Disc ceramic membrane emulsifying device

Abstract

The utility model discloses a disc ceramic membrane emulsifying device. The disc ceramic membrane emulsifying device comprises a vertical rotary disc ceramic membrane unit, a dispersed phase storage tank, a continuous phase storage tank, a gas driving unit and a control unit, the membrane surface shearing force is provided through rotation, the shearing force can be adjusted and relatively controllable through the rotating speed of the membrane, and the double-shaft staggered rotation can overcome the overlarge shearing force difference at different positions, so that a dispersed phase is separated from the surface of a membrane layer and is not easy to swallow on the surface of the membrane, and a more uniform emulsion particle size is formed; the membrane passing frequency of the dispersed phase is reduced, and generally, membrane passing is performed once.

Description

Technical Field

[0001] The utility model specifically relates to a disc ceramic membrane emulsification device. Background Art

[0002] Emulsion is a multiphase system, that is, at least one liquid is evenly dispersed in another immiscible liquid in the form of liquid droplets. Emulsions are mainly used in a large number of occasions such as pesticides, food, cosmetics, metal processing, fuel emulsification, medicine, emulsion polymerization and ultrafine powder preparation, and are widely used in many fields. Due to the requirements for the stability, particle size uniformity, controllability and repeatability of the emulsion, the preparation method of monodisperse emulsion with uniform particle size has always been a hot topic in this field. The traditional emulsion preparation method relies on the input of a large amount of energy, and the main equipment used is a mixer, a high-pressure homogenizer, a colloid mill, an ultrasonic emulsification and a homogenizing emulsification pump. The emulsion prepared in this way has poor stability, a wide and uneven particle size distribution, poor controllability and repeatability, high energy consumption and slow preparation speed.

[0003] At present, in order to meet the preparation of uniform and controllable emulsions and microcapsules and microspheres, membrane emulsification technology and microfluidic chip emulsification technology have gradually developed. Compared with membrane emulsification technology, the emulsion prepared by microfluidic technology is more uniform, but its efficiency is too low. The SPG membrane emulsification equipment technology (CN101912734B) developed by Professor Ma Guanghui's team can be used to quickly prepare nano-scale and tens of micron-scale emulsions. The prepared emulsion droplet particle size is uniform and the emulsion is stable. However, in the actual operation process, this technical solution uses a tubular SPG membrane or a conventional tubular ceramic membrane to prepare the emulsion, but both methods require the flow rate of the fluid to provide shear force on the membrane surface, or an external magnetic stirrer to disturb the membrane surface to provide shear force to produce a more uniform emulsion particle size. The manufacturing difficulty of SPG membrane is relatively high. The manufacturing difficulty is relatively high, and the production of uniform emulsion requires repeated membrane passing. The main reason is the shear force of the dispersed phase on the membrane. When the shear force is insufficient, it is easy for the dispersed phase to fail to leave the membrane surface in time, and the emulsion will appear on the membrane surface. The particle size becomes larger and the particle size is uneven. Because it needs to pass through the membrane multiple times, the complexity of the overall system and the difficulty of control will increase. Utility Model Content

[0004] The utility model aims to overcome the defects of the prior art and provide a disc ceramic membrane emulsification device.

[0005] The technical solution of the utility model is as follows:

[0006] A disc ceramic membrane emulsification device comprises a vertical rotating disc ceramic membrane unit, a dispersed phase storage tank, a continuous phase storage tank, a gas driving unit and a control unit.

