JP2003144903A - Gas-liquid contact column type apparatus and gas-liquid contact method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a gas-liquid contact column type apparatus preventing the deposition of a solid at any place even in such a case that a hydrolyzable compound in inert gas containing the hydrolyzable compound in a gaseous or misty state is reacted with water to form the solid, generating no clogging and capable of being continuously operated over a long period of time, and a gas-liquid contact method. SOLUTION: In the gas-liquid contact column type apparatus for bringing the inert gas containing the hydrolyzable compound in a gaseous or misty state into contact with water, a gas introducing pipe is attached to the top part of the body part of the column type apparatus almost downwardly and a liquid introducing pipe is attached to the body part of the column type apparatus horizontally or obliquely downwardly in an almost tangential direction with respect to the outer periphery of the body part. The gas-liquid contact method using the column type apparatus is also disclosed.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a gas-liquid contact tower apparatus for contacting water with a gas or mist-like inert gas containing a hydrolyzable compound, and a gas or mist using the tower apparatus. The present invention relates to a gas-liquid contacting method of bringing a hydrolyzable compound in the form of a water into contact with water. In particular, even when the compound in the gaseous or mist-like hydrolyzable compound-containing inert gas reacts with water to produce a solid matter, it may be anywhere in the tower apparatus. Solids do not accumulate,
The present invention relates to a gas-liquid contact tower device and a gas-liquid contact method capable of continuing gas-liquid contact for a long period of time without blockage in the tower device.

[0002]

[Prior Art and Problems] The operation and reaction of bringing gas and liquid into contact are as follows: absorption tower, cyclone scrubber, venturi scrubber, mixing scrubber, spray tower, wetting wall tower, packed tower, plate tower, bubble tower, bubble stirring tank. It is widely used in chemical factories, gas manufacturing factories, waste gas treatment plants, etc. In this case, the gas and the liquid are separately supplied into the gas-liquid contacting device so as to be brought into contact with each other, and the liquid is usually discharged from the nozzle into the gas, or the liquid is sprayed into the gas with a spray nozzle or the like. There are known methods such as spraying into the liquid or blowing gas into the liquid through a nozzle or a porous plate (March 30, 1989).
See "Chemical Equipment Handbook 2nd Edition" edited by The Japan Society of Chemical Engineering, published by Himaru Zen Co., Ltd.).

However, gas and liquid react with each other,
Alternatively, when the component in the gas reacts with the liquid or the component in the liquid to produce a solid substance, in any of the above methods and apparatuses, the solid substance is generated in the vicinity of the gas introduction part or the liquid introduction part. The present inventors have noticed that there is a problem in that it is generated and gradually grows to block the tip of a gas introduction tube or a liquid introduction tube or the inside of a gas-liquid contactor. When solid matter is deposited, it is necessary to stop the operation and remove the adhered solid matter, which is complicated and inefficient.

[0004]

Therefore, the inventors of the present invention completed the present invention through intensive research to solve the problems of the prior art. The object of the present invention is to contact gas and liquid even when the hydrolyzable compound in a gaseous or mist-like hydrolyzable compound-containing inert gas reacts with water to produce a solid. Provided is a tower-type apparatus for gas-liquid contact and a gas-liquid contact method capable of continuing a long-term operation without solid matter being deposited on any part of the tower-type apparatus and causing no blockage in the tower-type apparatus. To do.

[0005]

SUMMARY OF THE INVENTION The present invention relates to a gas-liquid contact tower apparatus for contacting water with a gaseous or mist-like inert gas containing a hydrolyzable compound, and a tower unit of the tower apparatus. A gas introduction pipe is attached to the top in a substantially downward direction, and a liquid introduction pipe is attached to the body of the tower type device in a substantially tangential direction with respect to the outer periphery of the body and horizontally or obliquely downward. In the gas-liquid contacting tower type apparatus, and the gas-liquid contacting method of contacting water with a gaseous or mist-like inert gas containing a hydrolyzable compound, the inert gas is Introduced into the body from a gas introduction tube attached to the top of the body of the mold device substantially downward,
The present invention relates to a gas-liquid contact method characterized in that water is introduced into the body to flow down while rotating on the outer peripheral surface of the gas introducing pipe and on the inner peripheral surface of the body.

