CN111250283B - Atomizing nozzle with auxiliary heating device suitable for rapid freezing environment - Google Patents

Abstract

The utility model provides a take auxiliary heating device's atomizing nozzle suitable for under rapid freezing environment, be applicable to biological sample under the ultra-low temperature environment, the freeze-drying preparation of hyperfine aerosol granule such as dry powder sample, including gas circuit joint, nozzle main part, liquid circuit joint, the heating ring, the thermal control module, the lagging casing, the low temperature jar flange, shower nozzle and sealing washer, the atomizing under the realization ultra-low temperature environment that makes the nozzle can be smooth through the auxiliary heating of thermal control device and temperature control, atomize into tiny fog droplet to liquid biological sample, form tiny freezing ice crystal to the fog droplet quick-freeze in the ultra-low temperature environment that liquid nitrogen formed, prepare into dry powder granule through sublimation processing again.

Description

An atomizing nozzle with auxiliary heating device suitable for rapid freezing environment

technical field

The invention relates to an atomizing nozzle with an auxiliary heating device suitable for a rapid freezing environment, which is suitable for the freeze-drying preparation of ultrafine aerosol particles such as biological samples and dry powder samples in an ultra-low temperature environment.

Background technique

The spray ultra-low temperature quick-freezing-vacuum freeze-drying cascade coupling aerosolizable biological particle dry powder preparation technology is divided into two key steps: the liquid biological sample is atomized into fine droplets by the atomizing nozzle, and the mist is formed by the ultra-low temperature environment formed by liquid nitrogen. Drops are quick-frozen to form fine frozen particles; the frozen particles are vacuum freeze-dried by the principle of sublimation, and finally the dried fine particles are obtained.

Liquid atomization refers to the process of liquid becoming liquid mist or small droplets in a gas environment under the action of external energy. In order to prepare biological samples such as pathogens that meet the requirements, the aerodynamic diameter of the atomized droplets needs to be controlled within 3-5 μm.

In order to ensure the activity of biological samples, the flow rate and pressure of the spray are relatively low, and once the spray enters the low temperature chamber, it must be rapidly frozen, and the low temperature range is -100 ° C ~ -194 ° C. This ultra-low temperature environment will cause the nozzles working with low flow and low pressure to freeze and condense soon after working, and the internal flow channels are blocked, making it impossible to continue the preparation of biological samples.

SUMMARY OF THE INVENTION

The technical problem solved by the present invention is: to overcome the deficiencies of the prior art, to provide an atomizing nozzle with an auxiliary heating device suitable for a rapid freezing environment, and to solve the problem that the ultra-low temperature environment will cause the nozzle to work at low flow and low pressure to work soon. The phenomenon of freezing and condensation occurs, and the internal flow channel is blocked.

The technical scheme of the present invention is: an atomizing nozzle with an auxiliary heating device suitable for a rapid freezing environment, comprising: the nozzle includes a gas path joint, a nozzle body, a liquid path joint, a heating ring, a thermal control module, a thermal insulation Shell, cryogenic tank flange and spray head; wherein, the nozzle body is a rotary structure, and the inside of the nozzle body is provided with a first eccentric through hole, a second eccentric through hole and a center through hole, wherein, The first eccentric through hole and the second eccentric through hole are arranged in parallel, the second eccentric through hole is connected with the central through hole, and the center through hole is located at the lower part of the second eccentric through hole; the nozzle body The upper part of the side wall is provided with a first cylindrical boss interface, the first cylindrical boss interface is butted with the gas path joint, and the channel opened inside the gas path joint is communicated with the first eccentric straight hole The top end of the nozzle body is provided with a second cylindrical boss interface, the second cylindrical boss interface is butted with the liquid path joint, and the channel opened inside the liquid path joint is connected with the second eccentric straight hole The middle part of the nozzle body is provided with a step with an external thread, and the step with the external thread is connected with the internal thread of the heating ring by screwing; The outer wall of the cylindrical section is provided with two to three protruding guide sections, which are inserted into the inner hole of the nozzle; the thermal control module is sleeved on the outer surface of the heating ring, and the thermal insulation shell is sleeved on the outer surface of the thermal control module for heat preservation. The side wall of the thermal insulation shell is provided with a wire outlet window, through which the lead wire of the thermal control module is drawn out; the outer thread of the heating ring is connected with the inner thread of the low temperature tank flange.

