JP4537268B2 - Gravity settling tank - Google Patents

Gravity settling tank Download PDF

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JP4537268B2
JP4537268B2 JP2005182050A JP2005182050A JP4537268B2 JP 4537268 B2 JP4537268 B2 JP 4537268B2 JP 2005182050 A JP2005182050 A JP 2005182050A JP 2005182050 A JP2005182050 A JP 2005182050A JP 4537268 B2 JP4537268 B2 JP 4537268B2
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solid content
wall
supernatant
gravity
stirring blade
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JP2007000735A (en
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敦志 古谷
裕隆 金丸
憲幸 奥山
和幸 永川
直司 多田
真一 松田
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Kobe Steel Ltd
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Description

本発明は、重力沈降法によりスラリーを固形分濃縮液と上澄み液とに分離するための重力沈降槽に関するものである。   The present invention relates to a gravity sedimentation tank for separating a slurry into a solid concentrate and a supernatant by a gravity sedimentation method.

例えば、スラリーを固形分と液とに分離するには膜分離、遠心分離など、さまざまな方式があるが、重力沈降法を用いる重力沈降槽は構造が簡素で最も経済的な方式である。この重力沈降槽が開示されているものとして下記特許文献１がある。
特開２００５−４６７８６号公報 For example, there are various methods such as membrane separation and centrifugal separation for separating the slurry into solid and liquid, but the gravity settling tank using the gravity settling method has the simple structure and the most economical method. Patent Document 1 listed below discloses this gravity settling tank.
JP-A-2005-46786

本発明者らは、この特許文献１と同様の重力沈降槽で、石炭を溶剤中で加熱抽出したあとのスラリーを上澄み液（抽出液）と固形分濃縮液とに分離しようとしたが、抽出液中の溶質が再析出してしまい、分離効率が著しく低下してしまう現象が認められた。   The inventors tried to separate the slurry after the coal was heated and extracted in a solvent in the same gravity sedimentation tank as in Patent Document 1, but separated into a supernatant (extract) and a solid concentrate. A phenomenon was observed in which the solute in the liquid reprecipitated and the separation efficiency was significantly reduced.

本発明はこのような状況に鑑み、石炭の溶媒抽出プロセスに係る反応性に富んだスラリー等でも分離できる重力沈降槽を提供することにある。   In view of such a situation, the present invention is to provide a gravity sedimentation tank capable of separating even a slurry having a high reactivity related to a solvent extraction process of coal.

課題を解決するための手段及び効果Means and effects for solving the problems

発明者らは上記課題を解決すべく鋭意検討を重ねた結果、重力沈降槽を外部から例えば３００〜４００℃程度まで加温し、抽出液、及び固形分濃縮液を３００〜４００℃に保温することによって、溶質の再析出を防止できることなどを見出した。しかしながら、分離が進行し固形分の濃縮が進むと重力沈降槽の内壁に固形分が固着するという新たな問題が発生した。この現象を解明すべく更に検討を行った結果、筒状胴部と逆円錐形状の底部の境界付近で流動性が低下することによるよどみが生じ、壁面からの加熱保温による熱変性が起こり、よどみ部分で固形分が壁面に固着するという現象が起こるためであることを突き止め、本件発明を想到するに至った。   As a result of intensive studies to solve the above-mentioned problems, the inventors warmed the gravity sedimentation tank from the outside to, for example, about 300 to 400 ° C., and kept the extract and the solid content concentrate at 300 to 400 ° C. It has been found that solute reprecipitation can be prevented. However, as separation progresses and solids concentration progresses, a new problem arises that solids adhere to the inner wall of the gravity settling tank. As a result of further investigation to clarify this phenomenon, stagnation occurs due to the decrease in fluidity near the boundary between the cylindrical body and the bottom of the inverted conical shape, and thermal denaturation occurs due to heat insulation from the wall surface. As a result, the present inventors have come up with the present invention by ascertaining that the phenomenon in which the solid content sticks to the wall surface occurs at the portion.

即ち、本発明は、筒状の胴部と、逆円錐形状の底部とを備え、石炭を溶剤中で加熱抽出したあとのスラリー中の固形分を沈降させて固形分濃縮液と上澄み液に分離する重力沈降槽であって、前記胴部の下端部内壁及び前記底部の内壁に沿って回転自在であり、沈降した前記固形分濃縮液を攪拌する攪拌翼と、前記胴部及び／又は前記底部を加熱する加熱手段とをさらに備え、前記攪拌翼は、前記胴部の下端部内壁及び前記底部の内壁に沿った形状に形成されていることを特徴とする。 That is, the present invention comprises a cylindrical body and an inverted conical bottom, and precipitates solids in the slurry after heat extraction of coal in a solvent to separate it into a solids concentrate and a supernatant. A gravity settling tank, which is rotatable along a lower end inner wall and a bottom inner wall of the barrel, and agitating blades for stirring the settled solid concentrate, the barrel and / or the bottom The stirring blade is formed in a shape along the inner wall of the lower end portion of the trunk portion and the inner wall of the bottom portion .