[0007] The vertical rotating disc ceramic membrane unit comprises a membrane unit cavity, two rotating hollow shafts, a plurality of rotating disc ceramic membranes and a driving assembly; a continuous phase input port is arranged at the lower part of the membrane unit cavity, and a continuous phase reflux outlet is arranged at the upper part; the two rotating hollow shafts are vertically arranged in the membrane unit cavity, a plurality of rotating disc ceramic membranes are arranged in parallel with the sealing sleeve at the lower part of each rotating hollow shaft, the membrane unit cavity of the rotating hollow shaft is connected with the internal flow channel of the plurality of rotating disc ceramic membranes, the rotating disc ceramic membranes on the adjacent two rotating hollow shafts are staggered and parallel to each other, and the upper part of each rotating hollow shaft is connected with the mechanical seal and the shaft through ... A first stainless steel circular plate is sleeved on the rotating hollow shaft adjacent to the rotating disc ceramic membrane located at the uppermost end of the cavity of the membrane unit, and the first stainless steel circular plate is staggered parallel to and located above the rotating disc ceramic membrane located at the uppermost end, and a second stainless steel circular plate is sleeved on the rotating hollow shaft adjacent to the rotating disc ceramic membrane located at the lowermost end, and the second stainless steel circular plate is staggered parallel to and located below the rotating disc ceramic membrane located at the lowermost end; a driving component drives the upper parts of the two rotating hollow shafts to connect and make the two rotating hollow shafts rotate in the same direction;

[0008] The continuous phase storage tank has a heat preservation jacket connected to the thermostatic tank on its peripheral wall, a continuous phase discharge port on its lower part, and a continuous phase reflux inlet on its upper part.

[0009] The dispersed phase storage tank has a dispersed phase discharge port at the bottom and a driving gas input port at the top.

[0010] The gas drive unit includes a high-pressure gas storage tank containing high-pressure gas.

[0011] The continuous phase discharge port of the continuous phase storage tank is connected to the continuous phase input port of the membrane unit cavity through a first automatic valve and a feed pump in sequence, the continuous phase reflux outlet of the membrane unit cavity is connected to the continuous phase reflux inlet of the continuous phase storage tank through a second automatic valve, the dispersed phase discharge port of the dispersed phase storage tank is connected to the membrane unit cavity of the two rotating hollow shafts of the vertical rotating disc ceramic membrane unit, the high-pressure gas storage tank of the gas drive unit is connected to the driving gas input port of the dispersed phase storage tank through a third automatic valve and a gas filter in sequence, and the control unit is electrically connected to the above-mentioned first to third automatic valves, drive components and feed pump control.

[0012] In a preferred embodiment of the present utility model, the driving assembly includes a driving motor and a transmission mechanism arranged on the upper part of the two rotating hollow shafts connected in sequence, and the control unit is electrically connected to the driving motor control.

[0013] In a preferred embodiment of the present invention, the continuous phase storage tank is connected to subsequent discharge via a fourth automatic valve electrically connected to the control unit.

[0014] In a preferred embodiment of the present invention, the continuous phase input port of the membrane unit cavity is connected to the subsequent discharge through a fifth automatic valve electrically connected to the control unit.

[0015] In a preferred embodiment of the present invention, the dispersed phase discharge port of the dispersed phase storage tank is connected to subsequent discharge via a sixth automatic valve electrically connected to the control unit.

[0016] Further preferably, the gas filter is connected to the driving gas input port of the dispersed phase storage tank through a one-way valve.

[0017] More preferably, the driving gas input port is connected to a muffler via a seventh automatic valve electrically connected to the control unit.

[0018] In a preferred embodiment of the present invention, the lower portion of the membrane unit cavity is conical to facilitate the discharge of the material therein.

[0019] The beneficial effects of the utility model are:

[0020] 1. The utility model provides shear force on the membrane surface by rotation. The magnitude of the shear force can be adjusted by the rotation speed of the membrane, which is relatively controllable. The staggered rotation of the two axes can overcome the large difference in shear force at different positions, thereby achieving the separation of the dispersed phase from the membrane surface, and it is not easy to swallow each other on the membrane surface, thereby forming a more uniform emulsion particle size, reducing the number of times the dispersed phase passes through the membrane, and usually passing through the membrane once.

[0021] 2. The utility model is easy to clean and is beneficial for subsequent use. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a schematic structural diagram of the disc ceramic membrane emulsification device of Example 1 of the utility model. DETAILED DESCRIPTION

[0023] The technical solution of the present utility model is further illustrated and described below through specific implementation modes in combination with the accompanying drawings.

