JP2012148228A - Fluidized bed apparatus - Google Patents

Fluidized bed apparatus Download PDF

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JP2012148228A
JP2012148228A JP2011008095A JP2011008095A JP2012148228A JP 2012148228 A JP2012148228 A JP 2012148228A JP 2011008095 A JP2011008095 A JP 2011008095A JP 2011008095 A JP2011008095 A JP 2011008095A JP 2012148228 A JP2012148228 A JP 2012148228A
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combustion
fluidized bed
gas supply
organic solvent
processing container
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JP5834411B2 (en
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Takuo Yanagi
拓男 柳
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Toyota Motor Corp
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

PROBLEM TO BE SOLVED: To provide a fluidized bed apparatus which can sinter a treating material while an organic solvent used for the coating of a particulate is not emitted into the atmosphere and the particulate is not deposited.SOLUTION: The fluidized bed apparatus 1 includes: a treatment container 3 to coat a particulate 2 while making it flow; a treatment liquid spray device 6 provided at the treatment container to spray a treatment liquid in the treatment container; a flow gas supply entrance 7 provided at the treatment container to make the particulate be a floatage; and a combustion device 8 provided at a slip stream channel of the treatment container to burn the organic solvent in the treatment liquid exhausted from the treatment container and to sinter the treating material.

Description

本発明は、流動層装置に関し、さらに詳しくは処理材で粉粒体を被覆するための被覆処理および処理材の焼結を連続的に行うことができる流動層装置に関する。   The present invention relates to a fluidized bed apparatus, and more particularly to a fluidized bed apparatus capable of continuously performing a coating process for coating a granular material with a treatment material and sintering of the treatment material.

近年、新素材の分野では、２つの特性を兼ね備えた粉粒体を得ることが必要となり、装置内で１つ以上の特性を有する粉粒体に他の特性を有する処理材を含む処理液を噴霧することによって粉粒体に処理材を被覆し、装置から取り出した被覆処理された粉粒体を別の焼結炉に入れて処理材を焼結するプロセスが採用されている。そのような被覆処理を行うための装置の１例として、装置内に熱風を流通させ、駆動源により回転盤を回転させて粉粒体を浮遊流動させながら処理液を噴霧して、粉粒体の表面を被覆処理する転動型の流動層装置が知られている。   In recent years, in the field of new materials, it is necessary to obtain a granular material having two characteristics, and a processing liquid containing a processing material having other characteristics in a granular material having one or more characteristics in an apparatus. A process is employed in which the particles are coated with the treatment material by spraying, and the coated particles taken out from the apparatus are placed in another sintering furnace to sinter the treatment material. As an example of an apparatus for performing such a coating process, hot air is circulated in the apparatus, a rotating liquid is rotated by a driving source, and the processing liquid is sprayed while the granular material is suspended and flowed. There is known a rolling type fluidized bed apparatus that coats the surface of the film.

しかし、このような粉粒体を流動処理する装置は、湿潤状態の粉粒体が装置の底部に堆積して長時間の被覆処理が行えないという問題を有しており、その解決のため様々な検討がされている。
例えば、特許文献１には、流動層容器内で粉粒体を気体により浮遊流動させながら被覆処理を行う流動層装置において、流動層容器に、粉粒体の処理を行う処理室と、該処理室の上方に位置し、固気分離用のフィルター部が配され、該フィルター部を昇降移動させるフィルター昇降機構が設けられている流動層装置が記載されている。そして、具体例として処理材を含むスプレー液を噴霧して流動気体による浮遊流動下に粉粒体を被覆処理し、排気ダクトを通って液の蒸気および気体を外部にそのまま排気した例が示されているが、スプレー液中の有機溶媒を回収した例は示されていない。 However, such an apparatus for fluidizing the granular material has a problem that the wet granular material accumulates on the bottom of the apparatus and cannot be coated for a long time. Consideration has been made.
For example, Patent Document 1 discloses that in a fluidized bed apparatus that performs a coating process while suspending and flowing a granular material with gas in a fluidized bed container, a processing chamber for processing the granular material in the fluidized bed container; There is described a fluidized bed apparatus which is located above the chamber, is provided with a filter unit for solid-gas separation, and is provided with a filter lifting mechanism for moving the filter unit up and down. As a specific example, an example is shown in which a spray liquid containing a treatment material is sprayed to coat the powder particles in a floating flow with a flowing gas, and the liquid vapor and gas are exhausted as they are through the exhaust duct. However, an example of recovering the organic solvent in the spray liquid is not shown.

