JPS5942040A - Reactor for making good contact of reactant in fine pore - Google Patents

Abstract

PURPOSE:To get good contact of gas and liquid, by submerging a cylindrical body rotating at high speed in a liquid phase, introducing gas into the cylinder from the upper opening, and making the liquid stream flow into the center of the cylinder in accompany with the gas. CONSTITUTION:When a shaft 8 is rotated at high speed, the liquid of a liquid phase 5 flows from the opening 4 of a porous cylindrical matter 1 to the center, collides with the inner surface of the cylinder wall 2 by a centrifugal force, passes through fine pores of the cylinder wall 2 being divided into fine streaks, and flows again to the opening 4. On the other hand, as a gas is introduced from a gas blowing pipe 10 into the cylinder 1, the gas is accompanied with the liquid circulating along curved lines as shown by arrows, passes through the fine pores of the cylinder 2, and contacts with the liquid effectively during this time. The gas is spouted from the outer surface of the cylinder wall 2 to the liquid, and becomes fine bubbles.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a contact reaction device in micropores between liquid and gas using a cylindrical body made of a porous material.

In general, in order to bring liquid into contact with a container filled with liquid, methods such as providing stirring blades inside the container to stir the liquid, or installing a baffle plate in the container to swirl the liquid in and out, etc. are considered. The idea is to establish liquid-liquid contact by installing a porous cylinder upright and rotating the cylinder at high speed to circulate the liquid from the inside of the cylinder to the outside through the porous pores by centrifugal force. , which had not been proposed at all in the past.

In addition, as a conventional gas-liquid contact method, multiple holes are bored in the wall of a cylinder made of solid wood, the cylinder is formed into an inverted bottom cylinder, and the cylinder is rotated at high speed in the liquid phase. A device was developed in the 4th year of the Tokuko Showa era, in which gas is introduced through an opening at the F end, and the thin film of gas wrapped around the cylinder wall is shredded by the surrounding slow-rotating liquid phase to generate small bubbles. +-15(] !1 Proposed in Publication No. n.

However, the hole drilled in the wall of this device from ff is a straight hole drilled perpendicularly to the wall.
It opens at right angles to the wall. Moreover, this hole (J mechanical?
Because the hole is drilled, it is a large hole of about 2 mm in diameter, and the gas that comes out of this hole travels straight toward the liquid phase outside, along the gap between the rotating cylinder wall and the liquid phase. The thin film that wraps the wall surface spreads out, wraps around the jacket surface, and is torn into pieces by the speed difference between the rotating body and the liquid flow, forming bubbles.As mentioned above, the pores are straight and the pore diameter is relatively small. Because of its large size, the amount of microbubbles that are effective for gas-liquid contact reactions is small even when taking into account the cylinder diameter, front height, rotation speed, etc., and bubbles are generated due to the vertical height of the position of the small hole drilled on the side of the cylinder. There were drawbacks such as lack of uniformity in bubble size.

Furthermore, a method of generating ultrafine bubbles in a liquid phase has been proposed in Japanese Patent Application Laid-Open No. 51-149175. This method uses a cylindrical body with a porous wall in which the majority of the pores have a diameter of 50 μm or less, and this cylindrical body is made of a porous material and is closed at both ends. ．．
1. Air is introduced through the liquid to generate microbubbles in the liquid. However, in this case, it is only air that flows out to the external liquid phase through the microbubbles of the porous phase, and moreover, it only passes through once. Therefore, there was no gas-liquid contact within the pores of the wafer U, and even if fine bubbles were generated, the gas-liquid contact was insufficient.

In view of this, the inventors of the present invention have conducted various studies in order to eliminate the above-mentioned conventional drawbacks, and have discovered the following phenomenon through experiments.

In other words, a rotor like the one shown in the m1 diagram (:3 Q
A size of mmφX45mmA1 and wall thickness 3+++s was made.