本発明によれば、胴部や底部の壁面の加熱によってスラリーが加温されるために、一度溶出した抽出液中の溶質の再析出を防止することができる。その上、撹拌翼の回転によって胴部下端部や底部の固形分濃縮液をゆっくりと流動させることによって胴部下端部および底部への固形分の初期付着を防止し、仮に付着してもその固形分を攪拌翼によって掻き取ることができるので、重力沈降槽の有効容積を減少させずに保持できる。つまり、溶質の再析出を防止することができる上、底部内壁だけでなく胴部下端部における固形分の付着を防止し、有効容積低下を抑制できる重力沈降槽を提供することができる。   According to the present invention, since the slurry is heated by heating the wall surface of the trunk portion and the bottom portion, it is possible to prevent re-precipitation of the solute in the extracted solution once eluted. In addition, the solid content concentrate at the lower end of the barrel and the bottom slowly flows by the rotation of the stirring blade to prevent initial solids from adhering to the lower end and the bottom of the barrel, Since the minute can be scraped off by the stirring blade, the effective volume of the gravity settling tank can be maintained without decreasing. That is, it is possible to provide a gravity sedimentation tank that can prevent reprecipitation of the solute and prevent the solid content from adhering not only to the inner wall of the bottom part but also to the lower end part of the body part and suppress the decrease in effective volume.

本発明の重力沈降槽は、前記胴部の上端に設けられた蓋部と、前記蓋部に貫設され、加圧条件下で分離された前記上澄み液を水平方向又は水平方向に対し所定角度の方向から流入させる開口部を先端に有している上澄み液排出管とをさらに備えていることが好ましい。   The gravity sedimentation tank of the present invention includes a lid portion provided at an upper end of the body portion, and the supernatant liquid penetrating the lid portion and separated under a pressurized condition at a predetermined angle with respect to a horizontal direction or a horizontal direction. It is preferable to further include a supernatant liquid discharge pipe having an opening at the tip thereof that flows in from the direction.

本発明によれば、沈降した固形分が、分離した固形分がほとんど分離された後のスラリー（ほぼ溶媒のみとなっている状態の溶液）の上向流に巻き上げられてしまうことを防止できるので、小型の重力沈降槽においても効率的な上澄み液の回収を行うことができる。また、固形分が難沈降性粒子のスラリーについても固形分濃縮液と上澄み液との分離を効率よく行うことができる。したがって、重力沈降槽の拡大による設備コストの増大や、処理量の低下などが原因の生産コストの増大を抑止できる。   According to the present invention, it is possible to prevent the settled solid content from being wound up in the upward flow of the slurry after the separated solid content is almost separated (a solution in a state of being almost solvent only). The supernatant can be efficiently recovered even in a small gravity sedimentation tank. In addition, the solid content liquid and the supernatant liquid can be efficiently separated from the slurry having the solid content of hardly settled particles. Therefore, it is possible to suppress an increase in production cost due to an increase in equipment cost due to the enlargement of the gravity sedimentation tank and a decrease in the processing amount.

次に、本発明の実施形態に係る重力沈降槽について説明する。図１は、本発明の実施形態に係る重力沈降槽を用いた低灰分高品質である石炭を製造するための固液分離装置の模式構成図である。図２は、図１に示した重力沈降槽の拡大断面図である。   Next, a gravity sedimentation tank according to an embodiment of the present invention will be described. FIG. 1 is a schematic configuration diagram of a solid-liquid separation apparatus for producing coal having high ash content and high quality using a gravity sedimentation tank according to an embodiment of the present invention. FIG. 2 is an enlarged cross-sectional view of the gravity settling tank shown in FIG.

本発明の実施形態に係る重力沈降槽を用いた固液分離装置１００は、粉体原料（石炭）と溶剤とを混合し、スラリーを生成するタンク１と、タンク１からスラリーを供給するためのポンプ２と、スラリーを加温するための予熱器３と、抽出処理を行う抽出槽４と、重力沈降を行って固形分を沈降させ、スラリーを抽出液（上澄み液、又は、上澄み液を含む溶液）と固形分濃縮液とに分離する重力沈降槽５と、この重力沈降槽５内で沈降した固形分濃縮液を回収する固形分濃縮液受器６と、重力沈降槽５内で分離された抽出液の上澄み液をろ過するフィルター部材７を有するフィルターユニット８と、上澄み液を回収する上澄み液受器９とを備えてなる。なお、抽出槽４、重力沈降槽５、固形分濃縮液受器６、及び上澄み液受器９のそれぞれの槽内には、攪拌機１０〜１３がそれぞれ設置されている。   A solid-liquid separation device 100 using a gravity sedimentation tank according to an embodiment of the present invention mixes a powder raw material (coal) and a solvent, generates a slurry, and supplies the slurry from the tank 1. The pump 2, the preheater 3 for heating the slurry, the extraction tank 4 for performing the extraction treatment, the gravity sedimentation is performed to settle the solid content, and the slurry is extracted liquid (supernatant liquid or supernatant liquid is included. Solution) and solid content concentrate, separated in the gravity sedimentation tank 5, solid content receiver 6 for collecting the solid content settled in the gravity sedimentation tank 5, and gravity sedimentation tank 5. A filter unit 8 having a filter member 7 for filtering the supernatant of the extracted liquid and a supernatant liquid receiver 9 for recovering the supernatant are provided. In each of the extraction tank 4, the gravity sedimentation tank 5, the solid content receiver 6, and the supernatant liquid receiver 9, stirrers 10 to 13 are installed.

