CN103908411B - Freezing and drying lyophilization is used to prepare Chinese medicinal granule equipment and prepare the method for Chinese medicinal granule - Google Patents
Freezing and drying lyophilization is used to prepare Chinese medicinal granule equipment and prepare the method for Chinese medicinal granule Download PDFInfo
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Abstract
The present invention discloses a kind of equipment and the method that use freezing granulation desiccating method to prepare Chinese medicinal granule, and its equipment comprises freezing cabin 1, shower nozzle 2, fluidisation air distribution plate 3, exhaust system 4, vibrating device 5 and freezing medium bucket 8; Freezing cabin 1 is made up of cover 11 and hold 12; Cover 11 and hold 12 are flexibly connected; The top of cover 11 is provided with circular hole 13; The shower nozzle 2 being connected with vibrating device 5 is arranged on directly over circular hole; Cover 11 is connected with exhaust system 4; Fluidisation air distribution plate 3 is arranged on bottom in hold 12; Shower nozzle is connected with material barrel by pipeline, is connected with freezing medium bucket 8 by pipeline bottom hold 12, and the top of freezing medium bucket 8 is provided with freezing medium inlet/outlet pipe 9 and high pressure gas enter pipe 10. The equipment of the present invention overcomes shortcoming in existing Chinese medicinal granule production technology, auxiliary material dependency is high, the vibration freezing solidification of spraying and fluidized drying is combined, and makes Chinese medicinal granule size controlling even, rule, good fluidity.
Description
Technical field
The present invention relates to Chinese medicine preparation equipment and method, particularly relate to a kind of material suitability wider, the Preparation equipment of the Chinese herbal granules that auxiliary material dependency is lower and method.
Background technology
Chinese medicinal granule is a kind of conventional Chinese medicine preparation, has easy administration, absorbs soon, stores and transport simple feature. The traditional processing technology of Chinese herbal granules, generally first uses to decoct and the method such as boils and crude drug carries out extraction purification concentrate, obtain preparing the fluid extract needed for granule or medicinal extract, then utilize extrude sieve, the method such as fluidized drying granulates. In addition, Chinese medicinal granule also can be passed through further processing, prepares other such as tablet, and the medicine of other formulation such as capsule, application is widely.
Based on the sticky nature of medicinal extract, it is shaped for granulating and ensures product dissolution rate, current Chinese medicinal granule preparation, all can add a large amount of auxiliary materials in concentrated obtained Chinese medical concrete and mix, such as: weighting agent (thinner), tackiness agent, disintegrating agent etc. And the content of these auxiliary materials accounts for granule composition more than 50% usually. Fluidized drying granulation technique is owing to have employed spray-fluidized mode so that auxiliary material content relatively tradition granulation of sieving decrease, but still auxiliary material is maintained certain dependency, obtained granule auxiliary material content is not less than 30% usually. High adjunct content causes medicine high cost and loaded down with trivial details operation, and material, production hour, equipment, energy consumption and quality examination aspect drop into bigger, and patient's dose is big.
For the product containing volatile oil component, often need to be prepared into tincture, or tincture soft capsule, add the difficulty carried and take; It is prepared into granule, then deposits and be easy to volatilization during the course, the problem that drug effect reduces, and the method for the current heating fluidized granulation that wet granulation generally adopts, owing to there being the process heated, further increase the loss of volatile oil component.
What the drying of current Chinese herbal granules was conventional is heating process, but owing to Chinese medical extract containing polysaccharose substance usually, make the more difficult drying in a heated state of the Chinese medical concrete under sticky state, easily harden, coking, it is thus desirable to add a large amount of auxiliary material to improve granulation drying and moulding and dispersing property.
How finding a kind of auxiliary material dependency lower, the scope of application is wider, and the applicable Chinese medicinal granule Preparation equipment in process volatile oil component and method, become the problem that development Chinese medicinal granule new preparation process merits attention.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of use freezing granulation desiccating method to prepare the equipment of Chinese medicinal granule.
2nd object of the present invention is to provide a kind of method using freezing and drying lyophilization to prepare Chinese medicinal granule.
