An ultra-low volatile silicone oil atomization low-volatile removal device and low-volatile removal process

Abstract

The application discloses a kind of super-low volatile silicone oil atomization low device and low process.The preheater is connected to the low device side feed inlet after the preheater, the bottom of the low device is provided with discharge port, the discharge port is connected with heavy component tank, the bottom of the low device is provided with light component outlet, and the light component outlet is connected with light component tank.Low viscosity silicone oil after preheating is pressed into the low device, and fine mist droplets are formed by nozzle and fall down.In a vacuum environment, low molecular in mist droplets is easily volatile, and volatile low molecular is condensed into liquid immediately after encountering condenser tube after passing through the hole of flower plate and is collected in light component tank, and remaining non-condensable gas is cooled in cold trap after passing through gas phase outlet to reduce gas pressure to ensure vacuum degree.Mist droplets remaining in the low device are collected in heavy component tank at the bottom.By atomization technology, energy consumption problem in silicone oil low is reduced, volatile matter in silicone oil is ≤1.00% (200℃*4h), and super-low volatile silicone oil is prepared.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of low silicon oil removal, in particular to a kind of ultra-low volatile silicon oil atomization low removal device and low removal process. BACKGROUND

[0002] Silicone oil, usually by octamethylcyclotetrasiloxane (D4), hexamethylcyclotrisiloxane (D3) or cyclotetrasiloxane mixture (DMC) as main body, add end-capping agent (such as hexamethyldisiloxane, tetramethyldivinylsiloxane, etc.), under acid / base conditions, polymerization, removal low molecule and are prepared.

[0003] With the widening of application field and the upgrading of product, the market demand for the quality of silicone oil is higher and higher, and volatile fraction is the most basic and important quality index of silicone oil. The volatile fraction in silicone oil has a great influence on the products in the fields of aerospace, electronic glue, medical glue, etc. In the field of chip semiconductor, the customer's requirement for the volatile fraction of silicone oil is increased from 0.5% (200℃*4h) to 0.3% (200℃*4h). For the volatile fraction of silicone oil, the low removal process of silicone oil in the market is gradually changed from single-kettle high-temperature vacuum low removal to thin-film evaporator low removal. If further reduction of volatile fraction of silicone oil is required, short-path distillation device is used again. The low removal technology has a certain improvement on the volatile fraction of silicone oil, but the energy consumption and efficiency are relatively not ideal. At present, the organic silicon market is in a downturn, and it is urgent to reduce cost and increase efficiency for the industry, so the low removal technology of silicone oil needs to be improved. SUMMARY

[0004] To produce ultra-low volatile silicone oil, the present application provides a kind of ultra-low volatile silicone oil atomization low removal device and low removal process.

[0005] The low removal device includes a preheater, a low removal device, a heavy component tank, a light component tank, a cold trap and a vacuum system. The preheater is connected to the side feed inlet of the low removal device. The bottom of the low removal device is provided with a discharge port, which is connected to the heavy component tank. The bottom of the low removal device is provided with a light component outlet, which is connected to the light component tank.

[0006] Further, the feed inlet of the low removal device is connected to a distribution pipe, and a plurality of nozzles are arranged on the distribution pipe. The angle of the nozzles is 90°-120°.

[0007] Further, a condenser pipe is arranged in the low removal device. The condenser pipe has a cold water inlet and a cold water outlet. Each condenser pipe has a flower plate on both sides. The lowest point of the area between the flower plates is connected to the light component outlet.

[0008] Further, a gas phase outlet is arranged on the side of the low removal device. The gas phase outlet is connected to the cold trap. The discharge port at the bottom of the cold trap is connected to the light component tank. The gas phase outlet of the cold trap is connected to the vacuum system.

[0009] Further, the cold trap has a chilled water inlet and a chilled water outlet, and is connected to -15 to -5℃ chilled water.

[0010] In the technical solution of the present application, the preheater is connected to a side feed inlet of the low-removal device, the feed inlet is connected to a distribution pipe, the distribution pipe has a plurality of nozzles for spraying the silicone oil in mist form, the bottom of the spraying area is provided with a heavy component outlet, the heavy component outlet is connected to a heavy component tank, the low-removal device is provided with a condensing pipe, each condensing pipe is provided with a flower plate on both sides, the lowest point between the flower plates is connected to a light component outlet, the light component outlet is connected to a light component tank, the low-removal device is provided with a gas phase outlet connected to a cold trap, the bottom outlet of the cold trap is connected to the light component tank, and the gas phase outlet of the cold trap is connected to a vacuum system. The low-viscosity silicone oil after preheating is pressed into the low-removal device, and fine mist droplets are formed by the nozzles and fall down. In a vacuum environment, the low molecules in the mist droplets are easily volatilized, the volatilized low molecules are condensed into liquid after passing through the holes of the flower plate and then immediately meeting the condensing pipe, and the liquid is collected in the light component tank, and the remaining non-condensed gas passes through the gas phase outlet and is cooled in the cold trap to reduce the gas pressure, so as to ensure the vacuum degree. The mist droplets remaining in the low-removal device are collected at the bottom and then collected in the heavy component tank. Through the atomization technology, the energy consumption problem in the silicone oil low-removal process can be greatly reduced, and the quality of the silicone oil is further improved.