Table 1 This “1-Evening is 1r ■ Diameter 10mmφ S U S 34
．． It is attached to the center of the 5US34 bottom plate of a transparent vinyl chloride liquid tank with an inner diameter of 110 mmφ x 650 mm using a vertical shaft made of aluminum. Three diameter 12mm φ x length zQQmtnhSUSjjjJ baffles were planted at symmetrical positions 18mm away from the tank bottom, and 15mm wide baffles were planted at 210mm away from the tank bottom.
Transparent vinyl chloride board 2, 5mm thick, 50mm long
The plates were fixed with their 11.15 mm x 5 inch surfaces facing each other at right angles to the inner wall surface of the liquid tank, and were installed as baffles to prevent swirling currents occurring in the upper liquid phase of the rotor.

First, water was poured into the liquid tank to a height of 500 mm from the bottom of the tank, several dozen small pellets T-(2mlnφX 2mm A, As a result, when the rotation of the rotor reached 1000 times per minute, the water flow 1 was 1.1 - 1.1 - 1.1 - 1. A little apart from the lower end, and the water flowed diagonally downward toward the center of the rotor and the cylinder It can be clearly seen that the liquid phase is moving from the micropores on the entire wall to the external liquid phase.

When the rotation speed of the rotor is set to 5,000 times per minute or more, the detection pellet particles collect and adhere to the inside of the cylinder (1 tl) for several minutes, and are no longer found in the liquid phase.As a result, the present inventor etc., a cylinder made of porous material with one end open and the other end closed is held vertically and rotated at high speed in the liquid. L1 liquid moves from the inside of the cylinder to the outside through the micropores of the porous material. I found out.

Next, with the rotor installed in the liquid tank, water or saline solution is filled from the bottom of the tank to a height of 500 mm, and air is introduced from the open port at the bottom of the rotor.
In the three BP groups BP-12 and BP-23, when the rotor is stationary, a large air mass comes out from the hole in the upper part of the rotor cylinder wall and rises, but in the two SP groups 5p-58 and 5P-8Q, the rotor is stationary. Sometimes 1] - Even minute air bubbles do not appear from the upper part of the tube wall, and large air masses only come out from the open opening at the lower end.

At this time, when rotating 1-1-Y and gradually increasing the speed, the large air mass disappears, and in the case of water only from the cylinder wall cavity in the BP croup and SP group, it becomes an adzuki bean (2 mm to 3 mmφ spherical) and 3% In the case of salt water, it becomes cloudy with fine bubbles.

In addition, for the sp croup of 5p-58 and SP-8Q, while rotating them in water or 80% saline solution at a rate of 5,000 times per minute, a very small amount of air, e.g. When the tube is injected, the air is observed to flow out into the liquid phase in the form of smoke through the micropores in the cylinder wall.

From the above observations, when a cylindrical body made of porous material is used in a gas-liquid contact reaction device, the high-speed rotation of the rotor causes the liquid to rise [from diagonally below the open opening at the lower end of the coater toward the center of the rotor], causing microscopic cavities on the cylinder wall. When gas is added to this reflux that flows through the holes into the external liquid phase, the gas follows the liquid flow, becomes a gas-liquid mixed linear flow, and forms microbubbles in the liquid phase around the []-ta. It was found that a group of microscopic bubbles, which were diffused and concentrated in the vicinity of the open opening at the lower end of the cylinder, were repeatedly connected to the microscopic holes in the cylinder wall via the center of the rotor.

Based on the above experiments, the present invention aims to provide a contact reaction device in micropores capable of efficient liquid-liquid contact, in which at least one end of the upper or lower side is open, and the other end is open. When a cylindrical body whose end is closed with solid wood is submerged in a liquid phase with its axis perpendicular to the liquid surface and rotated at high speed, the liquid force in the liquid phase will move from the opening of the cylindrical body. flowing towards the center,
Due to the centrifugal force, the liquid circulates through the fine pores of the porous material of the cylindrical body to return to the external liquid phase.