3rd object of the present invention is to provide the 2nd kind of equipment using freezing granulation desiccating method to prepare Chinese medicinal granule.
4th object of the present invention is to provide the 2nd kind of method using freezing and drying lyophilization to prepare Chinese medicinal granule.
The technical scheme of the present invention is summarized as follows:
Use freezing granulation desiccating method to prepare an equipment for Chinese medicinal granule, comprise freezing cabin 1, shower nozzle 2, fluidisation air distribution plate 3, exhaust system 4, vibrating device 5 and freezing medium bucket 8; Freezing cabin 1 is made up of cover 11 and hold 12; Cover 11 and hold 12 are flexibly connected; The top of cover 11 is provided with circular hole 13; The shower nozzle 2 being connected with vibrating device 5 is arranged on directly over circular hole; Cover 11 is connected with exhaust system 4; Fluidisation air distribution plate 3 is arranged on bottom in hold 12; Shower nozzle is connected with material barrel by pipeline, is connected with freezing medium bucket 8 by pipeline bottom hold 12, and the top of freezing medium bucket 8 is provided with freezing medium inlet/outlet pipe 9 and high pressure gas enter pipe 10.
Outside surface at shower nozzle is preferably provided with thermal insulation layer.
Use freezing and drying lyophilization to prepare a method for Chinese medicinal granule, comprise the steps:
1) prepare a kind of to use freezing granulation desiccating method to prepare the equipment of Chinese medicinal granule;
2) being inputted by pipeline by freezing medium bucket 8 by the freezing medium of liquid state in the hold 12 in freezing cabin 1 makes liquid freezing medium liquid level higher than fluidisation air distribution plate 3, by fluid Chinese medicine material or semi-fluid Chinese medicine material, it is delivered in shower nozzle 2 when transfer pressure is 1��10bar, make material spray from the nozzle of shower nozzle when the vertical vibration frequency of vibrating device 5 is 20Hz��20000Hz, it is dropped in liquid freezing medium by the circular hole 13 at cover 11 top, it is solidified into particle at ambient pressure, and make the freezing medium gasification of part, the freezing medium of gasification is discharged by exhaust system 4, liquid freezing medium in freezing medium liquid in freezing medium bucket 8 and freezing cabin 1 is extracted out by freezing medium inlet/outlet pipe 9,
3) compression nitrogen or pressurized air are entered pipe 10 from high pressure gas and input freezing medium bucket 8 with 3-20bar, input in freezing cabin 1 after freezing medium bucket 8 cushions, compression nitrogen or pressurized air after buffering pass through fluidisation air distribution plate 3 from bottom to top, make the step 2 being deposited on fluidisation air distribution plate 3) in obtained particle and be in boiling fluidized state, until particle drying.
The 2nd kind of freezing granulation desiccating method of use prepares the equipment of Chinese medicinal granule, comprises freezing cabin 1, shower nozzle 2, fluidisation air distribution plate 3, exhaust system 4, vibrating device 5 and freezing medium bucket 8; Freezing cabin 1 is made up of cover 11 and hold 12; Cover 11 and hold 12 are flexibly connected; The top of cover 11 is provided with circular hole 13; Shower nozzle 2 comprises multiple nozzle being made up of pipe core 14 and the outer tube 15 concentric with pipe core, and the shower nozzle 2 being connected with vibrating device 5 is arranged on directly over circular hole; Cover 11 is connected with exhaust system 4; Fluidisation air distribution plate 3 is arranged on bottom in hold 12; The pipe core of each nozzle of shower nozzle and outer tube are connected from different material barrels by pipeline respectively, are connected with freezing medium bucket 8 by pipeline bottom hold 12, and the top of freezing medium bucket 8 is provided with freezing medium inlet/outlet pipe 9 and high pressure gas enter pipe 10.
Outside surface at shower nozzle is preferably provided with thermal insulation layer.
