TWI457167B - Apparatus for flue gas desulfurization with zero emission using system for recovery and recycle of magnesium hydroxide - Google Patents
Apparatus for flue gas desulfurization with zero emission using system for recovery and recycle of magnesium hydroxide Download PDFInfo
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本發明係與廢氣脫硫處理有關，特別有關於一種使用氫氧化鎂溶液之廢氣脫硫處理。 The present invention relates to exhaust gas desulfurization treatment, and more particularly to an exhaust gas desulfurization treatment using a magnesium hydroxide solution.
電力需求一直是國內產業最重要的資源，尤其是大型企業如石化業、造紙業等，大多設置汽電共生廠，除可提供電力，同時也可利用發電後之蒸汽作為熱源。為節省燃料成本，目前國內汽電共生廠大多以燃煤鍋爐為主。鍋爐會產生硫氧化物、氮氧化物等空氣污染物；硫氧化物的排放，主要來自粉煤中之硫份，經由燃燒過程產生，使用排煙脫硫技術，除硫效率可達90%，甚至95%以上。 Electricity demand has always been the most important resource for domestic industries, especially for large enterprises such as petrochemical industry and paper industry. Most of them are equipped with steam and electricity symbiosis plants. In addition to providing electricity, steam can also be used as a heat source. In order to save fuel costs, most domestic steam and electricity symbiosis plants are mainly coal-fired boilers. The boiler will produce air pollutants such as sulfur oxides and nitrogen oxides; the emission of sulfur oxides mainly comes from the sulfur in the pulverized coal, which is produced through the combustion process, and uses the flue gas desulfurization technology to achieve a sulfur removal efficiency of 90%. Even 95% or more.
在台灣，污染防治排煙脫硫是以濕式系統為主要處理流程，整體市場的占有率達到95%以上，其中又以四種處理系統，包括氫氧化鈉法、氫氧化鎂法、石灰石法、海水法最為常用，並各有其優缺點和最適使用條件。在煙氣量小、且硫氧化物濃度不高情況下，以選擇氫氧化鈉法較為適合；中小型或中大型鍋爐所排放煙氣量較多，在運轉成本考量下，則建議選擇氫氧化鎂法；煙氣量大 、且硫氧化物濃度較高時，應以石灰石法為處理流程；而海水法之使用有其地理條件及漁業政策問題限制，否則應是最優選擇。 In Taiwan, pollution prevention and control of flue gas desulfurization is based on a wet system. The overall market share is over 95%, including four treatment systems, including sodium hydroxide, magnesium hydroxide, and limestone. The seawater method is the most commonly used, and each has its own advantages and disadvantages and optimum conditions for use. In the case of small amount of flue gas and low concentration of sulfur oxides, it is more suitable to select sodium hydroxide method; small and medium-sized or large-scale boilers emit more flue gas, and in consideration of operating cost, it is recommended to select hydroxide. Magnesium method; large amount of smoke When the concentration of sulfur oxides is high, the limestone method should be used as the treatment process; while the use of the seawater method has its geographical conditions and fishery policy problems, otherwise it should be the best choice.
其中，如上述的氫氧化鎂法雖然運轉成本較低，但仍須要使用大量的氫氧化鎂吸收液與含硫氧化物的煙道氣作用，以致於產生大量污泥。有鑑於此，本發明人為改善並解決上述之缺失，乃特潛心研究並配合學理之運用，終於提出一種設計合理且有效改善上述缺失之本發明。 Among them, although the above-described magnesium hydroxide method has a low running cost, it is necessary to use a large amount of magnesium hydroxide absorbing liquid and a sulfur oxide-containing flue gas so that a large amount of sludge is generated. In view of the above, the present inventors have made great efforts to improve and solve the above-mentioned shortcomings, and have finally made a proposal to rationally and effectively improve the above-mentioned defects.
本發明係一種汽電脫硫設備零排放及氫氧化鎂再生回收系統，可回收氫氧化鎂溶液，再次注入吸收塔中使用。 The invention relates to a zero-emission and magnesium hydroxide regeneration and recovery system for a steam-electric desulfurization device, which can recover the magnesium hydroxide solution and re-inject it into the absorption tower for use.