[0024] Example 1

[0025] like Figure 1 As shown, a disc ceramic membrane emulsification device includes a vertical rotating disc ceramic membrane unit 1, a dispersed phase storage tank 2, a continuous phase storage tank 3, a gas driving unit 4 and a control unit (not shown in the figure).

[0026] The vertical rotating disc ceramic membrane unit 1 comprises a membrane unit chamber 10 , two rotating hollow shafts 11 , a plurality of rotating disc ceramic membranes 12 and a driving assembly 13 .

[0027] The lower part of the membrane unit cavity 10 is provided with a continuous phase input port 101, and the upper part is provided with a continuous phase reflux outlet 102. Preferably, the lower part of the membrane unit cavity 10 is conical, which is convenient for discharging the material therein.

[0028] Two rotating hollow shafts 11 are vertically arranged in the membrane unit cavity 10, and a plurality of rotating disc ceramic membranes 12 are sealed and sleeved in parallel at the lower part of each rotating hollow shaft 11. The membrane unit cavity 10 of the rotating hollow shaft 11 is connected with the internal flow channels of the plurality of rotating disc ceramic membranes 12, and the rotating disc ceramic membranes 12 on the two adjacent rotating hollow shafts 11 are staggered and parallel to each other so that the centers of different rotating disc ceramic membranes 12 reach the same shear linear velocity.

[0029] The rotating disc ceramic membranes 12 are a kind of high-strength, uniform-pore-size internal multi-channel disc-type alumina ceramic membranes (see CN114249582B). The membrane pore size can be 0.05-20μm, the membrane pressure resistance is >60bar, and the operating pressure of membrane emulsification is 0-50bar. Emulsions of various particle sizes can be prepared by using different pore sizes. The smaller the pore size, the greater the operating force.

[0030] The upper part of each rotating hollow shaft 11 passes through the upper end of the membrane unit cavity 10 through a mechanical seal 110 and a bearing 114. A first stainless steel circular plate 111 is sleeved on the rotating hollow shaft 11 adjacent to the rotating disc ceramic membrane 12 located at the uppermost end. The first stainless steel circular plate 111 is staggered and parallel to and located above the rotating disc ceramic membrane 12 located at the uppermost end. A second stainless steel circular plate 112 is sleeved on the rotating hollow shaft 11 adjacent to the rotating disc ceramic membrane 12 located at the lowermost end. The second stainless steel circular plate 112 is staggered and parallel to and located below the rotating disc ceramic membrane 12 located at the lowermost end. The first stainless steel circular plate 111 and the second stainless steel circular plate 112 can enable the rotating disc ceramic membranes 12 at the lowermost and uppermost ends to reach the same biaxial shear linear velocity, and can cope with the fluid impact of the continuous phase inlet 101 and the continuous phase reflux outlet 102 of the membrane unit cavity 10.

[0031] The driving assembly 13 drives the upper parts of the two rotating hollow shafts 11 and makes the two rotating hollow shafts 11 rotate in the same direction. The driving assembly 13 includes a driving motor 130 and a transmission mechanism 131 arranged on the upper parts of the two rotating hollow shafts 11, which are connected in sequence to drive the two rotating hollow shafts 11 to rotate at a speed of 300-1000RPM.

[0032] The continuous phase storage tank 3 has a peripheral wall provided with an insulating jacket 32 ​​connected to a constant temperature tank (in some applications, the emulsion may undergo polymerization reaction, so the temperature needs to be controlled to control the polymerization reaction), a continuous phase discharge port 30 is provided at the lower part, a continuous phase reflux inlet 31 is provided at the upper part, and a first liquid level sensor 33 and a viscosity sensor 34 are also provided.

