JP2009179536A - Method and apparatus for producing titanium dioxide fiber - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method and an apparatus for producing a titanium dioxide fiber by drying a colloidal solution on a substrate, where the solution contains mono-dispersed titanium dioxide particles. <P>SOLUTION: The production method for the titanium dioxide fiber involves the processes of making the colloidal solution to adhere onto the surface of the substrate so as to form a titanium dioxide film; and drying the film by heating with a heating means 7. A dried portion of the titanium dioxide film on the substrate is moved by sequentially changing the posture of the substrate or relatively and sequentially moving the heating means 7 with respect to the substrate to cause temporary difference of a drying degree between the front and rear positions in the moving direction of the drying portion and generate cracks along the moving direction on the dried portion of the titanium dioxide film so as to form the titanium dioxide film. The titanium fiber-producing apparatus 1 is equipped with above-described treatment members. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a titanium dioxide fiber manufacturing method and apparatus for manufacturing titanium dioxide fibers by drying a colloidal solution in which titanium dioxide particles are monodispersed on a substrate.

Conventionally, a titanium dioxide fiber production method for producing a titanium dioxide fiber by drying a colloidal solution in which titanium dioxide particles are monodispersed on a substrate having good wettability with the colloidal solution is disclosed in Patent Document 1. It is already known.
In the titanium dioxide fiber production method of Patent Document 1, titanium dioxide fibers are produced by drying the colloidal solution on a substrate, and the resulting titanium dioxide fibers are dried at a predetermined temperature (200 ° C to 1000 ° C). ). In addition, as the concentration of the colloidal solution is increased by the solution drying process (ie, the solvent evaporation process), the titanium dioxide particles are regularly and densely packed on the substrate surface to form a dense packed layer of titanium dioxide particles, and the liquid level drops. Along with this, cracks parallel to the packed layer of titanium dioxide particles are developed at equal intervals on the substrate above the liquid surface to form fibers. As a result, a fiber having a micropore structure or a mesopore structure and a large effective specific surface area is formed, so that the adsorption performance is improved and the photocatalytic action is improved as well as the separation problem. It is intended to produce titanium dioxide fibers that can be permanently fixed without occurring.
JP 2004-091315 A

  However, the titanium dioxide fiber manufacturing method disclosed in Patent Document 1 evaporates the dispersion medium of the colloidal solution while the substrate with good wettability immersed in the colloidal solution is tilted from the horizontal and placed in the colloidal solution. In the substrate above the liquid level, cracks parallel to the packed layer of titanium dioxide particles develop at equal intervals in the substrate above the liquid level, but the formation of fibers depends on the drop in liquid level due to transpiration. Therefore, the production efficiency is low, and it takes a long time to form a long fiber in mass production, solution management to maintain the solution homogeneous over a long period of time, and the solution on the substrate tilted from the horizontal to a certain condition There are drawbacks such as complicated drying management. In addition, there is a problem in mass production such that the shape and characteristics of the obtained titanium dioxide fiber are likely to vary.

  First, a titanium dioxide fiber manufacturing method and apparatus for solving the above-described problems are obtained by attaching a colloidal solution in which titanium dioxide particles are dispersed to form a titanium dioxide film on the surface of the substrate 6, In the method of drying by heating the titanium dioxide film with the heating means 7, the posture of the substrate 6 is sequentially changed, or the heating means 7 is moved relative to the substrate 6 to sequentially move the titanium dioxide film on the substrate 6. The dried portion of the titanium dioxide film is moved, and a temporary difference is caused in the degree of drying of the titanium dioxide film at positions before and after the moving direction of the dried portion, so that the dried titanium dioxide film is cracked along the moving direction. It is characterized by forming titanium dioxide fibers.

  Second, the end portion of the substrate 6 is immersed in a colloidal solution in which titanium dioxide particles are dispersed.

  Third, in a container 3 that contains a colloidal solution in which titanium dioxide particles are dispersed, at least the surface side of the substrate 6 tilted with respect to the horizontal is immersed in the solution so that the solution adheres to the substrate 6. In the method of manufacturing titanium dioxide fibers by sequentially drying the attached solution as the liquid level descends toward the lower end side of the substrate, the inclination angle of the substrate 6 is changed in the direction in which the substrate 6 stands up. Thus, the liquid level is lowered relatively to move the dry portion.

  Fourth, the substrate 6 is a flat plate, and the substrate 6 is sequentially tilted in the upright direction with respect to the liquid surface.

  Fifth, the substrate 6 is a bottom plate of the dish-like container 3, and the container 3 itself is tilted in the direction in which the bottom plate stands.

  Sixth, after storing the solution in the container 3, the container 3 is carried into the drying chamber 8, and the substrate 6 is tilted in the standing direction in the drying chamber 8.

  Seventh, the tilt angle of the substrate 6 is changed while moving the container 3 in the drying chamber 8.

  Eighth, the colloidal solution in which the titanium dioxide particles are dispersed is discharged and supplied from the nozzle 82 which is close to the substrate 6 in the direction crossing the moving direction.

  Ninth, a colloidal solution in which titanium dioxide particles are dispersed is coated on the substrate 6.

  Tenth, a heating unit 7 that heats the internal atmosphere, a drying chamber 8 that includes a transfer device 2 that carries an object to be dried into the interior, and that is transported after drying, and a substrate 6 that is transferred by the transfer device 2 and tilted to the inside. And a container 3 that contains a colloidal solution in which titanium dioxide particles are dispersed so that the surface of the substrate 6 is immersed, and the substrate 6 of the container 3 that moves in the drying chamber 8 is raised. And an angle changing device 12 for sequentially changing the inclination angle.

  Eleventh, the container 3 includes a bottom plate made of a flat plate and a peripheral wall 6 a, and the bottom plate also serves as the substrate 6.

  Twelfth, the pallet 4 is configured such that the container 3 is pivotally supported by the fixed base 9 on which the transfer device 2 is placed so as to be swingable up and down by a swing support point 26 in a direction substantially orthogonal to the transfer direction. It is said.