特開２００７−３０７４４８号公報JP 2007-307448 A

しかし、上記の従来技術によって粉粒体に処理材を被覆処理しても、得られた粉粒体がそのままでは最終製品には適用できない場合は、被覆処理された粉粒体を別の焼結炉に入れて処理材を高温で焼結することが必要である。そのような場合、粉粒体を堆積させて焼結が行われるため、得られる粉粒体の品質の均一性が不十分な場合がある。このため、焼結後の粉粒体の品質の均一性を確保する必要性から、粉粒体が堆積していない状態で焼結することが望まれている。また、上記の従来技術においては、粉粒体の被覆処理に用いた有機溶媒は資源として利用されることなく大気中に放出されており、省資源、焼結に要するエネルギーの消費および環境上の観点から問題がある。   However, if the obtained granular material cannot be applied to the final product as it is even after the powder is coated with the treatment material by the above-mentioned conventional technology, the coated granular material is subjected to another sintering. It is necessary to sinter the treated material at a high temperature in a furnace. In such a case, since the granular material is deposited and sintered, the uniformity of the quality of the obtained granular material may be insufficient. For this reason, from the necessity of ensuring the uniformity of the quality of the sintered granular material, it is desired to sinter in a state where the granular material is not deposited. In the above prior art, the organic solvent used for the powder coating process is released into the atmosphere without being used as a resource, saving resources, consuming energy required for sintering, and environmentally friendly. There is a problem from the point of view.

従って、本発明の目的は、粉粒体の被覆処理に用いた有機溶媒を大気中に放出しないで、且つ粉粒体が堆積していない状態で粉粒体に被覆された処理材を焼結し得る流動層装置を提供することである。   Accordingly, an object of the present invention is to sinter the treatment material coated with the powder without releasing the organic solvent used for the powder coating to the atmosphere and without the powder being deposited. It is to provide a fluidized bed apparatus that can.

本発明は、粉粒体を浮遊流動させながら被覆処理するための処理容器、処理容器内に処理液を噴霧するために処理容器に設けられた処理液噴霧装置、粉粒体を浮遊流動させるために処理容器に設けられた流動用ガス供給口、および処理容器から排出された処理液中の有機溶媒を燃焼させて処理材を焼結するために処理容器の後流路に設けられた燃焼装置を備えてなる流動層装置に関する。   The present invention relates to a processing container for performing a coating process while floating powder particles, a processing liquid spraying device provided in the processing container for spraying the processing liquid in the processing container, and floating powder particles A gas supply port for flow provided in the processing vessel, and a combustion device provided in a rear flow path of the processing vessel for sintering the processing material by burning the organic solvent in the processing liquid discharged from the processing vessel It relates to the fluidized bed apparatus provided with.

本発明によれば、粉粒体の被覆処理に用いた有機溶媒を大気中に放出しないで、且つ粉粒体が堆積していない状態で粉粒体に被覆された処理材を焼結し得る流動層装置が得られる。   According to the present invention, it is possible to sinter the treatment material coated with the granular material without releasing the organic solvent used for the coating treatment of the granular material into the atmosphere and without the granular material being deposited. A fluidized bed apparatus is obtained.

図１は、従来の流動層装置の概略図である。FIG. 1 is a schematic view of a conventional fluidized bed apparatus. 図２は、従来の流動層装置により被覆処理された粉粒体の処理材を焼結炉に入れて焼結している状態を示す模式図である。FIG. 2 is a schematic view showing a state in which a granular material treated with a conventional fluidized bed apparatus is put in a sintering furnace and sintered. 図３は、本発明の第１の実施態様の流動層装置の概略図である。FIG. 3 is a schematic view of a fluidized bed apparatus according to the first embodiment of the present invention. 図４は、本発明の第２の実施態様の流動層装置の概略図である。FIG. 4 is a schematic view of a fluidized bed apparatus according to a second embodiment of the present invention. 図５は、本発明の第３の実施態様の流動層装置の概略図である。FIG. 5 is a schematic view of a fluidized bed apparatus according to a third embodiment of the present invention. 図６は、本発明の第２および第３の実施態様の燃焼装置における温度制御フローチャートである。FIG. 6 is a temperature control flowchart in the combustion apparatus of the second and third embodiments of the present invention. 図７は、本発明の第４の実施態様の流動層装置の概略図である。FIG. 7 is a schematic view of a fluidized bed apparatus according to a fourth embodiment of the present invention. 図８は、本発明の第４の実施態様の燃焼装置における温度制御フローチャートである。FIG. 8 is a temperature control flowchart in the combustion apparatus of the fourth embodiment of the present invention.

特に、本発明において、以下の実施態様を挙げることができる。
１）前記燃焼装置が、有機溶媒蒸気に着火させるための着火源および有機溶媒が燃焼して生じる炎を閉じ込めるための火炎制御装置を備えてなる前記流動層装置。
２）前記流動用ガス供給口が不活性ガス供給口であり、前記燃焼装置が前記着火源である燃焼触媒層、有機溶媒蒸気を燃焼させるために必要な空気又は酸素を供給する支燃ガス供給装置、および燃焼温度を測定するための熱電対を備えてなる前記流動層装置。
３）前記流動用ガス供給口が不活性ガス供給口であり、前記燃焼装置が前記着火源である放電装置、有機溶媒蒸気を燃焼させるために必要な空気又は酸素を供給する支燃ガス供給装置、燃焼温度を測定するための熱電対、および有機溶媒が燃焼して生じる炎を一定領域に閉じ込めるための火炎制御装置を備えてなる前記流動層装置。 In particular, in the present invention, the following embodiments can be mentioned.
1) The fluidized bed apparatus, wherein the combustion apparatus includes an ignition source for igniting the organic solvent vapor and a flame control apparatus for confining a flame generated by the combustion of the organic solvent.
2) The flow gas supply port is an inert gas supply port, and the combustion support layer supplies the air or oxygen necessary for burning the combustion catalyst layer, the organic solvent vapor, and the combustion device as the ignition source. The fluidized bed apparatus comprising a supply device and a thermocouple for measuring a combustion temperature.
3) The flow gas supply port is an inert gas supply port, and the combustion device is a discharge device that is the ignition source, and the combustion support gas supply that supplies air or oxygen necessary for burning the organic solvent vapor. The fluidized bed apparatus comprising an apparatus, a thermocouple for measuring a combustion temperature, and a flame control apparatus for confining a flame generated by burning an organic solvent in a certain region.

