CN110547969A - Production process and equipment of high-specific-surface-area nano slow-release micro powder - Google Patents
Production process and equipment of high-specific-surface-area nano slow-release micro powder Download PDFInfo
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- CN110547969A CN110547969A CN201910837141.1A CN201910837141A CN110547969A CN 110547969 A CN110547969 A CN 110547969A CN 201910837141 A CN201910837141 A CN 201910837141A CN 110547969 A CN110547969 A CN 110547969A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
- A61J3/02—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of powders
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J2200/00—General characteristics or adaptations
- A61J2200/40—Heating or cooling means; Combinations thereof
- A61J2200/44—Cooling means
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J2200/00—General characteristics or adaptations
- A61J2200/70—Device provided with specific sensor or indicating means
- A61J2200/72—Device provided with specific sensor or indicating means for temperature
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- Chemical & Material Sciences (AREA)
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- Pharmacology & Pharmacy (AREA)
- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicinal Preparation (AREA)
- Drying Of Solid Materials (AREA)
Abstract
The invention particularly discloses a production process and equipment of nano slow-release micro powder with high specific surface area. The production equipment comprises a powder quick-freezing system and a freeze-drying system, wherein the powder quick-freezing system comprises an ultralow temperature environment box, and a refrigerant chamber is arranged in the ultralow temperature environment box; the top of the ultra-low temperature environment box is provided with a quick-freezing groove, the bottom of the quick-freezing groove extends into the refrigerant chamber, and a tray is arranged in the quick-freezing groove; the powder quick-freezing system also comprises a powder spraying module, wherein the powder spraying module comprises a longitudinal guide rail arranged at the top of the ultralow-temperature environment box and a cross beam arranged above the quick-freezing groove; the transverse beam is connected with the longitudinal guide rail, and the longitudinal guide rail is provided with a first driving device for driving the transverse beam to move; the crossbeam is connected with a spray head mounting seat and a second driving device for driving the spray head mounting seat to move. The production process and the production equipment have high production efficiency and stable product quality.
Description
Technical Field
The invention relates to a production process and equipment of nano slow-release micro powder with high specific surface area.
background
The polypeptide biological medicine has the advantages of high biological activity, no toxic or side effect after degradation, direct administration and the like, but the blood concentration is influenced by the administration dosage form and the administration route, and a slow-release dosage form or the administration route needs to be found. Experiments prove that when the specific surface area of the medicine is increased, the dissolution performance of the medicine is reduced, and the medicine can play a role in slow release. The nanometer slow release granule preparation is developed in the industry at present, is administrated through a nasal cavity breathing mode, has good absorption, and can slowly release the peak value of blood concentration to play a slow release role.
The invention aims to provide a process and equipment for efficiently and stably producing high-specific-surface-area nano slow-release micro powder.
Disclosure of Invention
The invention aims to solve the technical problem of providing a production process and equipment of nano slow-release micro powder with high specific surface area, high production efficiency and stable product quality.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a production device of nano slow-release micro powder with high specific surface area comprises a powder quick-freezing system and a freeze-drying system, wherein the powder quick-freezing system comprises an ultralow temperature environment box, a closed refrigerant chamber is arranged in the ultralow temperature environment box, and the refrigerant chamber is provided with a refrigerant inlet and a refrigerant outlet; the top of the ultra-low temperature environment box is provided with a quick-freezing groove, the bottom of the quick-freezing groove extends into the refrigerant chamber, a tray is arranged in the quick-freezing groove, and the tray and the quick-freezing groove are arranged in a split manner; the powder quick-freezing system also comprises a powder spraying module, the powder spraying module comprises a powder storage tank and a spray head connected with a pipeline of the powder storage tank, and the spray head is provided with a control valve for controlling the spray head to work; the powder spraying module also comprises a longitudinal guide rail arranged at the top of the ultra-low temperature environment box and a cross beam arranged above the quick-freezing groove and arranged along the width direction of the quick-freezing groove, and the longitudinal guide rail extends along the length direction of the quick-freezing groove; the transverse beam is connected with the longitudinal guide rail, and the longitudinal guide rail is provided with a first driving device for driving the transverse beam to move along the length direction of the longitudinal guide rail; the cross beam is connected with a spray head mounting seat and a second driving device for driving the spray head mounting seat to move along the length direction of the cross beam; the freeze drying system comprises a vacuum drying oven.