重力沈降槽５は、中心軸が鉛直方向になるように構成された筒状の胴部１４と、この胴部１４の下端に設けられた逆円錐形状の底部１５と、攪拌機１１（駆動装置は図示せず）の一部であって、沈降した固形分濃縮液を攪拌する攪拌翼１６と、胴部１４及び／又は底部１５を加熱するヒータ（図示せず）と、胴部１４の上端部を密閉する蓋部１７と、蓋部１７に貫設され、胴部１４の下部まで延設されたスラリー供給管１８と、蓋部１７に貫設され、胴部１４の上部まで延設されており、加圧条件下で分離された溶媒の上澄み液を水平方向から流入させる開口部１９を先端に有している上澄み液排出管２０とを備えてなる。   The gravity settling tank 5 includes a cylindrical body portion 14 having a central axis in a vertical direction, an inverted conical bottom portion 15 provided at the lower end of the body portion 14, and a stirrer 11 (the driving device is A stirring blade 16 that stirs the settled solid content concentrate, a heater (not shown) that heats the body 14 and / or the bottom 15, and an upper end of the body 14. A lid portion 17 that seals the slurry, a slurry supply pipe 18 that extends through the lid portion 17 and extends to the lower portion of the body portion 14, and extends through the lid portion 17 and extends to the upper portion of the body portion 14. And a supernatant liquid discharge pipe 20 having an opening 19 at the tip for allowing the supernatant liquid of the solvent separated under pressure to flow in from the horizontal direction.

底部１５は、先端部（図２における底部１５最下部）に固形分濃縮液を固形分濃縮液受器６に排出するための排出口１５ａを有している。   The bottom 15 has a discharge port 15 a for discharging the solid content concentrate to the solid content receiver 6 at the tip (the bottom of the bottom 15 in FIG. 2).

攪拌翼１６は、胴部１４の下端部内壁及び底部１５の内壁に沿って回転自在なものである。例えば、図３（ａ）に示すように、２枚のブーメラン型形状の板である攪拌翼１６ａを、駆動装置からの駆動力を伝導する駆動力伝導棒２１ａとともにＴ字状部材を形成するように設けられた棒部材２２ａの各先端部に、駆動力伝導棒２１ａを中心として対照的に形成する。なお、図３（ｂ）に示すように、駆動力伝導棒２１ｂを中心として９０度毎に各棒部材２２ｂの先端部に攪拌翼１６ｂをそれぞれ設けた４枚方式であってもよい。又は図３（ｃ）に示すように、図３（ｂ）の変形例として、駆動力伝導棒２１ｃを中心として対照的に２枚のみ攪拌翼１６ｃを各棒部材２２ｃに設け、他の２枚として駆動力伝導棒２１ｃを中心として対照的に長方形状板２３を底部１５の内壁に沿って各棒部材２２ｃに設けるようなものであってもよい。なお、攪拌翼１６の設置数は、図３（ａ）〜（ｃ）に示したものに限られず、例えば１枚や３枚のもの、又は５枚以上のものであってもよい。また、攪拌翼１６ａ〜ｃのそれぞれは、各駆動力伝導棒２１ａ〜ｃに対して対照的に設けられていなくともよい。   The stirring blade 16 is rotatable along the inner wall of the lower end portion of the body portion 14 and the inner wall of the bottom portion 15. For example, as shown in FIG. 3A, a stirring blade 16a, which is two boomerang-shaped plates, is formed together with a driving force conducting rod 21a that conducts driving force from a driving device to form a T-shaped member. Contrastly, the driving force conducting rod 21a is formed at the tip of each of the rod members 22a provided at the center. In addition, as shown in FIG.3 (b), the 4 sheet system which each provided the stirring blade 16b in the front-end | tip part of each rod member 22b every 90 degree | times centering on the driving force conduction rod 21b may be sufficient. Alternatively, as shown in FIG. 3 (c), as a modification of FIG. 3 (b), only two stirring blades 16c are provided on each rod member 22c in contrast to the driving force conducting rod 21c, and the other two Alternatively, a rectangular plate 23 may be provided on each rod member 22c along the inner wall of the bottom portion 15 in contrast to the driving force conducting rod 21c. The number of the stirring blades 16 is not limited to that shown in FIGS. 3A to 3C, and may be one, three, or five or more, for example. Further, each of the stirring blades 16a to 16c may not be provided in contrast to the driving force conducting rods 21a to 21c.

なお、具体的な攪拌翼１６の設置位置は、攪拌翼１６における胴部１４の下端部内壁に沿って設けられている部分の先端が、胴部１４の下端から２０〜１００ｍｍ程度（好ましくは８０ｍｍ程度）上方に設置することが好ましい。短すぎると固形分の堆積を防止する効果が低く、長すぎると比較的澄んだ層や上澄み液まで攪拌してしまうことがあり、分離性能を低下させることがあるためである。また、攪拌翼１６の形状は、図３（ａ）〜（ｃ）に示したものに限られず、胴部１４の下端部内壁及び底部１５の内壁に沿って形成されているものであれば、どのようなものであってもよい。攪拌翼およびそれを支持する棒部材は攪拌により変形しない強度を有する程度の厚みが好ましい。厚すぎると有効面積を減少させるとともに攪拌翼や棒部材上面に固形分が堆積，固着するためである。攪拌翼，棒部材の上面は鋭角に加工されていれば，固形分の堆積を防止できるのでさらに好ましい。   The specific position of the stirring blade 16 is such that the tip of the portion of the stirring blade 16 provided along the inner wall of the lower end of the body portion 14 is about 20 to 100 mm (preferably 80 mm) from the lower end of the body portion 14. About) It is preferable to install upward. If it is too short, the effect of preventing the accumulation of solid content is low, and if it is too long, a relatively clear layer or supernatant may be stirred, which may reduce the separation performance. In addition, the shape of the stirring blade 16 is not limited to that shown in FIGS. 3A to 3C, as long as it is formed along the inner wall of the lower end portion of the trunk portion 14 and the inner wall of the bottom portion 15. Any thing is acceptable. The thickness of the stirring blade and the rod member that supports the stirring blade is preferably such that the stirring blade and the rod member that does not deform by stirring. If it is too thick, the effective area will be reduced and solid content will be deposited and fixed on the top surface of the stirring blade and bar member. If the upper surfaces of the stirring blade and the bar member are processed at an acute angle, it is more preferable because solid matter accumulation can be prevented.