４）前記流動用ガス供給口が空気又は酸素供給口であり、前記燃焼装置が、前記着火源である燃焼触媒層、燃焼温度が過度に上昇しないように制御するための不活性ガスを供給する不活性ガス供給装置、燃焼温度を測定するための熱電対、および有機溶媒が燃焼して生じる炎を一定領域に閉じ込めるための火炎制御装置を備えてなる前記流動層装置。
５）前記処理容器が、固体電池用活物質粒子にリチウムイオン伝導体を被覆するためのものである前記流動層装置。 4) The flow gas supply port is an air or oxygen supply port, and the combustion device supplies a combustion catalyst layer as the ignition source and an inert gas for controlling the combustion temperature so as not to rise excessively. The fluidized bed apparatus comprising: an inert gas supply device that performs the above operation, a thermocouple for measuring the combustion temperature, and a flame control device for confining a flame generated by burning the organic solvent in a certain region.
5) The fluidized bed apparatus, wherein the processing container is for covering the active material particles for a solid battery with a lithium ion conductor.

以下、図面を参照して本発明を詳説する。
従来の流動層装置１０は、図１に示すように、粉粒体２を浮遊流動させながら被覆処理するための処理容器３、該処理容器内の底部に設けられて粉粒体２を回転させるために水平回転する回転盤４と該処理容器の下部に設けられて回転盤を回転駆動するモーターなどの回転盤駆動手段５、処理容器内に処理液を噴霧するために処理容器に設けられた処理液噴霧装置６、粉粒体２を浮遊流動させるために処理容器の下方に設けられた流動用ガス導入口７、処理された粉粒体の系外への排出を防止するためのフィルター３０および気体排出口４０を備えてなるものである。 Hereinafter, the present invention will be described in detail with reference to the drawings.
As shown in FIG. 1, a conventional fluidized bed apparatus 10 is provided with a processing container 3 for performing a coating process while floating and flowing a powdered particle 2, and rotates the powdered particle 2 provided at the bottom of the processing container. In order to spray the processing liquid into the processing container, a rotating disk 4 that rotates horizontally and a rotating disk driving means 5 such as a motor that rotates and drives the rotating disk provided below the processing container are provided in the processing container. A treatment liquid spraying device 6, a flow gas introduction port 7 provided below the treatment container for floating and flowing the granular material 2, and a filter 30 for preventing the treated granular material from being discharged out of the system. And a gas discharge port 40.

そして、従来の流動層装置１０においては、浮遊流動状態にある粉粒体２はフィルター３０によって気体と分離され、処理液に通常含まれる有機溶媒、例えばアルコールが系外に排出され、省資源および環境上の問題が生じる。しかも、フィルターによる目詰まりの問題があるため、粒径が４μｍ以下の粉粒体は処理し得ない。
また、このようにして被覆処理された粉粒体はそのままでは最終製品に適用できない場合があり、図２に示すように、焼結炉に入れて粉粒体に被覆された処理材を焼結される。その際、粉粒体を堆積して高温での焼結が行われるため、堆積物の内部と表面とでは温度にむらが生じ、得られる粉粒体に品質の均一性が確保されない場合がある。 And in the conventional fluidized bed apparatus 10, the granular material 2 in a floating fluid state is separated from the gas by the filter 30, and the organic solvent, for example, alcohol normally contained in the treatment liquid is discharged out of the system, saving resources and Environmental problems arise. In addition, since there is a problem of clogging by the filter, it is impossible to process a powder having a particle size of 4 μm or less.
In addition, the granular material coated in this way may not be applied to the final product as it is, and as shown in FIG. 2, the processing material coated with the granular material is sintered in a sintering furnace. Is done. At that time, since the granular material is deposited and sintered at a high temperature, the temperature may vary between the inside and the surface of the deposit, and quality uniformity may not be ensured in the obtained granular material. .

