JP3265203B2 - Method and apparatus for pulverizing raw material particles in continuous hydrothermal reaction - Google Patents
Method and apparatus for pulverizing raw material particles in continuous hydrothermal reactionInfo
- Publication number
- JP3265203B2 JP3265203B2 JP31208596A JP31208596A JP3265203B2 JP 3265203 B2 JP3265203 B2 JP 3265203B2 JP 31208596 A JP31208596 A JP 31208596A JP 31208596 A JP31208596 A JP 31208596A JP 3265203 B2 JP3265203 B2 JP 3265203B2
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- JP
- Japan
- Prior art keywords
- raw material
- cyclone
- container
- material particles
- cyclone container
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Description
【０００１】[0001]
【発明の属する技術分野】本発明は、飽和蒸気温度を超
えた特には亜臨界および超臨界条件における連続水熱合
成反応において、原料スラリーをノズル噴霧によって粒
子を微細化する場合に、微細化が不十分なときや粒子が
凝集した場合などの粒子微細化を図って、水熱反応を効
率良く行なわせるための方法と装置である。BACKGROUND OF THE INVENTION The present invention relates to a method for producing fine particles by atomizing a raw material slurry by nozzle spraying in a continuous hydrothermal synthesis reaction under a saturated steam temperature, particularly under subcritical and supercritical conditions. A method and an apparatus for efficiently performing a hydrothermal reaction by reducing the size of particles when insufficient or when particles are aggregated.
【０００２】[0002]
【従来の技術】高温の水、特に高温、高圧の水の存在下
では高圧水蒸気、特に臨界温度以上の水にシリカ、アル
ミナをはじめ多くの酸化物の反応速度が速くなるため、
この現象を利用した水熱合成反応が広く行われている。2. Description of the Related Art In the presence of high-temperature water, especially high-temperature, high-pressure water, the reaction rate of silica, alumina, and other oxides to high-pressure steam, particularly water having a critical temperature or higher, increases.
Hydrothermal synthesis reactions utilizing this phenomenon are widely performed.
【０００３】現在、飽和蒸気温度を超える領域、特に臨
界温度（例えば水Ｔｃ＝３７４℃）を超える温度領域
で、かつ加圧条件下での粒子の水熱合成技術は、バッチ
式により行われている。しかし、大型バッチ方式では原
料をセットしてから目的とする温度、圧力の保持時間以
外に昇温、降温時間が長くかかる。又、バッチごとの生
産であるため、一つの装置で効率よく合成するには限界
がある。At present, the hydrothermal synthesis technique of particles in a region exceeding the saturated steam temperature, particularly in a temperature region exceeding a critical temperature (for example, water Tc = 374 ° C.), and under pressurized conditions is carried out by a batch method. I have. However, in the large-scale batch method, it takes a long time to raise and lower the temperature in addition to the target temperature and pressure holding time after setting the raw materials. In addition, since the production is performed on a batch basis, there is a limit in efficiently synthesizing with one apparatus.
【０００４】さらに配管を組んで連続的にスラリーを送
り込んで処理する方法は、例えば特開昭５３−５７１１
２号公報に開示されているが、これは粒子の水熱反応を
目的としたものではなく、本発明とは目的が異なる。そ
の他に特公平２−５１３６号公報に開示された技術もあ
るが、これは飽和水蒸気圧下で行われているものであ
る。特に臨界温度を超えるような温度で加圧状態を保つ
ような配管を組み、粒子の水熱反応を行い、その後、降
温、減圧して反応した粒子を排出するような連続製法技
術は未だ存在しない。Further, a method of treating the slurry by continuously feeding the slurry through pipes is disclosed in, for example, JP-A-53-5711.
Although it is disclosed in Japanese Patent Publication No. 2, it is not intended for a hydrothermal reaction of particles, and has a different purpose from the present invention. There is another technique disclosed in Japanese Patent Publication No. 2-5136, which is performed under a saturated steam pressure. In particular, there is no continuous manufacturing technology that constructs a pipe that maintains the pressurized state at a temperature exceeding the critical temperature, performs a hydrothermal reaction of the particles, and then lowers the temperature and reduces the pressure to discharge the reacted particles. .
