JP2008178805A - Fluid stirring method and fluid stirring device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a stirring method which enables a fluid in a container to be stirred at low cost by simple configuration. <P>SOLUTION: A heater 11 is installed in the outer periphery of a reaction container 1 to which reaction gas G1, a raw material of carbon nanotubes, is supplied and radiation heat absorption plates 12 are arranged at a plurality of points and prescribed intervals in the upper part of the reaction container 1 inside to locally heat the reaction gas G1, and the reaction gas G1 is stirred by spontaneous convection generated from the temperature difference. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a stirring method and a stirring device for stirring fluid in a container.

Conventionally, as an agitating device for agitating a liquid in a container, for example, a paddle-shaped agitating member is arranged in the container and rotated (for example, see Patent Document 1). In addition, when it is necessary to seal the container, the reaction container is rotatably arranged in the fixed container, and the stirring container is fixedly arranged in the reaction container. There is one in which only the reaction vessel is rotated by a rotating device arranged outside, and the liquid filled in the reaction vessel is stirred by relative movement with the stirring member (for example, Patent Document 2). reference).
Japanese Patent Laid-Open No. 2001-24760 Japanese Patent Laid-Open No. 11-244680

By the way, according to the structure of the stirring apparatus mentioned above, since the stirring member is arrange | positioned in the container, there exists a problem that the space in a container is restricted.
Furthermore, when it is necessary to maintain the hermeticity of the container as in Patent Document 2, it is necessary to drive the stirring member in the container from the outside, which makes the configuration complicated and increases the cost. There is a problem of sticking.

  Then, an object of this invention is to provide the stirring apparatus and stirring method which can stir the fluid in a container with simple structure and low cost.

  In order to solve the above problems, the fluid stirring method according to claim 1 of the present invention is caused by a temperature difference generated in the fluid by heating and / or cooling a container filled with the fluid or a predetermined region in the container. In this method, the fluid is stirred by natural convection.

A fluid stirring method according to claim 2 is a method of changing the heating rate or the cooling rate with time in the stirring method according to claim 1.
The fluid stirring method according to claim 3 is the stirring method according to claim 1 or 2, wherein the container is supplied with a carbon nanotube source gas from one end side to generate carbon nanotubes on the substrate. In this method, a cylindrical reaction vessel is used.

  The fluid stirring method according to claim 4 is the stirring method according to claim 1 or 2, wherein the container is supplied with the liquid to be separated from one end side and the membrane separator is inserted from the other end side. This is a method of forming a cylindrical separation container for performing membrane separation.

According to a fifth aspect of the present invention, there is provided a fluid agitation apparatus in which heating means and / or cooling means are arranged in a predetermined region of a side wall portion of a container filled with fluid.
According to a sixth aspect of the present invention, there is provided the fluid stirring apparatus according to the fifth aspect, further comprising a temperature control device for controlling the temperature of the heating means or the cooling means.

  According to a seventh aspect of the present invention, there is provided the fluid agitator according to the seventh aspect, wherein the container in the agitator according to the fifth or sixth aspect is a cylinder for generating carbon nanotubes on a substrate by supplying a carbon nanotube source gas from one end side And a heating means or a cooling means are arranged at the lower part or the upper part of the peripheral wall of the reaction container.

  Furthermore, in the fluid stirring device according to claim 8, the container in the stirring device according to claim 5 or 6 is formed with an opening through which the liquid to be separated can be supplied on one end side and membrane-separated from the other end side. A cylindrical separation container for performing membrane separation by inserting a body, and heating means or cooling means are arranged at the lower part or upper part of the peripheral wall portion of the separation container.

  According to the above stirring method and the configuration of the stirring device, the predetermined region in the container or the container is heated and / or cooled, and the fluid is stirred by natural convection due to the temperature difference generated in the fluid. For example, compared to the case where the inside of the container is agitated by the agitating member, the space in the container is not so much restricted, and the apparatus configuration is simplified, especially when the container needs to be sealed. The construction is very simple and inexpensive.

  Further, the stirring action can be more effectively performed by changing the heating rate or cooling rate in the vessel or the vessel with time.

[Embodiment 1]
Hereinafter, a fluid stirring device and a stirring method according to Embodiment 1 of the present invention will be described.
In Embodiment 1, when producing carbon nanotubes, the reaction gas is stirred in a reaction vessel, that is, the stirring device and the stirring method are part of the carbon nanotube manufacturing device and manufacturing method. explain.