The refrigerant chamber is stored in the refrigerant chamber, an ultralow temperature environment is created, the tray is cooled, and conditions are created for quick freezing of materials. The coolant is usually liquid nitrogen or other ultralow-temperature materials, a coolant inlet is used for introducing liquid coolant, and a coolant outlet is used for discharging gasified coolant. The powder in the powder storage tank is atomized by the spray head and sprayed out, and is rapidly condensed when contacting with the tray in a low-temperature state, and the product is obtained after freeze drying. The arrangement of the longitudinal guide rails and the cross beams realizes the orderly automatic movement of the spray head relative to the tray, improves the efficiency of spraying materials, and simultaneously improves the uniformity of material distribution in the tray, thereby ensuring the product quality.
preferably, the refrigerant chamber is provided with an insulating layer.
Preferably, the ultra-low temperature environment box is further provided with a temperature sensor for monitoring the indoor temperature of the refrigerant.
preferably, the bottom of the refrigerant chamber is provided with a discharge valve for discharging the refrigerant remaining in the refrigerant chamber after the completion of the processing.
Preferably, the first driving device and the second driving device respectively comprise a motor and a synchronous belt driven by the motor.
Preferably, the nozzle mounting seat is provided with a temperature sensor, and the temperature sensor controls the opening and closing of the control valve according to the temperature of the product in the tray.
Preferably, the bottom of the tray is in close contact with the bottom surface of the quick-freezing tank, so that the freezing efficiency is improved, and the uniformity of the temperature distribution of the tray is ensured.
the production process of the high-specific-surface-area nanometer slow-release micro powder based on the production equipment at least comprises the following steps:
Step one, raw material pretreatment: dissolving and diluting the raw materials to be processed, and then performing filter pressing on the raw materials into a powder storage tank;
Step two-speed freeze spraying: injecting a coolant with the temperature not higher than-100 ℃ into a refrigerant chamber, and precooling the tray until the temperature of the tray is not higher than-5 ℃;
Starting the first driving device and the second driving device, then starting the control valve, enabling the spray head and the cross beam to move relative to the tray respectively, and in the second process, enabling the spray head to perform scanning type material spraying in the tray, and enabling the raw materials sprayed to the tray to be rapidly condensed in an ultralow-temperature environment;
After the spraying is finished, the control valve is closed, and the cross beam and the spray head mounting seat are reset;
step three, freeze drying: pre-cooling the raw materials by a freeze dryer until the temperature in a vacuum drying box is 0 to-65 ℃, placing a tray loaded with the frozen raw materials in the vacuum drying box, and preserving heat and drying for at least 7 hours.
Preferably, the temperature of the refrigerant is not higher than-150 ℃, and the temperature of the tray in the quick-freezing spraying process is-5 ℃ to-35 ℃.
Preferably, during the quick-freezing spraying process, the thickness of the frozen powder in the tray is not more than 1.5 cm.
Drawings
FIG. 1 is a sectional view of a powder quick-freezing system in the production equipment for the nanometer slow-release micropowder with high specific surface area in the present embodiment;
Fig. 2 is a schematic structural diagram of a powder quick-freezing system in the production equipment for the nanometer slow-release micro powder with high specific surface area.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Examples
As shown in figures 1 and 2, the production equipment for the nano slow-release micro powder with the high specific surface area comprises a powder quick-freezing system and a freeze-drying system, wherein the powder quick-freezing system comprises an ultralow temperature environment box 3, a closed refrigerant chamber 5 is arranged in the ultralow temperature environment box 3, the refrigerant chamber 5 is provided with a refrigerant inlet and a refrigerant outlet, and the refrigerant chamber 5 is provided with a heat insulation layer 4. The ultra-low temperature environment box 3 is also provided with a temperature sensor for monitoring the temperature in the refrigerant chamber 5. The bottom of the refrigerant chamber 5 is provided with a discharge valve 33 for discharging the refrigerant remaining in the refrigerant chamber 5 after the process is completed.