As a characteristic of the porous material, the pore paths of the micropores are bent, and the pores open at an arbitrary angle with respect to the wall surface.
Therefore, the liquid that passes through the micropores is separated into fine lines when entering the same hole, and the liquid and liquid that form these lines repeatedly come into contact with each other and return to the external liquid, rotating at high speed. Due to the speed difference between the cylindrical body and the external hetaki, the filamentous liquid is torn into pieces, and extremely efficient liquid-liquid contact is performed, achieving the objective in a shorter time than in the conventional liquid-liquid contact method. In addition, the reaction apparatus can be made smaller and the cost can be reduced. .

In addition, the present invention provides Wl, 4, in which Koyoshi comes, which increases the degree of gas-liquid contact.
(The purpose is to provide a catalytic reaction device in a pore. A cylindrical body made of a porous material that rotates at high speed is sunk below the surface of the liquid phase, and at least one end of the cylindrical body is opened at the upper side or The liquid flow flowing from the lower opening towards the center of the cylinder is accompanied by the gas that has flowed into the cylinder from the opening, which causes the micropores of the porous 4=4 to be entrained. The gas flowing into the opening is narrowed and flows out through the pores that open at an arbitrary angle to the wall surface. Therefore, while passing through the bent pores of the micropores in the porous material, the gas is simultaneously subdivided into filaments. It makes efficient contact with the liquid passing through the assimilation channel, becomes fine bubbles, returns to the external liquid phase, and circulates through the pores, which has the effect of increasing the degree of gas-liquid contact.

Furthermore, the present invention provides a baffle plate for preventing eddy flow in the liquid phase around the cylindrical body that rotates at high speed and is submerged below the surface of the liquid in the liquid phase, thereby preventing the flow from the opening of the cylindrical body toward the center. This method is particularly effective when rotating a single-unit cylinder in a liquid phase. It is intended to provide a catalytic reaction device within the cavity.

Below, embodiments of the present invention will be described and explained with reference to the drawings.
The figure is a longitudinal cross-sectional view of a cylindrical body with the opening at the bottom, Figure 2 is a vertical cross-sectional view of the cylinder with the opening at the top, and Figure 3 is a vertical cross-sectional view of the cylinder with the opening at the top and bottom. FIG. 3 is a longitudinal cross-sectional view of a cylindrical body provided with a partition member made of solid wood.

In the figure, (1) is a cylindrical body, consisting of a cylindrical wall (2) made of porous material and a closing member (3) made of solid wood, and in the case of Fig. 1, the opening (4) is on the bottom side. The liquid phase (5
) so that the axis (7) is vertical below the liquid level (6). (8) is a drive shaft which is vertically erected, the upper end A and J parts (9) are screwed onto the closing member (3), and connected to a rotating mechanism (not shown). It is supposed to rotate.

Now, in Fig. 1, when the drive shaft (8) is rotated at high speed,
The liquid in the liquid phase (5) flows toward the center from the opening (4) of the cylinder (1), and the liquid in the cylinder wall (2) flows due to centrifugal force.
), the fine pores in the cylindrical wall (2) are exposed to the filament f.
The outer liquid 4f of the cylindrical body rotates at high speed through this division f.
Jc! : The speed difference l is more than 71. Then, while making liquid contact, the liquid circulates again to flow into the opening (.1) ζ (and makes further liquid contact.

(10) is a gas supply pipe, which supplies gas from the outside to the cylindrical body (1).
The sender W (10) is sent to the opening (
4) is inserted parallel to the inner surface of the cylindrical wall (2), and the gas ejection hole may be only at the tip of the inlet pipe (10), but a large number of holes are bored in the metal part. You may do so.

Now, when a gas is introduced into the cylinder (1 inch) from the gas supply pipe (10), this gas is carried along with the liquid that circulates and refluxes as indicated by the arrow above, and enters the fine pores in the cylinder wall (2). The bubbles pass through the bent pores, during which they come into efficient contact with the liquid, and are ejected from the outer surface of the cylindrical wall (2) into the liquid at an arbitrary angle, forming minute bubbles.

