An organosilicon oil-water liquid system

Abstract

This utility model relates to the field of organosilicon preparation equipment and discloses an organosilicon oil-water separation system. The separation system includes a reaction vessel, a siphon pipe, a receiving tank, and a vacuum pump connected in sequence. One end of the siphon pipe is retractable, allowing it to enter and exit the reaction vessel from the top. The top end of the siphon pipe is connected to the receiving tank. A capacitance detector is installed at the siphon pipe opening, and a level gauge is installed on the reaction vessel. The use of a liftable siphon device prioritizes the separation of the water layer and reduces waste caused by excessive separation of the oil layer. The separation system of this application is suitable for continuous production, has high equipment utilization, a simple and efficient process, reduces workflow, improves production efficiency, enhances product quality, and reduces personnel safety risks.

Description

Technical Field

[0001] This utility model relates to the field of organosilicon preparation equipment, and more specifically, to an organosilicon oil-water liquid system. Background Technology

[0002] The conventional process for preparing branched silicone oils and organosilicon resins includes the following steps:

[0003] 1) First step hydrolysis and condensation: After adding raw materials such as chlorosilane or alkoxysilane and solvent, add dropwise an aqueous solution of acidic or alkaline (in a few cases alkaline, because alkaline conditions are prone to excessive cross-linking) catalyst. The catalyst accelerates the hydrolysis and condensation of active groups. After the reaction is completed, let it stand and separate into layers. The oil layer is retained as the target primary product, and the water layer containing water, solvent, by-products of removed active groups and small molecule silicone oil is removed.

[0004] 2) Second step: neutralization and water washing: neutralize the oil layer first, then wash it with water 2-3 times until it is neutral. To promote separation, solvent is often added. After neutralization and water washing, let it stand to separate the layers and remove the water layer, leaving the neutral oil layer.

[0005] 3) The third step is to remove impurities: remove low molecular weight substances, solvents, water, etc. from the neutral oil layer to obtain the desired product.

[0006] However, existing technologies require the removal of the catalyst-containing water layer after hydrolysis-condensation and neutralization washing. Often, the hydrolysis-condensation products dissolve in the solvent, reducing the density of the water layer (i.e., the water layer is on top, and the silicone oil layer is below). Therefore, the lower oil layer must be discharged to a transfer device before the upper catalyst-containing waste water layer can be discharged. This process presents two problems: first, low efficiency. Discharging the oil layer first, then pumping the water layer back in, or transferring it to the next reaction device is cumbersome, leading to low reactor utilization and low production efficiency. Second, multiple discharges pose material quality and safety risks, as well as personnel safety hazards. Especially when the waste water layer after hydrolysis-condensation contains acidic or alkaline catalysts and solvents, the discharge process increases the risk of secondary contamination, while the catalyst and solvent during separation can easily harm operators and cause health hazards.

[0007] In summary, the existing production processes of branched silicone oils and silicone resins, especially the liquid separation process, suffer from problems such as cumbersome procedures, low efficiency, and safety hazards, which are detrimental to both improving production efficiency and ensuring safe production. Summary of the Invention

[0008] This invention addresses the shortcomings of existing technologies by providing an organosilicon oil-water liquid system, which can effectively improve production efficiency, enhance product quality, and reduce personnel safety risks.

[0009] To achieve the above objectives, the present invention adopts the following technical solution:

[0010] An organosilicon oil-water separation system, the separation system includes a reaction vessel, a siphon, a receiving tank and a vacuum pump connected in sequence. One end of the siphon is retractable and can enter and exit the reaction vessel from the top. The top end of the siphon is connected to the receiving tank.

[0011] The siphon tube is equipped with a capacitance detector at its opening, which can detect whether the opening is in a water layer or an oil layer, providing position guidance for the siphon tube; the siphon tube is also connected to a controller, which can adjust the raising and lowering based on the capacitance monitoring results to assist in achieving precise liquid separation;

[0012] The reactor is equipped with a level gauge, which can clearly identify the dynamic changes in liquid level during the stratification and separation process, and guide the separation process.

[0013] Preferably, the siphon tube has a funnel-shaped opening, which can increase the contact area between the siphon tube and the liquid.

[0014] Preferably, the controller is equipped with a power device for controlling the raising and lowering of the siphon tube and a capacitance monitoring and display device.

[0015] Preferably, the reactor is equipped with a stirring paddle.

[0016] Preferably, the receiving tank is provided with a drain port at the bottom.

[0017] Preferably, the level gauge is a radar level gauge, an ultrasonic level gauge, or a differential pressure level gauge.

[0018] Preferably, a vacuum buffer tank is provided between the receiving tank and the vacuum pump to prevent the vaporization of solvents, water, acids, etc. extracted under negative pressure from entering the vacuum pump and other equipment and damaging the vacuum system.

[0019] Preferably, the vacuum buffer tank contains an adsorbent and a desiccant.

[0020] This application addresses the problem of stratified drainage of silicone oil-water mixtures, particularly the issue of a water layer on top and an oil layer below, which leads to a cumbersome drainage process, low production efficiency, and potential safety hazards for materials and personnel. It designs a highly efficient silicone oil-water separation system. The system leverages the physical differences between silicone oil and water, employing a liftable siphon pipe to preferentially siphon the upper water layer (containing solvents and other waste liquid) out of the reactor under negative pressure. A capacitive sensor monitors the oil-water interface, allowing for real-time monitoring of the separation process and preventing excessive oil separation. Furthermore, by adjusting the negative pressure level for step-by-step siphoning, excessive oil layer loss can be effectively reduced. After the upper waste liquid is completely drained, the oil layer remains in the reactor, eliminating the need for the cumbersome process of first draining and then pumping in, allowing for the next steps of neutralization, washing, and stratification.

