JP6746104B2 - In-cell coating device and method for manufacturing reaction container using the same - Google Patents
In-cell coating device and method for manufacturing reaction container using the same Download PDFInfo
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Description
本発明は、ハニカム状反応容器の各セル内に複数の材料を塗布するためのセル内塗布装置、並びに、ハニカム状反応容器の各セル内に複数の材料が塗布された反応容器を製造する方法に関する。 The present invention is an in-cell coating device for coating a plurality of materials in each cell of a honeycomb-shaped reaction container, and a method for manufacturing a reaction container in which a plurality of materials are coated in each cell of a honeycomb-shaped reaction container. Regarding
自動車等に用いられる排ガス浄化用触媒としては、例えば、複数の貫通孔を有するハニカム基材と、このハニカム基材のセル内に塗布された触媒材料からなる触媒層とを備えるものが知られている。このような触媒層としては、従来、１種類の触媒材料を塗布して形成された単層の触媒層が用いられていたが、近年、触媒性能の向上のために、複数の触媒材料を塗布して形成された、組成が異なる複数の触媒層が排ガスの流れ方向（セルの長手方向）に分布している流れ方向分離型の触媒層や排ガスの流れ方向に垂直な方向（セルの短手方向又は半径方向）に分布している多層の触媒層が用いられるようになってきた。 As an exhaust gas purifying catalyst used for automobiles, for example, one provided with a honeycomb base material having a plurality of through holes and a catalyst layer made of a catalyst material applied in the cells of the honeycomb base material is known. There is. As such a catalyst layer, conventionally, a single-layer catalyst layer formed by applying one kind of catalyst material has been used, but in recent years, a plurality of catalyst materials are applied to improve the catalyst performance. A plurality of catalyst layers formed with different composition are distributed in the exhaust gas flow direction (longitudinal direction of the cell). The flow direction separation type catalyst layer and the direction perpendicular to the exhaust gas flow direction (short side of the cell). Multi-layered catalyst layers, distributed in the radial or radial direction, have come into use.
例えば、特開２００７−２６８４８４号公報（特許文献１）には、ハニカム基材のセル隔壁の表面に、複数のスラリーをハニカム基材の軸方向及び径方向の少なくとも一方で異なる分布パターンをもつようにコートする方法であって、前記分布パターンと略同一パターンとなるように複数のスラリーを筒状のコート治具に区画して充填し、このコート治具をハニカム基材の一端面に当接させ、前記コート治具の端面からスラリーをセル通路に導入するコート方法が記載されている。 For example, in Japanese Unexamined Patent Application Publication No. 2007-268484 (Patent Document 1), a plurality of slurries have different distribution patterns in at least one of the axial direction and the radial direction of the honeycomb base material on the surface of the cell partition walls of the honeycomb base material. A plurality of slurries are divided and filled in a cylindrical coating jig so as to have a pattern substantially the same as the distribution pattern, and the coating jig is brought into contact with one end face of the honeycomb substrate. Then, a coating method is described in which the slurry is introduced into the cell passage from the end surface of the coating jig.
また、国際公開第２０１０／１１４１３２号（特許文献２）には、複数の吐出口が設けられているノズルと、このノズルに接続されている流体供給装置とを備える排ガス浄化用触媒の製造装置が記載されている。また、特許文献２には、触媒層の原料を含んだ流体を前記ノズルからモノリスハニカム基材の一方の端面に吐出させて触媒層を形成し、次いで、異なる触媒層の原料を含んだ流体を前記ノズルからモノリスハニカム基材の他方の端面に吐出させて異なる触媒層を形成することによって、モノリスハニカム基材の上流部と下流部に異なる組成の触媒層が形成された排ガス浄化用触媒が得られることが記載されている。 Further, in International Publication No. 2010/114132 (Patent Document 2), there is provided an exhaust gas purifying catalyst manufacturing apparatus including a nozzle having a plurality of discharge ports and a fluid supply device connected to the nozzle. Have been described. Further, in Patent Document 2, a fluid containing a raw material of a catalyst layer is discharged from the nozzle onto one end face of a monolith honeycomb substrate to form a catalyst layer, and then a fluid containing a raw material of a different catalyst layer is formed. By forming different catalyst layers by discharging from the nozzle to the other end surface of the monolith honeycomb substrate, an exhaust gas purifying catalyst in which catalyst layers having different compositions are formed in the upstream portion and the downstream portion of the monolith honeycomb substrate is obtained. It is described that it is done.
さらに、特開２０１０−１３３３３２号公報（特許文献３）には、１つのハニカム担体に光発熱材のコート層と排ガス浄化用触媒の触媒層を塗り分けることによって、排気上流側又は下流側に光発熱体、下流側又は上流側に排ガス浄化用触媒が配置されている触媒装置が得られることが記載されている。 Further, in Japanese Patent Laid-Open No. 2010-133332 (Patent Document 3), one honeycomb carrier is coated with a coat layer of an optical heating material and a catalyst layer of an exhaust gas purifying catalyst so that light can be emitted upstream or downstream of the exhaust gas. It is described that a heating device and a catalyst device in which an exhaust gas purifying catalyst is arranged on the downstream side or the upstream side can be obtained.
また、特開２０１４−１８８４６６号公報（特許文献４）には、ハニカム構造部の入口セル側の隔壁表面に、微細原料粒子を塗布し、焼成して、複数の細孔を有する表面捕集層を形成し、ハニカム構造部の出口セル側の隔壁表面に、排ガス浄化用触媒を含むスラリーを塗工し、乾燥させて、前記排ガス浄化用触媒を担持させる排ガス浄化フィルターの製造方法が記載されている。 Further, in JP-A-2014-188466 (Patent Document 4), fine raw material particles are applied to the partition wall surface on the inlet cell side of the honeycomb structure portion and baked to form a surface collection layer having a plurality of pores. To form a wall surface of the partition wall on the outlet cell side of the honeycomb structure part, a slurry containing an exhaust gas purifying catalyst is applied and dried, and a method for manufacturing an exhaust gas purifying filter carrying the exhaust gas purifying catalyst is described. There is.
さらに、特開２０１６−２５３４号公報（特許文献５）には、シリンジ先端から、ウォールスルー型のフィルター基体のガス流入通路の封止端側の隔壁表面に粒子状物質酸化触媒の前駆体である触媒スラリーを圧入し、さらに、ガス流入通路の開口端側の隔壁表面にＮＯｘ浄化触媒の前駆体である触媒スラリーを圧入し、その後、乾燥、焼成を施す排ガス浄化用触媒の製造方法が記載されている。 Further, in Japanese Patent Laid-Open No. 2016-2534 (Patent Document 5), a precursor of a particulate matter oxidation catalyst is provided from the tip of a syringe to the surface of a partition wall on the sealing end side of a gas inflow passage of a wall-through type filter substrate. A method for producing an exhaust gas purifying catalyst is described, in which the catalyst slurry is press-fitted, the catalyst slurry that is the precursor of the NOx purification catalyst is further press-fitted onto the partition wall surface on the opening end side of the gas inflow passage, and then the catalyst slurry is dried and calcined. ing.
しかしながら、これらの特許文献に記載の方法は、複数のスラリー材料をハニカム基材のセルの長手方向や半径方向に分布した状態に塗布する方法であり、複数のスラリー材料をセルの内周に沿った方向に分布した状態に塗布することは困難であった。 However, the method described in these patent documents is a method of applying a plurality of slurry materials in a state of being distributed in the longitudinal direction and the radial direction of the cells of the honeycomb substrate, and a plurality of slurry materials are provided along the inner circumference of the cells. It was difficult to apply in a state of being distributed in different directions.
