JP3258469B2 - Gas-liquid separation device - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a gas-liquid separation apparatus for generating a gas from a liquid to be treated or a solute thereof by a chemical reaction and recovering the liquid after removing the gas.

[0002]

2. Description of the Related Art There have been proposed many devices for physically or chemically separating and removing dissolved substances contained in a liquid to be treated. For example, as a device for physically separating and removing dissolved substances from a liquid to be treated, a filtration and separation device using activated carbon, hollow fibers, or the like to remove chlorine and other impurities contained in tap water is well known. ing. Such a filtration and separation device is characterized in that filtration and separation are performed in a state in which chlorine is dissolved in an aqueous solution.
If sent to a separation device, water as a processing liquid can be obtained.

However, in this type of filtration and separation equipment, it is necessary to periodically replace activated carbon and hollow cotton yarn.
There was a problem that costs increased in the long term. There is also a problem that components to be filtered and separated cannot be taken out and used. So, without using filter media,
Many gas-liquid separation devices have been proposed which generate a gas component from a liquid to be treated to separate the liquid to be treated into a specific gas component and a residual solution component.

For example, as a first means for generating a gas component from a liquid to be treated, a container containing the liquid to be treated is depressurized by a vacuum pump and placed under a pressure condition lower than the saturated vapor pressure of the gas component. There is known a gas-liquid separation device that separates a gas component and a liquid component by realizing a state in which a gas component in a liquid to be processed is easily evaporated. As a second means, the solute (gas component) in the liquid to be treated is diffused and dissolved in the solvent by bringing the liquid to be treated into contact with the solvent via the semipermeable membrane, so that the solute (gas) in the liquid to be treated is There is known a gas-liquid separator in which only the solvent is removed by removing the component.

Further, as a third means, there is known a gas-liquid separation apparatus which lowers the solubility of a solute (gas component) contained in a liquid to be treated by heating the liquid to be treated and vaporizes and separates the gas component. Have been. Further, as a fourth means, by utilizing the difference between the boiling point of the solute (gas component) in the liquid to be treated and the boiling point of the solvent (liquid component), the liquid to be treated is distilled off by volatilization to separate the solvent and the solute from each other. There is known a gas-liquid separation device for performing vaporization separation.

[0006] As a fifth means, a gas-liquid separation is carried out by filling a liquid to be treated into a catalyst tank which is open to the atmosphere, stirring and promoting gas-liquid separation, and then allowing the liquid to stand to take out only the solvent from below. Devices are known.

[0007]

However, the conventional gas-liquid separator has the following problems. That is, a gas-liquid separation device that separates gas and liquid by placing the liquid under treatment under reduced pressure is a solute (gas component) at room temperature even when used for a liquid containing a solute having a high boiling point.
However, there is a problem in that the use of the liquid to be treated containing a solute having a low boiling point cannot be promoted, and the use thereof is limited. Further, since it is necessary to provide a vacuum pump or the like as a part of the apparatus, the apparatus becomes large, and when the solute in the liquid to be treated is a corrosive gas, the vacuum pump or the like is corroded and the gas-liquid separation apparatus May significantly shorten the product life,
Further, there is a problem that noise and vibration are generated with the operation of the vacuum pump and the like.

In a gas-liquid separation apparatus for removing a solute in a liquid to be treated using a membrane such as a semipermeable membrane, the gas-liquid separation time depends on the diffusion time (diffusion rate) of the solute in the solvent. However, there is a problem that it takes a long time to complete the gas-liquid separation. This problem is usually attributable to the slow diffusion rate of the solute into the solvent.However, the diffusion rate is a property value resulting from the interaction between the solvent and the solute, and it is not possible to greatly accelerate this. It is difficult, and it is necessary to increase the absolute diffusion amount by increasing the contact area between the solvent and the solute, and there is a problem that the apparatus becomes large.

