JP4482673B2 - Fluidization method and treatment method of sulfuric acid pitch - Google Patents

Fluidization method and treatment method of sulfuric acid pitch Download PDF

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JP4482673B2
JP4482673B2 JP2003343153A JP2003343153A JP4482673B2 JP 4482673 B2 JP4482673 B2 JP 4482673B2 JP 2003343153 A JP2003343153 A JP 2003343153A JP 2003343153 A JP2003343153 A JP 2003343153A JP 4482673 B2 JP4482673 B2 JP 4482673B2
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sulfuric acid
container
acid pitch
pitch
fluidizing
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JP2005103485A (en
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浩之 小野
博重 山内
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Dowa Eco Systems Co Ltd
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Description

本発明は，石油製品の硫酸洗浄で発生する硫酸ピッチの流動化方法および処理方法に関する。 The present invention relates to a fluidizing method and a processing method for sulfuric acid pitch generated by sulfuric acid washing of petroleum products.

石油製品を精製するために行われる硫酸洗浄では，硫酸ピッチが発生する。かかる硫酸ピッチは有害ガスを発し，悪臭を生じさせるので，これを無害化する必要がある。硫酸ピッチの硬さは，ガム状のもの，キャラメル状のもの，飴状のもの，と様々である。一方，硫酸ピッチは発生時には多少の（例えば１０Ｐ程度の）流動性を有しているものの，時間の経過とともに徐々に固化する性質がある。通常，硫酸ピッチは，処理するまでの間，ドラム缶などに入れて運搬，保管されるが，長期間経過して固化した硫酸ピッチは，流動性がなく，ドラム缶内から容易に取り出せなくなってしまう。このため，硫酸ピッチを処理する際のハンドリング性が劣るといった難点がある。   In sulfuric acid cleaning performed to refine petroleum products, sulfuric acid pitch is generated. Such sulfuric acid pitch emits harmful gases and produces bad odors, which need to be rendered harmless. The hardness of sulfuric acid pitch varies from gum-like, caramel-like, and bowl-like. On the other hand, although sulfuric acid pitch has some fluidity (for example, about 10 P) when it is generated, it has the property of gradually solidifying over time. Normally, sulfuric acid pitch is transported and stored in drums until it is processed, but sulfuric acid pitch that has solidified over a long period of time is not fluid and cannot be easily removed from the drum. For this reason, there exists a difficulty that the handleability at the time of processing a sulfuric acid pitch is inferior.

最近，ドラム缶に詰めた硫酸ピッチが山野に不法投棄され，腐食したドラム缶から漏れ出た硫酸ピッチによって周辺環境が汚染される問題が顕在化している。そのような不法投棄された硫酸ピッチは，発見までに長期間経過してることが多く，ドラム缶が腐食・破損して液分が流出し固形分のみが残っていたり，あるいは，時間の経過によってドラム缶内で硫酸ピッチが固化して流動性を失い，ハンドリング性が悪くなっている場合が多い。   Recently, sulfuric acid pitch packed in drums has been illegally dumped in Yamano, and the problem of contaminating the surrounding environment due to sulfuric acid pitch leaking from corroded drums has become apparent. Such illegally dumped sulfuric acid pitch often passes for a long time until discovery, and the drum can corrodes and breaks down, and the liquid flows out and only the solid content remains, or the drum can over time. In many cases, sulfuric acid pitch solidifies and loses fluidity, resulting in poor handling.

そこで，硫酸ピッチを流動化させるために，特開昭５３−２９５８号公報には，固形分の硫酸ピッチを焼却炉の排熱を利用して６０〜８０℃に加熱し，液状化させることが開示されている。また，特開２００２−１３９９号公報には，硫酸ピッチに発煙硫酸，廃硫酸等の溶解剤を混合し，硫酸ピッチ中の固形分を溶解させて焙焼処理する方法が開示されている。   Therefore, in order to fluidize the sulfuric acid pitch, Japanese Patent Laid-Open No. 53-2958 discloses that the sulfuric acid pitch of solid content is heated to 60-80 ° C. using the exhaust heat of the incinerator and liquefied. It is disclosed. Japanese Patent Laid-Open No. 2002-1399 discloses a method in which a solubilizing agent such as fuming sulfuric acid or waste sulfuric acid is mixed with sulfuric acid pitch, and a solid content in the sulfuric acid pitch is dissolved and roasted.

