CN105032312B - A kind of quick equipment and its application for continuously preparing drop microballoon - Google Patents

Abstract

The invention relates to a device for rapidly and continuously preparing liquid droplet microspheres and its application. The device includes a dispersed phase feeding device, a continuous phase feeding device, a continuous phase pressure tank and a rotating stirring device. The continuous phase pressure tank The top is connected with the continuous phase feeding device, the bottom of the continuous phase pressure tank is provided with a discharge port, and the side wall of the continuous phase pressure tank is provided with a discharge port, a dispersed phase inlet hole and an air distribution port from top to bottom. The dispersed phase feeding device communicates with the dispersed phase inlet hole, and the rotating stirring device is arranged in the continuous phase pressure tank. The present invention realizes rapid and continuous feeding by continuously conveying the continuous phase and the dispersed phase into the continuous phase pressure tank, and supplemented by rotating paddles to improve work efficiency, and the liquid droplets are brought into the discharge device through the air inlet of the air chamber, Finally, efficient, rapid and continuous preparation of droplet microspheres is realized.

Description

A device for rapid and continuous preparation of droplet microspheres and its application

technical field

The invention relates to a device for rapidly and continuously preparing droplet microspheres and an application thereof, belonging to the technical field of droplet microsphere preparation.

Background technique

Micro-droplets have many excellent properties, such as small size, no diffusion between droplets, avoidance of cross-contamination between droplets, stable reaction conditions, and controllable mixing, etc., and are more and more widely used. The droplet size uniformity (monodispersity) obtained by traditional mechanical stirring, colloid mill and other methods is poor; microfluidic technology based on hydrodynamics is currently the main method for manufacturing monodisperse microdroplets, but its rate is in the ml/ h level, although the growth rate of micro-droplets can be increased by integrating micro-channels, it is still difficult to reach the level of l/h, and the interaction between multiple channels is relatively large, which reduces the controllability and production continuity of the system. Can not meet the output of industrial production needs.

Contents of the invention

Aiming at the deficiencies of the prior art, the present invention provides a device for rapid and continuous preparation of liquid droplet microspheres, so as to realize a rapid, efficient, highly automated, and continuous production capacity of micro-droplet production equipment.

Technical scheme of the present invention is as follows:

A device for rapidly and continuously preparing droplet microspheres, said device comprising a dispersed phase feed device, a continuous phase feed device, a continuous phase pressure tank and a rotating agitation device, the top of the continuous phase pressure tank is connected to the continuous phase feed The device is connected, the bottom of the continuous phase pressure tank is provided with a discharge port, and the side wall of the continuous phase pressure tank is provided with a discharge port, a dispersed phase inlet hole and an air distribution hole from top to bottom, and the dispersed phase The feeding device communicates with the inlet hole of the dispersed phase, and the rotating stirring device is arranged through the pressure tank of the continuous phase.

Preferably, the dispersed phase feeding device comprises a dispersed phase normal pressure storage tank, a dispersed phase buffer storage tank and a dispersed phase high pressure storage tank connected from top to bottom, and the dispersed phase normal pressure storage tank and dispersed phase Two-valve communication is adopted between the phase buffer storage tanks, the dispersed phase buffer storage tank and the dispersed phase high-pressure storage tank.

Preferably, the continuous phase feeding device comprises a continuous phase normal pressure storage tank, a continuous phase buffer storage tank and a continuous phase high pressure storage tank connected from top to bottom, the continuous phase normal pressure storage tank and the continuous phase Two-valve communication is adopted between the phase buffer storage tanks, the continuous phase buffer storage tank and the continuous phase high-pressure storage tank.

Preferably, a dispersed phase pressure chamber and an air chamber are set on the outside of the continuous phase pressure tank, and the dispersed phase pressure chamber and the air chamber are independent of each other; the dispersed phase inlet hole is located in the dispersed phase pressure chamber, and the air distribution hole is located in the dispersed phase pressure chamber. In the air chamber, the dispersed phase pressure chamber communicates with the dispersed phase high-pressure storage tank through double valves.