In the above-mentioned atomizing nozzle with auxiliary heating device suitable for rapid freezing environment, the bottom end face of the nozzle body is provided with a swirler with a truncated truncated structure with several spiral grooves.

In the above-mentioned atomizing nozzle with auxiliary heating device suitable for rapid freezing environment, the outer wall of one end of the gas path joint is provided with an external thread, and the other end of the gas path joint is a first hollow cylinder with steps, A first hexagonal outer convex step is arranged in the middle of the gas path joint; wherein, the first cylindrical boss interface is connected with the first hollow cylinder of the step.

In the above-mentioned atomizing nozzle with auxiliary heating device suitable for rapid freezing environment, one end of the liquid path joint is a joint with an inner cone, and the other end of the liquid path joint is a second hollow cylinder with steps , a second hexagonal outer convex step is arranged in the middle of the liquid path joint; wherein, the second cylindrical boss interface is connected with the second hollow cylinder of the step.

In the above-mentioned atomizing nozzle with auxiliary heating device suitable for rapid freezing environment, the nozzle is a hollow revolving body with steps, which is sleeved on the outer side of the cylindrical section at the bottom end of the nozzle body, and the bottom end of the nozzle is round The table-shaped structure forms an air jet flow channel with the nozzle body. The outer surface of the top step of the nozzle is covered with a circular sealing ring, which is compressed by the threaded connection between the nozzle body and the heating ring to achieve sealing.

In the above-mentioned atomizing nozzle with auxiliary heating device suitable for rapid freezing environment, the heating ring is a hollow cylinder with steps.

In the above-mentioned atomizing nozzle with auxiliary heating device suitable for rapid freezing environment, the spiral groove of the swirler is processed along the direction of the generatrix of the swirler circular frustum, and the cross section of the groove can be triangular, rectangular or semicircular.

In the above-mentioned atomizing nozzle with auxiliary heating device suitable for rapid freezing environment, the thermal control module includes a heat conducting shell, a heating wire and a thermocouple; wherein, the heating wire and the thermocouple are alternately wound around the heat conducting shell the outer surface of the body.

In the above-mentioned atomizing nozzle with auxiliary heating device suitable for rapid freezing environment, the heating wire and the thermocouple are connected with a temperature controller, and the temperature controller performs temperature detection and feedback control through a PID algorithm, and adjusts the heating The input voltage and power consumption of the wire make the nozzle work within the normal temperature range.

In the above-mentioned atomizing nozzle with auxiliary heating device suitable for rapid freezing environment, the outer thread of one end of the gas path joint is a taper thread, and the taper thread is connected to the upstream gas pipeline, and the working pressure is Within 0.5MPa; the inner conical joint of the liquid path joint is connected with the upstream liquid path pipeline, and the working pressure is within 0.3MPa.

In the above-mentioned atomizing nozzle with auxiliary heating device suitable for the rapid freezing environment, the number of grooves of the spiral groove is as follows: n=2Q _g /Q _L ; wherein, Q _g is the volume flow of the assisting atomizing gas, and Q _L is the liquid Volume flow of the medium.

The beneficial effects of the present invention compared with the prior art are:

(1) The atomizing nozzle with auxiliary heating device proposed by the present invention is suitable for the rapid freezing environment, which has great demand in the current pharmaceutical, medical and biological fields, and can be used for batch preparation of stable and controllable bacteria , viruses, spores, toxins and other pathogen samples for multimodal spectroscopy analysis of various biological samples, and can also be used for various pharmaceutical preparations.

