CN100547017C - A kind of preparation method of luminous thermoplastic plastic parent particles - Google Patents
A kind of preparation method of luminous thermoplastic plastic parent particles Download PDFInfo
- Publication number
- CN100547017C CN100547017C CNB2007100159431A CN200710015943A CN100547017C CN 100547017 C CN100547017 C CN 100547017C CN B2007100159431 A CNB2007100159431 A CN B2007100159431A CN 200710015943 A CN200710015943 A CN 200710015943A CN 100547017 C CN100547017 C CN 100547017C
- Authority
- CN
- China
- Prior art keywords
- thermoplastics
- preparation
- luminous
- parent particles
- thermoplastic plastic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Luminescent Compositions (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The present invention is the novel method of a kind of preparation long-afterglow fluorescent material (luminescent powder) plastic master batch, novel process, its characteristics are earlier with fused thermoplastics parcel long-afterglow fluorescent material (luminescent powder), the course of processing afterwards reduces the friction of long-afterglow fluorescent material (luminescent powder) and metallic substance, alleviate the metallic pollution phenomenon, acquisition luminosity height, light-colored long-afterglow fluorescent material (luminescent powder) plastic master batch.
Description
Technical field
The invention belongs to functional field of new, relate to a kind of preparation method of luminous thermoplastic plastic parent particles.
Background technology
Rare earth. strontium aluminate class long-afterglow fluorescent material is a class long-afterglow fluorescent material (luminescent powder) of latest developments, because its high brightness and steady persistence time obtain widespread use.But this class material is because of the hardness height, and after ferruginous metallic substance friction, the ferro element powder can make the material color deepening, and brightness reduces, even loses illumination effect, claims this phenomenon to be " metallic pollution " in the industry.
Long-afterglow fluorescent material (luminescent powder) is mixed back preparation with plastics become the noctilucence master batch, and purposes is very widely arranged, and can prepare various luminous plastics goods with injection moulding, method such as extrude.Yet with traditional prepared plastic master batch, the inevitable and ferrous metal material strong friction of long-afterglow fluorescent material (luminescent powder) produces metallic pollution, can't obtain the good noctilucence master batch of illumination effect.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of preparation method of luminous thermoplastic plastic parent particles is provided.
The preparation method of luminous thermoplastic plastic parent particles of the present invention, it is characterized in that: long-afterglow fluorescent material (luminescent powder) is before producing friction with metal-working plant, with fused thermoplastics parcel, adopt traditional twin screw extruder or single screw extrusion machine granulation more earlier.
Preferably, long-afterglow fluorescent material (luminescent powder) is a strontium aluminate.
Preferably, long-afterglow fluorescent material (luminescent powder) particle size range is the 1-500 micron;
Preferably, thermoplastics is polyethylene (PE), polypropylene (PP), ABS, AS, polystyrene (PS), HIPS, EVA, nylon 6, nylon 66, PET, PBT, polycarbonate thermoplasticss such as (PC).
Preferably, the form of thermoplastics is a powdery, sheet or fibrous; Preferably, the median size of powder thermoplastic plastics is the 10-2000 micron; The thickness of sheet thermoplastics is the 50-2000 micron; Fibrous thermoplastic's diameter is the 2-1000 micron.
Preferably, the preparation method of luminous thermoplastic plastic parent particles of the present invention, comprise the following steps: long-afterglow fluorescent material (luminescent powder) 1-90 (weight) part, thermoplastics 10-99 (weight) part, oxidation inhibitor 0.1~10 (weight) part mix, be heated to 70 ℃~270 ℃ then, make mixture be bonded to piece, can apply suitable pressure in the process.The caked mixture that will bond is pulverized and is fritter, can use by straight forming, also can be the luminous thermoplastic plastic parent particles that hangs down metallic pollution with twin screw extruder or single screw extrusion machine granulation.Described thermoplastics is powder thermoplastic plastics or fibrous thermoplastic.
Preferably, the preparation method of luminous thermoplastic plastic parent particles of the present invention comprises the following steps: long-afterglow fluorescent material (luminescent powder) 1-100 part, thermoplastics 10-99 part, and oxidation inhibitor mixes for 0.1~10 part, as mixture; Mixture is clipped between the two-layer sheet thermoplastics then, applies suitable pressure, and be heated to 70 ℃~270 ℃, kept 10~100 minutes, cooling obtains flap then.Flap is cut into appropriate size, can uses by straight forming, also can be the luminous thermoplastic plastic parent particles that hangs down metallic pollution with twin screw extruder or single screw extrusion machine granulation.Described thermoplastics is powder thermoplastic plastics or fibrous thermoplastic.