Preferably, the continuous phase pressure tank includes an upper part of a cylindrical tank body and a lower part of a frustoconical tank body, the dispersed phase inlet hole is located on the side wall of the cylindrical tank body, and the air distribution hole is located on the frustoconical tank body. on the side wall of the tank.

Preferably, the device further includes a discharge tank and a discharge device, the discharge tank communicates with the discharge port through double valves, and the discharge device communicates with the discharge port through double valves.

Preferably, the rotating stirring device includes a motor, a stirring shaft and a rotating paddle, the stirring shaft is arranged through the continuous phase pressure tank, the upper end of the stirring shaft is connected to the motor, and the rotating paddle is arranged in the continuous phase pressure tank. on the stirring shaft in the pressure tank.

Preferably, the side wall of the continuous phase pressure tank is provided with a plurality of dispersed phase inlet holes, and the plurality of dispersed phase inlet holes are located on the same horizontal circumference.

Further preferably, the dispersed phase inlet hole is arranged obliquely, and the angle between the dispersed phase inlet hole and the vertical plane is greater than or equal to 0°.

Preferably, the diameter of the dispersed phase inlet hole is less than 2 mm, and the distance between the adjacent dispersed phase inlet holes is greater than or equal to twice the diameter of the dispersed phase inlet hole. The benefit of this design is that droplets smaller than 2mm in size can be produced with this device.

Preferably, a plurality of air distribution holes are provided on the side wall of the continuous phase pressure tank, and the plurality of air distribution holes are located on the same horizontal circumference.

Further preferably, the air distribution holes are arranged obliquely, and the angle between the air distribution holes and the horizontal plane is greater than or equal to 10°.

Preferably, the diameter of the air distribution holes is less than 5 mm, and the distance between adjacent air distribution holes is greater than or equal to twice the diameter of the air distribution holes.

Preferably, the wind speed of the air distribution holes is greater than 0.1m/s.

A method for using a device for rapidly and continuously preparing droplet microspheres, comprising the following steps,

The continuous phase and the dispersed phase are respectively added to the continuous phase normal pressure storage tank and the dispersed phase normal pressure storage tank, and the continuous phase passes through the continuous phase normal pressure storage tank, the continuous phase buffer storage tank and the continuous phase high pressure storage tank After entering the continuous phase pressure tank, at the same time, the dispersed phase enters the dispersed phase pressure chamber after passing through the dispersed phase normal pressure storage tank, the dispersed phase buffer storage tank and the dispersed phase high pressure storage tank, and enters the dispersed phase through the dispersed phase. The holes are injected into the continuous phase pressure tank;

In the continuous phase pressure tank, the continuous phase pressure tank is ventilated through the air distribution holes, the motor is started, the rotating paddles rotate to drive the continuous phase to generate a tangential velocity, and the continuous phase shears the dispersed phase to make the dispersed phase form droplets, and the liquid The drops move upwards under the action of their own buoyancy and the wind, and enter the discharge device through the discharge port.

The beneficial effects of the present invention are:

1. The present invention realizes the pressurized continuous feeding of the dispersed phase by setting the dispersed phase normal pressure storage tank, the dispersed phase buffer storage tank and the dispersed phase high pressure storage tank, and by setting the continuous phase normal pressure storage tank, the continuous phase The buffer storage tank and the continuous phase high-pressure storage tank realize the continuous feeding of the continuous phase under pressure, and finally realize the continuous supply of raw materials, ensure the continuous preparation of droplet microspheres, and realize continuous production.

2. The present invention arranges the rotating paddles in the continuous phase pressure tank, so that the rotating paddles drive the continuous phase to rotate, generate sufficient axial shear force, and shear the dispersed phase that enters the continuous phase pressure tank through the dispersed phase inlet hole The formation of droplets increases the speed of preparing droplet microspheres, and at the same time, the device of the invention can be used to produce microdroplets with particle diameters less than 2mm.