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION The body of the gas-liquid contact tower apparatus is preferably cylindrical because water easily swirls inside, but it may be barrel, ellipsoidal or spherical. A gas introduction pipe for introducing a gaseous or mist-like inert gas containing a hydrolyzable compound into the tower type apparatus is attached to the top of the tower type apparatus in a substantially downward direction, preferably downward. . The gas introducing pipe extends through the top of the body of the tower type apparatus and extends into the body, and the lower end thereof is preferably located above the lower end of the body. The gas introducing pipe is preferably attached to the center of the top portion, but may be attached to a position slightly displaced from the center. A liquid introducing pipe for introducing water is attached to the body portion in a substantially tangential direction to the outer periphery of the body portion and horizontally or obliquely downward. That is, when the tower type apparatus is viewed from directly above, the liquid introducing pipe is substantially tangential to the outer periphery of the body, that is, the tangential direction, or the tangent to the central axis of the liquid introducing pipe. It is attached so that the angle it makes is 45 degrees or less. Further, when the tower type apparatus is viewed from the side, the liquid introduction pipe is installed horizontally or obliquely downward, that is, the liquid introduction pipe is attached so as to be lowered as it approaches the body. That is, the angle formed by the central axis of the body and the liquid introduction tube is 90 degrees to 1
It is attached at 5 degrees, preferably 90 degrees to 30 degrees. The liquid introducing pipe is preferably attached to the side wall of the body, but may be attached to the peripheral end of the top of the body. As a result, even in the case where the gaseous or mist-like hydrolyzable compound in the inert gas reacts with water to produce a solid, the gas is introduced on the outer peripheral surface of the pipe and the tower type apparatus. Since the water flows down on the inner peripheral surface of the body of the body so that the solid matter is constantly washed away, solid matter does not accumulate on any of the gas introduction pipe, the liquid introduction pipe, and the body, Therefore, it is possible to continue the operation for a long time without the blockage in the tower type device.

The material of the body, gas inlet pipe and liquid inlet pipe of the tower type apparatus is steel, stainless steel, duralumin, etc. when the hydrolyzable compound and its hydrolyzate are not corrosive. Preferred is glass-lined metal, enamel, ceramic, or tetrafluoroethylene resin when the hydrolyzable compound or its hydrolysis product is corrosive. In the present invention, the inert gas means a gas inert to the hydrolyzable compound or water, and examples thereof include air, nitrogen gas, argon gas, and helium gas. Inert gas is generally at room temperature,
It may be 2 ° C to 70 ° C.

The gaseous or mist-type hydrolyzable compound is a silicon compound having three or more silicon atom-bonded hydrolyzable groups in one molecule, such as tetramethoxysilane, trimethoxysilane, methyl (trimethoxy) silane, Alkoxysilanes such as tetraethoxysilane and triethoxysilane; halogenosilanes such as tetrachlorosilane, trichlorosilane and tetrafluorosilane; tri (N, N-dimethylamino) methylsilane and metal atom bond hydrolyzability Examples thereof include metal compounds having three or more groups in one molecule, such as tetramethoxytitanium, tetrachlorotitanium, tetramethoxyzirconium, tetrachlorozirconium, trimethoxyaluminum, and trichloroaluminum. Since these compounds have three or four silicon atom-bonded hydrolyzable groups or metal atom-bonded hydrolyzable groups, they are condensed while hydrolyzing to form a solid. Most of them have a boiling point higher than normal temperature, but since the vapor pressure is large, they can exist in the form of gas or mist if the concentration of the inert gas is low. These silicon compounds may be a mixture with a silicon compound having one or two silicon atom-bonded hydrolyzable groups in one molecule. Further, these metal compounds may be a mixture with a metal compound having one or two metal atom-bonded hydrolyzable groups.

The inert gas containing a hydrolyzable compound in the form of a gas or a mist is used when the hydrolyzable compound or a mixture of the hydrolyzable compound and another compound is purged with an inert gas, or the hydrolyzable compound or It is often formed when a mixture of a hydrolyzable compound and another compound is stripped in the presence of an inert gas.

Water is used to wash out and hydrolyze hydrolyzable compounds in an inert gas. Water is suitable when the hydrolyzable compound is one that is extremely easily hydrolyzed (eg, a silicon halide compound such as tetrachlorosilane and trichlorosilane, a metal halide compound), but must be acidic or basic. If it is difficult to hydrolyze (eg, alkoxysilane such as tetramethoxysilane or trimethoxysilane, or an alkoxy metal compound), water containing a water-soluble base (eg, caustic soda, potassium hydroxide) or water-soluble acid (eg, hydrochloric acid) , Sulfuric acid) -containing water is preferred. When the water used for gas-liquid contact is reused, it may contain hydrochloric acid or alcohol (methyl alcohol, ethyl alcohol) produced by hydrolysis.
Fine powder or other liquid mist or vapor may be mixed in the hydrolyzable compound-containing inert gas.