本発明の第１の実施態様の流動層装置１は、図３に示すように、粉粒体２を浮遊流動させながら被覆処理するための処理容器３、該処理容器内の底部に設けられて粉粒体２を回転させるために回転する回転盤４と該処理容器の下部に設けられて回転盤を回転駆動する回転盤駆動手段５、処理容器３内に処理液を噴霧するために処理容器に設けられた処理液噴霧装置６、粉粒体を浮遊流動させるために処理容器の下方に設けられた流動用ガス供給口７、それぞれ処理容器の後流路２０に設けられた、処理容器から排出された処理液中の有機溶媒蒸気を燃焼させて処理材を焼結させるための燃焼装置８、焼結粉粒体を回収するための焼結粉粒体回収容器４０、および気体排出口５０を備えている。
前記第１の実施態様においては回転盤４と回転盤駆動手段５とを備えているが、流動用ガスのみによって粉粒体を浮遊流動させることも可能である。 As shown in FIG. 3, the fluidized bed apparatus 1 of the first embodiment of the present invention is provided at a bottom of the processing container 3 for coating the powder 2 while floating and flowing the granular material 2. A rotating disk 4 that rotates to rotate the granular material 2, a rotating disk drive means 5 that is provided below the processing container to rotate the rotating disk, and a processing container for spraying the processing liquid into the processing container 3. From the processing container provided in the rear flow path 20 of the processing container, the gas supply port 7 for the flow provided in the lower part of the processing container to float and flow the granular material, respectively. Combustion device 8 for burning the organic solvent vapor in the discharged treatment liquid to sinter the treatment material, sintered powder collection container 40 for collecting the sintered powder, and gas outlet 50 It has.
In the first embodiment, the rotating disk 4 and the rotating disk driving means 5 are provided. However, it is also possible to float and flow the granular material only by the flowing gas.

本発明の前記実施態様の流動層装置１によれば、処理容器の後流路に有機溶媒蒸気を燃焼させて処理材を焼結させるための燃焼装置８を備えていることにより、被覆処理された粉粒体は燃焼装置８を気体とともに通過中に堆積していない状態で焼結され、また粉粒体の被覆処理に用いた有機溶媒は焼結用燃料として利用される。そして、フィルターを用いる必要がないため、粒径が４μｍ以下、例えば２μｍ程度の粉粒体であっても処理され得る。   According to the fluidized-bed apparatus 1 of the said embodiment of this invention, it is coated by having the combustion apparatus 8 for burning an organic solvent vapor | steam in the back flow path of a processing container, and sintering a processing material. The powder particles are sintered in a state where they are not deposited while passing through the combustion device 8 with the gas, and the organic solvent used for the coating treatment of the powder particles is used as a fuel for sintering. And since it is not necessary to use a filter, even if it is a granular material with a particle size of 4 micrometers or less, for example, about 2 micrometers, it can be processed.

本発明における粉粒体としては、特に制限はなく１つ以上の特性を有する粉粒体に他の特性を有する処理材を含む処理液を噴霧して粉粒体に処理材を被覆する必要のある任意の技術分野の粉粒体が挙げられ、例えばＡｌ２Ｏ３、Ａｌ（ＯＨ）３、ＴｉＯ２、ＺｒＯ２、ＳｉＯ２、ＣｅＯ２、固体電池用活物質粒子などの粉粒体が挙げられる。特に、本発明は、湿式コーティングの適用が困難である固体電池用活物質粒子にリチウムイオン伝導体を被覆する場合に特に好適に適用し得る。 The granular material in the present invention is not particularly limited, and it is necessary to spray the treatment liquid containing a treatment material having other characteristics on the granular material having one or more characteristics to cover the granular material with the treatment material. Examples include powders of an arbitrary technical field, such as powders such as Al 2 O 3 , Al (OH) 3 , TiO 2 , ZrO 2 , SiO 2 , CeO 2 , and active material particles for solid batteries. It is done. In particular, the present invention can be particularly suitably applied when a lithium ion conductor is coated on active material particles for a solid battery, which are difficult to apply wet coating.

本発明における処理液としては、特に制限はなく、粉粒体とは異なる所定の特性を有する処理材、例えばリチウムイオン伝導体（焼結体）がＬｉ４ＳｉＯ４である場合、その原料である（Ｃ２Ｈ５Ｏ）４ＳｉおよびＣＨ３ＣＯＯＬｉ・２Ｈ２Ｏなどのリチウムイオン伝導体前駆体又はその加水分解物を含む有機溶媒、例えばアルコール溶液が挙げられる。前記処理液は、例えば貯蔵槽６０から供給され得る。
また、本発明における流動用ガスとしては、特に制限はなく、不活性ガス、例えば窒素や空気、酸素などが挙げられる。
また、本発明における処理液の噴霧装置としては、一般的な液送ポンプと噴霧ノズルを組み合わせて使用し得る。
また、本発明の処理液噴霧装置に用いる気体（ガス）としては、処理液を噴霧させるために通常は噴出用ガス、例えば窒素などの不活性ガス又は空気が用いられる。 The treatment liquid in the present invention is not particularly limited, the processing material having a different predetermined characteristic than the granular material, for example, when a lithium ion conductor (sintered body) is Li 4 SiO 4, is the raw material Examples include (C 2 H 5 O) 4 Si and an organic solvent containing a lithium ion conductor precursor such as CH 3 COOLi · 2H 2 O or a hydrolyzate thereof, for example, an alcohol solution. The processing liquid can be supplied from the storage tank 60, for example.
Moreover, there is no restriction | limiting in particular as the gas for flow in this invention, For example, inert gas, for example, nitrogen, air, oxygen etc. are mentioned.
Moreover, as a spray apparatus for the treatment liquid in the present invention, a general liquid feed pump and a spray nozzle can be used in combination.
Further, as the gas (gas) used in the treatment liquid spraying apparatus of the present invention, an ejection gas, for example, an inert gas such as nitrogen or air is usually used to spray the treatment liquid.