  Thirteenth, the angle changing device 12 is installed in the drying chamber 8 along the transfer direction of the transfer device 2 and is provided on the rail-shaped inclined guide 29 having a guide surface in the transfer direction and on the swinging side of the container 3. It is characterized by comprising a driven guide 28 that is guided along the guide surface along with the transfer of the container 3 and changes the inclination angle of the substrate 6.

  14th, the carrying-in side stocker 13 which stocks and sequentially supplies the container 3 to the transfer device 2 is provided on the drying object carry-in side of the drying chamber 8, and after the drying carried out by the transfer device 2 on the dry object carry-out side The delivery stocker 14 for stocking the containers 3 sequentially is provided.

  Fifteenth, a solution supply unit 18 for supplying a colloidal solution in which titanium dioxide particles are dispersed to the container 3 between the upper part of the carry-in stocker 13 or between the carry-in stocker 13 and the carry-in port 56 of the drying chamber 8. It is characterized by providing.

  Sixteenth, an actuator that drives the transfer device 2 to sequentially transfer the container 3 from the carry-in side to the carry-out side, and an actuator that operates the carry-in side stocker 13 in a standby posture to transfer the container 3 to the transfer device 2; An actuator for driving the discharge side stocker 14 to a standby posture to sequentially receive the containers 3 from the transfer device 2 side and a control device 22 for controlling each actuator are provided.

The titanium dioxide fiber manufacturing method and apparatus configured as described above have the following effects. By producing a titanium dioxide fiber by forming cracks along the moving direction in the dried titanium dioxide film in the form of fibers by changing the posture of the substrate or moving relative to the heating means, a uniform titanium dioxide fiber is obtained. It can be manufactured easily and efficiently continuously.
Further, the solution can be easily supplied to the substrate by immersing the substrate in the solution. Further, if the solution is supplied from a nozzle that is close to the direction intersecting the moving direction of the substrate or is applied to the substrate, the amount of solution may be supplied to the substrate only by forming the titanium dioxide film. Can be efficiently attached without waste.

  In a container containing a colloidal solution in which titanium dioxide particles are dispersed, at least the surface side of the substrate inclined with respect to the horizontal is immersed in the solution to attach the solution, and the liquid level toward the lower end side of the substrate In order to produce titanium dioxide fiber by sequentially drying the attached solution with the relative descent of the substrate, the liquid level is lowered relatively by changing the inclination angle of the substrate in the direction of raising the substrate. Thus, the titanium dioxide film can be sequentially dried while being formed. As a result, it is possible to easily and efficiently form a uniform titanium dioxide fiber in which the cracks along the transfer direction are generated and the thicknesses of the upper end side and the lower end side of the fiber generated by the cracks are substantially constant.

  The substrate is the bottom plate of a dish-shaped container, and the amount of solution attached by tilting the container itself in the direction in which the bottom plate stands up and tilting in the direction in which the bottom plate stands in the state where the solution is stored and stored in the container. It is possible to facilitate the formation of a titanium dioxide fiber having a uniform thickness while keeping the temperature constant, and to facilitate the supply of the solution to the substrate.

  After the solution is stored in the container, the container is carried into the drying chamber, and the substrate is tilted in the standing direction in the drying chamber, so that the solution in the container is attached to the substrate by the tilting of the substrate in the drying chamber. Since it is made to dry, making it constant sequentially, formation of a titanium dioxide fiber can be performed easily and rapidly.

  A drying chamber provided with a heating means for heating the internal atmosphere and a transfer device for carrying an object to be dried into the interior and carrying it out after drying, and a substrate which is transferred by the transfer device and is inclined in either direction before or after the transfer direction. A container that contains a colloidal solution in which titanium dioxide particles are dispersed so as to immerse the surface of the substrate, and a container that moves in the drying chamber in order to dry the titanium dioxide particles attached to the substrate. By changing the inclination angle of the substrate in the direction to erect the substrate, the liquid level is relatively lowered. Thus, mass production of homogeneous titanium dioxide fibers can be carried out efficiently and easily. In addition, since homogeneous fibers can be continuously produced through a relatively short drying process, the production apparatus can be reduced in size and the production cost can be reduced.

  The container includes a flat plate and a peripheral wall, and the bottom plate also serves as a substrate, so that the angle can be easily changed in the direction in which the container is raised by the angle changing device. Can be made simple and inexpensive. In addition, it is possible to easily perform maintenance work such as supply of the solution and cleaning and arrangement of the container after fiber formation.

  The container is transported through the fixed base of the pallet by configuring the pallet by pivotally supporting the fixed base on which the container is placed on the transfer device so that it can swing up and down by a swinging fulcrum in a direction substantially perpendicular to the transfer direction. It can be stably placed on the apparatus, the substrate can be tilted with high accuracy, and the formation of titanium dioxide fibers can be made homogeneous.

  An angle changing device is installed in the drying chamber along the transfer direction of the transfer device, a rail-shaped inclined guide having a guide surface in the transfer direction, and the guide surface provided on the swinging side of the container along with the transfer of the container. And a follower guide that changes the tilt angle of the substrate guided along the direction of the substrate. Since the titanium dioxide film formed by lowering the surface relatively is sequentially dried, mass production of homogeneous titanium dioxide fibers can be easily and reliably performed.

  A carry-in side stocker is provided on the carry-in side of the drying object in the drying chamber to stock and sequentially feed the container, and the carry-out side in which the container is sequentially stocked after drying is carried out by the transfer apparatus on the dry object carry-out side By providing a stocker, a plurality of containers can be collected and stocked in the carry-in stocker, and the stocked containers can be sequentially supplied to the transfer device and the containers after the drying process can be stocked together in the carry-out stocker. It can be automated, and the convenience in handling containers can be enhanced.

