Freeze drying device for strip-shaped decalcified bone matrix

The freeze-drying device, designed with multi-layer sample racks, gradient temperature control, and inert gas protection, solves the problems of low drying efficiency, uneven temperature control, and sample deformation in existing equipment, achieving a highly efficient and precise freeze-drying process and ensuring the bioactivity of the decalcified bone matrix and the quality of the finished product.

CN224162842UActive Publication Date: 2026-04-24SHANGHAI YAPENG BIOLOGICAL TECHNOLOGY CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
SHANGHAI YAPENG BIOLOGICAL TECHNOLOGY CO LTD
Filing Date
2025-03-26
Publication Date
2026-04-24

AI Technical Summary

Technical Problem

Existing freeze-drying equipment suffers from low drying efficiency, uneven temperature control, risk of sample deformation, and insufficient protection of activity in the processing of strip-shaped decalcified bone matrix, and is also highly complex to operate.

Method used

Employing a multi-layer sample holder, gradient temperature control design, inert gas protection, and an integrated control system, combined with a detachable sample holder and hydrophobic coating, it ensures efficient drying, precise temperature control, and morphological fixation, while reducing the risk of oxidation.

Benefits of technology

It achieves efficient drying, precise temperature control, sample morphology fixation, and bioactivity protection, improving production efficiency and product consistency while reducing operational complexity.

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Abstract

The utility model discloses a freeze-drying device for strip-shaped decalcified bone matrix, which comprises a drying chamber, a rack, a multi-layer sample rack, a cold trap, a compressor, a vacuum pump and a touch screen, the drying chamber is fixed at the top of the rack, the multi-layer sample rack and the cold trap are adjacently arranged in the drying chamber, and the compressor is fixed on the rack. The compressor, the vacuum pump and the touch screen are respectively arranged on the rack, the compressor is arranged close to the vacuum pump, the touch screen is arranged close to the drying chamber, a heating partition plate is further arranged at the bottom of the multi-layer sample rack, and a temperature sensor is arranged at the bottom of the heating partition plate. Efficient drying is achieved, the space utilization rate is increased through the multi-layer sample frame design, and the single-time handling capacity is greatly improved; the cold trap is directly connected with the compressor to shorten a condensation path, so that the drying period is shortened. Gradient temperature control is achieved through each layer of independent heating partition plate and a temperature sensor, and it is guaranteed that the strip-shaped gel is heated evenly, and the pore structure is complete. And the shape is fixed: the strip-shaped sample groove and the hydrophobic coating prevent gel deformation or adhesion.
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Description

Technical Field

[0001] This invention belongs to the technical field of biomaterial preparation equipment, specifically relating to a freeze-drying device for strip-shaped decalcified bone matrix. Background Technology

[0002] Decalcified bone matrix is ​​a commonly used bio-derived material in bone tissue engineering. Derived from bone tissue, it is a self-degrading, antigen-inactivated xenogeneic or allogeneic bone. Furthermore, decalcified bone exhibits good biocompatibility, bioactivity, and biodegradability, and readily fuses with surrounding bone, supporting the growth of new bone tissue. Decalcified bone also retains its natural network porosity system, making its structure and composition more physiologically compatible with human needs.

[0003] Decalcified bone matrix (DBM) gel is an important bone repair material, and its preparation requires freeze-drying to remove moisture and form a porous structure. Existing freeze-drying equipment suffers from the following problems in processing strip-shaped DBM gels: Low drying efficiency: Traditional equipment uses a single-layer sample holder, resulting in low space utilization, small batch throughput, and insufficient condensation efficiency due to the large distance between the cold trap and the drying chamber, prolonging the drying cycle. Uneven temperature control: Existing equipment relies on a single temperature sensor, making it difficult to monitor the temperature gradient of multiple sample layers in real time, leading to localized overheating or overcooling and damaging the gel structure. Risk of sample deformation: Ordinary sample holders lack a fixing design, and strip-shaped gels are prone to curling or sticking together in a vacuum environment, affecting the shape and pore uniformity of the finished product. Operational complexity: Low equipment integration; components such as vacuum pumps and cold traps require manual coordination, making operation cumbersome and prone to contamination. Insufficient activity protection: The lack of inert gas protection during drying allows residual oxygen to potentially cause oxidative degradation of the gel, reducing biocompatibility. Furthermore, existing improved freeze-drying equipment is not specifically designed to adapt to the morphology and material properties of strip-shaped DBM gels.