[0033] The dispersed phase storage tank 2 is provided with a dispersed phase discharge port 20 at the bottom, a driving gas input port 21 at the top, and a second liquid level sensor 23. The dispersed phase storage tank 2 is generally not provided with an insulation jacket because the gas is used as the driving force, and the dispersed phase will not be heated up. However, if the ambient temperature is too high, it is preferred to configure the above insulation jacket to control the dispersed phase temperature like the continuous phase storage tank 3, because the temperature will affect the dispersed phase viscosity and accelerate the polymerization reaction. The volume of the dispersed phase storage tank 2 matches the amount of the dispersed phase liquid, and 10% of the space is reserved to prevent the volume from being too large and causing gas waste. At the same time, the top of the dispersed phase storage tank 2 can be fully opened to add the dispersed phase, and the bottom is arc-shaped, which is convenient for discharge and does not cause the liquid to be retained therein, and the dispersed phase storage tank 2 can withstand a pressure of more than 70 bar.

[0034] The gas drive unit 4 includes a high-pressure gas storage tank 40 containing high-pressure gas, which is preferably nitrogen, argon or helium.

[0035] The continuous phase outlet 30 of the continuous phase storage tank 3 is connected to the continuous phase input port 101 of the membrane unit cavity 10 through a first automatic valve 51 and a feed pump 6 in sequence, and is connected to the subsequent discharge through a fourth automatic valve 54; a first pressure gauge 1011 and a first pressure sensor 1012 are provided on the pipeline between the feed pump 6 and the continuous phase input port 101. Preferably, the feed pump 6 is a low shear force pump to prevent shearing of the emulsion, and can adapt to viscosity changes of 1-2000cP.

[0036] The continuous phase reflux outlet 102 of the membrane unit cavity 10 is connected to the continuous phase reflux inlet 31 of the continuous phase storage tank 3 through a second automatic valve 52, and the continuous phase input port 101 is connected to the subsequent discharge through a fifth automatic valve 55; a second flow meter 1021, a second pressure sensor 1022 and a second pressure gauge 1023 are provided on the pipeline between the continuous phase reflux outlet 102 and the second automatic valve 52.

[0037] The dispersed phase discharge port 20 of the dispersed phase storage tank 2 is connected to the membrane unit cavity 10 of the two rotating hollow shafts 11 of the vertical rotating disc ceramic membrane 12 unit 1, and is connected to subsequent discharge through a sixth automatic valve 56; a first flow meter 201, a third pressure sensor 203 and a third pressure gauge 204 are provided on the pipeline between the dispersed phase discharge port 20 and the two rotating hollow shafts 11.

[0038] The high-pressure gas storage tank 40 of the gas drive unit 4 is connected to the driving gas input port 21 of the dispersed phase storage tank 2 through a third automatic valve 53, a gas filter 41 and a one-way valve 42 in sequence, and the driving gas input port 21 is connected to a muffler 22 through a seventh automatic valve 57.

[0039] The control unit is electrically connected to the first to seventh automatic valves 57 , the drive motor 130 of the drive assembly 13 and the feed pump 6 .

[0040] The working status of the disc ceramic membrane emulsification device is as follows:

[0041] (1) Membrane emulsification: The continuous phase in the continuous phase storage tank 3 is transported to the membrane unit cavity 10 via the feed pump 6, and then flows back to the continuous phase storage tank 3; the plurality of rotating disc ceramic membranes 12 rotate in the membrane unit cavity 10; the dispersed phase in the dispersed phase storage tank 2 is driven by the high-pressure gas output by the gas drive unit 4, and is dispersed to the continuous phase in the membrane unit cavity 10 through the two rotating hollow shafts 11, the internal flow channels of the plurality of rotating disc ceramic membranes 12, and the membrane surfaces of the plurality of rotating disc ceramic membranes 12, and is emulsified to form an emulsion; the emulsion flows back to the continuous phase storage tank 3 driven by the feed pump, and is mixed with the continuous phase therein. During the whole process, the control unit ensures that the second automatic valve 52 is fully opened, and the second pressure gauge 1023 and the second pressure sensor 1022 are kept at 0. During the membrane emulsification process, the viscosity of the continuous phase in the continuous phase storage tank 3 may increase significantly. During the membrane emulsification process, the liquid level of the dispersed phase storage tank 2 is monitored. When the liquid level reaches the predetermined target, the third automatic valve 53 is closed and the seventh automatic valve 57 is opened to discharge the gas in the dispersed phase storage tank 2. If high-pressure gas enters the vertical rotating disc ceramic membrane 12 unit 1, a large number of bubbles are easily generated because the continuous phase contains a surfactant.