3. The present invention supplies air through the air chamber, which helps the droplet microspheres to quickly enter the discharge device, promotes the production speed of the droplet microspheres, and realizes the rapid and efficient production of the equipment.

Description of drawings

Fig. 1 is the schematic structural view of the device for rapidly and continuously preparing droplet microspheres of the present invention;

Fig. 2 is the sectional view of part A-A in Fig. 1;

Fig. 3 is the enlarged view of dispersed phase inlet hole in Fig. 2;

Fig. 4 is an enlarged view of the air distribution hole in Fig. 1;

Among them: 1. Dispersed phase feeding device; 2. Dispersed phase normal pressure storage tank; 3. Double valves; 4. Dispersed phase buffer storage tank; 5. Double valves; 6. Dispersed phase high pressure storage tank; 7. Double valve; 8. Double valve; 9. Dispersed phase inlet hole; 10. Air distribution hole; 11. Double valve; 12. Unloading tank; 13. Double valve; 14. Air chamber; 15. Rotating paddle; 16. Dispersed phase pressure chamber; 17. Discharge device; 18. Double valves; 19. Continuous phase pressure tank; 20. Motor; 21. Continuous phase high-pressure storage tank; 22. Double valves; 23. Continuous phase buffer storage tank; 24. Double valves; 25. Continuous phase atmospheric pressure storage tank; 26. Continuous phase feeding device.

detailed description

The present invention will be further described below through the embodiments and in conjunction with the accompanying drawings, but not limited thereto.

Example 1:

The present embodiment provides a kind of equipment for rapidly and continuously preparing droplet microspheres, as shown in Figure 1, this equipment comprises dispersed phase feeding device 1, continuous phase feeding device 26, continuous phase pressure tank 19 and rotating agitation device, continuous The top of the phase pressure tank 19 communicates with the continuous phase feeding device 26, the bottom of the continuous phase pressure tank 19 is provided with a discharge port, and the side wall of the continuous phase pressure tank 19 is provided with a discharge port from top to bottom, The dispersed phase inlet hole 9 and the air distribution hole 10 , the dispersed phase feeding device 1 communicates with the dispersed phase inlet hole 9 , and the rotating stirring device is arranged in the continuous phase pressure tank 19 .

Wherein, the dispersed phase feeding device 1 comprises a dispersed phase normal pressure storage tank 2 connected from top to bottom, a dispersed phase buffer storage tank 4 and a dispersed phase high pressure storage tank 6, a dispersed phase normal pressure storage tank 2 and a dispersed phase Two valves 3 and 5 are used to communicate between the phase buffer storage tanks 4 and between the dispersed phase buffer storage tank 4 and the dispersed phase high-pressure storage tank 6 .

The continuous phase feeding device 26 comprises the continuous phase normal pressure storage tank 25, the continuous phase buffer storage tank 23 and the continuous phase high pressure storage tank 21 connected from top to bottom, the continuous phase normal pressure storage tank 25 and the continuous phase buffer storage tank 25. Two valves 24 and 22 are used to communicate between the storage tanks 23 , between the continuous phase buffer storage tank 23 and the continuous phase high-pressure storage tank 21 .

The dispersed phase pressure chamber 16 and the wind chamber 14 are sleeved on the outside of the continuous phase pressure tank 19, and the dispersed phase pressure chamber 16 and the wind chamber 14 are independent of each other; the dispersed phase inlet hole 9 is located in the dispersed phase pressure chamber 16, and the air distribution hole 10 is located In the air chamber 14 , the dispersed phase pressure chamber 16 communicates with the dispersed phase high-pressure storage tank 6 through the double valve 7 , and the air chamber 14 is connected with the external fan through the double valve 11 .

In addition, the device also includes a discharge tank 12 and a discharge device 17 , the discharge tank 12 communicates with the discharge port through a double valve 13 , and the discharge device 17 communicates with the discharge port through a double valve 18 .