Further, in a gas-liquid separation apparatus for simply separating a gas component and a liquid component by simply heating the liquid to be treated, fine bubbles appearing in the liquid to be treated due to heating are extremely difficult to separate and recover from the liquid component. For this reason, there is a problem that the separation accuracy is extremely poor unless some other separation and collection means is provided. Further, in a gas-liquid separation device that separates a liquid to be treated into a solute and a solution by distillation, a heating device is required to evaporate a desired gas component in the liquid to be treated, and the energy cost becomes extremely high. , Distillation apparatus such as a distillation column must be provided, and the entire apparatus is significantly increased in size.
In addition, there is a problem that equipment costs increase.

In a gas-liquid separation apparatus using a catalyst tank, the gas-liquid separation operation is a batch operation in which the gas components in the liquid to be treated are kept in a batch process waiting for release into the atmosphere. Is difficult to perform, and there is a problem that the processing ability is inferior. Further, even if the fine bubbles generated by decomposition do not readily deaerate from the solution and the solvent is taken out from the lower layer of the catalyst tank, separation from the solvent is difficult, and the gas-liquid separation accuracy is poor. .

The present invention has been made in order to solve the above-mentioned problems, and can perform gas-liquid separation without being affected by the boiling point of a solute, and can perform gas-liquid separation with high gas-liquid separation and purification ability. It is another object of the present invention to provide a gas-liquid separation device which does not require high energy cost, does not generate noise and vibration, and is excellent in space saving.

[0012]

In order to achieve this object, a gas-liquid separation device according to the present invention is provided in a space partitioned by a porous wall through which a liquid can pass. A chemical reaction medium that chemically reacts with the treatment liquid to generate a gas is provided, and the separated liquid after removing the gas generated by the chemical reaction medium is extracted and separated through the porous wall. It is a gist of the invention. Examples of the chemical reaction medium used at this time include a catalyst and an enzyme.

In this case, a porous wall partitioning the space is constituted by a porous tube, a chemical reaction medium is provided in the porous tube, and a chemical reaction medium is supplied from the liquid to be treated fed into the porous tube. Either the separation liquid excluding the gas generated by the reaction medium is configured to be extracted to the outside of the porous tube through the porous wall of the porous tube, or the porous tube having the porous wall is The chemical reaction medium is provided around the perimeter , and a separated liquid obtained by removing the gas generated by the chemical reaction medium from the liquid to be treated fed around the porous tube is passed through the porous wall of the porous tube. It is good to be constituted so that it may be extracted in a body tube. It is desirable that the space is held at a pressure lower than the bubble point pressure of the porous wall that partitions the space.

[0014]

According to the gas-liquid separation device of the present invention having the above-described structure, the liquid to be treated fed into the space partitioned by the porous wall having the gap through which the liquid can pass is provided in the space. In contact with the chemical reaction medium, and a gas is generated by a chemical reaction with the chemical reaction medium.

The generated gas does not leak out of the void of the porous wall because the space partitioned by the porous wall is pressurized to the bubble point pressure or lower, so that the gas to be treated can be prevented. The separated liquid from which gas has been removed from the liquid is extracted from the pores of the porous wall to the outside of the porous wall. The gas left in the space is separated and collected separately. In the case where the chemical reaction medium is provided in the porous tube, when the liquid to be treated is fed into the porous tube, the liquid to be treated comes into contact with the chemical reaction medium to generate gas. Then, the separated liquid from which the generated gas has been removed is extracted to the outside of the porous tube through the space of the porous tube.

On the other hand, in the case where the chemical reaction medium is provided around the porous tube, the liquid to be treated is supplied around the porous tube.
When it is sent, gas is generated from the liquid to be treated, and the separated liquid after removing the gas is extracted into the inside of the porous tube through the pores of the porous wall, and passes through the porous tube. Will be collected.

The bubble point pressure of the porous wall is obtained by immersing the porous wall in a liquid (for example, water), applying gas pressure from one side of the porous wall to push out the liquid in the pores, and from the other side to generate air bubbles. Can be determined from the gas pressure at which the gas begins to appear (bubble point method). The bubble point pressure P is calculated by using the maximum pore diameter r of the porous wall, the surface tension γ of the liquid, the contact angle θ between the liquid and the porous wall, and the shape factor K of the pore, P = K · 4πγ · It is known that the relational expression of cos θ · 1 / r is approximately satisfied, and it is possible to estimate the range of the pore diameter according to the processing pressure from this equation.