[0042] (2) Discharge of sewage: After the membrane emulsification is completed, the two rotating hollow shafts 11 are stopped, and the fourth automatic valve 54 and the fifth automatic valve 55 are opened by the control unit to collect the continuous phase in the continuous phase storage tank 3, the vertical rotating disc ceramic membrane 12 unit 1 and the pipeline between them, and the sixth automatic valve is opened to collect the dispersed phase remaining in the dispersed phase storage tank 2 and the connected pipeline.

[0043] (3) Cleaning: controlled by the control unit,

[0044] A. Discharging: Open the high-pressure gas storage tank 40 to squeeze out the dispersed phase remaining inside the two rotating hollow shafts 11 and discharge it from the cavity. During this process, the two rotating hollow shafts 11 do not rotate.

[0045] B. Filtration and cleaning: Use pure water or a prepared cleaning agent in the continuous phase storage tank 3, transport it through the feed pump 6, circulate it in the membrane unit cavity 10, and return it to the continuous phase storage tank 3. Adjust the second automatic valve 52 to control the internal pressure of the membrane unit cavity 10, adjust the pressure to 3-5 bar, or even higher pressure, and use filtering to squeeze out the remaining dispersed phase of the two rotating hollow shafts 11 and discharge it through the sixth automatic valve. The selected agent can be a surfactant of a certain concentration or an organic solvent that can dissolve the polymer of emulsion polymerization.

[0046] C. Backwashing: Similar to the above-mentioned membrane emulsification process, pure water or prepared cleaning agent is used in the continuous phase storage tank 3 and the dispersed phase storage tank 2, which is transported to the membrane unit cavity 10 via the feed pump 6 and then refluxed to the continuous phase storage tank 3; the plurality of rotating disc ceramic membranes 12 rotate in the membrane unit cavity 10; the pure water or cleaning agent in the dispersed phase storage tank 2 is driven by the high-pressure gas output by the gas drive unit 4 and is dispersed into the membrane unit cavity 10 in turn through the two rotating hollow shafts 11, the internal flow channels of the plurality of rotating disc ceramic membranes 12 and the membrane surfaces of the plurality of rotating disc ceramic membranes 12. In this process, pay attention to the liquid level in the continuous phase storage tank 3. As the cleaning proceeds, the liquid level in the continuous phase storage tank 3 will continue to rise, and it is discharged or shut down in time to prevent overflow;

[0047] D. Prepare cleaning agents in the continuous phase storage tank and the dispersed phase storage tank. The selected agent can be a surfactant of a certain concentration or an organic solvent that can dissolve the polymer of emulsion polymerization. Chemical cleaning is carried out through the above-mentioned membrane emulsification method, and the cleaning agent is discharged. The gas driving pressure can be adjusted according to the cleaning flow rate during the cleaning process.

[0048] Repeat steps B and C for several times, and clean with pure water or detergent. The flux can be basically fully restored, preparing for the next membrane emulsification.

[0049] The above is only a preferred embodiment of the present invention, and therefore cannot be used to limit the scope of implementation of the present invention. That is, equivalent changes and modifications made according to the patent scope of the present invention and the content of the specification should still fall within the scope covered by the present invention.