為了達成上述之目的，本發明係為一種廢氣脫硫處理後的廢水處理系統，包括：一吸收塔，使用氫氧化鎂乳泥與含硫氧化物的廢氣在其中接觸，產生含硫酸鎂之廢水；一底灰攪拌池，接受氯化鈣溶液與該含硫酸鎂之廢水在其中反應，產生氯化鎂溶液與硫酸鈣溶液；一第一分離槽，分離該氯化鎂溶液與該硫酸鈣溶液；一反應槽，接受該氯化鎂溶液與氫氧化鈣乳泥在其中反應，產生氯化鈣溶液與氫氧化鎂溶液；一第二分離槽，分離該氯化鈣溶液與該氫氧化鎂溶液；以及一氫氧化鎂緩衝槽，接受該氫氧化鎂溶液且輸送回流至該吸收塔中。 In order to achieve the above object, the present invention is a wastewater treatment system after desulfurization of exhaust gas, comprising: an absorption tower in which a magnesium hydroxide emulsion is contacted with an exhaust gas containing sulfur oxides to produce wastewater containing magnesium sulfate. a bottom ash mixing tank, receiving a calcium chloride solution and reacting the magnesium sulfate-containing wastewater therein to produce a magnesium chloride solution and a calcium sulfate solution; a first separation tank separating the magnesium chloride solution from the calcium sulfate solution; Receiving the magnesium chloride solution and the calcium hydroxide emulsion to react therein to produce a calcium chloride solution and a magnesium hydroxide solution; a second separation tank separating the calcium chloride solution from the magnesium hydroxide solution; and a magnesium hydroxide The buffer tank receives the magnesium hydroxide solution and delivers the reflux to the absorption tower.
本發明設有獨特迴路連通之氧化鎂儲槽、氧化鎂熱解槽、氫氧化鎂儲槽、吸收塔、底灰攪拌池、氯化鈣儲槽、反應槽、氫氧化鈣儲槽、氧化鈣攪拌槽、氧化鈣儲槽、第一分離槽、第二分離槽，而能將廢水處理所產生物質分離成氫氧化鎂溶液及硫酸鈣泥，不 會有排放廢水之二次污染。 The invention provides a unique circuit connecting magnesium oxide storage tank, magnesium oxide pyrolysis tank, magnesium hydroxide storage tank, absorption tower, bottom ash mixing tank, calcium chloride storage tank, reaction tank, calcium hydroxide storage tank, calcium oxide The stirring tank, the calcium oxide storage tank, the first separation tank and the second separation tank can separate the substances produced by the wastewater treatment into magnesium hydroxide solution and calcium sulfate mud, There will be secondary pollution of discharged wastewater.
又，本發明之整體系統運作，呈自動循環，不會有排放廢水之困擾。而且，可在節省空間、處理快速之情況，使例如汽電共生設備產生的廢氣處理後之廢水處理，達極佳之環保功效。 Moreover, the overall system of the present invention operates in an automatic cycle and does not suffer from the discharge of waste water. Moreover, in the case of space saving and rapid processing, the waste water treated by the exhaust gas generated by the steam-electricity symbiosis equipment can be treated to achieve an excellent environmental protection effect.
10‧‧‧氧化鎂儲槽 10‧‧‧Magnesium Oxide Storage Tank
11a、11b‧‧‧氧化鎂熱解槽 11a, 11b‧‧‧Magnesium oxide pyrolysis tank
12‧‧‧氫氧化鎂儲槽 12‧‧‧Magnesium Hydroxide Storage Tank
13‧‧‧吸收塔 13‧‧‧ absorption tower
14‧‧‧氧化槽 14‧‧‧oxidation tank
15‧‧‧底灰攪拌池 15‧‧‧ bottom ash mixing tank
16‧‧‧氯化鈣儲槽 16‧‧‧ calcium chloride storage tank
17‧‧‧第一分離槽 17‧‧‧First separation tank
18‧‧‧鍋爐水封 18‧‧‧Boiler water seal
19‧‧‧反應槽 19‧‧‧Reaction tank
20‧‧‧氧化鈣貯槽 20‧‧‧calcium oxide storage tank
21a、21b‧‧‧氧化鈣攪拌槽 21a, 21b‧‧‧ Calcium Oxide Stirring Tank
22‧‧‧氫氧化鈣儲槽 22‧‧‧calcium hydroxide storage tank
23‧‧‧氫氧化鎂緩衝槽 23‧‧‧Magnesium hydroxide buffer tank
24‧‧‧第二分離槽 24‧‧‧Second separation tank
130‧‧‧除霧器 130‧‧‧ defogger
第一圖 為本發明之一實施例的汽電脫硫設備零排放及氫氧化鎂再生回收系統示意圖。 The first figure is a schematic diagram of a zero discharge and a magnesium hydroxide regeneration and recovery system for a steam desulfurization equipment according to an embodiment of the present invention.
