WO2017084161A1

WO2017084161A1 - Heating and drying means and method for spray freeze drying apparatus

Info

Publication number: WO2017084161A1
Application number: PCT/CN2015/098806
Authority: WO
Inventors: 郑效东
Original assignee: 上海东富龙科技股份有限公司
Priority date: 2015-11-17
Filing date: 2015-12-24
Publication date: 2017-05-26
Also published as: CN105300063A; CN105300063B

Abstract

A heating and drying means for a spray freeze drying apparatus, comprising an outer cylindrical container for forming a closed space, a rotary dryer, and a temperature controlling circulating system. The rotary dryer that is partially provided inside the outer cylindrical container is used for accommodating and dynamically heating a material; the temperature controlling circulating system is connected to the rotary dryer and is used for controlling the heating temperature of the rotary dryer. The outer cylindrical container comprises an outer cylinder (1), which is provided with a material feeding pipe (2), a pumping port (3), and a material discharging port (4). The rotary dryer comprises a rotating cylinder (11), a motor (13), and a rotating shaft (12). A heating circulating system comprises a rotary joint (21), a heat exchanger (22), an electrical heater (23), and a fluid pump (24) that form a closed loop. The heating and drying method for a spray freeze drying apparatus comprises: adding a material to the rotating cylinder (11) by means of the material feeding pipe (2), wherein the rotating cylinder (11) continuously rotates during the drying process, such that the granular material keeps tumbling, so as to be heated by means of full and even contact with the cylinder wall.

Description

Heating drying device and method for spray freeze-drying equipment

Technical field

The invention relates to a heating and drying device, in particular to a heating and drying device for a spray freeze-drying device.

Background technique

In the conventional freeze-drying process, as shown in FIG. 1, the liquid A to be lyophilized needs to be pre-filled into a container B such as a glass bottle or a tray, and the container B is placed on the flat layer C to be frozen. In the ice, the temperature of the plate is heated in a vacuum environment to heat the ice, and the water vapor sublimates and leaves a dry substance. During the drying process, the material to be dried is always allowed to stand, and only a small area of the bottom is in contact with the plate layer, and heat transfer is limited, especially when the material is pre-loaded into a container of a poorly-conducted conductor such as a glass bottle for lyophilization. The heat effect is poor, and the drying time is long; the upper surface of the static material is first dried, and the dry layer gradually descends toward the frozen layer. At this stage, the dry layer becomes a hindrance to the outward diffusion of the sublimated water vapor of the frozen layer, and the mass transfer effect is poor. The drying time is further extended; in addition, static drying imposes high requirements on the uniformity of the sheet temperature.

Later, a dynamic freeze-drying apparatus was introduced in which the material previously frozen into ice particles was placed in a conical dryer, and the animal feed was turned using a rotary-driven agitator which heated the material by a cone wall. The stirrer flips to apply mechanical force to the material, and the friction and collision action easily destroy the original shape state of the material; and the material must be piled up to a certain height in the cone to be flipped by the agitator, and this accumulation also hinders the bottom sublimation water vapor direction. External diffusion; in addition, the conical dryer can only be dried in several stages.

In summary, how to improve the drying rate of materials in freeze-drying, improve the heat and mass transfer effect in this process, and how to avoid destroying the original shape of the material during the drying process, how to make the freeze-drying continuous Problems to be solved by those skilled in the art are urgently solved.

Summary of the invention

The technical problem to be solved by the invention is how to make the material in the drying stage in the freeze-drying process to be heated sufficiently and uniformly heated, so that the sublimation gas can be rapidly diffused outward, the drying efficiency is improved, the drying process is further continuous, and the drying process is not destroyed. The original shape of the material.

In order to solve the above technical problem, the technical solution of the present invention is to provide a heating method for a spray freeze-drying device. a drying device, comprising: an outer cylinder container for forming a closed space; a rotary dryer portion for accommodating and dynamically heating the material is disposed in the outer cylinder container; and a temperature control cycle for controlling the heating temperature of the rotary dryer The system is connected to a rotary dryer.

Preferably, the outer cylinder container is a closed container, including an outer cylinder, and the outer cylinder is provided with

Used for connecting other devices to add the material to be dried to the feed pipe of the rotary dryer;

a suction port for evacuating the outer cylinder container and discharging the sublimation gas out of the container during the drying process;

And a discharge port for discharging the dry material, and a discharge valve is arranged at the discharge port.