The rotary stirring device comprises a motor 20, a stirring shaft and a rotating paddle 15, the stirring shaft runs through the continuous phase pressure tank 19, the upper end of the stirring shaft is connected with the motor 20, and the rotating paddle 15 is arranged on the stirring shaft located in the continuous phase pressure tank superior.

The side wall of the continuous phase pressure tank 19 is provided with 12 dispersed phase inlet holes 9, and the 12 dispersed phase inlet holes are on the same horizontal circumference. The dispersed phase inlet hole 9 is arranged obliquely, and the angle between the dispersed phase inlet hole 9 and the vertical plane is 30°.

The diameter of the dispersed phase inlet hole 9 is less than 2 mm, and the distance between adjacent dispersed phase inlet holes is 6 mm. In the actual manufacturing process, the diameter of the dispersed-phase inlet and the spacing between the dispersed-phase inlets can be set according to the user's production volume, but the minimum distance between adjacent dispersed-phase inlets is twice the diameter of the dispersed-phase inlet.

The side wall of the continuous phase pressure tank is provided with 12 air distribution holes 10, and the 12 air distribution holes are located on the same horizontal circumference. The air distribution holes 10 are arranged obliquely, and the included angle between the air distribution holes 10 and the horizontal plane is 10°.

The aperture of the air distribution hole 10 is less than 5mm. The wind speed entering the air distribution hole 10 from the air chamber is greater than 0.1m/s.

Example 2:

This embodiment provides a kind of equipment for rapid and continuous preparation of droplet microspheres, the structure is as described in Embodiment 1, the difference is that the continuous phase pressure tank 19 includes a cylindrical tank body on the upper part and a frustoconical tank on the lower part body, the dispersed phase inlet hole 9 is located on the side wall of the cylindrical tank body, and the air distribution hole 10 is located on the side wall of the truncated conical tank body.

Example 3:

A. The specific operation steps of continuous feeding of dispersed phase are as follows:

(1) Add the dispersed phase to the dispersed phase normal pressure storage tank 2, close the double valve 5 between the dispersed phase buffer storage tank 4 and the dispersed phase high pressure storage tank 6, and open the dispersed phase normal pressure storage tank 2 With the double valve 3 between the dispersed phase buffer storage tank 4, the dispersed phase flows into the dispersed phase buffer storage tank 4 from the dispersed phase normal pressure storage tank 2;

(2) When the dispersed phase in step (1) enters the 3/4 position in the dispersed phase buffer storage tank 4, close the double valve between the dispersed phase normal pressure storage tank 2 and the dispersed phase buffer storage tank 4 3. Stamping into the dispersed phase buffer storage tank 4;

(3) After the pressure value in the dispersed phase buffer storage tank 4 is the same as the pressure value in the dispersed phase high pressure storage tank 6, stop punching, open the gap between the dispersed phase buffer storage tank 4 and the dispersed phase high pressure storage tank 6 Double valve 5, the dispersed phase flows in the dispersed phase high pressure storage tank 6, then close the double valve 5 between the dispersed phase buffer storage tank 4 and the dispersed phase high pressure storage tank 6, at the same time, open the dispersed phase normal pressure storage tank The double valve 3 between the material tank 2 and the dispersed phase buffer storage tank 4 releases pressure, opens the double valve 7 between the dispersed phase high pressure storage tank 6 and the dispersed phase pressure chamber 16, and the dispersed phase enters the dispersed phase pressure chamber 16 and injected into the continuous phase pressure tank 19 through the dispersed phase inlet hole 9.

