An automatic reaction liquid separation system for methyl chloroacetate

Abstract

The utility model relates to the field of chemical equipment discloses a kind of methyl chloroacetate reaction automatic liquid separation systems, including reaction kettle, the left side of the reaction kettle is equipped with spiral plate condenser group, the right side of the spiral plate condenser group is equipped with liquid separator tank, the front portion of the liquid separator tank is equipped with water tank, the right side of the liquid separator tank is equipped with methyl chloroacetate tank, the upper portion of the liquid separator tank is equipped with balance pipe fitting.The utility model is with the coherent flow of reaction, condensation, separation collection as core, through the accurate control of each pipeline valve and equipment collaborative operation, the automation operation of methyl chloroacetate reaction whole process is realized, whole process does not need artificial frequent intervention material transfer and separation operation, simultaneously through the mutual cooperation between partition and other components can effectively reduce material disturbance, accelerate two-phase stratification, significantly shorten separation period, compared with traditional manual liquid separation mode, production efficiency is significantly improved.

Description

Technical Field

[0001] This utility model relates to the field of chemical equipment, and in particular to an automatic liquid separation system for methyl chloroacetate reaction. Background Technology

[0002] During the production of intermediate AM, water is generated in the reaction system, which has a significant adverse effect on subsequent reactions. It can lead to decreased reaction efficiency, reduced purity of the target product, and even side reactions, seriously restricting production quality and efficiency. Therefore, it is urgent to separate and remove water efficiently in a timely manner during the reaction process. In existing technologies, the water generated from the intermediate AM reaction and the excess methyl chloroacetate form an azeotrope, which becomes the core target for water separation. However, traditional separation methods are ill-suited to the separation requirements of this system: on the one hand, manual separation is not only inefficient but also highly susceptible to human factors such as operating experience and reaction rhythm, making it impossible to achieve real-time and precise water separation, resulting in poor reaction stability; on the other hand, conventional simple separation devices lack specific designs for the characteristics of methyl chloroacetate-water azeotropes, making it difficult to achieve efficient stratification and automatic collection of the two. Furthermore, under the negative pressure conditions required for the intermediate AM reaction, problems such as poor separation and material retention are prone to occur, further affecting the separation effect. Meanwhile, methyl chloroacetate (MCC) has high recycling value as a raw material. Traditional liquid separation methods easily lead to the loss of MCC during the separation process, which increases raw material costs and may cause environmental risks due to material waste. Furthermore, if the generated water is not collected and treated in a timely and standardized manner, it will also put pressure on the stable operation of subsequent wastewater biological treatment systems. With the increasing demands for automation, efficiency, and green production in the chemical industry, developing a liquid separation system that can adapt to negative pressure reaction environments and achieve automatic stratification and collection based on the characteristics of MCC-water azeotropes, in order to shorten reaction time, reduce energy consumption, improve raw material utilization, and enhance the automation level of the equipment, has become an urgent technical problem to be solved in the intermediate AM production field. Utility Model Content

[0003] To overcome the above shortcomings, this utility model provides an automatic liquid separation system for methyl chloroacetate reaction, which aims to improve the problems of low efficiency in manual liquid separation in the prior art, and the lack of special design for the characteristics of methyl chloroacetate-water azeotrope in conventional simple liquid separation devices, making it difficult to achieve efficient stratification and automatic collection of the two.

[0004] To achieve the above objectives, the present invention adopts the following technical solution: an automatic liquid separation system for methyl chloroacetate reaction, comprising a reaction vessel, a spiral plate condenser assembly installed on the left side of the reaction vessel, a liquid separator tank installed on the right side of the spiral plate condenser assembly, a water tank installed at the front of the liquid separator tank, a methyl chloroacetate tank installed on the right side of the liquid separator tank, a balancing pipe installed at the top of the liquid separator tank, a conveying pipe connected to the right side of the reaction vessel and the spiral plate condenser assembly, a connecting pipe connected to the top of the liquid separator tank and the spiral plate condenser assembly, a liquid delivery pipe connected to the left side of the liquid separator tank and the water tank, and a feed pipe connected to the right side of the liquid separator tank and the methyl chloroacetate tank.

[0005] As a further description of the above technical solution: A vacuum tube is installed on the top of the separator tank.

[0006] As a further description of the above technical solution: An azeotropic liquid tube is installed on the left side of the separator tank, and the top of the azeotropic liquid tube is fixedly connected to the connecting pipe.

[0007] As a further description of the above technical solution: A water inlet is installed on the left side of the liquid separator tank, and the liquid inlet pipe is fixedly connected to the water inlet. A material inlet pipe is connected through and fixedly connected to the right side of the liquid separator tank, and the material inlet pipe is fixedly connected to the material inlet pipe.

[0008] As a further description of the above technical solution: A baffle is fixedly connected to the inner wall of the separator tank.

[0009] As a further description of the above technical solution: The balancing pipe fitting includes a balancing pipe one, which is fixedly connected to the top of the separator tank. A balancing pipe three is connected to the right side of the balancing pipe one via a tee connector. A balancing pipe four is connected to the lower part of the balancing pipe one via a tee connector. The balancing pipe four is connected to the conveying pipe via a tee connector.