(2) For the atomizing nozzle with auxiliary heating device proposed by the present invention, auxiliary temperature control is performed on the nozzle through a thermal control module integrating heating and temperature measurement functions, and a PID controller is used for feedback control, so that the nozzle can work in an ideal long-term operation. within the scope of work.

(3) The atomizing nozzle with auxiliary heating device proposed by the present invention transfers the heat of the heating wire efficiently and concentratedly to the vortexer and the vicinity of the nozzle through the high thermal conductivity heating ring and the outer thermal insulation shell, so that the atomization of the nozzle is achieved. The quality is stable and guaranteed.

(4) The atomizing nozzle with auxiliary heating device proposed by the present invention utilizes gas swirl to assist the impinging liquid jet to achieve uniform and efficient atomization. In certain cases, heating gas can also be used for auxiliary atomization to further improve the low temperature environment. fog effect.

Description of drawings

Fig. 1 is the structural representation of the atomizing nozzle with auxiliary heating device;

Fig. 2 is a schematic diagram of the structure of the air flow channel;

Fig. 3 is a schematic diagram of the structure of a liquid channel;

Fig. 4 is a schematic diagram of external mixing impact atomization;

5 is a schematic structural diagram of a heating module;

Detailed ways

The specific embodiments of the present invention will be further described in detail below with reference to the accompanying drawings.

As shown in FIG. 1 , the present invention provides an atomizing nozzle with auxiliary heating device suitable for rapid freezing environment, comprising a gas path connector 1, a nozzle body 2, a liquid path connector 3, a heating ring 4, and a thermal control module 5. Thermal insulation shell 6, low temperature tank flange 7, nozzle 8 and sealing ring 9; among them,

The nozzle main body 2 is a revolving body structure. The inside of the nozzle main body 2 is provided with a first eccentric through hole 21, a second eccentric through hole 22 and a central through hole 23. The first eccentric through hole 21 and the second eccentric through hole 23 The eccentric through holes 22 are arranged in parallel, the second eccentric through holes 22 are communicated with the center through holes 23, and the center through holes 23 are located at the lower part of the second eccentric through holes 22; the upper part of the side wall of the nozzle body 2 is provided with The first cylindrical boss interface 24, the first cylindrical boss interface 24 is docked with the air joint 1, and the channel opened inside the gas joint 1 is communicated with the first eccentric straight hole 21; the top of the nozzle body 2 is provided with a The second cylindrical boss interface 25, the second cylindrical boss interface 25 is butted with the liquid path joint 3, and the channel opened inside the liquid path joint 3 is communicated with the second eccentric straight hole 22; the middle of the nozzle body 2 is provided with a A step 26 with an external thread, the step 26 with an external thread is connected with the inner thread of the heating ring 4 by screwing; the cylindrical section 27 of the nozzle body 2 is arranged at the lower part of the step 26, and the outer wall of the cylindrical section 27 is provided with a Two to three protruding guide sections are inserted into the inner hole of the nozzle 8; the thermal control module 5 is sleeved on the outer surface of the heating ring 4, and the thermal insulation shell 6 is sleeved on the outer surface of the thermal control module 5 for thermal insulation. A wire outlet window is opened on the side wall of the heating ring, so that the lead wire of the thermal control module 5 can be drawn out; the outer thread of the heating ring 4 is connected with the inner thread of the low temperature tank flange 7.

Specifically, the nozzle body 2 is a revolving body structure with an eccentric through hole on the outside of the sheet, an eccentric round hole on the top and a center through hole at the bottom, and the eccentric hole on the inner side is connected to the center The through holes are connected; there is a cylindrical boss interface on the side of the top end of the nozzle body 2 that is docked with the gas path joint 1, wherein the circular hole of the cylindrical boss docked with the gas path joint 1 is connected with the outer eccentric straight hole; the nozzle There is a cylindrical boss interface above the top of the main body 2 which is connected with the liquid circuit joint 3; there is a step with an external thread in the middle of the nozzle main body 2, which is connected with the internal thread of the heating ring 4 by screwing; The cylindrical section has two to three protruding guide sections on its outer wall, which are inserted into the inner hole of the nozzle 8. On the one hand, the guide section is used for positioning to ensure the centering of the assembly, and on the other hand, the flow channel for the gas to pass through is reserved. ; The bottom end of the main body 2 of the nozzle is a swirl device with a truncated structure with a number of spiral grooves processed on the surface.