[0011] The present application also provides a low-removal process method for ultra-low volatile silicone oil by using the low-removal device.

[0012] (1) Silicone oil preheating: the low-viscosity silicone oil is preheated and then enters the distribution pipe.

[0013] (2) Low-removal: the low-viscosity silicone oil after preheating is sprayed from the nozzles in the distribution pipe to form mist oil droplets in the low-removal device, the gaseous low molecules in the oil droplets are volatilized under high temperature and high vacuum conditions, and the oil droplets flow into the heavy component tank from the bottom outlet of the low-removal device.

[0014] In the step (1), the temperature of the low-viscosity silicone oil after preheating is 130 to 220℃.

[0015] In the step (2), the nozzles are 2 to 10 groups, the particle size of the mist oil droplets realized by the nozzles is 2 to 10μm, and the flow rate of the mist oil droplets sprayed from the nozzles is 140 to 200kg / h.

[0016] In the step (2), the vacuum degree in the low-removal device is 10 to 50Pa, and the material temperature is 140 to 240℃.

[0017] In the low-removal process of the present application, the process of the low-molecule system also includes the following steps: the volatilized gaseous low molecules pass through the flower plate and then meet the condensing pipe to be condensed into liquid and then flow into the light component tank from the bottom of the low-removal device; the remaining high-temperature non-condensed gas passes through the gas phase pipe and then enters the cold trap to be cooled, so as to reduce the absolute pressure and ensure the high vacuum degree. The condensing pipe is connected to 10 to 20℃ circulating water, and the cold trap is connected to -15 to -5℃ chilled water.

[0018] The silicon oil will have small molecular weight siloxane ring body and short chain removed in the low removal process. The higher the molecular weight, the higher the boiling point, and the more difficult to remove. After the conventional low removal method, part of the small molecular weight siloxane ring body and short chain are removed, but the siloxane ring body and short chain that cannot be removed by the method are still present. These siloxane molecules have relatively slightly larger molecular weight and higher boiling point.

[0019] The present application disperses the silicon oil into oil droplets through the nozzle, increases the specific surface area of the silicon oil, and rapidly condenses the just removed gaseous low molecules into liquid state through the built-in condenser tube of the low removal equipment, and reduces the gas pressure to form high vacuum by reducing the temperature of the high-temperature non-condensable gas through the cold trap. The low removal equipment itself does not need to pass through the heat conducting oil and does not need the motor, thereby saving energy and reducing consumption. Finally, the volatile matter in the silicon oil is ≤2.00% (200℃*4h), preferably ≤1.0% (200℃*4h), and more preferably ≤0.10% (200℃*4h), thereby preparing the ultra-low volatile silicon oil. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 It is a schematic diagram of the device of the present application.

[0021] Figure 2 It is a structural schematic diagram of the low removal device.

[0022] Figure 3 It is a spraying structure schematic diagram.

[0023] In the figure: 1, preheater; 2, low removal device; 3, heavy component tank; 4, light component tank; 5, cold trap; 6, vacuum system; 7, distribution pipe; 8, nozzle; 9, condenser tube; 10, flower plate; N1, feed inlet; N2, discharge outlet; N3, light component outlet; N4, gas phase outlet; N5, cold trap discharge outlet; N6, cold trap gas phase outlet; N7, cold water inlet; N8, cold water outlet; N9, chilled water inlet; N10, chilled water outlet. DETAILED DESCRIPTION

[0024] The embodiments of the device of the present application will be further specifically described below by combining the embodiments with the drawings.

[0025] Example 1

[0026] An ultra-low volatile silicon oil atomization low removal device. The low removal device comprises a preheater 1, a low removal equipment 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 feed inlet N1 of the low removal equipment 2, the bottom of the low removal equipment 2 is provided with a discharge outlet N2, the discharge outlet N2 is connected to the heavy component tank 3, the bottom of the low removal equipment 2 is provided with a light component outlet N3, and the light component outlet N3 is connected to the light component tank 4.

[0027] The low-boiling point removal device 2 is connected with a distribution pipe 7, and the distribution pipe 7 is provided with six nozzles 8, and the angle of the nozzles is 90°.

