CN101029168A - PC/ABS alloy and its production - Google Patents
PC/ABS alloy and its production Download PDFInfo
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- CN101029168A CN101029168A CN 200610157851 CN200610157851A CN101029168A CN 101029168 A CN101029168 A CN 101029168A CN 200610157851 CN200610157851 CN 200610157851 CN 200610157851 A CN200610157851 A CN 200610157851A CN 101029168 A CN101029168 A CN 101029168A
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- 229920007019 PC/ABS Polymers 0.000 title claims abstract description 29
- 239000000956 alloy Substances 0.000 title claims abstract description 23
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000004417 polycarbonate Substances 0.000 claims abstract description 22
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 21
- 239000003063 flame retardant Substances 0.000 claims abstract description 17
- 239000000314 lubricant Substances 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 claims description 38
- 229920000728 polyester Polymers 0.000 claims description 19
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000003112 inhibitor Substances 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- -1 pentaerythritol ester Chemical class 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- 239000003999 initiator Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 5
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 4
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 238000002329 infrared spectrum Methods 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002174 Styrene-butadiene Substances 0.000 claims description 2
- 229920000402 bisphenol A polycarbonate polymer Polymers 0.000 claims description 2
- 150000001649 bromium compounds Chemical group 0.000 claims description 2
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 2
- 239000011258 core-shell material Substances 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 125000005313 fatty acid group Chemical group 0.000 claims description 2
- 238000005453 pelletization Methods 0.000 claims description 2
- 239000011115 styrene butadiene Substances 0.000 claims description 2
- 229920006305 unsaturated polyester Polymers 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000005452 bending Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 239000003963 antioxidant agent Substances 0.000 abstract description 2
- 230000003078 antioxidant effect Effects 0.000 abstract description 2
- 238000003466 welding Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 239000012745 toughening agent Substances 0.000 abstract 1
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 28
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229920009204 Methacrylate-butadiene-styrene Polymers 0.000 description 1
- 229920006834 PC+ABS Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000088 plastic resin Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A PC/ABS alloy and its production are disclosed. The process is carried out by taking ABS/polyester-g-MAH as compatible agent, mixing polycarbonate with ABS, ABS/polyester-g-MAH, antioxidant, lubricating agent, fire retardant and toughening agent proportionally, entering into double helix extruder, discharging, cooling, drying and dicing to obtain the final product. It has excellent tensile, bending and ultrasonic welding performances and impact and heat resistances.
Description
Technical field
The present invention relates to technical field of polymer materials, relate in particular to a kind of PC/ABS Alloy And Preparation Method.
Background technology
Polycarbonate (PC) transparency is good, the thermotolerance height, and good light stability, dimensional stability is good, be the best engineering plastics of toughness, but it is to the breach sensitivity, and the product internal stress is big, and the melt viscosity height is mobile poor, difficult forming.Acrylonitrile-styrene-butadienecopolymer (ABS) resin is a kind of interchangeable heat plastic resin with good impact resistance and good moulding processability, it has higher P/C ratio, be easy to plating, mechanical workout, dimensional stability is good, but its thermotolerance and weathering resistance are poor.
PC and ABS resin are that the blend of main raw material is a kind of important engineering polyblend, this material has good moulding flowing property, the use range that is widely used in behind the fire retardant is more wide, yet there is the shortcoming of consistency difference in the simple blend of PC/ABS.SAN solubility parameter among PC and the ABS is more approaching, and PC is 9.8 (cal/cm
3)
0.5, SAN is 9.3-9.6 (cal/cm
3)
0.5, the consistency of SAN and PC is better, however the polyhutadiene among PC and the ABS is difficult to compatible, can cause weak connection between them, and physicals is descended.Existing increase is as SMA in preparation process in order to improve the consistency of ABS and PC, and PMMA, MBS, ACR, ABS-g-MA etc. are as the compatilizer of PC/ABS alloy, but the mechanical property of its PC/ABS alloy and processing characteristics still can not be improved significantly.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of PC/ABS Alloy And Preparation Method, makes the mechanical property of PC/ABS alloy and processing characteristics be significantly improved.
For solving the problems of the technologies described above, the objective of the invention is to be achieved through the following technical solutions.
A kind of PC/ABS alloy, its composition (weight %) is: polycarbonate 50-90%; Acrylonitrile-styrene-butadienecopolymer ABS 0-60%; Polyester is 1-10%; ABS/ polyester-g-MAH 0-10%; Oxidation inhibitor 0.2-1.0%; Lubricant 0.1-0.5%; Fire retardant 5-20%; Toughner 5-15%.