【０００５】[0005]
【発明が解決しようとする課題】水熱反応を連続配管内
で一貫して行うには、原料スラリーの送り込みの問題や
配管内を高温加熱状態に保持する問題、合成された粒子
の取出しの問題など種々の困難があるが、本発明では、
特に原料スラリーの反応室内への供給の際の課題を解決
するものである。すなわち、飽和蒸気温度を超え、特に
臨界温度を超える範囲で配管内に原料スラリーを流して
も、水が水蒸気となっているため、スラリー中の固体分
が分離してしまい、配管内に詰まる可能性がある。そこ
で、本発明では、スラリー中の固体分が配管内に詰まる
ことなく、かつ、反応が効率良く行われるように固体分
を微粉砕して反応室に供給するものである。In order to conduct a hydrothermal reaction consistently in a continuous pipe, there is a problem of feeding raw material slurry, a problem of keeping the inside of the pipe at a high temperature heating state, and a problem of taking out synthesized particles. There are various difficulties, but in the present invention,
In particular, the present invention solves a problem in supplying a raw material slurry into a reaction chamber. In other words, even if the raw material slurry is flown in the pipe at a temperature exceeding the saturated steam temperature, particularly exceeding the critical temperature, since water is water vapor, solid components in the slurry are separated and may be clogged in the pipe. There is. Therefore, in the present invention, the solid component is finely pulverized and supplied to the reaction chamber so that the solid component in the slurry is not clogged in the pipe and the reaction is efficiently performed.
【０００６】[0006]
【課題を解決するための手段】本発明は、飽和蒸気温度
を超えて加圧加熱した水質液体と飽和蒸気温度未満に加
圧加熱した原料スラリーとを噴霧器の噴霧口直前で混合
して噴霧し、ついで混合流体を筒状のサイクロン容器の
一端よりその内壁に沿うように送り込み、比較的大きな
微粒子をサイクロン内壁に擦ることによって更に微粉砕
し、混合流体をサイクロン容器他端より送り出すことを
特徴とする連続水熱反応における原料粒子の微細化方法
である。SUMMARY OF THE INVENTION According to the present invention, a water-based liquid pressurized and heated above a saturated steam temperature and a raw material slurry pressurized and heated below a saturated steam temperature are mixed and sprayed immediately before a spray port of a sprayer. Then, the mixed fluid is sent from one end of the cylindrical cyclone container along the inner wall thereof, and relatively large fine particles are further pulverized by rubbing against the inner wall of the cyclone, and the mixed fluid is sent out from the other end of the cyclone container. This is a method for refining raw material particles in a continuous hydrothermal reaction.
【０００７】すなわち、原料スラリーと水質流体とを分
離して、水質流体は飽和蒸気温度を超えて加圧加熱して
おき、原料スラリーは飽和蒸気温度未満に加熱加圧し
て、水質流体を噴霧器から噴霧する直前に原料スラリー
を該水質流体に混合して噴霧することによって原料を水
蒸気分離を起こすことなく搬送することができ、かつ、
熱的な勾配をもつ２つの系を飽和蒸気を超える領域、特
には臨界温度を超える温度領域の条件下においても均一
な噴霧混合が可能となる。しかしながら、この前段工程
のみでは原料の微粉砕が不十分な場合があるので、本発
明ではさらに前記噴霧混合した混合流体を円筒状のサイ
クロン容器の一端よりその内壁に沿うように送り込み、
比較的大きな微粒子をサイクロン内壁に擦ることによっ
てさらに微粉砕し、混合流体をサイクロン容器他端より
反応室に向って送り出す。That is, the raw material slurry and the water-based fluid are separated, and the water-based fluid is pressurized and heated above the saturated steam temperature, and the raw-material slurry is heated and pressurized below the saturated steam temperature, and the water-based fluid is discharged from the sprayer. The raw material can be transported without causing steam separation by mixing and spraying the raw material slurry with the water-based fluid just before spraying, and
Even when two systems having a thermal gradient are in a region in which the temperature exceeds the saturated vapor, particularly in a temperature region in which the temperature exceeds the critical temperature, uniform spray mixing can be performed. However, there is a case where the pulverization of the raw material is insufficient only in the former step, so in the present invention, the mixed fluid spray-mixed is further fed from one end of the cylindrical cyclone container along the inner wall thereof,
The relatively large fine particles are further pulverized by rubbing against the inner wall of the cyclone, and the mixed fluid is sent out from the other end of the cyclone container toward the reaction chamber.
