A continuous hydrolysis system for silicone

Abstract

The application relates to the field of organic silicon production equipment, and particularly discloses a continuous hydrolysis system for organic silicon, which comprises a hydrolysis unit, a separation unit and a post-treatment pipe group. The hydrolysis unit comprises a reaction pipeline, a circulating pump and a hydrolysis cooler. One end of the reaction pipeline is connected with the circulating pump. A first conveying pipeline is connected between the circulating pump and the reaction pipeline. A second conveying pipeline is connected between the circulating pump and the hydrolysis cooler. The bottom of the hydrolysis cooler is a liquid inlet, and the top of the hydrolysis cooler is a liquid outlet. The second conveying pipeline is connected with the liquid inlet. The separation unit comprises an oil-water separator which is connected with the hydrolysis cooler and a water washing kettle which is connected with the oil-water separator. The top of the oil-water separator is an oil outlet, and the bottom of the oil-water separator is a water outlet. The bottom of the water washing kettle is a discharge outlet. The discharge outlet is connected with the post-treatment pipe group. The continuous hydrolysis system for organic silicon has the effects of improving yield and reaction efficiency.

Description

Technical Field

[0001] This application relates to the field of organosilicon production equipment, and in particular to a continuous organosilicon hydrolysis system. Background Technology

[0002] Organosilicon materials, with their excellent temperature resistance, weather resistance, electrical insulation and physiological inertness, are widely used in aerospace, electronics, medical care, new energy and construction and other fields. The basic raw material of organosilicon materials is polysiloxane, and the synthesis of polysiloxane depends heavily on the key intermediate - hydroxyl silicone oil or cyclosiloxane.

[0003] These intermediates are mainly prepared by hydrolysis of organosilicon monomers (such as trimethylchlorosilane). Therefore, the hydrolysis process is the "heart" of the entire organosilicon industry chain, and its technological level directly determines the quality of the final organosilicon product.

[0004] In some existing equipment, batch hydrolysis is commonly used. This process typically involves directly feeding a fixed amount of water and chlorosilane monomers into a large reactor for a vigorous reaction. After the reaction is complete, the mixture is allowed to settle, separated, and washed to obtain the product. However, this batch feeding method is prone to uneven reactant concentrations, leading to intense competition between hydrolysis and condensation side reactions, which in turn reduces product yield and reaction efficiency. Utility Model Content

[0005] To improve yield and reaction efficiency, this application provides a continuous organosilicon hydrolysis system.

[0006] The organosilicon continuous hydrolysis system provided in this application adopts the following technical solution: An organosilicon continuous hydrolysis system, comprising: The hydrolysis unit includes a reaction pipeline, a circulation pump, and a hydrolysis cooler. A first delivery pipeline connects the circulation pump to the reaction pipeline, and a second delivery pipeline connects the circulation pump to the hydrolysis cooler. The bottom of the hydrolysis cooler is an inlet, and the top of the hydrolysis cooler is an outlet. The second delivery pipeline is connected to the inlet. The separation unit includes an oil-water separator connected to a hydrolysis cooler and a water washing tank connected to the oil-water separator. The top of the oil-water separator is an oil outlet and the bottom is a water outlet. The bottom of the water washing tank is a discharge outlet, and the discharge outlet is connected to a post-processing pipe assembly.

[0007] By adopting the above technical solution, the reaction pipeline enables materials to flow, react, and be output continuously, achieving uninterrupted production. Furthermore, since the feed rates of materials and water are constant, uniform mixing of reactants can be achieved, avoiding local over-concentration from the source. This ensures that the hydrolysis reaction can proceed in a dominant manner, thereby improving the selectivity of siloxanes and enhancing product quality.

[0008] Optionally, a first check valve is provided at one end of the reaction pipeline near the first delivery pipeline.