本発明は、上記従来技術の有する課題に鑑みてなされたものであり、複数の材料をハニカム状反応容器のセル内の任意の位置に互いに分離した状態（特に、セルの内周に沿った方向（内周方向）に分布した状態）に塗布することを可能とするセル内塗布装置、及び複数の材料がハニカム状反応容器のセル内の任意の位置に互いに分離した状態（特に、セルの内周方向に分布した状態）に塗布されている反応容器を製造する方法を提供することを目的とする。 The present invention has been made in view of the above problems of the prior art, a state in which a plurality of materials are separated from each other at any position in the cells of the honeycomb-shaped reaction vessel (in particular, the direction along the inner circumference of the cells). In-cell coating device that enables coating in a state (distributed in the inner peripheral direction), and a state in which a plurality of materials are separated from each other at arbitrary positions in the cells of the honeycomb-shaped reaction container (particularly in the cells). It is an object of the present invention to provide a method for producing a reaction container coated in a circumferentially distributed state).
本発明者らは、上記目的を達成すべく鋭意研究を重ねた結果、独立した複数の材料吐出口と前記複数の材料吐出口にそれぞれ独立に連結している複数の材料流路とが形成されている吐出管を用い、この吐出管をハニカム状反応容器のセル内の任意の方向に自在に移動させたり、各セルの長手方向の中心軸に対して相対的に回転させたりすることによって、複数の材料をハニカム状反応容器のセル内の任意の位置に互いに分離した状態（特に、セルの内周方向に分布した状態）に塗布できることを見出し、本発明を完成するに至った。 As a result of intensive studies to achieve the above object, the present inventors have formed a plurality of independent material discharge ports and a plurality of material flow paths that are independently connected to the plurality of material discharge ports. Using a discharge pipe that is, by freely moving this discharge pipe in any direction within the cells of the honeycomb-shaped reaction vessel, or by rotating it relative to the central axis in the longitudinal direction of each cell, The inventors have found that a plurality of materials can be applied to arbitrary positions in cells of a honeycomb reactor in a state of being separated from each other (particularly, a state of being distributed in the inner circumferential direction of cells), and have completed the present invention.
すなわち、本発明のセル内塗布装置は、ハニカム状反応容器の各セル内に複数の材料を塗布するためのセル内塗布装置であって、
独立した複数の材料吐出口と前記複数の材料吐出口にそれぞれ独立に連結している複数の材料流路とが形成されており、前記セル中に挿入可能な吐出管、及び
前記複数の材料流路に前記複数の材料をそれぞれ独立に供給するための複数の材料供給装置
を備えていることを特徴とするものである。
That is, the in-cell coating device of the present invention is an in-cell coating device for coating a plurality of materials in each cell of the honeycomb-shaped reaction container,
A plurality of independent material discharge ports and a plurality of material flow paths that are independently connected to the plurality of material discharge ports are formed, and a discharge pipe that can be inserted into the cell, and the plurality of material flows. A plurality of material supply devices for independently supplying the plurality of materials to the passage are provided.
本発明のセル内塗布装置においては、前記複数の材料吐出口が、前記吐出管の周に沿った方向の異なる位置に配置されていることが好ましい。また、前記吐出管に、気体を吹き付けるための気体吐出口と前記気体吐出口に連結している気体流路とが更に形成されており、かつ、前記気体流路に気体を供給するための気体供給装置を更に備えていることが好ましい。さらに、前記ハニカム状反応容器の、前記吐出管が挿入される側の端面とは反対側の端面から前記セル内を吸引するための吸引装置を更に備えていることが好ましい。 In the in-cell coating device of the present invention, it is preferable that the plurality of material discharge ports are arranged at different positions along the circumference of the discharge pipe. Further, the discharge pipe is further formed with a gas discharge port for spraying gas and a gas flow path connected to the gas discharge port, and a gas for supplying gas to the gas flow path. It is preferable to further include a supply device. Furthermore, it is preferable to further include a suction device for sucking the inside of the cell from the end surface of the honeycomb-shaped reaction container opposite to the end surface on the side where the discharge pipe is inserted.
さらに、本発明のセル内塗布装置において、前記吐出管は前記ハニカム状反応容器の各セルの長手方向の中心軸に対して相対的に回転可能なものであることが好ましく、また、前記複数の材料吐出口が前記吐出管の外周面に形成されていることも好ましい。 Further, in the in-cell coating device of the present invention, it is preferable that the discharge pipe is rotatable relative to a central axis in the longitudinal direction of each cell of the honeycomb-shaped reaction container, and the plurality of It is also preferable that the material discharge port is formed on the outer peripheral surface of the discharge pipe.
本発明の反応容器の製造方法は、前記本発明のセル内塗布装置を用いてハニカム状反応容器の各セル内に複数の材料が塗布された反応容器を製造する方法であって、
前記ハニカム状反応容器のセル中に前記吐出管を挿入する吐出管挿入工程と、
前記複数の材料を、前記複数の材料供給装置からそれぞれ独立に前記複数の材料流路に供給し、前記複数の材料吐出口からそれぞれ独立に吐出させることにより、前記ハニカム状反応容器の各セル内に前記複数の材料を塗布する塗布工程と、
を含むことを特徴とする方法である。
The method for producing a reaction container of the present invention is a method for producing a reaction container in which a plurality of materials are applied in each cell of a honeycomb-shaped reaction container using the in-cell coating device of the present invention,
A discharge pipe inserting step of inserting the discharge pipe into the cells of the honeycomb-shaped reaction container,
In the cells of the honeycomb-shaped reaction container, by supplying the plurality of materials to the plurality of material flow paths independently from the plurality of material supply devices and independently discharging the plurality of material discharge ports, respectively. An applying step of applying the plurality of materials to
The method is characterized by including.
本発明の反応容器の製造方法においては、前記塗布工程において、気体を、前記気体供給装置から前記気体流路に供給し、前記気体吐出口から吹き付けながら、前記複数の材料を塗布することが好ましい。また、前記塗布工程において、前記吸引装置を用いて、前記ハニカム状反応容器の、前記吐出管が挿入される側の端面とは反対側の端面から前記セル内を吸引しながら、前記複数の材料を塗布することも好ましい。さらに、前記塗布工程において、前記吐出管を、前記ハニカム状反応容器の各セルの長手方向の中心軸に対して相対的に回転させながら、前記複数の材料を塗布することも好ましい。 In the method for manufacturing a reaction container of the present invention, in the applying step, it is preferable that a plurality of materials are applied while supplying gas from the gas supply device to the gas flow path and blowing from the gas discharge port. .. Further, in the coating step, using the suction device, while suctioning the inside of the cell from the end surface of the honeycomb-shaped reaction container opposite to the end surface on the side where the discharge pipe is inserted, the plurality of materials It is also preferable to apply. Further, in the coating step, it is also preferable to coat the plurality of materials while rotating the discharge pipe relative to the central axis in the longitudinal direction of each cell of the honeycomb-shaped reaction container.
本発明によれば、複数の材料をハニカム状反応容器のセル内の任意の位置に互いに分離した状態（特に、セルの内周方向に分布した状態）に塗布することが可能となる。 According to the present invention, it is possible to apply a plurality of materials to arbitrary positions in a cell of a honeycomb-shaped reaction container in a state of being separated from each other (particularly, a state of being distributed in the inner peripheral direction of the cell).
以下、図面を参照しながら本発明の好適な実施形態について詳細に説明するが、本発明は前記図面に限定されるものではない。なお、以下の説明及び図面中、同一又は相当する要素には同一の符号を付し、重複する説明は省略する。 Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings, but the present invention is not limited to the drawings. In the following description and drawings, the same or corresponding elements will be denoted by the same reference symbols, without redundant description.