  As shown in FIG. 1 and FIG. 2, this manufacturing apparatus includes a reaction gas (a raw material gas, which is a raw material gas of carbon nanotubes (hereinafter referred to as CNT), specifically, acetylene and a helium gas as a carrier gas. The mixture ratio is, for example, 3% acetylene and the remainder is a carrier gas. A horizontal cylindrical reaction vessel in which G1 is flowed from one end side to the other end side (can be called a stirring vessel) 1, a semi-cylindrical mounting table 2 disposed in the reaction vessel 1 for generating CNTs by vapor phase growth, and a peripheral wall portion (also a side wall portion) of the reaction vessel 1 corresponding to the mounting table 2 The heating means 3 is disposed on the upper inner surface (inner peripheral surface) of the slab, and the temperature control device 4 controls the temperature of the heating means 3.

  The heating means 3 includes a heater 11 disposed around the peripheral wall portion of the reaction vessel 1 (annularly), and an upper and lower center line (hereinafter, referred to as “upper center line”) on the upper inner surface of the peripheral wall portion of the reaction vessel 1. Alternately (in a staggered manner) on both sides of the vertical center line), for example, 5 locations (not limited to the number, may be 3 locations, 4 locations, 6 locations, 7 locations, etc.) A radiant heat absorption plate (for example, a plate made of carbon or silicon) 12 is used to generate a high temperature partially, that is, locally (predetermined region). A reaction gas G1 supply nozzle 5 is provided on one end wall 1a of the reaction vessel 1, and a discharge nozzle 6 for discharging the reaction gas G1 is provided on the other end wall 1b. Is provided.

  The heating means 3 is disposed at the central portion of the peripheral wall portion of the reaction vessel 1. Therefore, when the reaction vessel 1 is viewed thermally in the length direction, the central portion becomes the heating portion A, one end side portion, and the other. The end-side portion is a cooling section B or C where no heating means is arranged.

  In the above configuration, when producing CNTs, the reaction gas G1 is supplied into the reaction vessel 1 from the supply nozzle 5 while the inside of the reaction vessel 1 is heated to a predetermined temperature by the heating means 3. Then, the reactive gas G1 flows toward the other end, and CNTs are generated by vapor phase growth on the substrate K placed on the mounting table 2, and in the heating part A, heat is generated by the heater 11 of the heating means 3. While being supplied, heat is absorbed by the radiant heat absorbing plate 12 disposed in this portion, and a high temperature portion is locally generated. That is, a temperature difference occurs between the place where the radiant heat absorption plate 12 is provided and the place where the radiant heat absorption plate 12 is not provided, and convection (natural convection) is generated and stirred (mixed) in the reaction gas G1, so that a gas having a more uniform concentration. Since it becomes a flow, CNT with good quality can be obtained.

  In the heating means 3, the temperature control device 4 turns the heater 11 on and off at a predetermined time interval (for example, every 3 to 10 minutes), that is, changes the temperature at the radiant heat absorbing plate 12. (On / off control is not performed when sufficient natural convection is obtained without changing the temperature). Instead of turning the heater on and off, a temperature change (change in heating rate) may be given to the heater itself.

FIGS. 3A to 3C show changes in the flow of the reaction gas G1 in the cross section of the heating part A over time.
Further, in the cooling sections B and C on the inlet side and the outlet side of the reaction vessel 1, a vortex V is generated in a part of the reaction gas G1.

  According to the configuration of the first embodiment, the reaction gas is stirred by natural convection due to a temperature difference generated in the reaction gas by locally heating the inside of the reaction vessel. For example, a mechanical stirring member Compared to the case where the reaction vessel is agitated, the space in the reaction vessel is not so limited, and the apparatus configuration is simplified, especially when the reaction vessel requires a tight seal. The construction is very simple and inexpensive. Moreover, the stirring action can be more effectively performed by changing the heating rate in the reaction vessel with time.

  By the way, in Embodiment 1 described above, the radiant heat absorption plate 12 is arranged on the inner peripheral surface of the reaction vessel 1, but as shown in FIGS. 4 and 5, the outer peripheral surface of the mounting table 2 is spaced at predetermined intervals and You may make it affix the double radiation heat absorption board 12 on both sides of a vertical center line alternately (staggeredly). In this case, a portion having a high temperature and a portion having a low temperature are generated on the mounting table 2 and many natural convection portions are generated in the reaction gas G1, so that the reaction gas G1 is efficiently stirred.

  Further, as shown in FIGS. 6 and 7, the radiation heat absorbing plate 12 may be attached to the upper inner surface of the peripheral wall portion of the reaction vessel 1 and the outer circumferential surface of the mounting table 2, respectively. However, the radiant heat absorption plate 12 affixed to the reaction vessel 1 side and the radiant heat absorption plate 12 affixed to the mounting table 2 side are alternately (zigzag) arranged on both sides of the vertical center line.

  Also in this case, since the radiant heat absorption plate 12 is arranged on the reaction vessel 1 side and the mounting table 2 side, a difference in temperature can be locally provided, so that natural convection is further generated in the reaction gas G1, Stirring is performed effectively.

