CN101560306B - Surface processing method for medicinal rubber stopper - Google Patents
Surface processing method for medicinal rubber stopper Download PDFInfo
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- CN101560306B CN101560306B CN2008100495422A CN200810049542A CN101560306B CN 101560306 B CN101560306 B CN 101560306B CN 2008100495422 A CN2008100495422 A CN 2008100495422A CN 200810049542 A CN200810049542 A CN 200810049542A CN 101560306 B CN101560306 B CN 101560306B
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- rubber stopper
- plug
- carbon dioxide
- surface treatment
- supercritical carbon
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Closures For Containers (AREA)
- Medical Preparation Storing Or Oral Administration Devices (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a surface processing method for a medicinal rubber stopper, which comprises the following steps: cleaning the surface of a molded rubber stopper; putting the cleaned rubber stopper in a supercritical carbon dioxide system containing fluorine substances for processing for 8-10 hours and taking out; cleaning the rubber stopper processed through the carbon dioxide system, and drying the rubber stopper at 50-60 DEG C to obtain the rubber stopper with a processed surface. The method has simple process and is easy for realizing industrialized operation. The rubber stopper processed by the method does not influence the tightness of an original halogenated butyl rubber stopper, keeps the physical and chemical performance of the original rubber stopper and has good surface property in the aspects of the water resistance and solvent resistance of the surface.
Description
Technical field
The present invention relates to a kind of rubber surface treating process, be specifically related to the treatment process on a kind of rubber plug surface.
Background technology
No. 462 files specify of state food medicine Bureau of Technical Supervision, on January 1st, 2005 rose, and all drug packaging bottles are stopped using the natural rubber bottle stopper without exception, use isoprene-isobutylene rubber instead or are coated with, cover plug.But the use butyl rubber stoppers exists particulate to come off and uses the phenomenon of silicone oil silication, influence the clarity and the drug quality of medicine, so the improvement work of medical rubber plug becomes the emphasis of drug packaging reform.
Medical rubber plug is direct and contacted the packing of medicine used special rubber item, so chemical property, physical and mechanical properties and the biological property of sizing material all had strict requirement.For overcoming the shortcoming in the butyl rubber plug use, a large amount of research work have been carried out both at home and abroad.At present, the medicinal halogenated butyl rubber bottle stopper of domestic enterprise all carries out surface siliconization to be handled, if do not handle, will have influence on the last machine situation of plug, production efficiency is reduced, waste increases, but there is apparent in view shortcoming, hang pearl and silicone oil skewness etc. as the extension water that produces to the absorption of medicinal powder, to the infusion bottle wall, and the silicone oil during silication might come off, the quality of medicine is produced certain influence.
The CN1552301A patent application discloses a kind of preparation method of medicinal overlay film plug, smears binding agent on the plug surface, after polymeric membrane compound sticking being pressed on the plug under vacuum condition made.Its binding agent is smeared complexity, and might include harmful substances.CN 1389334A patent application discloses a kind of preparation of laminated rubber plug, utilizes method of plasma processing, makes the relative lamination with the unvulcanized rubber sheet of PTFE material processing face and hot-forming.The one, its complex treatment process is unfavorable for industrialization; The 2nd, the stretching of PTFE material and rebound resilience and rubber have bigger difference, easily produce gauffer, influence the quality of medicine; The 3rd, because the poor flexibility of PTFE material, the sealing property of plug is subjected to certain influence, has reduced the shelf lives of medicine.On the whole, domestic patent of invention major part is to utilize film covering methods such as physics heat seal, reach the isolation purpose of rubber plug body and soup, patent application discloses a kind of surface at rubber plug as CN1751973A, cover the method for one deck macromolecule member material close, avoided contacting of plug and soup with the rubber fusing point.
The major part that above-mentioned patented technology adopted all is the multiple film of physical method, the processing condition relative complex, and operative technique is higher.
Summary of the invention
The objective of the invention is to overcome the above-mentioned shortcoming that exists in the prior art, a kind of surface treatment method of medicinal rubber stopper is provided.