As shown in fig. 1 and 2, a quick-freezing groove 6 is arranged at the top of the ultra-low temperature environment box 3, the bottom of the quick-freezing groove 6 extends into the refrigerant chamber 5, a tray 8 is arranged in the quick-freezing groove 6, the tray 8 and the quick-freezing groove 6 are arranged in a split manner, the bottom of the tray 8 is in close contact with the bottom surface of the quick-freezing groove 6, the freezing efficiency is improved, and the uniformity of the temperature distribution of the tray 8 is ensured. The refrigerant chamber 5 is stored in the refrigerant chamber 5, an ultralow temperature environment is created, the tray 8 is cooled, and conditions are created for quick freezing of materials.
as shown in fig. 1 and 2, the powder quick-freezing system further comprises a powder spraying module, the powder spraying module comprises a powder storage tank 1 and a spray head 2 connected with the powder storage tank 1 through a pipeline, and a control valve 33 used for controlling the spray head 2 to work is arranged on the spray head 2. The nozzle mounting base 10 is provided with an infrared sensor, and the infrared sensor controls the opening and closing of the control valve 33 according to the temperature of the product in the tray 8.
as shown in fig. 1 and 2, the powder spraying module further comprises a longitudinal guide rail 9 arranged at the top of the ultra-low temperature environment box 3, and a cross beam 7 arranged above the quick-freezing tank 6 and arranged along the width direction of the quick-freezing tank 6, wherein the longitudinal guide rail 9 extends along the length direction of the quick-freezing tank 6. The beam 7 is connected with the longitudinal guide rail 9, and the longitudinal guide rail 9 is provided with a first driving device 91 for driving the beam 7 to move along the length direction of the longitudinal guide rail 9. The cross beam 7 is connected with a nozzle mounting base 10 and a second driving device 71 for driving the nozzle mounting base 10 to move along the length direction of the cross beam 7. The first driving device 91 and the second driving device 71 respectively comprise a motor and a synchronous belt driven by the motor. The arrangement of the longitudinal guide rails 9 and the cross beams 7 realizes the orderly automatic movement of the spray head 2 relative to the tray 8, improves the efficiency of spraying materials, and simultaneously improves the uniformity of material distribution in the tray 8, thereby ensuring the product quality.
The freeze drying system comprises a vacuum drying machine, and the freeze drying machine comprises a drying box, a condenser, a freezing unit, a vacuum pump and a cooling device. Since the freeze drying system is the prior art, the present application is directed to improvements in freeze drying systems, and therefore, will not be described herein.
The production process of the high-specific-surface-area nanometer slow-release micro powder based on the production equipment at least comprises the following steps:
step one, raw material pretreatment: dissolving and diluting the raw materials to be processed, and then filter-pressing the raw materials into a powder storage tank 1 through a 0.22 micron filter membrane.
Step two-speed freeze spraying: a coolant with the temperature not higher than-100 ℃ is selected to be injected into the refrigerant chamber 5 to pre-cool the tray 8, the temperature of the refrigerant is preferably not higher than-150 ℃, and liquid nitrogen is usually adopted as the refrigerant; until the temperature of the tray 8 is not higher than-5 ℃, the temperature of the tray 8 is preferably-5 ℃ to-35 ℃;
starting the first driving device 91 and the second driving device 71, then starting the control valve 33, enabling the spray head 2 and the cross beam 7 to respectively move relative to the tray 8, and in the second process, enabling the spray head 2 to perform scanning type material spraying in the tray 8, enabling the raw material sprayed to the tray 8 to be rapidly condensed in an ultralow temperature environment, wherein in the quick-freezing spraying process, the thickness of the frozen powder in the tray 8 is not more than 1.5 cm; after the material spraying is finished, the control valve 33 is closed, and the cross beam 7 and the nozzle mounting base 10 are reset.
