High-pressure reactor liquid adding device for laboratory

Abstract

The utility model discloses a high-pressure reactor liquid adding device for a laboratory, and belongs to the technical field of liquid adding of pressure containers. Comprising a liquid adding funnel, a storage tank, a nitrogen inlet pipe, a hydrogen inlet pipe, a nitrogen exhaust pipe and a hydrogen exhaust pipe, the liquid adding funnel is provided with a top cover, a liquid outlet pipe of the liquid adding funnel is provided with a liquid adding valve and penetrates through a top plate of the storage tank to extend into the lower portion of the storage tank, and the top plate of the storage tank is provided with a main gas inlet pipe and the nitrogen exhaust pipe. A hydrogen exhaust pipe is arranged on a branch of a liquid discharge pipe of the liquid adding funnel, the nitrogen inlet pipe and the hydrogen inlet pipe are connected to the main gas inlet pipe in parallel, a main liquid discharge pipe is arranged at the bottom of the storage tank, and a bypass liquid discharge pipe is arranged on a branch of the main liquid discharge pipe. The device is more suitable for practical application of cyclohexanol preparation reaction in a laboratory; the device is simple in structure and reproducible; the storage tank can be conveniently subjected to gas replacement, and the gas combustion and explosion risks can be effectively reduced.

Description

Technical Field

[0001] The utility model relates to a liquid adding device, in particular to a liquid adding device for a high-pressure reactor in a laboratory. Background Art

[0002] As an important cornerstone of modern industry and high-tech, new nylon materials are widely used in industries such as chemical fiber and engineering plastics. Cyclohexanol is a key intermediate in the production of nylon 66 and nylon 6, mainly used in the production of adipic acid, caprolactam, etc., and the demand is increasing year by year. At present, the main production processes of cyclohexanol are phenol hydrogenation method, cyclohexane oxidation method and cyclohexene hydration method. Among them, the cyclohexene hydration method has gradually become the main process for cyclohexanol production due to its advantages such as high safety, high selectivity and low hydrogen consumption.

[0003] To study the process technical parameters in the production process of cyclohexanol, small-scale experiments need to be carried out in the laboratory. This experiment is divided into two parts. The first part is the hydrogenation of benzene to cyclohexene, and the second part is the hydration of cyclohexene to cyclohexanol. During the hydrogenation process, since the reaction kettle is in a pressurized state, liquid cannot be added in the normal way of height difference. Therefore, a liquid adding device for a pressurized reactor is required, and the existing liquid adding device does not have a process for replacing the storage tank. As Figure 1 shown, before the reaction starts, the reactor is purged with gas, then vented to atmospheric pressure and the exhaust valve remains open. Prepare benzene in advance and add it to the liquid adding funnel 1. Open the liquid adding valve 2, and the benzene naturally flows into the reactor. Then, nitrogen and hydrogen are sequentially introduced for replacement. Close the exhaust valve and the liquid adding valve 2, and start the reaction. This method can add a certain amount of benzene for the reaction, but when adding liquid, the reactor needs to be depressurized, which affects the accuracy of the experimental results in terms of liquid adding time, and there is a possibility of hydrogen contacting air, affecting the reaction data and posing a safety hazard. Summary of the Utility Model

[0004] The purpose of the utility model is to solve the problems of unsmooth material flow and more components used in the prior art, and to propose a liquid adding device for a high-pressure reactor in a laboratory.

[0005] In order to achieve the above purpose, the utility model adopts the following technical scheme:

[0006] A liquid adding device for a high-pressure reactor in a laboratory includes a liquid adding funnel, a storage tank, a nitrogen inlet pipe, a hydrogen inlet pipe, a nitrogen exhaust pipe and a hydrogen exhaust pipe. The liquid adding funnel is provided with a top cover, and a liquid adding valve is provided on the liquid outlet pipe of the liquid adding funnel. The liquid outlet pipe of the liquid adding funnel passes through the top plate of the storage tank and extends into the lower part of the storage tank. A main inlet pipe and a nitrogen exhaust pipe are provided on the top plate of the storage tank. A hydrogen exhaust pipe is branched on the liquid discharge pipe of the liquid adding funnel. The nitrogen inlet pipe and the hydrogen inlet pipe are connected in parallel to the main inlet pipe. A main liquid discharge pipe is provided at the bottom of the storage tank, and a bypass liquid discharge pipe is branched on the main liquid discharge pipe.

[0007] Furthermore, a nitrogen inlet valve is provided on the nitrogen inlet pipe, a hydrogen inlet valve is provided on the hydrogen inlet pipe, a main inlet valve and a gas pressure gauge are provided on the main inlet pipe, a hydrogen exhaust valve is provided on the hydrogen exhaust pipe, a nitrogen exhaust valve is provided on the nitrogen exhaust pipe, a main drain valve is provided on the main drain pipe, and a bypass drain valve is provided on the bypass drain pipe.

[0008] Furthermore, the bottoms of the liquid adding funnel and the storage tank are both conical.

[0009] Compared with the prior art, the advantages of the present utility model are as follows: it is more suitable for the actual application of the cyclohexanol reaction in the laboratory; the device structure is simple and reproducible; it is convenient to replace the gas in the storage tank, and can effectively reduce the risks of gas combustion and explosion. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] Figure 1 is a schematic structural diagram of the existing liquid adding device.

[0011] Figure 2 is a schematic structural diagram of the present utility model.