The outer wall of one end of the gas path fitting 1 is provided with an external thread, the other end of the gas path fitting 1 is a first hollow cylinder with steps, and the middle part of the gas path fitting 1 is provided with a first hexagonal convex step; Wherein, the first cylindrical boss interface 24 is connected with the first hollow cylinder of the step.

Specifically, the gas path connector 1 is a hollow cylinder with a thread at one end and a step at the other end, and a hexagonal convex step in the middle, which is used for wrench fixing to tighten the thread; the gas path connector 1 is inserted into the cylindrical protrusion on the top side of the nozzle body 2 In the inner hole of the table, and connected and fixed by welding method.

One end of the liquid path joint 3 is a joint with an inner cone, the other end of the liquid path joint 3 is a second hollow cylinder with steps, and the middle of the liquid path joint 3 is provided with a second hexagonal convex step. ; Wherein, the second cylindrical boss interface 25 is connected with the second hollow cylinder of the step.

Specifically, the liquid path joint 3 is a hollow cylinder with an inner conical quick joint at one end and a step at the other end, and a hexagonal outer convex step in the middle, which is used for wrench fixing, and is inserted into the inner hole of the cylindrical boss above the top of the nozzle body 2 , and fixed by welding.

The nozzle 8 is a hollow revolving body with steps, which is sleeved on the outer side of the cylindrical section at the bottom end of the nozzle main body 2, and is tightly fitted with two to three convex guide sections; 2 constitutes an air jet flow channel, and the outer side of the top step is covered with a circular sealing ring 9, which is pressed by the screw connection of the nozzle body 2 and the heating ring 4 to achieve sealing.

The heating ring 4 is a hollow cylinder with steps, which is sleeved on the outside of the nozzle 8, and its external thread is butted with the internal thread of the low temperature tank flange 7 to realize the connection between the nozzle and the low temperature tank; the thermal control module 5 is sleeved on the heating ring 4. The outer side of the thermal control module 5 is tightly fitted and contacted for effective heat transfer; the lead wires of the heater and the temperature measuring device are thrown out from the top; Module 5 leads can be drawn from it.

As shown in FIG. 2 , the gas for auxiliary atomization enters the nozzle body 2 through the inner hole of the gas path joint 1, and after flowing through the right-angle flow channel of the nozzle body 2, it enters the inner cavity formed by the nozzle body 2 and the nozzle 8. Finally, it is ejected through the swirler flow channel of the nozzle body 2 to generate a swirling airflow with a circumferential velocity.

As shown in Figure 3, the liquid working medium used to prepare the aerosol sample enters the nozzle body 2 from the inner hole of the liquid connection 3, flows through the eccentric straight through hole, and then enters the injection hole in the center of the nozzle. ejected in the form of a jet.

As shown in Figure 4, the liquid working medium is ejected from the central hole at the bottom of the nozzle body 2 to form a single-hole jet, while the air flow for auxiliary atomization is ejected from the spiral groove of the vortexer of the nozzle body 2, and after rotation, it reaches the impact point position. The jet is broken, broken and atomized to form uniform and fine droplets with aerodynamic diameter of 3-5μm, which are sprayed into the low-temperature freezing chamber, directly sprayed on the surface of liquid nitrogen at a distance of about 10cm, and rapidly frozen into ice crystals. Sublimation completes the final dry powder sample preparation.

As shown in FIG. 5 , the thermal control module 5 includes a heat-conducting housing, a heating wire and a thermocouple; wherein, the heating wire and the thermocouple are alternately wound on the outer surface of the heat-conducting housing. Specifically, the copper heat-conducting shell of the thermal control module 5 has good heat transfer capability. In the winding window inside the shell, several turns of high-power heating wires and thermocouples can be evenly wound to make the thermal control Module 5 has both heating and temperature measurement functions. The leads of the heating wire and the thermocouple are thrown out of the top cabin and connected to the temperature controller for PID feedback control and temperature adjustment.