Of course, the temperature control similar to that of the first embodiment is also performed by the temperature control device in the configuration of the above-described modified example.
[Embodiment 2]
Next, a fluid stirring device and a stirring method according to Embodiment 2 of the present invention will be described.

  In the second embodiment, for example, when water (hereinafter referred to as a separation liquid) is subjected to membrane separation from water-containing ethanol (hereinafter referred to as a liquid to be separated) to obtain anhydrous ethanol, that is, the stirring device and the stirring method are referred to as a membrane separation device. And a part of the membrane separation method.

  As shown in FIGS. 8 and 9, this membrane separation apparatus has an opening 21a to which a separation liquid G2 is supplied from one end side, and a concentrated liquid (the separation liquid is removed from the separation liquid on the other end side). And a horizontal cylindrical separation container (which can be referred to as a stirring container) 21 provided with a take-out nozzle 22 for taking out the product) and an end wall portion 21b on the other end side of the separation container 21 to be inserted inside. A cylindrical separation membrane body 23, and a heater (as a heating means) at a plurality of locations below the peripheral wall portion (also a side wall portion) of the separation container 21 and corresponding to the separation membrane body 23. For example, a resistance heating type heater is used) 24 are arranged at predetermined intervals along the axial direction and alternately (staggered) at a plurality of locations (for example, 5 locations) on both sides of the vertical center line. And each of these Temperature controller 25 for controlling the temperature of 24 is provided.

  The heater 24 is not disposed around the separation container 21 as described in the first embodiment, but is locally disposed and heated. As shown in the drawing, the heater 24 is disposed on the peripheral wall portion. Embedded.

  The separation membrane body 23 includes a cylindrical support 23a as a framework and a separation membrane 23b that covers the entire outer peripheral surface of the support 23a. If it demonstrates concretely, many opening parts will be formed in the surrounding wall part of a cylindrical member.

  In the above configuration, when the liquid G2 to be separated is supplied into the separation container 21 from the opening 21a, the liquid G2 is moved toward the other end, but the separation liquid G2 is separated from the separation membrane 23b provided on the surface. Through the support 23a, and the liquid G2 to be separated is concentrated.

  At this time, the heater 24 disposed in the separation container 21 is locally heated to generate a temperature difference, that is, natural convection is generated and the annular space S between the separation container 21 and the separation film body 23 is generated. Thus, the stirring action is performed, and therefore the concentration of the liquid G2 to be separated in the annular space S can be made uniform, so that the separation action can be performed efficiently. The concentrated liquid is taken out from the take-out nozzle 22.

  Also in the second embodiment, similarly to the first embodiment, the heater 24 is turned on and off locally at a predetermined time interval (for example, every 3 to 10 minutes) by the temperature control device 25. A temperature change is applied (when sufficient natural convection is obtained without changing the temperature, on / off control is not performed). Instead of turning the heater on and off, a temperature change (change in heating rate) may be given to the heater itself.

  As described above, since the heaters 24 are arranged at a plurality of locations on the peripheral wall portion of the separation container 21, the liquid to be separated can be stirred in the separation container 21 without using a mechanical stirring member. That is, compared with a device that stirs using a mechanical stirring member, the configuration is simple and an inexpensive device can be provided.

  In the second embodiment, the heater 24 is disposed below the peripheral wall portion of the separation container 21. However, as shown in FIGS. 10 and 11, cooling means (specifically, a finned cooler or a water cooler). The mold coolers 31) may be alternately arranged at predetermined intervals and on both sides of the vertical center line. The cooling means 31 is also turned on and off at predetermined time intervals by the temperature control device 25 to change the temperature (when sufficient natural convection can be obtained without changing the temperature). Is not controlled on / off). Instead of turning the cooling means 31 on and off, a temperature change (change in cooling rate) may be given to the cooling means itself.

Also in this case, since the liquid to be separated in the annular space S is cooled at appropriate intervals, a downward flow (natural convection) is generated, so that the liquid to be separated is stirred.
Further, as shown in FIGS. 12 and 13, a cooling means 31 is disposed at the upper part of the peripheral wall portion of the separation container 21, and a heater 24 as a heating means is disposed at the lower part. Further, the cooling means 31 and the heater 24 are pivoted. You may make it arrange | position alternately with a predetermined space | interval in a heart direction.

  Also in this case, since the liquid to be separated in the annular space portion S is cooled at an appropriate interval and heated at the upper part and heated at the lower part, a downward flow and an upward flow due to a temperature difference occur simultaneously. The liquid to be separated is further stirred.

  Further, in the configuration according to the second embodiment, the heating unit or the cooling unit is arranged at intervals. However, as shown in FIGS. 14 and 15, and FIGS. 16 and 17, the heating unit or the cooling unit has a predetermined length. It may be arranged continuously (for example, over the distance from one end side to the front end position of the separation membrane body and the other end side to the position before the extraction nozzle 22).

