Ultralow volatile silicone oil atomization low-content removal device

Abstract

The utility model discloses an ultra-low volatile silicone oil atomization low-content removal device. The rear part of the preheater is connected with a feed port at the side part of the low-component removal equipment, the feed port is connected with a distribution pipe, a plurality of nozzles are arranged on the distribution pipe, silicone oil can be sprayed out in a mist form, a heavy component discharge port is arranged at the bottom of a mist spraying area and is connected with a heavy component tank, condensation pipes are arranged in the low-component removal equipment, pattern plates are arranged on two sides of each condensation pipe, and the pattern plates are connected with the nozzles. The lowest point of the area between the pattern plates is communicated with a light component discharging port, the light component discharging port is connected with a light component tank, a gas phase outlet is formed in the side portion of the low-component removal equipment and connected with a cold trap, a discharging port in the bottom of the cold trap is connected with the light component tank, and the gas phase outlet of the cold trap is connected into a vacuum system. By means of the atomization technology, the energy consumption problem in silicone oil removal can be greatly reduced, and the quality of silicone oil is further improved. Finally, the volatile matter in the silicone oil is less than or equal to 1.00% (200 DEG C * 4 hours), and preferably, the volatile matter is less than or equal to 0.10% (200 DEG C * 4 hours), so that the ultra-low volatile matter silicone oil is prepared.

Description

Technical Field

[0001] This utility model relates to the field of silicone oil descaling, specifically to an ultra-low volatile silicone oil atomization descaling device. Background Technology

[0002] Silicone oil is typically made by polymerizing and removing low-molecular-weight substances from octamethylcyclotetrasiloxane (D4), hexamethylcyclotrisiloxane (D3), or a mixture of cyclosiloxanes (DMC) as the main body, with the addition of end-capping agents (such as hexamethyldisiloxane, tetramethyldivinyldisiloxane, etc.) under acid / alkali conditions.

[0003] With the expansion of application areas and product upgrades, the market demand for high-quality silicone oils is increasing, and volatile matter is the most basic and important quality indicator for silicone oils. The volatile matter in silicone oils has a significant impact on products in aerospace, electronic adhesives, and medical adhesives. For example, in the semiconductor chip industry, customers have increased their requirements for silicone oil volatile matter from 0.5% (200℃*4h) to 0.3% (200℃*4h). Regarding the volatile matter in silicone oils, the current market trend for silicone oil removal processes has shifted from single-reactor high-temperature vacuum removal to thin-film evaporator removal. If further reduction of volatile matter is needed, a short-path distillation process is used again. This removal technology improves the volatile matter content of silicone oils to some extent, but its energy consumption and efficiency are relatively unsatisfactory. Given the current sluggish market for organosilicon products, there is an urgent need for cost reduction and efficiency improvement in the industry; therefore, silicone oil removal technology still needs further development. Summary of the Invention

[0004] To produce ultra-low volatile silicone oil, this utility model provides an ultra-low volatile silicone oil atomization and de-lowering device.

[0005] The de-lowering device includes a preheater, a de-lowering equipment, a heavy component tank, a light component tank, a cold trap, and a vacuum system. The preheater is connected to the side inlet of the de-lowering equipment, the bottom of the de-lowering equipment has an outlet connected to the heavy component tank, and the bottom of the de-lowering equipment has a light component outlet connected to the light component tank.

[0006] Furthermore, the feed inlet of the de-slimming device is connected to a distribution pipe, and the distribution pipe is equipped with multiple nozzles with nozzle angles of 90° to 120°.

[0007] Furthermore, the de-lowering device is equipped with condenser tubes, which have cold water inlets and outlets. Each condenser tube has a perforated plate on both sides, and the lowest point of the area between the perforated plates is connected to the outlet of the light component.

[0008] Furthermore, the side of the de-lowering device is equipped with a gas phase outlet, which is connected to a cold trap. The bottom outlet of the cold trap is connected to a light component tank, and the gas phase outlet of the cold trap is connected to a vacuum system.

[0009] Furthermore, the cold trap has a chilled water inlet and a chilled water outlet, through which chilled water at -15 to -5°C is introduced.

