CN1480255A - Catalyzer for preparing olefine in low carbon number through catalytic cracking and its preparing method and application - Google Patents
Catalyzer for preparing olefine in low carbon number through catalytic cracking and its preparing method and application Download PDFInfo
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Abstract
A catalyst for preparing low-carbon olefin by catalytic cracking is prepared from alumina, magnesium oxide, sodium vanadate, calcium carbonate, RE metal oxide, kaliophilite or potash feldspar, Cr2O3 and MnO2. Its advantages are high catalytic activity and selectivity, long service life and low reaction temp.
Description
Technical field
The invention relates to petroleum hydrocarbon catalytic pyrolysis and produce the catalyst and the application thereof of olefine in low carbon number, more particularly, the invention relates to catalyst and application thereof that petroleum hydrocarbon catalytic pyrolysis is produced ethene and propylene.
Background technology
Hydro carbons tube furnace steam heat cracking system alkene is the main method that current petroleum chemical industry is produced olefine in low carbon number.But hydro carbons tube furnace steam heat cracking system alkene technology is gradually improved, and further improved potentiality are little; Simultaneously, it is again the process of a large amount of consumes energy, and has adopted harsh process conditions, thereby makes it be subjected to certain restriction on economy and tubing.
In order to improve the selectivity of cracking process alkene, further increase the yield of ethene, propylene, reach and improve the purpose that hydrocarbon cracking generates purpose alkene, people have just carried out many significant researchs since the sixties, developed the method for some new system alkene, as gas heat carrier cracking process (homogeneous phase cracking), solid thermal carriers cracking process, pressurization cracking process and heterogeneous catalysis cracking process in the presence of hydrogen, but methods of these system alkene also have a certain distance apart from commercial Application.
Think that at present one of the most promising method of improving cracking process is to adopt the Deep Catalytic Cracking process of heterogeneous catalysis under existing, this is owing to it is generally acknowledged that Deep Catalytic Cracking process helps improving the degree of depth and the selectivity of cracking reaction, and under the condition that more relaxes than steam heat cracking condition, can obtain higher olefin yields, thereby help cutting down the consumption of energy, increase economic efficiency.
Deep Catalytic Cracking process generally is divided into two kinds, and a kind of fluidized-bed process that is based on is as CN1222558, CN1211470 etc.; Another kind is based on fixed bed reactors, as patent SU910728, SU910729, SU968055, SU1011236 etc.
Be that the basis is carried out hydrocarbon catalytic cracking and produced in the catalyst of olefine in low carbon number with the fixed-bed process, SU910728 discloses a kind of loaded catalyst, contain percentage by weight in this catalyst and be 0.5～2.5% silica, 0.19～3.15% ferrous oxide, 0.01～0.15% magnesia, 0.01～0.15% potassium oxide, 0.01～0.25% titanium dioxide, 0.01～0.15% calcium oxide, 0.01～0.15% sodium oxide molybdena, 0.5～3.6% potassium vanadate and aluminium oxide etc.Its reaction condition is: cracking temperature is 740～800 ℃, and the time of staying is 0.05～0.1 second, and the steam feed ratio is 0.5～1: 1.But the anti-coking poor-performing of this catalyst.It is the catalyst of component that SU910729 discloses with silica, potassium vanadate, ferrous oxide, sodium oxide molybdena, Alpha-alumina, added 0.1～3% potash on this basis, the effect of the potash that adds is mainly the inhibition coking, but its shortcoming is that loss speed is very fast.
SU968055 has reported the float stone catalyst that adopts 20% potassium chloride, and with ammoniacal liquor as the catalytic pyrolysis initator.Its reaction condition is: cracking temperature is 750～850 ℃, and the time of staying is 0.05～0.4 second, and the steam feed ratio is 0.5～1: 1.SU1011236 has reported and has consisted of potassium vanadate, synthetic corundum, has been the catalyst of auxiliary agent with the boron oxide.The used catalyst of thermocatalytic cracking (TCSC) catalyst of patent DD233584, DD2243708 report mainly comprises: (1) is at zeolite, TiO
2, MgO alumino-silicate, ZrO
2Deng the metal oxide of going up supported V, Cr, Ni, Fe, Cu, In, Mn, Sn, Nb, rare earth metal and silver.(2) alkaline-earth metal and alkali-metal aluminate, Mg-Cr spinelle, Al
2O
3With the mixture of alkali metal or alkaline earth oxide, MgO, Al
2O
3, HfO
2, ZrO
2Basic anhydride.