特開昭５３−２９５８号公報Japanese Patent Laid-Open No. 53-2958 特開２００２−１３９９号公報JP 2002-1399 A

しかしながら，時間が経過して固化した硫酸ピッチは，６０〜８０℃に加熱してもわずかに流動性を増す程度である。不法投棄されて完全に固化したような硫酸ピッチは，もはや加熱しても流動化させることが困難である。一方，硫酸を用いて硫酸ピッチを溶解させる方法は，溶解時に大量の亜硫酸ガスを発生させるので，密閉性の高い中和設備やガス処理設備などが必要となってしまう。また，硫酸ピッチを硫酸で溶解させると，処理の困難な強酸性汚泥を多量に生じてしまう。そして従来の方法は，いずれも固化した硫酸ピッチを流動化させるには非常に長い時間がかかってしまう。   However, the sulfuric acid pitch solidified over time is only slightly increased in fluidity even when heated to 60-80 ° C. Sulfuric acid pitch that has been dumped illegally and completely solidified is difficult to fluidize even when heated. On the other hand, in the method of dissolving sulfuric acid pitch using sulfuric acid, a large amount of sulfurous acid gas is generated at the time of dissolution, which necessitates highly sealed neutralization equipment and gas processing equipment. In addition, when sulfuric acid pitch is dissolved with sulfuric acid, a large amount of strongly acidic sludge that is difficult to treat is produced. In each of the conventional methods, it takes a very long time to fluidize the solidified sulfuric acid pitch.

本発明の目的は，不法投棄物のような固化した硫酸ピッチでも，短時間で流動化させることにある。   An object of the present invention is to fluidize a solidified sulfuric acid pitch such as illegal dumping in a short time.

本発明によれば，硫酸ピッチと複数の粉砕媒体を容器内に入れ，容器内に分散溶媒であるＮａＯＨを添加して，容器を回転させ，前記容器内において，攪拌羽根によって粉砕媒体が持ち上げる運動と，攪拌羽根から粉砕媒体が落下させる運動を繰り返して行わせることにより，硫酸ピッチを流動化させることを特徴とする，硫酸ピッチの流動化方法が提供される。 According to the present invention, sulfuric acid pitch and a plurality of grinding media are put in a container, NaOH as a dispersion solvent is added to the container , the container is rotated, and the grinding medium is lifted by stirring blades in the container. And a method of fluidizing the sulfuric acid pitch, characterized by fluidizing the sulfuric acid pitch by repeatedly performing the movement of dropping the grinding medium from the stirring blade .

前記粉砕媒体は，例えば複数の粒状であり，金属もしくはセラミックスからなるボールが例示される。また，前記粉砕媒体は，例えば直径が２０〜７０ｍｍの鉄球である。 The pulverizing medium is, for example, a plurality of particles, and a ball made of metal or ceramics is exemplified . The grinding medium is an iron ball having a diameter of 20 to 70 mm, for example.

これら流動化方法によって流動化させた硫酸ピッチを焼却することもできる。   The sulfuric acid pitch fluidized by these fluidization methods can also be incinerated.

また，鉛直から傾斜した中心軸周りに回転駆動される容器を備え，該容器の内面に攪拌羽根が取り付けられていることを特徴とする，硫酸ピッチの流動化装置が提供される。 In addition, a sulfuric acid pitch fluidizing device is provided, which includes a container that is rotationally driven around a central axis inclined from the vertical, and has a stirring blade attached to the inner surface of the container.

前記容器には，例えば，硫酸ピッチと複数の粒状の粉砕媒体を容器内に出し入れさせる開口部が設けられており，該開口部を上方に向けた姿勢と下方に向けた姿勢とにさせるように容器を揺動させる揺動機構を備える。   For example, the container is provided with an opening through which the sulfuric acid pitch and a plurality of granular pulverizing media are taken in and out of the container, and the opening is configured to be in an upward orientation and a downward orientation. A rocking mechanism for rocking the container is provided.