[0009] By adopting the above technical solution, the first check valve can effectively prevent the reaction liquid from flowing back into the reaction pipeline, thereby ensuring the unidirectional and stable flow of materials and ensuring the stability of continuous reaction.

[0010] Optionally, a second check valve is provided at the end of the second delivery pipeline near the circulating pump.

[0011] By adopting the above technical solution, the second check valve can effectively prevent materials from flowing back from the second conveying pipe or hydrolysis cooler to the circulating pump, thereby ensuring the safety of the circulating pump equipment and the stable conveying of the circulating circuit.

[0012] Optionally, at least two washing tanks are arranged in parallel. By adopting the above technical solution, multiple washing tanks can operate alternately, allowing materials to continuously enter the separation unit from upstream without accumulating or interrupting due to the intermittent nature of the washing process. This ensures continuous and stable operation of the entire system from hydrolysis to washing, effectively increasing production.

[0013] Optionally, the post-treatment pipe assembly includes a strong acid recovery pipe, a weak acid recovery pipe, a wastewater treatment pipe, and a material recovery pipe.

[0014] By adopting the above technical solution, the water discharged from the washing tank multiple times can enter different pipes according to different pH values. Strong acidic wastewater can be discharged from the strong acid recovery pipe and recycled for the preparation of hydrochloric acid as a by-product. Weak acidic wastewater can be recycled as water for hydrolysis and washing processes, thereby improving resource utilization.

[0015] Optionally, a flow meter is installed at the end of the first delivery pipeline near the circulating pump.

[0016] Optionally, the water outlet is connected to an acid outlet pipe, and the acid outlet pipe is equipped with a liquid level controller.

[0017] By adopting the above technical solution, the level controller can effectively control the opening and closing of the acid outlet pipe, thereby controlling the water phase level in the oil-water separator. Optionally, the oil-water separator is equipped with a level transmitter, which is used to transmit the level signal to the level controller.

[0018] By adopting the above technical solution, the level transmitter can accurately measure the interface position inside the oil-water separator, thereby preventing "oil spill" or "acid spill" accidents caused by uncontrolled level, and ensuring production safety and the stability of downstream processes.

[0019] In summary, this application has the following beneficial effects: 1. By setting up hydrolysis and separation units, the entire reaction process can be made uninterrupted by hydrolysis, and the reaction products can be continuously separated and purified.

[0020] 2. By setting up post-treatment pipe groups, different treatments can be carried out according to the composition of the washing wastewater, thereby effectively improving resource utilization. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the structure of the organosilicon continuous hydrolysis system according to an embodiment of this application; Figure 2 This is a schematic diagram of the structure of the hydrolysis unit according to an embodiment of this application; Figure 3 This is a schematic diagram of the structure of the separation unit in an embodiment of this application; Figure 4 This is a schematic diagram of the structure of the oil-water separator according to an embodiment of this application; Explanation of reference numerals in the attached drawings: 1. Hydrolysis unit; 11. Reaction pipeline; 111. First check valve; 12. Circulation pump; 13. Hydrolysis cooler; 131. Inlet; 132. Outlet; 14. First conveying pipeline; 141. Flow meter; 15. Second conveying pipeline; 151. Second check valve; 2. Separation unit; 21. Oil-water separator; 211. Oil outlet; 212. Water outlet; 213. Level transmitter; 22. Washing vessel; 221. Discharge outlet; 23. Acid outlet pipe; 231. Level controller; 3. Post-treatment pipeline assembly; 31. Strong acid recovery pipe; 32. Weak acid recovery pipe; 33. Wastewater treatment pipe; 34. Material recovery pipe. Detailed Implementation

[0022] The following is in conjunction with the appendix Figure 1-4 This application will be described in further detail.