有關本發明之詳細說明及技術內容，配合圖式說明如下，然而所附圖式僅提供參考與說明用，並非用來對本發明加以限制者。 The detailed description and technical content of the present invention are set forth in the accompanying drawings.
請參照第一圖，第一圖為本發明汽電脫硫設備零排放及氫氧化鎂再生回收系統示意圖。首先，將儲存在氧化鎂儲槽10中的氧化鎂粉末卸下至氧化鎂熱解槽11a、11b中，加水攪拌，並在攪拌之過程予加入少量之熱水或蒸汽，以使氧化鎂熱解成為氫氧化鎂乳泥，再經輸送泵浦予以泵送至氫氧化鎂儲槽12，上述氧化鎂熱解槽11a、11b可以切換使用。貯存在氫氧化鎂儲槽12的氫氧化鎂乳泥持續予以攪拌，並配設輸送泵浦予加注至吸收塔13中。 Please refer to the first figure. The first figure is a schematic diagram of the zero discharge and magnesium hydroxide regeneration and recovery system of the steam desulfurization equipment of the present invention. First, the magnesium oxide powder stored in the magnesium oxide storage tank 10 is discharged into the magnesia pyrolysis tanks 11a, 11b, stirred with water, and a small amount of hot water or steam is added during the stirring to make the magnesia hot. The magnesium hydroxide emulsion is decomposed and pumped to the magnesium hydroxide storage tank 12 via a transfer pump, and the magnesium oxide pyrolysis tanks 11a and 11b can be switched. The magnesium hydroxide emulsion stored in the magnesium hydroxide storage tank 12 is continuously stirred, and is supplied with a delivery pump to be charged into the absorption tower 13.
吸收塔13內之由上層往下噴淋之循環吸收液與由下往上升的煙氣流接觸反應，以吸收煙氣流中之硫氧化物。吸收塔13上部設有除霧器130以去除通過煙氣中所含的水分，使通過吸收塔頂端之煙氣排出口的煙氣符合環保標準。吸收塔13內部循環吸收液需加入氫氧化鎂乳泥，吸收反應後之產物為硫酸鎂或亞硫酸鎂廢液，並予抽送至氧化槽14再處理，使殘餘之亞硫酸鎂氧化成硫酸鎂。 The circulating absorbent in the absorption tower 13 which is sprayed downward from the upper layer is brought into contact with the rising flue gas stream to absorb the sulfur oxides in the flue gas stream. The demister 130 is disposed on the upper portion of the absorption tower 13 to remove moisture contained in the flue gas, so that the flue gas passing through the flue gas discharge port at the top of the absorption tower conforms to environmental protection standards. The absorption liquid in the absorption tower 13 is required to be added with magnesium hydroxide emulsion, and the product after absorption reaction is magnesium sulfate or magnesium sulphate waste liquid, and is pumped to the oxidation tank 14 for further treatment to oxidize residual magnesium sulfate to magnesium sulfate. .
