino)hafnium.

[0003] Industrially, dimethylamine gas is produced by the methanol amination process, where methanol and ammonia react in the presence of a catalyst to generate methylamine. Methylamine then reacts with methanol to produce dimethylamine and trimethylamine. Alternatively, dimethylamine can be synthesized directly from methylamine and methanol. In the laboratory, dimethylamine gas is commonly produced by mixing an aqueous solution of dimethylamine with sodium hydroxide, or by directly heating an aqueous solution of dimethylamine. However, both methods require the use of dimethylamine aqueous solution, which is difficult to store. Furthermore, a heat source is needed during the gas production process, making the reaction difficult to control and posing certain safety hazards. Utility Model Content

[0004] (a) Technical problems to be solved

[0005] To address the problems existing in the prior art, this utility model provides a laboratory dimethylamine gas generator, which solves the technical problem mentioned in the background art that the existing methods for producing dimethylamine gas all require the use of dimethylamine aqueous solution, which is difficult to store.

[0006] (II) Technical Solution

[0007] To achieve the above objectives, this utility model provides the following technical solution: a laboratory dimethylamine gas generator, comprising a constant pressure dropping funnel, a gas generating bottle, a first suction head, a bubbler, a drying tower, a serpentine condenser, a reaction flask, a second suction head, a U-shaped bubbler, a first magnetic stirrer, and a second magnetic stirrer. One end of the gas generating bottle is connected to the constant pressure dropping funnel, and the other end of the gas generating bottle is connected to the first suction head. The gas generating bottle is positioned above the first magnetic stirrer. The suction head is fitted with a first rubber tube, the other end of which is connected to the inlet of the bubbler. The outlet of the bubbler is connected to the inlet of the drying tower via a second rubber tube. The outlet of the drying tower is connected to the inlet of the serpentine condenser via a third rubber tube. The outlet of the serpentine condenser is connected to the reaction flask, which is positioned above the second magnetic stirrer. The other outlet of the reaction flask is connected to the second suction head, and the second suction head is connected to the inlet of the U-shaped bubbler via a fourth rubber tube.

[0008] The present invention is further configured such that the gas generating bottle and the reaction bottle are two-necked or three-necked bottles, which facilitates the operation process.

[0009] The present invention is further configured such that all grinding joints in the device are sealed with vacuum silicone grease or PTFE tape, thereby ensuring stable operation.

[0010] The present invention is further configured such that the liquid in the constant pressure dropping funnel is N,N-dimethylformamide (DMF), which makes the operation more convenient.

[0011] The present invention is further configured such that the liquid in the gas generating bottle is an aqueous solution of sodium hydroxide, which makes the operation steps more convenient.

[0012] The present invention is further configured such that the liquid in the bubbler is paraffin wax, thereby making the operation steps faster by using paraffin wax.

[0013] The present invention is further configured such that the solid in the drying tower is sodium hydroxide, thereby making the drying process more convenient by using sodium hydroxide.

[0014] The present invention is further configured such that the refrigerant temperature inside the serpentine condenser is -10℃, thereby making the operation more practical by using a specific temperature.

[0015] The present invention is further configured such that one side of the U-shaped bubbler is empty and the other side is filled with water, so that the operation steps can be carried out stably by using the U-shaped bubbler.

[0016] (III) Beneficial Effects

[0017] Compared with the prior art, this utility model provides a laboratory dimethylamine gas generator, which has the following beneficial effects:

[0018] 1. The devices described are all common laboratory glassware or consumables, which are easy to install, safe to operate, and have an anti-backflow function. The generation rate of dimethylamine gas can be adjusted and controlled at any time, which greatly improves experimental efficiency and meets the needs of the laboratory for using dimethylamine gas.

[0019] 2. This utility model provides a laboratory dimethylamine gas generator. The experimental device is simple and readily available, easy to install, safe to operate, and the dimethylamine gas generation rate can be adjusted and controlled at any time, greatly improving experimental efficiency and meeting the needs of laboratory use of dimethylamine gas.

[0020] 3. The experimental apparatus is simple and readily available, easy to install, and safe to operate. The generation rate of dimethylamine gas can be adjusted and controlled at any time, which greatly improves experimental efficiency and meets the needs of laboratory use of dimethylamine gas. In addition, all ground joints in the apparatus are sealed with vacuum silicone grease or PTFE tape to ensure good airtightness of the system. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the overall structure of a laboratory dimethylamine gas generator according to the present invention;

[0022] Figure 2 This is a partial structural schematic diagram of the present invention;

[0023] Figure 3 This is a partial side view of the structure of this utility model;

[0024] Figure 4 This is a partial cross-sectional structural schematic diagram of the present invention;

[0025] Figure 5 This is a partial cross-sectional side view of the structure of this utility model.

