High-vacuum freeze dryer for pharmaceutical chemical industry

Through the series vacuum separation assembly and secondary vacuum pump technology of the high-vacuum freeze dryer, the problem that existing freeze dryers are difficult to quickly remove water and solvents in drugs is solved, and an efficient freeze-drying process is achieved, which improves production efficiency and drug quality.

CN120488642APending Publication Date: 2025-08-15孙泽洋
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Patent Information

Application Number
CN202510881042.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-27
Publication Date
2025-08-15

AI Technical Summary

Technical Problem

When existing lyophilized machines deal with drugs containing water and solvents, they cannot quickly remove solvents, resulting in extended lyophilized procedures, reduced production efficiency, and potential impact on drug quality.

Method used

Using a high vacuum freeze dryer, the vacuum degree of the lyophilization chamber is increased to ≤0.05Pa through a series vacuum separation assembly and a secondary vacuum pump, and combined with a solvent collection tank and heater, the efficient removal of moisture and solvent is achieved.

Benefits of technology

The preparation time of freeze-dried products is shortened, production efficiency is improved, and the potential impact of solvent residues on drug quality is reduced.

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Abstract

The invention belongs to the technical field of freeze drying, and particularly relates to a pharmaceutical chemical high-vacuum freeze dryer which comprises a freeze vacuum dryer body, the lower end of a cavity of a condenser of the freeze vacuum dryer body is connected with a solvent collecting tank in a penetrating mode, and a tandem type vacuum separation assembly is arranged on the freeze vacuum dryer body. The tandem type vacuum separation assembly comprises a secondary vacuum pump, the secondary vacuum pump is arranged between the vacuum pump and the condenser of the freezing vacuum dryer, and the pumping-in end of the secondary vacuum pump is connected with the condenser of the freezing vacuum dryer through a first pipeline. The output end of the secondary vacuum pump is connected with the vacuum pump input end of the freezing vacuum dryer through a second pipeline; when the vacuum pump vacuumizes the freeze-drying chamber to be smaller than or equal to 10 pa, the secondary vacuum pump is controlled to be started to vacuumize the freeze-drying chamber to be smaller than or equal to 0.05 pa, the freeze-drying chamber reaches high vacuum through secondary vacuum, moisture and dissolution in a freeze-dried product are reduced, the preparation time of the product is shortened, and the working efficiency is improved.
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Description

Technical Field

[0001] The invention belongs to the technical field of freeze drying, and in particular relates to a high vacuum freeze drying machine for pharmaceutical and chemical industries. Background Art

[0002] A vacuum freeze dryer, or freeze dryer for short, consists of a freeze drying chamber, condenser, vacuum pump unit, refrigeration compressor unit, heating device, and control system. This advanced equipment utilizes a vacuum environment and low temperatures to freeze the water in water-containing materials into ice, then sublimates the ice directly into water vapor under vacuum conditions, thereby drying the material. Its ability to maximize the preservation of active ingredients, structure, and appearance of materials has led to its critical applications in the pharmaceutical and chemical industries.

[0003] Currently, freeze dryers on the market perform well in terms of water removal capabilities, generally meeting the typical water removal requirements of most products. However, in the pharmaceutical industry, a field with extremely stringent product quality and process requirements, the situation is different. During the production process of many pharmaceuticals, raw materials or intermediates contain solvents such as ethanol in addition to water. When processing such products, traditional freeze dryers generally follow a sequential process of removing water first and then removing solvents.

[0004] Furthermore, while freeze dryers currently on the market claim to achieve relatively low vacuum levels, in practice they typically operate at 0.3 Pa. However, at this vacuum level, they are unable to quickly remove the solvent from products containing both water and solvents. This results in a longer freeze-drying process and reduced production efficiency. Furthermore, prolonged solvent residues may potentially impact drug quality. Summary of the Invention

[0005] In order to solve the above problems, the present invention proposes a high vacuum freeze dryer for pharmaceutical and chemical industries.