接著，氧化槽14中的硫酸鎂溶液流至底灰攪拌池15與來自氯化鈣儲槽16中的氯化鈣反應，產生氯化鎂與硫酸鈣。接著，將氯化鎂與硫酸鈣溶液抽送至第一分離槽17，產生沈澱作用，分成上層氯化鎂溶液及下層硫酸鈣泥。上層氯化鎂溶液導入反應槽19中與氫氧化鈣乳泥反應，產生氯化鈣溶液與氫氧化鎂溶液。下層硫酸鈣泥輸送至鍋爐水封18加強分離成水與硫酸鈣灰泥，水處於上層，溢流至底灰攪拌池15，而硫酸鈣灰泥則輸送到底灰儲槽(圖未示)回收再利用。亦即，鍋爐水封18可用於將第一分離槽17下層的硫酸鈣泥刮除。 Next, the magnesium sulfate solution in the oxidation tank 14 is passed to the bottom ash agitation tank 15 to react with calcium chloride from the calcium chloride storage tank 16, to produce magnesium chloride and calcium sulfate. Next, the magnesium chloride and calcium sulfate solution are pumped to the first separation tank 17, and a precipitation action is generated, which is divided into an upper magnesium chloride solution and a lower calcium sulfate slurry. The upper magnesium chloride solution is introduced into the reaction tank 19 to react with the calcium hydroxide emulsion to produce a calcium chloride solution and a magnesium hydroxide solution. The lower layer of calcium sulfate mud is transported to the boiler water seal 18 to be separated into water and calcium sulfate stucco. The water is in the upper layer and overflows to the bottom ash mixing tank 15, while the calcium sulfate mortar is transported to the bottom ash storage tank (not shown). Reuse. That is, the boiler water seal 18 can be used to scrape the calcium sulfate slurry in the lower layer of the first separation tank 17.
上述氫氧化鈣乳泥係由氧化鈣加水而形成。本實施例之廢水處理系統係將儲存在氧化鈣儲槽20中的氧化鈣卸下至氧化鈣攪拌槽21a、21b中加水，予以攪拌均勻而形成氫氧化鈣乳泥，再配設輸送泵浦輸送至氫氧化鈣儲槽22，上述氧化鈣攪拌槽21a、21b可以切換使用。接著，將儲存在氫氧化鈣儲槽22中的氫氧化鈣乳泥，配設輸送泵浦輸送至反應槽19中。 The above calcium hydroxide emulsion is formed by adding calcium oxide to water. In the wastewater treatment system of the present embodiment, the calcium oxide stored in the calcium oxide storage tank 20 is removed into the calcium oxide stirring tanks 21a and 21b, and water is added thereto to be uniformly stirred to form calcium hydroxide emulsion, and then a transport pump is disposed. It is sent to the calcium hydroxide storage tank 22, and the said calcium oxide stirring tank 21a, 21b can be used interchangeably. Next, the calcium hydroxide emulsion stored in the calcium hydroxide storage tank 22 is sent to the reaction tank 19 by a delivery pump.
接著，將反應槽19中產生氯化鈣溶液與氫氧化鎂溶液輸送至第二分離槽24，產生沈澱作用，分成上層氯化鈣溶液及下層氫氧化鎂溶液。上層氯化鈣溶液流回底灰攪拌池15與來自分離槽14中的硫酸鎂溶液反應。下層的氫氧化鎂水溶液則輸送至氫氧化鎂緩衝槽23後，再輸送至吸收塔13中作為循環吸收液，俾再經脫硫吸收，及分離槽14、底灰攪拌池15、第一分離槽17、反應槽19、第二分離槽24之循環作用處理。 Next, the calcium chloride solution and the magnesium hydroxide solution generated in the reaction tank 19 are sent to the second separation tank 24 to cause precipitation, and are divided into an upper calcium chloride solution and a lower magnesium hydroxide solution. The upper calcium chloride solution is returned to the bottom ash stirred tank 15 to react with the magnesium sulfate solution from the separation tank 14. The lower magnesium hydroxide aqueous solution is sent to the magnesium hydroxide buffer tank 23, and then sent to the absorption tower 13 as a circulating absorption liquid, which is then subjected to desulfurization absorption, and the separation tank 14, the bottom ash mixing tank 15, and the first separation. The circulation of the tank 17, the reaction tank 19, and the second separation tank 24 is treated.
以下詳細說明本發明之獨特作用及功效： The unique effects and effects of the present invention are described in detail below:
(一)多次循環處理廢水中物質，回收氫氧化鎂溶液： (1) Recycling the material in the wastewater several times to recover the magnesium hydroxide solution:
本發明係採用「連續循環」處理，第一分離槽17使該氯化鎂溶液與該硫酸鈣溶液，產生沈澱作用，分成上層氯化鎂溶液及下層硫酸鈣泥。上層氯化鎂溶液導入反應槽19中與氫氧化鈣乳泥反應，產生氯化鈣溶液與氫氧化鎂溶液。下層硫酸鈣泥輸送至底灰儲槽(圖未示)，回收再利用。 The invention adopts a "continuous cycle" process, and the first separation tank 17 causes the magnesium chloride solution and the calcium sulfate solution to precipitate, and is divided into an upper magnesium chloride solution and a lower calcium sulfate mud. The upper magnesium chloride solution is introduced into the reaction tank 19 to react with the calcium hydroxide emulsion to produce a calcium chloride solution and a magnesium hydroxide solution. The lower layer of calcium sulfate mud is transported to the bottom ash storage tank (not shown) for recycling.