【０００８】又、サイクロン容器内において、混合流体
の流量を変化させることによって、粒子の微粉砕度を調
整することができる。このようにすることによって水熱
合成反応に望まれる微細な原料粒子を有効に得ることが
できる。In addition, the degree of fine pulverization of the particles can be adjusted by changing the flow rate of the mixed fluid in the cyclone container. By doing so, fine raw material particles desired for the hydrothermal synthesis reaction can be effectively obtained.
【０００９】本発明は又、飽和蒸気温度を超えて加圧加
熱した水質流体の噴霧器の噴霧口の内側に飽和蒸気温度
未満に加圧加熱した原料スラリーの供給口を設け、前記
噴霧口に続いて筒状のサイクロン容器を設け、該サイク
ロン容器の一端の側部には混合流体の噴射供給部を、
又、サイクロン容器の他端には排出部を設けたことを特
徴とする連続水熱反応における原料粒子の微細化装置で
あるこの発明は、上記方法の発明を実施するに適した装
置であって、噴霧器とサイクロン容器とを連続的に設け
たものである。サイクロン容器内には、その中央部に噴
射供給部側より容器内に突出するスピンドルを設け、該
スピンドルにはその容器内への突出長さを調節する調節
手段を設け、混合流体の流量を変化させる。スピンドル
の容器内への突出長さの調節手段としてはねじ方式が簡
単でよい。According to the present invention, a supply port for a raw material slurry pressurized and heated to a temperature lower than the saturated steam temperature is provided inside the spray port of the sprayer for the water-based fluid pressurized and heated to a temperature higher than the saturated steam temperature. To provide a cylindrical cyclone container, an injection supply unit of a mixed fluid on the side of one end of the cyclone container,
Further, the present invention, which is an apparatus for refining raw material particles in a continuous hydrothermal reaction, characterized in that a discharge section is provided at the other end of the cyclone container, is an apparatus suitable for carrying out the method of the invention. , A sprayer and a cyclone container are continuously provided. In the cyclone container, a spindle is provided at the center of the cyclone container and protrudes into the container from the injection supply unit side. Let it. As a means for adjusting the projecting length of the spindle into the container, a screw system may be simple.
【００１０】[0010]
【発明の実施の形態】本発明は、アルミナ（Ａｌ
2Ｏ3）、ジルコニア（ＺｒＯ2）、クロミア（Ｃｒ
2Ｏ3）、ハフニア（ＨｆＯ2）、チタニア（ＴｉＯ2）な
どの金属酸化物の水熱合成反応および物質からの有効成
分の抽出に適用できる。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an alumina (Al)
2 O 3 ), zirconia (ZrO 2 ), chromia (Cr
The present invention can be applied to hydrothermal synthesis of metal oxides such as 2 O 3 ), hafnia (HfO 2 ), and titania (TiO 2 ) and extraction of an active ingredient from a substance.
【００１１】以下、実施例を図面に基づいて具体的に説
明する。Hereinafter, embodiments will be specifically described with reference to the drawings.
【００１２】[0012]
【実施例】図１は本発明実施例装置の一例で、図中１は
噴霧器であり、２、３は配管、４は噴霧口である。５は
混合室、６は円筒状のサイクロン容器、７は噴射供給
口、８はサイクロン容器６内に設けたスピンドルで、ね
じ９でサイクロン容器６内への突出長さを調節できるよ
うにしてある。1 is an example of an apparatus according to an embodiment of the present invention, in which 1 is a sprayer, 2 and 3 are pipes, and 4 is a spray port. Reference numeral 5 denotes a mixing chamber, 6 denotes a cylindrical cyclone container, 7 denotes an injection supply port, 8 denotes a spindle provided in the cyclone container 6, and the length of the protrusion into the cyclone container 6 can be adjusted by a screw 9. .
