JP4441760B2 - Method for fluidizing ultrafine powder in gas-phase fluidized bed reactor - Google Patents
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本発明は微粉の気相流動層に関するものである。詳しくは、１μｍ以下の超微粒子を流動化する方法に関する。 The present invention relates to a fine powder gas phase fluidized bed. Specifically, the present invention relates to a method for fluidizing ultrafine particles of 1 μm or less.
流動層においては、５０〜１５０μｍ程度の粒子を流動化すると、極めて均一な流動化状態となるので、広く利用されてきた。しかるに、４０μｍ以下の微粒子は難流動性で、流動層には不適当な粒子とされてきた。
このような微粒子の流動化について、特殊な方法として、流動層全体を機械的に振動させて微粒子を流動化させる振動流動層がある。しかし、装置全体を振動させることから、小型の流動層に限られ、１０００℃前後の高温反応流動層や爆発性、有毒性ガスの使用に対しては適用が困難で、工業的な利用が限定される。
一方、通常の流動層において、数μｍ程度の微粒子についてはその付着凝集性を利用して、粉粒流動層が本発明者らによって発明された。この粉粒流動層では、数１００μｍ程度の媒体粒子をガスで流動化しているところに、数μｍ程度の微粒子を連続供給し、媒体粒子と共に流動化させる方法である。これに関して、本発明者らは多くの発表や特許出願を行ってきた。（例えば、非特許文献１から５２、特許文献１から８参照。）
As a special method for fluidizing such fine particles, there is a vibrating fluidized bed in which the whole fluidized bed is mechanically vibrated to fluidize the fine particles. However, since the entire apparatus is vibrated, it is limited to a small fluidized bed, and it is difficult to apply to the use of high-temperature reaction fluidized beds around 1000 ° C or explosive or toxic gases, and industrial use is limited Is done.
On the other hand, in a normal fluidized bed, a fine particle fluidized bed was invented by the present inventors by utilizing the adhesion and aggregation properties of fine particles of about several μm. In this granular fluidized bed, medium particles of about several hundred μm are fluidized with gas, and fine particles of about several μm are continuously supplied and fluidized together with the medium particles. In this regard, the inventors have made many announcements and patent applications. (For example, see Non-Patent Documents 1 to 52 and Patent Documents 1 to 8.)
このように粉粒流動層は微粒子を流動化する方法であるが、粉粒流動層においては、供給された微粒子は媒体粒子に付着して流動化するので、付着性の強い微粒子ほど滞留時間が長くなる。（例えば、非特許文献５３、Ｆｉｇ．１０参照。）このため、微粒子が１μｍ以下となると、この微粒子ホールドアップ量が時間と共に上昇し、均一な流動化はしなくなる。そこで、微粒子の流動化に関して、粉粒流動層でも安定して流動化できない１μｍ以下の超微粒子の流動化方法が必要である。
微粒子が分散した一次粒子で存在したとしてこれが流動化すれば、微粒子の終末速度は極端に低く、従って空塔基準のガス速度も極端に低くなり、生産性の高い装置の運転は不可能である。しかし、実際は微粒子は粒径が小さくなるほど付着凝集性が強くなり、微粒子は流動層ではチャネリングを起こして流動化が困難である。しかし、振動流動層においては、逆にこの性質の働きにより流動化をさせている。すなわち、流動層全体を機械的に振動することで、微粒子はガス流中で凝集した二次粒子を形成し、これが流動化していることが観察される。
特に１μｍ以下の超微粒子では、この粒子間の付着凝集力が極端に強く、単一の分散粒子で存在するよりは凝集群となる方が安定である。通常の流動層においても、この性質を利用して超微粒子を流動化できることを見出した。
すなわち、１μｍ以下の超微粒子を気相中で目開き４ｍｍ以下、望ましくは２〜１ｍｍの篩で篩った粉体を分散板上のガス流中に供給することで、安定して超微粒子が流動化することを見出した。