開口部１９は、例えば、図４（ａ）〜（ｃ）に示されるものが挙げられる。以下それぞれを具体的に説明する。図４（ａ）に示す開口部１９ａは、上澄み液排出管２０の本管に接続及び連通が自在な管部材２４と、この管部材２４が中心に貫設されている円盤状部材２５と、この円盤状部材２５の管部材２４と反対側の面に９０°間隔で固設された板部材２６（図示していないが計４枚であり、管部材２４の先端部を閉塞してしまわないように設けられている）と、この板部材２６に対し円盤状部材２５と対照的に固設され、板部材２６及び円盤状部材２５と共に４つの流入口を形成する円盤状部材２７とを備えてなる。これにより、４つの流入口と管部材２４とは連通している構成を有しているものとなり、上澄み液を水平方向から流入させることができる。なお、板部材２６は必ずしも４枚用いていなければならないものではなく、管部材２４の先端部を閉塞してしまわないことを条件に、１枚以上用いるものであればよい。また、板部材２６のそれぞれの固設間隔は、規則正しいものでなくともよいし、用いる枚数によってその間隔を適宜変更してもよい。   Examples of the opening 19 include those shown in FIGS. 4 (a) to 4 (c). Each will be specifically described below. The opening 19a shown in FIG. 4 (a) includes a tube member 24 that can be connected to and communicated with the main tube of the supernatant liquid discharge tube 20, and a disk-like member 25 through which the tube member 24 penetrates at the center. Plate members 26 fixed on the surface of the disk-like member 25 opposite to the tube member 24 at intervals of 90 ° (not shown, but a total of four plates do not block the tip of the tube member 24). And a disk-shaped member 27 which is fixed to the plate member 26 in contrast to the disk-shaped member 25 and forms four inlets together with the plate member 26 and the disk-shaped member 25. It becomes. Thereby, the four inflow ports and the pipe member 24 are configured to communicate with each other, and the supernatant liquid can be introduced from the horizontal direction. Note that four plate members 26 are not necessarily used, and one or more plate members 26 may be used as long as the distal end portion of the tube member 24 is not blocked. Further, the fixed intervals of the plate members 26 may not be regular, and the intervals may be appropriately changed depending on the number of sheets used.

図４（ｂ）に示す開口部１９ｂは、上澄み液排出管２０の本管に接続及び連通が自在な管部材２８と、この管部材２８が中心に貫設されている四角形状部材２９と、この四角形状部材２９の管部材２８と反対側の面に中心と四角形状部材２９の角部とを結ぶ直線状に固設された板部材３０（図示していないが計４枚、管部材２８の先端部を閉塞してしまわないように設けられている）と、この板部材３０に対し四角形状部材２９と対照的に固設され、板部材３０及び四角形状部材２９と共に４つの流入口を形成する四角形状部材２９とを備えてなる。これにより、４つの流入口と管部材２８とは連通している構成を有しているものとなり、上澄み液を水平方向から流入させることができる。なお、板部材３０は必ずしも４枚用いていなければならないものではなく、管部材２８の先端部を閉塞してしまわないことを条件に、１枚以上用いるものであればよい。また、板部材３０のそれぞれの固設間隔は、中心と四角形状部材２９の角部とを結ぶ直線状になくともよいし、用いる枚数によってその間隔を適宜変更してもよい。   The opening 19b shown in FIG. 4 (b) includes a tube member 28 that can be connected to and communicated with the main tube of the supernatant liquid discharge tube 20, and a quadrangular member 29 through which the tube member 28 extends. A plate member 30 (four plates in total, not shown), which is fixed in a straight line connecting the center and the corner of the square member 29 on the surface of the square member 29 opposite to the tube member 28. In contrast, the plate member 30 is fixed to the plate member 30 in contrast to the square-shaped member 29, and four inlets are provided together with the plate member 30 and the square-shaped member 29. And a rectangular member 29 to be formed. As a result, the four inlets and the pipe member 28 are configured to communicate with each other, and the supernatant liquid can be introduced from the horizontal direction. Note that four plate members 30 are not necessarily used, and one or more plate members 30 may be used as long as the distal end portion of the tube member 28 is not blocked. Further, the fixing intervals of the plate members 30 do not have to be a straight line connecting the center and the corners of the quadrangular member 29, and the intervals may be appropriately changed depending on the number of sheets used.