The invention provides a kind of unformed metal compound as catalyst, this catalyst can be issued in the reaction temperature low than thermal cracking and even surpass yield of light olefins with the same level of thermal cracking based on fixed bed reactors.
Summary of the invention
Provided by the inventionly be used for the catalyst that catalytic cracking to prepare lower carbon is counted alkene, it is a kind of unformed metal compound as catalyst, with following component is raw material, and the method by solid mixture moulding and co-precipitation or dipping makes, by weight percentage, aluminium oxide is 10～70%, magnesia is 5～30%, and sodium vanadate is 5～30%, and calcium carbonate is 2～30%, rare-earth oxide is 1～15%, and kaliophilite or potassic feldspar are 10～30%.
The percentage by weight of preferred each component is: aluminium oxide is 20～60%, and magnesia is 10～25%, and sodium vanadate is 8～22%, and calcium carbonate is 8～20%, and rare-earth oxide is 1～10%, and kaliophilite or potassic feldspar are 10～20%.
The preferred boehmite of wherein said aluminium oxide.
The preferred lanthana of wherein said rare-earth oxide.
Preferred described catalytic component also comprises 1～5% chrome green or its nitrate.
Preferred described catalytic component also comprises 1～10% manganese dioxide or its nitrate.
Preparation of catalysts method of the present invention is on the basis of solid mixture moulding, adopts the active constituent of the method supported catalyst of dipping or co-precipitation simultaneously.
The method of solid mixture moulding specifically may further comprise the steps:
(1) pressed powder with aluminium oxide, magnesia, sodium vanadate, calcium carbonate, rare-earth oxide, kaliophilite or potassic feldspar mixes by weight percentage;
(2) in the mixture of step (1) gained, add binding agent, with slurry kneading, the moulding that forms, drying, shaping, roasting.
Wherein said calcium carbonate preferably uses nanometer grade powder.
Wherein said binding agent can be selected hydroxyethylcellulose, sodium carboxymethylcellulose, starch, sesbania powder etc. for use, is preferably hydroxyethylcellulose, sesbania powder etc.
Preferred described shaping of catalyst is a bar, and drying is 6～12 hours under 60～150 ℃, at 800～1600 ℃ of roasting 6～12hr.
Preferred sodium vanadate or rare-earth oxide can also adopt the method for co-precipitation or dipping to load on the catalyst that makes by the solid mixture forming method.This method specifically may further comprise the steps:
(1) pressed powder with aluminium oxide, magnesia, calcium carbonate, kaliophilite or potassic feldspar mixes by weight percentage;
(2) in the mixture of step (1) gained, add binding agent, with slurry kneading, the moulding that forms, drying, shaping, roasting;
(3) adopt the method for co-precipitation or dipping to load on the resulting catalyst of step (2) sodium vanadate, rare-earth oxide.
Immersion condition is: at 60～100 ℃ of following dippings 0.5～2 hour, then 80～150 ℃ dry 2～5 hours down, at last at 800～1600 ℃ of roasting 6～12hr.
Chromium trioxide be or/and manganese dioxide can adopt the method for solid mixture moulding to add in the catalyst, also can be with chromic nitrate or/and manganese nitrate solution adopt on the catalyst that the method for co-precipitation or the dipping method by the solid mixture moulding that loads to makes.
The main crystalline phase that contains in the unformed metal compound as catalyst provided by the invention is MgAl
2O
4, Mg
3(VO)
2, CaAl
2O
4, CaAl
4O
7, Ca
3Al
2O
6, Ca
12Al
14O
33, CaAl
12O
19Deng.
Catalyst provided by the invention can be applicable to hydro carbons is converted in the catalytic cracking method of olefine in low carbon number, particularly ethene, propylene, can realize by following scheme.
At first catalyst of the present invention is placed fixed bed reactors, will contact with catalyst with diluent through the hydrocarbon raw material of preheating and under certain process conditions, react; The Pintsch process gas that produces carries out chilling earlier, and then further refrigerated separation, makes cracking gas and tar separation.The process conditions of reaction are: reaction temperature is 740～850 ℃, and reaction pressure is 0～5 atmospheric pressure, and the time of staying of reaction is 0.05～2 second, and the weight ratio of diluent and hydro carbons is 0.2～2: 1.
Wherein said hydrocarbon raw material can be selected from a kind of in light diesel fuel, naphtha, hydrogenation tail oil, the vacuum gas oil (VGO) or their mixture; Used diluent is a steam.
After wherein catalyst uses a period of time, can in the atmosphere in the presence of steam and the air, regenerate and recover active.The concrete grammar of catalyst regeneration is: feed steam with certain flow when (1) reaction system is warming up to 200～600 ℃ of left and right sides; When (2) the reaction system temperature rises to 300～900 ℃ of left and right sides with certain flow bubbling air; (3) catalyst recovers active behind the 2～8hr that regenerates under the atmosphere of aerobic and water vapour.
Catalyst of the present invention and catalytic cracking method have the following advantages:
1. compare with contrast test under identical process conditions, catalyst provided by the invention can improve nearly 9 percentage points of the yield of ethene in the pyrolysis product, propylene, butadiene.
2. catalyst provided by the invention has the ability of the coke of vaporizing preferably, and has service life and regenerability preferably.
3. the present invention has adopted potassic feldspar or kaliophilite to improve the anti-coking performance of catalyst, compares with the anti-coking performance that prior art adopts potash to improve catalyst, and its characteristics are to reduce greatly the speed of potassium lost.
4. the present invention has adopted manganese dioxide and/or chrome green, has improved the ability of catalyst gasification cracking raw material.
5. the present invention has adopted rare-earth oxide, has improved selection of catalysts and activity, and very favourable to the temperature that reduces cracking reaction.
The specific embodiment
Following example will further describe catalyst provided by the invention.
What contrast test of the present invention adopted is the inertia quartz sand, and the appreciation condition of process conditions and catalyst is identical.
Testing used potassic feldspar is provided by China University of Geosciences.
Used potassic feldspar is composed as follows:
Potassic feldspar component content mass percent
| SiO 2 | TiO 2 | Al 2O 3 | Fe 2O 3 | FeO | MnO | MgO | CaO | Na 2O | K 2O | P 2O 5 |
| 67.38 | 0.09 | 16.21 | 0.53 | 0.61 | 0.04 | 0.96 | 1.07 | 2.35 | 9.75 | 0.17 |
Catalyst used in the example is as follows:
The preparation method of catalyst A is: be 55% with 100 gram solid mixture powder boehmites at first, magnesia is 12%, and potassic feldspar is 14%, and calcium carbonate is 8%, sodium vanadate is 6%, lanthana is 2%, and the content of manganese dioxide is 3%, after fully mixing, adding 8 gram binding agent hydroxyethylcelluloses, 30 ml waters and 25 milliliters of rare nitric acid then mediates, and the formation slurry, slurry is carried out extruded moulding by make-up machine, at 80 ℃ above-mentioned strip was carried out drying 12 hours again; Carry out shaping after the strip drying again, make it form length uniformly; And then under 1100 ℃, catalyst was carried out roasting 12 hours, form the catalyst that performance meets the demands at last.
Catalyst B adopts the method preparation identical with catalyst A.The percentage by weight of each component is: boehmite is 24%, and magnesia is 15%, and potassic feldspar is 13%, and nanometer grade calcium carbonate is 15%, and sodium vanadate is 14%, and lanthana is 10%, and chrome green is 2%, and manganese dioxide is 7%.
Catalyst C is preparation like this.At first adopt the preparation method identical with catalyst A, the percentage by weight of each component is: boehmite is 40%, and magnesia is 17%, and potassic feldspar is 5%, and nanometer grade calcium carbonate is 17%, and manganese dioxide is 5%, and lanthana is 4%; Adopt the method for dipping then, earlier 8% sodium vanadate solution (concentration is 10%) is impregnated on the above-mentioned catalyst, then 4% the chrome green form with chromic nitrate (concentration is 15%) solution is impregnated on the catalyst of above-mentioned steps.
Comparative catalyst D adopts the method preparation identical with catalyst A.The percentage by weight of each component is: boehmite is 65%, and magnesia is 12%, and potash is 4%, and calcium carbonate is 8%, and sodium vanadate is 6%, and lanthana is 2%, and manganese dioxide is 3%.
The rerum natura of the various feedstock oils that evaluation test of the present invention is used sees Table 1.
Table 1 test raw material oil properties
| Raw material | Light diesel fuel AGO | Naphtha NAP | |
| Proportion (d 15.6 15.6) | ????0.8138 | ????0.7560 | |
| Aromatic index BMCI | ????14.94 | ????11.19 | |
| Boiling range (℃) | Initial boiling point 10 30 50 70 90 is done | ????209 ????234 ????258.5 ????284 ????314.5 ????364 ????370 | ????44.5 ????77 ????105 ????123 ????137 ????153 ????254 |
Example 1
This example explanation catalytic performance of catalyst A of the present invention, contrast test 1 and contrast test 2 replace catalyst with the inertia quartz sand.The evaluating catalyst test has been carried out 20 hours.Process conditions and result of the test are listed in table 2.Wherein catalyst surface coking percentage is that coking amount accounts for catalyst weight percentage.Result of the test shows that the yield of ethene and propylene has improved nearly 8 percentage points than blank test.The coking amount of catalyst surface accounts for about 1.5% of catalyst gross weight.
Example 2
The explanation of this example is cracking stock with the catalytic performance of catalyst B of the present invention with the light diesel fuel.The evaluating catalyst test has been carried out 20 hours.Process conditions and result of the test are listed in table 2.Wherein catalyst surface coking percentage is that coking amount accounts for catalyst weight percentage.Result of the test shows that the yield of ethene and propylene has improved nearly 8 percentage points than blank test.The coking amount of catalyst surface accounts for about 0.5% of total catalyst weight.
Example 3
The catalyst C that estimates in this example has carried out 500 hours life tests, and result of the test shows that this catalyst has service life and regenerability preferably.The condition of regeneration is to carry out under the atmosphere in the presence of steam and the air.Evaluation test result such as the table 3 of catalyst C.
Example 4
This example has contrasted the result of the test of catalyst D and catalyst A.Test is estimated with catalyst D catalyst A under identical condition, the element composition to catalyst A and catalyst D after reacting 100 hours is analyzed the result such as the table 4 of its key component content.The result of table 4 shows that the potassium lost speed in the catalyst A has bigger reduction than the loss speed of catalyst D.
Table 2
| Feedstock oil | Naphtha | Light diesel fuel | ||||
| Test code number | Catalyst A | Catalyst B | Contrast test 1 | Catalyst A | Catalyst B | Contrast test 2 |
| Cracking temperature, ℃ | ??820 | ??820 | ????820 | ????780 | ????780 | ????780 |
| The time of staying, second | ??0.1 | ??0.1 | ????0.1 | ????0.07 | ????0.07 | ????0.07 |
| Water-oil factor, wt/wt | ??0.56 | ??0.56 | ????0.56 | ????0.75 | ????0.75 | ????0.75 |
| Carbon dioxide | ??1.38 | ??2.13 | ????0.09 | ????1.30 | ????0.67 | ????0.08 |
| Methane | ??12.99 | ??12.71 | ????12.07 | ????7.67 | ????8.08 | ????6.74 |
| Ethene | ??30.37 | ??30.41 | ????25.35 | ????29.91 | ????30.61 | ????24.86 |
| Propylene | ??16.28 | ??16.27 | ????13.12 | ????16.01 | ????16.56 | ????13.27 |
| Butylene | ??5.56 | ??5.45 | ????5.56 | ????6.59 | ????6.46 | ????5.88 |