先ず、本発明のセル内塗布装置について説明する。本発明のセル内塗布装置は、ハニカム状反応容器の各セル内に複数の材料を塗布するためのセル内塗布装置であって、前記セル中に挿入可能な吐出管及び前記複数の材料をそれぞれ独立に供給するための複数の材料供給装置を備えるものである。前記吐出管には、独立した複数の材料吐出口と前記複数の材料吐出口にそれぞれ独立に連結している複数の材料流路とが形成されている。また、前記複数の材料流路には、前記複数の材料供給装置がそれぞれ独立に連結されている。 First, the in-cell coating device of the present invention will be described. The in-cell coating device of the present invention is an in-cell coating device for coating a plurality of materials in each cell of a honeycomb-shaped reaction container, and a discharge pipe insertable in the cell and the plurality of materials, respectively. It is provided with a plurality of material feeding devices for feeding independently. The discharge pipe is formed with a plurality of independent material discharge ports and a plurality of material flow paths that are independently connected to the plurality of material discharge ports. Further, the plurality of material supply devices are independently connected to the plurality of material flow paths.
このような本発明のセル内塗布装置を用いて各セル内に複数の材料を塗布することが可能なハニカム状反応容器としては、材料の塗布時に既にハニカム形状になっているもの（一体化されているもの）であれば特に制限はなく、例えば、一体成型された公知のハニカム状反応容器を使用することができる。 As a honeycomb-shaped reaction container capable of coating a plurality of materials in each cell using such an in-cell coating device of the present invention, a honeycomb-shaped reaction vessel that is already in a honeycomb shape at the time of coating the materials (integrated There is no particular limitation as long as it is the same), and for example, a known honeycomb-shaped reaction container integrally molded can be used.
図１は本発明のセル内塗布装置の好適な一実施形態を示す模式縦断面図である。図１に示す本発明のセル内塗布装置は、ハニカム状反応容器１の各セル１ａ内に２種類の材料Ａ及び材料Ｂを塗布するためのものであり、セル１ａ中に挿入可能な吐出管２と、吐出管２に材料Ａ及び材料Ｂをそれぞれ独立に供給するための材料供給装置３Ａ及び材料供給装置３Ｂとを備えている。そして、吐出管２には、独立した材料吐出口５Ａ及び材料吐出口５Ｂと、材料吐出口５Ａに連結している材料流路６Ａと、材料吐出口５Ｂに連結している材料流路６Ｂとが形成されている。さらに、材料流路６Ａには材料供給装置３Ａが、材料流路６Ｂには材料供給装置３Ｂがそれぞれ独立に連結されている。これにより、材料供給装置３Ａから材料流路６Ａに材料Ａを、材料供給装置３Ｂから材料流路６Ｂに材料Ｂをそれぞれ独立に供給し、材料Ａを材料吐出口５Ａから、材料Ｂを材料吐出口５Ｂからそれぞれ独立に吐出させることができ、材料Ａ及び材料Ｂをハニカム状反応容器１のセル１ａ内に混合させずに互いに分離した状態に塗布することが可能となる。 FIG. 1 is a schematic vertical sectional view showing a preferred embodiment of the in-cell coating device of the present invention. The in-cell coating device of the present invention shown in FIG. 1 is for coating two types of materials A and B in each cell 1a of the honeycomb-shaped reaction container 1, and a discharge pipe that can be inserted into the cell 1a. 2 and a material supply device 3A and a material supply device 3B for independently supplying the material A and the material B to the discharge pipe 2. The discharge pipe 2 has independent material discharge ports 5A and 5B, a material flow channel 6A connected to the material discharge port 5A, and a material flow channel 6B connected to the material discharge port 5B. Are formed. Further, the material supply device 3A is connected to the material flow path 6A, and the material supply device 3B is connected to the material flow path 6B, respectively. Thereby, the material A is independently supplied from the material supply device 3A to the material flow path 6A, the material B is supplied from the material supply device 3B to the material flow path 6B, and the material A is discharged from the material discharge port 5A. It is possible to discharge each independently from the outlet 5B, and it is possible to apply the material A and the material B to the cells 1a of the honeycomb reaction container 1 in a separated state without mixing them.
また、本発明のセル内塗布装置においては、独立した３つ以上の材料吐出口と各材料吐出口にそれぞれ独立に連結されている３つ以上の材料流路とが形成されている吐出管、及び、各材料流路にそれぞれ独立に連結されている３つ以上の材料供給装置を用いることもできる。これにより、３種類以上の材料を、混合させずに分離した状態で、ハニカム状反応容器の各セル内に塗布することが可能となる。 In addition, in the in-cell coating device of the present invention, a discharge pipe in which three or more independent material discharge ports and three or more material flow paths independently connected to each material discharge port are formed, Also, it is possible to use three or more material supply devices that are independently connected to each material flow path. As a result, three or more kinds of materials can be applied in each cell of the honeycomb reaction container in a separated state without being mixed.
本発明のセル内塗布装置においては、吐出管２を、ハニカム状反応容器１の端面９上の任意の方向に自在に移動させることが可能であるため、ハニカム状反応容器１の任意のセル１ａ内に材料を塗布することができる。また、吐出管２を、セル１ａの長手方向及び短手方向（又は半径方向）に移動させることが可能である。さらに、吐出管２をハニカム状反応容器１の各セル１ａの長手方向の中心軸に対して相対的に回転させることも可能である。例えば、ハニカム状反応容器１を回転させずに吐出管２を回転（又は吐出管２に取り付けた回転軸４を回転）させたり、或いは、吐出管２を回転させずにハニカム状反応容器１を回転させたりすること等によって、吐出管２を相対的に回転させることができる。本発明のセル内塗布装置においては、吐出管をセル内の任意の方向に自在に移動させたり、各セルの長手方向の中心軸に対して相対的に回転させたりすることが可能であるため、複数の材料をセル内の任意の位置に互いに分離した状態に塗布することができる。特に、吐出管をセルの長手方向に移動させながら複数の材料を塗布することによって、セルの内周に沿った方向（内周方向）に複数の材料層が分布している反応容器を製造することが可能となる。また、吐出管をセル内でセルの長手方向の中心軸に対して相対的に回転かつセルの長手方向に移動させながら複数の材料を吐出させることによって、複数の材料をセル内に螺旋状に塗布するができ、内壁が滑らかな流路（セル）を有する、圧力損失が少ない反応容器を製造することが可能となる。 In the in-cell coating device of the present invention, since the discharge pipe 2 can be freely moved in any direction on the end surface 9 of the honeycomb reaction container 1, any cell 1a of the honeycomb reaction container 1 can be moved. The material can be applied within. Further, the discharge pipe 2 can be moved in the longitudinal direction and the lateral direction (or the radial direction) of the cell 1a. Furthermore, it is possible to rotate the discharge pipe 2 relative to the central axis in the longitudinal direction of each cell 1a of the honeycomb reaction container 1. For example, the discharge pipe 2 may be rotated (or the rotating shaft 4 attached to the discharge pipe 2 may be rotated) without rotating the honeycomb reaction container 1, or the honeycomb reaction container 1 may be rotated without rotating the discharge pipe 2. The discharge pipe 2 can be relatively rotated by rotating or the like. In the in-cell coating device of the present invention, it is possible to freely move the discharge pipe in any direction within the cell, or to rotate it relative to the central axis in the longitudinal direction of each cell. , A plurality of materials can be applied to arbitrary positions in a cell in a state of being separated from each other. In particular, by applying a plurality of materials while moving the discharge pipe in the longitudinal direction of the cell, a reaction container in which a plurality of material layers are distributed in a direction along the inner circumference of the cell (inner circumference direction) is manufactured. It becomes possible. Further, by discharging the plural materials while rotating the discharge pipe in the cell relative to the central axis of the longitudinal direction of the cell and moving in the longitudinal direction of the cell, the plural materials are spirally formed in the cell. It becomes possible to manufacture a reaction vessel which can be applied and has a flow path (cell) whose inner wall is smooth and which has a small pressure loss.
本発明に用いられる吐出管の外径（吐出管の横断面が円状でない場合には、外接円の直径）としては、セル内に挿入可能な大きさであれば特に制限はないが、セルの内径（セルの横断面が円状でない場合には、内接円の直径）の９０％以下であることが好ましい。 The outer diameter of the discharge pipe used in the present invention (the diameter of the circumscribing circle when the cross section of the discharge pipe is not circular) is not particularly limited as long as it is a size that can be inserted into the cell. 90% or less of the inner diameter (the diameter of the inscribed circle when the cross section of the cell is not circular).
また、本発明に用いられる吐出管においては、複数の材料吐出口が吐出管の周に沿った方向（周方向）の異なる位置に配置されていることが好ましい。図２は、このような吐出管の例を示す模式横断面図である。図２（Ａ）は、２つの材料吐出口が吐出管の周方向の異なる位置に配置されている吐出管の模式横断面図であり、材料流路６Ａと材料流路６Ｂが吐出管２の周方向の異なる位置に配置されている。図２（Ｂ）は、３つの材料吐出口が吐出管の周方向の異なる位置に配置されている吐出管の模式横断面図であり、材料流路６Ａと材料流路６Ｂと材料流路６Ｃが吐出管２の周方向の異なる位置に配置されている。図２（Ｃ）は、４つの材料吐出口が吐出管の周方向の異なる位置に配置されている吐出管の模式横断面図であり、材料流路６Ａと材料流路６Ｂと材料流路６Ｃと材料流路６Ｄが吐出管２の周方向の異なる位置に配置されている。このように、複数の材料吐出口及び複数の材料流路が吐出管の周方向の異なる位置に配置されている吐出管を用いることによって、複数の材料をセル内に互いに分離した状態に塗布することが可能となる。なお、前記材料流路を形成する複数の配管は、図２（Ａ）に示すように、溶接等（図示なし）により束ねられていてもよいし、図２（Ｂ）及び（Ｃ）に示すように、外筒管７内に収容されていてもよい。 Further, in the discharge pipe used in the present invention, it is preferable that the plurality of material discharge ports are arranged at different positions in the direction (circumferential direction) along the circumference of the discharge pipe. FIG. 2 is a schematic cross-sectional view showing an example of such a discharge pipe. FIG. 2A is a schematic cross-sectional view of a discharge pipe in which two material discharge ports are arranged at different positions in the circumferential direction of the discharge pipe, and the material flow passage 6A and the material flow passage 6B correspond to the discharge pipe 2. They are arranged at different positions in the circumferential direction. FIG. 2B is a schematic cross-sectional view of a discharge pipe in which three material discharge ports are arranged at different positions in the circumferential direction of the discharge pipe, and the material flow passage 6A, the material flow passage 6B, and the material flow passage 6C. Are arranged at different positions in the circumferential direction of the discharge pipe 2. FIG. 2C is a schematic cross-sectional view of a discharge pipe in which four material discharge ports are arranged at different positions in the circumferential direction of the discharge pipe, and the material flow passage 6A, the material flow passage 6B, and the material flow passage 6C. The material flow paths 6D are arranged at different positions in the circumferential direction of the discharge pipe 2. As described above, by using the discharge pipe in which the plurality of material discharge ports and the plurality of material flow paths are arranged at different positions in the circumferential direction of the discharge pipe, the plurality of materials are applied to the cells in a state of being separated from each other. It becomes possible. It should be noted that the plurality of pipes forming the material flow path may be bundled by welding or the like (not shown) as shown in FIG. 2(A), or as shown in FIGS. 2(B) and (C). Thus, it may be housed in the outer tube 7.
また、本発明に用いられる吐出管においては、複数の材料吐出口が吐出管の外周面に形成されていることが好ましい。これにより、複数の材料を混合させずに互いに分離した状態で塗布することが可能となる。 Further, in the discharge pipe used in the present invention, it is preferable that a plurality of material discharge ports are formed on the outer peripheral surface of the discharge pipe. This makes it possible to apply a plurality of materials in a state where they are separated from each other without being mixed.
さらに、本発明に用いられる吐出管においては、気体を吹き付けるための気体吐出口と前記気体吐出口に連結している気体流路とが更に形成されていることが好ましく、前記気体流路には、気体を供給するための気体供給装置が連結されていることが好ましい。空気等の気体を吹き付けながら材料を塗布することによって、材料をセルの内壁に確実に密着させることができ、さらに、余分な材料が除去されてセルの内壁が平滑となり、圧力損失が少なく、内壁が滑らかな流路（セル）を有する反応容器を製造することが可能となる。図３は、このような気体吐出口と気体流路とが形成されている吐出管の模式横断面図を示す。図３（Ａ）は、２つの材料吐出口と２つの気体吐出口とが吐出管の周方向の異なる位置に配置されている吐出管の模式横断面図であり、材料流路６Ａと材料流路６Ｂと２つの気体流路８とが吐出管２の周方向の異なる位置に配置されている。図３（Ｂ）は、３つの材料吐出口と３つの気体吐出口とが吐出管の周方向の異なる位置に配置されている吐出管の模式横断面図であり、材料流路６Ａと材料流路６Ｂと材料流路６Ｃと３つの気体流路８とが吐出管２の周方向の異なる位置に配置されている。図３（Ｃ）は、４つの材料吐出口と１つの気体吐出口とが吐出管の周方向の異なる位置に配置されている吐出管の模式横断面図であり、材料流路６Ａと材料流路６Ｂと材料流路６Ｃと材料流路６Ｄと１つの気体流路８とが吐出管２の周方向の異なる位置に配置されている。 Further, in the discharge pipe used in the present invention, it is preferable that a gas discharge port for spraying a gas and a gas flow path connected to the gas discharge port are further formed, and the gas flow path is formed. It is preferable that a gas supply device for supplying gas is connected. By applying the material while spraying a gas such as air, the material can be firmly adhered to the inner wall of the cell, and the excess material is removed to make the inner wall of the cell smooth, reducing the pressure loss and reducing the inner wall. It becomes possible to manufacture a reaction container having a smooth flow path (cell). FIG. 3 shows a schematic cross-sectional view of a discharge pipe in which such a gas discharge port and a gas flow path are formed. FIG. 3A is a schematic cross-sectional view of a discharge pipe in which two material discharge ports and two gas discharge ports are arranged at different positions in the circumferential direction of the discharge pipe. The passage 6B and the two gas passages 8 are arranged at different positions in the circumferential direction of the discharge pipe 2. FIG. 3(B) is a schematic cross-sectional view of a discharge pipe in which three material discharge ports and three gas discharge ports are arranged at different positions in the circumferential direction of the discharge pipe. The passage 6B, the material passage 6C, and the three gas passages 8 are arranged at different positions in the circumferential direction of the discharge pipe 2. FIG. 3C is a schematic cross-sectional view of a discharge pipe in which four material discharge ports and one gas discharge port are arranged at different positions in the circumferential direction of the discharge pipe. The passage 6B, the material passage 6C, the material passage 6D and one gas passage 8 are arranged at different positions in the circumferential direction of the discharge pipe 2.