前記処理容器としては、処理温度が１００℃未満である通常の処理条件では特に制限はなく、例えば剛性を有する樹脂製、例えばアクリル樹脂製あるいはステンレス製の略円筒状の装置を使用できる。本発明における前記回転盤と回転盤駆動手段とを備えた処理容器として、例えば一般的な転動流動層コーティング装置、例えば株式会社パウレック製のマルチプレックス（ＭＰシリーズ）や回転盤部に解砕機構を備えた装置（ＭＰ−ＳＦＰシリーズ）やフロイント産業株式会社のフローコーター、コートマイザーなどを使用することができる。   The processing vessel is not particularly limited under normal processing conditions where the processing temperature is less than 100 ° C., and for example, a substantially cylindrical apparatus made of a resin having rigidity, for example, an acrylic resin or stainless steel can be used. As a processing container provided with the said rotating disk and rotating disk drive means in this invention, for example, a general rolling fluidized bed coating apparatus, for example, a multiplex (MP series) manufactured by Paulek Co., Ltd. (MP-SFP series), a flow coater manufactured by Freund Sangyo Co., Ltd., a coater, etc. can be used.

本発明において、前記燃焼装置として、有機溶媒に着火させるための着火源および有機溶媒が燃焼して生じる炎を閉じ込めるための火炎制御装置の組み合わせが挙げられる。
また、本発明において、前記処理容器への粉粒体の導入は、バッチ式に処理前に処理容器内に一度に加えられてもよくあるいは、粉粒体導入口（図示せず）を介して連続的又は逐次的に処理容器内に加えてもよい。前記の粉粒体をバッチ式に処理前に処理容器内に一度に加える場合、処理容器としては開閉可能な構造を有している必要があり、開閉部はシーリング部材、例えばオーリングによって処理容器の上部と下部とが粒体導入後は密閉され得る。 In the present invention, examples of the combustion apparatus include a combination of an ignition source for igniting an organic solvent and a flame control apparatus for confining a flame generated by burning the organic solvent.
In the present invention, the introduction of the granular material into the processing container may be added to the processing container at one time before the processing in a batch manner, or through a granular material inlet (not shown). You may add in a processing container continuously or sequentially. In the case where the above-mentioned powder particles are added to the processing container at once before processing in a batch type, the processing container needs to have a structure that can be opened and closed, and the opening and closing part is a sealing container, for example, an O-ring. The upper part and the lower part of can be sealed after the introduction of the granules.

また、本発明の第２の実施態様の流動層装置１は、図４に示すように、前記流動用ガス供給口７が不活性ガス供給口であり、燃焼装置８として、処理容器の後流路２０に設けられた、有機溶媒を燃焼させるための着火源としての燃焼触媒層２１、有機溶媒蒸気を燃焼させるために必要な空気又は酸素を供給する支燃ガス供給装置２２、燃焼温度を測定するための熱電対２３、および有機溶媒が燃焼して生じる炎を一定領域に閉じ込めるための火炎制御装置２４が備えられている。また、前記の流動層装置１においては、図４に示すように、処理液を噴霧するために処理容器に設けられた処理液噴霧装置６には噴霧ガスとして不活性ガス、例えば窒素（Ｎ２）が供給され得る。 In addition, as shown in FIG. 4, the fluidized bed apparatus 1 according to the second embodiment of the present invention is configured such that the fluid gas supply port 7 is an inert gas supply port, and the combustion apparatus 8 serves as a wake of the processing vessel. Combustion catalyst layer 21 as an ignition source for burning organic solvent, combustion support gas supply device 22 for supplying air or oxygen necessary for burning organic solvent vapor, and combustion temperature A thermocouple 23 for measurement and a flame control device 24 for confining a flame generated by burning an organic solvent in a certain region are provided. Further, in the fluidized bed apparatus 1, as shown in FIG. 4, an inert gas such as nitrogen (N 2) is used as a spray gas in the process liquid spray apparatus 6 provided in the process container for spraying the process liquid. ) May be provided.