[0023] This application discloses a continuous organosilicon hydrolysis system. (Refer to...) Figure 1 , Figure 2The organosilicon continuous hydrolysis system includes a hydrolysis unit 1 and a separation unit 2. The hydrolysis unit 1 includes a reaction pipeline 11, a circulating pump 12 and a hydrolysis cooler 13. There are two reaction pipelines 11. The inlet of the circulating pump 12 is fixedly connected to a first delivery pipeline 14. Both reaction pipelines 11 are connected to the first delivery pipeline. A second delivery pipeline 15 is connected between the circulating pump 12 and the hydrolysis cooler 13. The bottom of the hydrolysis cooler 13 is the liquid inlet 131 and the top is the liquid outlet 132. The second delivery pipeline 15 is connected to the liquid inlet 131.

[0024] During the hydrolysis reaction, water and chlorosilane enter the reaction pipe 11 and undergo hydrolysis. The flow of materials in the reaction pipe 11 is close to plug flow, and the residence time of all materials is highly consistent. This means that the material per unit volume undergoes the exact same reaction process, avoiding the phenomenon of excessively high local concentrations. This ensures that the hydrolysis reaction dominates the reaction process, and the condensation reaction is effectively suppressed, thereby improving the selectivity of siloxanes and ensuring product quality.

[0025] Reference Figure 1 , Figure 2 A first check valve 111 is installed at the end of the reaction pipeline 11 near the first conveying pipeline 14. The first check valve 111 can effectively prevent material from flowing back from the first conveying pipeline 14 into the reaction pipeline 11, thereby ensuring stable mixing of material in the reaction pipeline 11 and ensuring the stability of continuous reaction. A second check valve 151 is installed at the end of the second conveying pipeline 15 near the circulating pump 12. In order to ensure that the material is fully cooled by the hydrolysis cooler 13, the circulating pump 12 needs to pump the material from a lower position to an upper position. The second check valve 151 can effectively prevent the material from flowing back into the circulating pump 12, and prevent the material from the hydrolysis cooler 13 from backflowing and impacting the pump body when the pump stops unexpectedly, causing the pump to reverse and be damaged.

[0026] Reference Figure 1 , Figure 2 A flow meter 141 is installed at one end of the first conveying pipe 14 near the circulating pump 12. The flow meter 141 can effectively reflect the flow rate of the first conveying pipe at this time, thereby controlling the liquid flow rate so that the material in the hydrolysis cooler 13 can move slowly and be fully cooled.

[0027] Reference Figure 1 , Figure 3 , Figure 4The separation unit 2 includes an oil-water separator 21 connected to the hydrolysis cooler 13 and a washing tank 22 connected to the oil-water separator 21. The top of the oil-water separator 21 is an oil outlet 211, and the bottom is a water outlet 212. The bottom of the washing tank 22 is a discharge outlet 221, and the discharge outlet 221 is fixedly connected to the post-processing pipe assembly 3. After the hydrolysis reaction, the material enters the oil-water separator 21 and is left to stand. At this time, the material will begin to separate into layers. The upper layer is an oil layer, mainly containing siloxanes, and the lower layer is a water layer, mainly containing hydrochloric acid. The hydrochloric acid can be output from the water outlet 212, and the siloxanes in the upper layer can enter the washing tank 22 from the oil outlet 211 for washing. After washing, the material is output from the discharge outlet 221 and stored.

[0028] In this embodiment, two washing tanks 22 are arranged in parallel; in other embodiments, the washing tanks 22 can also be arranged in series. In comparison, the parallel arrangement of the washing tanks 22 allows multiple washing tanks 22 to operate alternately during the hydrolysis process, so that the material can continuously enter the separation unit 2 without being accumulated or interrupted due to the intermittent nature of the washing process, thereby ensuring the continuous and stable operation of the entire system.

[0029] Reference Figure 3 , Figure 4 The outlet 212 is fixedly connected to an acid outlet pipe 23, which is equipped with a level controller 231. The oil-water separator 21 contains a level transmitter 213, which transmits signals to the level controller 231. Because an interface exists between the oil and water layers, the level transmitter 213 can identify the interface height and transmit the signal to the level controller 231. The level controller 231 controls the opening and closing of the acid outlet pipe 23 based on the signal, thereby controlling the water phase height within the oil-water separator 21. This prevents oil or acid spillage due to uncontrolled level fluctuations, ensuring production safety.