[0010] This invention also provides a method for atomizing and removing ultra-low volatile silicone oil using the above-mentioned removal device:

[0011] (1) Silicone oil preheating: The low viscosity silicone oil is preheated before entering the distribution pipe;

[0012] (2) De-lowering: After preheating, the low-viscosity silicone oil is sprayed out from the nozzle in the distribution pipe and forms mist-like oil droplets in the de-lowering equipment. Under high temperature and high vacuum conditions, the gaseous low molecules in the oil droplets evaporate and the oil droplets flow into the recombining tank from the bottom outlet of the de-lowering equipment.

[0013] In step (1), the temperature of the low-viscosity silicone oil after preheating is 130-220℃.

[0014] In step (2), there are 2-10 sets of nozzles, the particle size of the mist-like oil droplets produced by the nozzles is 2-10μm, and the flow rate sprayed from the nozzles is 140-200kg / h.

[0015] In step (2), the vacuum degree inside the de-vacuuming equipment is 10-50 Pa; the material temperature is 140-240℃.

[0016] The device of this invention also includes a low-molecular-weight system treatment process during the de-lowering process: the volatilized gaseous low molecules pass through the perforated plate, condense into liquid in the condenser tube, and then flow into the light component tank from the bottom of the de-lowering equipment; the remaining high-temperature non-condensable gas passes through the gas phase tube and enters the cold trap for cooling to reduce the absolute pressure and ensure a high vacuum. The condenser tube is circulated with 10-20°C circulating water, and the cold trap is circulated with -15 to -5°C chilled water.

[0017] During the descaling process of silicone oil, small molecular weight siloxane rings and short chains are released. The larger the molecular weight, the higher the boiling point, and the more difficult it is to remove. After conventional descaling methods remove some small molecular weight siloxane rings and short chains, some siloxane rings and short chains that cannot be removed by other methods remain. These siloxanes have relatively larger molecular weights and higher boiling points.

[0018] This invention disperses silicone oil into droplets through a nozzle, increasing the specific surface area of ​​the silicone oil. Secondly, the de-oxidation device uses a built-in condenser to rapidly condense the newly de-oxidized gaseous low-molecular-weight molecules into a liquid state, and uses a cold trap to cool the high-temperature non-condensable gas to reduce the gas pressure and form a high vacuum. Thirdly, the de-oxidation device itself does not require heat transfer oil or a motor, thus saving energy and reducing consumption. Ultimately, the volatile matter content in the silicone oil can be ≤1.00% (200℃*4h), and more preferably ≤0.10% (200℃*4h), resulting in ultra-low volatile silicone oil. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the device of this utility model.

[0020] In the diagram: 1. Preheater; 2. De-allocation device; 3. Heavy component tank; 4. Light component tank; 5. Cold trap; 6. Vacuum system; 7. Distribution pipe; 8. Nozzle; 9. Condenser; 10. Tube plate; N1. Inlet; N2. Outlet; N3. Light component outlet; N4. Gas phase outlet; N5. Cold trap outlet; N6. Cold trap gas phase outlet; N7. Cold water inlet; N8. Cold water outlet; N9. Chilled water inlet; N10. Chilled water outlet.

[0021] Figure 2 This is a left view of the device of this utility model.

[0022] Figure 3 Main view of the spray. Detailed Implementation

[0023] The embodiments of this utility model will be further described in detail below with reference to the accompanying drawings.

[0024] Example 1

[0025] An ultra-low volatile silicone oil atomization de-lowering device is disclosed. The de-lowering device includes a preheater 1, a de-lowering device 2, a heavy component tank 3, a light component tank 4, a cold trap 5, and a vacuum system 6. The preheater 1 is connected to the side inlet N1 of the de-lowering device 2. The bottom of the de-lowering device 2 is provided with an outlet N2, which is connected to the heavy component tank 3. The bottom of the de-lowering device 2 is provided with a light component outlet N3, which is connected to the light component tank 4.

[0026] The feed inlet N1 of the de-slimming device 2 is connected to the distribution pipe 7, which is equipped with 6 nozzles 8 with a nozzle angle of 90°.

[0027] The de-lowering device 2 is equipped with a condenser pipe 9, which has a cold water inlet N7 and a cold water outlet N8. Each condenser pipe 9 has a perforated plate 10 on both sides, and the lowest point of the area between the perforated plates 10 is connected to the light component outlet N3.

[0028] The aforementioned de-lowering device 2 is provided with a gas phase outlet N4 on its side, which is connected to a cold trap 5. The bottom outlet N5 of the cold trap 5 is connected to a light component tank, and the gas phase outlet N6 of the cold trap 5 is connected to a vacuum system 6.