Described oxidation inhibitor is selected EBS for use.
The novel method of preparation long-afterglow fluorescent material of the present invention (luminescent powder) plastic master batch, novel process can at utmost alleviate the metallic pollution of preparation process, obtains the luminosity height, light-colored long-afterglow fluorescent material (luminescent powder) plastic master batch.
Embodiment
Following examples are to further specify of the present invention, but the present invention is not limited thereto.
Embodiment 1:
Luminescent powder strontium aluminate 4KG, polypropylene powder 6KG and EBS0.04KG mix, and are tiled in enamel or the stainless steel pallet the about 1-2 of thickness centimetre.The pallet that compound is housed is put into the baking oven that is heated to 180-200 ℃, charge into shielding gas such as nitrogen or argon gas in the baking oven simultaneously.Heated 10-20 minute, polypropylene melts.Pallet is taken out cooling in baking oven.From pallet, take out the caked material of bonding, be fritter less than 1 centimetre with the special-purpose pulverizer pulverizing of plastics.Use dual-screw pelletizer, 200-220 ℃ with fritter granulation again, be the polypropylene noctilucence master batch of low metallic pollution, the content of luminescent powder is 40%.Fritter can not wanted granulation, directly is used for injection moulding luminous plastics goods.
Embodiment 2:
Luminescent powder strontium aluminate 1KG, polyethylene powder 99KG and EBS 0.5KG mix, and are tiled in enamel or the stainless steel pallet the about 1-2 of thickness centimetre.The pallet that compound is housed is put into the baking oven that is heated to 180-200 ℃, charge into shielding gas such as nitrogen or argon gas in the baking oven simultaneously.Heated 10-20 minute, polyethylene melts.Pallet is taken out cooling in baking oven.From pallet, take out the caked material of bonding, be fritter less than 1 centimetre with the special-purpose pulverizer pulverizing of plastics.Use dual-screw pelletizer, 200-220 ℃ with fritter granulation again, be the polyethylene noctilucence master batch of low metallic pollution, the content of luminescent powder is 40%.Fritter can not wanted granulation, directly is used for injection moulding luminous plastics goods.
Embodiment 3:
Luminescent powder strontium aluminate 90KG, ABS powder 10KG and EBS 1.5KG mix, and are tiled in enamel or the stainless steel pallet the about 1-2 of thickness centimetre.The pallet that compound is housed is put into the baking oven that is heated to 180-200 ℃, charge into shielding gas such as nitrogen or argon gas in the baking oven simultaneously.Heated 10-20 minute, ABS melts.Pallet is taken out cooling in baking oven.From pallet, take out the caked material of bonding, be fritter less than 1 centimetre with the special-purpose pulverizer pulverizing of plastics.Use dual-screw pelletizer, 200-220 ℃ with fritter granulation again, be the ABS noctilucence master batch of low metallic pollution, the content of luminescent powder is 40%.Fritter can not wanted granulation, directly is used for injection moulding luminous plastics goods.
Embodiment 4:
Luminescent powder strontium aluminate 2KG, polycarbonate (PC) powder 8KG and EBS0.04KG, mix, be tiled between polycarbonate (PC) sheet of two 0.5 mm thick, about 1 centimetre of the thickness of mixed powder is clipped between sizeable two metal forms then, puts on the vulcanizing press that is heated to 260 ℃, apply suitable pressure, kept 10--15 minute.Take out template, cooling.From template, take out and be pressed into flaky material, be cut into the length of side less than 1 centimetre fritter.Use single screw pelletizer, 260-280 ℃ with fritter granulation again, be polycarbonate (PC) the noctilucence master batch of low metallic pollution, the content of luminescent powder is 19%.Fritter can not wanted granulation, directly is used for injection moulding luminous plastics goods.
Embodiment 5:
Luminescent powder strontium aluminate 2KG, polystyrene powder 98KG and EBS0.05KG, mix, be tiled between the polystyrene sheet of two 0.5 mm thick, about 1 centimetre of the thickness of mixed powder is clipped between sizeable two metal forms then, puts on the vulcanizing press that is heated to 260 ℃, apply suitable pressure, kept 10--15 minute.Take out template, cooling.From template, take out and be pressed into flaky material, be cut into the length of side less than 1 centimetre fritter.Use single screw pelletizer, 260-280 ℃ with fritter granulation again, be the polystyrene noctilucence master batch of low metallic pollution, the content of luminescent powder is 19%.Fritter can not wanted granulation, directly is used for injection moulding luminous plastics goods.