Further, the other device connected to the feed pipe may be a spray freeze granulation device;

Further, a feed valve is arranged on the feed pipe;

Preferably, the rotary dryer comprises

a drum for containing material;

a rotating shaft for connecting the drum to the motor;

A motor used to power the rotation of a shaft.

Preferably, all of the drum, a part of the rotating shaft is disposed in the outer cylinder container, and another part of the rotating shaft is connected to the motor outside the outer cylinder container.

Further, the rotating shaft and the outer cylinder are connected by a shaft seat.

Preferably, at least one hollow jacket is disposed outside the drum, and the fluid in the hollow jacket causes the wall to heat up or cool down.

Further, the hollow jacket has a rectangular cross-sectional shape and is arranged around the outer circumference of the rotating cylinder; the hollow jacket is one or more segments arranged in a straight line along the center line of rotation; each hollow jacket is provided The fluid enters and exits the pipeline, and the internal fluid circulation causes the cylinder wall to heat up or cool down.

Preferably, the inner wall of the rotating drum is provided with at least one guiding groove at an angle to the rotation center line of the rotating drum. When the rotating drum rotates in the forward direction, the material is guided by the guiding groove to migrate toward the discharging port; when the rotating drum rotates in the opposite direction The material is brought back.

Preferably, the temperature control circulation system comprises a rotary joint, a heat exchanger, an electric heater and a fluid pump which are sequentially connected to form a closed loop, and the circulating fluid is closed in the closed loop.

More preferably, the rotary joint is a device for one-side fixed connection, one side for connecting the rotary body and continuously conveying the fluid in any continuous or discontinuous rotational movement of the rotary body, and continuously delivering current. .

Further, the rotating shaft is internally provided with a passage for fluid circulation, and one side of the passage is connected to one or more hollow jackets on the rotating drum in the outer cylinder container; the other side of the passage is outside The outside of the canister is connected to the rotary joint. The rotary joint causes the fluid in the closed circuit to be continuously conveyed within the hollow jacket during any rotationally continuous or discontinuous rotational movement of the rotary shaft.

Further, the fluid is water or silicone oil.

Further, a detector for detecting material information is provided in the rotating drum, the information may be temperature; a detector is connected to the rotary joint; and the rotary joint rotates in any continuous or discontinuous rotational motion of the rotating shaft. The current is delivered without interruption.

The invention also provides a heating drying method for a spray freeze-drying device, which is characterized in that first, the outer cylinder container is evacuated into a vacuum, and the material pre-frozen into ice particles is fed into the rotating drum through the feeding tube; the temperature of the rotating drum Controlled by the temperature control circulation system; the drum continuously rotates during the drying process. When it rotates in the forward direction, the material rolls at the bottom of the drum, and is uniformly and uniformly heated in contact with the cylinder wall; the guide groove rotates with the drum to take the material from the drum When the bottom is brought up, the material slides on the guiding groove toward the discharge port. When the guiding groove continues to rotate with the rotating drum, the material falls to the bottom of the rotating cylinder due to gravity; the material is fed at an appropriate rate by controlling the feeding amount and the rotating speed of the rotating drum. The material port migrates and evenly spreads at the bottom of the drum without depositing, so that the sublimation gas is quickly discharged from the surface of the material and the gap of the particles; the material is continuously tumbling through the rotating drum and gradually moving forward, and gradually drying in the drum Until it is completely dry before discharge.

The appropriate rate is such that the material can be evenly dispersed at the bottom of the drum, does not form a pile, and is just completely dried when the material migrates to the discharge port to achieve continuous discharge.

The method can make the material continuously dried, or can be batch-dried by rotating the drum forward and reverse rotation. And the material in the drying device mainly relies on its own gravity to roll or migrate, and its original shape state is protected.

The device and the method provided by the invention overcome the deficiencies of the prior art, enable the lyophilized material to dynamically roll in the drum, fully and uniformly heat, and rapidly discharge the sublimation gas, thereby improving the drying efficiency and shortening the drying time of the material. The drying process is continued.