Wherein, described ABS/ polyester-g-MAH is made by following materials of weight proportions: ABS 69.9%, polyester 28%, maleic anhydride (MAH) 1.5%, initiator DCP 0.1%, stearic acid 0.5%.
Wherein, described PC is that molecular weight is the bisphenol A polycarbonate of 20000-30000.
Wherein, weight proportion is among the described ABS: styrene content 30-70%, acrylonitrile content 20-35%, butadiene content 10-30%.
Wherein, described polyester is unsaturated polyester or saturated linear polyesters.
Wherein, described oxidation inhibitor is four [β-(3,5-di-tert-butyl 4-hydroxy phenyl) propionic acid] pentaerythritol ester and three (2, the 4-di-tert-butylphenol) phosphorous acid ester.
Wherein, described lubricant is a fatty acid amide.
Wherein, described fire retardant is a bromide fire retardant.
Wherein, toughner is the core-shell copolymerized thing of esters of acrylic acid.
A kind of preparation method of described according to claim 1 PC/ABS alloy comprises:
A: take by weighing raw material by weight ratio;
B: prepare ABS/ polyester-g-MAH earlier
Specific as follows: ABS 69.9%, polyester 28%, maleic anhydride (MAH) 1.5%, initiator DCP 0.1%, stearic acid 0.5% is by twin screw extruder production, complete processing is as follows: 200 ℃ of district's temperature, 220 ℃ of two district's temperature, 225 ℃ of three district's temperature, 220 ℃ of four district's temperature, 220 ℃ of five district's temperature, 210 ℃ of six district's temperature, engine speed is 450 rev/mins, the about 20kg/ of output hour, the percentage of grafting by the examination of infrared spectrum material was 0.5%.
C: polycarbonate, vinyl cyanide one styrene-butadiene multipolymer, ABS/ polyester-g-MAH, oxidation inhibitor, lubricant, fire retardant, toughner are entered twin screw extruder after mixing by weight ratio, by twin screw extruder production, complete processing is as follows: a district temperature 220-240 ℃, two district temperature 240-250 ℃, three district temperature 240-260 ℃, four district temperature 240-260 ℃, five district temperature 240-260 ℃, six district temperature 230-250 ℃, engine speed 300-450 rev/min.
D: discharging, extrude postcooling, drying, pelletizing and get product.
Above technical scheme as can be seen, the present invention has following beneficial effect:
The present invention adopts the compatilizer of ABS/ polyester-g-MAH as PC/ABS in preparation PC/ABS alloy process, make PC/ABS alloy tensile property, bending property, impact property and the resistance toheat made all be improved significantly, and the ultrasonic welding performance of material also improve.
Embodiment
PC+ABS alloy provided by the invention, its composition (weight %) is: PC 50-90, ABS 0-60, polyester are 1-10, ABS/ polyester-g-MAH 0-10, oxidation inhibitor 0.2-1.0, lubricant 0.1-0.5, fire retardant 5-20, toughner 5-15%.
It is four [β-(3, this policy of 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester that oxidation inhibitor is selected chemical name for use; Auxiliary antioxidant is selected three (2, the 4-di-tert-butylphenol) phosphorous acid ester for use;
Among the present invention, prepare ABS/ polyester-g-MAH earlier, specific as follows: ABS 69.9%, polyester 28%, maleic anhydride (MAH) 1.5%, initiator DCP 0.1%, stearic acid 0.5%, by twin screw extruder production, complete processing is as follows: 200 ℃ of district's temperature, 220 ℃ of two district's temperature, 225 ℃ of three district's temperature, 220 ℃ of four district's temperature, 220 ℃ of five district's temperature, 210 ℃ of six district's temperature, engine speed is 450 rev/mins, the about 20kg/ of output hour, the percentage of grafting by the examination of infrared spectrum material was 0.5%.
Weigh up each component raw material by proportion again, by twin screw extruder production, complete processing is as follows: a district temperature 220-240 ℃, two district temperature 240-250 ℃, three district temperature 240-260 ℃, four district temperature 240-260 ℃, five district temperature 240-260 ℃, six district temperature 230-250 ℃, engine speed 300-450 rev/min.
Use saturated linear polyesters among the present invention, transesterification reaction can take place with PC in saturated linear polyesters, has increased the fusion performance of PC/ABS and other materials, makes the PC/ABS alloy that good ultrasonic wave performance be arranged.
For ease of the present invention is further understood, now describe the present invention in conjunction with specific embodiments.