[0006] The technical solution adopted by the present invention is as follows: The present invention provides a high vacuum freeze dryer for pharmaceutical and chemical industries, comprising a freeze vacuum dryer, wherein the lower end of the cavity of the condenser of the freeze vacuum dryer is connected through a solvent collection tank, the freeze vacuum dryer is provided with a series vacuum separation component, the series vacuum separation component includes a secondary vacuum pump, a secondary vacuum pump is provided between the vacuum pump and the condenser of the freeze vacuum dryer, the suction end of the secondary vacuum pump is connected to the condenser of the freeze vacuum dryer through a first pipe, the output end of the secondary vacuum pump is connected to the vacuum pump input end of the freeze vacuum dryer through a second pipe, one end of a first vacuum tube is connected through the outer wall of the first tube, the other end of the first vacuum tube is connected through the outer wall of the second tube, and the first vacuum tube is provided with a solenoid valve.

[0007] Furthermore, one end of the coil of the condenser of the freeze vacuum dryer is connected to one end of the third pipe, the other end of the third pipe is connected to the input end of the circulation pump, the output end of the circulation pump is connected to one side of the cavity, the other side of the cavity is connected to one end of the fourth pipe, the other pipe of the fourth pipe is connected to the other end of the coil of the condenser of the freeze vacuum dryer, and a heater is provided in the cavity, and the heater is connected to the compressor.

[0008] Furthermore, a first check valve is provided in the first pipeline.

[0009] Furthermore, a second check valve is provided in the second pipeline.

[0010] The beneficial effects achieved by the present invention using the above structure are as follows: When the vacuum pump draws the vacuum of the freeze-drying chamber to ≤10Pa, the secondary vacuum pump is controlled to draw the vacuum of the freeze-drying chamber to ≤0.05Pa. The secondary vacuum is used to make the freeze-drying chamber reach high vacuum, shortening the time for removing moisture and dissolving the freeze-dried product, shortening the product preparation time, and improving work efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] In order to more clearly illustrate the technical solution of the present invention, the following is a brief introduction to the drawings required for the description. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0012] Figure 1 This is a structural schematic diagram of a high vacuum freeze dryer for pharmaceutical and chemical industries according to the present invention.

[0013] Among them, 1. solvent collection tank, 2. secondary vacuum pump, 3. solenoid valve, 4. first vacuum tube, 5. freeze vacuum dryer, 6. compressor, 7. circulation pump, 9. heater, 10. cavity. DETAILED DESCRIPTION

[0014] In order to make the purpose, features, and advantages of the present invention more obvious and easy to understand, the technical solutions of the present invention will be clearly and completely described below in conjunction with the drawings in this specific embodiment. Obviously, the embodiments described below are only part of the embodiments of the present invention, not all of them. Based on the embodiments in this patent, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of this patent.

[0015] like Figure 1As shown, the present invention proposes a high vacuum freeze dryer for pharmaceutical and chemical industries, comprising a freeze vacuum dryer 5, wherein the lower end of the cavity of the condenser of the freeze vacuum dryer 5 is connected to the solvent collection tank 1 through a through hole, and the freeze vacuum dryer 5 is provided with a series vacuum separation component, which includes a secondary vacuum pump 2, and a secondary vacuum pump 2 is provided between the vacuum pump and the condenser of the freeze vacuum dryer 5. The suction end of the secondary vacuum pump 2 is connected to the condenser of the freeze vacuum dryer 5 through a first pipe, and the output end of the secondary vacuum pump 2 is connected to the vacuum pump input end of the freeze vacuum dryer 5 through a second pipe. The outer wall of the first pipe is connected to the first vacuum pipe. 4, the outer side wall of the second pipe is connected to the other end of the first vacuum tube 4, the first vacuum tube 4 is provided with a solenoid valve 3, one end of the coil of the condenser of the frozen vacuum dryer 5 is connected to one end of the third pipe, the other end of the third pipe is connected to the input end of the circulating pump 7, the output end of the circulating pump 7 is connected to one side of the cavity 10, the other side of the cavity 10 is connected to one end of the fourth pipe, the other pipe of the fourth pipe is connected to the other end of the coil of the condenser of the frozen vacuum dryer 5, a heater 9 is provided in the cavity 10, the heater 9 is connected to the compressor 6, a first check valve is provided in the first pipe, and a second check valve is provided in the second pipe.