[0026] In the diagram: 1. Constant pressure dropping funnel, 2. Gas generator bottle, 3. Vacuum head one, 4. Bubbler, 5. Drying tower, 6. Snake condenser, 7. Reaction flask, 8. Vacuum head two, 9. U-shaped bubbler, 10. Magnetic stirrer one, 11. Magnetic stirrer two, 12. Rubber tube one, 13. Rubber tube two, 14. Rubber tube three, 15. Rubber tube four. Detailed Implementation

[0027] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0028] It should be noted that, unless otherwise specified, all technical and scientific terms used in this application have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains.

[0029] In this utility model, unless otherwise stated, the orientations used, such as "up" and "down", usually refer to the direction shown in the accompanying drawings, or to the vertical, perpendicular, or gravitational direction; similarly, for ease of understanding and description, "left" and "right" usually refer to the left and right shown in the accompanying drawings; "inner" and "outer" refer to the inner and outer contours of each component itself, but the above directional terms are not used to limit this utility model.

[0030] Please see Figures 1-5 A laboratory dimethylamine gas generator includes a constant-pressure dropping funnel 1, a gas generating bottle 2, a suction head 3, a bubbler 4, a drying tower 5, a serpentine condenser 6, a reaction flask 7, a second suction head 8, a U-shaped bubbler 9, a magnetic stirrer 10, and a second magnetic stirrer 11. One end of the gas generating bottle 2 is connected to the constant-pressure dropping funnel 1, and the other end of the gas generating bottle 2 is connected to the suction head 3. The gas generating bottle 2 is positioned above the magnetic stirrer 10, and the suction head 3 is fitted with a rubber tube 12. The other end of rubber tube 12 is connected to the air inlet of bubbler 4. The air outlet of bubbler 4 is connected to the air inlet of drying tower 5 through rubber tube 2 13. The air outlet of drying tower 5 is connected to the air inlet of serpentine condenser 6 through rubber tube 3 14. The air outlet of serpentine condenser 6 is connected to reaction flask 7. Reaction flask 7 is placed above magnetic stirrer 2 11. The other outlet of reaction flask 7 is connected to suction head 2 8. Suction head 2 8 is connected to the air inlet of U-shaped bubbler 9 through rubber tube 4 15.

[0031] Gas generator 2 and reaction flask 7 are either two-necked or three-necked flasks.

[0032] All ground joints in the device are sealed with vacuum silicone grease or PTFE tape.

[0033] The liquid in constant pressure dropping funnel 1 is N,N-dimethylformamide (DMF).

[0034] The liquid in gas cylinder 2 is an aqueous solution of sodium hydroxide.

[0035] The liquid in bubbler 4 is paraffin.

[0036] The solid in drying tower 5 is sodium hydroxide.

[0037] The refrigerant temperature inside the serpentine condenser tube 6 is -10℃.

[0038] The U-shaped bubbler 9 has one side empty and the other side filled with water.

[0039] In this embodiment, during the experiment, a certain amount of N,N-dimethylformamide was added to the constant-pressure dropping funnel 1, and a corresponding amount of sodium hydroxide aqueous solution was added to the two-necked flask 2. The magnetic stirrer 10 was started to stir. When DMF was added dropwise to the two-necked flask 2, dimethylamine gas was rapidly generated. The vacuum head 3 was opened, and the dimethylamine gas entered the drying tower 5 through the bubbler 4. The sodium hydroxide in the drying tower 5 dried the dimethylamine gas. The dried dimethylamine gas was condensed and liquefied after passing through the serpentine condenser 6 and added dropwise to the reaction flask 7. Excess dimethylamine gas was absorbed when passing through the U-shaped bubbler 9. During the experiment, the generation rate of dimethylamine gas could be controlled by adjusting the piston of the constant-pressure dropping funnel 1. To prevent backflow and to avoid the emission of excess dimethylamine gas into the atmosphere, which could cause environmental pollution and harm to human health, the reaction flask 7 was connected to the U-shaped bubbler 9. The U-shaped bubbler serves both as an anti-backflow device and a tail gas remover. Excess gas is absorbed by the water on the right side of the U-shaped bubbler. When backflow occurs, the water on the right side will flow into the empty branch tube on the left side instead of entering the reaction flask, thus preventing backflow.