硫酸ピッチと例えば複数の粒状の粉砕媒体を容器内に入れ，容器内に分散溶媒であるＮａＯＨを添加して，容器を回転させることにより，不法投棄物のような固化した硫酸ピッチでも，大量の亜硫酸ガスを発生させずに，短時間で流動化させることができる。容器の内面に攪拌羽根を取り付け，容器を鉛直から傾斜した中心軸周りに回転させることにより，容器の回転に伴って，攪拌羽根によって容器内の硫酸ピッチと粉砕媒体が持ち上げられる運動と，攪拌羽根から硫酸ピッチと粉砕媒体が落下する運動が繰り返して行われる。これにより，硫酸ピッチの粉砕が促進される。こうして粉砕され，流動化した硫酸ピッチはハンドリング性に優れ，例えば，硫酸ピッチを焼却炉に投入して焼却処理することも可能である。 A large amount of sulfuric acid pitch, such as illegally dumped waste, can be obtained by placing sulfuric acid pitch and, for example, a plurality of granular grinding media in a container, adding NaOH as a dispersion solvent into the container, and rotating the container. It can be fluidized in a short time without generating sulfurous acid gas. By attaching a stirring blade to the inner surface of the container and rotating the container around a central axis inclined from the vertical, the movement of the sulfuric acid pitch and the grinding medium in the container to be lifted by the stirring blade as the container rotates, and the stirring blade The movement of dropping the sulfuric acid pitch and the grinding media is repeated. This promotes the pulverization of sulfuric acid pitch. The sulfuric acid pitch thus pulverized and fluidized is excellent in handling properties. For example, the sulfuric acid pitch can be put into an incinerator and incinerated.

以下，本発明の好ましい実施の形態を図面を参照に説明する。図１は，容器１０の開口部１１を上に向けた姿勢を示す本発明の実施の形態にかかる流動化装置１の側面図である。図２は，容器１０の開口部１１を下に向けた姿勢を示す流動化装置１の側面図である。図３は，容器１０の縦断面図である。図４は，開口部１１から容器１０の内部を見た状態を示す図面である。   Hereinafter, preferred embodiments of the present invention will be described with reference to the drawings. FIG. 1 is a side view of a fluidizing apparatus 1 according to an embodiment of the present invention showing a posture in which the opening 11 of the container 10 is directed upward. FIG. 2 is a side view of the fluidizing apparatus 1 showing a posture in which the opening 11 of the container 10 is directed downward. FIG. 3 is a longitudinal sectional view of the container 10. FIG. 4 is a view showing a state in which the inside of the container 10 is viewed from the opening 11.

流動化装置１は，略紡錘体形状をなす容器１０を備えている。容器１０の上面は開口部１１になっている。後述するように，この開口部１１を通じて，容器１０の内部に硫酸ピッチａと複数の粒状の粉砕媒体ｂが出し入れされるようになっている。   The fluidizing apparatus 1 includes a container 10 having a substantially spindle shape. The upper surface of the container 10 is an opening 11. As will be described later, through this opening 11, the sulfuric acid pitch a and a plurality of granular grinding media b are taken in and out of the container 10.

容器１０の胴部には，容器１０を回転自在に支持するリング形状の軸受部材１２が装着してある。軸受部材１２は，ベース１５に立設された支柱１６の上端に軸１７を介して回転自在に支持されている。また，軸受部材１２には，開口部１１の方向に延びるリンク２０が取付けてある。一方，ベース１５には，容器１０を揺動させる揺動機構としてのシリンダー装置２１の下端が回転自在に取り付けてある。リンク２０の先端には，このシリンダー装置２１のピストンロッド２２の先端が，回転自在に接続されている。   A ring-shaped bearing member 12 that rotatably supports the container 10 is attached to the body of the container 10. The bearing member 12 is rotatably supported via a shaft 17 on the upper end of a support column 16 provided upright on the base 15. Further, a link 20 extending in the direction of the opening 11 is attached to the bearing member 12. On the other hand, a lower end of a cylinder device 21 as a swinging mechanism for swinging the container 10 is rotatably attached to the base 15. The tip of the piston rod 22 of the cylinder device 21 is rotatably connected to the tip of the link 20.

ここで，図１は，シリンダー装置２１の伸張稼動によってピストンロッド２２が伸びた状態を示している。このようにシリンダー装置２１が伸張稼動した場合は，リンク２０の先端が上方に持ち上げられ，それに伴って，容器１０は軸１７を中心にして開口部１１を斜め上方に向けた姿勢に（図１中において反時計回転方向に）揺動するようになっている。   Here, FIG. 1 shows a state in which the piston rod 22 is extended by the extension operation of the cylinder device 21. In this way, when the cylinder device 21 is extended, the tip of the link 20 is lifted upward, and accordingly, the container 10 is in a posture in which the opening 11 is directed obliquely upward about the shaft 17 (FIG. 1). (In the counterclockwise direction).