[0028] The low-boiling point removal device 2 is provided with a condensing pipe 9, the condensing pipe has a cold water inlet N7 and a cold water outlet N8, and each condensing pipe 9 is provided with a flower plate 10 on both sides, and the lowest point of the area between the flower plates 10 is connected with a light component outlet N3.

[0029] The low-boiling point removal device 2 is provided with a gas phase outlet N4, the gas phase outlet N4 is connected with a cold trap 5, the bottom outlet N5 of the cold trap 5 is connected with a light component tank, and the gas phase outlet N6 of the cold trap 5 is connected with a vacuum system 6.

[0030] The cold trap has a refrigerated water inlet N9 and a refrigerated water outlet N10.

[0031] Example 2

[0032] An atomization low-boiling point removal process of ultra-low volatile silicone oil is carried out by using the device in Example 1, and the silicone oil with a volatile content of 1.36% is preheated to 160°C by the preheater 1 and then enters the low-boiling point removal device 2, is sprayed out from each nozzle 8 of the distribution pipe 7 at a flow rate of 160 kg / h to form 90° fan-shaped mist oil droplets with a particle size of 6 μm, and under the action of the vacuum system 6 with a system vacuum degree of 30 Pa, the light components in the oil mist volatilize and immediately pass through the flower plate 10 to meet the condensing pipe 9 to be condensed into liquid and flow into the light component tank 4 from the bottom, the temperature of the cold water in the condensing pipe is 10-20°C. The non-condensable gas volatilized is introduced into the cold trap 5 through the gas phase outlet N4, cooled and then introduced into the vacuum system 6, the temperature of the refrigerated water in the cold trap is-10--5°C. The heavy components in the oil mist which do not volatilize are collected in the heavy component tank 3 through the outlet N2.

[0033] The volatile content of the heavy components is detected as follows: after the silicone oil is kept at a constant temperature of 25±0.5°C for 2 h, 2±0.1 g of the sample is accurately weighed (accurate to 0.1 mg) and dropped into a dry dish, the dry dish is placed into a forced air drying oven, kept at 200±5°C and ventilated, taken out after 4 h, placed into a desiccator and cooled to room temperature, weighed, and the volatile content is calculated according to the weight difference.

[0034] Example 3

[0035] The operation steps are the same as those in Example 2a, and only the initial silicone oil in Example 2 is adjusted to 0.75%.

[0036] Example 4

[0037] The operation steps are the same as those in Example 2a, and only the initial silicone oil in Example 2 is adjusted to 1.85%.

[0038] Comparative Example 5

[0039] The procedure was the same as in Example 2a, except that the initial silicone oil in Example 2 was adjusted to 2.53%.

[0040] Comparative Example 6

[0041] The procedure was the same as in Example 2a, except that the initial silicone oil in Example 2 was adjusted to 3.02%.

[0042] The results of the silicone oil volatile portion test are shown in Table 1 for Examples 2 to 4 and Comparative Examples 5 and 6.

[0043] Table 1 Effect of initial silicone oil volatile portion on treated volatile portion

[0044]

[0045] Example 7

[0046] The procedure was the same as in Example 2, except that the particle size of the silicone oil sprayed from the nozzle in Example 2 was adjusted to 2 μm.

[0047] Example 8

[0048] The procedure was the same as in Example 2, except that the particle size of the silicone oil sprayed from the nozzle in Example 2 was adjusted to 10 μm.

[0049] Comparative Example 9

[0050] The procedure was the same as in Example 2, except that the particle size of the silicone oil sprayed from the nozzle in Example 2 was adjusted to 15 μm.

[0051] Comparative Example 10

[0052] The procedure was the same as in Example 2, except that the particle size of the silicone oil sprayed from the nozzle in Example 2 was adjusted to 25 μm.

[0053] The results of the silicone oil volatile portion test are shown in Table 2 for Examples 2, 7, 8 and Comparative Examples 9 and 10.

[0054] Table 2 Effect of particle size of silicone oil sprayed from nozzle on volatile portion

[0055]

[0056] Comparative Example 11

[0057] The procedure was the same as in Example 2, except that the misting angle of the silicone oil sprayed from the nozzle in Example 2 was adjusted to 30°.

[0058] Comparative Example 12

[0059] The procedure was the same as in Example 2, except that the misting angle of the silicone oil sprayed from the nozzle in Example 2 was adjusted to 60°.

[0060] Example 13

[0061] The operating procedure is the same as that of Example 2, except that the angle of the nozzle in Example 2 is adjusted to 120°.