  Transfer from the loading stocker by providing a solution supply unit that supplies the colloidal solution in which titanium dioxide particles are dispersed to the container above the loading stocker or between the loading side stocker and the inlet of the drying chamber. The solution can be supplied immediately before being carried into the drying chamber by the apparatus. Moreover, the stock of the container with respect to the loading side stocker can be simplified.

  An actuator that drives the transfer device to sequentially transfer the container from the carry-in side to the carry-out side, an actuator that operates the loading-side stocker in a standby position to transfer the container to the transfer device, and a container that is sequentially received from the transfer device side Mass production of titanium dioxide fibers can be labor-saving and economically performed by providing an actuator for driving the discharge-side stocker in a standby position and a control device for controlling each actuator.

  An embodiment of the present invention will be described with reference to the drawings. FIG. 1 is a front view showing an overall structure of a titanium dioxide fiber manufacturing apparatus 1 according to the present invention, and FIG. 2 is a plan view of FIG. 3 is a left side view of FIG. 1, and FIG. 4 is a right side view of FIG. FIG. 5 is a left side view showing the configuration of the transfer device 2 of FIG. FIG. 6 is a front view showing the configuration and operation of the pallet 4 having the container 3 transferred by the transfer device 2 and the angle changing device. 7 is a front view showing an embodiment of the substrate 6 and the pallet 4 of the container 3, FIG. 8 is a plan view of FIG. 7, FIG. 9 is a bottom view, and FIG. 10 is a left side view of FIG. FIG. 11 is a right side view of FIG. FIG. 12 is a perspective view showing the overall structure of the manufacturing apparatus 1 according to another embodiment. FIG. 13 is a front view showing the overall structure of the manufacturing apparatus 1 according to another embodiment.

  In this titanium dioxide fiber manufacturing apparatus 1, a pallet 4 provided with a heating means 7 for heating an internal atmosphere and a container 3 for storing a solution as a drying object, which will be described later, is provided at a substantially central portion of the apparatus body 11 by a transfer device 2. A drying chamber 8 is provided for carrying it in and carrying it out after drying. The transfer device 2 can transfer the substrate 6 inclined in any direction before and after the transfer direction, and in this embodiment, a plurality of pallets 4 each including a container 3 for storing a solution so as to wet the surface of the substrate 6. And an angle changing device 12 that sequentially changes the inclination angle in the direction in which the substrate 6 of the container 3 moving in the drying chamber 8 is raised.

The transfer device 2 has the front and rear sides extended to both the front and rear sides of the drying chamber 8, and the loading side stocker 13 that stocks and sequentially feeds the containers 3 to the front side (drying object loading side), and the rear side (drying target). An unloading side stocker 14 for sequentially storing and stocking the containers 3 transferred and unloaded from the drying chamber 8 is connected to the unloading side).
Further, a pallet supply device 16 that supplies the pallet 4 including the container 3 from the carry-in side stocker 13 to the transfer device 2 is provided on the dry object carry-in side of the transfer device 2. Further, a pallet unloading device 17 for supplying the container 3 from the transfer device 2 to the unloading side stocker 14 is provided on the drying object unloading side.

Above the transfer device 2, a solution supply unit 18 for supplying a colloidal solution in which titanium dioxide particles are dispersed to the container 3 is disposed between the loading-side stocker 13 and the drying chamber 8, and the solution supply unit 18 can automatically supply the solution from above to the container 3 of the pallet 4 being transferred from the supply pipe 19.
The manufacturing apparatus 1 includes actuators provided on the front side of the apparatus main body 11 such as the transfer device 2, the heating means 7, the carry-in stocker 13, the carry-out stocker 14, the pallet supply device 16, and the pallet carry-out device 17. There is provided a control device 22 for controlling the operation. That is, the control device 22 transfers from the loading-side stocker 13 to the transfer device 2, loads and unloads the container 3 before and after drying into the drying chamber 8, transfers it to the unloading-side stocker 14, and supplies the solution to the container 3. It is possible to perform automatic operation or manual operation by a program in which is set.

  In the manufacturing apparatus 1 configured as described above, at least the surface side of the substrate 6 inclined with respect to the horizontal in the container 3 for storing the solution is immersed in the solution to attach the solution, and titanium dioxide by the attached solution is used. A method of manufacturing titanium dioxide fibers by sequentially drying the film can be employed. At this time, the substrate 6 is changed with respect to the substrate 6 by changing the inclination angle of the substrate 6 in the direction in which the substrate 6 is erected by the angle changing device 12. Thus, the liquid level can be lowered relatively (moving the drying site) to speed up drying, facilitating mass production of titanium dioxide fibers, and reducing production costs.

Hereinafter, the configuration and operation of each part of the manufacturing apparatus 1 will be described in detail. First, the container 3 and the pallet 4 will be described with reference to FIGS. The container 3 is a rectangular dish in plan view, and a bottom plate made of a recessed plate is also used as the substrate 6, and a peripheral wall 6 a is erected on the outer periphery of the substrate 6. In addition, the container 3 in the illustrated example has a rectangular shape of about 330 mm in length and width, has a depth of about 20 mm, and contains about 530 g of solution therein.
The pallet 4 is supported on a fixed base 9 that can be placed on the transfer device 2 so that the container 3 can be swung up and down by a swing fulcrum in a direction perpendicular to the transfer direction. 6 is tilted and changed with a predetermined conveyance angle, which will be described later, to facilitate drying in the drying chamber 8.

In other words, the pallet 4 is pivotally supported by a rotating shaft 26 provided on the upper side in the transfer direction with respect to the fixed base 9 so as to swing up and down, and a buffer member 27 made of a coiled spring is provided on the lower side in the transfer direction. Provided.
Further, the pallet 4 in the illustrated example rotatably supports a roller 28 as a driven guide that protrudes outward from the left and right peripheral walls 6a on the lower side in the transfer direction, and the roller 28 is rotatably supported by the transfer device 2. When the container 3 rolls on the guide surface of an inclined guide (guide rail) 29 provided along the right and left of the container 3, the container 3 is moved upward with the rotation shaft 26 as a fulcrum, and the substrate 6 also serving as a bottom plate is directed upward in the transfer direction. The solution can be transferred while changing the solution drying inclination angle.