Embodiment 6:
Luminescent powder strontium aluminate 98KG, PBT powder 2KG and EBS0.04KG, mix, be tiled between the PBT sheet of two 0.5 mm thick, about 1 centimetre of the thickness of mixed powder is clipped between sizeable two metal forms then, puts on the vulcanizing press that is heated to 260 ℃, apply suitable pressure, kept 10--15 minute.Take out template, cooling.From template, take out and be pressed into flaky material, be cut into the length of side less than 1 centimetre fritter.Use single screw pelletizer, 260-280 ℃ with fritter granulation again, be the PBT noctilucence master batch of low metallic pollution, the content of luminescent powder is 19%.Fritter can not wanted granulation, directly is used for injection moulding luminous plastics goods.
Claims (7)
1. the preparation method of a luminous thermoplastic plastic parent particles is characterized in that: long-afterglow fluorescent material with fused thermoplastics parcel, adopted traditional twin screw extruder or single screw extrusion machine granulation earlier again before producing friction with metal-working plant; Described long-afterglow fluorescent material is a strontium aluminate; Described thermoplastics is selected from polyethylene, polypropylene, acrylonitrile-butadiene-styrene copolymer, acrylonitritrile-styrene resin, high impact polystyrene, vinyl acetate copolymer, nylon 6, nylon 6,6, polyethylene terephthalate, polybutylene terephthalate, or polycarbonate.
2. the preparation method of a luminous thermoplastic plastic parent particles as claimed in claim 1, it is characterized in that: the long-afterglow fluorescent material particle size range is the 1-500 micron.
3. the preparation method of a luminous thermoplastic plastic parent particles as claimed in claim 1, it is characterized in that: the form of thermoplastics is a powdery, sheet or fibrous.
4. preparation method as claim 1 or 3 described luminous thermoplastic plastic parent particles, it is characterized in that: the median size of powder thermoplastic plastics is the 10-2000 micron; The thickness of sheet thermoplastics is the 50-2000 micron; Fibrous thermoplastic's diameter is the 2-1000 micron.
5. the preparation method of a luminous thermoplastic plastic parent particles as claimed in claim 1, comprise the following steps: long-afterglow fluorescent material 1-90 weight part, thermoplastics 10-99 weight part, oxidation inhibitor 0.1~10 weight part mix, be heated to 70 ℃~270 ℃ then, make mixture be bonded to piece, apply suitable pressure in the process; The caked mixture that will bond is pulverized and is fritter, and straight forming uses, or with twin screw extruder or single screw extrusion machine granulation, is the luminous thermoplastic plastic parent particles that hangs down metallic pollution; Described thermoplastics is powder thermoplastic plastics or fibrous thermoplastic.
6. the preparation method of a luminous thermoplastic plastic parent particles as claimed in claim 1 comprises the following steps: long-afterglow fluorescent material 1-100 part, and thermoplastics 0-99 part, oxidation inhibitor mix for 0.1~10 part, as mixture; Mixture is clipped between the two-layer sheet thermoplastics then, applies suitable pressure, and be heated to 70 ℃~270 ℃, kept 10~100 minutes, cooling obtains flap then; Flap is cut into appropriate size, and straight forming uses, or with twin screw extruder or single screw extrusion machine granulation, is the luminous thermoplastic plastic parent particles that hangs down metallic pollution; Described thermoplastics is powder thermoplastic plastics or fibrous thermoplastic.