Embodiment 1:
The PC weight ratio is 65% (below be weight ratio), ABS 9.2%, ABS/ polyester-g-MAH3%, polyester 5%, 1010/168 0.1/0.2%, bromide fire retardant 12%, lubricant 0.5%, toughner 5%. in super mixer with said components mixing at room temperature, afterwards in twin screw extruder production, processing conditions is: 220 ℃ of district's temperature, 235 ℃ of two district's temperature, 240 ℃ of three district's temperature, 240 ℃ of four district's temperature, 240 ℃ of five district's temperature, 230 ℃ of six district's temperature, 450 rev/mins of engine speeds.
Embodiment 2
With the PC weight ratio is 65%, and the ABS weight ratio is that 17.2%, 1010/168 weight ratio is 0.1/0.2%, bromide fire retardant 12%, lubricant 0.5%, toughner 5% are at room temperature done at super mixer and are mixed, afterwards in twin screw extruder production, processing conditions is: 220 ℃ of district's temperature, 240 ℃ of two district's temperature, 240 ℃ of three district's temperature, 235 ℃ of four district's temperature, 230 ℃ of five district's temperature, 230 ℃ of six district's temperature, 450 rev/mins of engine speeds.
Embodiment 3
With the PC weight ratio is 65%, and the ABS weight ratio is 12.2%, polyester 5%, 1010/168 weight ratio is 0.1/0.2%, bromide fire retardant 12%, lubricant 0.5%, toughner 5% are at room temperature done at super mixer and are mixed, afterwards in twin screw extruder production, processing conditions is: 220 ℃ of district's temperature, 240 ℃ of two district's temperature, 240 ℃ of three district's temperature, 240 ℃ of four district's temperature, 235 ℃ of five district's temperature, 230 ℃ of six district's temperature, 450 rev/mins of engine speeds.
Embodiment 4
With the PC weight ratio is 65%, and the ABS weight ratio is 11.2%, and ABS/ polyester-g-MAH weight ratio is 1%, polyester 5%, 1010/168 weight ratio is 0.1/0.2%, bromide fire retardant 12%, lubricant 0.5%, toughner 5% are at room temperature done at super mixer and are mixed, afterwards in twin screw extruder production, processing conditions is: 220 ℃ of district's temperature, 240 ℃ of two district's temperature, 240 ℃ of three district's temperature, 240 ℃ of four district's temperature, 235 ℃ of five district's temperature, 230 ℃ of six district's temperature, 450 rev/mins of engine speeds.
Embodiment 5
With the PC weight ratio is 65%, and the ABS weight ratio is 10.2%, and ABS/ polyester-g-MAH weight ratio is 2%, polyester 5%, 1010/168 weight ratio is 0.1/0.2%, bromide fire retardant 12%, lubricant 0.5%, toughner 5% are at room temperature done at super mixer and are mixed, afterwards in twin screw extruder production, processing conditions is: 220 ℃ of district's temperature, 240 ℃ of two district's temperature, 240 ℃ of three district's temperature, 240 ℃ of four district's temperature, 235 ℃ of five district's temperature, 230 ℃ of six district's temperature, 450 rev/mins of engine speeds.
Performance test:
Tensile strength is tested by GB/T 1040 standards.Specimen types is the I type, batten size (mm): 170 (length) * (20 ± 0.2) (end width) * (4 ± 0.2) (thickness), and draw speed is 50mm/min;
Flexural strength and modulus in flexure are tested by GB 9341/T standard.Specimen types is specimen size (mm): (80 ± 2) * (10 ± 0.2) * (4 ± 0.2), rate of bending are 20mm/min;
Notched Izod impact strength is tested by GB/T 1043 standards.Specimen types is the I type, specimen size (mm): (80 ± 2) * (10 ± 0.2) * (4 ± 0.2); The breach type is a category-A, and the breach residual thickness is 3.2mm.
Embodiment 1～5 prescription and performance see Table 1:
Table 1
| Embodiment | 1 | 2 | 3 | 4 | 5 |
| PC-1225Y | 65 | 65 | 65 | 65 | 65 |
| ABS GP 22 | 9.2 | 17.2 | 12.2 | 11.2- | 10.2 |
| ABS/ polyester-g-MAH | 3 | 0 | 0 | 1 | 2 |
| Polyester | 5 | 0 | 5 | 5 | 5 |
| 1010/168 | 0.1/0.2 | 0.1/0.2 | 0.1/0.2 | 0.1/0.2 | 0.1/0.2 |
| Bromide fire retardant | 12 | 12 | 12 | 12 | 12 |
| Lubricant | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Toughner | 5 | 5 | 5 | 5 | 5 |
| Notched Izod impact strength (kJ/m 2) | 43.4 | 48.9 | 36.1 | 38.9 | 42.4 |
| Unnotched impact strength (kJ/m 2) | 85 | 82 | 85 | 79 | 83 |
| Tensile strength (MPa) | 52.25 | 54.76 | 47.2 | 49.02 | 51.5 |
| Flexural strength (MPa) | 83.1 | 84 | 79.5 | 80.61 | 82 |
| Modulus in flexure (MPa) | 2276 | 2156 | 2106 | 2182 | 2227 |
| MFR (g/10min)(260℃/5KG) | 25.5 | 26 | 23.5 | 24.9 |
As can be seen from the above table, under the identical PC content situation, material has the good ultrasonic wave performance that gets if desired, the impact property, bending property, the tensile strength that then contain the system PC/ABS alloy of ABS/ polyester-g-MAH expanding material are all improved in various degree, particularly notched Izod impact strength has a more substantial increase, and illustrates that ABS/ polyester-g-MAH is the good compatilizer of PC/ABS alloy.