軸受部材１２にはモータ２５が取付けてあり，このモータ２５の回転動力が容器１０に伝達されて，容器１０が軸受部材１２の内側において回転するようになっている。図１に示すように，シリンダー装置２１の伸張稼動で容器１０の開口部１１が斜め上方に向けられた姿勢では，軸受部材１２に支持された容器１０の回転中心は，鉛直から傾斜した中心軸Ｌ（容器１０の開口部１１が斜め上方に向けるように鉛直から傾斜した中心軸Ｌ）に一致するようになっている。そして，このように中心軸Ｌを回転中心にして開口部１１を斜め上方に向けた姿勢で，モータ２５の回転動力で容器１０が回転するようになっている。   A motor 25 is attached to the bearing member 12, and the rotational power of the motor 25 is transmitted to the container 10 so that the container 10 rotates inside the bearing member 12. As shown in FIG. 1, when the cylinder device 21 is extended and the opening 11 of the container 10 is directed obliquely upward, the rotation center of the container 10 supported by the bearing member 12 is a central axis inclined from the vertical. L (center axis L inclined from the vertical so that the opening 11 of the container 10 faces obliquely upward). The container 10 is rotated by the rotational power of the motor 25 in such a posture that the opening 11 is directed obliquely upward with the central axis L as the rotation center.

一方，図２は，シリンダー装置２１の短縮稼動によってピストンロッド２２が縮んだ状態を示している。このようにシリンダー装置２１が短縮稼動した場合は，リンク２０の先端が下方に引下げられ，それに伴って，容器１０は軸１７を中心にして開口部１１を斜め下方に向けた姿勢に（図２中において時計回転方向に）揺動するようになっている。   On the other hand, FIG. 2 shows a state where the piston rod 22 is contracted by the shortening operation of the cylinder device 21. In this way, when the cylinder device 21 is shortened, the tip of the link 20 is pulled downward, and accordingly, the container 10 is in a posture in which the opening 11 is directed obliquely downward about the shaft 17 (FIG. 2). (In the clockwise direction).

図３，４に示すように，略紡錘体形状をなす容器１０の底側の内周面には，容器１０の内部に向って突出する４枚の攪拌羽根３０が取り付けられている。これら攪拌羽根３０は，いずれも，容器１０の底面から開口部１１に向う方向に沿って配置されている。   As shown in FIGS. 3 and 4, four stirring blades 30 projecting toward the inside of the container 10 are attached to the inner peripheral surface of the bottom side of the container 10 having a substantially spindle shape. These stirring blades 30 are all arranged along the direction from the bottom surface of the container 10 toward the opening 11.

前述のように，中心軸Ｌを回転中心にして開口部１１を斜め上方に向けた姿勢で，モータ２５の回転動力で容器１０が回転することにより，これら攪拌羽根３０も，中心軸Ｌを回転中心にして回転し，攪拌羽根３０は中心軸Ｌの下側と中心軸Ｌの上側を交互に移動するようになっている。そして，後述するように，攪拌羽根３０が下方から上方に移動する際には，容器１０の内部に入れられた硫酸ピッチａと粉砕媒体ｂを，攪拌羽根３０によって掻き上げて行くようになっている。一方，攪拌羽根３０が上方まで移動した際，あるいは，更に上方から下方に移動する際には，攪拌羽根３０によって掻き上げられた硫酸ピッチａと粉砕媒体ｂが攪拌羽根３０から離れて落下し，容器１０の底部に衝突するようになっている。   As described above, when the container 10 is rotated by the rotational power of the motor 25 with the opening 11 directed obliquely upward with the central axis L as the rotation center, the stirring blades 30 also rotate the central axis L. The stirring blade 30 rotates about the center, and moves alternately below the center axis L and above the center axis L. As will be described later, when the stirring blade 30 moves from the lower side to the upper side, the sulfuric acid pitch a and the pulverizing medium b put in the container 10 are scraped up by the stirring blade 30. Yes. On the other hand, when the stirring blade 30 moves upward, or further moves downward from above, the sulfuric acid pitch a and the pulverization medium b picked up by the stirring blade 30 fall away from the stirring blade 30, It collides with the bottom of the container 10.

さて，以上のように構成された流動化装置１にあっては，予め，シリンダー装置２１を伸張稼動させることにより，容器１０を軸１７を中心にして図１中において反時計回転方向に揺動させ，図１に示すように，容器１０の開口部１１を斜め上方に向けた姿勢にする。これにより，軸受部材１２に支持された容器１０の回転中心を，鉛直から傾斜した中心軸Ｌ（容器１０の開口部１１を斜め上方に向けるように鉛直から傾斜した中心軸Ｌ）に一致させる。   Now, in the fluidizing device 1 configured as described above, the container device 10 is swung in the counterclockwise direction in FIG. Then, as shown in FIG. 1, the opening 11 of the container 10 is in a posture directed obliquely upward. Thereby, the rotation center of the container 10 supported by the bearing member 12 is made to coincide with the central axis L inclined from the vertical (the central axis L inclined from the vertical so that the opening 11 of the container 10 is directed obliquely upward).

そして，斜め上方に向けた開口部１１から，容器１０の内部に硫酸ピッチａと複数の粒状の粉砕媒体ｂを投入する。硫酸ピッチａは，例えばガソリン，灯油，軽油，重油，潤滑油などといった石油製品の精製あるいは再生油の製造などにおいて行われる硫酸洗浄で生ずるものであり，例えばタール油，石油製品中の硫黄分，アスファルト質，ガム状物質，各種スルホン酸，硫酸等を含み，そのままでは有害な亜硫酸ガスを発生する。容器１０内に投入される硫酸ピッチａの性状は，ガム状のもの，キャラメル状のもの，飴状のもの，と様々である。時間の経過によって固化した流動性のない硫酸ピッチａであっても良い。   Then, sulfuric acid pitch a and a plurality of granular grinding media b are introduced into the container 10 from the opening 11 directed obliquely upward. Sulfuric acid pitch a is produced by sulfuric acid washing performed in, for example, refining petroleum products such as gasoline, kerosene, light oil, heavy oil, and lubricating oil, or producing reclaimed oil. For example, tar oil, sulfur content in petroleum products, Contains asphalt, gum-like substances, various sulfonic acids, sulfuric acid, etc., and produces harmful sulfurous acid gas. The properties of the sulfuric acid pitch a put into the container 10 are various, such as gum, caramel, and bowl. The non-fluidic sulfuric acid pitch a solidified with the passage of time may be used.

硫酸ピッチａと一緒に容器１０内に投入される粉砕媒体ｂとは，例えば，金属もしくはセラミックスからなるボールであり，直径が２０〜７０ｍｍの鉄球などが例示される。粉砕媒体ｂは，市販されているもので良い。また，その形状は，球状以外の棒状などでも良い。容器１０内への粉砕媒体ｂの投入量は，硫酸ピッチａ中の固形分の量によるが，容器１０内へ投入される硫酸ピッチａの固形分に対して例えば５〜１０重量倍程度である。特に硫酸ピッチａの固形分が大きい場合は，大きな衝撃破壊力を得る必要があるため，大きい粉砕媒体ｂを多く使用すると良い。逆に硫酸ピッチａの固形分が小さい場合は，接触磨り剥がし効果を得るために小さい粉砕媒体ｂをも多く使用すると良い。   The grinding medium b put into the container 10 together with the sulfuric acid pitch a is, for example, a ball made of metal or ceramics, and an iron ball having a diameter of 20 to 70 mm is exemplified. The grinding medium b may be a commercially available one. The shape may be a rod shape other than a spherical shape. The amount of the pulverizing medium b introduced into the container 10 depends on the amount of solid content in the sulfuric acid pitch a, but is, for example, about 5 to 10 times the solid content of the sulfuric acid pitch a introduced into the container 10. . In particular, when the solid content of the sulfuric acid pitch a is large, it is necessary to obtain a large impact breaking force. Conversely, when the solid content of the sulfuric acid pitch a is small, it is preferable to use a large amount of a small grinding medium b in order to obtain a contact abrasion effect.

容器１０内への硫酸ピッチａと粉砕媒体ｂの投入の順序は，いずれが先でも良いし，容器１０内へ硫酸ピッチａと粉砕媒体ｂを一緒に投入しても良い。   Either order may be sufficient as the order of injection of sulfuric acid pitch a and grinding medium b into container 10, and sulfuric acid pitch a and grinding medium b may be thrown into container 10 together.

そして，モータ２５の回転動力により，開口部１１を斜め上方に向けた姿勢で，中心軸Ｌを回転中心にして容器１０を回転させる。なお，容器１０を先に回転させておいて，容器１０内へ硫酸ピッチａと粉砕媒体ｂを投入しても良い。   Then, the container 10 is rotated with the central axis L as the center of rotation in a posture in which the opening 11 is directed obliquely upward by the rotational power of the motor 25. In addition, the container 10 may be rotated first, and the sulfuric acid pitch a and the grinding medium b may be put into the container 10.

また，容器１０内には，アルカリ金属の水酸化物の水溶液もしくは極性のある有機系の液体を分散溶媒として添加しても良い。アルカリ金属の水酸化物の水溶液として，例えば水酸化ナトリウム水溶液を用いることができる。また，極性のある有機系の液体として，例えばアルコールやアセトンなどを用いることができる。これら分散溶媒の添加量は，容器１０内へ投入される硫酸ピッチａの固形分に対して１〜１０倍重量程度である。   Further, an aqueous solution of an alkali metal hydroxide or a polar organic liquid may be added to the container 10 as a dispersion solvent. As an aqueous solution of an alkali metal hydroxide, for example, an aqueous sodium hydroxide solution can be used. Further, for example, alcohol or acetone can be used as the polar organic liquid. The amount of the dispersion solvent added is about 1 to 10 times the weight of the solid content of sulfuric acid pitch a introduced into the container 10.

そして，このように容器１０内に硫酸ピッチａと粉砕媒体ｂを入れ，更に，分散溶媒としてアルカリ金属の水酸化物の水溶液もしくは極性のある有機系の液体を容器１０に適宜添加して，容器１０を中心軸Ｌの周りで回転させる。すると，容器１０の内面に設けられた攪拌羽根３０が中心軸Ｌの周りで回転し，攪拌羽根３０は中心軸Ｌの下側と中心軸Ｌの上側を交互に移動する。これにより，攪拌羽根３０が下方から上方に移動する際には，容器１０の内部に入れられた硫酸ピッチａと粉砕媒体ｂを，攪拌羽根３０によって掻き上げ，一方で，攪拌羽根３０が上方まで移動した際，あるいは，更に上方から下方に移動する際には，攪拌羽根３０によって掻き上げられた硫酸ピッチａと粉砕媒体ｂが攪拌羽根３０から離れて落下し，容器１０の底部に衝突する。これにより，固化したような硫酸ピッチであっても，容器１０の底部への衝突による衝撃と，粉砕媒体ｂから硫酸ピッチａに加わる摩擦力やせん断力によって，硫酸ピッチａは徐々に粉砕されていく。また，容器１０内にアルカリ金属の水酸化物の水溶液や極性のある有機系の液体を添加している場合は，容器１０の回転に伴って，硫酸ピッチａが攪拌されて，それら分散溶媒中に硫酸ピッチａの一部もしくは全部が分散，溶解していく。なお，このように容器１０内にて硫酸ピッチａを粉砕している間，容器１０の開口部１１は常に斜め上方に向いているので，容器１０内から硫酸ピッチａと粉砕媒体ｂがこぼれる心配がない。   Then, the sulfuric acid pitch a and the grinding medium b are put in the container 10 in this way, and further, an aqueous solution of an alkali metal hydroxide or a polar organic liquid is appropriately added to the container 10 as a dispersion solvent. 10 is rotated around the central axis L. Then, the stirring blade 30 provided on the inner surface of the container 10 rotates around the central axis L, and the stirring blade 30 alternately moves below the central axis L and above the central axis L. Thereby, when the stirring blade 30 moves from the lower side to the upper side, the sulfuric acid pitch a and the pulverizing medium b put in the container 10 are scraped up by the stirring blade 30 while the stirring blade 30 is moved upward. When moving, or when moving further downward from above, the sulfuric acid pitch a and the grinding medium b scraped up by the stirring blade 30 fall away from the stirring blade 30 and collide with the bottom of the container 10. As a result, even if the sulfuric acid pitch is solidified, the sulfuric acid pitch a is gradually crushed by the impact caused by the collision with the bottom of the container 10 and the frictional force and shearing force applied from the grinding medium b to the sulfuric acid pitch a. Go. In addition, when an aqueous solution of an alkali metal hydroxide or a polar organic liquid is added to the container 10, the sulfuric acid pitch a is agitated as the container 10 rotates, and the dispersion solvent contains In addition, part or all of the sulfuric acid pitch a is dispersed and dissolved. In addition, while the sulfuric acid pitch a is pulverized in the container 10 in this way, the opening 11 of the container 10 always faces obliquely upward, so that the sulfuric acid pitch a and the pulverizing medium b may spill from the container 10. There is no.