7. the preparation method of a luminous thermoplastic plastic parent particles as claimed in claim 6, it is characterized in that: oxidation inhibitor is selected ethylenebisstearamide for use.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2007100159431A CN100547017C (en) | 2007-06-18 | 2007-06-18 | A kind of preparation method of luminous thermoplastic plastic parent particles |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2007100159431A CN100547017C (en) | 2007-06-18 | 2007-06-18 | A kind of preparation method of luminous thermoplastic plastic parent particles |
Publications (2)
Publication Number | Publication Date |
---|---|
CN101070392A CN101070392A (en) | 2007-11-14 |
CN100547017C true CN100547017C (en) | 2009-10-07 |
Family
ID=38897818
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2007100159431A Expired - Fee Related CN100547017C (en) | 2007-06-18 | 2007-06-18 | A kind of preparation method of luminous thermoplastic plastic parent particles |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN100547017C (en) |
Families Citing this family (34)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9028717B2 (en) * | 2010-09-03 | 2015-05-12 | Stephen Roy Nagel | Glow-in-the dark for a lighting source including flexible packaging for such light source |
CN102002230A (en) * | 2010-11-02 | 2011-04-06 | 苏州市科创聚合物有限公司 | Environmentally-friendly luminous nylon 12 material |
CN101982501A (en) * | 2010-11-02 | 2011-03-02 | 苏州市科创聚合物有限公司 | Noctilucent nylon material for injection molding |
CN101974182A (en) * | 2010-11-02 | 2011-02-16 | 苏州市科创聚合物有限公司 | Luminous polystyrene transparent material for green environment-friendly injection molding |
CN103242587B (en) * | 2012-02-09 | 2016-08-10 | 辽宁辽杰科技有限公司 | A kind of Fluorescent thermoplastic resin composite material and preparation method thereof |
CN102731913A (en) * | 2012-07-23 | 2012-10-17 | 西南科技大学 | Novel fluorescent plastic and preparation method thereof |
CN102863811A (en) * | 2012-08-31 | 2013-01-09 | 苏州博云塑业有限公司 | Underwater luminous master batch and preparation process thereof |
CN102888670A (en) * | 2012-09-22 | 2013-01-23 | 仪征市星海化纤有限公司 | Light storage silk and production process thereof |
CN104231426A (en) * | 2013-06-24 | 2014-12-24 | 黑龙江鑫达企业集团有限公司 | Polypropylene self-luminescent material and preparation method thereof |
CN103509363B (en) * | 2013-09-10 | 2016-01-13 | 宁波市德明夜光科技有限公司 | A kind of preparation method of luminous plastics moulding |
CN103724969A (en) * | 2013-12-27 | 2014-04-16 | 吴江市东泰电力特种开关有限公司 | Antibacterial fluorescent PET/PC (Polyethylene Terephthalate/Polycarbonate) alloy and preparation method thereof |
CN103694687A (en) * | 2013-12-28 | 2014-04-02 | 宁波金富亮塑料科技有限公司 | Anti-static anti-UV (ultraviolet) nylon color masterbatch |
CN103694683A (en) * | 2013-12-28 | 2014-04-02 | 宁波金富亮塑料科技有限公司 | Color master batch for nylon |
CN103709733A (en) * | 2013-12-28 | 2014-04-09 | 宁波金富亮塑料科技有限公司 | Orange anti-UV color master batch for nylon |
CN104312143B (en) * | 2014-09-19 | 2016-11-23 | 金发科技股份有限公司 | A kind of polyamide false-proof film and preparation method thereof |
CN104262814A (en) * | 2014-10-21 | 2015-01-07 | 常熟市帅红塑料制品厂 | Noctilucent plastic product |
CN104552878A (en) * | 2015-01-28 | 2015-04-29 | 王莉 | Preparation method of noctilucent panel |
CN104774456A (en) * | 2015-04-01 | 2015-07-15 | 芜湖市鸿坤汽车零部件有限公司 | Connecting piece of noctilucent nylon socket |
CN105482395A (en) * | 2016-01-05 | 2016-04-13 | 华南协同创新研究院 | Light-emitting PLA wire for 3D printing and preparation method and application thereof |
CN106674710A (en) * | 2016-12-13 | 2017-05-17 | 福建鑫邦新材料科技有限公司 | EVA (Ethylene Vinyl Acetate) master batch as well as preparation method and application thereof |
CN106589853A (en) * | 2016-12-20 | 2017-04-26 | 佛山市高明区塑料行业协会 | Novel fluorescent modified polybutylene terephthalate |
CN106589646A (en) * | 2016-12-20 | 2017-04-26 | 佛山市高明区塑料行业协会 | Novel polystyrene modified fluorescent material |
CN106945314A (en) * | 2017-03-06 | 2017-07-14 | 五行科技股份有限公司 | A kind of noctilucence flexible pipe and its manufacture method for conveying fracturing fluid backwater |
CN107189250A (en) * | 2017-06-27 | 2017-09-22 | 苏州菱慧电子科技有限公司 | A kind of electronic luminescent material |
CN109749182B (en) * | 2017-11-01 | 2021-09-24 | 国家能源投资集团有限责任公司 | Light-storing polyethylene composition, light-storing polyethylene material, and preparation method and application thereof |
CN107815018B (en) * | 2017-11-06 | 2023-11-24 | 安特普工程塑料(苏州)有限公司 | Noctilucent plastic, double-screw extruder for preparing noctilucent plastic and preparation method |