(11j is a baffle plate attached to the liquid phase (5) around the cylindrical body (1) for preventing eddy currents, and the liquid and gas injected from the outer opening of the cylindrical wall (2) are finely divided. Dispersed in the liquid, and the rotation of the liquid is restricted by the baffle plate (7)'4]7
This results in uniform miniaturization.

Figure 2 shows the case where the cylindrical body (1) is submerged with the open part (1) facing upward; in this case, the liquid is sucked in from the second side (t1) and the liquid level (G) If they are installed close to each other, the gas on the liquid surface (6) passes through the opening (4) and is sucked along with the sucked liquid, so that there is no gas-liquid contact.

In this case as well, the gas inlet pipe (1) and the baffle plate (11
) can be installed as shown in Figure 1.

In Figure 8, the upper and lower cylindrical walls (2) (2) are connected using partitions (3) (3) in the middle so that they are open, respectively, and the effects of Figures 1 and 2 are achieved. This is accomplished at the same time. In this case as well, the gas supply pipe (++11) and the baffle plate (11) can be installed.In addition, in any of the cases shown in Figs. However, this drive shaft may be installed so that it hangs down into the liquid from above the liquid level, and in this case, the bearing does not need to be installed in the liquid, making the sealing mechanism easier. .

The present invention will be explained in detail below using the following specific examples.

(Example 1.) Rotor using Palcon of each product number in Table 1 (30mmφX
4.5 mm A1 porous material wall thickness 8 mm), (1,
IQ 27m in 2m01/l sodium sulfate solution,
Inject i rL of air, fl (1(1(I R, P
, what happens when it rotates M?1. After confirming that all of the injected air turned into bubbles and that no air masses were found, the next experiment was carried out. Add 1 mole of sodium sulfite to the above liquid tank and add 1 mole of diluted powder to pure water.
Send air at 1/min, and rotate +1 - evening (SO00R).

The oxidation completion time is fixed with P and M l constant. : When the power during the reaction was determined, the second result was obtained.

Table 2 is illustrated. ! : No. 4, the oxidation rate is not necessarily high if the pore size of Palcon is small. B.P.
-12 has the shortest oxidation completion time, and the maximum oxidation amount per hour, oxygen utilization rate, and oxidation amount per unit dynamic force.

(Example 2.) Next, using BP 12, the same concentration as above (0.2 m”
/l) Start the reaction with 5 tons of sulfite solution at a liquid temperature of 50'C, and set the rotation speed at 600 ORlP.

M is kept constant, oxidation is performed by changing only the amount of air supplied, and the oxidation rate is determined as shown in Table 3. It showed.

Table 8: As can be seen from Table 3, the more fine the air is, the shorter the oxidation completion time, the less power required during that time, and the greater the amount of oxidation per unit power. However, this (J this (-1)
- It is accurate up to the limit where there is no slight appearance of bubbles in the range where RlP and M bubbles are formed. (Example 3) Cylindrical body Q
In order to compare the performance with the "Tsuki" and "Yu", among the porous material cylinders, as mentioned above, when air is supplied while stationary in the liquid, the E3P croup, which at first glance resembles a densely packed cylinder, appears only from the open opening at the bottom end. Select Nonorucon 5P-58 from 75 tomoφx i
A rotor was made of a cylinder with a wall thickness of 3 mm (7) with an open bottom end and a lid made of hard vinyl chloride (thickness 10 m + n) at the top end, and a vertical shaft made of 5US34 with a diameter of 10 mm was attached to this lid. Hard vinyl chloride was selected as the solid material, and it was a q5mmφ×llO+nmA, two-walled cylinder with an open bottom end and a closed top end with a smooth vertical surface.
#! Make a rotor with III and attach these parts to 1. Mo2
10mm diameter x 1.000mm transparent acrylic liquid tank 5
Installed vertically at the center of the bottom plate made of US34, parallel to the outer circumferential side of the rotor, perpendicular to the tank bottom, and radially to the rotor cross section Width: 5 mm, height 360 mm, height: ; Place the three sheets at a distance of 12.5 m from the outer circumferential side of the coater.
m IJlt, L,, fixed as an IUζ baffle plate at a distance of 20.5 mm from the tank inner wall surface, and further 4.0 mm from the tank bottom.
Place two transparent acrylic plates with a width of 5 mm, a length of 80 mm, and a thickness of 5 mm at a high position 0 mm apart.It is 7.5 mm.
x 15 mm were glued to the inner surface of h1 and planted so as to face each other at right angles to the wall surface to serve as a baffle plate for preventing eddy currents caused by rotation of the rotor.