こうして，容器１０内において，硫酸ピッチａは粉砕され，あるいは更にアルカリ金属の水酸化物の水溶液や極性のある有機系の液体に分散，溶解することにより，硫酸ピッチａを流動化させることができる。そして，このように硫酸ピッチａを流動化させた後，シリンダー装置２１を短縮稼動させることによって，図２に示すように，容器１０を軸１７を中心にして図２中において時計回転方向に揺動させ，開口部１１を斜め下方に向けた姿勢にする。これにより，容器１０内において流動化した硫酸ピッチａは，容器１０内から開口部１１を通って排出されることになる。こうして排出された硫酸ピッチａは，例えば焼却炉に投入して焼却処理することも可能である。   Thus, in the container 10, the sulfuric acid pitch a can be pulverized or further dispersed and dissolved in an aqueous solution of an alkali metal hydroxide or a polar organic liquid, whereby the sulfuric acid pitch a can be fluidized. . Then, after the sulfuric acid pitch a is fluidized in this way, the cylinder device 21 is shortened to move the container 10 about the shaft 17 in the clockwise direction in FIG. 2 as shown in FIG. To move the opening 11 obliquely downward. Thus, the sulfuric acid pitch a fluidized in the container 10 is discharged from the container 10 through the opening 11. The sulfuric acid pitch a thus discharged can be put into, for example, an incinerator and incinerated.

以上，本発明の好ましい実施の形態の一例を示したが，本発明はここに例示した形態に限定されない。例えば，容器１０の内周面に配置される攪拌羽根３０は必ずしも４枚でなくても良く，３枚以下，あるいは５枚以上でも良い。なお，アルカリ金属の水酸化物の水溶液や極性のある有機系の液体を分散溶媒として容器１０内に添加する場合，それら分散溶媒を先に容器１０内に入れておき，硫酸ピッチを分散溶媒中に投入するようにすると良い。分散溶媒としてアルカリ金属の水酸化物の水溶液を用いる場合は，容器１０内に予め充分な量の水酸化ナトリウム水溶液を充填しておき，容器１０内に投入された硫酸ピッチが，水酸化ナトリウム水溶液中に完全に浸漬するようにすると良い。また，容器１０内に充填されている水酸化ナトリウム水溶液の塩基の当量が，容器１０内に投入される硫酸ピッチａの酸の当量を上回るようにすると良い。そうすれば，硫酸ピッチａを完全に中和することができる。その他，アルカリ金属の水酸化物の水溶液や極性のある有機系の液体の代りに，水や硫酸等の酸を分散溶媒に用いても良い。   As mentioned above, although an example of preferable embodiment of this invention was shown, this invention is not limited to the form illustrated here. For example, the number of the stirring blades 30 arranged on the inner peripheral surface of the container 10 is not necessarily four, but may be three or less, or five or more. When an aqueous solution of an alkali metal hydroxide or a polar organic liquid is added to the container 10 as a dispersion solvent, the dispersion solvent is first placed in the container 10 and the sulfuric acid pitch is added to the dispersion solvent. It is better to put it in When an aqueous solution of an alkali metal hydroxide is used as the dispersion solvent, a sufficient amount of sodium hydroxide aqueous solution is filled in the container 10 in advance, and the sulfuric acid pitch charged into the container 10 is used as the sodium hydroxide aqueous solution. It is better to completely immerse it inside. Further, it is preferable that the equivalent of the base of the aqueous sodium hydroxide solution filled in the container 10 exceeds the equivalent of the acid of the sulfuric acid pitch a charged in the container 10. By doing so, the sulfuric acid pitch a can be completely neutralized. In addition, instead of an alkali metal hydroxide aqueous solution or a polar organic liquid, an acid such as water or sulfuric acid may be used as a dispersion solvent.

（実施例１）
図１〜４で説明した流動化装置を用いて，硫酸ピッチを処理した。実施例１，２及び比較例における容器内への硫酸ピッチ投入量，硫酸ピッチ中の固形分比率，固形分の最大径，容器の回転数，容器容積と最大内径，粉砕媒体の比重，粉砕媒体の最大径，全粉砕媒体の重量，分散溶媒の種類，分散溶媒の添加量を表１に示す。実施例１では，粉砕媒体として直径２０〜７０ｍｍの鋼鉄製ボールを用いた。実施例２では，粉砕媒体として直径１２．５ｍｍの鋼鉄製ボールを用いた。一方，比較例では，粉砕媒体は使用しなかった。そして，実施例１，２及び比較例のいずれの場合も，３０分間容器を回転させて流動化処理を施し，処理後の硫酸ピッチを１ｍｍの篩に通過させた。 Example 1
The sulfuric acid pitch was processed using the fluidizing apparatus described in FIGS. In Examples 1 and 2 and Comparative Example, the amount of sulfuric acid pitch introduced into the container, the solid content ratio in the sulfuric acid pitch, the maximum solid content diameter, the container rotation speed, the container volume and maximum internal diameter, the specific gravity of the grinding medium, the grinding medium Table 1 shows the maximum diameter, the weight of all grinding media, the type of dispersion solvent, and the amount of dispersion solvent added. In Example 1, a steel ball having a diameter of 20 to 70 mm was used as a grinding medium. In Example 2, a steel ball having a diameter of 12.5 mm was used as a grinding medium. On the other hand, no grinding media was used in the comparative example. In each of Examples 1 and 2 and Comparative Example, the vessel was rotated for 30 minutes for fluidization treatment, and the treated sulfuric acid pitch was passed through a 1 mm sieve.