| Ethene+propylene | ??46.65 | ??46.68 | ????38.47 | ????46.91 | ????47.17 | ????38.13 |
| The catalyst surface coking, % | ??0.98 | ??0.43 | ?????--- | ????1.01 | ????0.53 | ????--- |
Table 3
| Feedstock oil | Light diesel fuel | ||
| Cracking temperature, ℃ | ????????????????780 | ||
| The time of staying, second | ????????????????0.07 | ||
| Water-oil factor, wt/wt | ????????????????0.75 | ||
| The catalyst code name | Catalyst C | Contrast test 1 | Regeneration test |
| Carbon dioxide | ????0.67 | ????0.08 | ????0.64 |
| Methane | ????8.08 | ????6.74 | ????8.12 |
| Ethene | ????30.61 | ????24.86 | ????30.12 |
| Propylene | ????16.56 | ????13.27 | ????16.41 |
| Butylene | ????6.46 | ????5.88 | ????6.64 |
| Ethene+propylene | ????47.17 | ????38.13 | ????46.53 |
Table 4
| Element is formed | Vanadium | Aluminium | Calcium | Magnesium | Potassium | |
| Catalyst A | Before the reaction | ????3.55 | ????12.23 | ????5.20 | ????5.52 | ????3.51 |
| After the reaction | ????3.38 | ????12.67 | ????5.53 | ????4.26 | ????2.78 | |
| Catalyst D | Before the reaction | ????3.41 | ????12.36 | ????5.66 | ????5.72 | ????3.21 |
| After the reaction | ????3.28 | ????13.47 | ????5.89 | ????5.13 | ????0.98 | |
Claims (11)
1, a kind ofly is used for the catalyst that catalytic cracking to prepare lower carbon is counted alkene, it is characterized in that: with following component is raw material, method by solid mixture moulding and co-precipitation or dipping makes, by weight percentage, aluminium oxide is 10～70%, and magnesia is 5～30%, sodium vanadate is 5～30%, calcium carbonate is 2～30%, and rare-earth oxide is 1～15%, and kaliophilite or potassic feldspar are 10～30%.
According to the described catalyst of claim 1, it is characterized in that 2, aluminium oxide is 20～60%, magnesia is 10～25%, and sodium vanadate is 8～22%, and calcium carbonate is 8～20%, and rare-earth oxide is 1～10%, and kaliophilite or potassic feldspar are 10～20%.
3, according to the described catalyst of claim 1, wherein said aluminium oxide is a boehmite.
4, according to the described catalyst of claim 1, wherein said rare-earth oxide is a lanthana.
5, according to the described catalyst of claim 1, wherein said component also comprises 1～5% chrome green or its nitrate.
6, according to claim 1 or 5 described catalyst, wherein said component also comprises 1～10% manganese dioxide or its nitrate.
7, the described Preparation of catalysts method of claim 1 is characterized in that may further comprise the steps:
(1) pressed powder with aluminium oxide, magnesia, sodium vanadate, calcium carbonate, rare-earth oxide, kaliophilite or potassic feldspar mixes by weight percentage;
(2) in the mixture of step (1) gained, add binding agent, with slurry kneading, the moulding that forms, drying, shaping, roasting.
8, the described Preparation of catalysts method of claim 1 is characterized in that may further comprise the steps:
(1) pressed powder with aluminium oxide, magnesia, calcium carbonate, kaliophilite or potassic feldspar mixes by weight percentage;
(2) in the mixture of step (1) gained, add binding agent, with slurry kneading, the moulding that forms, drying, shaping, roasting;
(3) adopt the method for co-precipitation or dipping to load on the resulting catalyst of step (2) sodium vanadate, rare-earth oxide.
9, according to claim 7 or 8 described preparation methods, wherein said calcium carbonate is nanometer grade powder.
10, according to claim 7 or 8 described preparation methods, it is characterized in that being shaped to bar, 60～150 ℃ of dryings 6～12 hours, 800～1600 ℃ of roastings 6～12 hours.