  The container 3 of the present embodiment is configured such that the substrate 6 provided on the fixed base 9 is a container. For example, as indicated by a dotted line in FIG. 3 may be configured to be detachably mounted on the peripheral wall 6a. In this case, since the container 3 can be easily removed from the pallet 4, the cleaning and handling of the container 3 can be simplified. Moreover, the said container 3 can be utilized as a container for a baking process as it is by using what was used in the fiber manufacturing process by forming with a heat resistant material.

  The substrate 6 is preferably a metal substrate, sapphire substrate, ceramic or the like having good wettability to the colloidal solution. When the dispersion medium is water, it is a glass substrate, and when the dispersion medium is alcohol, a glass substrate or a plastic substrate. (Polypropylene or the like) is preferably used. Here, the wettability means that the solution wets well with respect to the substrate, and phenomenologically means that the droplet does not repel on the substrate. In most cases, good wettability means that the surface tension is not large.

Next, the manufacturing apparatus 1 will be described with reference to FIGS. In this manufacturing apparatus 1, the transfer device 2 for carrying the pallet 4 into the drying chamber 8 and carrying it out after drying is widened so that the pallet is stably placed as a scallop-like endless belt conveyor, and the conveying surface side is in a horizontal state. In the drying chamber 8, the pallet 4 is placed and the pallet 4 is transferred at a slow speed of about 5 mm per minute.
The transfer device 2 is wound around the extension wheels 31 and 32 that are pivotally supported on the front and rear ends of the apparatus main body 11, and the drive wheel 33 and the plurality of rolling wheels 33 a on the non-conveyance side. A conveyor guide (not shown) is provided between the two, and the transfer device 2 is supported so as to maintain the transfer horizontal state, and the placed pallet 4 can be transferred without being vibrated in a stable posture.

Further, the angle changing device 12 shown in FIG. 6 provided in the transfer device 2 is configured such that the inclined guide 29 is arranged along the conveyor from the device main body 11 side. As a result, when the transfer device 2 transfers the pallet 4 mounted, the angle changing device 12 changes the inclination angle of the substrate 6 to promote drying of the solution (titanium dioxide film) adhering to the substrate 6. Titanium fibers are formed promptly and uniformly.
That is, the angle changing device 12 according to the embodiment is installed in the drying chamber 8 along the transfer direction of the transfer device 2, and has a rail-shaped inclined guide 29 having a guide surface in the transfer direction, and a swing side of the container 3. A driven guide (roller in the illustrated example) 28 that is provided along the guide surface and changes the inclination angle of the substrate 6 along with the transfer of the container 3 is provided.

The illustrated inclination guide 29 is provided along the drying chamber 8 having a total length of about 1000 mm, and the inclination angle of the guide surface is such that the inlet inclination angle α near the entrance of the drying chamber 8 is about 0.33 degrees. None, the entire system is inclined so that the exit inclination angle θ in the vicinity of the exit is about 1.49 degrees. Further, an upwardly inclined surface and a downwardly inclined surface are formed at both ends of the inclined guide 29 so that the roller 28 is smoothly guided to the inclined guide 29, and the container 3 of the pallet 4 unloaded from the drying chamber 8 is smoothly lowered. I try to do a guide.
As a result, the angle changing device 12 has a gentle upward movement of about 0.348 ° / h in the direction of raising the substrate 6 of the container 3 during the period from the initial drying stage to the final drying stage when the pallet 4 is transferred through the drying chamber 8. An angle change amount is given. As a result, the tilt guide 29 rolls the roller 28 and sequentially changes the tilt angle of the substrate 6 so that the titanium dioxide film formed of the adhering solution has a more uniform thickness and is set for each zone in the drying chamber 8 to be described later. Since the drying is carried out at a given temperature, the solution can be quickly dried and the titanium dioxide fiber can be produced uniformly.

  In addition, the container 3 of the embodiment includes a bottom plate made of a flat plate and a peripheral wall 6a, and the bottom plate also serves as the substrate 6 so that the angle change device 12 sequentially changes the inclination angle in the direction in which the container 3 stands. Therefore, the structure for changing the angle of the substrate 6 can be made simple and inexpensive, but the substrate 6 formed of a separate flat plate is tilted by the angle changing device 12 while being immersed in the solution in the container 3. In this case, the titanium dioxide fiber can be produced by attaching the solution to the surface of the substrate 6 with the container 3 fixed.

The pallet supply device 16 installed above the front portion of the transfer device 2 extends so that the tip of the pallet supply device 16 faces the substantially central portion of the pallet width above the carry-in stocker 13. The fed pallet 4 is relayed to the transfer device 2.
That is, the pallet supply device 16 in the illustrated example is provided with the chain frame 41 and the motor 42 facing the upper side of the transfer device 2 from the apparatus main body 11 side, and a driven sprocket 43 that is pivotally supported at the tip of the chain frame 41. And a drive sprocket 44 of the motor 42 is wound around a chain 47 in which a plurality of carry-in claws 46 are provided with a predetermined interval.

  On the other hand, the pallet carry-out device 17 is installed at the rear part of the drying chamber 8 and extends so that the front end portion faces the substantially central portion of the pallet width above the carry-out side stocker 14 and is sent out from the drying chamber 8. The pallet 4 can be transferred from the transfer device 2 to the pallet unloading device 17 and stored. The pallet carry-out device 17 has the same drive and chain tension structure as the pallet supply device 16, and the chain 47 is also provided with a claw-shaped carry-out claw 46a similar to the carry-in claw 46. 4 can be accommodated in the pallet unloading device 17 from the transfer device 2.