図４（ｃ）に示す開口部１９ｃは、上澄み液排出管２０の本管に接続及び連通が自在な管部材３２と、この管部材３２が貫設され内部と連通している角筒状部材３３とを備えてなる。角筒状部材３３は、その一端及び多端それぞれに流入口を有している。   The opening 19c shown in FIG. 4C includes a tube member 32 that can be connected to and communicated with the main tube of the supernatant liquid discharge tube 20, and a rectangular tube-shaped member through which the tube member 32 extends and communicates with the inside. 33. The rectangular tubular member 33 has inflow ports at one end and multiple ends thereof.

なお、開口部１９は、図４（ａ）〜（ｃ）に示されるものに限られず、流入口のそれぞれが、水平方向に対し４５°程度まで下方に傾斜して設けられているものであってもよい。また、それぞれの流入口の傾斜の程度が異なるものであってもよい。   The openings 19 are not limited to those shown in FIGS. 4A to 4C, and each of the inlets is provided to be inclined downward to about 45 ° with respect to the horizontal direction. May be. Moreover, the degree of inclination of each inlet may be different.

次に、固液分離装置１００の動作について説明する。まず、タンク１において、粉体原料（石炭）と溶剤とを混合し、スラリーを生成させる。続いて、ポンプ２によってタンク１からスラリーを予熱器３に所定量供給し、スラリーを３００〜３７０℃程度まで加温する。そして、加温したスラリーを抽出槽４に所定量供給し，３００〜４００℃で加熱攪拌しながら抽出処理を行う。次に、抽出処理を行ったスラリーを、スラリー供給管１８を介して重力沈降槽５へ所定量供給し、重力沈降を行う。具体的には、スラリーを上澄み液と固形分濃縮液とに分離し、攪拌機１１によって胴部１４下端部及び底部１５付近に沈降した固形分濃縮液を攪拌するとともに、上澄み液を開口部１９を介して上澄み液排出管２０から所定量排出する。重力沈降槽内は，原料（石炭）から溶出した溶質の再析出を防止するため，３００〜４００℃に加熱される。このとき、攪拌機１１の攪拌翼１６は、胴部１４下端部及び底部１５の内壁に沿って数ｒｐｍ程度の回転数で回転させているので、固形分濃縮液の攪拌だけでなく、胴部１４下端部及び底部１５の内壁に付着した固形分を掻き取ることも行っている。そして、重力沈降槽５内で沈降した固形分濃縮液は、排出口１５ａから固形分濃縮液受器６に所定量排出・回収され、重力沈降槽５内から排出された上澄み液はフィルターユニット８によってろ過され、上澄み液受器９に回収される。   Next, the operation of the solid-liquid separator 100 will be described. First, in the tank 1, a powder raw material (coal) and a solvent are mixed to produce a slurry. Subsequently, a predetermined amount of slurry is supplied from the tank 1 to the preheater 3 by the pump 2, and the slurry is heated to about 300 to 370 ° C. Then, a predetermined amount of the heated slurry is supplied to the extraction tank 4 and an extraction process is performed while heating and stirring at 300 to 400 ° C. Next, a predetermined amount of the extracted slurry is supplied to the gravity settling tank 5 through the slurry supply pipe 18 to perform gravity settling. Specifically, the slurry is separated into a supernatant and a solid concentrate, and the solid concentrate that has settled near the lower end of the barrel 14 and the bottom 15 is stirred by the stirrer 11 and the supernatant is passed through the opening 19. A predetermined amount is discharged from the supernatant liquid discharge pipe 20. The gravity settling tank is heated to 300 to 400 ° C. to prevent reprecipitation of the solute eluted from the raw material (coal). At this time, the stirring blade 16 of the stirrer 11 is rotated at a rotational speed of about several rpm along the lower end portion of the body portion 14 and the inner wall of the bottom portion 15, so that the body portion 14 is not only stirred. The solid content adhered to the lower end and the inner wall of the bottom 15 is also scraped off. Then, a predetermined amount of the solid content liquid settled in the gravity sedimentation tank 5 is discharged and collected from the discharge port 15 a to the solid content liquid receiver 6, and the supernatant liquid discharged from the gravity sedimentation tank 5 is the filter unit 8. And collected in the supernatant liquid receiver 9.

上記実施形態によれば、重力沈降槽５の胴部１４や底部１５壁面の加熱によってスラリーが加温されるために、抽出液中の溶質の再析出を防止することができる。その上、撹拌翼１６の回転によって胴部１４下端部や底部１５の固形分濃縮液をゆっくりと流動させる胴部１４下端部および底部への固形分の初期付着を防止し、仮に付着してもその固形分を攪拌翼１６によって掻き取ることができるので、重力沈降槽５の有効容積を減少させずに保持できる。つまり、溶質の再析出を防止することができる上、底部１５内壁だけでなく胴部１４下端部における固形分の付着を防止し、容積減少にともなう沈降分離性能の低下を抑制できる重力沈降槽５を提供することができる。   According to the above embodiment, since the slurry is heated by heating the barrel 14 and the bottom 15 wall surface of the gravity settling tank 5, reprecipitation of the solute in the extract can be prevented. In addition, the rotation of the stirring blade 16 prevents the initial attachment of the solid content to the lower end portion and the bottom portion of the body portion 14 where the solid content concentrate at the lower end portion of the body portion 14 and the bottom portion 15 slowly flows, and even if temporarily attached. Since the solid content can be scraped off by the stirring blade 16, the effective volume of the gravity settling tank 5 can be maintained without decreasing. That is, the gravity settling tank 5 can prevent reprecipitation of the solute, and can prevent the solid content from adhering not only to the inner wall of the bottom portion 15 but also to the lower end portion of the trunk portion 14 and suppress the decrease in the sedimentation performance due to the volume reduction. Can be provided.

また、上記実施形態によれば、加圧条件下において、沈降した固形分が、分離した上澄み液側に巻き上げられてしまうことを防止できるので、小型の重力沈降槽５としても効率的な上澄み液の回収を行うことができる。また、分離される固形分が難沈降性粒子であるスラリーについても固形分と抽出液との分離を効率よく行うことができる。したがって、重力沈降槽５の拡大による設備コストの増大や、処理量の低下などが原因の生産コストの増大を抑止できる。   In addition, according to the above embodiment, it is possible to prevent the settled solid content from being wound up to the separated supernatant liquid side under the pressurized condition, so that the supernatant liquid is also effective as a small gravity sedimentation tank 5. Can be recovered. Moreover, also about the slurry whose solid content isolate | separated is a hard-to-settling particle | grain, a solid content and an extract can be isolate | separated efficiently. Therefore, it is possible to suppress an increase in production cost due to an increase in equipment cost due to the expansion of the gravity sedimentation tank 5 and a decrease in the processing amount.

次に、実施例及び比較例を示して、具体的に本発明を説明する。なお、下記実施例及び比較例で用いた重力沈降槽には、胴部の直径が２９０ｍｍ、高さ１０００ｍｍ（胴部の高さが７００ｍｍ、底部の高さが３００ｍｍ）、有効容積５０Ｌのものを用いた。   Next, an Example and a comparative example are shown and this invention is demonstrated concretely. The gravity sedimentation tank used in the following examples and comparative examples has a body diameter of 290 mm, a height of 1000 mm (a body height of 700 mm, a bottom height of 300 mm), and an effective volume of 50 L. Using.

（実施例１）
図１の固液分離装置１００と同構成の装置を用いて、本発明に係る重力沈降槽５の攪拌翼１６には図３（ａ）に示した形状と同様の攪拌翼を有する部材を用いた。具体的には、図５に示すように、駆動力伝導棒を嵌合固定可能な嵌合部４１と、この嵌合部４１に対し垂直に設けられた棒部材４２ａ〜４２ｄと、棒部材４２ａ、４２ｂによって固定支持された攪拌翼４３と、棒部材４２ｃ、４２ｄによって固定支持された攪拌翼４４とを有し、これらの各部位の中心線が同一平面状に存在している部材を用いた。なお、図５（ａ）は攪拌翼を有する部材の上視図、図５（ｂ）は図５（ａ）の正面図、図５（ｃ）は、図５（ｂ）の点線で囲った部位の一部断面図である。また、図５における寸法の単位はｍｍである。また、重力沈降槽５内において、攪拌翼４３、４４の上部先端が、胴部と底部との境界から８０ｍｍだけ上になるように、図５に示す部材を設置した。また、上澄み液排出管２０の開口部１９には図４（ａ）に示した構成のものであって、直径８０ｍｍの円盤２枚をこれらの間隙が１０ｍｍとなるように板４枚に固定したものを使用）について固形分の固着が発生するかを検証した。具体的には、上記固液分離装置におけるタンク１、ポンプ２、予熱器３、及び抽出槽４を用いて、メチルナフタレン８０ｗｔ％と石炭２０ｗｔ％との混合スラリーを３７０℃で抽出処理した後、内部を３５０℃に保温した重力沈降槽５に流量１５ｋｇ／ｈで導入し、重力沈降槽５の底部１５の排出口１５ａから１２ｋｇ／ｈで固形分を固形分濃縮液受器６に排出し、また、上澄み液排出管２０の開口部１９から３ｋｇ／ｈで抽出液の上澄み液を排出し、フィルターユニット８でろ過した後、上澄み液受器９に回収した上で検証を行った。 Example 1
A member having a stirring blade similar to the shape shown in FIG. 3 (a) is used for the stirring blade 16 of the gravity settling tank 5 according to the present invention using an apparatus having the same configuration as the solid-liquid separation device 100 of FIG. It was. Specifically, as shown in FIG. 5, a fitting portion 41 capable of fitting and fixing a driving force conducting rod, rod members 42a to 42d provided perpendicular to the fitting portion 41, and a rod member 42a. , 42b, and a stirring blade 44 fixedly supported by the rod members 42c and 42d, and a member in which the center lines of these portions are present on the same plane is used. . 5 (a) is a top view of a member having a stirring blade, FIG. 5 (b) is a front view of FIG. 5 (a), and FIG. 5 (c) is surrounded by a dotted line in FIG. 5 (b). It is a partial cross section figure of a site | part. Moreover, the unit of the dimension in FIG. 5 is mm. Moreover, the member shown in FIG. 5 was installed in the gravity settling tank 5 so that the upper tips of the stirring blades 43 and 44 would be 80 mm above the boundary between the trunk and the bottom. The opening 19 of the supernatant liquid discharge pipe 20 has the structure shown in FIG. 4A, and two disks having a diameter of 80 mm are fixed to the four plates so that the gap between them is 10 mm. It was verified whether solid matter sticking occurred. Specifically, after extracting the mixed slurry of methyl naphthalene 80 wt% and coal 20 wt% at 370 ° C. using the tank 1, pump 2, preheater 3, and extraction tank 4 in the solid-liquid separator, The inside was introduced at a flow rate of 15 kg / h into the gravity settling tank 5 kept at 350 ° C., and the solid content was discharged from the discharge port 15a at the bottom 15 of the gravity settling tank 5 to the solid content receiver 6 at 12 kg / h. Further, the supernatant of the extract was discharged from the opening 19 of the supernatant discharge pipe 20 at 3 kg / h, filtered through the filter unit 8, and then collected in the supernatant receiver 9 for verification.