B. The specific operation steps of the continuous phase continuous feeding are as follows:

(1) The continuous phase is added to the continuous phase normal pressure storage tank 25, close the double valve 22 between the continuous phase buffer storage tank 23 and the continuous phase high pressure storage tank 21, and open the continuous phase normal pressure storage tank 25 With the double valve 24 between the continuous phase buffer storage tank 23, the continuous phase flows into the continuous phase buffer storage tank 23 by the continuous phase normal pressure storage tank 25;

(2) When the continuous phase in step (1) enters the 3/4 position in the continuous phase buffer storage tank 23, close the double valve between the continuous phase normal pressure storage tank 25 and the continuous phase buffer storage tank 23 24, stamping into the continuous phase buffer storage tank 23;

(3) After the pressure value in the continuous phase buffer storage tank 23 is the same as the pressure value in the continuous phase high pressure storage tank 21, stop stamping, open the continuous phase buffer storage tank 23 and the continuous phase high pressure storage tank 21 Double valve 22, the continuous phase flows in the continuous phase high pressure storage tank 21, then close the double valve 22 between the continuous phase buffer storage tank 23 and the continuous phase high pressure storage tank 21, at the same time, open the continuous phase normal pressure storage tank The double valve 24 between the material tank 25 and the continuous phase buffer storage tank 23 is depressurized, and the double valve 8 between the continuous phase high pressure storage tank 21 and the continuous phase pressure tank 19 is opened, and the continuous phase enters the continuous phase pressure tank 19 Inside.

C. In the continuous phase pressure tank 19, the continuous phase pressure tank 19 is ventilated through the air distribution holes 10, the motor 20 is started, and the rotating paddle 15 rotates to drive the continuous phase to produce a tangential velocity, and the continuous phase shears the dispersed phase so that The dispersed phase forms liquid droplets, and the liquid droplets move upward under the action of their own buoyancy and the wind, and enter the discharge device 17 through the discharge port.

This embodiment provides a method for using a device for rapidly and continuously preparing droplet microspheres, including the following steps,

(1) Water (W) is the continuous phase and oil (O) is the dispersed phase. Add the oil phase into the dispersed phase pressure chamber 16 according to the operation steps of A above; add the water phase into the continuous phase pressure tank 19 according to the operation steps of B.

(2) Set 36 dispersed phase inlet holes 9 inclined at an angle of 45°, the distance between adjacent dispersed phase inlet holes 9 is 1 mm, and the aperture is less than 100 μm; the inclination angle of the air distribution holes 10 is 60°, and the circumferential direction is evenly arranged 36 One, the aperture is 1.5~2mm, and the inlet gas velocity is 3m/s.

(3) The working pressure of the dispersed phase pressure chamber 16 is 1Mpa; the working pressure of the continuous phase pressure tank 19 is 0.1Mpa.

(4) The motor 20 rotates counterclockwise at a speed of 300 rpm; the water phase driving the continuous phase pressure tank 19 has a certain tangential speed.

(5) The oil phase in the dispersed phase pressure chamber 16 enters the continuous phase pressure tank 19 through the dispersed phase inlet hole 9 under pressure. The water phase with a certain tangential velocity shears the dispersed phase to form oil droplets with a particle size of less than 2mm.

(6) The oil droplets move upwards under the action of their own buoyancy and the carrying effect of the wind passing through the air distribution hole 10; the double valves 18 are opened, and under the action of the water phase with a certain tangential velocity, the oil droplets are collected to the outlet In the feeder 17.

The continuous feeding of the dispersed phase under pressure is realized by setting the dispersed phase normal pressure storage tank, the dispersed phase buffer storage tank and the dispersed phase high pressure storage tank, and by setting the continuous phase normal pressure storage tank and the continuous phase buffer storage tank , The continuous phase high-pressure storage tank realizes the continuous feeding of the continuous phase under pressure, and finally realizes the continuous supply of raw materials, ensures the continuous preparation of droplet microspheres, and realizes continuous production. The ball quickly enters the discharge device, which promotes the production speed of droplet microspheres, and realizes the rapid and efficient production of this equipment.