【００１３】配管３からは飽和蒸気温度を超えて加圧加
熱した水質流体を供給し、配管２からは飽和蒸気温度未
満に加圧加熱した原料スラリーを供給して、噴霧口の直
前で両者を混合し、混合室５内へ噴霧混合する。この際
原料中の粒子は微細に粉砕される。混合された流体はサ
イクロン容器６へ進み、噴射供給口７よりサイクロン容
器６内に噴出する。噴射供給口７はサイクロン容器６の
側壁に設けられ、混合流体はサイクロン容器６の内壁面
に沿って供給され、旋回流となって出口側に向うが、そ
の間に比較的大きな微粒子はサイクロン内壁に擦られ
て、一層微粒子化する。ねじ９をもってスピンドル８の
サイクロン容器内への突出長さを調節することによって
混合流体の流量を変化させ、微粉砕の程度を調節するこ
とができる。A water quality fluid pressurized and heated above the saturated steam temperature is supplied from a pipe 3, and a raw material slurry pressurized and heated to a temperature below a saturated steam temperature is supplied from a pipe 2, and both are supplied immediately before the spray port. Mix and spray mix into mixing chamber 5. At this time, the particles in the raw material are finely pulverized. The mixed fluid advances to the cyclone container 6 and is ejected from the injection supply port 7 into the cyclone container 6. The injection supply port 7 is provided on the side wall of the cyclone container 6, and the mixed fluid is supplied along the inner wall surface of the cyclone container 6 and forms a swirling flow toward the outlet, while relatively large fine particles are supplied to the cyclone inner wall. It is rubbed and becomes finer. By adjusting the projecting length of the spindle 8 into the cyclone container with the screw 9, the flow rate of the mixed fluid can be changed, and the degree of pulverization can be adjusted.
【００１４】[0014]
【発明の効果】本発明によれば、飽和蒸気温度を超え
た、特には亜臨界および超臨界条件における連続水熱反
応を行うに当って、水質流体と原料スラリーとに分離し
て、水質流体は飽和蒸気温度を超え、原料スラリーは飽
和蒸気温度未満に加熱加圧して搬送の問題を解決し、か
つ、反応に有利なように原料の微粒子化を達成すること
ができる。したがって、アルミナ、ジルコニア、クロミ
ア、ハフニア、チタニアなどの金属酸化物の連続水熱合
成反応や、各種物質からの有効成分の連続抽出反応に適
用して有効である。According to the present invention, in performing a continuous hydrothermal reaction at a temperature exceeding the saturated steam temperature, particularly under subcritical and supercritical conditions, the watery fluid and the raw material slurry are separated into watery fluids. Is higher than the saturated steam temperature, and the raw material slurry is heated and pressurized to a temperature lower than the saturated steam temperature to solve the problem of transportation and to achieve finer particles of the raw material so as to be advantageous for the reaction. Therefore, it is effective when applied to a continuous hydrothermal synthesis reaction of metal oxides such as alumina, zirconia, chromia, hafnia, and titania, and a continuous extraction reaction of an active ingredient from various substances.
【図１】本発明の実施装置の一例の説明図である。FIG. 1 is an explanatory diagram of an example of an embodiment of the present invention.