（比較例１）
次に、比較例１として、重力沈降槽の攪拌翼及び上澄み液排出管の開口部の構成以外、図１と同様の構成を有する固液分離装置を用いて、重力沈降槽への固形分の固着が発生するかの検証を実施例１と同様の工程を用いて行った。なお、攪拌翼は底部にのみ沿って設けられている従来のもの（図３（ａ）における攪拌翼１６ａから胴部１４に沿って設けられた部位を取ったもの）であり、上澄み液排出管の開口部は、単なる筒状管部材の一端からなる流入口が一つのものである。 (Comparative Example 1)
Next, as Comparative Example 1, except for the configuration of the stirring blade of the gravity sedimentation tank and the opening of the supernatant liquid discharge pipe, the solid content in the gravity sedimentation tank was obtained using a solid-liquid separation device having the same configuration as in FIG. Whether or not the sticking occurred was verified using the same process as in Example 1. The stirring blade is a conventional one provided only along the bottom (taken from the stirring blade 16a in FIG. 3 (a) along the body 14), and the supernatant discharge pipe The opening has a single inlet formed of one end of a simple tubular tube member.

実施例１では、固液分離装置を約５０時間運転しても、重力沈降槽の内壁には固形分の固着は認められなかった。これに対し、比較例１では、約５０時間の運転中に重力沈降槽の内壁のうち、スラリー、抽出液、固形分濃縮液のいずれか一つ以上と接する部分全体において、厚さ３０ｍｍ程度の固形分の固着が生じた。   In Example 1, even if the solid-liquid separator was operated for about 50 hours, solid matter was not fixed on the inner wall of the gravity settling tank. On the other hand, in Comparative Example 1, the entire portion of the inner wall of the gravity settling tank that is in contact with one or more of the slurry, the extract, and the solid concentrate during the operation for about 50 hours has a thickness of about 30 mm. Solid matter sticking occurred.

以上に示すように、スラリー中の抽出液と固着性を有する固形分とを重力沈降により分離する実施例１の重力沈降槽において、逆円錐形状の底部を攪拌する攪拌翼を胴部の下端部の所定部分に達するように設けたので、攪拌翼が回転した際に、胴部下端部の内壁及び底部内壁への固形分の固着を防止し、有効容積を減少させずに保持でき、槽内部の清掃頻度を低下できた。その結果として、固液分離装置の安定した長時間の運転を可能にすることができた。   As described above, in the gravity settling tank of Example 1 that separates the extract in the slurry and the solid content having adhesiveness by gravity settling, the stirring blade that stirs the bottom of the inverted conical shape is provided at the lower end of the barrel. When the stirring blade rotates, it prevents solids from sticking to the inner wall of the lower end of the barrel and the inner wall of the bottom, and can be held without reducing the effective volume. The frequency of cleaning was reduced. As a result, the solid-liquid separation device can be operated stably for a long time.

（実施例２）
重力沈降槽５に流量１０ｋｇ／ｈで導入し、重力沈降槽５の底部１５の排出口１５ａから５ｋｇ／ｈで固形分を固形分濃縮液受器６に排出し、また、上澄み液排出管２０の開口部１９から５ｋｇ／ｈで抽出液の上澄み液を排出した以外、実施例１と同様の装置及び工程とし、重力沈降槽５から排出された上澄み液の固形分濃度と、フィルターユニット８の閉塞時間とを測定した。 (Example 2)
It is introduced into the gravity settling tank 5 at a flow rate of 10 kg / h, the solid content is discharged from the discharge port 15a at the bottom 15 of the gravity settling tank 5 to the solid content receiver 6 at 5 kg / h, and the supernatant discharge pipe 20 Except that the supernatant of the extract was discharged from the opening 19 at 5 kg / h, the apparatus and process were the same as in Example 1, and the solid content concentration of the supernatant discharged from the gravity sedimentation tank 5 and the filter unit 8 The occlusion time was measured.

（比較例２）
比較例１と同様の装置及び実施例２と同様の工程で、重力沈降槽５から排出された上澄み液の固形分濃度と、フィルターユニット８の閉塞時間とを測定した。 (Comparative Example 2)
In the same apparatus as in Comparative Example 1 and the same process as in Example 2, the solid content concentration of the supernatant discharged from the gravity sedimentation tank 5 and the blocking time of the filter unit 8 were measured.

実施例２では、上澄み液中の固形分濃度は０．８ｗｔ％であり、フィルターユニット８が閉塞するまでの時間は３５時間であった。これに対し、比較例２では、上澄み液中の固形分濃度は１．８ｗｔ％であり、フィルターユニット８が閉塞するまでの時間は２０時間であった。   In Example 2, the solid content concentration in the supernatant was 0.8 wt%, and the time until the filter unit 8 was blocked was 35 hours. On the other hand, in Comparative Example 2, the solid content concentration in the supernatant was 1.8 wt%, and the time until the filter unit 8 was blocked was 20 hours.

