Circulating device for volatile liquid and non-volatile liquid or soluble solid solution

Abstract

The utility model discloses a circulating device for volatile liquid and non-volatile liquid or soluble solid solution, and belongs to the technical field of chemical reaction equipment. The device comprises a gas collection container, a liquid-solid reaction operation container and a magnetic stirrer, a pressure release valve is arranged at the top of a container body, and a scale feeding pipe extending into the bottom of the container is arranged; the liquid-solid reaction operation container is a round flask, the lower part of the flask body is connected with a sample receiving pipeline, a reaction monitoring sample receiving switch is arranged on the pipeline, and the bottom of the flask body is also connected with a graduated shunt tube and is provided with a valve; the liquid-solid reaction operation container is placed on the magnetic stirrer, and the gas collection container and the liquid-solid reaction operation container are connected through a diaphragm pump pipeline and a reflux pipeline, so that gas of volatile liquid is pumped into the liquid-solid reaction bottle and enters the gas collection container again through the reflux pipeline under the action of pressure, and recycling of the liquid is realized. The continuous reaction is ensured. The overall design of the equipment is simple and easy to operate, and the equipment has good corrosion resistance and safety.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical reaction equipment, and particularly relates to a circulation device for volatile liquids and non-volatile liquids or soluble solid solutions. Background Art

[0002] When reacting between a volatile liquid and a non-volatile liquid or solid, it is often necessary for the equipment to simultaneously meet the requirements of controlling the reaction pressure, recycling the reactants, and monitoring the reaction progress in real time. However, existing equipment usually cannot effectively achieve continuous cyclic reactions between volatile and non-volatile substances, resulting in low reaction efficiency and difficult-to-control reaction conditions. Therefore, it is particularly important to design a device that can meet the cyclic reaction of volatile liquids. Summary of the Utility Model

[0003] In order to solve the problems of low cyclic utilization efficiency of volatile liquids and difficulty in maintaining stable reaction pressure in the prior art, the utility model provides a circulation device for volatile liquids and non-volatile liquids or soluble solid solutions.

[0004] A circulation device for volatile liquids and non-volatile liquids or soluble solid solutions, characterized in that: it includes a gas collection container, a liquid-solid reaction operation container, and a magnetic stirrer. The container mouth of the gas collection container is sealed by a polytetrafluoroethylene cover. A pressure relief valve is provided at the top of the container body, and a graduated feeding pipe extending to the bottom of the container is provided. The liquid-solid reaction operation container is a round flask, the bottle mouth is sealed by a polytetrafluoroethylene cover, a ground glass feeding port No. 24 is provided at the upper part of the bottle body, a sampling pipeline is led out from the lower part of the bottle body, and a reaction monitoring sampling switch is arranged on the pipeline. A graduated shunt pipe is also led out from the bottom of the bottle body and is provided with a valve. The liquid-solid reaction operation container is placed on the magnetic stirrer, and contactless stirring is achieved through the internal magnetic stir bar. The gas collection container and the liquid-solid reaction operation container are connected by a diaphragm pump pipeline and a reflux pipeline. Both pipelines penetrate into the containers through the polytetrafluoroethylene covers of the two containers. A diaphragm pump is provided on the diaphragm pump pipeline, which extends to a position above the liquid level in the gas collection container and below the liquid level in the liquid-solid reaction operation container. The reflux pipeline extends to the bottom position in the gas collection container and the top position in the liquid-solid reaction operation container.

[0005] The beneficial effects of the present utility model are as follows: The gas collection container and the liquid-solid reaction operation container are connected by a diaphragm pump pipeline, which is used to pump the gas of the volatile liquid into the liquid-solid reaction flask to realize the circulation of the reaction gas. The unreacted part of the volatile liquid re-enters the gas collection container under pressure through the reflux pipeline, realizing the recycling of the volatile liquid and ensuring the continuous progress of the reaction. By circulating the volatile liquid and non-volatile substances, the reaction efficiency can be effectively improved. The pressure relief valve is used to maintain the pressure balance of the reaction system and add a liquid seal layer when needed to prevent the leakage of volatile gases. The graduated feeding pipe and the shunt pipe help to achieve quantitative feeding and by-product shunting during the reaction process. The overall design of the equipment is simple and easy to operate, with good corrosion resistance and safety, and is suitable for various chemical reaction experiments. Description of the Drawings

[0006] Figure 1 It is a schematic structural diagram of a circulation device for volatile liquids and non-volatile liquids or soluble solid solutions.

[0007] Figure 2 It is the reaction chemical formula of benzyl-substituted aryl sulfide and chlorine gas.

[0008] Wherein: 1 - gas collection container, 2 - liquid-solid reaction operation container, 3 - magnetic stirrer, 4 - pressure relief valve, 5 - graduated feeding pipe, 6 - PTFE cover, 7 - ground glass feeding port No. 24, 8 - reaction monitoring sampling switch, 9 - graduated shunt pipe, 10 - diaphragm pump, 11 - reflux pipeline, 12 - liquid chlorine, 13 - liquid seal layer. Detailed Embodiments

[0009] Embodiment 1: A circulation device for volatile liquids and non-volatile liquids or soluble solid solutions, including a gas collection container 1, a liquid-solid reaction operation container 2 and a magnetic stirrer 3. The gas collection container 1 is used to load volatile liquids, such as liquid bromine. The container mouth is sealed by a PTFE cover 6. A pressure relief valve 4 is provided at the top of the container body to maintain the pressure balance of the reaction system and add a liquid seal layer 13, such as water, when needed to prevent the leakage of volatile gases. And a graduated feeding pipe 5 extending to the bottom of the container is provided.