  Next, the drying chamber 8 will be described with reference to FIGS. In the drying chamber 8, heating means (heaters) 7 for heating the internal atmosphere are arranged vertically along the transfer device 2, and a blower 52 for supplying heated air toward the container 3 is installed in the apparatus main body 11. A nozzle 53 that communicates with the blower 52 is provided facing each zone. Further, the drying chamber 8 is covered with a cover 54, and a carry-in port 56 and a carry-out port 57 for carrying in and carrying out the pallet 4 are formed by passing the carrying surface side of the transfer device 2 through the front and rear covers of the drying chamber 8. Yes.

With this configuration, the drying chamber 8 can carry the pallet 4 into the inside via the transfer device 2 and carry it out after drying. The heating means 7 and the blower 52 make the internal atmosphere a suitable drying environment for the solution, and transpiration. It is designed to promote the drying efficiency of the solution by ventilating and draining the generated water.
In addition, the drying chamber 8 of the embodiment has a total length of about 1000 mm and is divided into three zones at substantially equal intervals, and the heating (drying) temperature of each zone is about 130 ° C. in the first zone A on the carry-in side, The intermediate second zone B is set to about 120 ° C., and the third zone C on the carry-out side is set to about 130 ° C. As a result, the temperature drop during loading and unloading facing the outside of the machine is suppressed, and each zone is set to an average temperature to perform uniform drying. The blowing temperature sent from the blower 52 is about 110 ° C., and the temperature for each zone is set and adjusted by adjusting the temperature with the heating means 7.

  Next, the carry-in side stocker 13 and the carry-out side stocker 14 will be described. The carry-in stocker 13 has a stocker 58 formed with a shelf that allows the pallet 4 to be stored in the upper and lower stages, and is placed on a lifter 61 installed on the machine frame 59 so as to be moved up and down. The stocker 58 is formed in a U shape in plan view by connecting four support frames 58a with a horizontal frame 62 forming a shelf, and the U-shaped open portion faces the pallet supply device 16 side. When set, the uppermost horizontal frame 62 can be positioned at a height equal to or slightly higher than the height of the transfer device 2 starting end.

With the above configuration, the carry-in stocker 13 may have the pallet 4 stored in the uppermost shelf as shown in the example shown in FIG. it can. Then, when the chain 47 of the pallet supply device 16 is rotated in the transfer direction, the carry-in claw 46 is engaged with the peripheral wall 6a forming the container 3 at an appropriate position of the pallet 4, that is, in the embodiment, the pallet 4 is rotated in the transfer direction. It is carried on the moving transfer device 2.
The pallet supply device 16 is set at a higher speed than the transfer speed of the transfer device 2. When the pallet 4 is transferred to a predetermined position and the loading claw 46 is detached from the pallet 4, the pallet supply device 16 is subsequently transferred at a lower speed by the transfer device 2. Subsequently, the pallet 4 receives the supply of the solution from the solution supply unit 18 at the initial stage of transfer, and is carried into the drying chamber 8.

  Further, when the carry-in and transfer of the first pallet 4 is completed and the start side of the transfer device 2 makes the next pallet 4 ready to be carried in, the lifter 61 is operated by detecting the situation or by controlling the program. The pallet 4 can be brought directly under the pallet supply device 16 and stopped at the loading posture position. As a result, the second pallet 4 can be supplied to the transfer device 2 by the pallet supply device 16 and the transfer by the transfer device 2 is started. At this time, a predetermined transfer interval K is provided between the first pallet 4 and the second pallet 4 and between the subsequent pallets 4, and it is possible to carry in, transfer, and carry out continuously.

On the other hand, the carry-out stocker 14 performs the operation with the same configuration as the carry-in stocker 13, and a redundant description of the structure is omitted. The parts are set facing each other. As shown in FIG. 4, the stocker 58 stands by at the position where the initial work position is raised by the lifter 61, and the lowermost shelf of the stocker 58 is equal to the height of the end of the transfer device 2 or Positioned at a slightly lower height.
Thereby, the carry-out side stocker 14 can quickly store the pallet 4 engaged and transferred to the carry-out claw 46 a of the pallet carry-out device 17 in the shelf formed by the lowermost horizontal frame 62.

  Next, when the first storage operation is completed, the stocker 58 stands by at the storage posture position where the pallet 4 can be stored in the second shelf by the one-step lowering operation of the lifter 61. Therefore, the storage operation is continued by the same operation. Can be done. The lifter 61 in the illustrated example shows an example in which a pantograph-type link mechanism is expanded and contracted by an actuator (not shown), but is arranged along a cylinder mechanism or a column frame 58a that operates the stocker 58 with hydraulic pressure or pneumatic pressure. The screw mechanism for rotating the screw rod and the stocker 58 can be moved up and down.

Next, the solution supply part 18 installed in the front part side of the transfer apparatus 2 is demonstrated. The solution supply unit 18 in the illustrated example is configured to supply a colloidal solution in which titanium dioxide particles are dispersed to the container 3 that is stably placed on the transfer device 2 from the carry-in side stocker 13 and reaches the angle changing device 12. Solution supply without spillage can be performed quickly.
The solution supply unit 18 in this embodiment includes a tank 18a for storing a titanium dioxide sol, a tank 18b for storing a silicon dioxide sol, and a tank 18c for storing water. By mixing in the mixing tank 18d, a colloidal solution in which titanium dioxide particles are monodispersed is formed, and the above solution is automatically supplied to the container 3 of the pallet 4 being transferred by the nozzle 19 from the upper side for every batch required amount. I am trying to supply.

  Each of the above solutions uses a commercially available one for the purpose of economical mass production. For example, the titanium dioxide sol per batch required amount is a 31.78 g 20% solution containing about 6.36 g of solid content, The silicon dioxide sol is set as a 23.22 g 20% solution having a solid content of about 4.64 g, and a solution of about 532.96 g is added to and mixed with about 477.96 g of water. That is, in this manufacturing apparatus 1, the amount of solution required for one batch supplied and accommodated in one container 3 is about 532.96 g including 11 g of solid content, and the solid content with respect to the total amount is about 2%. I am doing so.