また、図１に示す本発明のセル内塗布装置においては、ハニカム状反応容器１の、吐出管２が挿入される側の端面９とは反対側の端面１０からセル１ａ内を吸引するための吸引装置（図示なし）を更に備えていることが好ましい。セル１ａ内を吸引することによって、余分な材料が除去されてセルの内壁が平滑となり、圧力損失が少なく、内壁が滑らかな流路（セル）を有する反応容器を製造することが可能となる。 Further, in the in-cell coating apparatus of the present invention shown in FIG. 1, for sucking the inside of the cell 1a from the end surface 10 of the honeycomb-shaped reaction container 1 opposite to the end surface 9 on the side where the discharge pipe 2 is inserted. It is preferable to further include a suction device (not shown). By suctioning the inside of the cell 1a, the excess material is removed, the inner wall of the cell becomes smooth, the pressure loss is small, and it becomes possible to manufacture a reaction vessel having a flow passage (cell) with a smooth inner wall.
さらに、本発明のセル内塗布装置においては、超音波処理装置を備えていることが好ましい。これにより、材料吐出口を超音波洗浄することが可能となり、材料吐出口付近での材料（特に、スラリー状材料）の詰まりを防止することができる。 Furthermore, the in-cell coating device of the present invention preferably includes an ultrasonic treatment device. This makes it possible to ultrasonically clean the material discharge port and prevent clogging of the material (particularly, slurry-like material) near the material discharge port.
以上、本発明のセル内塗布装置の好適な実施形態について説明したが、本発明のセル内塗布装置は上記実施形態に限定されるものではない。例えば、上記実施形態においては、セル内に挿入される吐出管は１本であるが、複数の吐出管を備えていてもよい。これにより、複数の吐出管を複数のセル内に同時に挿入して複数のセル内で同時に塗布することが可能となり、塗布時間の短縮を図ることができる。また、材料（特に、スラリー状材料）の詰まりや沈降を防止することができ、塗布不良による歩留まりの低下を抑制することができる。 Although the preferred embodiment of the in-cell coating device of the present invention has been described above, the in-cell coating device of the present invention is not limited to the above embodiment. For example, in the above embodiment, the number of discharge pipes inserted into the cell is one, but a plurality of discharge pipes may be provided. This makes it possible to insert a plurality of discharge pipes into a plurality of cells at the same time and simultaneously apply the plurality of cells to a plurality of cells, thereby shortening the application time. In addition, it is possible to prevent clogging and sedimentation of the material (particularly, the slurry-like material), and it is possible to suppress a decrease in yield due to coating failure.
次に、本発明の反応容器の製造方法について説明する。本発明の反応容器の製造方法は、前記本発明のセル内塗布装置を用いて、ハニカム状反応容器の各セル内に複数の材料が塗布された反応容器を製造する方法であって、前記ハニカム状反応容器のセル中に前記吐出管を挿入する吐出管挿入工程と、前記複数の材料を、前記複数の材料供給装置からそれぞれ独立に前記複数の材料流路に供給し、前記複数の材料吐出口からそれぞれ独立に吐出させることにより、前記ハニカム状反応容器の各セル内に前記複数の材料を塗布する塗布工程と、を含む方法である。 Next, a method for manufacturing the reaction container of the present invention will be described. The method for producing a reaction container of the present invention is a method for producing a reaction container in which a plurality of materials are applied in each cell of a honeycomb-shaped reaction container using the in-cell coating device of the present invention, wherein the honeycomb Discharge tube insertion step of inserting the discharge pipe into the cell of the reaction vessel, and the plurality of materials are independently supplied from the plurality of material supply devices to the plurality of material flow paths to discharge the plurality of material discharge paths. A coating step of coating the plurality of materials in each cell of the honeycomb-shaped reaction container by independently discharging from the outlet.
本発明に用いられるハニカム状反応容器としては、材料の塗布時に既にハニカム形状になっているもの（一体化されているもの）であれば特に制限はなく、例えば、一体成型された公知のハニカム状反応容器を使用することができる。 The honeycomb-shaped reaction vessel used in the present invention is not particularly limited as long as it is already in a honeycomb shape at the time of applying the material (integrated), for example, a known honeycomb shape integrally molded. A reaction vessel can be used.
また、本発明に用いられる、ハニカム状反応容器のセル内に塗布される材料としては、前記本発明のセル内塗布装置を用いてハニカム状反応容器のセル内に塗布できるものであれば特に制限はなく、液状のものであってもスラリー状のものであってもよいが、材料供給装置や材料流路、材料吐出口において、材料（特に、スラリー状材料）の目詰まりや沈降が起こらないように、材料の粘度や粒度・固形分の割合等を適宜調整する必要がある。 Further, the material used in the cells of the honeycomb reaction container used in the present invention is not particularly limited as long as it can be applied in the cells of the honeycomb reaction container using the in-cell coating device of the present invention. The material may be liquid or slurry, but the material supply device, the material flow path, and the material discharge port do not cause clogging or sedimentation of the material (particularly, the slurry material). As described above, it is necessary to appropriately adjust the viscosity of the material, the particle size, the ratio of the solid content, and the like.
図１に示すセル内塗布装置を用いた本発明の反応容器の製造方法においては、先ず、吐出管２をハニカム状反応容器１の端面９から挿入し、吐出管２の先端部をハニカム状反応容器の端面１０まで到達させる（吐出管挿入工程）。次に、材料Ａを材料供給装置３Ａから材料流路６Ａに、材料Ｂを材料供給装置３Ｂから材料流路６Ｂにそれぞれ独立に供給し、材料Ａを材料吐出口５Ａから、材料Ｂを材料吐出口５Ｂからそれぞれ独立に吐出させて、材料Ａ及び材料Ｂをハニカム状反応容器１のセル１ａ内に混合させずに互いに分離した状態に塗布し、ハニカム状反応容器１の隔壁１ｂに材料Ａからなる層（材料Ａ層）１０１Ａ及び材料Ｂからなる層（材料Ｂ層）１０１Ｂを互いに分離した状態で形成する（塗布工程）。このとき、吐出管２の動きを制御することによって、様々な構造の材料層を形成することができる。 In the method for manufacturing a reaction container of the present invention using the in-cell coating device shown in FIG. 1, first, the discharge pipe 2 is inserted from the end face 9 of the honeycomb-shaped reaction container 1, and the tip portion of the discharge pipe 2 is subjected to the honeycomb-shaped reaction. The end surface 10 of the container is reached (discharge pipe insertion step). Next, the material A is independently supplied from the material supply device 3A to the material flow path 6A, the material B is independently supplied from the material supply device 3B to the material flow path 6B, and the material A is discharged from the material discharge port 5A and the material B is discharged. The materials A and B are separately discharged from the outlets 5B and applied in a state where they are separated from each other without being mixed in the cells 1a of the honeycomb reaction container 1, and the material A and the material B are applied to the partition walls 1b of the honeycomb reaction container 1 from the material A. The layer (material A layer) 101A and the layer (material B layer) 101B made of the material B are formed in a state of being separated from each other (application step). At this time, material layers having various structures can be formed by controlling the movement of the discharge pipe 2.