[0010] The liquid-solid reaction operation container 2 is a round flask, which loads non-volatile liquids or soluble solids. The bottle mouth is sealed by a PTFE cover 6. A ground glass feeding port No. 24 7 is provided at the upper part of the bottle body for feeding solids or liquids. A sampling pipeline is led out from the lower part of the bottle body and a reaction monitoring sampling switch 8 is set on the pipeline for real-time sampling and monitoring of the reaction process. A graduated shunt pipe 9 is also led out from the bottom of the bottle body and a valve is provided for shunting the by-products generated during the reaction, such as water or other reaction products. The liquid-solid reaction operation container 2 is placed on the magnetic stirrer 3, and non-contact stirring is realized through the internal magnetic stirrer to ensure uniform progress of the reaction.

[0011] The gas collection container 1 and the liquid-solid reaction operation container 2 are connected by a diaphragm pump pipeline and a reflux pipeline 11. Both pipelines penetrate into the containers through the PTFE covers 6 of the two containers. A diaphragm pump 10 is provided on the diaphragm pump pipeline, which extends to a position above the liquid level in the gas collection container 1 and below the liquid level in the liquid-solid reaction operation container 2. The reflux pipeline 11 extends to the bottom position in the gas collection container 1 and the top position in the liquid-solid reaction operation container 2. The diaphragm pump pipeline is used to pump the gas of the volatile liquid in the gas collection container 1 into the liquid-solid reaction operation container 2 through the diaphragm pump 10. The unreacted part of the volatile liquid can re-enter the gas collection container 1 from the liquid-solid reaction operation container 2 under the action of pressure through the reflux pipe, realizing the circulation of the volatile liquid and the reaction gas and ensuring the continuous progress of the reaction.

[0012] Halogen addition reaction: In organic synthesis, this device can be used for the addition reaction of volatile halogens, such as liquid bromine and olefins. The liquid bromine in the right container volatilizes to form a gas, and the diaphragm pump is used to pump the gas into the reaction flask to react with the reactants. Due to the circulation system of this device, the unreacted bromine gas can be refluxed to the gas collection system, avoiding the waste of halogens and ensuring the continuity and safety of the reaction at the same time.

[0013] Acid-base neutralization reaction: When carrying out the neutralization reaction of organic acids or bases, organic acids can be added to the liquid-solid reaction operation container 2, and ammonia or other basic volatile liquids can be added to the gas collection container 1. Through the recycling of gases, the controllability of the reaction is achieved, and the stability of the reaction system is maintained by the set pressure balance device at the same time.

[0014] Gas-liquid reaction of soluble solids: In material preparation or experimental research, this device can be used for the gas-liquid phase reaction of volatile reagents with non-volatile liquids or soluble solid reactants. For example, most aliphatic sulfonyl chlorides are obtained by reacting corresponding thiols and their derivatives with chlorosulfonating reagents, such as chlorine gas. Therefore, the reaction of thiols and their derivatives with gaseous chlorosulfonating reagents is an important means for synthesizing aliphatic sulfonyl chlorides. The reaction process controls the reaction conditions through a real-time monitoring system to ensure the yield and purity of the product. The reaction chemical formula is as Figure 2 shown.

[0015] In this experimental case, this device is used for the reaction of benzyl-substituted aryl sulfides and chlorine gas. The liquid chlorine 12 in the gas collection container 1 volatilizes to form a gas, and the diaphragm pump 10 is used to pump the gas into the liquid-solid reaction operation container 2 to react with the reactants. Due to the circulation system of this device, the unreacted chlorine gas can be refluxed to the gas collection container 1, avoiding the waste of chlorine gas and ensuring the continuity and safety of the reaction at the same time. And this device can safely control chlorine gas, avoiding chlorine poisoning and the volatilization of the smell of sulfides.

[0016] Photocatalytic reaction: The device is also applicable to the cyclic reaction of volatile substances involved in the photocatalytic process. For example, volatile organic compounds are added to the gas collection container 1, and the catalyst in the liquid-solid reaction operation container 2 can accelerate the reaction to generate the target product under light illumination. Through the recycling of the reaction gas, the full utilization of volatile organic compounds is ensured and environmental pollution is reduced.

[0017] These examples demonstrate the wide applicability of the device in various chemical reactions and the characteristics of efficient recycling, which helps to improve the efficiency and safety in the experimental and industrial production processes.

Claims

1. A circulation device for a volatile liquid and a non-volatile liquid or a soluble solid solution, characterized in that: It includes a gas collection container, a liquid-solid reaction operation container and a magnetic stirrer. The mouth of the gas collection container is sealed by a PTFE cover. A pressure relief valve is provided at the top of the container body, and a graduated feeding pipe extending to the bottom of the container is provided. The liquid-solid reaction operation container is a round flask, the mouth of which is sealed by a PTFE cover. A ground glass feeding port No. 24 is provided at the upper part of the flask body. A sampling pipe is led out from the lower part of the flask body, and a reaction monitoring sampling switch is arranged on the pipe. A graduated shunt pipe is also led out from the bottom of the flask body and is provided with a valve. The liquid-solid reaction operation container is placed on the magnetic stirrer, and contactless stirring is achieved through the internal magnetic stir bar. The gas collection container and the liquid-solid reaction operation container are connected by a diaphragm pump pipe and a reflux pipe. Both pipes penetrate into the containers through the PTFE covers of the two containers. A diaphragm pump is provided on the diaphragm pump pipe, which extends to a position above the liquid level in the gas collection container and below the liquid level in the liquid-solid reaction operation container. The reflux pipe extends to the bottom position in the gas collection container and the top position in the liquid-solid reaction operation container.

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