これは超微粒子が凝集し易いため、これをを篩で篩うことにより平均粒径３００μｍ前後の見掛け二次凝集粒が形成され、これが流動層内で保持されるためである。より大きな凝集粒子同士が付着し、さらに大きな粒子に成長して行く現象は見られない。これは、大きな粒子同士はその付着力が流動運動に比し小さいため、結び付くよりは壊れ易いためである。そして、より大きな凝集粒は壊れ易く、実際、壊れるが、それが小さな見掛け粒子になると強度的に強固になるので壊れにくくなり、二次凝集粒が維持される。一方、見掛け上小さな粒子も存在するが、その滞留時間はそれが層内を通過すると考えた理論滞留時間よりも極端に大きな値となる。これは粉粒流動層における微粒子と媒体粗粒子の関係と同じで、大きな凝集粒子が媒体粒子として安定した流動層を形成し、付着性の強い微粒子が媒体粒子表面上で付着捕集されるためと考えられる。このため、ガスに同伴する粒子の飛び出し量は、理論的に考えられる量に比べ、著しく低く抑えられる。If the fine particles are present as dispersed primary particles and they are fluidized, the final velocity of the fine particles will be extremely low, and therefore the gas velocity based on the superficial column will be extremely low, making it impossible to operate a highly productive apparatus. . However, in actuality, the smaller the particle size, the stronger the adhesion and aggregation properties, and the fine particles cause channeling in the fluidized bed and are difficult to fluidize. However, in the oscillating fluidized bed, on the contrary, fluidization is performed by the function of this property. That is, by mechanically vibrating the fluidized bed as a whole, it is observed that the fine particles form secondary particles aggregated in the gas flow and are fluidized.
In particular, in the case of ultrafine particles of 1 μm or less, the adhesion and cohesion force between these particles is extremely strong, and it is more stable to become an aggregation group than to exist as a single dispersed particle. It was found that even in a normal fluidized bed, ultrafine particles can be fluidized using this property.
That is, ultrafine particles of 1 μm or less can be stably formed by supplying powder, which is sieved with a sieve having a mesh size of 4 mm or less, desirably 2 to 1 mm, in the gas phase into the gas flow on the dispersion plate. I found it fluidized.
This is because the ultrafine particles tend to aggregate, and by sieving this with a sieve, apparent secondary aggregated particles having an average particle size of about 300 μm are formed and retained in the fluidized bed. There is no phenomenon in which larger agglomerated particles adhere to each other and grow into larger particles. This is because large particles tend to be broken rather than connected because their adhesion force is smaller than the flow motion. Larger agglomerated particles are easily broken and actually break, but when they become small apparent particles, they become stronger and hard to break, and secondary agglomerated particles are maintained. On the other hand, apparently small particles are also present, but the residence time is extremely larger than the theoretical residence time that is considered to pass through the layer. This is the same as the relationship between fine particles and medium coarse particles in a powder fluidized bed, because large aggregated particles form a stable fluidized bed as medium particles, and highly adherent fine particles adhere to and collect on the surface of the medium particles. it is conceivable that. For this reason, the pop-out amount of the particles accompanying the gas can be suppressed significantly lower than the theoretically conceivable amount.