  Of course, also in this case, the liquid G2 to be separated is heated in the lower part in the annular space S, or the liquid G2 to be separated is cooled in the upper part in the annular space S. Since natural convection occurs in the liquid, the liquid to be separated is stirred.

That is, since the concentration of the liquid to be separated is made uniform by agitation by natural convection of the liquid to be separated, the membrane separation action is efficiently performed.
In Embodiment 2 described above, the heater and the cooling means as the heating means are illustrated as being embedded in the peripheral wall portion (side wall portion) of the container, but of course, the heater and the cooling means are disposed on the inner surface or the outer surface of the peripheral wall portion of the container. May be.

It is a longitudinal cross-sectional view of the CNT manufacturing apparatus using the stirring apparatus which concerns on Embodiment 1 of this invention. It is a figure which shows the cross section of the same CNT manufacturing apparatus, (a) is D1-D1 sectional drawing of FIG. 1, (b) is D2-D2 sectional drawing of FIG. It is a cross-sectional view which shows the convection state of the reactive gas in the center position of the CNT manufacturing apparatus in time series. It is a longitudinal cross-sectional view of the CNT manufacturing apparatus which concerns on the modification of Embodiment 1 of this invention. It is a figure which shows the cross section of the CNT manufacturing apparatus which concerns on the modification, (a) is D3-D3 sectional drawing of FIG. 4, (b) is D4-D4 sectional drawing of FIG. It is a longitudinal cross-sectional view of the CNT manufacturing apparatus which concerns on the other modification of Embodiment 1 of this invention. It is a figure which shows the cross section of the CNT manufacturing apparatus which concerns on the other modification, (a) is D5-D5 sectional drawing of FIG. 6, (b) is D6-D6 sectional drawing of FIG. It is a longitudinal cross-sectional view of the membrane separator using the stirring apparatus which concerns on Embodiment 2 of this invention. It is a figure which shows the cross section of the same membrane separator, (a) is E1-E1 sectional drawing of FIG. 8, (b) is E2-E2 sectional drawing of FIG. It is a longitudinal cross-sectional view of the membrane separator which concerns on the other modification of Embodiment 2 of this invention. It is a figure which shows the cross section of the same membrane separator, (a) is E3-E3 sectional drawing of FIG. 10, (b) is E4-E4 sectional drawing of FIG. It is a longitudinal cross-sectional view of the membrane separator which concerns on the other modification of Embodiment 2 of this invention. It is a figure which shows the cross section of the same membrane separator, (a) is E5-E5 sectional drawing of FIG. 12, (b) is E6-E6 sectional drawing of FIG. It is a longitudinal cross-sectional view of the membrane separator which concerns on the other modification of Embodiment 2 of this invention. It is E7-E7 sectional drawing of FIG. It is a longitudinal cross-sectional view of the membrane separator which concerns on the other modification of Embodiment 2 of this invention. It is E8-E8 sectional drawing of FIG.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Reaction container 2 Mounting stand 3 Heating means 4 Temperature control apparatus 5 Supply nozzle 6 Discharge nozzle 11 Heater 12 Radiant heat absorption board 21 Separation container 21a Opening part 22 Extraction nozzle 23 Separation film body 24 Heater 25 Temperature control apparatus 31 Cooling means

Claims (8)

  A fluid stirring method comprising heating and / or cooling a container filled with a fluid or a predetermined region in the container, and stirring the fluid by natural convection due to a temperature difference generated in the fluid.   2. The fluid stirring method according to claim 1, wherein the heating rate or the cooling rate is changed with time.   The fluid stirring method according to claim 1 or 2, wherein the container is a cylindrical separation container for supplying a carbon nanotube source gas from one end side to generate carbon nanotubes on a substrate.   The fluid according to claim 1 or 2, wherein the container is a cylindrical separation container in which a liquid to be separated is supplied from one end side and a membrane separator is inserted from the other end side to perform membrane separation. Stirring method.   A fluid stirring apparatus, wherein heating means and / or cooling means are arranged in a predetermined region of a side wall portion of a container filled with fluid.   6. The fluid stirring device according to claim 5, further comprising a temperature control device for controlling the temperature of the heating means or the cooling means.   The vessel is a cylindrical reaction vessel for supplying carbon nanotube raw material gas from one end side to generate carbon nanotubes on the substrate, and the heating means or cooling means is provided below or above the peripheral wall portion of the reaction vessel. The fluid agitating device according to claim 5 or 6, wherein the fluid agitating device is disposed.   The container is a cylindrical separation container in which an opening capable of supplying a liquid to be separated is formed on one end side and a membrane separator is inserted from the other end side to perform membrane separation, and heating means or cooling The fluid stirring device according to claim 5 or 6, wherein the means is disposed at a lower portion or an upper portion of the peripheral wall portion of the separation container.

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