１ 噴霧器 ２ 配管 ３ 配管 ４ 噴霧口 ５ 混合質 ６ サイクロン容器 ７ 噴射供給口 ８ スピンドル ９ ねじ DESCRIPTION OF SYMBOLS 1 Sprayer 2 Piping 3 Piping 4 Spray port 5 Mixture 6 Cyclone container 7 Injection supply port 8 Spindle 9 Screw
───────────────────────────────────────────────────── フロントページの続き (72)発明者 前田 彰寛 神奈川県川崎市宮前区有馬８−20−32 (72)発明者 福田 雄史 富山県黒部市沓掛844−２ (72)発明者 森村 剛 富山県黒部市堀切1300 (56)参考文献 特開 昭48−42976（ＪＰ，Ａ) 特公 平２−5136（ＪＰ，Ｂ２) (58)調査した分野(Int.Cl.7，ＤＢ名) B02C 19/06 B01J 3/02 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Akihiro Maeda 8-20-32 Arima, Miyamae-ku, Kawasaki-shi, Kanagawa (72) Inventor Yushi Fukuda 844-2 Kutsukake, Kurobe-shi, Toyama (72) Inventor Go Morimura Toyama 1300 Horikiri, Kurobe-shi (56) References JP-A-48-42976 (JP, A) JP 2-5136 (JP, B2) (58) Fields investigated (Int. Cl. 7 , DB name) B02C 19 / 06 B01J 3/02
Claims (4)
液体と飽和蒸気温度未満に加圧加熱した原料スラリーと
を噴霧器の噴霧口直前で混合して噴霧し、ついで混合流
体を筒状のサイクロン容器の一端よりその内壁に沿うよ
うに送り込み、比較的大きな微粒子をサイクロン内壁に
擦ることによって更に微粉砕し、混合流体をサイクロン
容器他端より送り出すことを特徴とする連続水熱反応に
おける原料粒子の微細化方法。1. A water-based liquid pressurized and heated above a saturated steam temperature and a raw material slurry pressurized and heated below a saturated steam temperature are mixed and sprayed immediately before a spray port of a sprayer, and then the mixed fluid is formed into a cylindrical shape. Raw material particles in a continuous hydrothermal reaction, wherein the raw material particles are fed from one end of the cyclone container along the inner wall, further pulverized by rubbing relatively large fine particles against the inner wall of the cyclone, and sending out a mixed fluid from the other end of the cyclone container. Method of miniaturization.
量を変化させる請求項１記載の連続水熱反応における原
料粒子微細化方法。2. The method for refining raw material particles in a continuous hydrothermal reaction according to claim 1, wherein the flow rate of the mixed fluid in the cyclone vessel is changed.
流体の噴霧器の噴霧口の内側に飽和蒸気温度未満に加圧
加熱した原料スラリーの供給口を設け、前記噴霧口に続
いて筒状のサイクロン容器を設け、該サイクロン容器の
一端の側部には混合流体の噴射供給部を、又、サイクロ
ン容器の他端には排出部を設けたことを特徴とする連続
水熱反応における原料粒子の微細化装置。3. A supply port for a raw material slurry pressurized and heated to a temperature lower than the saturated steam temperature is provided inside a spray port of a sprayer for a water-based fluid pressurized and heated to a temperature higher than the saturated steam temperature, and a cylindrical shape is formed following the spray port. Raw material particles in a continuous hydrothermal reaction, characterized in that a cyclone container is provided, a jet supply portion of a mixed fluid is provided at one end of the cyclone container, and a discharge portion is provided at the other end of the cyclone container. Miniaturization equipment.
射供給部側より容器内に突出するスピンドルを設け、該
スピンドルにはその容器内への突出長さを調節する調節
手段を設けたことを特徴とする請求項３記載の連続水熱
反応における原料粒子微細化装置。4. A cyclone container is provided with a spindle projecting into the container from the injection supply section at the center thereof, and an adjusting means for adjusting the length of the cyclone container projecting into the container. The apparatus for pulverizing raw material particles in a continuous hydrothermal reaction according to claim 3, characterized in that:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31208596A JP3265203B2 (en) | 1996-11-22 | 1996-11-22 | Method and apparatus for pulverizing raw material particles in continuous hydrothermal reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31208596A JP3265203B2 (en) | 1996-11-22 | 1996-11-22 | Method and apparatus for pulverizing raw material particles in continuous hydrothermal reaction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10151359A JPH10151359A (en) | 1998-06-09 |
| JP3265203B2 true JP3265203B2 (en) | 2002-03-11 |
Family
ID=18025063
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31208596A Expired - Fee Related JP3265203B2 (en) | 1996-11-22 | 1996-11-22 | Method and apparatus for pulverizing raw material particles in continuous hydrothermal reaction |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3265203B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8235314B2 (en) * | 2009-02-12 | 2012-08-07 | Linde Aktiengesellschaft | Nonequilibrium humidity control for jet milling |
-
1996
- 1996-11-22 JP JP31208596A patent/JP3265203B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH10151359A (en) | 1998-06-09 |
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