１μｍ以下の超微粒子は著しい付着性、凝集性があり、このため、通常の流動層での流動化が困難とされてきた。しかし、超微粉を篩で篩っただけの緩い凝集粒であっても、適当な凝集粒径にすれば、超微粒子の著しい付着性、凝集性により流動層内で顆粒が維持され、安定した流動状態を保持できる。
気相中で形成された緩い凝集粉であるため、高温の流動層において、焼結による一次粒子径の成長が少ない。従って、得られた製品を解砕することで、元の超微粒子に戻すことが容易である。
超微粉末を原料粉とし湿式で顆粒を製造し、これを使用すれば、通常の流動層の流動化条件に入るので、流動化することができる。しかし、この方法においては、超微粉末に水又は結合剤を含んだ水を添加して混練し、スラリー又はケーキとし、これを乾燥後、粉砕し、篩分けするか、混練後造粒し乾燥するかして顆粒を製造するため、この工程に伴う設備費、熱エネルギー、労務費等の運転費は大きい。
また、湿式で顆粒を作った場合、粒子間距離の短い固い凝集となるため、数百℃以上の流動層においては超微粒子ほど焼結による一次粒子同士の粒成長が著しく、簡単に１μｍ以上の粒径に成長する。一般に機械的には１μｍ以下まで粉砕できないので、原料粉が超微粒子であっても、製品を超微粉に戻すことができなくなる。Ultrafine particles of 1 μm or less have remarkable adhesion and agglomeration, and for this reason, fluidization in a normal fluidized bed has been difficult. However, even if loose agglomerated particles are obtained by simply sieving ultrafine powder with a sieve, if the appropriate agglomerated particle size is obtained, the granules are maintained in the fluidized bed due to the remarkable adhesion and agglomeration properties of the ultrafine particles, and are stable. A fluid state can be maintained.
Since it is a loose agglomerated powder formed in the gas phase, there is little growth of the primary particle size due to sintering in the high temperature fluidized bed. Therefore, it is easy to return to the original ultrafine particles by crushing the obtained product.
If ultrafine powder is used as a raw material powder and granules are produced by a wet process and used, fluidizing conditions can be obtained because the fluidizing conditions of a normal fluidized bed are entered. However, in this method, water or water containing a binder is added to the ultrafine powder and kneaded to obtain a slurry or cake, which is dried, crushed and sieved, or granulated after kneading and dried. However, since the granules are manufactured, the operation costs such as equipment costs, thermal energy, labor costs and the like associated with this process are large.
In addition, when a granule is made by a wet process, it becomes a hard agglomeration with a short interparticle distance. Therefore, in a fluidized bed of several hundred degrees C or higher, the growth of primary particles due to sintering becomes more remarkable with ultrafine particles. Grows to particle size. In general, since it cannot be mechanically pulverized to 1 μm or less, even if the raw material powder is ultrafine particles, the product cannot be returned to the ultrafine powder.
以下、本発明の実施の形態について説明する。
１μｍ以下の超微粉を気相中で目開き４ｍｍ以下、望ましくは２〜１ｍｍの篩で篩い、その全量を通過させ見掛け平均粒径で１００〜５００μｍの凝集粒群とする。このとき、目開き４ｍｍを超える篩では、篩った後、超微粉がまた一体のバルクに戻るので望ましくない。また、篩が１ｍｍ以下になると、篩網の強度がなくなることと超微粉の目詰まりが著しくなり、量産には向かなくなる。
この凝集粒群を分散板上のガス流に供給すると、この超微粒子からなる凝集粒が安定した流動層を形成する。Embodiments of the present invention will be described below.
Ultrafine powder of 1 μm or less is sieved with a sieve having an opening of 4 mm or less, preferably 2 to 1 mm in the gas phase, and the whole amount is passed through to form an aggregate particle group having an apparent average particle diameter of 100 to 500 μm. At this time, if the sieve has an opening of more than 4 mm, it is not desirable because after the sieving, the ultrafine powder returns to the integral bulk. On the other hand, when the size of the sieve is 1 mm or less, the strength of the sieve screen is lost and the clogging of the ultrafine powder becomes remarkable, which is not suitable for mass production.
When this aggregated particle group is supplied to the gas flow on the dispersion plate, the aggregated particles composed of the ultrafine particles form a stable fluidized bed.