Step three, freeze drying: pre-cooling by a freeze dryer until the temperature in a vacuum drying box is 0 to-65 ℃, placing a tray 8 loaded with the frozen raw materials in the vacuum drying box, and performing heat preservation and drying for at least 7 hours; packing the solid active components in the freeze dryer under the condition that the humidity is less than 40.0% to obtain the high-activity polypeptide or protein raw material.
The specific surface area of the obtained product is related to the temperature of the tray, and the lower the temperature of the tray is, the larger the specific surface area of the product is, and the specific correspondence is shown in table 1.
TABLE 1 comparison table of specific surface area of product and tray temperature
| Controlling temperature point | Obtaining specific surface of active matter |
| -5℃ | 13.1m2/g |
| -10℃ | 20.6m2/g |
| -20℃ | 27.2m2/g |
| -25℃ | 28.5m2/g |
| -30℃ | 31.9m2/g |
| -35℃ | 41.3m2/g |
The product molding quality of the freeze-drying step is related to the temperature, drying time and vacuum degree, and the specific correspondence is shown in table 2.
Table 2 freeze drying process test data
in conclusion, the above description is only for the preferred embodiment of the present invention and should not be construed as limiting the present invention, and any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A production device of nanometer slow-release micro powder with high specific surface area is characterized in that: comprises a powder quick-freezing system and a freeze-drying system,
The powder quick-freezing system comprises an ultralow temperature environment box (3), wherein a closed refrigerant chamber (6) is arranged in the ultralow temperature environment box (3), and the refrigerant chamber (6) is provided with a refrigerant inlet and a refrigerant outlet; the top of the ultra-low temperature environment box (3) is provided with a quick-freezing groove (6), the bottom of the quick-freezing groove (6) extends into the refrigerant chamber (5), a tray (8) is arranged in the quick-freezing groove (6), and the tray (8) and the quick-freezing groove (6) are arranged in a split manner;
The powder quick-freezing system also comprises a powder spraying module, the powder spraying module comprises a powder storage tank (1) and a spray head (2) connected with the powder storage tank (1) through a pipeline, and a control valve (21) used for controlling the spray head (2) to work is arranged on the spray head (2);
The powder spraying module further comprises a longitudinal guide rail (9) arranged at the top of the ultra-low temperature environment box (3), and a cross beam (7) arranged above the quick-freezing groove (6) and arranged along the width direction of the quick-freezing groove (6), wherein the longitudinal guide rail (9) extends along the length direction of the quick-freezing groove (6); the cross beam (7) is connected with the longitudinal guide rail (9), and a first driving device (91) for driving the cross beam (7) to move along the length direction of the longitudinal guide rail (9) is arranged on the longitudinal guide rail (9); the cross beam (7) is connected with a spray head mounting seat (10) and a second driving device (71) for driving the spray head mounting seat (10) to move along the length direction of the cross beam (7);
The freeze drying system comprises a vacuum drying oven.
2. The production apparatus according to claim 1, wherein: the refrigerant chamber (5) is provided with an insulating layer (4).
3. The production apparatus according to claim 1, wherein: the ultra-low temperature environment box (3) is also provided with a temperature sensor (32) for monitoring the temperature in the refrigerant chamber (5).
4. The production apparatus according to claim 1, wherein: and a discharge valve (33) is arranged at the bottom of the refrigerant chamber (6).
5. The production apparatus according to claim 1, wherein: the first driving device (91) and the second driving device (71) respectively comprise a motor and a synchronous belt driven by the motor.
6. The production apparatus according to claim 1, wherein: the spray head mounting seat (10) is provided with an infrared sensor, and the infrared sensor controls the opening and closing of the control valve (21) according to the temperature of the product in the tray (8).
7. The production apparatus according to any one of claims 1 to 6, wherein: the bottom of the tray (8) is tightly contacted with the bottom surface of the quick-freezing groove (6).