[0004] Therefore, there is an urgent need for a specialized device that can achieve efficient drying, precise temperature control, and shape fixation. Utility Model Content

[0005] In view of the problems mentioned in the background art, the purpose of this utility model is to provide a freeze-drying device for strip-shaped decalcified bone matrix, which solves the problems of low efficiency, sample deformation and activity loss of existing equipment through multi-layer sample rack, gradient temperature control and inert gas protection design.

[0006] To achieve the above-mentioned technical objectives, the technical solution adopted by this utility model is as follows:

[0007] A freeze-drying apparatus for strip-shaped decalcified bone matrix includes a drying chamber, a frame, a multi-layer sample rack, a cold trap, a compressor, a vacuum pump, and a touch screen. The drying chamber is fixed to the top of the frame. The multi-layer sample rack and the cold trap are arranged adjacent to each other inside the drying chamber. The compressor, vacuum pump, and touch screen are respectively mounted on the frame. The compressor is positioned close to the vacuum pump, and the touch screen is positioned close to the drying chamber. A heating partition is also provided at the bottom of the multi-layer sample rack, and a temperature sensor is provided at the bottom of the heating partition.

[0008] Furthermore, the multi-layer sample holder is a detachable design, with each layer having a strip-shaped sample groove. The inner wall of the sample groove is covered with a hydrophobic coating, and the spacing between adjacent sample grooves is 2-5 mm. This structural design can be used to fix the morphology of strip-shaped decalcified bone matrix gel.

[0009] Further specified, the cold trap is located on the right side of the drying chamber, the cold trap is connected to the compressor through a ring pipe, the temperature of the cold trap is -60℃ to -80℃, and its condensation area is ≥0.5㎡.

[0010] Further specified, the vacuum pump is connected to the drying chamber and the cold trap via a three-way valve, and the vacuum level of the vacuum pump can be adjusted to 0.01-0.1 mbar.

[0011] Furthermore, the touchscreen integrates a PLC controller for real-time display of the drying chamber temperature, vacuum level, and cold trap status.

[0012] Furthermore, the rack sidewall is provided with an inert gas filling valve, which is connected to the drying chamber pipeline. The inert gas filling valve can fill nitrogen or argon during the drying process and maintain the oxygen concentration <1%.

[0013] Further specified, the heating partition is an aluminum honeycomb structure, with heating wires evenly distributed on the surface of the heating partition, and its heating temperature range is -40℃ to 50℃, with a temperature control accuracy of ±0.5℃.

[0014] Further specifying, the front side of the drying chamber is provided with a door and a connector, the door is connected to the side wall of the drying chamber through the connector, the edge of the door is embedded with a sealing ring, the door is equipped with an observation port and a handle, and the observation port is double-layered anti-fog glass.

[0015] The beneficial effects of this utility model are:

[0016] 1. High-efficiency drying: The multi-layer sample rack design improves space utilization and significantly increases the single-batch processing capacity; the direct connection between the cold trap and the compressor shortens the condensation path, thus shortening the drying cycle.

[0017] 2. Precise temperature control: Each layer has an independent heating partition and temperature sensor to achieve gradient temperature control, ensuring that the strip gel is heated evenly and the pore structure is intact.

[0018] 3. Fixed shape: The strip-shaped sample groove and hydrophobic coating prevent gel deformation or adhesion, and the shape consistency of the finished product reaches more than 98%.

[0019] 4. Activity protection: The inert gas filling valve reduces the risk of oxidation, and the retention rate of gel bioactivity is increased to over 95%.

[0020] 5. Easy to operate: Integrated control via touch screen, one-button start of gradient drying mode, reducing manual intervention and improving production efficiency and quality stability. Attached Figure Description

[0021] This utility model can be further illustrated by the non-limiting embodiments given in the accompanying drawings;

[0022] Figure 1 This is a front view of an embodiment of a freeze-drying apparatus for strip-shaped decalcified bone matrix according to the present invention;

[0023] Figure 2 This is a side view of an embodiment of a freeze-drying apparatus for strip-shaped decalcified bone matrix according to the present invention.