超微粉としてＢＥＴ粒径０．１８μｍ（ＢＥＴ比表面積８．０平方ｍ／ｇ）の二酸化チタン３ｋｇを、大気中で目開き１．２ｍｍの篩で篩い見掛け平均粒径２５０μｍの凝集粉とした。これを標準状態換算１０立方ｍ／ｈの常温の窒素ガスを流した分散板を有す内径１５５ｍｍ、高さ１２００ｍｍの円筒管に供給すると流動層を形成した。流動状態は安定で、５ｈ経過してもその状態に変化はなかった。時間当たりの平均飛び出し量は３０ｇ／ｈであった。 As an ultrafine powder, 3 kg of titanium dioxide having a BET particle size of 0.18 μm (BET specific surface area of 8.0 square m / g) was sieved with a sieve having an opening of 1.2 mm in the atmosphere to obtain an aggregated powder having an apparent average particle size of 250 μm. When this was supplied to a cylindrical tube having an inner diameter of 155 mm and a height of 1200 mm having a dispersion plate in which nitrogen gas at room temperature of 10 cubic m / h in standard state was passed, a fluidized bed was formed. The flow state was stable and the state did not change even after 5 hours. The average amount of protrusion per hour was 30 g / h.
実施例１と同じ超微粉３ｋｇを、篩を通す前処理をせず、直接、実施例１と同条件の円筒管の窒素ガス流中に供給した。超微粉は部分的にしか流動化せず、数分後、チャネリングを起こし流動状態を停止した。 3 kg of the same ultrafine powder as in Example 1 was supplied directly into a nitrogen gas flow in a cylindrical tube under the same conditions as in Example 1 without performing pretreatment through a sieve. The ultrafine powder was only partially fluidized, and after a few minutes, channeling occurred and the fluidized state was stopped.
実施例１と同じく、超微粉としてＢＥＴ粒径０．１８μｍ（ＢＥＴ比表面積８．０平方ｍ／ｇ）の二酸化チタン３ｋｇを、大気中で目開き１．２ｍｍの篩で篩い見掛け平均粒径２５０μｍの凝集粉とした。この白色粉体を標準状態換算５立方ｍ／ｈの水素ガスを流した分散板を有す内径１５５ｍｍ、高さ１２００ｍｍの円筒管に供給し、層内温度を９００℃に維持した。５ｈ経過後、冷却し凝集粉を取り出すと、一様に黒く還元され、流動層内が均一に維持されていたことが分かった。
この凝集粉を解砕すると、ＢＥＴ粒径０．１８μｍ（ＢＥＴ比表面積８．０平方ｍ／ｇ）の黒色の超微粉が得られた。As in Example 1, 3 kg of titanium dioxide having a BET particle size of 0.18 μm (BET specific surface area of 8.0 square m / g) as an ultrafine powder was screened with a sieve having an opening of 1.2 mm in the atmosphere, and an apparent average particle size of 250 μm. Agglomerated powder. This white powder was supplied to a cylindrical tube having an inner diameter of 155 mm and a height of 1200 mm having a dispersion plate in which hydrogen gas of 5 cubic m / h in terms of standard condition was passed, and the temperature in the layer was maintained at 900 ° C. When 5 hours passed and cooled and the agglomerated powder was taken out, it was found that the powder was uniformly reduced to black and the fluidized bed was maintained uniformly.
When this agglomerated powder was pulverized, a black ultrafine powder having a BET particle size of 0.18 μm (BET specific surface area of 8.0 square m / g) was obtained.
実施例２と同じ超微粉３ｋｇを、篩を通す前処理をせず、直接、実施例２と同条件の円筒管の水素ガス流中に供給した。５ｈ経過後、冷却し円筒管内を観察すると、チャネリングによるラットホールがあり、その内表面のみが黒く還元されているだけで、バルクは白色粉体のままで還元されていなかった。 3 kg of the same ultrafine powder as in Example 2 was supplied directly into a hydrogen gas flow in a cylindrical tube under the same conditions as in Example 2 without pretreatment through a sieve. After 5 hours, the tube was cooled and the inside of the cylindrical tube was observed. As a result, there was a rathole due to channeling, and only the inner surface was reduced to black, and the bulk remained white powder and not reduced.