As a result, it is possible to produce titanium dioxide fibers with a yield of 70.5% or more, which is much higher than the conventional yield (54.0%) by drying with the production apparatus 1 in one batch solution having a solution concentration of about 2% did it.
In the drying experiment in which the concentration of the solution is set using the manufacturing apparatus 1, when the solution concentration is about 2% or less, the fiber is not efficiently formed and the yield is lowered, and the solvent concentration is about 2%. In the case described above, although the fibers were formed, they were thin and fragile, making them difficult to use. Further, when the solution having a solvent concentration of 2% is dried in the drying step without using the angle changing device 12 while maintaining the tilt angle of the substrate 6 at 1.33 degrees, the yield is reduced and the titanium dioxide fiber formed. In other words, the upper end side of the substrate 6 is thin and the lower end side is thick, resulting in uneven thickness and unevenness in fiber strength.

  Next, the operation mode of the control operation preset by the control device 22 will be described with respect to the operation of manufacturing the titanium dioxide fiber by the manufacturing apparatus 1 configured as described above. First, when the production apparatus 1 is started to operate, the atmosphere in the drying chamber 8 is set to a set temperature by the heating means 7 and the blower 52, the transfer device 2 and the pallet supply device 16 are operated, and the pallet supply device 16 is brought into a work standby posture. The pallet 4 is transferred from the first shelf of the side stocker 13 to the transfer device 2, and the colloidal solution is supplied from the solution supply unit 18 to the container 3 at the liquid supply position in the initial stage of transfer.

  Next, the pallet 4 containing the solution in the container 3 is transferred to the inclined guide 29 side, and the next pallet 4 is sequentially sent to the start end of the transfer device 2, so that 3 in the drying chamber 8 as shown in FIG. Each pallet 4 has a transfer interval K and sequentially proceeds to the drying step. Next, the pallet 4 containing the titanium dioxide fibers formed by the above drying is released from the transfer by the transfer device 2 and the inclined guide 29 and is sequentially stored in the unloading side stocker 14 by the pallet unloading device 17, and a series of fiber manufacturing operations are performed. Completed.

Therefore, the manufacturing apparatus 1 having the above-described configuration forms fibers by continuously drying a plurality of containers 3 while simultaneously transferring a plurality of containers 3 in the drying chamber 8 even if the transfer speed of the pallet 4 by the transfer apparatus 2 is reduced. Since it collect | recovers sequentially, mass production of a titanium dioxide fiber can be performed easily.
And since the container 3 which formed the fiber through the drying process as described above is stored in a predetermined number in the carry-out side stocker 14, it can be easily transferred to the next firing process. Since the batch-stored fibers can be collectively brought into a firing furnace and fired, firing operations that are batch-processed can be efficiently performed.

In the above baking process, the titanium dioxide fiber formed by drying is fired at a temperature of 600 ° C. to 1000 ° C., thereby promoting solidification and producing anatase type titanium dioxide fiber. The catalytic activity of the titanium dioxide fiber produced by the apparatus 1 can be increased.
As described above, the solution supplied to the container 3 is fibrillated by efficient drying accompanying the tilting of the substrate 6 in the standing direction.

  Then, when drying is performed in the drying chamber 8, the inclination angle of the substrate 6 is promoted while the heat evaporation of the solution is promoted by the ambient temperature and the gentle transfer speed for each of the plurality of zones determined over the entire length in the drying chamber 8. The titanium dioxide film adhering to the substrate 6 can be sequentially dried by changing the height of the substrate 6 in the direction in which the substrate 6 is raised and moving the liquid level relatively downward. Thereby, in the drying chamber 8, the substrate 6 of the container 3 gradually changes greatly in the direction in which the inclination rises, and therefore, the boundary of the adhering liquid descends sequentially every time the inclination changes, A constant thin titanium dioxide film having a predetermined thickness can be formed, and when drying sequentially from the formed titanium dioxide film side, a difference in the degree of drying occurs before and after the drying site. , Causing cracks along the transfer direction. Further, at this time, as the inclination gradually increases with the transfer, the thickness of the upper end side and the lower end side of the fiber caused by the crack becomes substantially constant, and a uniform titanium dioxide fiber can be easily formed. .

  As a result, in the manufacturing apparatus 1 according to the present invention, it was possible to secure a production amount of about 111 g or more per day, which is higher in each stage than that manufactured by the conventional batch method. The obtained fibers have an average length of 190 mm or more, an average width of 193 μm, and an average thickness of about 81 μm. Furthermore, almost all of the fibers had a uniform fiber length and good handleability, and the fired fibers could be produced with sufficient strength.

Further, when the fiber was used by being inserted and filled as a water purification member in a water purification column installed in a water pipe, it was able to sufficiently withstand 0.3 MPa, which is the discharge pressure of tap water. Further, as a result of the photocatalytic performance evaluation test, the catalyst activity was able to be an excellent titanium dioxide fiber that achieves a NOx decomposition rate of 100%.
And since the manufacturing apparatus 1 which performs the above manufacturing methods can manufacture a uniform fiber continuously with a comparatively short drying process, size reduction of an apparatus can be achieved and manufacturing cost can be reduced. It was possible to significantly reduce.

  Next, the manufacturing method and apparatus of the titanium dioxide fiber which concerns on another embodiment of this invention shown in FIG. 12, FIG. 13 are demonstrated. In addition, description is abbreviate | omitted about the structure and effect | action similar to the thing of the said embodiment. First, the manufacturing apparatus 1 shown in FIG. 12 attaches a colloidal solution in which titanium dioxide particles are dispersed so as to form a titanium dioxide film having a uniform thickness on the surface of the inclined substrate 6. When heating and drying by the heating means 7, the substrate 6 and the heating means 7 are sequentially moved relative to each other to change the heating part relatively, and the degree of drying of the titanium dioxide film at the front and rear positions in the movement direction of the heating part. By making this difference, it is possible to produce titanium dioxide fibers by causing cracks along the moving direction to form fibers in the dried titanium dioxide film.