2nd kind of use freezing and drying lyophilization prepares the method for Chinese medicinal granule, comprises the steps:
1) the 2nd kind of equipment using freezing granulation desiccating method to prepare Chinese medicinal granule is prepared;
2) being inputted by pipeline by freezing medium bucket 8 by the freezing medium of liquid state in the hold 12 in freezing cabin 1 makes liquid freezing medium liquid level higher than fluidisation air distribution plate 3, by fluid Chinese medicine material or semi-fluid Chinese medicine material, it is delivered in the outer tube 15 of each nozzle when transfer pressure is 1��10bar, simultaneously, by one other fluid Chinese medicine material or semi-fluid Chinese medicine material, it is that 1��10bar is delivered in the pipe core 14 of each nozzle at transfer pressure, make material spray from outer tube 15 and pipe core 14 when the vertical vibration frequency of vibrating device 5 is 20Hz��20000Hz, it is dropped in liquid freezing medium by the circular hole 13 at cover 11 top, it is solidified into particle at ambient pressure, and make the freezing medium gasification of part, the freezing medium of gasification is discharged by exhaust system 4, liquid freezing medium in freezing medium liquid in freezing medium bucket 8 and freezing cabin 1 is extracted out by freezing medium inlet/outlet pipe 9,
3) compression nitrogen or pressurized air are entered pipe 10 from high pressure gas and input freezing medium bucket 8 with 3-20bar, input in freezing cabin 1 after freezing medium bucket 8 cushions, compression nitrogen or pressurized air after buffering pass through fluidisation air distribution plate 3 from bottom to top, make the step 2 being deposited on fluidisation air distribution plate 3) in obtained particle and be in boiling fluidized state, until particle drying.
The advantage of the present invention:
1) changing droplet thermal curing methods is freezing solidification, thus overcomes and the shortcoming that auxiliary material dependency is high obtains zero to the product of low auxiliary material content in existing Chinese medicinal granule production technology.
2) utilize common extract to be easy to the feature of solidification compared with volatile oil, it may also be useful to multilayer shower nozzle, make outer extract wrapping inner layer volatile oil, reduce volatile oil loss in process of production.
3) vibration sprayed freezing solidification and fluidized drying combines, it is provided that a kind of size controlling evenly, particle form is more regular, the better freezing granulation method of mobility and integrated equipment.
4) the Chinese medicine microparticle obtained in above process, auxiliary material content is low, even particle size distribution, good fluidity, more it is convenient to later use fluidized coating technology, particle is carried out effective constituent weightening finish, slow control release or enteric coating, this also administration number of times and dosage for reducing medicine further provide basis. And freezing medium used in the present invention, volatilizing rapidly at normal temperatures, nontoxic residue-free, it also avoid follow-up except freezing medium operation so that proceed follow-up fluidized coating in an equipment and become possibility.
Accompanying drawing explanation
Fig. 1 is a kind of device structure schematic diagram using freezing granulation desiccating method to prepare Chinese medicinal granule of the present invention.
Fig. 2 is the 2nd kind of device structure schematic diagram using freezing granulation desiccating method to prepare Chinese medicinal granule of the present invention.
Fig. 3 is the structural representation that the 2nd kind of the present invention equipment connection using freezing granulation desiccating method to prepare Chinese medicinal granule has material barrel.
Embodiment
The present invention is further illustrated for accompanying drawing below.
Use freezing granulation desiccating method to prepare an equipment (see figure 1) for Chinese medicinal granule, comprise freezing cabin 1, shower nozzle 2, fluidisation air distribution plate 3, exhaust system 4, vibrating device 5 and freezing medium bucket 8; Freezing cabin 1 is made up of cover 11 and hold 12;Cover 11 and hold 12 are flexibly connected; The top of cover 11 is provided with circular hole 13; The shower nozzle 2 being connected with vibrating device 5 is arranged on directly over circular hole; Cover 11 is connected with exhaust system 4; Fluidisation air distribution plate 3 is arranged on bottom in hold 12; Shower nozzle is connected with material barrel by pipeline, is connected with freezing medium bucket 8 by pipeline bottom hold 12, and the top of freezing medium bucket 8 is provided with freezing medium inlet/outlet pipe 9 and high pressure gas enter pipe 10.
Outside surface at shower nozzle is preferably provided with thermal insulation layer.