接著，將反應槽19中產生的氯化鈣溶液與氫氧化鎂溶液輸送至第二分離槽24，產生沈澱作用，分成上層氯化鈣溶液及下層氫氧化鎂溶液。上層氯化鈣溶液流回底灰攪拌池15與來自氧化槽14中的硫酸鎂溶液反應。下層的氫氧化鎂水溶液則輸送至氫氧化鎂緩衝槽23後，再輸送至吸收塔13中作為循環吸收液。 Next, the calcium chloride solution and the magnesium hydroxide solution generated in the reaction tank 19 are sent to the second separation tank 24 to cause precipitation, and are divided into an upper calcium chloride solution and a lower magnesium hydroxide solution. The upper calcium chloride solution is returned to the bottom ash agitation tank 15 to react with the magnesium sulfate solution from the oxidation tank 14. The lower magnesium hydroxide aqueous solution is sent to the magnesium hydroxide buffer tank 23, and then sent to the absorption tower 13 as a circulating absorption liquid.
(二)零廢水排放： (2) Zero wastewater discharge:
由上述可知，本發明之廢水處理系統多次循環處理廢水中物質，回收氫氧化鎂溶液。本發明在小場地中即可使用，形成一種「再生回收」之處理系統，不會有廢水排放至外部之困擾。 As apparent from the above, the wastewater treatment system of the present invention recycles the substance in the wastewater a plurality of times to recover the magnesium hydroxide solution. The invention can be used in a small field to form a "recycling and recycling" treatment system, which does not have the trouble of discharging waste water to the outside.
(三)本發明之廢水處理系統中的化學反應： (iii) Chemical reactions in the wastewater treatment system of the present invention:
1.於吸收塔13中，有下列之反應：Mg(OH)2+SO2 → MgSO3+H2O MgSO3+SO2+H2O → Mg(HSO3)2 1. In the absorption column 13, there is the following reaction: Mg(OH) 2 + SO 2 → MgSO 3 + H 2 O MgSO 3 + SO 2 + H 2 O → Mg(HSO 3 ) 2
2.上述MgSO3與Mg(HSO3)2於氧化槽14中部份或絕大部份氧化成MgSO4，其反應式如下： MgSO3+1/2 O2+7 H2O → MgSO4．7H2O Mg(HSO3)2+O2+7 H2O → MgSO4．7H2O+H2SO4 2. The above MgSO 3 and Mg(HSO 3 ) 2 are partially or substantially oxidized to MgSO 4 in the oxidation tank 14, and the reaction formula is as follows: MgSO 3 + 1/2 O 2 + 7 H 2 O → MgSO 4 . 7H 2 O Mg(HSO 3 ) 2 +O 2 +7 H 2 O → MgSO 4 . 7H 2 O+H 2 SO 4
3.底灰攪拌池15中，有下列之反應：MgSO4+CaCl2 → MgCl2+CaSO4 3. In the bottom ash stirred tank 15, the following reaction is carried out: MgSO 4 + CaCl 2 → MgCl 2 + CaSO 4
4.反應槽19中，有下列之反應：Ca(OH)2+MgCl2 → Mg(OH)2+CaCl2 4. In the reaction tank 19, there is the following reaction: Ca(OH) 2 + MgCl 2 → Mg(OH) 2 + CaCl 2
以上所述僅為本發明之較佳實施例，非用以限定本發明之專利範圍，其他運用本發明之專利精神之等效變化，均應俱屬本發明之專利範圍。 The above is only the preferred embodiment of the present invention, and is not intended to limit the scope of the invention, and other equivalent variations of the patent spirit of the present invention are all within the scope of the invention.