超微粉としてＢＥＴ粒径０．０３μｍ（ＢＥＴ比表面積５０平方ｍ／ｇ）の二酸化チタン３ｋｇを、大気中で目開き１．２ｍｍの篩で篩い見掛け平均粒径３００μｍの凝集粉とした。この白色粉体を標準状態換算６立方ｍ／ｈの水素ガスを流した分散板を有す内径１５５ｍｍ、高さ１２００ｍｍの円筒管に供給し、層内温度を７００℃に維持した。５ｈ経過後、冷却し凝集粒を取り出すと、一様に黒く還元され、流動層内が均一に維持されていたことが分かった。 As an ultrafine powder, 3 kg of titanium dioxide having a BET particle size of 0.03 μm (BET specific surface area of 50 square m / g) was sieved with a sieve having an opening of 1.2 mm in the atmosphere to obtain an aggregated powder having an apparent average particle size of 300 μm. This white powder was supplied to a cylindrical tube having an inner diameter of 155 mm and a height of 1200 mm having a dispersion plate in which hydrogen gas of 6 cubic m / h in standard state was passed, and the temperature in the layer was maintained at 700 ° C. After 5 hours, the mixture was cooled and the agglomerated grains were taken out, and it was found that the particles were uniformly reduced to black and the fluidized bed was maintained uniformly.
実施例１と同じ超微粉３ｋｇを、大気中で目開き１．２ｍｍの樋型の振動篩で篩い凝集粉とした。これを実施例１と同じ条件で流動層を形成させ、安定した流動状態を維持できた。
同じく、樋型の振動篩に替えて、円型の振動篩で形成させた凝集粉によっても、安定した流動層を維持できた。
さらに、振動篩に替えて、円筒回転篩で形成させた凝集粉によっても、安定した流動層を維持できた。3 kg of the same ultrafine powder as in Example 1 was sieved into agglomerated powder in the atmosphere using a vertical vibrating screen having a mesh opening of 1.2 mm. A fluidized bed was formed under the same conditions as in Example 1, and a stable fluidized state could be maintained.
Similarly, a stable fluidized bed could be maintained by using agglomerated powder formed by a circular vibrating sieve instead of a bowl-shaped vibrating sieve.
Furthermore, a stable fluidized bed could be maintained by using agglomerated powder formed by a cylindrical rotary sieve instead of the vibrating sieve.
実施例４において、篩網上に多数個のボールを置き、その運動により粉体の篩網の通過を促す振動篩で篩い、超微粉を凝集形成させた。この粉体によっても安定した流動層を維持できた。
同じく、振動篩に代えて、篩網円筒内に多数個のボールを入れた回転篩で形成させた凝集粉によっても、安定した流動層を維持できた。In Example 4, a large number of balls were placed on a sieve mesh and sieved with a vibrating sieve that encouraged the movement of the powder sieve mesh by its movement to agglomerate and form ultrafine powder. A stable fluidized bed could be maintained with this powder.
Similarly, a stable fluidized bed could be maintained by using agglomerated powder formed by a rotating sieve having a large number of balls in a sieve screen cylinder instead of the vibrating sieve.
実施例４および５において、振動篩で篩うことにより凝集形成された粉体を、さらにそれに続く平板上で振動により転動させることで球状凝集粒子粉を形成させた。この粉体によっても安定した流動層を維持できた。
同じく、実施例４および５において、回転篩で篩うことにより凝集形成された粉体を、さらにそれに続く円筒板上で回転により転動させることで球状凝集粒子粉を形成させた。この粉体によっても安定した流動層を維持できた。
さらに、振動篩で篩うことにより凝集形成された粉体を、平板上に代えて、より細かい篩網上で転動させることで球状凝集粒子粉を形成させた。この粉体によっても安定した流動層を維持できた。
同じく、回転篩で篩うことにより凝集形成された粉体を、円筒板上に代えて、より細かい篩網上で転動させることで球状凝集粒子粉を形成させた。この粉体によっても安定した流動層を維持できた。In Examples 4 and 5, the powder formed by agglomeration by sieving with a vibration sieve was further rolled by vibration on a subsequent flat plate to form spherical agglomerated particles. A stable fluidized bed could be maintained with this powder.