例えば、ハニカム状反応容器１及び吐出管２を回転させずに、図２（Ａ）や図３（Ａ）に示す吐出管２をセル１ａの長手方向に沿ってハニカム状反応容器１の端面１０から端面９まで移動させながら、材料Ａと材料Ｂとを塗布することによって、ハニカム状反応容器１の隔壁１ｂに、セル１ａの長手方向には組成が均一であり、内周方向には図４Ａ及び図４Ｂに示すように分布している材料Ａからなる層（材料Ａ層）１０１Ａと材料Ｂからなる層（材料Ｂ層）１０１Ｂとを形成することができる。また、ハニカム状反応容器１及び吐出管２を回転させずに、図２（Ａ）や図３（Ａ）に示す吐出管２をセル１ａの長手方向に沿って移動させながら、材料Ａと材料Ｂとを塗布した後、ハニカム状反応容器１又は吐出管２を回転させること等によって吐出管２を各セル１ａの長手方向の中心軸に対して相対的に回転させ、再び、ハニカム状反応容器１及び吐出管２を回転させずに、吐出管２をセル１ａの長手方向に沿って移動させながら、材料Ａと材料Ｂとを塗布し、これらの操作を繰り返すことによって、ハニカム状反応容器１の隔壁１ｂに、セル１ａの長手方向には組成が均一であり、内周方向には図４Ｃに示すように分布している材料Ａからなる層（材料Ａ層）１０１Ａと材料Ｂからなる層（材料Ｂ層）１０１Ｂとを形成することもできる。なお、図４Ａ〜図４Ｃは、本発明の製造方法によって得られる反応容器の例を示す模式横断面図である。 For example, without rotating the honeycomb-shaped reaction container 1 and the discharge pipe 2, the discharge pipe 2 shown in FIG. 2(A) and FIG. 3(A) is attached to the end face 10 of the honeycomb-shaped reaction container 1 along the longitudinal direction of the cell 1a. The material A and the material B are applied to the partition walls 1b of the honeycomb reaction vessel 1 while moving from the end surface 9 to the end surface 9 so that the composition is uniform in the longitudinal direction of the cells 1a and the inner peripheral direction of FIG. Further, as shown in FIG. 4B, it is possible to form a layer (material A layer) 101A composed of the material A and a layer (material B layer) 101B composed of the material B which are distributed. Further, the material A and the material A are moved while moving the discharge pipe 2 shown in FIG. 2A and FIG. 3A along the longitudinal direction of the cell 1a without rotating the honeycomb reaction container 1 and the discharge pipe 2. After applying B, the discharge tube 2 is rotated relative to the central axis of each cell 1a in the longitudinal direction by rotating the honeycomb reaction vessel 1 or the discharge tube 2, and the honeycomb reaction vessel is again formed. The material A and the material B are applied while the discharge pipe 2 is moved along the longitudinal direction of the cell 1a without rotating the discharge pipe 1 and the discharge pipe 2, and by repeating these operations, the honeycomb reaction container 1 In the partition wall 1b, a layer composed of the material A (material A layer) 101A and a material B having a uniform composition in the longitudinal direction of the cell 1a and distributed in the inner peripheral direction as shown in FIG. 4C. (Material B layer) 101B can also be formed. 4A to 4C are schematic cross-sectional views showing examples of reaction vessels obtained by the production method of the present invention.
また、図２（Ａ）や図３（Ａ）に示す吐出管２を、ハニカム状反応容器１の各セル１ａの長手方向の中心軸に対して相対的に回転させ、かつ、セル１ａの長手方向に沿ってハニカム状反応容器１の端面１０から端面９まで移動させながら、材料Ａと材料Ｂとを塗布することによって、図５に示すように、ハニカム状反応容器１の隔壁１ｂに螺旋状に配置されている材料Ａからなる層（材料Ａ層）１０１Ａと材料Ｂからなる層（材料Ｂ層）１０１Ｂとを形成することができる。吐出管２を相対的に回転させる方法としては、ハニカム状反応容器１を回転させずに吐出管２を回転（又は吐出管２に取り付けた回転軸４を回転）させる方法や、吐出管２を回転させずにハニカム状反応容器１を回転させる方法等が挙げられる。なお、図５は、本発明の製造方法によって得られる反応容器の例を示す模式縦断面図である。 In addition, the discharge pipe 2 shown in FIGS. 2A and 3A is rotated relative to the central axis in the longitudinal direction of each cell 1a of the honeycomb-shaped reaction container 1, and the length of the cell 1a is longer. By coating the material A and the material B while moving from the end surface 10 to the end surface 9 of the honeycomb reaction container 1 along the direction, as shown in FIG. 5, the partition walls 1b of the honeycomb reaction container 1 are spirally formed. It is possible to form a layer made of the material A (material A layer) 101A and a layer made of the material B (material B layer) 101B, which are arranged in As a method of relatively rotating the discharge pipe 2, a method of rotating the discharge pipe 2 without rotating the honeycomb reaction container 1 (or rotating a rotary shaft 4 attached to the discharge pipe 2), or a method of rotating the discharge pipe 2 Examples thereof include a method of rotating the honeycomb reaction container 1 without rotating it. Note that FIG. 5 is a schematic vertical cross-sectional view showing an example of a reaction container obtained by the production method of the present invention.
さらに、ハニカム状反応容器１及び吐出管２を回転させずに、図２（Ｂ）や図３（Ｂ）に示す吐出管２をセル１ａの長手方向に沿ってハニカム状反応容器１の端面１０から端面９まで移動させながら、材料Ａと材料Ｂと材料Ｃとを塗布することによって、ハニカム状反応容器１の隔壁１ｂに、セル１ａの長手方向には組成が均一であり、内周方向には図６に示すように分布している材料Ａからなる層（材料Ａ層）１０１Ａと材料Ｂからなる層（材料Ｂ層）１０１Ｂと材料Ｃからなる層（材料Ｃ層）１０１Ｃとを形成することができる。なお、図６は、本発明の製造方法によって得られる反応容器の例を示す模式横断面図である。 Furthermore, without rotating the honeycomb reaction container 1 and the discharge tube 2, the discharge tube 2 shown in FIG. 2B or FIG. 3B is connected to the end face 10 of the honeycomb reaction container 1 along the longitudinal direction of the cell 1a. By applying the material A, the material B, and the material C while moving from the end surface 9 to the end surface 9, the partition walls 1b of the honeycomb-shaped reaction container 1 have a uniform composition in the longitudinal direction of the cells 1a and an inner peripheral direction. Forms a layer (material A layer) 101A composed of the material A, a layer (material B layer) 101B composed of the material B, and a layer (material C layer) 101C composed of the material C, which are distributed as shown in FIG. be able to. 6 is a schematic cross-sectional view showing an example of a reaction container obtained by the manufacturing method of the present invention.
また、ハニカム状反応容器１及び吐出管２を回転させずに、図２（Ｃ）や図３（Ｃ）に示す吐出管２をセル１ａの長手方向に沿ってハニカム状反応容器１の端面１０から端面９まで移動させながら、材料Ａと材料Ｂと材料Ｃと材料Ｄとを塗布することによって、ハニカム状反応容器１の隔壁１ｂに、セル１ａの長手方向には組成が均一であり、内周方向には図７に示すように分布している材料Ａからなる層（材料Ａ層）１０１Ａと材料Ｂからなる層（材料Ｂ層）１０１Ｂと材料Ｃからなる層（材料Ｃ層）１０１Ｃと材料Ｄからなる層（材料Ｄ層）１０１Ｄとを形成することができる。なお、図７は、本発明の製造方法によって得られる反応容器の例を示す模式横断面図である。 Further, without rotating the honeycomb reaction container 1 and the discharge pipe 2, the discharge pipe 2 shown in FIG. 2(C) or FIG. 3(C) is attached to the end face 10 of the honeycomb reaction container 1 along the longitudinal direction of the cell 1a. By applying the material A, the material B, the material C, and the material D while moving from the end surface 9 to the end surface 9, the partition walls 1b of the honeycomb reaction container 1 have a uniform composition in the longitudinal direction of the cells 1a, In the circumferential direction, as shown in FIG. 7, a layer made of the material A (material A layer) 101A, a layer made of the material B (material B layer) 101B, and a layer made of the material C (material C layer) 101C are provided. A layer made of the material D (material D layer) 101D can be formed. FIG. 7 is a schematic cross-sectional view showing an example of a reaction container obtained by the manufacturing method of the present invention.