[0021] The beneficial effects of this utility model are:

[0022] (1) The use of a liftable siphon device can prioritize the separation of the water layer, eliminating the need for the cumbersome process of draining the oil layer before pumping it in, thus reducing the workflow, improving production efficiency, and reducing the quality risks of secondary pollution from material exposure and personnel health and safety risks.

[0023] (2) Real-time detection using a capacitance detector can effectively guide the liquid separation process and reduce waste caused by excessive liquid separation of the oil layer.

[0024] (3) The liquid separation system of this application is suitable for continuous production, with high equipment utilization and simple and efficient process. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the structure of an organosilicon oil-water liquid system.

[0026] Figure reference numerals: 1-Reaction vessel, 101-Water layer, 102-Oil layer, 11-Agitator, 2-Siphon, 201-Port, 21-Controller, 3-Receiving tank, 301-Drain outlet, 4-Vacuum pump, 5-Vacuum buffer tank. Detailed Implementation

[0027] The technical solutions in the embodiments of this utility model will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model.

[0028] In the description of this application, it should be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this application.

[0029] An organosilicon oil-water liquid system, such as Figure 1 As shown, the liquid separation system includes a reaction vessel 1, a siphon pipe 2, a receiving tank 3, a vacuum buffer tank 5, and a vacuum pump 4 connected in sequence. The receiving tank 3, the vacuum buffer tank 5, and the vacuum pump 4 are interconnected by pipes. The receiving tank 3 is used to receive and store the water layer 101 sucked out by the negative pressure siphon process, and a drain port 301 is provided at its bottom. The vacuum buffer tank 5 contains an adsorbent and a desiccant.

[0030] The siphon 2 has a retractable port 201 at one end, allowing it to enter and exit the reactor 1 from the top. The top end of the siphon 2 is connected to the receiving tank 3, with the connection point located at the top of the receiving tank 3. The port 201 of the siphon 2 is funnel-shaped and equipped with a capacitance detector. A controller 21 is also connected to the siphon 2, which includes a power unit for controlling the lifting and lowering of the siphon 2 and a capacitance monitoring and display device.

[0031] The reactor 1 is equipped with a stirring paddle 11 for stirring operations during the initial hydrolysis-condensation, water washing, and neutralization processes before stratification. During the static stratification process, the stirring paddle 11 remains stationary. The reactor 1 is also equipped with a level gauge, which can be a radar level gauge, an ultrasonic level gauge, or a differential pressure level gauge, or other level gauges not mentioned in this application. It can be installed inside or outside the reactor 1 to clearly identify the dynamic changes in liquid level during stratification and separation, further guiding the separation operation of the separation system.

[0032] The operating procedure for the silicone oil-water liquid system is as follows:

[0033] After the reaction in reactor 1 is completed, the agitator 11 stops operating, and the liquid in reactor 1 begins to separate into layers. After the separation is complete, the controller 21 controls the movable siphon tube 2, with its port 201, to move to a position 3-5 cm above the boundary between the silicone oil and water layers, based on the indications of the capacitance detector and the level gauge. Then, the vacuum pump 4 is turned on, maintaining a vacuum of -0.1 to -0.3 MPa. The siphon tube 2 performs negative pressure siphoning, drawing the water layer 101 into the receiving tank 3 until no more liquid is drawn out. The vacuum pump 4 is then turned off. Next, the port 201 of the siphon tube 2 is slowly moved down to a position 0.5-1 cm above the boundary between the silicone oil and water layers. The vacuum pump 4 is then slowly turned on again, maintaining a vacuum of 0.3 to -0.5 MPa, slowly drawing the remaining liquid in the water layer 101 into the receiving tank 3 until no more liquid is drawn out. At this point, it can be considered that the water layer 101 has been completely drawn into the receiving tank 3.

[0034] The above description of embodiments of the present invention, through which those skilled in the art are able to implement or use the present invention, will be readily apparent to those skilled in the art. Various modifications to these embodiments will be readily apparent to those skilled in the art. The general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novelty disclosed herein.

Claims

1. An organosilicon oil-water liquid system, characterized in that, The liquid separation system includes a reaction vessel (1), a siphon (2), a receiving tank (3), and a vacuum pump (4) connected in sequence. One end of the siphon (2) port (201) is retractable and can enter and exit the reaction vessel (1) from the top. The top end of the siphon (2) is connected to the receiving tank (3). A capacitance detector is provided on the inlet (201) of the siphon (2), and a controller (21) is also connected to the siphon (2). A level gauge is installed on the reactor (1).

2. The silicone oil-water liquid system according to claim 1, characterized in that, The siphon tube (2) has a funnel-shaped opening (201).

3. The silicone oil-water liquid system according to claim 1, characterized in that, The controller (21) is equipped with a power device for controlling the lifting and lowering of the siphon (2) and a capacitor monitoring and display device.

4. The organosilicon oil-water liquid system according to claim 1, characterized in that, The reactor (1) is equipped with a stirring paddle (11).

5. The silicone oil-water liquid system according to claim 1, characterized in that, The receiving tank (3) is provided with a drain port (301) at the bottom.

6. The silicone oil-water liquid system according to claim 1, characterized in that, The level gauge is a radar level gauge, an ultrasonic level gauge, or a differential pressure level gauge.

7. A silicone oil-water liquid system according to any one of claims 1-6, characterized in that, A vacuum buffer tank (5) is provided between the receiving tank (3) and the vacuum pump (4).

8. The silicone oil-water liquid system according to claim 7, characterized in that, The vacuum buffer tank (5) contains an adsorbent and a desiccant.

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