The objective of the invention is to be achieved through the following technical solutions:
The surface treatment method of medicinal rubber stopper of the present invention is: rubber plug carries out surface cleaning processing to being shaped; Placing the supercritical carbon dioxide systems that contains fluorine class material to handle after 8～10 hours cleaned rubber plug takes out; Plug cleaning 50～60 ℃ of oven dry in back after carbon dioxide system is handled are promptly obtained the surface treatment plug.
It is to be 1% hydrochloric acid soln cleaning again with mass percentage concentration after 0.2% sodium hydroxide solution cleans that surface cleaning processing described in the inventive method is meant earlier with mass percentage concentration.
Used supercritical carbon dioxide systems temperature is 40～60 ℃ in the inventive method, and pressure is 10～15Mpa.Described fluorine class material is polyvinylidene difluoride (PVDF) or poly(vinylidene fluoride).
Contain dispersion aids in the used supercritical carbon dioxide systems in the inventive method.Described dispersion aids is N, dinethylformamide or methymethacrylate.
In the inventive method in the supercritical carbon dioxide systems addition of fluorine class material calculate according to the surface-area of plug and the quantity of used plug, should reach on every plug every square centimeter in 0.2～0.35 microgram; The addition of dispersion aids is 5～10% of a fluorine class material addition.
The plug surface is after clean, be positioned in the supercritical carbon dioxide systems, because supercritical carbon dioxide systems can be dissolved the part fluorine-containing material, and the surface energy of fluorine-containing material is all lower, has superior surface property, therefore by cleaning and the part hole swelling of supercritical carbon dioxide systems, fluorine-containing material is filled into the plug top layer, thereby reaches any surface finish and the inertia that improves plug plug.
The inventive method technology is simple, is easy to realize the industrialization operation.The plug that after present method is handled, obtains, do not influence the stopping property of original halogenated butyl rubber plug, the physical and chemical performance that has kept original plug, and good surface property arranged, be embodied in its surperficial water tolerance and solvent resistance, can intercept the soluble substance in natural rubber or the synthetic rubber effectively, and the inactive surfaces after the treated cleaning guarantees plug and liquid medicine stability, guaranteed the quality and the safety of medicine.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Be to be 1% hydrochloric acid soln cleaning again with mass percentage concentration after 0.2% sodium hydroxide solution cleans earlier with mass percentage concentration.
It is 40 ℃ that above-mentioned cleaned rubber plug is placed the temperature that contains polyvinylidene difluoride (PVDF), and pressure is to handle after 10 hours in the 10Mpa supercritical carbon dioxide systems to take out; Will the plug after carbon dioxide system is handled clean back 50 ℃ of oven dry and promptly obtain the surface treatment plug.
Embodiment 2
Be to be 1% hydrochloric acid soln cleaning again with mass percentage concentration after 0.2% sodium hydroxide solution cleans earlier with mass percentage concentration.
It is 60 ℃ that above-mentioned cleaned rubber plug is placed the temperature that contains poly(vinylidene fluoride), and pressure is to handle after 8 hours in the 15Mpa supercritical carbon dioxide systems to take out; Will the plug after carbon dioxide system is handled clean back 60 ℃ of oven dry and promptly obtain the surface treatment plug.
Embodiment 3
Be to be 1% hydrochloric acid soln cleaning again with mass percentage concentration after 0.2% sodium hydroxide solution cleans earlier with mass percentage concentration.
Above-mentioned cleaned rubber plug placed contain polyvinylidene difluoride (PVDF) and N, the temperature of dinethylformamide is 50 ℃, and pressure is to handle in the 12Mpa supercritical carbon dioxide systems after 8～10 hours to take out; Will the plug after carbon dioxide system is handled clean back 55 ℃ of oven dry and promptly obtain the surface treatment plug.
Embodiment 4
Be to be 1% hydrochloric acid soln cleaning again with mass percentage concentration after 0.2% sodium hydroxide solution cleans earlier with mass percentage concentration.
Above-mentioned cleaned rubber plug placed contain poly(vinylidene fluoride) and the methymethacrylate temperature is 45 ℃, pressure is to handle after 8.5 hours in the 11Mpa supercritical carbon dioxide systems to take out; Will the plug after carbon dioxide system is handled clean back 52 ℃ of oven dry and promptly obtain the surface treatment plug.