Similarly, in Examples 4 and 5, the powder formed by agglomeration by sieving with a rotary sieve was further rolled by rotation on a subsequent cylindrical plate to form spherical agglomerated particle powder. A stable fluidized bed could be maintained with this powder.
Furthermore, the powder formed by agglomeration by sieving with a vibrating sieve was replaced with a flat plate and rolled on a finer mesh screen to form spherical agglomerated particle powder. A stable fluidized bed could be maintained with this powder.
Similarly, spherical agglomerated particle powder was formed by rolling the powder agglomerated by sieving with a rotary sieve on a finer mesh screen instead of the cylindrical plate. A stable fluidized bed could be maintained with this powder.
実施例１と同じ超微粉を、大気中で目開き１．２ｍｍの篩で篩い、さらに目開き０．３ｍｍの篩で篩うことにより、見掛け凝集粉粒径分布を狭く整粒した。この粉体３ｋｇを実施例１と同じ条件で流動層を形成させた。流動状態は安定で、５ｈ経過してもその状態に変化はなかった。時間当たりの平均飛び出し量は２５ｇ／ｈであった。 The same ultrafine powder as in Example 1 was sieved in the air with a sieve having an opening of 1.2 mm, and further sieved with a sieve having an opening of 0.3 mm, whereby the apparent agglomerated powder particle size distribution was narrowly sized. A fluidized bed was formed on 3 kg of this powder under the same conditions as in Example 1. The flow state was stable and the state did not change even after 5 hours. The average amount of protrusion per hour was 25 g / h.
実施例１と同じ超微粉を、大気中で目開きの異なる１．２ｍｍと０．３ｍｍの二重の篩網を有する振動篩で篩うことにより、見掛け凝集粉粒径分布を狭く整粒した。この粉体３ｋｇを実施例１と同じ条件で流動層を形成させ、安定した流動状態を維持できた。
同じく、振動篩に替えて、目開きの異なる二重の同心篩網円筒を有する回転篩で整粒した凝集粉によっても、安定した流動層を維持できた。By sieving the same ultrafine powder as in Example 1 with a vibrating sieve having a double sieve screen of 1.2 mm and 0.3 mm having different openings in the atmosphere, the apparent agglomerated powder particle size distribution was narrowly sized. . A fluidized bed was formed on 3 kg of this powder under the same conditions as in Example 1, and a stable fluidized state could be maintained.
Similarly, a stable fluidized bed could be maintained by using agglomerated powder that was sized with a rotary sieve having double concentric sieve mesh cylinders with different openings instead of the vibrating sieve.
実施例１と同じ超微粉を、振動板上で転動させ凝集を促した後、目開き１．２ｍｍの篩で篩い凝集粉とした。この粉体３ｋｇを実施例１と同じ条件で流動層を形成させ、安定した流動状態を維持できた。
同じく、実施例１と同じ超微粉を、傾斜パン型の回転皿上で転動運動させ凝集を促した後、目開き１．２ｍｍの篩で篩い凝集粉とした。この粉体３ｋｇを実施例１と同じ条件で流動層を形成させ、安定した流動状態を維持できた。
同じく、実施例１と同じ超微粉を、回転円筒内で転動運動させ凝集を促した後、目開き１．２ｍｍの篩で篩い凝集粉とした。この粉体３ｋｇを実施例１と同じ条件で流動層を形成させ、安定した流動状態を維持できた。The same ultrafine powder as in Example 1 was rolled on the diaphragm to promote aggregation, and then sieved into a sieved aggregated powder with a sieve having an opening of 1.2 mm. A fluidized bed was formed on 3 kg of this powder under the same conditions as in Example 1, and a stable fluidized state could be maintained.