The inert gas containing a hydrolyzable compound in the form of gas or mist introduced into the body of the tower type apparatus for gas-liquid contact through the gas introduction pipe fills the body of the tower type apparatus, It comes into contact with the water introduced into the gas-liquid contact tower device through the liquid introduction pipe. Since water is introduced substantially tangentially to the outer periphery of the body of the tower type device and horizontally or obliquely downward, the water is introduced on the outer peripheral surface of the gas introducing pipe and the inner peripheral surface of the body of the tower type device. It flows down while turning above. Even if the hydrolyzable compound is hydrolyzed to form a solid, it is washed away, so that the solid does not deposit on the outer peripheral surface of the gas introduction pipe and the inner peripheral surface of the body.

If the hydrolysis is rapid, the inert gas, water and hydrolysis products will flow out through the outlet of the barrel of the tower apparatus. If the hydrolysis is not fast,
Inert gas, water, undecomposed hydrolyzable compounds and hydrolysis products flow out through the outlet. In addition,
When water contains a hydrolysis catalyst such as a water-soluble base or acid, it flows out from the outlet as base-containing water or acid-containing water. When the hydrolysis is not rapid, it is advisable to connect a structure or a storage tank for further promoting gas-liquid contact to the discharge port, and complete the hydrolysis in the structural portion or the storage tank. When the inert gas is separated from other substances after completion of hydrolysis, it becomes an inert gas containing no hydrolyzable compound, and can be reused or used for other purposes. Since it contains no impurities, it may be released into the atmosphere as it is. The water containing the hydrolysis product can be reused as it is, or can be separated and removed for reuse. Alternatively, it may be treated as a waste liquid.

[0013]

EXAMPLES Gas-liquid contact in Examples and Comparative Examples was carried out at 20 ° C.

[0014]

Example 1 In the cylindrical body 6 (inner diameter: 150 mm, height: 500 mm) of the tower device 1 for gas-liquid contact shown in FIG.
Caustic soda water-containing 4 (concentration: 4% by weight) was introduced from the liquid introducing pipe 3 (inner diameter: 25 mm). Here, the liquid introduction tube 3 is provided on the side wall of the cylindrical body portion 6 in a tangential direction to the outer periphery thereof and in an obliquely downward direction (angle between the central axis of the cylindrical body portion 6 and the central axis of the liquid introduction tube 3) Is 80 degrees). At the same time, the gas introduction pipe 2 (inner diameter: 50 m) that is attached downward through the top of the tower type device 1
m, length: 300 mm), and nitrogen gas 5 (tetrachlorosilane concentration: 10 ppm) containing gaseous or mist-like tetrachlorosilane was supplied into the cylindrical body 6 (flow rate: 3 m ³ / hr). The caustic soda-containing water 4 constantly flowed down so as to swirl on the outer peripheral surface of the gas introduction pipe 2 and the inner peripheral surface of the cylindrical body portion 6 (flow rate: 13 m ³ / hr). When the operation was continued for 350 hours under these conditions, the gas inlet pipe 2
No solid matter is deposited on the outer circumferential surface and the tip of the liquid, the opening of the liquid introduction tube 3, and the inner circumferential surface of the cylindrical body 6, and the blockage in the gas-liquid contact tower apparatus 1 due to the deposition is caused. I was able to continue operation without happening.

[0015]

[Embodiment 2] In the cylindrical body 6 (inner diameter: 150 mm, height: 500 mm) of the gas-liquid contact tower apparatus 1 shown in FIG.
A caustic soda aqueous solution (concentration: 4% by weight) was introduced from the liquid introduction pipe 3 (inner diameter: 25 mm). Here, the liquid introducing pipe 3
Is on the side wall of the cylindrical body 4, in a tangential direction to its outer periphery,
In addition, it is attached in an obliquely downward direction (the angle between the central axis of the cylindrical body 6 and the central axis of the liquid introduction tube 3 is 80 degrees). At the same time, a nitrogen gas 5 containing a gaseous or mist-like tetramethoxysilane is supplied from a gas introduction pipe 2 (inner diameter: 50 mm, length: 300 mm) that is attached downward through the top of the tower type apparatus 1. Tetramethoxysilane concentration: 10 ppm) was supplied into the cylindrical body portion 6 (flow rate: 3 m ³ / hr). The caustic soda-containing water 4 constantly flowed down so as to swirl on the outer peripheral surface of the gas introduction pipe 2 and the inner peripheral surface of the cylindrical body portion 6 (flow rate: 13 m ³ / hr). When the operation was continued for 350 hours under these conditions, the gas inlet pipe 2
No solid matter is deposited on the outer peripheral surface and the tip portion, the opening portion of the liquid introduction portion 3, and the inner peripheral surface of the cylindrical body portion 6, and the blockage in the gas-liquid contact tower apparatus 1 due to the deposition is caused. I was able to continue operation without happening.