前記の燃焼触媒層としては、例えば、触媒成分としてＰｔ、Ａｇ、ＡｕやＭｏＯ３をベースとする複合モリブデン酸やＳｂ複合酸化物、Ｗ、Ｃｏの酸化物などの粉末又は顆粒の固定床であり得て、特に急激な燃焼が起こらず温度制御が容易である前記燃焼触媒成分を担持させたハニカムを設置することが好適である。
また、燃焼触媒層には、少なくとも１ヶ所に熱電対２３が設置され、燃焼温度を測定する。
また、前記支燃ガス供給装置には、通常高い精度で支燃ガスを供給するためにマスフローコントローラが備えられ得る。
また、前記火炎制御装置としては、熱を奪うために高熱伝導性のステンレス等の金属で作製され、一般的にフレームアレスタ又は逆火防止装置と呼ばれるフィルター付の弁が挙げられる。前記フレームアレスタは通常着火源の前後に備えられ、炎は燃焼域内に閉じ込められる。フレームアレスタによって、運転状態が非定常状態となって大きな炎が形成されても、燃焼による炎が出口あるいは処理容器側に噴き出ることを防止し得る。
前記の後流路２０の火炎制御装置の後の位置に、必要であればクーラーなどを設けて排出される粉粒体および気体を室温まで冷却してもよい。 The combustion catalyst layer is, for example, a fixed bed of powder or granules such as a composite molybdic acid or Sb composite oxide based on Pt, Ag, Au or MoO 3 as a catalyst component, or an oxide of W or Co. In particular, it is preferable to install a honeycomb on which the combustion catalyst component is supported, in which rapid combustion does not occur and temperature control is easy.
Moreover, the thermocouple 23 is installed in at least one place in the combustion catalyst layer, and the combustion temperature is measured.
In addition, the combustion support gas supply device may be provided with a mass flow controller in order to supply the combustion support gas with high accuracy.
The flame control device includes a filter valve made of a metal such as stainless steel having high thermal conductivity in order to take heat away, and generally called a flame arrester or a backfire prevention device. The flame arrestor is usually provided before and after the ignition source, and the flame is confined in the combustion zone. Even if the operation state becomes an unsteady state and a large flame is formed by the flame arrester, it is possible to prevent the flame due to combustion from being ejected to the outlet or the processing container side.
If necessary, a cooler or the like may be provided at a position after the flame control device in the rear flow path 20 to cool the discharged granular material and gas to room temperature.

また、本発明の第３の実施態様の流動層装置１は、図５に示すように、前記流動用ガス供給口７が不活性ガス供給口であり、燃焼装置８として、処理容器の後流路２０に設けられた、有機溶媒を燃焼させるための着火源としての放電装置３１、有機溶媒蒸気を燃焼させるために必要な空気又は酸素を供給する支燃ガス供給装置３２、燃焼温度を測定するための熱電対３３、および有機溶媒が燃焼して生じる炎を一定領域に閉じ込めるための火炎制御装置３４が備えられている。また、前記の流動層装置１においては、図５に示すように、処理液を噴霧するために処理容器に設けられた処理液噴霧装置６において噴霧ガスとして不活性ガス、例えば窒素（Ｎ２）が供給され得る。
前記の放電装置３１としては、パルス放電や連続放電などが用いられ得る。
そして、前記支燃ガス供給装置には、通常高い精度で支燃ガスを供給するためにマスフローコントローラが備えられ得る。 In addition, as shown in FIG. 5, the fluidized bed apparatus 1 of the third embodiment of the present invention is such that the fluid gas supply port 7 is an inert gas supply port, and the combustion device 8 serves as a wake of the processing vessel. Discharge device 31 provided as an ignition source for burning organic solvent provided in passage 20, combustion support gas supply device 32 for supplying air or oxygen necessary for burning organic solvent vapor, and measuring combustion temperature And a flame control device 34 for confining a flame generated by burning an organic solvent in a certain region. In the fluidized bed apparatus 1, as shown in FIG. 5, an inert gas such as nitrogen (N 2 ) is used as a spray gas in the processing liquid spraying apparatus 6 provided in the processing container for spraying the processing liquid. Can be supplied.
As the discharge device 31, pulse discharge, continuous discharge, or the like can be used.
The combustion support gas supply device may be provided with a mass flow controller in order to supply combustion support gas with high accuracy.

本発明の第２、第３の実施態様の装置により有機溶媒蒸気を燃焼させる際に、図６に示すように、燃焼温度を測定し、測定温度と設定温度とを比較し、フローチャートに従って、測定温度が設定温度より低い場合は空気又は酸素の支燃ガス流量を増やし、測定温度が設定温度より高い場合は空気又は酸素の支燃ガス流量を減らして、支燃ガス供給装置からの支燃ガスの供給を調整することによって、燃焼温度を設定温度に保つことができる。この設定温度は、処理材の種類によって異なり、例えば固体電池用活物質粒子にリチウムイオン伝導体を被覆する場合は焼結に必要な燃焼温度は３００〜５００℃の範囲内であり得る。   When the organic solvent vapor is burned by the apparatus of the second and third embodiments of the present invention, as shown in FIG. 6, the combustion temperature is measured, the measured temperature is compared with the set temperature, and the measurement is performed according to the flowchart. If the temperature is lower than the set temperature, increase the support gas flow rate of air or oxygen, and if the measured temperature is higher than the set temperature, decrease the support gas flow rate of air or oxygen to reduce the support gas from the support gas supply device. The combustion temperature can be kept at the set temperature by adjusting the supply of. This set temperature varies depending on the type of the treatment material. For example, when the solid material active material particles are coated with a lithium ion conductor, the combustion temperature required for sintering may be in the range of 300 to 500 ° C.