More than a kind of PC/ABS Alloy And Preparation Method provided by the present invention is described in detail, used specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof; Simultaneously, for one of ordinary skill in the art, according to thought of the present invention, the part that all can change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.
Claims (10)
1, a kind of PC/ABS alloy is characterized in that, its composition (weight %) is:
Polycarbonate 50-90%;
Acrylonitrile-styrene-butadienecopolymer ABS 0-60%;
Polyester is 1-10%;
ABS/ polyester-g-MAH 0-10%;
Oxidation inhibitor 0.2-1.0%;
Lubricant 0.1-0.5%;
Fire retardant 5-20%;
Toughner 5-15%.
2, PC/ABS alloy according to claim 1, it is characterized in that: described ABS/ polyester-g-MAH is made by following materials of weight proportions: ABS 69.9%, polyester 28%, maleic anhydride (MAH) 1.5%, initiator DCP 0.1%, stearic acid 0.5%.
3, PC/ABS alloy according to claim 1, it is characterized in that: described PC is that molecular weight is the bisphenol A polycarbonate of 20000-30000.
4, described as claimed in claim 1 or 2 PC/ABS alloy, it is characterized in that: weight proportion is among the described ABS: styrene content 30-70%, acrylonitrile content 20-35%, butadiene content 10-30%.
5, described as claimed in claim 1 or 2 PC/ABS alloy is characterized in that: described polyester is unsaturated polyester or saturated linear polyesters.
6, described as claimed in claim 1 or 2 PC/ABS alloy is characterized in that: described oxidation inhibitor is four [β-(3,5-di-tert-butyl 4-hydroxy phenyl) propionic acid] pentaerythritol ester and three (2, the 4-di-tert-butylphenol) phosphorous acid ester.
7, described as claimed in claim 1 or 2 PC/ABS alloy is characterized in that: described lubricant is a fatty acid amide.
8, described as claimed in claim 1 or 2 PC/ABS alloy is characterized in that: described fire retardant is a bromide fire retardant.
9, described as claimed in claim 1 or 2 PC/ABS alloy is characterized in that: toughner is the core-shell copolymerized thing of esters of acrylic acid.
10, a kind of preparation method of the alloy of PC/ABS according to claim 1 is characterized in that, comprises step:
A: take by weighing raw material by weight ratio;
B: prepare ABS/ polyester-g-MAH earlier
Specific as follows: ABS 69.9%, polyester 28%, maleic anhydride (MAH) 1.5%, initiator DCP 0.1%, stearic acid 0.5% is by twin screw extruder production, complete processing is as follows: 200 ℃ of district's temperature, 220 ℃ of two district's temperature, 225 ℃ of three district's temperature, 220 ℃ of four district's temperature, 220 ℃ of five district's temperature, 210 ℃ of six district's temperature, engine speed is 450 rev/mins, the about 20kg/ of output hour, the percentage of grafting by the examination of infrared spectrum material was 0.5%.
C: polycarbonate, vinyl cyanide one styrene-butadiene multipolymer, ABS/ polyester-g-MAH, oxidation inhibitor, lubricant, fire retardant, toughner are entered twin screw extruder after mixing by weight ratio, by twin screw extruder production, complete processing is as follows: a district temperature 220-240 ℃, two district temperature 240-250 ℃, three district temperature 240-260 ℃, four district temperature 240-260 ℃, five district temperature 240-260 ℃, six district temperature 230-250 ℃, engine speed 300-450 rev/min.
D: discharging, extrude postcooling, drying, pelletizing and get product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101578512A CN101029168B (en) | 2006-12-22 | 2006-12-22 | PC/ABS alloy and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101578512A CN101029168B (en) | 2006-12-22 | 2006-12-22 | PC/ABS alloy and its production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101029168A true CN101029168A (en) | 2007-09-05 |
| CN101029168B CN101029168B (en) | 2012-01-18 |
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