[0029] The cold trap has a chilled water inlet N9 and a chilled water outlet N10.

[0030] Example 2

[0031] A process for removing ultra-low volatile silicone oil via atomization employs the apparatus of Example 1. Silicone oil with a volatile content of 1.36% is preheated to 160°C by preheater 1 and then enters the removal device 2. It is sprayed from nozzles 8 through distribution pipes 7 at a flow rate of 160 kg / h, forming 90° fan-shaped atomized oil droplets with a particle size of 6 μm. Under the action of vacuum system 6 (vacuum degree 30 Pa), the light components in the oil mist volatilize and immediately pass through the perforated plate 10, encountering condenser tubes 9 and condensing into liquid, flowing from the bottom into the light component tank 4. The temperature of the cold water in the condenser tubes is 10–20°C. The volatilized non-condensable gases reach the cold trap 5 through the gas phase outlet N4, are cooled, and then enter the vacuum system 6. The temperature of the chilled water in the cold trap is -10 to -5°C. The unvaporized heavy components in the oil mist are collected in the heavy component tank 3 through outlet N2.

[0032] Detection of volatile components: After the silicone oil is kept at a constant temperature of 25±0.5℃ for 2 hours, take 2±0.1g and drop it into a desiccator. Accurately weigh the sample (accurate to 0.1mg). Place the desiccator in a forced-air drying oven at 200±5℃ with ventilation. After 4 hours, take it out and place it in a desiccator to cool to room temperature. Weigh it and calculate the percentage content of volatile substances based on the weight difference.

[0033] Example 3

[0034] The operating steps are the same as in Example 2a, except that the initial silicone oil in Example 2 is adjusted to 0.75%.

[0035] Example 4

[0036] The operating steps are the same as in Example 2a, except that the initial silicone oil in Example 2 is adjusted to 1.85%.

[0037] Comparative Example 5

[0038] The operating steps are the same as in Example 2a, except that the initial silicone oil in Example 2 is adjusted to 2.53%.

[0039] Comparative Example 6

[0040] The operating steps are the same as in Example 2a, except that the initial silicone oil in Example 2 is adjusted to 3.02%.

[0041] The results of the detection of volatile silicone oil in Examples 2-4 and Comparative Examples 5 and 6 are shown in Table 1.

[0042] Table 1. Effect of initial volatile matter content of silicone oil on volatile matter content after treatment.

[0043] Examples or comparative examples 2 3 4 5 6 Initial volatile matter content of silicone oil (%) 1.36 0.75 1.85 2.53 3.02 Volatile matter (%) 0.07 0.06 0.09 0.13 0.21

[0044] The above description is merely a preferred embodiment of this utility model and is not intended to limit the utility model. Various modifications and variations can be made to this utility model by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. A device for atomizing and removing ultra-low volatile silicone oil, the device comprising a preheater (1), a removal device (2), a heavy component tank (3), a light component tank (4), a cold trap (5), and a vacuum system (6); characterized in that, The preheater (1) is connected to the side inlet (N1) of the de-sinking device (2). The bottom of the de-sinking device (2) is provided with an outlet (N2), which is connected to the heavy component tank (3). The bottom of the de-sinking device (2) is provided with a light component outlet (N3), which is connected to the light component tank (4). The inlet (N1) of the de-sinking device (2) is connected to the distribution pipe (7). The distribution pipe (7) is provided with multiple nozzles (8) with nozzle angles of 90° to 120°. The de-sinking device (2) is provided with a condenser (9), which has a cold water inlet (N7) and a cold water outlet (N8). Each condenser (9) has a perforated plate (10) on both sides, and the lowest point of the area between the perforated plates (10) is connected to the light component outlet (N3).

2. The ultra-low volatile silicone oil atomization and de-oxidation device according to claim 1, characterized in that, The side of the de-lowering device (2) is provided with a gas phase outlet (N4), which is connected to the cold trap (5).

3. The ultra-low volatile silicone oil atomization and de-oxidation device according to claim 2, characterized in that, The bottom outlet (N5) of the cold trap (5) is connected to the light component tank, and the gas phase outlet (N6) of the cold trap (5) is connected to the vacuum system (6).

4. The ultra-low volatile silicone oil atomization and de-oxidation device according to claim 1, characterized in that, The cold trap has a chilled water inlet (N9) and a chilled water outlet (N10).

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