[0024] The symbols for the main components are as follows: 1. Drying chamber; 2. Frame; 3. Multi-layer sample rack; 4. Cold trap; 5. Door; 6. Connector; 7. Handle; 8. Observation port; 9. Compressor; 10. Vacuum pump; 11. Touch screen; 12. Inert gas filling valve; 13. Heating partition; 14. Temperature sensor. Detailed Implementation

[0025] In the description of this utility model, it should be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicating orientation or positional relationships based on the orientation or positional relationships shown in the accompanying drawings, are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model. Furthermore, the terms "first," "second," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, features defined with "first," "second," etc., may explicitly or implicitly include one or more of that feature. In the description of this utility model, unless otherwise stated, "a plurality of" means two or more.

[0026] In the description of this utility model, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0027] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0028] Example 1: As Figure 1 As shown, the present invention discloses a freeze-drying device for strip-shaped decalcified bone matrix, comprising a drying chamber 1, a frame 2, a multi-layer sample rack 3, a cold trap 4, a compressor 9, a vacuum pump 10, and a touch screen 11. The drying chamber 1 is fixed to the top of the frame 2. The multi-layer sample rack 3 and the cold trap 4 are arranged adjacent to each other inside the drying chamber 1. The compressor 9, the vacuum pump 10, and the touch screen 11 are respectively arranged on the frame 2. The compressor 9 is arranged close to the vacuum pump 10, and the touch screen 11 is arranged close to the drying chamber 1. The bottom of the multi-layer sample rack 3 is also provided with a heating partition 13, and the bottom of the heating partition 13 is provided with a temperature sensor 14.

[0029] In the practical application of this embodiment, the multi-layer sample holder 3 is a detachable design, with each layer having a strip-shaped sample groove. The inner wall of the sample groove is covered with a hydrophobic coating, and the spacing between adjacent sample grooves is 2-5 mm. This structural design can be used to fix the morphology of strip-shaped decalcified bone matrix gel.

[0030] In the practical application of this embodiment, the cold trap 4 is located on the right side of the drying chamber 1. The cold trap 4 is connected to the compressor 9 through an annular pipeline. The temperature of the cold trap 4 is -60℃ to -80℃, and its condensation area is ≥0.5㎡.

[0031] In the practical application of this embodiment, the vacuum pump 10 is connected to the drying chamber 1 and the cold trap 4 via a three-way valve, and the vacuum degree of the vacuum pump 10 can be adjusted to 0.01-0.1 mbar. Specifically, the vacuum pump is equipped with a pressure feedback system, which can provide real-time feedback on the current pressure value to avoid poor product quality due to excessive or insufficient pressure.

[0032] In the practical application of this embodiment, the touch screen 11 integrates a PLC controller for real-time display of the temperature, vacuum level, and status of the cold trap 4 in the drying chamber 1. The PLC controller has a preset "gradient drying mode" in the touch screen 11, which supports segmented temperature control.

[0033] In the practical application of this embodiment, an inert gas filling valve 12 is provided on the side wall of the frame 2. The inert gas filling valve 12 is connected to the pipeline of the drying chamber 1. The inert gas filling valve 12 can fill nitrogen or argon during the drying process and maintain the oxygen concentration <1%.

[0034] In the practical application of this embodiment, the heating partition 13 is an aluminum honeycomb structure, and the heating wires are evenly distributed on the surface of the heating partition 13. Its heating temperature range is -40℃ to 50℃, and the temperature control accuracy is ±0.5℃.

[0035] In the practical application of this embodiment, the front side of the drying chamber 1 is provided with a door 5 and a connector 6. The door 5 is connected to the side wall of the drying chamber 1 through the connector 6. The edge of the door 5 is embedded with a sealing ring. The door 5 is equipped with an observation port 8 and a handle 7. The observation port 8 is a double-layer anti-fog glass.

[0036] The assembly process of the device in this embodiment is as follows:

[0037] The frame 2 is fixed to the ground, the drying chamber 1 is embedded in the frame 2, and the cold trap 4 is connected to the inside of the drying chamber through a flange. A multi-layer sample rack 3 is installed, with each layer connected by welding to ensure a levelness error of <0.1mm. The vacuum pump 10 is connected to the cold trap 4 and the drying chamber 1 through pressure-resistant pipelines. After installation, its sealing performance is tested.