4. Add anhydrous sulfite to this liquid tank. Pour in a solution with a concentration of 0°287 mOL/l, which is obtained by dissolving 14 t of pure water.
After the liquid temperature reached 45°C, the rotor was rotated at 260 OR, PlM while supplying air at a rate of 20 t7mil.
An oxidation experiment was carried out with the temperature constant at , and the results shown in Table 4 were obtained.

In Table 4 and above, 5P-58 was selected because the emphasis was placed on comparison with solid wood, but BP-58 was selected for practical use of porous material rotors.
It is estimated from Table 2 that if 2 is adopted, the oxidation rate will be further increased. In addition, in the present invention, the porous material is not limited to Palcon alone, but can be made into a porous material by solidifying porous carbon, sintered alumina, sintered metal, bisque, or particles with catalytic ability, depending on the purpose of use. It shall be possible to select as appropriate from among the following.

As mentioned above, the gas-liquid contact reaction rate of a cylinder made of porous material does not depend solely on the fineness of the bubbles, but is proportional to the multiplicative product of the fineness of the bubbles and the frequency with which the bubbles circulate through the fine pores. This shows a high reaction rate that is far beyond the reach of conventional cylinders with tight fittings. That is, since the gas-liquid contact reaction rate of the present invention is increased by using a porous material cylinder, it is an extremely economical invention that leads to the downsizing of the reaction apparatus.

In addition, although the present invention describes exclusively gas-liquid contact reactions, if the present invention is utilized between liquid-liquid and solid-liquid, the development of unexplored fields of contact reactions within micropores is expected.

[Brief explanation of drawings]

FIGS. 1, 2, and 8 are longitudinal sectional views of an apparatus showing examples of the present invention, and FIG. 4 is a diagram showing the relationship between time and oxidation rate. Explanation of main parts of the figure■...Cylindrical body 2...Cylindrical wall 8...Closing member 4. ...Opening part 5...Liquid phase
7... Axis line 8... Drive shaft 10... Gas feed pipe 6/liquid level 11. baffle board

Claims (3)

[Claims] (1) A cylindrical body made of porous material with at least one upper or lower end open and the other end closed with solid wood, the axis of which is perpendicular, and connected to a rotating mechanism. A catalytic reaction device in micropores, which is submerged below the surface of a liquid in a liquid phase so as to rotate at high speed. (2) A cylindrical body made of porous material with at least one upper or lower end open and the other end closed with solid wood, the axis of which is perpendicular, and connected to a rotating mechanism. 1. A catalytic reaction device in micropores, characterized in that the cylindrical body is submerged below the liquid surface in a liquid phase so as to rotate at high speed, and is provided with means for flowing gas into the cylindrical body from the outside. (3) A cylindrical body made of a porous material, with at least one upper or lower end open and the other end closed with a solid material,
The cylindrical body is submerged below the liquid surface in the liquid phase so that its axis is perpendicular and connected to a rotation mechanism to rotate at high speed, and a baffle plate for preventing eddy currents is attached to the liquid phase around the cylindrical body. A catalytic reaction device in micropores characterized by: