CN100368065C - Production of polyolefin microporous membrane - Google Patents
Production of polyolefin microporous membrane Download PDFInfo
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- CN100368065C CN100368065C CNB2004100514374A CN200410051437A CN100368065C CN 100368065 C CN100368065 C CN 100368065C CN B2004100514374 A CNB2004100514374 A CN B2004100514374A CN 200410051437 A CN200410051437 A CN 200410051437A CN 100368065 C CN100368065 C CN 100368065C
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- 229920000098 polyolefin Polymers 0.000 title claims abstract description 76
- 238000004519 manufacturing process Methods 0.000 title description 2
- 239000012982 microporous membrane Substances 0.000 title 1
- 239000002904 solvent Substances 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000012528 membrane Substances 0.000 claims description 35
- 238000002360 preparation method Methods 0.000 claims description 15
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 230000006835 compression Effects 0.000 claims description 9
- 238000007906 compression Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 6
- 229930195733 hydrocarbon Natural products 0.000 claims description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims description 6
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 4
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 claims description 4
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 claims description 4
- 150000002170 ethers Chemical class 0.000 claims description 3
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 18
- 238000005266 casting Methods 0.000 abstract description 3
- 238000003490 calendering Methods 0.000 abstract description 2
- 229920005672 polyolefin resin Polymers 0.000 abstract 1
- 239000011347 resin Substances 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 239000000203 mixture Substances 0.000 description 7
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 3
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 125000004836 hexamethylene group Chemical class [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 2
- 229920001903 high density polyethylene Polymers 0.000 description 2
- 239000004700 high-density polyethylene Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to a method for making a microporous polyolefin film, which comprises the following steps that a, polyolefin resin and a solvent are melted and mixed into a uniform solution; b, the solution is extruded from a mould head of an extruder and is cooled on a sheet casting roller to be cast into a thick sheet; d, the thick sheet is stretched in double directions to be made into a film; e, the solvent on the film is eluted; the microporous polyolefin film is obtained after heat treatment is carried out on the film. The present invention is characterized in that the thick sheet is firstly preheated before the step (d) is carried out; subsequently, the thick sheet is calendered and then is stretched in double directions. The microporous polyolefin film made by the method has the characteristics of smooth appearance, homogeneous thickness, uniform intensity, etc.
Description
Technical field
The present invention relates to the preparation method of polyolefin micro porous polyolefin membrane, particularly relate to a kind of preparation method that can effectively improve the polyolefin micro porous polyolefin membrane of polyolefin micro porous polyolefin membrane thickness evenness.
Background technology
Polyolefin micro porous polyolefin membrane is a kind of film shape material that contains micropore, and it is widely used in the making of battery with nonaqueous electrolyte barrier film, capacitor diaphragm, various diffusion barrier, membrane for water treatment etc.
The preparation method of polyolefin micro porous polyolefin membrane comprises solvent method, stretching perforate method etc., generally adopts solvent method.Known solvent method is that polyolefin and solvent heating and melting are mixed into uniform solution, this solution is extruded through extruder die head, and sheet is cast in cooling on slab roller, sheet becomes film through biaxial tension, this film just obtains polyolefin micro porous polyolefin membrane by heat treatment then through extractant wash-out solvent wherein.
The surface smoothness of sheet and the uniformity of its thickness directly have influence on the final film thickness and the homogeneous of performance, therefore, must at first produce high-quality sheet in the production process of solvent method.Present preparation method is that polyolefin solution is extruded from the less die lip of the opening degree of extruder mostly, then directly on slab roller cooling cast sheet, this method has a detailed description in the Japan Patent JP2001-81221 of the Japan Patent JP2001-200082 of Tonen and Asahi.The Japan Patent JP2002-367590 of Nitto then discloses a kind of method of extruding from the bigger die lip of opening degree, and its method is to cool off earlier to cast thicker sheet on slab roller, becomes relatively thinner sheet through hot calender then.
Japan Patent JP2001-200082, JP2001-81221 etc. disclose the method for direct casting sheet, the integral thickness of its sheet can be controlled by die lip, but its surperficial flatness is relatively poor, particularly when the viscosity of polyolefin solution hour, form trickle longitudinal stripe (there is trickle fluctuation in the sheet transverse gage) in the extrusion easily, the film that makes biaxial tension obtain produces longitudinal stripe, and promptly transverse gage is inhomogeneous.The method of Japan Patent JP2002-367590 can improve the smooth degree on sheet surface, but it has carried out the calendering of big multiplying power on calender, cause the inhomogeneous of sheet integral thickness easily.