本発明にかかる塗布工程において、各材料は、材料供給装置から材料流路に、一定の流量で連続的に供給してもよいし、流量を変動させながら供給してもよいし、間欠的に供給してもよい。一定の流量で連続的に供給することによって均一な厚さの材料層を形成することができる。また、流量を変動させながら供給したり、間欠的に供給したりすることによって、材料層の厚さに分布を持たせることが可能となる。材料層の厚さに分布がある反応容器においては、反応基質ガス等の流体がセル内を乱流で流通するため、セル内での流体の混合効率が向上する。 In the coating step according to the present invention, each material may be continuously supplied from the material supply device to the material flow path at a constant flow rate, or may be supplied while varying the flow rate, or intermittently. May be supplied. A material layer having a uniform thickness can be formed by continuously supplying the material layer at a constant flow rate. Further, by supplying while changing the flow rate or by supplying intermittently, it becomes possible to give a distribution to the thickness of the material layer. In a reaction container in which the material layer has a thickness distribution, a fluid such as a reaction substrate gas flows in a turbulent flow in the cell, so that the mixing efficiency of the fluid in the cell is improved.
本発明にかかる塗布工程においては、空気等の気体を、気体供給装置から気体流路に供給し、気体吐出口から吹き付けながら、材料を塗布することが好ましい。これにより、材料をセルの内壁に確実に密着させることができ、さらに、余分な材料が除去されてセルの内壁が平滑となり、圧力損失が少なく、内壁が滑らかな流路（セル）を有する反応容器を製造することが可能となる。 In the coating step according to the present invention, it is preferable that a gas such as air is supplied to the gas flow path from the gas supply device and the material is applied while being sprayed from the gas discharge port. As a result, the material can be surely brought into close contact with the inner wall of the cell, and the excess material is removed so that the inner wall of the cell becomes smooth, the pressure loss is small, and the reaction has a smooth inner wall flow passage (cell). It becomes possible to manufacture a container.
また、本発明にかかる塗布工程においては、吸引装置を用いてハニカム状反応容器１の端面１０からセル１ａ内を吸引しながら、材料を塗布することが好ましい。これにより、余分な材料が除去されてセルの内壁が平滑となり、圧力損失が少なく、内壁が滑らかな流路（セル）を有する反応容器を製造することが可能となる。 Further, in the coating step according to the present invention, it is preferable to coat the material while sucking the inside of the cell 1a from the end face 10 of the honeycomb-shaped reaction container 1 using a suction device. As a result, the excess material is removed, the inner wall of the cell becomes smooth, the pressure loss is small, and it becomes possible to manufacture a reaction vessel having a flow passage (cell) with a smooth inner wall.
以上、本発明の反応容器の製造方法の好適な実施形態について説明したが、本発明の反応容器の製造方法は上記実施形態に限定されるものではない。例えば、上記実施形態においては、１本の吐出管を１つのセル内に挿入して複数の材料を塗布しているが、複数の吐出管を複数のセル内に同時に挿入して複数のセル内で同時に塗布してもよい。これにより、塗布時間の短縮を図ることができる。また、材料（特に、スラリー状材料）の詰まりや沈降を防止することができ、塗布不良による歩留まりの低下を抑制することができる。 Although the preferred embodiment of the method for producing a reaction container of the present invention has been described above, the method for producing a reaction container of the present invention is not limited to the above embodiment. For example, in the above embodiment, one discharge pipe is inserted into one cell and a plurality of materials are applied, but a plurality of discharge pipes are simultaneously inserted into a plurality of cells and a plurality of cells are applied. May be applied simultaneously. Thereby, the application time can be shortened. In addition, it is possible to prevent clogging and sedimentation of the material (particularly, the slurry-like material), and it is possible to suppress a decrease in yield due to coating failure.
以下、実施例及び比較例に基づいて本発明をより具体的に説明するが、本発明は以下の実施例に限定されるものではない。 Hereinafter, the present invention will be described more specifically based on Examples and Comparative Examples, but the present invention is not limited to the following Examples.
（実施例１）
図１に示すセル内塗布装置を用いて、一体成型されたハニカム状反応容器（断面積：６ｃｍ２、長さ：５０ｍｍ、セル形状：６角セル、セル径（内接円の直径）：１．２６ｍｍ）のセル内に２種類のスラリー材料を塗布した。スラリー材料としては、スラリー材料Ａ（固体成分：セリアとジルコニアとを主成分とする複合酸化物、固形分：３０質量％、粘度：３００Ｐａ・ｓ以下）及びスラリー材料Ｂ（固体成分：Ｌａ−Ｆｅ−Ｚｒを主成分とする複合酸化物、固形分：３０質量％、粘度：３００Ｐａ・ｓ以下）を調製した。吐出管２としては、２本のステンレスパイプ（外径：０．５１ｍｍ、内径：０．３９ｍｍ）を束ねたものを使用した。この吐出管は、図２（Ａ）に示す横断面を有するものであり、その外径（外接円の直径）は１．０５ｍｍ以下であった。
(Example 1)
Using the in-cell coating device shown in FIG. 1, a honeycomb-shaped reaction container integrally molded (cross-sectional area: 6 cm 2 , length: 50 mm, cell shape: hexagonal cell, cell diameter (diameter of inscribed circle): 1 Two kinds of slurry materials were applied in a (.26 mm) cell. As the slurry material, slurry material A (solid component: complex oxide containing ceria and zirconia as main components, solid content: 30 mass%, viscosity: 300 Pa·s or less) and slurry material B (solid component: La-Fe) A composite oxide containing -Zr as a main component, solid content: 30 mass%, viscosity: 300 Pa·s or less) was prepared. As the discharge pipe 2, a bundle of two stainless pipes (outer diameter: 0.51 mm, inner diameter: 0.39 mm) was used. This discharge pipe had a cross section shown in FIG. 2(A), and its outer diameter (diameter of the circumscribing circle) was 1.05 mm or less.
先ず、図１に示すセル内塗布装置において、吐出管２をハニカム状反応容器１の端面９から挿入し、吐出管２の先端部をハニカム状反応容器１の端面１０まで到達させた。次に、ハニカム状反応容器１及び吐出管２を回転させずに、吐出管２をセル１ａの長手方向に沿って４ｍｍ／秒の速さで端面１０から端面９の方向に移動させながら、前記スラリー材料Ａを材料供給装置３Ａから材料流路６Ａに約１ｍｇ／秒の流量で、前記スラリー材料Ｂを材料供給装置３Ｂから材料流路６Ｂに約１ｍｇ／秒の流量で、それぞれ独立に連続的に供給し、前記スラリー材料Ａを材料吐出口５Ａから、前記スラリー材料Ｂを材料吐出口５Ｂからそれぞれ独立に吐出させた。これにより、ハニカム状反応容器１の隔壁１ｂに、前記スラリー材料Ａと前記スラリー材料Ｂとが塗布された反応容器が得られた。 First, in the in-cell coating device shown in FIG. 1, the discharge pipe 2 was inserted from the end surface 9 of the honeycomb reaction container 1, and the tip of the discharge pipe 2 reached the end surface 10 of the honeycomb reaction container 1. Next, while moving the discharge tube 2 along the longitudinal direction of the cell 1a at a speed of 4 mm/sec from the end face 10 to the end face 9 without rotating the honeycomb reaction container 1 and the discharge pipe 2, Slurry material A from the material supply device 3A to the material flow passage 6A at a flow rate of about 1 mg/sec, and the slurry material B from the material supply device 3B to the material flow passage 6B at a flow rate of about 1 mg/sec. And the slurry material A was independently discharged from the material discharge port 5A, and the slurry material B was separately discharged from the material discharge port 5B. As a result, a reaction container was obtained in which the partition wall 1b of the honeycomb-shaped reaction container 1 was coated with the slurry material A and the slurry material B.