11, a kind of hydro carbons is converted into the catalytic cracking method of olefine in low carbon number, it is characterized in that adopting described catalyst of one of claim 1-6 and hydrocarbon raw material and diluent, in fixed bed reactors, contact and react through preheating.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408526C (en) * | 2005-08-15 | 2008-08-06 | 中国石油化工股份有限公司 | Method for producing ethene, propylene through catalytic cracking |
| CN101423776A (en) * | 2007-10-31 | 2009-05-06 | 中国石油化工股份有限公司 | Catalytic pyrolysis method combining hydrogen oxidation technique |
| US7686942B2 (en) | 2005-08-15 | 2010-03-30 | Shanghai Research Institute Of Petrochemical Technology Sinopec | Method for preparation of ethylene and propylene by catalytic cracking using a fluid-bed catalyst |
| CN101134160B (en) * | 2006-08-30 | 2010-06-30 | 中国石油天然气股份有限公司 | Reaction device for producing low-carbon olefins by catalytic cracking |
| CN101239866B (en) * | 2007-02-07 | 2010-12-01 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene from oxygen-containing compounds |
| CN103182304A (en) * | 2011-12-29 | 2013-07-03 | 中国石油化工股份有限公司 | Catalyst with cracking and gasification effects and its preparation method |
| US9024100B2 (en) | 2007-07-19 | 2015-05-05 | China Petroleum & Chemical Corporation | Process for producing olefins |
| CN105478162A (en) * | 2014-10-11 | 2016-04-13 | 中国石油化工股份有限公司 | Catalyst for reducing green coke and producing more low-carbon olefins |
| US9480975B2 (en) | 2005-08-15 | 2016-11-01 | China Petroleum & Chemical Corporation | Catalyst for catalytic cracking in a fluidized bed |
| CN111013511A (en) * | 2018-10-09 | 2020-04-17 | 中国石油化工股份有限公司 | Microreactor, system and method for producing low-carbon olefin from petroleum hydrocarbon |
| CN111203225A (en) * | 2020-01-09 | 2020-05-29 | 中国石油大学(华东) | A kind of hydrocarbon catalytic cracking catalyst for producing light olefins and preparation method thereof |
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2002
- 2002-09-03 CN CN02129551.4A patent/CN1218783C/en not_active Expired - Lifetime
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408526C (en) * | 2005-08-15 | 2008-08-06 | 中国石油化工股份有限公司 | Method for producing ethene, propylene through catalytic cracking |
| US9480975B2 (en) | 2005-08-15 | 2016-11-01 | China Petroleum & Chemical Corporation | Catalyst for catalytic cracking in a fluidized bed |
| US7686942B2 (en) | 2005-08-15 | 2010-03-30 | Shanghai Research Institute Of Petrochemical Technology Sinopec | Method for preparation of ethylene and propylene by catalytic cracking using a fluid-bed catalyst |
| CN101134160B (en) * | 2006-08-30 | 2010-06-30 | 中国石油天然气股份有限公司 | Reaction device for producing low-carbon olefins by catalytic cracking |
| CN101239866B (en) * | 2007-02-07 | 2010-12-01 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene from oxygen-containing compounds |
| US9024100B2 (en) | 2007-07-19 | 2015-05-05 | China Petroleum & Chemical Corporation | Process for producing olefins |
| CN101423776B (en) * | 2007-10-31 | 2013-09-25 | 中国石油化工股份有限公司 | Catalytic pyrolysis method combining hydrogen oxidation technique |
| CN101423776A (en) * | 2007-10-31 | 2009-05-06 | 中国石油化工股份有限公司 | Catalytic pyrolysis method combining hydrogen oxidation technique |
| CN103182304B (en) * | 2011-12-29 | 2015-01-14 | 中国石油化工股份有限公司 | Catalyst with cracking and gasification effects and its preparation method |
| CN103182304A (en) * | 2011-12-29 | 2013-07-03 | 中国石油化工股份有限公司 | Catalyst with cracking and gasification effects and its preparation method |
| CN105478162A (en) * | 2014-10-11 | 2016-04-13 | 中国石油化工股份有限公司 | Catalyst for reducing green coke and producing more low-carbon olefins |
| CN111013511A (en) * | 2018-10-09 | 2020-04-17 | 中国石油化工股份有限公司 | Microreactor, system and method for producing low-carbon olefin from petroleum hydrocarbon |
| CN111013511B (en) * | 2018-10-09 | 2021-11-12 | 中国石油化工股份有限公司 | Microreactor, system and method for producing low-carbon olefin from petroleum hydrocarbon |
| CN111203225A (en) * | 2020-01-09 | 2020-05-29 | 中国石油大学(华东) | A kind of hydrocarbon catalytic cracking catalyst for producing light olefins and preparation method thereof |
| CN111203225B (en) * | 2020-01-09 | 2023-07-04 | 中国石油大学(华东) | Catalyst for preparing low-carbon olefin by hydrocarbon catalytic pyrolysis and preparation method thereof |
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|---|---|
| CN1218783C (en) | 2005-09-14 |
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