DRAWINGS

Figure 1 is a schematic view showing the structure of a conventional freeze-drying apparatus;

2 is a schematic diagram of the spray lyophilization apparatus provided in Example 1 when the material is continuously dried by a heating and drying device. Figure

3 is a schematic view showing the spray lyophilization apparatus provided in Example 2 using a heating and drying device to dry materials in batches.

detailed description

The invention is further illustrated below in conjunction with specific embodiments. It is to be understood that the examples are not intended to limit the scope of the invention. In addition, it should be understood that various changes and modifications may be made by those skilled in the art in the form of the present invention.

Example 1

2 is a schematic structural view of a heating and drying device for a spray freeze-drying device according to the embodiment, wherein the spray drying device for the spray freeze-drying device comprises: an outer tube 1, a feed tube 2, an air suction port 3, and a discharge port. 4 is a closed container for forming a confined space and protecting the material in the space from environmental pollution or polluting the environment; a rotary dryer composed of the drum 11, the rotating shaft 12, the motor 13, and at least one shaft seat, for the drum 11 To accommodate and dry the material, the rotating shaft 12 is used to transmit the rotational power of the motor 13 to the drum 11; a temperature-controlled circulating system composed of the rotary joint 21, the heat exchanger 22, the electric heater 23, and the fluid pump 24.

At least one hollow jacket 15 is disposed on the outer side of the rotating drum 11, and each hollow jacket 15 is provided with a fluid inlet and outlet pipe, and at least one fluid inlet and outlet pipe of the hollow jacket 15 is connected with the passage inside the rotating shaft 12, and is turned. All of the cylinder 11 and a part of the rotating shaft 12 are installed in the hermetic container; the rotating shaft 12 and the outer cylinder 1 are connected by a shaft seat; the other part of the rotating shaft 12 is connected to the motor 13 outside the hermetic container, and the internal passage and the rotary joint 21 of the portion The rotary joint 21 is a device for one side for fixed connection and one side for connecting the rotary shaft 12 and continuously conveying the fluid in the continuous or discontinuous rotational movement of the rotary shaft 12 without any interruption. The fluid introduced into the temperature control circulation system is silicone oil, and the silicone oil is heated by the electric heater 23 and regulated by the heat exchanger 22 and circulated by the fluid pump 24 to raise or lower the temperature of the jacket wall of the jacket 15.

The outer cylinder 1 draws a vacuum into the vessel through the suction port 3 before the device is dried, and the feed pipe 2 is connected to other devices through a valve to add the pre-frozen ice particles into the drum 11. The rotating drum 11 continuously rotates during the drying process, and the material is tumbling at the bottom of the rotating drum, and is uniformly and uniformly heated in contact with the cylinder wall; the guiding groove 14 rotates with the rotating drum to bring the material from the bottom of the rotating drum, and the material acts on the guiding groove by gravity. Slide in the direction of the discharge port 4, When the guiding groove continues to rotate with the rotating drum, the material falls by gravity to the bottom of the rotating cylinder; by controlling the feeding amount of the feeding pipe 2 and the rotation speed of the motor 13, the material is migrated to the discharging port 4 at an appropriate rate and evenly dispersed at the bottom of the rotating drum. Without accumulation, the sublimation gas is quickly discharged from the surface of the material and the gap between the particles, and is withdrawn through the suction port 3; the material is continuously tumbling through the rotating drum and gradually moving to the discharge port, and gradually drying in the drum until The completely dry drop into the discharge port 4 is transferred to the receiving tank or other device through the discharge valve. The heating and drying device continuously dries the material.

Example 2

3 is a schematic structural view of a heating and drying device for a spray freeze-drying device according to the embodiment, wherein the spray drying device uses a heating and drying device similar to that of Embodiment 1, except that the feed pipe 2 passes through a valve and the like. The device is connected to add a quantity of pre-frozen ice particles to the drum 11. During the feeding process, the rotating drum 11 rotates, and the material rolls at the bottom of the rotating drum. At this time, the temperature control circulating system does not heat; after the feeding is completed, the temperature control circulating system starts to heat, and the rotating drum 11 is driven by the motor 13 for a certain period of time and then reversed, after several times. The secondary rotation direction is switched, and the material is gradually dried in the drum; until the material to be added is completely dried, the drum is continuously rotated forward to discharge it. The heating and drying device dries the material in batches.