また、本発明の第４実施態様の流動層装置１は、図７に示すように、前記流動用ガス供給口７が空気又は酸素供給口であり、前記燃焼装置として、前記着火源としての燃焼触媒層４１、燃焼温度が過度に上昇しないように制御するための不活性ガスを供給する不活性ガス供給装置４２、燃焼温度を測定するための熱電対４３、および有機溶媒が燃焼して生じる炎を一定領域に閉じ込めるための火炎制御装置４４が備えられている。また、前記の流動層装置１においては、図７に示すように、処理液を噴霧するために処理容器に設けられた処理液噴霧装置６において噴霧ガスとして空気又は酸素（Ｏ２）が供給され得る。
そして、前記不活性ガス供給装置には、通常高い精度で不活性ガスを供給するためにマスフローコントローラが備えられ得る。 Further, in the fluidized bed apparatus 1 of the fourth embodiment of the present invention, as shown in FIG. 7, the fluid gas supply port 7 is an air or oxygen supply port, and the combustion device is the ignition source. Combustion catalyst layer 41, an inert gas supply device 42 for supplying an inert gas for controlling the combustion temperature so as not to rise excessively, a thermocouple 43 for measuring the combustion temperature, and an organic solvent are burned. A flame control device 44 is provided to confine the flame in a certain area. Further, in the fluidized bed apparatus 1, as shown in FIG. 7, air or oxygen (O 2 ) is supplied as a spray gas in the processing liquid spraying apparatus 6 provided in the processing container for spraying the processing liquid. obtain.
The inert gas supply device may be provided with a mass flow controller for supplying an inert gas with high accuracy.

本発明の第４の実施態様の装置により有機溶媒蒸気を燃焼させる際に、図８に示すように、燃焼温度を測定し、測定温度と設定温度とを比較し、フローチャートに従って、測定温度が設定温度より高い場合は不活性ガス流量を増やし、測定温度が設定温度より低い場合は不活性ガス流量を減らして、不活性ガス供給装置からの不活性ガスの供給量を調整することによって、燃焼温度を設定温度に保つことができる。
本発明の第４実施態様の流動層装置によれば、不活性ガスの使用量を大幅に低減し得るので特に好適である。 When the organic solvent vapor is burned by the apparatus of the fourth embodiment of the present invention, as shown in FIG. 8, the combustion temperature is measured, the measured temperature is compared with the set temperature, and the measured temperature is set according to the flowchart. The combustion temperature is increased by increasing the inert gas flow rate when the temperature is higher than the temperature, and decreasing the inert gas flow rate when the measurement temperature is lower than the set temperature, thereby adjusting the supply amount of the inert gas from the inert gas supply device. Can be kept at the set temperature.
The fluidized bed apparatus according to the fourth embodiment of the present invention is particularly suitable because the amount of inert gas used can be greatly reduced.

本発明によって、粉粒体の表面全体又は表面の一部に焼結処理材が被覆又は堆積した被覆処理粉粒体を、省資源、エネルギー消費および環境等の従来の問題を生じることなく連続的に得ることができる。
特に、熱電対で温度測定し、支燃ガス流量又は不活性ガス流量、特に支燃ガス流量にフィードバックすることにより、安定した燃焼温度を維持することが可能となり、品質の安定した焼結粉粒体を得ることができる。 According to the present invention, the coated powder particles in which the sintered material is coated or deposited on the entire surface or a part of the surface of the powder particles can be continuously produced without causing conventional problems such as resource saving, energy consumption and environment. Can get to.
In particular, it is possible to maintain a stable combustion temperature by measuring the temperature with a thermocouple and feeding it back to the combustion support gas flow rate or inert gas flow rate, particularly the combustion support gas flow rate. You can get a body.

本発明の流動層装置によって、粉粒体の被覆処理に用いた有機溶媒は大気中に放出しないで、且つ粉粒体が堆積していない状態で焼結した被覆処理粉粒体を連続的に得ることができる。   By using the fluidized bed apparatus of the present invention, the organic solvent used for the coating treatment of the powder particles is not released into the atmosphere, and the coated powder particles sintered in a state where the powder particles are not deposited are continuously formed. Obtainable.