The manufacturing apparatus 1 includes a transfer substrate device 63 constituting a moving belt-like substrate 6, a solution supply unit 18 for supplying and attaching a solution to the lower end side of the substrate 6, and a titanium dioxide fiber formed by the substrate 6 at the upper end. And a fiber recovery unit 66 for recovering the baked titanium dioxide fibers baked by the baking unit 64.
In the transfer substrate device 63, the substrate 6 is formed as a flat endless belt 6b. The belt 6b is wound around a driving wheel 66 and a driven wheel 67, and the transfer surface side is supported by a flat plate-shaped guide member 68. It has a configuration. Then, the transfer substrate device 63 is inclined between the solution supply unit 18 and the baking device 64 so that the transfer surface of the substrate 6 composed of the belt 6b has the same upward inclination angle as in the above embodiment. A heating means 7 is provided along the transfer surface.

The solution supply unit 18 immerses the lower end side of the belt 6 b of the transfer substrate device 63 in a supply container 71 that stores the solution supplied from the supply pipe 19.
The firing unit 64 includes a firing transfer device 72 that transports the titanium dioxide fibers received from the transfer substrate device 63 toward the fiber recovery unit 66, and a firing device 73 that fires the titanium dioxide fibers being transferred by the firing transfer device 72. Is done. The baking transfer device 72 is configured such that a flat endless belt 74 having heat resistance is wound around a drive wheel 76 and a driven wheel 77 and the transfer surface side is supported by a flat plate-shaped guide member 74a.
The fiber recovery unit 66 in the illustrated example uses a winding drum 78 that winds and collects titanium dioxide fibers fed from the firing transfer device 72.

  In the manufacturing apparatus 1 configured as described above, the belt 6b of the transfer substrate device 63 immersed in the supply container 71 causes the solution to adhere to the surface of the substrate 6 as it rotates and transfers the solution in the tilt direction. be able to. At this time, the adhering solution is lowered from the upper side toward the lower side and returned into the supply container 71, so that a titanium dioxide film can be formed on the surface of the substrate 6 with a constant layer thickness, while the titanium dioxide film is being transferred. Drying is accelerated by the heating means 7, and it is possible to sequentially dry from the upper side, and it is possible to form a crack in the belt direction to form titanium dioxide fibers as in the above embodiment. Then, the titanium dioxide fiber is continuously transferred from the end of the belt 6 b to the belt 74 of the baking transfer device 72.

Next, the titanium dioxide fibers on the belt 74 are baked by the baking device 73 and are baked into titanium dioxide fibers during the transfer, and are continuously recovered by the fiber recovery unit 66.
As described above, the manufacturing apparatus 1 relatively moves the substrate 6 and the heating means 7 in order to relatively change the heating part, and the difference in the degree of drying of the titanium dioxide film at the front and rear positions in the movement direction of the heating part. As a result, cracks along the moving direction are formed in the dried titanium dioxide film in the form of fibers, and long titanium dioxide fibers can be easily and continuously produced efficiently.

Next, the manufacturing apparatus 1 shown in FIG. 13 will be described. In the manufacturing apparatus 1, the transfer substrate device 63 is configured as a large-diameter drum that rotates a flat belt-like substrate 6 around a rotation shaft 79. The transfer substrate device 63 constitutes a drying chamber 8 provided with a heating means 7 and the like on the upper part of the drum. The solution supply unit 18 is installed on the upper side in the rotational direction from the drying chamber 8, and the fiber recovery unit 66 including the scraper 81 that is in sliding contact with the substrate 6 is installed on the lower side in the rotational direction from the drying chamber 8.
In the illustrated example, the solution supply unit 18 is provided with a supply container 71 for immersing the lower part of the transfer substrate device 63 in the solution as in the above-described embodiment, so that the transfer substrate device 63 rotates on the surface of the substrate 6 as the transfer substrate device 63 rotates. Let the solution adhere.

  In the manufacturing apparatus 1 configured as described above, the substrate 6 of the transfer substrate device 63 immersed in the supply container 71 causes the solution to adhere to the surface of the substrate 6 as the substrate 6 rotates so that the substrate 6 is directed in the inclination direction of the curved drum. Can be transported. At this time, since the adhering solution is lowered from the upper side toward the lower side and returned to the supply container 71, a titanium dioxide film is formed on the surface of the substrate 6 with a constant layer thickness and is transferred by the heating means 7 while being transferred. Drying can be promoted, and the titanium dioxide fibers can be formed in the same manner as in the above embodiment by sequentially drying from the lower side in the rotation direction (transfer direction) and causing cracks in the drum rotation direction. Accordingly, homogeneous and long titanium dioxide fibers can be produced easily and efficiently.

  Further, the solution supply means for the transfer substrate device 63 of each of the above embodiments is close to the direction crossing the moving direction on the entire width of the substrate 6 as shown in FIG. When the nozzle 82 is provided, the solution can be supplied to the substrate 6 without waste. That is, the nozzle 82 in this case has a nozzle shape that uniformly attaches the solution to the supply pipe 19 of the solution supply unit 18 over the entire width of the substrate 6, so that a necessary amount of solution sufficient to form a titanium dioxide film can be obtained. Therefore, it is possible to save and simplify management such as precipitation diffusion of the solution without wasting the solution as compared with the means for immersing.

In addition to the above, the solution supply unit 18 can easily form a titanium dioxide film using a brush (not shown) for applying the solution onto the substrate 6. In this case, if the solution is continuously supplied to the vibrating brush, the solution can be saved and the formation management of the titanium dioxide film can be simplified.
The drum rotation type transfer substrate device 63 is easy to extend in the width direction and is suitable for mass production of fibers, and can be formed into a polygonal drum, and the flat substrate 6 formed by the polygon. The titanium dioxide fibers having a fiber length for each length can be easily and continuously produced.