Figure 0004482673
Figure 0004482673

実施例１では，全量篩を通過し，固形分は残っていなかった。実施例２では，添加した硫酸ピッチの４４％が篩上に残った。一方，比較例では，添加した硫酸ピッチの８４％が篩上に残った。   In Example 1, the whole amount passed through the sieve and no solid content remained. In Example 2, 44% of the added sulfuric acid pitch remained on the sieve. On the other hand, in the comparative example, 84% of the added sulfuric acid pitch remained on the sieve.

本発明は，硫酸ピッチの処理に利用される。本発明は，不法投棄など長期間経過して固化することによりハンドリング性が劣化した硫酸ピッチの処理にも利用される。   The present invention is used for the treatment of sulfuric acid pitch. The present invention is also used for the treatment of sulfuric acid pitch whose handling property has deteriorated due to solidification after a long period of time such as illegal dumping.

容器の開口部を上に向けた姿勢を示す本発明の実施の形態にかかる流動化装置の側面図である。It is a side view of the fluidization apparatus concerning an embodiment of the invention showing the posture which turned up the opening of a container. 容器の開口部を下に向けた姿勢を示す流動化装置の側面図である。It is a side view of the fluidization apparatus which shows the attitude | position which orient | assigned the opening part of the container downward. 容器の縦断面図である。It is a longitudinal cross-sectional view of a container. 開口部から容器の内部を見た状態を示す図面である。It is drawing which shows the state which looked at the inside of the container from the opening part.

符号の説明Explanation of symbols

ａ 硫酸ピッチ
ｂ 粉砕媒体
１ 流動化装置
１０ 容器
１１ 開口部
２１ シリンダー装置
２５ モータ
３０ 攪拌羽根 a sulfuric acid pitch b grinding media 1 fluidizing device 10 container 11 opening 21 cylinder device 25 motor 30 stirring blade

Claims (4)

硫酸ピッチと複数の粉砕媒体を容器内に入れ，容器内に分散溶媒であるＮａＯＨを添加して，容器を回転させ，前記容器内において，攪拌羽根によって粉砕媒体が持ち上げる運動と，攪拌羽根から粉砕媒体が落下させる運動を繰り返して行わせることにより，硫酸ピッチを流動化させることを特徴とする，硫酸ピッチの流動化方法。 A sulfuric acid pitch and a plurality of grinding media are put in a container, NaOH as a dispersion solvent is added to the container , the container is rotated, and in the container, the grinding media is lifted by a stirring blade and pulverized from the stirring blade. A method for fluidizing sulfuric acid pitch, characterized by fluidizing sulfuric acid pitch by repeatedly performing a motion of dropping the medium . 前記粉砕媒体は，金属もしくはセラミックスからなるボールであることを特徴とする，請求項１に記載の硫酸ピッチの流動化方法。The method for fluidizing sulfuric acid pitch according to claim 1, wherein the grinding medium is a ball made of metal or ceramics. 前記粉砕媒体は，直径が２０〜７０ｍｍの鉄球であることを特徴とする，請求項１に記載の硫酸ピッチの流動化方法。The method for fluidizing a sulfuric acid pitch according to claim 1, wherein the grinding medium is an iron ball having a diameter of 20 to 70 mm. 請求項１，２又は３に記載の硫酸ピッチの流動化方法によって流動化させた硫酸ピッチを焼却することを特徴とする，硫酸ピッチの処理方法。A method for treating sulfuric acid pitch, characterized in that the sulfuric acid pitch fluidized by the sulfuric acid pitch fluidizing method according to claim 1, 2 or 3 is incinerated.
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