１ 本発明の実施態様の流動層装置
２ 粉粒体
３ 処理容器
４ 回転盤
５ 回転盤駆動手段
６ 処理液噴霧装置
７ 流動用ガス導入口
８ 燃焼装置
１０ 従来の流動層装置
２０ 後流路
２１、４１ 燃焼触媒層
２２、３２ 支燃ガス供給装置
２３、３３、４３ 熱電対
２４、３４、４４ 火炎制御装置
３０ フィルター
３１ 放電装置
４０ 焼結粉粒体回収容器
４１ 不活性ガス供給装置
５０ 気体排出口
６０ 処理液貯蔵槽 DESCRIPTION OF SYMBOLS 1 Fluidized bed apparatus of embodiment of this invention 2 Powder body 3 Processing container 4 Rotating disk 5 Rotating disk drive means 6 Processing liquid spraying apparatus 7 Gas inlet for flow 8 Combustion apparatus 10 Conventional fluidized bed apparatus 20 Rear flow path 21 , 41 Combustion catalyst layer 22, 32 Combustion gas supply device 23, 33, 43 Thermocouple 24, 34, 44 Flame control device 30 Filter 31 Discharge device 40 Sintered powder recovery container 41 Inert gas supply device 50 Gas exhaust Outlet 60 Treatment liquid storage tank

Claims (6)

粉粒体を浮遊流動させながら被覆処理するための処理容器、処理容器内に処理液を噴霧するために処理容器に設けられた処理液噴霧装置、粉粒体を浮遊流動させるために処理容器に設けられた流動用ガス供給口、および処理容器から排出された処理液中の有機溶媒を燃焼させて処理材を焼結するために処理容器の後流路に設けられた燃焼装置を備えてなる流動層装置。   A processing container for carrying out a coating process while floating particles and powder, a processing liquid spraying device provided in the processing container for spraying the processing liquid in the processing container, and a processing container for floating and flowing the particles. A flow gas supply port provided; and a combustion device provided in a rear flow path of the processing container for burning the organic solvent in the processing liquid discharged from the processing container to sinter the processing material. Fluidized bed equipment. 前記燃焼装置が、着火源および有機溶媒が燃焼して生じる炎を閉じ込めるための火炎制御装置を備えてなる請求項１に記載の流動層装置。   The fluidized bed apparatus according to claim 1, wherein the combustion apparatus includes a flame control apparatus for confining a flame generated by combustion of an ignition source and an organic solvent. 前記流動用ガス供給口が不活性ガス供給口であり、前記燃焼装置が前記着火源である燃焼触媒層、有機溶媒蒸気を燃焼させるために必要な空気又は酸素を供給する支燃ガス供給装置、および燃焼温度を測定するための熱電対を備えてなる請求項２に記載の流動層装置。   The flow gas supply port is an inert gas supply port, the combustion device is a combustion catalyst layer that is the ignition source, and the combustion support gas supply device that supplies air or oxygen necessary for burning the organic solvent vapor. And a fluidized bed device according to claim 2, comprising a thermocouple for measuring the combustion temperature. 前記流動用ガス供給口が不活性ガス供給口であり、前記燃焼装置が前記着火源である放電装置、有機溶媒蒸気を燃焼させるために必要な空気又は酸素を供給する支燃ガス供給装置、燃焼温度を測定するための熱電対、および有機溶媒が燃焼して生じる炎を一定領域に閉じ込めるための火炎制御装置を備えてなる請求項１又は２に記載の流動層装置。   The gas supply port for flow is an inert gas supply port, the discharge device is the ignition source, the combustion support gas supply device for supplying air or oxygen necessary for burning the organic solvent vapor, The fluidized bed apparatus according to claim 1 or 2, comprising a thermocouple for measuring a combustion temperature and a flame control apparatus for confining a flame generated by burning an organic solvent in a certain region. 前記流動用ガス供給口が空気又は酸素供給口であり、前記燃焼装置が前記着火源である燃焼触媒層、燃焼温度が過度に上昇しないように制御するための不活性ガスを供給する不活性ガス供給装置、燃焼温度を測定するための熱電対、および有機溶媒が燃焼して生じる炎を一定領域に閉じ込めるための火炎制御装置を備えてなる請求項１又は２に記載の流動層装置。   The flow gas supply port is an air or oxygen supply port, the combustion device is a combustion catalyst layer that is the ignition source, and an inert gas that supplies an inert gas for controlling the combustion temperature so as not to rise excessively. The fluidized bed apparatus according to claim 1 or 2, comprising a gas supply apparatus, a thermocouple for measuring a combustion temperature, and a flame control apparatus for confining a flame generated by burning an organic solvent in a certain region. 前記処理容器が、固体電池用活物質粒子にリチウムイオン伝導体を被覆するためのものである請求項１〜５のいずれか１項に記載の流動層装置。   The fluidized bed apparatus according to any one of claims 1 to 5, wherein the processing container is for coating a solid ion active material particle with a lithium ion conductor.
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CN109585797A (en) * 2017-09-29 2019-04-05 横店集团东磁股份有限公司 A kind of coating modification electrode material and preparation method thereof
CN109585797B (en) * 2017-09-29 2020-12-25 横店集团东磁股份有限公司 Coated modified electrode material and preparation method thereof
WO2021107257A1 (en) * 2019-11-27 2021-06-03 에스티엑스건설 주식회사 Highly efficient and highly rigid dual fluidized bed reactor
KR20210066052A (en) * 2019-11-27 2021-06-07 에스티엑스건설 주식회사 High efficiency, high rigidity dual fluidized bed reactor
KR102376472B1 (en) 2019-11-27 2022-03-18 에스티엑스건설 주식회사 High efficiency, high rigidity dual fluidized bed reactor

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