Similarly, the same ultrafine powder as in Example 1 was rolled on a tilt pan-type rotating dish to promote aggregation, and then sieved with a sieve having an opening of 1.2 mm to obtain agglomerated powder. A fluidized bed was formed on 3 kg of this powder under the same conditions as in Example 1, and a stable fluidized state could be maintained.
Similarly, the same ultrafine powder as in Example 1 was rolled in a rotating cylinder to promote agglomeration, and then sieved to agglomerated powder with a sieve having an opening of 1.2 mm. A fluidized bed was formed on 3 kg of this powder under the same conditions as in Example 1, and a stable fluidized state could be maintained.
実施例１と同じ超微粉を、大気中で機械的に圧粉後、目開き１．２ｍｍの篩で篩い凝集粉とした。この粉体３ｋｇを実施例１と同じ条件で流動層を形成させ、安定した流動状態を維持できた。 The same ultrafine powder as in Example 1 was mechanically compressed in the air, and then sieved to a coagulated powder with a sieve having a mesh size of 1.2 mm. A fluidized bed was formed on 3 kg of this powder under the same conditions as in Example 1, and a stable fluidized state could be maintained.
実施例１と同じ超微粉を、撹拌しながら水蒸気で加湿し、水分１ｗｔ％を含有する粉体とした後、目開き１．２ｍｍの篩で篩い凝集粉とした。この粉体３ｋｇを実施例１と同じ条件で流動層を形成させ、安定した流動状態を維持できた。
同じく、実施例１と同じ超微粉を、撹拌しながら水を添加し、水分１ｗｔ％を含有する粉体とした後、目開き１．２ｍｍの篩で篩い凝集粉とした。この粉体３ｋｇを実施例１と同じ条件で流動層を形成させ、安定した流動状態を維持できた。
同じく、実施例１と同じ超微粉を、撹拌しながらポリビニールアルコールの５ｗｔ％水溶液を添加し、水溶液１ｗｔ％を含有する粉体とした後、目開き１．２ｍｍの篩で篩い凝集粉とした。この粉体３ｋｇを実施例１と同じ条件で流動層を形成させ、安定した流動状態を維持できた。The same ultrafine powder as in Example 1 was humidified with water vapor while stirring to obtain a powder containing 1 wt% of water, and then sieved with a sieve having an opening of 1.2 mm to obtain agglomerated powder. A fluidized bed was formed on 3 kg of this powder under the same conditions as in Example 1, and a stable fluidized state could be maintained.
Similarly, water was added to the same ultrafine powder as in Example 1 with stirring to obtain a powder containing 1 wt% of water, and then sieved with a sieve having an opening of 1.2 mm to obtain agglomerated powder. A fluidized bed was formed on 3 kg of this powder under the same conditions as in Example 1, and a stable fluidized state could be maintained.
Similarly, a 5 wt% aqueous solution of polyvinyl alcohol was added to the same ultra fine powder as in Example 1 to obtain a powder containing 1 wt% of the aqueous solution, and then sieved with a sieve having an opening of 1.2 mm to obtain an agglomerated powder. . A fluidized bed was formed on 3 kg of this powder under the same conditions as in Example 1, and a stable fluidized state could be maintained.
実施例７で発生した目開き０．３ｍｍの篩下粉末を、大気中で機械的に圧粉後、目開き１．２ｍｍの篩で篩い凝集粉とした。この粉体３ｋｇを実施例１と同じ条件で流動層を形成させ、安定した流動状態を維持できた。 The under-sieving powder having a mesh size of 0.3 mm generated in Example 7 was mechanically compressed in the air, and then sieved to a coagulated powder with a sieve having a mesh size of 1.2 mm. A fluidized bed was formed on 3 kg of this powder under the same conditions as in Example 1, and a stable fluidized state could be maintained.
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