The heating power of the heating wire is P _heating =A·C·d·Δt _m ; among them, P heating is the heating power, A is the effective heat exchange area, C is the heating efficiency, d is the material specific heat, and Δt _m is the logarithmic average temperature difference. The heating power of the heating wire is obtained according to the above formula, which can better efficiently transfer the heat of the heating wire to the vortexer and the vicinity of the nozzle of the nozzle, so that the atomization quality of the nozzle can be stably guaranteed.

The air joint 1, the nozzle body 2, the liquid joint 3, and the nozzle 8 are all made of titanium alloy, which has good biocompatibility.

The sealing ring 9 is made of polytetrafluoroethylene plastic, which has good biocompatibility and good sealing performance.

The heat-conducting shells of the heating ring 4 and the thermal control module 5 should be made of metal materials with good thermal conductivity, such as brass and red copper, to improve the heat transfer efficiency.

The thermal insulation shell 6 should be processed with materials with good thermal insulation, such as Teflon materials.

The spiral groove of the swirler at the bottom end of the nozzle body 2 is processed along the generatrix direction of the swirl truncated cone, and the cross section of the groove can be triangular, rectangular or semicircular.

The number of grooves of the spiral groove is as follows: n=2Q _g /QL ; wherein, Q _g is the volume flow of the assisting atomizing gas, and Q _L is the volume flow of the liquid medium _. The number of grooves of the spiral groove is obtained according to the above formula, which can better obtain multiple uniform rotating airflows to achieve the impact on the liquid jet, and better improve the uniformity and neutrality of atomization.

The conical inner hole at the bottom end of the nozzle 8 is tightly fitted with the outer wall of the vortex of the nozzle body 2 to ensure that the main air flow is sprayed along the spiral groove flow channel.

The gas path joint 1 is generally connected with the upstream gas path pipeline by a one-point taper thread, and the working pressure is generally within 0.5MPa, and is connected to the nozzle body 2 by laser welding or electron beam welding.

The liquid path joint 3 is generally connected to the upstream liquid path pipeline by an inner cone type quick joint, and the working pressure is generally within 0.3MPa, and is connected to the nozzle body 2 by laser welding or electron beam welding.

Contents that are not described in detail in the specification of the present invention belong to the well-known technology of those skilled in the art.

Claims (10)

1. An atomizing nozzle with an auxiliary heating device suitable for a rapid freezing environment, comprising: the nozzle comprises a gas path joint (1), a nozzle main body (2), a liquid path joint (3), a heating ring (4), a thermal control module (5), a heat-insulating shell (6), a low-temperature tank flange (7) and a spray head (8); wherein,

the nozzle main body (2) is of a revolving body structure, a first eccentric through round hole (21), a second eccentric through round hole (22) and a central through small hole (23) are formed in the nozzle main body (2), wherein the first eccentric through round hole (21) and the second eccentric through round hole (22) are arranged in parallel, the second eccentric through round hole (22) is communicated with the central through small hole (23), and the central through small hole (23) is positioned at the lower part of the second eccentric through round hole (22);

a first cylindrical boss interface (24) is arranged at the upper part of the side wall of the nozzle main body (2), the first cylindrical boss interface (24) is in butt joint with the gas circuit connector (1), and a channel formed in the gas circuit connector (1) is communicated with a first eccentric straight-through round hole (21);

a second cylindrical boss interface (25) is arranged at the top end of the nozzle main body (2), the second cylindrical boss interface (25) is in butt joint with the liquid path joint (3), and a channel formed in the liquid path joint (3) is communicated with a second eccentric straight-through round hole (22);

the middle part of the nozzle main body (2) is provided with a step (26) with an external thread, and the step (26) with the external thread is screwed with the internal thread of the heating ring (4) through the thread;