[0038] Operating procedures:

[0039] Open the chamber door 5, spread the strip-shaped DBM gel evenly in the sample chamber, close the chamber door 5, and set the drying parameters via the touch screen 11: for example, pre-freezing stage -40℃ for 2 hours, sublimation stage -10℃ with a vacuum of 0.05 mbar, and desorption stage 25℃ for 4 hours. Activate the inert gas filling valve 12 to fill with nitrogen until the oxygen concentration is <1%, monitor the temperature sensor 14 data in real time, and adjust the power of the heating partition 13 to ensure that the temperature difference between each layer is <1℃.

[0040] Example 2:

[0041] The similarities between this embodiment and Embodiment 1 will not be repeated here. The difference is that, in this embodiment, for high-viscosity gels, the sample groove spacing is adjusted to 5 mm, and argon gas is introduced in the later stage of drying to further reduce oxidation.

[0042] The above embodiments are merely illustrative of the principles and effects of this utility model and are not intended to limit the scope of this utility model. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of this utility model. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in this utility model should still be covered by the claims of this utility model.

Claims

1. A freeze-drying apparatus for strip-shaped decalcified bone matrix, characterized in that: The device includes a drying chamber (1), a frame (2), a multi-layer sample rack (3), a cold trap (4), a compressor (9), a vacuum pump (10), and a touch screen (11). The drying chamber (1) is fixed to the top of the frame (2). The multi-layer sample rack (3) and the cold trap (4) are arranged adjacent to each other inside the drying chamber (1). The compressor (9), the vacuum pump (10), and the touch screen (11) are respectively arranged on the frame (2). The compressor (9) is arranged close to the vacuum pump (10), and the touch screen (11) is arranged close to the drying chamber (1). The bottom of the multi-layer sample rack (3) is also provided with a heating baffle (13), and the bottom of the heating baffle (13) is provided with a temperature sensor (14).

2. The freeze-drying apparatus for strip-shaped decalcified bone matrix according to claim 1, characterized in that: The multi-layer sample rack (3) is detachable. Each layer of the sample rack is provided with a strip-shaped sample groove. The inner wall of the sample groove is covered with a hydrophobic coating, and the distance between adjacent sample grooves is 2-5mm.

3. The freeze-drying apparatus for strip-shaped decalcified bone matrix according to claim 1, characterized in that: The cold trap (4) is located on the right side of the drying chamber (1). The cold trap (4) is connected to the compressor (9) through a ring pipe. The temperature of the cold trap (4) is -60℃ to -80℃, and its condensation area is ≥0.5㎡.

4. The freeze-drying apparatus for strip-shaped decalcified bone matrix according to claim 1, characterized in that: The vacuum pump (10) is connected to the drying chamber (1) and the cold trap (4) via a three-way valve. The vacuum level of the vacuum pump (10) can be adjusted to 0.01-0.1 mbar.

5. The freeze-drying apparatus for strip-shaped decalcified bone matrix according to claim 1, characterized in that: The touch screen (11) integrates a PLC controller for real-time display of the temperature, vacuum level, and status of the cold trap (4) in the drying chamber (1).

6. The freeze-drying apparatus for strip-shaped decalcified bone matrix according to claim 1, characterized in that: An inert gas filling valve (12) is provided on the side wall of the frame (2). The inert gas filling valve (12) is connected to the drying chamber (1) pipe. The inert gas filling valve (12) can fill nitrogen or argon during the drying process and maintain the oxygen concentration <1%.

7. The freeze-drying apparatus for strip-shaped decalcified bone matrix according to claim 1, characterized in that: The heating baffle (13) is an aluminum honeycomb structure. The heating baffle (13) has heating wires evenly distributed on its surface. Its heating temperature range is -40℃ to 50℃, and the temperature control accuracy is ±0.5℃.

8. The freeze-drying apparatus for strip-shaped decalcified bone matrix according to claim 1, characterized in that: The front side of the drying chamber (1) is provided with a door (5) and a connector (6). The door (5) is connected to the side wall of the drying chamber (1) through the connector (6). The edge of the door (5) is inlaid with a sealing ring. The door (5) is equipped with an observation port (8) and a handle (7). The observation port (8) is a double-layer anti-fog glass.