Use freezing and drying lyophilization to prepare a method for Chinese medicinal granule, comprise the steps:
1) prepare a kind of to use freezing granulation desiccating method to prepare the equipment of Chinese medicinal granule;
2) being inputted by pipeline by freezing medium bucket 8 by the freezing medium of liquid state in the hold 12 in freezing cabin 1 makes liquid freezing medium liquid level higher than fluidisation air distribution plate 3, by fluid Chinese medicine material or semi-fluid Chinese medicine material, it is delivered in shower nozzle 2 when transfer pressure is 5bar, make material spray from the nozzle of shower nozzle when the vertical vibration frequency of vibrating device 5 is 10000Hz, it is dropped in liquid freezing medium by the circular hole 13 at cover 11 top, it is solidified into particle at ambient pressure, and make the freezing medium gasification of part, the freezing medium of gasification is discharged by exhaust system 4, liquid freezing medium in freezing medium liquid in freezing medium bucket 8 and freezing cabin 1 is extracted out by freezing medium inlet/outlet pipe 9,
Transfer pressure can also be selected to regulate arbitrarily between 1-10bar;
The vertical vibration frequency of vibrating device 5 can also be different according to product, the optional frequency being set as between 20-20000Hz;
3) compression nitrogen or pressurized air are entered pipe 10 from high pressure gas and input freezing medium bucket 8 with 10bar, input in freezing cabin 1 after freezing medium bucket 8 cushions, compression nitrogen or pressurized air after buffering pass through fluidisation air distribution plate 3 from bottom to top, make the step 2 being deposited on fluidisation air distribution plate 3) in obtained particle and be in boiling fluidized state, the rapid sublimation drying of moisture in particle, until particle drying forms the dried particles of fluff structure.
Compression nitrogen or pressurized air from high pressure gas enter pipe 10 input the pressure of freezing medium bucket 8 can also be different according to product, any force value being set as in 3-20bar.
The 2nd kind of freezing granulation desiccating method of use prepares the equipment (see Fig. 2 and Fig. 3) of Chinese medicinal granule, comprises freezing cabin 1, shower nozzle 2, fluidisation air distribution plate 3, exhaust system 4, vibrating device 5 and freezing medium bucket 8; Freezing cabin 1 is made up of cover 11 and hold 12; Cover 11 and hold 12 are flexibly connected; The top of cover 11 is provided with circular hole 13; Shower nozzle 2 comprises multiple nozzle being made up of pipe core 14 and the outer tube 15 concentric with pipe core, and the shower nozzle 2 being connected with vibrating device 5 is arranged on directly over circular hole; Cover 11 is connected with exhaust system 4; Fluidisation air distribution plate 3 is arranged on bottom in hold 12; The pipe core of each nozzle of shower nozzle and outer tube are connected from different material barrels 6 and 7 by pipeline respectively, are connected with freezing medium bucket 8 by pipeline bottom hold 12, and the top of freezing medium bucket 8 is provided with freezing medium inlet/outlet pipe 9 and high pressure gas enter pipe 10.
Outside surface at shower nozzle is preferably provided with thermal insulation layer.