[0010] As a further description of the above technical solution: Valves are installed in the middle of the first balance pipe, the second balance pipe, the third balance pipe, as well as the infusion pipe and the feed pipe.

[0011] This utility model has the following beneficial effects: 1. In this utility model, the continuous process of reaction, condensation, separation and collection is the core. Through the precise control of valves in each pipeline and the coordinated operation of equipment, the entire process of methyl chloroacetate reaction is automated. There is no need for frequent manual intervention in material transfer and separation operations. At the same time, the cooperation between components such as baffles can effectively reduce material disturbance, accelerate the two-phase stratification, and significantly shorten the separation cycle. Compared with the traditional manual liquid separation method, the production efficiency is significantly improved.

[0012] 2. In this utility model, a baffle is set in the separator tank to form a stable separation zone, avoiding the stratification disorder caused by material impact. The pressure of the separator tank, methyl chloroacetate tank and pipelines of each tank is balanced in real time by setting up balancing pipe fittings, which effectively avoids the impact of pressure fluctuation on separation accuracy. In addition, the negative pressure environment not only lowers the boiling point of azeotrope to improve condensation efficiency, but also reduces the contact between materials and air, reducing the risk of impurity introduction. The multiple structural designs effectively ensure the separation effect and operational stability of the device. Attached Figure Description

[0013] Figure 1 This is a schematic diagram of the overall front three-dimensional structure of an automatic liquid separation system for methyl chloroacetate reaction proposed in this utility model; Figure 2 This is a schematic diagram of the overall right-side three-dimensional structure of an automatic liquid separation system for methyl chloroacetate reaction proposed in this utility model; Figure 3 This is a three-dimensional cross-sectional view of the separator tank of an automatic liquid separation system for methyl chloroacetate reaction proposed in this utility model.

[0014] Legend: 1. Reactor; 2. Spiral plate condenser assembly; 3. Separator tank; 4. Water tank; 5. Methyl chloroacetate tank; 6. Balancing pipe fittings; 7. Valves; 11. Delivery pipe; 31. Connecting pipe; 32. Liquid delivery pipe; 33. Feed delivery pipe; 34. Vacuum pipe; 61. Balancing pipe one; 62. Balancing pipe two; 63. Balancing pipe three; 64. Balancing pipe four; 301. Azeotropic liquid pipe; 302. Water delivery connector; 303. Baffle; 304. Feed delivery pipe. Detailed Implementation

[0015] 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.

[0016] Reference Figures 1-3This utility model provides an embodiment of an automatic liquid separation system for the reaction of methyl chloroacetate, including a reaction vessel 1, which is the core reaction unit of the automatic liquid separation system. A spiral plate condenser group 2 is installed on the left side of the reaction vessel 1 to realize the condensation of materials. A liquid separator tank 3 is installed on the right side of the spiral plate condenser group 2 to cooperate in realizing the automatic liquid separation of the methyl chloroacetate reaction. A water tank 4 is installed at the front of the liquid separator tank 3 to collect the water generated in the reaction. A methyl chloroacetate tank 5 is installed on the right side of the liquid separator tank 3 for recovering methyl chloroacetate. A balancing pipe 6 is installed at the top of the liquid separator tank 3 to balance the pressure of each tank.

[0017] Furthermore, a conveying pipe 11 is installed on the right side of the reactor 1 and the spiral plate condenser group 2 to transport the azeotrope generated by the reaction to the condensation stage. A connecting pipe 31 is installed on the upper part of the separator tank 3 and the spiral plate condenser group 2 to realize the transfer of materials after condensation. A liquid delivery pipe 32 is installed on the left side of the separator tank 3 and the water tank 4 to collect the separated aqueous phase. A feed pipe 33 is installed on the right side of the separator tank 3 and the methyl chloroacetate tank 5 to recover the separated methyl chloroacetate phase. A vacuum pipe 34 is installed on the top of the separator tank 3, which is connected to a vacuum device to provide a negative pressure environment for the entire system.

[0018] Furthermore, an azeotropic liquid pipe 301 is installed on the left side of the separator tank 3. The top of the azeotropic liquid pipe 301 is fixedly connected to the connecting pipe 31, so that the condensed azeotrope can directly enter the interior of the separator tank 3. A water supply connector 302 is installed on the left side of the separator tank 3 to provide a connection point for the liquid supply pipe 32 for collecting the separated aqueous phase. The liquid supply pipe 32 is fixedly connected to the water supply connector 302. A feed pipe 304 is fixedly connected through and fixedly connected to the right side of the separator tank 3. The feed pipe 304 is fixedly connected to the feed pipe 33 and connected to the methyl chloroacetate tank 5 through the feed pipe 33 for recovering the separated methyl chloroacetate phase. A baffle 303 is fixedly connected to the inner wall of the separator tank 3 to cooperate in forming a separation zone.