[0016]

Comparative Example 1 A caustic soda aqueous solution (concentration: 4% by weight) was obtained from a large number of spray nozzles attached to the upper part of the cylindrical body (inner diameter: 100 mm, height 500 mm) of a conventionally known tower device for gas-liquid contact. While spraying downward (spray amount:
0.05 m ³ / hr), nitrogen gas containing tetramethoxysilane in gaseous or mist form (flow rate: 0.3 m ³ / h)
r, tetramethoxysilane concentration: 10 ppm) is supplied to the inside of the cylindrical body from a gas supply section opened at the lower part of the side wall of the cylindrical body, and discharged from a discharge port opened at the top of the cylindrical body. It was When the operation was continued for 350 hours under these conditions, a solid substance considered to be silica was deposited around the spray nozzle, and the clogging of the cylindrical body part was caused accordingly.

[0017]

EFFECT OF THE INVENTION When a gas-liquid contact tower apparatus and a gas-liquid contacting method according to the present invention are used to bring a gaseous or mist-containing inert gas containing a hydrolyzable compound into contact with water, the hydrolyzable compound is produced. Even in the case of hydrolyzing to form solids, solids do not accumulate in any of the gas supply pipe, the liquid supply pipe, and the body, and clogging of the tower-type apparatus occurs due to the accumulation. It is possible to continue the operation for a long period of time.

[0018]

[Brief description of drawings]

FIG. 1 is a side view of a gas-liquid contact tower apparatus 1 used in Examples 1 and 2 of the present invention.

FIG. 2 is a sectional view taken along the line AA of FIG.

FIG. 3 is a perspective view of the gas-liquid contact tower apparatus 1 used in Examples 1 and 2 of the present invention.

[Explanation of symbols]

1. Tower device for gas-liquid contact 2. Gas introduction pipe 3. Liquid introduction tube 4. Water containing caustic soda 5. Silane-containing nitrogen gas 6. Cylindrical body

   ─────────────────────────────────────────────────── ─── Continued front page    (72) Inventor Junichi Maejima             2-2 Chikusaigan, Ichihara-shi, Chiba Toray Dow             Corning Silicone Co., Ltd. Production Division             Inside the engineering department (72) Inventor Shigenori Nojiri             Yachi Toray Douco, Kanazu Town, Sakai District, Fukui Prefecture             Fukui Production Headquarters Ning Silicone Co., Ltd.             in the factory F-term (reference) 4D020 AA08 BA23 CB34 CC03                 4D032 BB18                 4G075 AA03 BA05 BB04 BB05 BD03                       BD08 BD13 BD26 DA02 EB21

Claims (9)

[Claims] 1. A tower apparatus for contacting gas and liquid in which a gaseous or mist-like inert gas containing a hydrolyzable compound is contacted with water, wherein a gas introduction pipe is provided at the top of the body of the tower apparatus. A gas-liquid contact tower, which is attached downward, and in which the liquid introduction pipe is attached in a substantially tangential direction to the outer periphery of the body and horizontally or obliquely downward. Mold device. 2. The tower device for contact according to claim 1, wherein the body is cylindrical. 3. The tower type apparatus for gas-liquid contact according to claim 1, wherein the tower type apparatus for gas-liquid contact is a scrubber. 4. A gas-liquid contacting method in which a gaseous or mist-like inert gas containing a hydrolyzable compound is contacted with water, wherein the inert gas is attached downward to the top of the body of a tower type apparatus. Introduced into the body from the gas introduction pipe,
A gas-liquid contacting method, characterized in that water is introduced into the body to flow down while rotating on the outer peripheral surface of the gas introducing pipe and on the inner peripheral surface of the body. 5. Water is introduced into the body through a liquid introducing pipe attached to the body in a direction substantially tangential to the outer periphery of the body and horizontally or obliquely downward. The gas-liquid contact method according to claim 4. 6. The gas-liquid contact reaction method according to claim 4, wherein the hydrolysis product is a solid substance. 7. The gaseous or mist-like hydrolyzable compound is a silicon compound having three or more silicon atom-bonded hydrolyzable groups in one molecule.
~ The gas-liquid contact method according to claim 6. 8. The gas-liquid contact method according to claim 7, wherein the silicon compound is tetraalkoxysilane or tetrachlorosilane. 9. The gas-liquid contact method according to claim 4, wherein the water is base-containing water or acid-containing water.