the cylindrical section (27) of the nozzle main body (2) is arranged at the lower part of the step (26), and the outer wall of the cylindrical section (27) is provided with two to three convex guide sections which are inserted into an inner hole of the spray head (8);

the thermal control module (5) is sleeved on the outer surface of the heating ring (4), the heat insulation shell (6) is sleeved on the outer surface of the thermal control module (5) for heat insulation, and the side wall of the heat insulation shell (6) is provided with a wire outlet window so that a lead of the thermal control module (5) is led out;

the external thread of the heating ring (4) is connected with the internal thread of the low-temperature tank flange (7).

2. An atomizing nozzle with auxiliary heating device suitable for use in a rapid freezing environment according to claim 1, wherein: the bottom end face of the nozzle main body (2) is provided with a plurality of whirlpools with spiral grooves and truncated cone-shaped structures.

3. An atomizing nozzle with auxiliary heating device suitable for use in a rapid freezing environment according to claim 1, wherein: the outer wall of one end of the gas circuit joint (1) is provided with an external thread, the other end of the gas circuit joint (1) is a first hollow cylinder with steps, and the middle of the gas circuit joint (1) is provided with a first hexagonal outer convex step; wherein the first cylindrical boss interface (24) is connected with the first hollow cylinder of the step.

4. An atomizing nozzle with auxiliary heating device suitable for use in a rapid freezing environment according to claim 1, wherein: one end of the liquid path joint (3) is a joint with an inner cone shape, the other end of the liquid path joint (3) is a second hollow cylinder with steps, and the middle part of the liquid path joint (3) is provided with a second hexagonal outer convex step; wherein the second cylindrical boss interface (25) is connected with a second hollow cylinder of the step.

5. An atomizing nozzle with auxiliary heating device suitable for use in a rapid freezing environment according to claim 1, wherein: the spray head (8) is a hollow rotary body with steps and is sleeved on the outer side of a cylindrical section at the bottom end of the nozzle main body (2), the bottom end of the spray head (8) is of a round table-shaped structure and forms a gas path spraying flow channel with the nozzle main body (2), the outer surface of the step at the top end of the spray head (8) is sleeved with a circular sealing ring (9), and the spray head is tightly connected with the heating ring (4) through threads of the nozzle main body (2) to realize sealing.

6. An atomizing nozzle with auxiliary heating device suitable for use in a rapid freezing environment according to claim 2, wherein: the spiral groove of the swirler is processed along the generatrix direction of the circular truncated cone of the swirler, and the section of the groove can be triangular, rectangular or semicircular.

7. An atomizing nozzle with auxiliary heating device suitable for use in a rapid freezing environment according to claim 1, wherein: the thermal control module (5) comprises a heat conduction shell, a heating wire and a thermocouple; wherein,

the heating wire and the thermocouple are wound on the outer surface of the heat conducting shell alternately.

8. An atomizing nozzle with auxiliary heating device suitable for use in a rapid freezing environment according to claim 7, wherein: the heating wire and the thermocouple are connected with a temperature controller, the temperature controller carries out temperature detection and feedback control through a PID algorithm, and the input voltage and the power consumption of the heating wire are adjusted, so that the nozzle works in a normal temperature range.

9. An atomizing nozzle with auxiliary heating device suitable for use in a rapid freezing environment according to claim 3, wherein: the external thread at one end of the gas circuit joint (1) is a tapered thread, the tapered thread is connected with an upstream gas circuit pipeline, and the working pressure is within 0.5 MPa; the inner conical joint of the liquid path joint (3) is connected with an upstream liquid path pipeline, and the working pressure is within 0.3 MPa.

10. An atomizing nozzle with auxiliary heating device suitable for use in a rapid freezing environment according to claim 6, wherein: the number of the spiral grooves is as follows: n is 2Q_g/Q_L(ii) a Wherein Q is_gTo assist the volumetric flow of atomising gas, Q_LIs the volumetric flow rate of the liquid medium.

Images