[0016] When in use, the medicine to be freeze-dried is placed in the freezing chamber of the freeze vacuum dryer 5, and the freeze vacuum dryer 5 is started (the solenoid valve 3 is in the open state at this time). The air in the freezing chamber enters the condenser, and a large amount of solvent is vacuumed into the collection tank 1 and then discharged; it is pumped out by the vacuum pump of the freeze vacuum dryer 5. When the vacuum in the freezing chamber of the freeze vacuum dryer 5 is pumped to ≤10Pa, the secondary vacuum pump 2 is started, and the solenoid valve 3 is closed at the same time. The vacuum in the freezing chamber is pumped to ≤0.05Pa by the secondary vacuum pump 2 and the vacuum pump of the freeze vacuum dryer 5, and the secondary vacuum pump is used to pump the solvent into the collection tank 1. The air makes the freeze-drying chamber reach high vacuum, and the moisture in the product in the freeze-drying chamber and the small amount of solvent contained in it condense into frost after the condenser. When the frost in the condenser reaches a certain amount and affects the vacuum degree of the equipment, the valve between the freeze-drying chamber and the condenser is closed, and the condenser is turned on to defrost the frost state. The melted ice water enters the solvent collection tank 1 and is discharged, shortening the removal of moisture and dissolution of the freeze-dried product, shortening the product preparation time, and improving work efficiency. The setting of the first check valve and the second check valve prevents the gas from flowing back into the condenser. The above is the overall working process of the present invention. You can repeat this step when you use it next time.

[0017] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A high vacuum freeze dryer for pharmaceutical and chemical industries, comprising a freeze vacuum dryer (5), characterized in that: The lower end of the cavity of the condenser of the freeze vacuum dryer (5) is connected to the solvent collection tank (1). The freeze vacuum dryer (5) is provided with a series vacuum separation component, and the series vacuum separation component includes a secondary vacuum pump (2). A secondary vacuum pump (2) is provided between the vacuum pump of the freeze vacuum dryer (5) and the condenser. The suction end of the secondary vacuum pump (2) is connected to the condenser of the freeze vacuum dryer (5) through a first pipe, and the output end of the secondary vacuum pump (2) is connected to the vacuum pump input end of the freeze vacuum dryer (5) through a second pipe. One end of the first vacuum tube (4) is connected to the outer wall of the first pipe, and the other end of the first vacuum tube (4) is connected to the outer wall of the second pipe. The first vacuum tube (4) is provided with a solenoid valve (3).

2. A high vacuum freeze dryer for pharmaceutical and chemical industry according to claim 1, characterized in that: One end of the coil of the condenser of the freeze vacuum dryer (5) is connected to one end of the third pipe, the other end of the third pipe is connected to the input end of the circulation pump (7), the output end of the circulation pump (7) is connected to one side of the cavity (10), the other side of the cavity (10) is connected to one end of the fourth pipe, the other end of the fourth pipe is connected to the other end of the coil of the condenser of the freeze vacuum dryer (5), a heater (9) is provided in the cavity (10), and the heater (9) is connected to the compressor (6).

3. A high vacuum freeze dryer for pharmaceutical and chemical industry according to claim 2, characterized in that: A first check valve is provided in the first pipeline.

4. A high vacuum freeze dryer for pharmaceutical and chemical use according to claim 3, characterized in that: A second check valve is provided in the second pipeline.