Summary of the invention
The present invention aims to provide a kind of preparation method of improved polyolefin micro porous polyolefin membrane, to improve the smooth degree on sheet surface, improve the uniformity of slab thicknesses, obtain high-quality sheet, so produce flat appearance, thickness evenly, the polyolefin micro porous polyolefin membrane of uniform intensity.
For achieving the above object, the invention provides a kind of preparation method of polyolefin micro porous polyolefin membrane, this method may further comprise the steps: a, vistanex is become uniform solution with the solvent melting mixing; B, described solution is extruded by the die head of extruder, and sheet is cast in cooling on slab roller; C, sheet is carried out preheating, preheat temperature is 80～120 ℃, after the preheating sheet is carried out press polish and handles, and it is 2%～20% that sheet is carried out the thickness compression ratio that press polish handles; D, sheet is made film through biaxial tension; E, with described film eluting solvent, after heat treatment obtain polyolefin micro porous polyolefin membrane again, it is characterized in that step (d) is preceding carries out preheating earlier with described sheet carrying out, then carry out press polish and handle, and then carry out biaxial tension.
Among the step a, the vistanex that is used to make micro-porous film can be one or more polyolefinic mixtures, preferably contains the extrahigh-molecular weight polyolefins resin.The extrahigh-molecular weight polyolefins resin can be polyolefinic single polymers or copolymers such as ethene, propylene, 1-butylene, 4-methyl-1-pentene, 1-hexene, or their mixture.The micro-porous film that obtains with these extrahigh-molecular weight polyolefins resins has characteristics such as high strength, high broken film temperature.The weight average molecular weight of extrahigh-molecular weight polyolefins resin should be 1 * 10
6～1 * 10
7, be higher than 1 * 10
7The time vistanex melt viscosity too big, be difficult to and the solvent melting mixing; Be lower than 1 * 10
6The time do not reach the purpose that improves film-strength and broken film temperature again.The weight of extrahigh-molecular weight polyolefins resin account for the resin total amount more than 20% for well, its preferred value is 30～90%.
The vistanex that except the extrahigh-molecular weight polyolefins resin, also should contain other, require from high strength micro-porous film, add the high density polyolefins resin, as polyolefinic single polymers or copolymers such as ethene, propylene, 1-butylene, 4-methyl-1-pentene, 1-hexenes, or their mixture effect is better.The weight average molecular weight of this resin should be 1 * 10
4～1 * 10
6, its preferred weight average molecular weight is 5 * 10
4～3 * 10
5
In order to reduce the closed pore temperature of micro-porous film, can add a small amount of low density polyolefin, as polyolefinic single polymers or copolymers such as ethene, propylene, 1-butylene, 4-methyl-1-pentene, 1-hexenes, or their mixture.Consider that adding low density polyolefin can reduce film strength, thus weight account for the resin total amount below 20% for well.
For making vistanex and solvent be easy to melting mixing, the solvent of the vistanex in step a can be a kind of in the aliphatic hydrocarbons such as nonane, decane, hendecane, dodecane, naphthalane, atoleine, preferably is difficult to the atoleine that volatilizees.The kinematic viscosity that atoleine is 40 ℃ should be chosen between 30～150cst, the low excessively melting mixing that is unfavorable for solvent and vistanex of viscosity, and viscosity is too high to be unfavorable for by the extractant wash-out.The content of solvent accounts for the 40～90% better of vistanex and solvent gross weight, and content is too low, and the micro-porous film void content that obtains is low, and permeability is poor, and content is too high, vistanex solution difficult forming.
The melting mixing method of vistanex among the step a and solvent can have multiple choices, can heat the pressurization stirring regular hour earlier in stirred tank and fully mix, and extrudes with single screw extrusion machine again; Also can add double screw extruder to vistanex earlier, add solvent by the side direction spout again, directly mix and extrude with double screw extruder.Generally more than vistanex mixture melting point 20～60 ℃ of melting temperatures.
Among the step b, polyolefin solution is extruded by the extruder die head, and sheet is cast in cooling on slab roller.In order to prevent that phase process from producing big phase region, after extruding, should cool off rapidly vistanex solution, and the temperature of slab roller should can also use water-bath, ice bath, cryosel bath etc. to accelerate cooling velocity below 30 ℃.
Among the step c, preheating can be the infrared ray preheating, also can be the preheat roll preheating, and be 10～30s preheating time, and preheat temperature is 80～120 ℃.The sheet temperature should be more than polyolefinic softening temperature, below the crystalline melt temperature after the preheating.Temperature is low excessively, and sheet is softening insufficient, easily sheet is produced damage in the burnishing process; Temperature is too high, polyolefin crystallization fusion, and the two-phase dispersing morphology changes.