このようにして得られた反応容器のセル内の状態を光学顕微鏡により観察した。その結果を図８に示す。図８に示したように、ハニカム状反応容器の隔壁（セルの内壁）には、セルの長手方向には組成が均一であり、内周方向には分布している材料Ａからなる層（材料Ａ層）と材料Ｂからなる層（材料Ｂ層）とが形成されていることが確認された。 The inside of the cell of the reaction container thus obtained was observed with an optical microscope. The result is shown in FIG. As shown in FIG. 8, on the partition walls (inner walls of the cells) of the honeycomb-shaped reaction vessel, a layer (material (material) having a uniform composition in the longitudinal direction of the cells and distributed in the inner circumferential direction) It was confirmed that a layer A) and a layer made of the material B (material B layer) were formed.
以上説明したように、本発明のセル内塗布装置によれば、複数の材料をハニカム状反応容器のセル内の任意の位置に互いに分離した状態（特に、セルの内周方向に分布した状態）に塗布することが可能となる。 As described above, according to the in-cell coating device of the present invention, a plurality of materials are separated from each other at arbitrary positions in the cells of the honeycomb reaction container (particularly, a state in which they are distributed in the inner circumferential direction of the cells). Can be applied to.
したがって、本発明の反応容器の製造方法は、このような本発明のセル内塗布装置を用いているため、例えば、近接して共存すると反応容器の性能（例えば、耐久性）が向上するが、混合された状態になると反応容器の性能（例えば、耐久性）が低下するといった、共存状態によって相反する特性が発現する複数の材料がハニカム状反応容器のセル内の任意の位置に互いに分離した状態（特に、セルの内周方向に分布した状態）に塗布されている反応容器等を製造する方法として有用である。 Therefore, the method for producing a reaction container of the present invention uses such an in-cell coating device of the present invention, and therefore, when coexisting in close proximity, the performance (for example, durability) of the reaction container is improved, A state in which multiple materials exhibiting contradictory properties depending on the coexistence state, such as the performance (for example, durability) of the reaction vessel decreasing when mixed, are separated from each other at any position in the cells of the honeycomb reaction vessel. It is useful as a method for producing a reaction vessel or the like coated (particularly in a state of being distributed in the inner peripheral direction of the cell).
１：ハニカム状反応容器、１ａ：ハニカム状反応容器１のセル、１ｂ：ハニカム状反応容器１の隔壁、２：吐出管、３Ａ，３Ｂ：材料供給装置、４：回転軸、５Ａ，５Ｂ：材料吐出口、６Ａ，６Ｂ，６Ｃ，６Ｄ：材料流路、７：外筒管、８：気体流路、９：ハニカム状反応容器１の、吐出管２が挿入される側の端面、１０：ハニカム状反応容器１の端面９とは反対側の端面、１０１Ａ：材料Ａからなる層（材料Ａ層）、１０１Ｂ：材料Ｂからなる層（材料Ｂ層）、１０１Ｃ：材料Ｃからなる層（材料Ｃ層）、１０１Ｃ：材料Ｄからなる層（材料Ｄ層）、１０２Ａ：除去された余分な材料Ａ、１０２Ｂ：除去された余分な材料Ｂ 1: Honeycomb-shaped reaction container, 1a: Cell of the honeycomb-shaped reaction container 1, 1b: Partition of the honeycomb-shaped reaction container 1, 2: Discharge pipe, 3A, 3B: Material supply device, 4: Rotating shaft, 5A, 5B: Material Discharge port, 6A, 6B, 6C, 6D: Material flow path, 7: Outer cylinder tube, 8: Gas flow path, 9: End surface of honeycomb-shaped reaction vessel 1 on the side where the discharge tube 2 is inserted, 10: Honeycomb 101A: Layer made of material A (material A layer), 101B: Layer made of material B (material B layer), 101C: Layer made of material C (material C) Layer), 101C: layer made of material D (material D layer), 102A: removed extra material A, 102B: removed extra material B
Claims (10)
独立した複数の材料吐出口と前記複数の材料吐出口にそれぞれ独立に連結している複数の材料流路とが形成されており、前記セル中に挿入可能な吐出管、及び
前記複数の材料流路に前記複数の材料をそれぞれ独立に供給するための複数の材料供給装置
を備えていることを特徴とするセル内塗布装置。 An in-cell coating device for coating a plurality of materials in each cell of the honeycomb-shaped reaction container,
A plurality of independent material discharge ports and a plurality of material flow paths that are independently connected to the plurality of material discharge ports are formed, and a discharge pipe that can be inserted into the cell, and the plurality of material flows. An in-cell coating device comprising a plurality of material supply devices for independently supplying the plurality of materials to the passage.
前記気体流路に気体を供給するための気体供給装置を更に備えている
ことを特徴とする請求項１又は２に記載のセル内塗布装置。 In the discharge pipe, a gas discharge port for spraying gas and a gas flow path connected to the gas discharge port are further formed, and a gas supply device for supplying gas to the gas flow path is provided. The in-cell coating device according to claim 1 or 2, further comprising:
前記ハニカム状反応容器のセル中に前記吐出管を挿入する吐出管挿入工程と、
前記複数の材料を、前記複数の材料供給装置からそれぞれ独立に前記複数の材料流路に供給し、前記複数の材料吐出口からそれぞれ独立に吐出させることにより、前記ハニカム状反応容器の各セル内に前記複数の材料を塗布する塗布工程と、
を含むことを特徴とする反応容器の製造方法。 A method for producing a reaction container in which a plurality of materials are applied in each cell of a honeycomb-shaped reaction container by using the in-cell application device according to any one of claims 1 to 6,
A discharge pipe inserting step of inserting the discharge pipe into the cells of the honeycomb-shaped reaction container,
In the cells of the honeycomb-shaped reaction container, by supplying the plurality of materials to the plurality of material flow paths independently from the plurality of material supply devices and independently discharging the plurality of material discharge ports, respectively. An applying step of applying the plurality of materials to
A method for producing a reaction container, comprising:
前記塗布工程において、気体を、前記気体供給装置から前記気体流路に供給し、前記気体吐出口から吹き付けながら、前記複数の材料を塗布することを特徴とする請求項７に記載の反応容器の製造方法。 A method for producing a reaction container in which a plurality of materials are applied in each cell of a honeycomb-shaped reaction container by using the in-cell application device according to claim 3.
The reaction vessel according to claim 7, wherein in the coating step, a plurality of materials are coated while supplying gas from the gas supply device to the gas flow path and spraying the gas from the gas discharge port. Production method.
前記塗布工程において、前記吸引装置を用いて、前記ハニカム状反応容器の、前記吐出管が挿入される側の端面とは反対側の端面から前記セル内を吸引しながら、前記複数の材料を塗布することを特徴とする請求項７又は８に記載の反応容器の製造方法。 A method for producing a reaction container in which a plurality of materials are applied in each cell of a honeycomb-shaped reaction container by using the in-cell application device according to claim 4,
In the coating step, the plurality of materials are coated while suctioning the inside of the cell from the end surface of the honeycomb-shaped reaction container opposite to the end surface on the side where the discharge pipe is inserted, using the suction device. The method for producing a reaction container according to claim 7, wherein
前記塗布工程において、前記吐出管を、前記ハニカム状反応容器の各セルの長手方向の中心軸に対して相対的に回転させながら、前記複数の材料を塗布することを特徴とする請求項７〜９のうちのいずれか一項に記載の反応容器の製造方法。 A method for producing a reaction container in which a plurality of materials are applied in each cell of a honeycomb-shaped reaction container by using the in-cell coating device according to claim 5,
8. In the coating step, the plurality of materials are coated while rotating the discharge pipe relative to the central axis in the longitudinal direction of each cell of the honeycomb-shaped reaction container. 10. The method for manufacturing the reaction container according to any one of 9.
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