Embodiment 5
Be to be 1% hydrochloric acid soln cleaning again with mass percentage concentration after 0.2% sodium hydroxide solution cleans earlier with mass percentage concentration.
Above-mentioned cleaned rubber plug placed contain polyvinylidene difluoride (PVDF) and the methymethacrylate temperature is 55 ℃, pressure is to handle after 9.5 hours in the 14Mpa supercritical carbon dioxide systems to take out; Will the plug after carbon dioxide system is handled clean back 58 ℃ of oven dry and promptly obtain the surface treatment plug.
Claims (4)
1. the surface treatment method of a medicinal rubber stopper, it is characterized in that: rubber plug carries out surface cleaning processing to being shaped; Placing the supercritical carbon dioxide systems that contains fluorine class material to handle after 8～10 hours cleaned rubber plug takes out; Plug cleaning 50～60 ℃ of oven dry in back after carbon dioxide system is handled are promptly obtained the surface treatment plug; It is to be 1% hydrochloric acid soln cleaning again with mass percentage concentration after 0.2% sodium hydroxide solution cleans that described surface cleaning processing is meant earlier with mass percentage concentration; Described fluorine class material is polyvinylidene difluoride (PVDF) or poly(vinylidene fluoride).
2. the surface treatment method of medicinal rubber stopper according to claim 1, it is characterized in that: the temperature of described supercritical carbon dioxide systems is 40～60 ℃, pressure is 10～15MPa.
3. the surface treatment method of medicinal rubber stopper according to claim 1 is characterized in that: contain dispersion aids in the described supercritical carbon dioxide systems.
4. the surface treatment method of medicinal rubber stopper according to claim 3, it is characterized in that: described dispersion aids is N, dinethylformamide or methyl methacrylate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100495422A CN101560306B (en) | 2008-04-14 | 2008-04-14 | Surface processing method for medicinal rubber stopper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100495422A CN101560306B (en) | 2008-04-14 | 2008-04-14 | Surface processing method for medicinal rubber stopper |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101560306A CN101560306A (en) | 2009-10-21 |
| CN101560306B true CN101560306B (en) | 2011-05-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100495422A Active CN101560306B (en) | 2008-04-14 | 2008-04-14 | Surface processing method for medicinal rubber stopper |
Country Status (1)
| Country | Link |
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| CN (1) | CN101560306B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4614276A (en) * | 1984-05-22 | 1986-09-30 | Daikin Industries | Laminated rubber stopper |
| CN1552301A (en) * | 2003-06-04 | 2004-12-08 | 上海天汇化学有限公司 | Preparation of medicinal film coated rubber plug |
| CN1751973A (en) * | 2005-10-19 | 2006-03-29 | 刘永红 | Compound film rubber cork and its preparation method |
-
2008
- 2008-04-14 CN CN2008100495422A patent/CN101560306B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4614276A (en) * | 1984-05-22 | 1986-09-30 | Daikin Industries | Laminated rubber stopper |
| CN1552301A (en) * | 2003-06-04 | 2004-12-08 | 上海天汇化学有限公司 | Preparation of medicinal film coated rubber plug |
| CN1751973A (en) * | 2005-10-19 | 2006-03-29 | 刘永红 | Compound film rubber cork and its preparation method |
Non-Patent Citations (2)
| Title |
|---|
| JP特开2002-361667A 2002.12.18 |
| 刘海洪.丁基胶塞的膜技术现状与发展趋势.《中国橡胶》.2007,第23卷(第16期),28-30. * |
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| Publication number | Publication date |
|---|---|
| CN101560306A (en) | 2009-10-21 |
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| C06 | Publication | ||
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Owner name: ZHENGZHOU AOXIANG PHARMACEUTIAL PACKING CO., LTD. Free format text: FORMER NAME: ZHENGZHOU AOXIANG PHARMACEUTICAL PACKING CO., LTD. |
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| CP03 | Change of name, title or address |
Address after: 452483 hi tech Industrial Park, three li, Dengfeng, Henan, Zhengzhou Patentee after: ZHENGZHOU AOXIANG PHARMACEUTICAL PACKING CO., LTD. Address before: 452483 hi tech Industrial Park, three li, Henan, Dengfeng Patentee before: Zhengzhou Aoxiang Pharmaceutical Packing Co., Ltd. |