CN108822393A (en) * | 2018-07-16 | 2018-11-16 | 东莞市兴茂橡塑科技有限公司 | A kind of footwear material efficient noctilucence master batch and noctilucence footwear material |
CN109486020B (en) * | 2018-12-27 | 2021-06-15 | 广东省稀有金属研究所 | PP (polypropylene) luminous master batch and preparation method thereof |
CN110437527B (en) * | 2019-08-19 | 2021-12-17 | 广东省稀有金属研究所 | Long-afterglow PE master batch, preparation method thereof, PE plastic product and preparation method thereof |
CN112852178A (en) * | 2020-12-23 | 2021-05-28 | 张文俊 | Noctilucent plastic injection molding part |
CN113789048A (en) * | 2021-08-25 | 2021-12-14 | 南京聚隆科技股份有限公司 | Long-afterglow weather-resistant noctilucent nylon plastic and preparation method thereof |
CN113845744B (en) * | 2021-10-25 | 2023-11-03 | 金发科技股份有限公司 | Color marking laser marking material with noctilucent effect and application thereof |
CN114702778A (en) * | 2022-03-23 | 2022-07-05 | 浙江一马新材料有限公司 | ABS plastic based on long afterglow material and preparation method thereof |
CN115044320A (en) * | 2022-07-11 | 2022-09-13 | 广州市优伟家居用品有限公司 | Luminous paste and manufacturing method thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1974187A (en) * | 2006-12-19 | 2007-06-06 | 沙萍 | Making process of luminous heat shrinkable casing |
-
2007
- 2007-06-18 CN CNB2007100159431A patent/CN100547017C/en not_active Expired - Fee Related
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1974187A (en) * | 2006-12-19 | 2007-06-06 | 沙萍 | Making process of luminous heat shrinkable casing |
Non-Patent Citations (2)
Title |
---|
添加铝酸盐类长余辉发光粉的夜光塑料性能研究. 崔文秀,苑会林.塑料工业,第34卷. 2006 |
添加铝酸盐类长余辉发光粉的夜光塑料性能研究. 崔文秀,苑会林.塑料工业,第34卷. 2006 * |
Also Published As
Publication number | Publication date |
---|---|
CN101070392A (en) | 2007-11-14 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN100547017C (en) | A kind of preparation method of luminous thermoplastic plastic parent particles | |
CN103854844B (en) | A kind of method that the 3D of utilization printing technique prepares complicated shape bonded permanent magnet | |
CN104140591A (en) | Highly filled micro foamed polypropylene composite material and preparation method thereof | |
CN101708617B (en) | Anti-ageing wood-plastic composite board and preparation method thereof | |
WO2009091987A3 (en) | Melt molding polymer composite and method of making and using the same | |
CN102731881B (en) | For cross-linked polyolefin composition for rotational molding and preparation method thereof | |
EP0662103A4 (en) | Degradable polymer composition. | |
CN105037929B (en) | A kind of great surface quality lightweight exempts from spray coating polypropylene material and preparation method thereof | |
CN102816336B (en) | Method for preparing high filling plastic masterbatch for polypropylene woven bag | |
CN108841076A (en) | A kind of low smell, it is low distribute, flame-retardant polypropylene composite material and preparation method thereof | |
EP0391372A3 (en) | Processes for manufacturing thermoplastic resin compositions and shaped articles thereof | |
US20140227485A1 (en) | Composite profile and producing method thereof | |
CN1566196A (en) | Polypropylene composite materials | |
CN104072843B (en) | A kind of multiple dimensioned composite functional agglomerate and preparation method thereof | |
CN104558783A (en) | Rotational molding polyolefin composition and preparation method thereof | |
CN104530569A (en) | Environment-friendly high-glossiness colorful polypropylene material and manufacturing method thereof | |
CN103709479A (en) | Aluminum-plastic composite panel with high rigidity and high bending strength and preparation method of aluminum-plastic composite panel | |
CN103756238A (en) | Enhanced ABS (Acrylonitrile Butadiene Styrene)/PMMA (Polymethyl Methacrylate) alloy material | |
CN104530909A (en) | Powder coating for low-temperature solidified wine bottle and preparation method thereof | |
CA2581880A1 (en) | Buoyant detectable cable tie | |
CN107501578A (en) | A kind of high temperature resistant, organic smooth opening agent of low migration and master batch that thus opening agent is prepared | |
CN101798400A (en) | Environmental-friendly degradable composite modified master batch and preparation method thereof | |
CN101698747A (en) | Composite material for manufacturing gas stove valve body assembly and preparation method thereof | |
CN109320873B (en) | Paint-spraying-free lamp plastic with metal effect and preparation method thereof | |
CN112795179A (en) | Preparation method of thermoplastic high-specific-gravity composite material |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091007 Termination date: 20130618 |