Claims

A heating and drying device for a spray freeze-drying device, comprising: an outer cylinder container for forming a sealed space; a rotary dryer portion for accommodating and dynamically heating the material is disposed in the outer cylinder container; for controlling the rotation The temperature control circulation system of the dryer heating temperature is connected to the rotary dryer.
A heating and drying device for a spray freeze-drying device according to claim 1, wherein the outer cylinder container is a closed container, comprising an outer cylinder (1), and the outer cylinder (1) is provided

a feed pipe (2) for adding the material to be dried to the rotary dryer;

The suction port (3) for evacuating the inside of the outer cylinder (1) and discharging the sublimation gas out of the outer cylinder (1) during the drying process;

And a discharge port (4) for discharging dry materials.
A heating and drying device for a spray freeze-drying device according to claim 2, wherein said rotary dryer comprises

a drum (11) for containing material;

a rotating shaft (12) for connecting the drum (11) to the motor (13);

The motor (13) for powering the rotation of the shaft (12).
A heating and drying device for a spray freeze-drying device according to claim 3, wherein a part of the rotating drum (11) and a part of the rotating shaft (12) are disposed in the outer cylindrical container, the rotating shaft Another part of (12) is connected to the motor (13) outside the outer cylinder container, and the rotating shaft (12) and the outer cylinder (1) are connected by a shaft seat.
A heating and drying device for a spray freeze-drying device according to claim 3, wherein at least one hollow jacket (15) is disposed outside the drum (11), and the hollow jacket (15) is fluid-passed. Warm or cool the wall of the barrel.
The heating and drying device for a spray freeze-drying device according to claim 5, wherein the inner wall of the rotating drum (11) is provided with at least one guiding groove (14) at an angle to the rotation center line of the rotating drum. When the drum (11) rotates in the forward direction, the material is guided by the guiding groove (14) to migrate toward the discharge port; when the drum (11) is rotated in the reverse direction, the material is brought back.
A heating and drying device for a spray freeze-drying device according to claim 6, wherein said temperature-controlled circulation system comprises a rotary joint (21), a heat exchanger (22), and electricity which are sequentially connected to form a closed loop. The heater (23) and the fluid pump (24) pass through the circulating fluid in the closed loop.
A heating and drying device for a spray freeze-drying device according to claim 7, wherein the rotating shaft (12) is internally provided with a passage for fluid circulation, and one side of the passage is inside the outer cylinder container. One or more hollow jackets (15) on the drum (11) are connected; the other side of the channel is connected to the rotary joint (21) outside the outer cylinder container; the rotary joint (21) is on the rotating shaft (12) The fluid in the closed loop is continuously transported within the hollow jacket (15) in any continuous or discontinuous rotational motion.
A heating and drying device for a spray freeze-drying device according to claim 7 or 8, wherein the drum (11) is provided with a detector for detecting material information, and the detector and the rotation The joint (21) is connected, and the rotary joint (21) continuously supplies electric current during any continuous or discontinuous rotational movement of the rotary shaft (12).
A method for heating and drying a spray freeze-drying device, comprising the heat drying device for a spray freeze-drying device according to any one of claims 6 to 9, wherein first, the inner container is evacuated and passed through a vacuum. The material pipe (2) adds the material pre-frozen into ice particles into the rotating drum (11); the temperature of the rotating drum (11) is controlled by the temperature-controlled circulation system; the rotating drum (11) continuously rotates during the drying process, and the material is in the rotating drum (11) The bottom is tumbling, and is uniformly and uniformly heated in contact with the cylinder wall; the guiding groove (14) is rotated with the rotating drum (11) to bring the material from the bottom of the rotating drum (11), and the material acts on the guiding groove (14) due to gravity. Slide to the discharge port (4). When the guide groove (14) continues to rotate with the drum, the material falls to the bottom of the rotary cylinder (11) due to gravity; by controlling the feed pipe feed amount and the motor (13) rotation speed, the material is Appropriate rate migrates to the discharge port (4) and evenly spreads at the bottom of the drum (11), without accumulation, the sublimation gas is quickly discharged from the material surface and the particle gap, and is pumped through the suction port (3); The revolving drum (11) rotates continuously and tumbling and progressively moves forward, in the drum (11) Gradually dry until completely dry and discharged through the discharge port (4).