[0012] In the figure: 1. Liquid adding funnel; 2. Liquid adding valve; 3. Main inlet valve; 4. Gas pressure gauge; 5. Top cover; 6. Nitrogen inlet valve; 7. Hydrogen exhaust valve; 8. Hydrogen inlet valve; 9. Nitrogen exhaust valve; 10. Storage tank; 11. Main drain valve; 12. Bypass drain valve. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0013] The technical solutions in the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the present utility model. Obviously, the described embodiments are only a part of the embodiments of the present utility model, rather than all of the embodiments.

[0014] Embodiment 1

[0015] Referring to Figure 2 , a liquid adding device for a high-pressure reactor in a laboratory includes a liquid adding funnel 1, a storage tank 10, a nitrogen inlet pipe, a hydrogen inlet pipe, a nitrogen exhaust pipe, and a hydrogen exhaust pipe. The liquid adding funnel 1 is provided with a top cover 5. A liquid adding valve 2 is provided on the liquid outlet pipe of the liquid adding funnel 1, and the liquid outlet pipe of the liquid adding funnel 1 passes through the top plate of the storage tank 10 and extends into the lower part of the storage tank 10. A main inlet pipe and a nitrogen exhaust pipe are provided on the top plate of the storage tank 10. A hydrogen exhaust pipe is branched on the liquid drain pipe of the liquid adding funnel 1. The nitrogen inlet pipe and the hydrogen inlet pipe are connected in parallel to the main inlet pipe. A main drain pipe is provided at the bottom of the storage tank 10, and a bypass drain pipe is branched on the main drain pipe.

[0016] Among them, a nitrogen inlet valve 6 is provided on the nitrogen inlet pipeline, a hydrogen inlet valve 8 is provided on the hydrogen inlet pipeline, a main inlet valve 3 and a gas pressure gauge 4 are provided on the total inlet pipeline, a hydrogen exhaust valve 7 is provided on the hydrogen exhaust pipeline, a nitrogen exhaust valve 9 is provided on the nitrogen exhaust pipeline, a main drain valve 11 is provided on the main drain pipe, and a bypass drain valve 12 is provided on the bypass drain pipe.

[0017] Furthermore, the bottoms of the liquid addition funnel 1 and the storage tank 10 are both conical.

[0018] With all valves in the closed state, open the nitrogen inlet valve 6, the main inlet valve 3, and the nitrogen exhaust valve 9 for nitrogen replacement. After the nitrogen replacement is completed, close the nitrogen inlet valve 6 and the nitrogen exhaust valve 9, and open the hydrogen inlet valve 8 and the hydrogen exhaust valve 7 for hydrogen replacement. After the hydrogen replacement is completed, close the hydrogen inlet valve 8, the main inlet valve 3, and the hydrogen exhaust valve 7 respectively. Open the top cover 5 and pour a certain amount of benzene reagent into the liquid addition funnel 1. Open the liquid addition valve 2 and the nitrogen exhaust valve 9. After the benzene reagent flows into the storage tank 10, cover the top cover 5 and close the liquid addition valve 2 and the nitrogen exhaust valve 9. If the reaction kettle is in an atmospheric pressure state at this time, the main drain valve 11 can be directly opened to add the benzene reagent to the reaction kettle; if the reaction kettle is in a pressurized state, the hydrogen inlet valve 8 and the main inlet valve 3 need to be opened to pressurize the storage tank. The pressure value of the storage tank is monitored in real time through the gas pressure gauge 4. When the pressure value of the storage tank is slightly higher than the pressure of the reaction kettle, slightly vent the reaction kettle and open the main drain valve 11. The benzene reagent is added to the reaction kettle under the action of the pressure difference. Then close the main drain valve 11, the hydrogen inlet valve 8, and the main inlet valve 3 in sequence. If you want to determine whether all the benzene reagent has flowed into the reaction kettle, you can also check by opening the bypass drain valve 12.

[0019] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A liquid adding device for a laboratory high pressure reactor, characterized in that: The utility model comprises a liquid adding funnel, a storage tank, a nitrogen inlet pipe, a hydrogen inlet pipe, a nitrogen exhaust pipe and a hydrogen exhaust pipe. The liquid adding funnel is provided with a top cover. The liquid outlet pipe of the liquid adding funnel is provided with a liquid adding valve. The liquid outlet pipe of the liquid adding funnel passes through the top plate of the storage tank and extends into the lower part of the storage tank. The top plate of the storage tank is provided with a total air inlet pipe and a nitrogen exhaust pipe. The upper branch of the liquid discharge pipe of the liquid adding funnel is provided with a hydrogen exhaust pipe. The nitrogen inlet pipe and the hydrogen inlet pipe are connected in parallel to the total air inlet pipe. The bottom of the storage tank is provided with a main liquid discharge pipe, and the upper branch of the main liquid discharge pipe is provided with a bypass liquid discharge pipe.

2. The liquid adding device for a laboratory high pressure reactor according to claim 1, characterized in that: A nitrogen inlet valve is provided on the nitrogen inlet pipeline, a hydrogen inlet valve is provided on the hydrogen inlet pipeline, a main inlet valve and a gas pressure gauge are provided on the main inlet pipeline, a hydrogen exhaust valve is provided on the hydrogen exhaust pipe, a nitrogen exhaust valve is provided on the nitrogen exhaust pipe, a main drain valve is provided on the main drain pipe, and a bypass drain valve is provided on the bypass drain pipe.

3. The liquid adding device for a laboratory high pressure reactor according to claim 1, characterized in that: The bottoms of the liquid adding funnel and the storage tank are both conical.

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