[0019] Specifically, the balancing fitting 6 includes a balancing pipe 1 61, which is fixedly connected to the top of the liquid separator tank 3. The right side of the balancing pipe 1 61 is connected to the balancing pipe 3 63 via a tee connector. The lower part of the balancing pipe 1 61 is connected to the balancing pipe 4 64 via a tee connector. The balancing pipe 4 64 is connected to the feed pipe 33 via a tee connector for balancing pressure. Valves 7 are installed in the middle of the balancing pipe 1 61, the balancing pipe 2 62, the balancing pipe 3 63, the liquid delivery pipe 32, and the feed pipe 33 for precise control of the opening and closing of each pipeline and the flow rate.

[0020] Working Principle: The reaction for the formation of methyl chloroacetate occurs in reactor 1. During the reaction, the materials undergo a chemical reaction to form an azeotrope containing methyl chloroacetate and water. At this time, the conveying pipe 11 between the right side of reactor 1 and the spiral plate condenser group 2 is open. Under system pressure, the azeotrope is stably conveyed to the spiral plate condenser group 2 through the conveying pipe 11. After entering the spiral plate condenser group 2, the high-temperature azeotrope comes into full contact with the cooling medium through the heat exchange structure inside the condenser, causing the temperature to drop rapidly and transforming from a gaseous state to a liquid state. The condensed liquid azeotrope needs to be transferred to the separator tank 3. At this time, the valve 7 of the connecting pipe 31 between the upper part of the separator tank 3 and the spiral plate condenser group 2 is opened, and the liquid azeotrope flows through the connecting pipe 31 and... The azeotropic liquid flows into the separator tank 3 through the pipe 301. A stable separation zone is formed within the separator tank 3 by the obstruction and guidance of the baffle 303, allowing for two-phase separation. After the two-phase separation is complete in the separator tank 3, the aqueous phase and methyl chloroacetate phase are recovered separately by controlling the valves 7 of each pipeline. The valve 7 of the delivery pipe 32 between the water connector 302 on the left side of the separator tank 3 and the water tank 4 is opened. Under the pressure difference, the aqueous phase flows through the water connector 302 into the delivery pipe 32 and is ultimately transported to the water tank 4 for collection. Simultaneously, the valve 7 of the delivery pipe 33 between the material delivery connector 304 on the right side of the separator tank 3 and the methyl chloroacetate tank 5 is opened. The methyl chloroacetate phase enters the delivery pipe 33 through the material delivery connector 304 and is then transferred to the methyl chloroacetate tank 5 for recovery.

[0021] Finally, it should be noted that the above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Although the present utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. An automated liquid-liquid separation system for methyl chloroacetate reaction, comprising a reaction vessel (1), characterized in that: A spiral plate condenser assembly (2) is installed on the left side of the reactor (1), a separator tank (3) is installed on the right side of the spiral plate condenser assembly (2), a water tank (4) is installed at the front of the separator tank (3), a methyl chloroacetate tank (5) is installed on the right side of the separator tank (3), a balance pipe (6) is installed on the upper part of the separator tank (3), a conveying pipe (11) is installed between the right side of the reactor (1) and the spiral plate condenser assembly (2), a connecting pipe (31) is installed between the upper part of the separator tank (3) and the spiral plate condenser assembly (2), a liquid delivery pipe (32) is installed between the left side of the separator tank (3) and the water tank (4), and a feed pipe (33) is installed between the right side of the separator tank (3) and the methyl chloroacetate tank (5).

2. The automatic liquid-liquid separation system for methyl chloroacetate reaction according to claim 1, characterized in that: A vacuum tube (34) is installed on the top of the separator tank (3).

3. The automatic liquid-liquid separation system for methyl chloroacetate reaction according to claim 1, characterized in that: An azeotropic liquid tube (301) is installed on the left side of the separator tank (3), and the top of the azeotropic liquid tube (301) is fixedly connected to the connecting pipe (31).

4. The automatic liquid-liquid separation system for methyl chloroacetate reaction according to claim 1, characterized in that: A water inlet connector (302) is installed on the left side of the liquid separator tank (3), and the liquid inlet pipe (32) is fixedly connected to the water inlet connector (302). A material inlet pipe (304) is connected through and fixedly connected to the right side of the liquid separator tank (3), and the material inlet pipe (304) is fixedly connected to the material inlet pipe (33).

5. The automatic liquid-liquid separation system for methyl chloroacetate reaction according to claim 1, characterized in that: The inner wall of the separator tank (3) is fixedly connected with a baffle (303).

6. The automatic liquid-liquid separation system for methyl chloroacetate reaction according to claim 1, characterized in that: The balancing fitting (6) includes a balancing pipe one (61), which is fixedly connected to the top of the liquid separator tank (3). The right side of the balancing pipe one (61) is connected to a balancing pipe three (63) via a three-way connector. The lower part of the balancing pipe one (61) is connected to a balancing pipe four (64) via a three-way connector. The balancing pipe four (64) is connected to the conveying pipe (33) via a three-way connector.

7. The automatic liquid-liquid separation system for methyl chloroacetate reaction according to claim 6, characterized in that: Valves (7) are installed in the middle of the first balance pipe (61), the second balance pipe (62), the third balance pipe (63), the infusion pipe (32), and the feed pipe (33).

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