It is most important characteristic of the present invention that press polish among the step c is handled, and it carries out on calender, and the roller temperature of calender is 80～120 ℃.Above-mentioned calender is a three-roller calendar, by the press polish effect of three-roller calendar, can improve the smooth degree on sheet surface, eliminates the trickle fluctuation of sheet transverse gage simultaneously, obtains high-quality sheet.By regulating the calender clearance between roll, can control slab thicknesses compressed ratio after press polish.
Among the step c, the thickness compression ratio that sheet is carried out the press polish processing is 2%～20%, and preferred thickness compression ratio is 4～10%.Compression factor is too little, does not have the effect of press polish; Compression factor is too big, causes the sheet longitudinal thickness inhomogeneous easily.
In the steps d, be the biaxial tension of longitudinal and transverse two directions to the biaxial tension of sheet, the total multiplying power of vertically and horizontally stretching is 10～100 times.Stretching ratio is too little, and the porosity of the micro-porous film that obtains is low, permeability is poor, and intensity is low; Stretching ratio is excessive, and stretcher can't meet the demands.Draft temperature is 90 ℃-140 ℃.
Eluting solvent among the step e is to use the extractant eluting solvent, and described extractant can be a kind of in hydro carbons, chlorohydrocarbon, fluorinated hydrocarbons and the ethers, and the residual volume of solvent is below 1wt% behind the eluting solvent.Extractant can be hydro carbons such as pentane, hexane, heptane, decane, chlorohydrocarbons such as chloromethanes, carbon tetrachloride, and three fluoridize fluorinated hydrocarbons such as ethane, ethers such as ether, dioxane, the easy volatile solvent of ketones such as acetone, butanone.The residual volume of washing back solvent should counted below 1% with weight %.
Among the step e, in order to prevent micro-porous film contraction distortion in use, particularly in the contraction of the condition of high temperature, the micro-porous film that obtains must be heat-treated, and heat treatment temperature is 100～30 ℃, and heat treatment time is 10～100s.
Contribution of the present invention is that it efficiently solves polyolefin micro porous polyolefin membrane flat appearance and the uniform problem of thickness of how making.The present invention is owing to carry out preheating and press polish processing earlier before sheet is carried out biaxial tension, thereby improved the flatness on sheet surface greatly, improved the uniformity of slab thicknesses, and therefore obtained high-quality sheet, and then produce flat appearance, thickness evenly, the polyolefin micro porous polyolefin membrane of uniform intensity.
Description of drawings
Fig. 1 is embodiments of the invention 1 perforated membrane thickness homogeneity schematic diagrames.
Fig. 2 is embodiments of the invention 2 perforated membrane thickness homogeneity schematic diagrames.
Fig. 3 is embodiments of the invention 3 perforated membrane thickness homogeneity schematic diagrames.
Fig. 4 is embodiments of the invention 4 perforated membrane thickness homogeneity schematic diagrames.
Fig. 5 is a comparative example perforated membrane thickness homogeneity schematic diagram.
The specific embodiment
The following example is to further explanation of the present invention and explanation, and the present invention is not constituted any limitation.
Embodiment 1
High density polyethylene (HDPE) (weight average molecular weight 2.7 * 10 with 24 (weight %)
5, fusing point), the UHMWPE (weight average molecular weight 1.0 * 10 of 6 (weight %)
6, fusing point) drop in the double screw extruder (diameter 78mm, L/D=48, strong mixed milling type), with the atoleine (kinematic viscosity 90cst/40 ℃) of measuring pump by side direction spout adding 70 (weight %), melting mixing is modulated into polyethylene solution under 160 ℃, 150 rev/mins condition.
Polyethylene solution by T pattern head (die lip opening degree 1.2mm, width of cloth 260mm), is extruded with the speed of 3m/min, is cooling casting sheet on 10 ℃ the slab roller in surface temperature, obtains the sheet of thickness 1.0mm.Place 120 ℃ infrared preheating cabinet preheating to enter the three-roller calendar press polish after 20 seconds this sheet, roller temperature is 100 ℃, and the thickness compression factor is 5%.
Sheet after the press polish is carried out progressively biaxial tension, stretching ratio for vertical * horizontal=5 * 7 times, wherein vertical 110 ℃ of the preheat temperatures, 100 ℃ of draft temperatures of drawing; Horizontal 120 ℃ of the preheat temperatures of drawing, 110 ℃ of draft temperatures.The film that obtains after the stretching is clean, dry with heptane, and makes polyolefin micro porous polyolefin membrane 110 ℃ of heat treatments after 20 seconds.This routine polyolefin micro porous polyolefin membrane thickness homogeneity as shown in Figure 1.