2nd kind of use freezing and drying lyophilization prepares the method for Chinese medicinal granule, comprises the steps:
1) the 2nd kind of equipment using freezing granulation desiccating method to prepare Chinese medicinal granule is selected;
2) being inputted by pipeline by freezing medium bucket 8 by the freezing medium of liquid state in the hold 12 in freezing cabin 1 makes liquid freezing medium liquid level higher than fluidisation air distribution plate 3, by fluid Chinese medicine material or semi-fluid Chinese medicine material, it is delivered in the outer tube 15 of each nozzle when transfer pressure is 5bar, simultaneously, by one other fluid Chinese medicine material or semi-fluid Chinese medicine material, it is that 50bar is delivered in the pipe core 14 of each nozzle at transfer pressure, make material spray from outer tube 15 and pipe core 14 when the vertical vibration frequency of vibrating device 5 is 10000Hz, it is dropped in liquid freezing medium by the circular hole 13 at cover 11 top, it is solidified into particle at ambient pressure, and make the freezing medium gasification of part, the freezing medium of gasification is discharged by exhaust system 4, liquid freezing medium in freezing medium liquid in freezing medium bucket 8 and freezing cabin 1 is extracted out by freezing medium inlet/outlet pipe 9,
Transfer pressure can also be different according to product, any force value being set as in 1-10bar;
The vertical vibration frequency of vibrating device 5 can also be different individual according to product, the optional frequency being set as in 20-20000Hz;
3) compression nitrogen or pressurized air are entered pipe 10 from high pressure gas, freezing medium bucket 8 is inputted with 6bar, input in freezing cabin 1 after freezing medium bucket 8 cushions, compression nitrogen or pressurized air after buffering pass through fluidisation air distribution plate 3 from bottom to top, make the step 2 being deposited on fluidisation air distribution plate 3) in obtained particle and be in boiling fluidized state, the rapid sublimation drying of moisture in particle, until particle drying forms the dried particles of fluff structure.
Compression nitrogen or pressurized air enter, from high pressure gas, the pressure that pipe 10 inputs freezing medium bucket 8, different according to product, it is also possible to any pressure being set as in 3-20bar.
First material barrel 6, the structure of the 2nd material barrel 7 and freezing medium bucket 8 can be identical, top comprises the pipeline at the bottom of reaching barrel (for input or extract material/freezing medium out), high-pressure air input aperture, and breathing mouth (can according to technique needs, selection directly communicates with indoor, or connection respiratory organ, wherein be placed on can on lifting table for freezing medium bucket 8, and position is adjustable, utilizes law of connected vessels to control freezing medium liquid level (liquid level can obtain) according to process calculation with freezing chamber;
The effect of fluidisation air distribution plate 3: for making uniform stream distribute, to obtain good fluidisation operating mode; The bed bed of material of supported in rest; And formation gas-flow resistance, maintain the stable of fluidized-bed layer.
The fluidisation air distribution plate form of current industrial fluidized bed upper employing is more, and common air distribution plate type is once-through type air distribution plate and side-flow type air distribution plate, and wherein, side-flow type air distribution plate can be divided into again blast cap formula, ram-type and built-up type. Above-mentioned current industrial conventional all kinds of air distribution plate forms, all applicable in this equipment.
The outside surface of shower nozzle is provided with thermal insulation layer, makes Chinese medicine material when spraying, and is not subject to the temperature radiation impact of cryogenic freezing medium in freezing cabin.
The configurable automation control system of the equipment of the present invention, makes respectively suddenly automatically to have run under setting parameter step by step.
Claims (3)
1. one kind uses the equipment that freezing and drying lyophilization prepares Chinese medicinal granule, it is characterized in that comprising freezing cabin (1), shower nozzle (2), fluidisation air distribution plate (3), exhaust system (4), vibrating device (5) and freezing medium bucket (8); Freezing cabin (1) is made up of cover (11) and hold (12); Cover (11) and hold (12) are flexibly connected; The top of cover (11) is provided with circular hole (13); Shower nozzle (2) comprises multiple nozzle being made up of pipe core (14) and the outer tube (15) concentric with pipe core, and the shower nozzle (2) being connected with vibrating device (5) is arranged on directly over circular hole; Cover (11) is connected with exhaust system (4); Fluidisation air distribution plate (3) is arranged on bottom in hold (12); The pipe core of each nozzle of shower nozzle and outer tube are connected from different material barrels by pipeline respectively, hold (12) bottom is connected with freezing medium bucket (8) by pipeline, and the top of freezing medium bucket (8) is provided with freezing medium inlet/outlet pipe (9) and high pressure gas enter pipe (10).
2. a kind of equipment using freezing and drying lyophilization to prepare Chinese herbal granules according to claim 1, is characterized in that the outside surface of described shower nozzle (2) is provided with thermal insulation layer.