It is a front view which shows the whole structure of the manufacturing apparatus of the titanium dioxide fiber concerning this invention. It is a top view of FIG. It is a left view of FIG. It is a right view of FIG. It is a left view which shows the structure of the drying chamber of FIG. It is a front view which shows the structure and effect | action of an angle change apparatus. It is a front view which shows the structure of a pallet. FIG. 8 is a plan view of FIG. 7. FIG. 8 is a bottom view of FIG. 7. FIG. 8 is a left side view of FIG. 7. It is a right view which shows the state which lowered | hung the container of FIG. 7 and leveled it. It is a perspective view which shows the whole structure of the manufacturing apparatus which concerns on another embodiment of this invention. It is a front view which shows the whole structure of the manufacturing apparatus which concerns on another embodiment of this invention.

Explanation of symbols

1 Manufacturing equipment 2 Transfer equipment 3 Container 4 Pallet 6 Substrate (bottom plate)
6a Peripheral wall 7 Heating means 8 Drying chamber 12 Angle changing device 13 Carry-in side stocker 14 Carry-out side stocker 22 Control device 26 Oscillating fulcrum 28 Followed guide (roller)
29 Inclined guide 82 Nozzle

Claims (16)

  In a method in which a colloidal solution in which titanium dioxide particles are dispersed is attached to the surface of a substrate (6) so as to form a titanium dioxide film, and the titanium dioxide film is dried by heating with a heating means (7). The dried portion of the titanium dioxide film on the substrate (6) is moved by sequentially changing the posture of the substrate (6) or sequentially moving the heating means (7) relative to the substrate (6). And causing a temporary difference in the degree of drying of the titanium dioxide film at the front and back positions in the movement direction of the drying site, thereby causing cracks along the movement direction in the dried titanium dioxide film to form titanium dioxide fibers. A method for producing titanium dioxide fibers.   The method for producing titanium dioxide fibers according to claim 1, wherein the end of the substrate (6) is immersed in a colloidal solution in which titanium dioxide particles are dispersed.   In a container (3) containing a colloidal solution in which titanium dioxide particles are dispersed, at least the surface side of the substrate (6) inclined with respect to the horizontal is immersed in the solution to attach the solution to the substrate ( 6) In the method for producing titanium dioxide fibers by sequentially drying the attached solution as the liquid level descends toward the lower end side, the substrate (6) is tilted at an inclination angle. The manufacturing method of the titanium dioxide fiber of Claim 1 or 2 which moves a dry site | part by lowering | releasing a liquid level relatively by changing to the direction to make.   The method for producing a titanium dioxide fiber according to claim 3, wherein the substrate (6) comprises a flat plate and the substrate (6) is sequentially tilted with respect to the liquid surface in the standing direction.   The method for producing titanium dioxide fibers according to claim 3 or 4, wherein the substrate (6) is a bottom plate of the dish-like container (3), and the container (3) is tilted in a direction in which the bottom plate stands.   The container (3) is loaded into the drying chamber (8) after the solution is stored in the container (3), and the substrate (6) is tilted in the standing direction in the drying chamber (8). A method for producing titanium dioxide fibers.   The method for producing a titanium dioxide fiber according to claim 8, wherein the inclination angle of the substrate (6) is changed while moving the container (3) in the drying chamber (8).   The method for producing titanium dioxide fibers according to claim 1, wherein the colloidal solution in which the titanium dioxide particles are dispersed is discharged and supplied onto the substrate (6) from a nozzle (82) close to the direction crossing the moving direction.   The method for producing titanium dioxide fibers according to claim 1 or 8, wherein a colloidal solution in which titanium dioxide particles are dispersed is applied onto a substrate (6).   A drying chamber (8) provided with a heating means (7) for heating the internal atmosphere and a transfer device (2) for carrying a dry object into the inside and carrying it out after drying, and the inside of the drying chamber (8) transferred by the transfer device (2). A container (3) having a tilted substrate (6) and containing a colloidal solution in which titanium dioxide particles are dispersed so as to immerse the surface of the substrate (6), and the inside of the drying chamber (8) An apparatus for producing titanium dioxide fibers, comprising: an angle changing device (12) that sequentially changes an inclination angle in a direction in which a substrate (6) in a moving container (3) is erected.   The manufacturing apparatus according to claim 10, wherein the container (3) includes a bottom plate made of a flat plate and a peripheral wall (6a), and the bottom plate also serves as the substrate (6).   12. A pallet (4) in which a container (3) is pivotally supported on a fixed base (9) mounted on a transfer device (2) by a swing fulcrum (26) so as to be swingable up and down. Manufacturing equipment for titanium dioxide fiber.   An inclined guide (29) having an angle change device (12) provided between the drying chamber (8) side and the container (3) side and having a guide surface in the transfer direction along the transfer direction of the transfer device (2); The titanium dioxide fiber according to claim 10, 11 or 12, which is constituted by a driven guide (28) which is guided along the guide surface along with the transfer of the container (3) and which changes the inclination angle of the substrate (6). Manufacturing equipment.   A loading-side stocker (13) that stocks the container (3) and sequentially supplies the container (3) to the transfer device (2) is provided on the drying object carry-in side of the drying chamber (8), and the transfer device (2) is placed on the drying object carry-out side. The apparatus for producing titanium dioxide fibers according to claim 10, 11 or 12, or 13, wherein a delivery-side stocker (14) for stocking the containers (3) after drying carried out by step (1) is provided. A colloidal solution in which titanium dioxide particles are dispersed is supplied to the container (3) between the upper part of the carry-in stocker (13) or the carry-in stocker (13) and the carry-in port (56) of the drying chamber (8). The apparatus for producing titanium dioxide fibers according to claim 14, further comprising a solution supply unit (18) that performs the operation.   An actuator that drives the transfer device (2) to sequentially transfer the container (3) from the carry-in side to the carry-out side, and a stand-by posture for the carry-in stocker (13) to transfer the container (3) to the transfer device (2) And an actuator for driving the discharge side stocker (14) to a standby posture so as to sequentially receive the containers (3) from the transfer device (2) side, and a control device (22) for controlling each actuator. The apparatus for producing titanium dioxide fibers according to claim 10, 11, 12, 13, 14 or 15.

Images