[0062] The results of the detection of the volatile portion of the silicone oil in Examples 2, 13 and Comparative Examples 11 and 12 are shown in Table 3.

[0063] Table 3 Effect of the angle of the nozzle on the volatile portion

[0064]

[0065] Comparative Example 14

[0066] The operating procedure is the same as that of Example 2, except that the vacuum degree in Example 2 is adjusted to 10 Pa.

[0067] Comparative Example 15

[0068] The operating procedure is the same as that of Example 2, except that the vacuum degree in Example 2 is adjusted to 50 Pa.

[0069] Comparative Example 16

[0070] The operating procedure is the same as that of Example 2, except that the vacuum degree in Example 2 is adjusted to 70 Pa.

[0071] Comparative Example 17

[0072] The operating procedure is the same as that of Example 2, except that the vacuum degree in Example 2 is adjusted to 100 Pa.

[0073] The results of the detection of the volatile portion of the silicone oil in Examples 2, 14 and 15 and Comparative Examples 16 and 17 are shown in Table 4.

[0074] Table 4 Effect of the vacuum degree on the volatile portion

[0075]

[0076] Comparative Example 18

[0077] The operating procedure is the same as that of Example 2a, except that the temperature of the chilled water supplied to the cold trap in Example 2 is adjusted to -20 to -15°C.

[0078] Example 19

[0079] The operating procedure is the same as that of Example 2a, except that the temperature of the chilled water supplied to the cold trap in Example 2 is adjusted to -15 to -10°C.

[0080] Comparative Example 20

[0081] The operating procedure is the same as that of Example 2a, except that the temperature of the chilled water supplied to the cold trap in Example 2 is adjusted to -5 to 0°C.

[0082] Comparative Example 21

[0083] The operating procedure was the same as in Example 2a, except that the temperature of the chilled water supplied to the cold trap in Example 2 was adjusted to 0-10°C.

[0084] Comparative Example 22

[0085] The operating procedure was the same as in Example 2a, except that the temperature of the chilled water supplied to the cold trap in Example 2 was adjusted to 10-20°C.

[0086] The results of the detection of volatile components in the silicone oils in Examples 2, 19, and Comparative Examples 18, 20-22 are shown in Table 5.

[0087] Table 5 Effect of Chilled Water Temperature on Volatile Components

[0088]

[0089] The above description is merely preferred embodiments of the present application, and is not intended to limit the present application. Any modifications, equivalent replacements, improvements, and the like made within the spirit and principle of the present application are intended to be included in the scope of the present application.

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-sliming device (2). The de-sliming device (2) has an outlet (N2) at the bottom, which is connected to the heavy component tank (3). The de-sliming device (2) has a light component outlet (N3) at the bottom, which is connected to the light component tank (4). The de-sliming device (2) is equipped with condenser pipes (9), which have 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 perforated plate (10) is separated from the other side. The lowest point of the domain is connected to the light component outlet (N3). The side of the de-lowering device (2) is provided with a gas phase outlet (N4). The gas phase outlet (N4) is connected to the cold trap (5). The bottom outlet (N5) of the cold trap (5) is connected to the light component tank. The gas phase outlet (N6) of the cold trap (5) is connected to the vacuum system (6). The feed inlet (N1) of the de-lowering device (2) is connected to the distribution pipe (7). The distribution pipe (7) is provided with multiple nozzles (8). The nozzle angle is 90° to 120°. The particle size of the mist oil droplets achieved by the nozzle is 2 to 10 μm.

2. 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), through which chilled water at -15 to -5°C is introduced.

3. The ultra-low volatile silicone oil atomization de-atomization process performed by the apparatus according to any one of claims 1-2, characterized in that, Includes the following steps: (1) Silicone oil preheating: The low viscosity silicone oil is preheated before entering the distribution pipe; (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.

4. The ultra-low volatile silicone oil atomization de-lowering process according to claim 3, characterized in that, In step (1), the temperature of the low-viscosity silicone oil after preheating is 130-220℃.

5. The ultra-low volatile silicone oil atomization de-lowering process according to claim 3, characterized in that, In step (2), there are 2-10 sets of nozzles, and the flow rate sprayed from the nozzles is 140-200 kg / h.

6. The ultra-low volatile silicone oil atomization de-lowering process according to claim 3, characterized in that, In step (2), the vacuum degree inside the de-vacuuming equipment is 10-50 Pa; the material temperature is 140-240℃.

7. The ultra-low volatile silicone oil atomization de-lowering process according to claim 3, characterized in that, In step (2), the volatilized gaseous low molecules pass through the tube sheet and are condensed into liquid by the condenser tube, then flow into the light component tank from the bottom of the de-lowering equipment; the condenser tube is filled with circulating water at 10-20℃.

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