For example, if the working pressure is set to ² kg / cm ² , the bubble point pressure P of the porous wall used must be at least higher than 2 kg / cm ² . Here, when the porous wall is an alumina ceramic porous body and the liquid to be treated is water, the surface tension of water is 73 dy.
ne / cm, the contact angle between water and alumina ceramic is 1
0, the pore shape coefficient of the porous alumina ceramic body is set to 0.
Assuming that 2, the maximum pore diameter r is 0.9 μm from the above relational expression.
m or less. Generally, the pore size distribution has a wide range. Therefore, it is preferable to select and use a porous body having a pore size taking this into consideration.

[0019]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of a gas-liquid separator embodying the present invention will be described below in detail with reference to the drawings. FIG. 1 is an explanatory view showing the overall schematic configuration of a gas-liquid separation device according to the present invention, and FIG. 2 is a schematic cross-sectional view of a porous tube containing a catalyst or an enzyme in the gas-liquid separation device. FIG.

The gas-liquid separation device D according to the present invention comprises a liquid storage tank T for storing the liquid to be processed, and a gas-liquid separation section S for separating the liquid to be processed into a gas component and a liquid component. In this embodiment, a 1% hydrogen peroxide solution (H ₂ O ₂ solution) is stored in the liquid storage tank T as a liquid to be treated. The to-be-treated liquid storage tank T has a to-be-treated liquid supply pipe 10 for connecting the to-be-treated liquid storage tank T and the gas-liquid separator S.
And the liquid to be treated from the liquid storage tank T to be treated
Pump 11 for forcibly supplying air to a certain pressure
Is installed.

The gas-liquid separation section S includes a liquid recovery casing 13.
And a plurality of (four in this embodiment) porous tubular bodies 12 (1
2a, 12b, 12c, 12d) are inserted in parallel, and the respective porous tubes 12 are connected via a joint tube J so as to form one continuous flow path. The starting end side porous tube body 12a is connected to the storage tank T via the liquid supply pipe 10 to be treated as described above. V
Is provided.

On the other hand, an outlet portion 14 for discharging the gas vaporized and separated in the gas-liquid separation portion S is formed in the terminal end side porous tube 12d. A pipe 16 is connected to the processing gas pipe 16,
A pressure regulating valve 15 for adjusting the pressure inside the porous tube 12 is provided.

Further, at the bottom of the liquid recovery casing 13 , a receiving portion 13a for receiving a solvent (water) extracted from the outer tube wall of each porous tube 12 is formed.
The receiving portion 13a is provided with a discharge port 22 for discharging the collected water as a processing liquid, and the discharge port 22 is connected to a discharge pipe 23 for sending the processing liquid to another device.

Here, referring to FIG.
Will be described in detail. In each of the porous tubes 12 constituting the gas-liquid separation unit S, a plurality of pores 17 are formed over the entire wall of a hollow tube having an outer diameter of 7 mm and an inner diameter of 5 mm. On the inner wall surface of the porous tube 12, a manganese dioxide powder layer 18 carrying manganese dioxide over the entire area is provided.
The porous tubing 12 is filled with a manganese dioxide carrier 19, which has been pulverized to a diameter of about 1 mm and granulated, so as to occupy about 50% of the internal space. FIG. 2 is a model diagram showing the porous tube body 12 in which the pores 17 are formed and the manganese dioxide powder layer 18, and does not exemplify the actual state of the pores 17.

The porous tube 12 is manufactured as follows. That is, alumina powder 1 having an average particle size of 5 μm
The respective raw materials were put into a mixer so that the mixing amounts were 20 g of wollastonite, 30 g of talc, 20 g of methylcellulose, and 100 g of water with respect to kg, and the materials were kneaded well. 7mm, 5.5m inside diameter
A hollow tubular body of m is manufactured. After the raw tube is naturally dried, it is baked at 1600 ° C. for about 3 hours to decompose and burn off the methylcellulose contained in the raw tube, and wollastonite and talc are used as sintering aids. By acting, the alumina particles are sintered. At that time, a porous tube body 12 having many continuous ventilation holes 17 in which ventilation voids (continuous ventilation holes) 17 are formed three-dimensionally between the alumina particles is obtained.