[0030] Reference Figure 3 The post-treatment pipe assembly 3 includes a strong acid recovery pipe 31, a weak acid recovery pipe 32, a wastewater treatment pipe 33, and a material recovery pipe 34, all of which are connected in parallel. Since the material in the washing tank 22 needs to be washed multiple times, the first discharged water, due to its high hydrochloric acid content, can be recovered through the strong acid recovery pipe 31 for use in preparing the byproduct hydrochloric acid. Subsequent discharged water, being weakly acidic, can be recycled for hydrolysis and washing processes. The water discharged from the final washing process directly enters the wastewater treatment pipe 33 for wastewater treatment, thereby improving resource utilization.

[0031] The implementation principle of the organosilicon continuous hydrolysis system in this application embodiment is as follows: chlorosilane and water enter the reaction pipeline 11 for hydrolysis, and are then cooled by the circulating pump 12 into the hydrolysis cooler 13 to generate siloxane and hydrochloric acid solution. The solution then enters the oil-water separator 21 for static stratification. The upper oil phase enters the water washing tank 22, and the lower water phase is discharged to the hydrochloric acid intermediate tank through the acid outlet pipe 23. After multiple water washings in the water washing tank 22, the water washing wastewater is recycled through different pipes according to different pH values. Finally, the product is output from the material recovery pipe 34 to the next process.

[0032] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A continuous organosilicon hydrolysis system, characterized in that, include: The hydrolysis unit (1) includes a reaction pipeline (11), a circulation pump (12), and a hydrolysis cooler (13). A first delivery pipeline (14) is connected between the circulation pump (12) and the reaction pipeline (11), and a second delivery pipeline (15) is connected between the circulation pump (12) and the hydrolysis cooler (13). The bottom of the hydrolysis cooler (13) is a liquid inlet (131), and the top of the hydrolysis cooler (13) is a liquid outlet (132). The second delivery pipeline (15) is connected to the liquid inlet (131). The separation unit (2) includes an oil-water separator (21) connected to the hydrolysis cooler (13) and a water washing tank (22) connected to the oil-water separator (21). The top of the oil-water separator (21) is an oil outlet (211) and the bottom is a water outlet (212). The bottom of the water washing tank (22) is a discharge outlet (221). The discharge outlet (221) is connected to a post-processing pipe assembly (3).

2. The organosilicon continuous hydrolysis system according to claim 1, characterized in that: A first check valve (111) is provided at one end of the reaction pipeline (11) near the first delivery pipeline (14).

3. The organosilicon continuous hydrolysis system according to claim 1, characterized in that: A second check valve (151) is provided at one end of the second delivery pipe (15) near the circulating pump (12).

4. The organosilicon continuous hydrolysis system according to claim 1, characterized in that: At least two of the washing tanks (22) are connected in parallel.

5. The organosilicon continuous hydrolysis system according to claim 1, characterized in that: The post-treatment pipe assembly (3) includes a strong acid recovery pipe (31), a weak acid recovery pipe (32), a wastewater treatment pipe (33), and a material recovery pipe (34).

6. The organosilicon continuous hydrolysis system according to claim 1, characterized in that: A flow meter (141) is installed at one end of the first delivery pipe (14) near the circulating pump (12).

7. The organosilicon continuous hydrolysis system according to claim 1, characterized in that: The outlet (212) is connected to an acid outlet pipe (23), and the acid outlet pipe (23) is equipped with a liquid level controller (231).

8. The organosilicon continuous hydrolysis system according to claim 7, characterized in that: The oil-water separator (21) is equipped with a level transmitter (213), which is used to transmit the level signal to the level controller (231).

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