10‧‧‧氧化鎂儲槽 10‧‧‧Magnesium Oxide Storage Tank
11a、11b‧‧‧氧化鎂熱解槽 11a, 11b‧‧‧Magnesium oxide pyrolysis tank
12‧‧‧氫氧化鎂儲槽 12‧‧‧Magnesium Hydroxide Storage Tank
13‧‧‧吸收塔 13‧‧‧ absorption tower
14‧‧‧氧化槽 14‧‧‧oxidation tank
15‧‧‧底灰攪拌池 15‧‧‧ bottom ash mixing tank
16‧‧‧氯化鈣儲槽 16‧‧‧ calcium chloride storage tank
17‧‧‧第一分離槽 17‧‧‧First separation tank
18‧‧‧鍋爐水封 18‧‧‧Boiler water seal
19‧‧‧反應槽 19‧‧‧Reaction tank
20‧‧‧氧化鈣貯槽 20‧‧‧calcium oxide storage tank
21a、21b‧‧‧氧化鈣攪拌槽 21a, 21b‧‧‧ Calcium Oxide Stirring Tank
22‧‧‧氫氧化鈣儲槽 22‧‧‧calcium hydroxide storage tank
23‧‧‧氫氧化鎂緩衝槽 23‧‧‧Magnesium hydroxide buffer tank
24‧‧‧第二分離槽 24‧‧‧Second separation tank
130‧‧‧除霧器 130‧‧‧ defogger
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Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW100142189A TWI457167B (en) | 2011-11-18 | 2011-11-18 | Apparatus for flue gas desulfurization with zero emission using system for recovery and recycle of magnesium hydroxide |
| CN2012100674664A CN102553418A (en) | 2011-11-18 | 2012-03-15 | Zero-emission magnesium hydroxide regeneration and recovery system of steam-electric desulfurization equipment |
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| Application Number | Priority Date | Filing Date | Title |
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| TW100142189A TWI457167B (en) | 2011-11-18 | 2011-11-18 | Apparatus for flue gas desulfurization with zero emission using system for recovery and recycle of magnesium hydroxide |
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| Publication Number | Publication Date |
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| TW201321071A TW201321071A (en) | 2013-06-01 |
| TWI457167B true TWI457167B (en) | 2014-10-21 |
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| TW100142189A TWI457167B (en) | 2011-11-18 | 2011-11-18 | Apparatus for flue gas desulfurization with zero emission using system for recovery and recycle of magnesium hydroxide |
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| CN104959012A (en) * | 2015-04-17 | 2015-10-07 | 熊天渝 | Magnesium-calcium based wet method desulphurization system and method for removing sulfur dioxide in flue gas and producing gypsum |
| CN105858692B (en) * | 2016-05-13 | 2017-12-15 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of method of lime method processing magnesium sulfate and magnesium sulfite waste water |
| CN106865827A (en) * | 2017-03-31 | 2017-06-20 | 湖南求是检测科技有限公司 | Sewage water treatment method and processing system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1143535A (en) * | 1995-08-22 | 1997-02-26 | 东洋工程株式会社 | Exhaust gas desulfurization process |
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| ATE147369T1 (en) * | 1991-11-20 | 1997-01-15 | Mitsubishi Heavy Ind Ltd | METHOD FOR PRODUCING SOLID SHAPED BODIES FROM BY-PRODUCTS OF THE LIME-GYPSUM WET DESULFURIZATION OF EXHAUST GASES |
| JP2000107559A (en) * | 1998-10-01 | 2000-04-18 | Chiyoda Engineering Kk | Fly ash and flue gas treatment method |
| TW508264B (en) * | 2001-12-25 | 2002-11-01 | Long Chen Paper Co Ltd | Discharge and regeneration system for cogeneration desulfurization device with zero discharge |
| CN1520921A (en) * | 2003-01-28 | 2004-08-18 | 荣成纸业股份有限公司 | Zero discharge and regeneration recovery system of steam-electric sweetener |
| CN101574619B (en) * | 2009-06-09 | 2012-07-04 | 陆泳凯 | Flue gas desulfurization process through calc-alkaline regeneration magnesium sulfite cycle absorption method |
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| CN1143535A (en) * | 1995-08-22 | 1997-02-26 | 东洋工程株式会社 | Exhaust gas desulfurization process |
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| TW201321071A (en) | 2013-06-01 |
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