Claims (9)

1. a kind of quick equipment for continuously preparing drop microballoon, it is characterised in that the equipment includes dispersed phase feed arrangement, connected Continuous phase feed arrangement, continuous phase pressurized tank and rotational agitation device, the top of the continuous phase pressurized tank is fed with continuous phase to be filled Connection is put, the bottom of the continuous phase pressurized tank is provided with discharge port, set from top to bottom on the side wall of the continuous phase pressurized tank There are discharging opening, dispersed phase to enter hole and wind distributing hole, the dispersed phase feed arrangement enters hole with dispersed phase and connected, the rotational agitation dress Put and be disposed through in continuous phase pressurized tank；

Dispersed phase normal pressure storage tank, the dispersed phase that the dispersed phase feed arrangement includes from top to bottom connecting buffer storage tank and divided Between dephasing high pressure storage tank, the dispersed phase normal pressure storage tank and dispersed phase buffering storage tank, dispersed phase buffering storage tank and Connected between dispersed phase high pressure storage tank using double valve.

2. the quick equipment for continuously preparing drop microballoon as claimed in claim 1, it is characterised in that the continuous phase charging dress Continuous phase normal pressure storage tank, continuous phase buffering storage tank and continuous phase high pressure storage tank including from top to bottom connecting are put, it is described Continuous phase normal pressure storage tank and continuous phase buffering storage tank between, continuous phase buffering storage tank and continuous phase high pressure storage tank between Connected using double valve.

3. the quick equipment for continuously preparing drop microballoon as claimed in claim 1, it is characterised in that in the continuous phase pressure Tank outer sheath is provided with dispersed phase balancing gate pit and air compartment, and the dispersed phase balancing gate pit and air compartment are separate；The dispersed phase enters hole In dispersed phase balancing gate pit, the wind distributing hole is located in air compartment, and the dispersed phase balancing gate pit is high by double valve and dispersed phase Press storage tank connection.

4. the quick equipment for continuously preparing drop microballoon as claimed in claim 1, it is characterised in that the continuous phase pressurized tank The truncated cone-shaped tank body of cylindrical tank and lower part including upper part, the dispersed phase enters hole position in the side wall of cylindrical tank On, the wind distributing hole is located on the side wall of truncated cone-shaped tank body.

5. the quick equipment for continuously preparing drop microballoon as claimed in claim 1, it is characterised in that the equipment also includes unloading Batch can and discharger, the discharge tank are connected by double valve with discharge port, and the discharger is connected by double valve and discharging opening It is logical.

6. the quick equipment for continuously preparing drop microballoon as claimed in claim 1, it is characterised in that the rotational agitation device Including motor, agitating shaft and rotation blade, the agitating shaft is disposed through continuous phase pressurized tank, the upper end of the agitating shaft with Motor connection, the rotation blade is arranged on the agitating shaft in continuous phase pressurized tank.

7. the quick equipment for continuously preparing drop microballoon as claimed in claim 1, it is characterised in that the continuous phase pressurized tank Side wall enter hole provided with multiple dispersed phases, multiple dispersed phases enter hole and are on same level circumference.

8. the quick equipment for continuously preparing drop microballoon as claimed in claim 1, it is characterised in that the continuous phase pressurized tank Side wall be provided with multiple wind distributing holes, multiple wind distributing holes be in same level circumference on.

9. a kind of application method of quick continuous equipment for preparing drop microballoon as described in any one of claim 1 to 8, including Following steps,

Continuous phase and dispersed phase are added separately in continuous phase normal pressure storage tank and dispersed phase normal pressure storage tank, continuous phase passes through Entered after continuous phase normal pressure storage tank, continuous phase buffering storage tank and continuous phase high pressure storage tank in continuous phase pressurized tank, with This simultaneously, dispersed phase is entered after buffering storage tank and dispersed phase high pressure storage tank by dispersed phase normal pressure storage tank, dispersed phase In dispersed phase balancing gate pit, and entered by dispersed phase in hole injection continuous phase pressurized tank；

In continuous phase pressurized tank, divulged information by wind distributing hole into continuous phase pressurized tank, electric motor starting, rotation blade rotating band is moved Continuous phase makes its produce tangential velocity, and continuous phase shearing dispersed phase makes dispersed phase formation drop, and drop is in natural buoyancy and wind Move, entered by discharging opening in discharger upwards under rolling action.