Claims

1. A disc ceramic membrane emulsification device, characterized in that: The invention comprises a vertical rotating disc ceramic membrane unit, a dispersed phase storage tank, a continuous phase storage tank, a gas driving unit and a control unit. The vertical rotating disc ceramic membrane unit comprises a membrane unit cavity, two rotating hollow shafts, a plurality of rotating disc ceramic membranes and a driving assembly; a continuous phase input port is arranged at the lower part of the membrane unit cavity, and a continuous phase reflux outlet is arranged at the upper part; the two rotating hollow shafts are vertically arranged in the membrane unit cavity, a plurality of rotating disc ceramic membranes are arranged in parallel with the sealing sleeve at the lower part of each rotating hollow shaft, the membrane unit cavity of the rotating hollow shaft is connected with the internal flow channel of the plurality of rotating disc ceramic membranes, the rotating disc ceramic membranes on the adjacent two rotating hollow shafts are staggered and parallel to each other, and the upper part of each rotating hollow shaft is connected with the mechanical seal and the shaft through ... A first stainless steel circular plate is sleeved on the rotating hollow shaft adjacent to the rotating disc ceramic membrane located at the uppermost end of the cavity of the membrane unit, and the first stainless steel circular plate is staggered parallel to and located above the rotating disc ceramic membrane located at the uppermost end, and a second stainless steel circular plate is sleeved on the rotating hollow shaft adjacent to the rotating disc ceramic membrane located at the lowermost end, and the second stainless steel circular plate is staggered parallel to and located below the rotating disc ceramic membrane located at the lowermost end; a driving component drives the upper parts of the two rotating hollow shafts to connect and make the two rotating hollow shafts rotate in the same direction; The continuous phase storage tank has a heat preservation jacket connected to the thermostatic tank on its peripheral wall, a continuous phase discharge port on its lower part, and a continuous phase reflux inlet on its upper part. The dispersed phase storage tank has a dispersed phase discharge port at the bottom and a driving gas input port at the top. The gas drive unit includes a high-pressure gas storage tank containing high-pressure gas. The continuous phase discharge port of the continuous phase storage tank is connected to the continuous phase input port of the membrane unit cavity through a first automatic valve and a feed pump in sequence, the continuous phase reflux outlet of the membrane unit cavity is connected to the continuous phase reflux inlet of the continuous phase storage tank through a second automatic valve, the dispersed phase discharge port of the dispersed phase storage tank is connected to the membrane unit cavity of the two rotating hollow shafts of the vertical rotating disc ceramic membrane unit, the high-pressure gas storage tank of the gas drive unit is connected to the driving gas input port of the dispersed phase storage tank through a third automatic valve and a gas filter in sequence, and the control unit is electrically connected to the above-mentioned first to third automatic valves, drive components and feed pump control.

2. A disc ceramic membrane emulsification device as claimed in claim 1, characterized in that: The driving assembly includes a driving motor and a transmission mechanism arranged on the upper part of the two rotating hollow shafts which are connected in sequence, and the control unit is electrically connected to the driving motor.

3. A disc ceramic membrane emulsification device as claimed in claim 1, characterized in that: The continuous phase storage tank is connected to subsequent discharge via a fourth automatic valve electrically connected to the control unit.

4. A disc ceramic membrane emulsification device as claimed in claim 1, characterized in that: The continuous phase input port of the membrane unit cavity is connected to subsequent discharge through a fifth automatic valve electrically connected to the control unit.

5. The disc ceramic membrane emulsification device according to claim 1, characterized in that: The dispersed phase discharge port of the dispersed phase storage tank is connected to subsequent discharge via a sixth automatic valve electrically connected to the control unit.

6. A disc ceramic membrane emulsification device as claimed in claim 5, characterized in that: The gas filter is connected to the driving gas input port of the dispersed phase storage tank through a one-way valve.

7. A disc ceramic membrane emulsification device as claimed in claim 6, characterized in that: The driving gas input port is connected to a muffler through a seventh automatic valve electrically connected to the control unit.

8. The disc ceramic membrane emulsification device according to claim 1, characterized in that: The lower part of the membrane unit cavity is conical, which is convenient for discharging the materials therein.

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