3. use freezing and drying lyophilization to prepare a method for Chinese medicinal granule, it is characterized in that comprising the steps:
1) equipment described in claim 1 is prepared;
2) being inputted by pipeline by freezing medium bucket (8) by the freezing medium of liquid state in the hold (12) of freezing cabin (1) makes liquid freezing medium liquid level higher than fluidisation air distribution plate (3), by fluid Chinese medicine material or semi-fluid Chinese medicine material, it is delivered in the outer tube (15) of each nozzle when transfer pressure is 1��10bar, simultaneously, by one other fluid Chinese medicine material or semi-fluid Chinese medicine material, it is that 1��10bar is delivered in the pipe core (14) of each nozzle at transfer pressure, make material in outer tube (15) when the vertical vibration frequency of vibrating device (5) is 20Hz��20000Hz and ejection in pipe core (14), it is dropped in liquid freezing medium by the circular hole (13) at cover (11) top, it is solidified into particle at ambient pressure, and make the freezing medium gasification of part, the freezing medium of gasification is discharged by exhaust system (4), by liquid freezing medium in freezing medium bucket (8) and in freezing cabin (1) liquid freezing medium by freezing medium inlet/outlet pipe (9) extract out,
3) compression nitrogen or pressurized air are entered pipe (10) from high pressure gas and input freezing medium bucket (8) with 3-20bar, input in freezing cabin (1) after freezing medium bucket (8) is cushioned, compression nitrogen or pressurized air after buffering pass through fluidisation air distribution plate (3) from bottom to top, make the step 2 being deposited on fluidisation air distribution plate (3)) in obtained particle and be in boiling fluidized state, until particle drying.
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| CN201410089715.9A CN103908411B (en) | 2014-03-12 | 2014-03-12 | Freezing and drying lyophilization is used to prepare Chinese medicinal granule equipment and prepare the method for Chinese medicinal granule |
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| CN201410089715.9A CN103908411B (en) | 2014-03-12 | 2014-03-12 | Freezing and drying lyophilization is used to prepare Chinese medicinal granule equipment and prepare the method for Chinese medicinal granule |
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| US10588822B2 (en) * | 2017-10-02 | 2020-03-17 | Ningbo Weston Powder Pharma Coatings Co., Ltd. | Apparatus for powder coating of particles |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4704873A (en) * | 1985-11-14 | 1987-11-10 | Taiyo Sanso Co., Ltd. | Method and apparatus for producing microfine frozen particles |
| US6284282B1 (en) * | 1998-04-29 | 2001-09-04 | Genentech, Inc. | Method of spray freeze drying proteins for pharmaceutical administration |
| 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 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1357900A2 (en) * | 2001-01-30 | 2003-11-05 | Board of Regents, The University of Texas System | Process for production of nanoparticles and microparticles by spray freezing into liquid |
| EP1915987A1 (en) * | 2006-10-27 | 2008-04-30 | MediGene AG | Spray-freeze-drying process for the preparation of pellets comprising percolation drying |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4704873A (en) * | 1985-11-14 | 1987-11-10 | Taiyo Sanso Co., Ltd. | Method and apparatus for producing microfine frozen particles |
| US6284282B1 (en) * | 1998-04-29 | 2001-09-04 | Genentech, Inc. | Method of spray freeze drying proteins for pharmaceutical administration |
| 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 |
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Effective date of registration: 20170608 Address after: 300000 Tianjin Tianjin high-end equipment manufacturing industrial park, Beichen Patentee after: TIANJIN YINUO MEDICINE INDUSTRIAL DESIGN CO., LTD. Address before: 300000, Hedong District, Tianjin Red Star Road to Ann Li, building 23, No. 4, unit 601 Co-patentee before: Zhao Yunxia Patentee before: Wang Shiqing |
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Effective date of registration: 20211229 Address after: 300000 No. 8, South Fenhe Road, Science Park, Tianjin Beichen economic and Technological Development Zone, Beichen District, Tianjin (Sanlin electric appliance Institute) Patentee after: YINUO (TIANJIN) TECHNOLOGY CO.,LTD. Address before: 300000 Tianjin high end equipment manufacturing industrial park, Beichen District, Tianjin Patentee before: TIANJIN YINUO MEDICINE INDUSTRIAL DESIGN Co.,Ltd. |