Embodiment 2
The slab thicknesses compression ratio is 8% in the three-roller calendar burnishing process, and other step is with embodiment 1.This routine polyolefin micro porous polyolefin membrane thickness homogeneity as shown in Figure 2.
Embodiment 3
Roller temperature is 110 ℃ in the three-roller calendar burnishing process, and other step is with embodiment 1.This routine polyolefin micro porous polyolefin membrane thickness homogeneity as shown in Figure 3.
Embodiment 4
Adopt hot-rolling two sides preheating before press polish is handled, 100 ℃ of preheat roll temperature, preheating time 30s, other step is with embodiment 1.This routine polyolefin micro porous polyolefin membrane thickness homogeneity as shown in Figure 4.
Comparative example 1
The T pattern head of extruder is extruded the sheet that obtains and is handled without press polish, directly carries out progressively biaxial tension, makes film, and other step is with embodiment 1.This routine polyolefin micro porous polyolefin membrane thickness homogeneity as shown in Figure 5.
With the contrast of embodiment and comparative example, and consult Fig. 1～5 as seen, after handling through press polish, the homogeneity of film thickness obviously improves, thus can obtain flat appearance, thickness evenly, the polyolefin micro porous polyolefin membrane of uniform intensity.
Claims (8)
1. the preparation method of a polyolefin micro porous polyolefin membrane, it may further comprise the steps: a, vistanex is become uniform solution with the solvent melting mixing; B, described solution is extruded by the die head of extruder, and sheet is cast in cooling on slab roller; C, sheet is carried out preheating, preheat temperature is 80～120 ℃, after the preheating sheet is carried out press polish and handles, and it is 2%～20% that sheet is carried out the thickness compression ratio that press polish handles; D, sheet is made film through biaxial tension; E, with described film eluting solvent, after heat treatment obtain polyolefin micro porous polyolefin membrane again, it is characterized in that step (d) is preceding carries out preheating earlier with described sheet carrying out, then carry out press polish and handle, and then carry out biaxial tension.
2. the preparation method of polyolefin micro porous polyolefin membrane as claimed in claim 1, it is characterized in that, the solvent of the vistanex in the step (a) can be a kind of in nonane, decane, hendecane, dodecane, naphthalane, the atoleine, and the content of solvent accounts for 40～90% of vistanex and solvent gross weight.
3. the preparation method of polyolefin micro porous polyolefin membrane as claimed in claim 1 is characterized in that, in the step (c), preheating can be the infrared ray preheating, also can be the preheat roll preheating, and be 10～30s preheating time, and preheat temperature is 80～120 ℃.
4. the preparation method of polyolefin micro porous polyolefin membrane as claimed in claim 1 is characterized in that, the press polish in the step (c) is handled and carried out on calender, and the roller temperature of calender is 80～120 ℃.
5. the preparation method of polyolefin micro porous polyolefin membrane as claimed in claim 1 is characterized in that, in the step (c), the thickness compression ratio that sheet is carried out the press polish processing is 4～10%.
6. the preparation method of polyolefin micro porous polyolefin membrane as claimed in claim 1 is characterized in that, in the step (d), is the biaxial tension of longitudinal and transverse two directions to the biaxial tension of sheet, and the total multiplying power of vertically and horizontally stretching is 10～100 times, and draft temperature is 90 ℃-140 ℃.
7. the preparation method of polyolefin micro porous polyolefin membrane as claimed in claim 1, it is characterized in that, eluting solvent in the step (e) is to use the extractant eluting solvent, described extractant can be a kind of in hydro carbons, chlorohydrocarbon, fluorinated hydrocarbons and the ethers, and the residual volume of solvent is being counted below 1% with weight percent behind the eluting solvent.
8. the preparation method of polyolefin micro porous polyolefin membrane as claimed in claim 1 is characterized in that, in the step (e), heat treatment temperature is 100～30 ℃, and heat treatment time is 10～100s.
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Cited By (1)
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| CN101747549B (en) * | 2008-12-18 | 2013-06-19 | 比亚迪股份有限公司 | Polyolefin micro porous polyolefin membrane and method for preparing same |
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| CN101535386B (en) * | 2006-10-30 | 2012-07-04 | 旭化成电子材料株式会社 | Polyolefin microporous membrane |
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| CN103816820B (en) * | 2014-03-13 | 2015-11-11 | 吉林大学 | A kind of semicrystalline polyether-ether-ketone porous film and preparation method thereof |
| JP6555252B2 (en) * | 2014-03-24 | 2019-08-07 | 東レ株式会社 | Method for producing microporous plastic film |
| CN107851766B (en) * | 2015-07-29 | 2021-02-26 | 东丽株式会社 | Battery separator and method for manufacturing same |
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| CN1745887A (en) | 2006-03-15 |
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