8. a production process of high-specific-surface-area nanometer slow-release micropowder based on the production equipment of any one of claims 1 to 7, characterized by at least comprising the following steps:
step one, raw material pretreatment: dissolving and diluting the raw materials to be processed, and then performing filter pressing on the raw materials into a powder storage tank (1);
Step two-speed freeze spraying: a coolant with the temperature not higher than-100 ℃ is injected into the refrigerant chamber (5) to pre-cool the tray (8) until the temperature of the tray (8) is not higher than-5 ℃;
Starting a first driving device (91) and a second driving device (71), then starting a control valve (21), enabling a spray head (2) and a cross beam (7) to move relative to a tray (8) respectively, and in the process, enabling the spray head (2) to perform scanning type spraying in the tray (8), and enabling raw materials sprayed on the tray (8) to be rapidly condensed in an ultralow-temperature environment;
After the spraying is finished, the control valve (21) is closed, and the cross beam (7) and the spray head mounting seat (10) are reset;
Step three, freeze drying: pre-cooling the raw materials by a freeze dryer until the temperature in a vacuum drying box is 0 to-65 ℃, placing a tray (8) loaded with the frozen raw materials in the vacuum drying box, and preserving the heat and drying for at least 7 hours.
9. The production process according to claim 8, characterized in that: the temperature of the refrigerant is not higher than-150 ℃, and the temperature of the tray (8) in the quick-freezing spraying process is-5 ℃ to-35 ℃.
10. The production process according to claim 8, characterized in that: in the quick-freezing spraying process, the thickness of the frozen powder in the tray (8) is not more than 1.5 cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910837141.1A CN110547969A (en) | 2019-09-03 | 2019-09-03 | Production process and equipment of high-specific-surface-area nano slow-release micro powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910837141.1A CN110547969A (en) | 2019-09-03 | 2019-09-03 | Production process and equipment of high-specific-surface-area nano slow-release micro powder |
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| CN110547969A true CN110547969A (en) | 2019-12-10 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1256628A (en) * | 1997-04-18 | 2000-06-14 | 药物生物技术公司 | Sustained-release compositions and method for preparing same |
| EP1666655A2 (en) * | 2004-12-02 | 2006-06-07 | Samsung Electronics Co., Ltd. | Eliminating wrinkles in laundry |
| CN101798100A (en) * | 2009-02-11 | 2010-08-11 | Ls空调株式会社 | Home-use freezing type salt extraction device |
| CN102226629A (en) * | 2011-04-22 | 2011-10-26 | 天津科技大学 | Equipment and method for carrying out spray freezing and drying on inert particles |
| CN203304107U (en) * | 2013-06-07 | 2013-11-27 | 宁波市北仑恒誉自动化科技有限公司 | Servo sprayer |
| CN107109342A (en) * | 2014-11-28 | 2017-08-29 | 科.汉森有限公司 | Spray chilling |
| CN108225987A (en) * | 2017-12-27 | 2018-06-29 | 天津科技大学 | Solve the System and method for that micron order drop hits spherical surface freezing coating |
| CN207649400U (en) * | 2017-12-08 | 2018-07-24 | 西安奥邦科技有限责任公司 | A kind of anti-freeze closed cooling tower |
-
2019
- 2019-09-03 CN CN201910837141.1A patent/CN110547969A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1256628A (en) * | 1997-04-18 | 2000-06-14 | 药物生物技术公司 | Sustained-release compositions and method for preparing same |
| EP1666655A2 (en) * | 2004-12-02 | 2006-06-07 | Samsung Electronics Co., Ltd. | Eliminating wrinkles in laundry |
| CN101798100A (en) * | 2009-02-11 | 2010-08-11 | Ls空调株式会社 | Home-use freezing type salt extraction device |
| CN102226629A (en) * | 2011-04-22 | 2011-10-26 | 天津科技大学 | Equipment and method for carrying out spray freezing and drying on inert particles |
| CN203304107U (en) * | 2013-06-07 | 2013-11-27 | 宁波市北仑恒誉自动化科技有限公司 | Servo sprayer |
| CN107109342A (en) * | 2014-11-28 | 2017-08-29 | 科.汉森有限公司 | Spray chilling |
| CN207649400U (en) * | 2017-12-08 | 2018-07-24 | 西安奥邦科技有限责任公司 | A kind of anti-freeze closed cooling tower |
| CN108225987A (en) * | 2017-12-27 | 2018-06-29 | 天津科技大学 | Solve the System and method for that micron order drop hits spherical surface freezing coating |
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