[0040] In summary, during the use or operation of the overall equipment: A certain amount of N,N-dimethylformamide is added to the constant-pressure dropping funnel 1, and a corresponding amount of sodium hydroxide aqueous solution is added to the two-necked flask 2. The magnetic stirrer 10 is started. When DMF is added dropwise to the two-necked flask 2, dimethylamine gas is rapidly generated. The vacuum head 3 is opened, and the dimethylamine gas enters the drying tower 5 through the bubbler 4. The sodium hydroxide in the drying tower 5 dries the dimethylamine gas. The dried dimethylamine gas is condensed and liquefied after passing through the serpentine condenser 6 and added dropwise to the reaction flask 7. Excess dimethylamine gas is absorbed when it passes through the U-shaped bubbler 9. During the experiment, the generation rate of dimethylamine gas can be controlled by adjusting the piston of the constant-pressure dropping funnel 1. To prevent backflow and to avoid the emission of excess dimethylamine gas into the atmosphere, which could cause environmental pollution and harm to human health, the reaction flask 7 is connected to the U-shaped bubbler 9. The U-shaped bubbler serves both as an anti-backflow device and a tail gas remover. Excess gas is absorbed by the water on the right side of the U-shaped bubbler. When backflow occurs, the water on the right side will flow into the empty branch tube on the left side instead of entering the reaction flask, thus preventing backflow.

[0041] Of all the solutions mentioned above, those involving the connection between two components can be selected according to the actual situation, such as welding, bolt and nut connection, bolt or screw connection, or other known connection methods, which will not be elaborated here. For all the fixed connections mentioned above, welding is preferred. Although embodiments of this utility model have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of this utility model. The scope of this utility model is defined by the appended claims and their equivalents.

Claims

1. A laboratory dimethylamine gas generator, characterized in that: The system includes a constant pressure dropping funnel (1), a gas generating bottle (2), a first suction head (3), a bubbler (4), a drying tower (5), a serpentine condenser (6), a reaction flask (7), a second suction head (8), a U-shaped bubbler (9), a first magnetic stirrer (10), and a second magnetic stirrer (11). One end of the gas generating bottle (2) is connected to the constant pressure dropping funnel (1), and the other end of the gas generating bottle (2) is connected to the first suction head (3). The gas generating bottle (2) is placed above the first magnetic stirrer (10). The first suction head (3) is fitted with a first rubber tube (12). The first rubber tube (12) is... The other end of the bubbler (4) is connected to the air inlet of the bubbler (4). The air outlet of the bubbler (4) is connected to the air inlet of the drying tower (5) through rubber tube two (13). The air outlet of the drying tower (5) is connected to the air inlet of the serpentine condenser (6) through rubber tube three (14). The air outlet of the serpentine condenser (6) is connected to the reaction flask (7). The reaction flask (7) is placed above the magnetic stirrer two (11). The other outlet of the reaction flask (7) is connected to the suction head two (8). The suction head two (8) is connected to the air inlet of the U-shaped bubbler (9) through rubber tube four (15).

2. The laboratory dimethylamine gas generator according to claim 1, characterized in that: The gas generating bottle (2) and the reaction bottle (7) are two-necked or three-necked bottles.

3. A laboratory dimethylamine gas generator according to claim 2, characterized in that: All ground joints in the device are sealed with vacuum silicone grease or PTFE tape.

4. A laboratory dimethylamine gas generator according to claim 3, characterized in that: The liquid in the constant pressure dropping funnel (1) is N,N-dimethylformamide (DMF).

5. A laboratory dimethylamine gas generator according to claim 4, characterized in that: The liquid in the gas-generating bottle (2) is an aqueous solution of sodium hydroxide.

6. A laboratory dimethylamine gas generator according to any one of claims 1-5, characterized in that: The liquid in the bubbler (4) is paraffin.

7. A laboratory dimethylamine gas generator according to claim 6, characterized in that: The solid in the drying tower (5) is sodium hydroxide.

8. A laboratory dimethylamine gas generator according to claim 7, characterized in that: The refrigerant temperature inside the serpentine condenser (6) is -10℃.

9. A laboratory dimethylamine gas generator according to claim 8, characterized in that: The U-shaped bubbler (9) has an empty side and a water side.

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