以上に示すように、実施例２においては、重力沈降槽５内の抽出液の固形分との再混合を抑止し、溢流する固形分を減少させることができるので、フィルターユニット８を長く使用することができる。   As described above, in Example 2, since remixing with the solid content of the extract in the gravity sedimentation tank 5 can be suppressed and the overflowing solid content can be reduced, the filter unit 8 is used for a long time. can do.

なお、本発明は、特許請求の範囲を逸脱しない範囲で設計変更できるものであり、上記実施形態や実施例に限定されるものではない。   The present invention can be changed in design without departing from the scope of the claims, and is not limited to the above-described embodiments and examples.

本発明の実施形態に係る重力沈降槽を用いた固液分離装置を示す模式構成図である。It is a schematic block diagram which shows the solid-liquid separation apparatus using the gravity sedimentation tank which concerns on embodiment of this invention. 図１に示した重力沈降槽の拡大断面図である。It is an expanded sectional view of the gravity settling tank shown in FIG. 図２の重力沈降槽で用いられる攪拌翼周辺の斜視図であって、（ａ）が２枚翼、（ｂ）が４枚翼、（ｃ）が（ｂ）の変形例を示す図である。FIG. 3 is a perspective view of the periphery of a stirring blade used in the gravity settling tank of FIG. 2, wherein (a) shows two blades, (b) shows four blades, and (c) shows a modification of (b). . 図２の重力沈降槽で用いられる上澄み液排出管の開口部を示す斜視図である。It is a perspective view which shows the opening part of the supernatant liquid discharge pipe used with the gravity settling tank of FIG. （ａ）は攪拌翼を有する部材の上視図、（ｂ）は（ａ）の正面図、（ｃ）は（ｂ）の点線で囲った部位の一部断面図である。(A) is a top view of the member which has a stirring blade, (b) is a front view of (a), (c) is a partial cross section figure of the site | part enclosed with the dotted line of (b).

符号の説明Explanation of symbols

１ タンク
２ ポンプ
３ 予熱器
４ 抽出槽
５ 重力沈降槽
６ 固形分濃縮液受器
７ フィルター部材
８ フィルターユニット
９ 上澄み液受器
１０、１１、１２、１３ 攪拌機
１４ 胴部
１５ 底部
１５ａ 排出口
１６、１６ａ、１６ｂ、１６ｃ 攪拌翼
１７ 蓋部
１８ スラリー供給管
１９、２３ 長方形状板
１９、１９ａ、１９ｂ、１９ｃ 開口部
２０ 上澄み液排出管
２１ａ、２１ｂ、２１ｃ 駆動力伝導棒
２２ａ、２２ｂ、２２ｃ 棒部材
２４、２８、３２ 管部材
２５、２７ 円盤状部材
２６、３０ 板部材
２９ 四角形状部材
３３ 角筒状部材
１００ 固液分離装置 DESCRIPTION OF SYMBOLS 1 Tank 2 Pump 3 Preheater 4 Extraction tank 5 Gravity sedimentation tank 6 Solid content concentrate receiver 7 Filter member 8 Filter unit 9 Supernatant liquid receiver 10, 11, 12, 13 Stirrer 14 Body 15 Bottom 15a Outlet 16, 16a, 16b, 16c Stirrer blade 17 Lid 18 Slurry supply pipe 19, 23 Rectangular plate 19, 19a, 19b, 19c Opening 20 Supernatant liquid discharge pipe 21a, 21b, 21c Driving force conducting rod 22a, 22b, 22c Bar member 24, 28, 32 Tube members 25, 27 Disc members 26, 30 Plate members 29 Square members 33 Square tubular members 100 Solid-liquid separator

Claims (2)

筒状の胴部と、逆円錐形状の底部とを備え、石炭を溶剤中で加熱抽出したあとのスラリー中の固形分を沈降させて固形分濃縮液と上澄み液とに分離する重力沈降槽であって、
前記胴部の下端部内壁及び前記底部の内壁に沿って回転自在であり、沈降した前記固形分濃縮液を攪拌する攪拌翼と、
前記胴部及び／又は前記底部を加熱する加熱手段とをさらに備え、
前記攪拌翼は、前記胴部の下端部内壁及び前記底部の内壁に沿った形状に形成されていることを特徴とする重力沈降槽。 A gravity settling tank that has a cylindrical body and an inverted conical bottom and settles solids in the slurry after heat extraction of coal in a solvent and separates it into a solid concentrate and a supernatant. There,
A stirring blade that is rotatable along the inner wall of the lower end portion of the trunk portion and the inner wall of the bottom portion, and stirs the settled solid content concentrate;
Heating means for heating the trunk and / or the bottom ,
The gravity settling tank is characterized in that the stirring blade is formed in a shape along an inner wall of a lower end portion of the body portion and an inner wall of the bottom portion . 前記胴部の上端に設けられた蓋部と、
前記蓋部に貫設され、加圧条件下で分離された前記上澄み液を水平方向又は水平方向に対し所定角度の方向から流入させる開口部を先端に有している上澄み液排出管とをさらに備えていることを特徴とする請求項１記載の重力沈降槽。 A lid portion provided at an upper end of the trunk portion;
A supernatant liquid discharge pipe penetrating through the lid part and having an opening at a tip thereof for allowing the supernatant liquid separated under pressure to flow in from a horizontal direction or a direction at a predetermined angle with respect to the horizontal direction; The gravity sedimentation tank according to claim 1, wherein the gravity sedimentation tank is provided.
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