The pores 17 formed in the porous tube 12
Has an average pore diameter of 0.8 μm, and a porosity indicating the amount of the pores 17 per unit area is 41%. The bubble point pressure, which indicates the boundary pressure at which only the liquid to be treated (liquid) is permeated but not the oxygen gas (gas), was measured by the above-mentioned bubble point method, and was 1.7 kg / kg.
cm ² . As long as the gas-liquid separation operation is performed at an operation pressure equal to or lower than the bubble point pressure obtained as described above, oxygen gas (gas component) is not extracted to the outside of the porous tube.

Next, a method for fixing the catalyst to the porous tube 12 will be described. Manganese dioxide powder (reagent) 1
Each of the raw materials was mixed by a ball mill for 18 hours to obtain a slurry so that the mixing amounts were 00 g, 60 g of water, and 1 g of polyvinyl alcohol, and the porous tube 12 having a wax agent applied to the outer surface was immersed in the slurry and the inner surface was filled with dioxide. The manganese powder layer 18 is formed by coating. After the porous tube 12 is naturally dried, it is baked at 1300 ° C. for about 1 hour to decompose and disappear the polyvinyl alcohol and the wax, thereby forming a porous film having a large number of pores 18a and a thickness of about 100 μm. A manganese dioxide powder layer 18 is formed on the inner wall surface of the porous tube 12.

Next, the operation of the gas-liquid separator D provided with the porous tube 12 manufactured as described above will be described. When the pump 11 is driven, the processing liquid storage tank T
Hydrogen peroxide solution stored in the liquid supply pipe 10
When the open / close valve V is opened, the gas is fed to the gas-liquid separation unit S via the starting end side porous tube 12a, and starts to flow inside the porous tube 12. When passing through the plurality of porous tubes 12a, 12b, 12c, and 12d, the hydrogen peroxide solution is formed on the inner wall surface of the porous tube 12 and is filled into the inside of the porous tube 12. It comes into contact with the manganese dioxide powder layer 18 and the manganese dioxide carrier 19 that function as a catalyst for decomposing hydrogen oxide water.

Here, manganese dioxide is well known as a catalyst for decomposing hydrogen peroxide (H ₂ O ₂ ) into water (H ₂ O) and oxygen (O ₂ ), and 2H ₂ O ₂ → 2H Hydrogen peroxide is decomposed into water and oxygen gas by a catalytic chemical reaction represented by ₂ O + O ₂ . Therefore, in this chemical decomposition reaction, there is no need to use any power or energy, and no vibration or noise is generated. In conjunction with this decomposition means, the porous tube 12 separates and recovers oxygen and water generated by the chemical decomposition reaction of hydrogen peroxide.

The porous tube 12 used here transmits only the liquid component (water) and does not transmit the gas component (oxygen) in the case of a gas-liquid separation operation in which the operating pressure is equal to or lower than the bubble point pressure. It has pores 17. Therefore, oxygen, which is a gas component, remains inside the porous tube 12 without being extracted outside the porous tube 12, and the fourth porous tube 12
The gas flows to the processing gas outlet 14 formed at 12 d and is stored in a processing gas container or the like via the pressure regulating valve 15 and the processing gas pipe 16.

The pressure regulating valve 15 is used to maintain the pressure inside the porous tube 12 constant to prevent the gas-liquid separation operation from being interrupted and to adjust the bubble point pressure. Thus, the porous tube 12
The internal pressure is maintained at a constant value because the pressure inside the porous tube 12 is reduced outside the porous tube 12 in order to extract water, which is the liquid component of the hydrogen peroxide solution after the generation of oxygen gas, to the outside. It must be kept higher than the pressure, and the pressure in the porous tube 12 should not exceed the bubble point pressure in order to prevent oxygen as a gas component from being extracted outside. It is necessary to adjust.

On the other hand, the liquid component (water) from which the gas component has disappeared
Can be freely extracted from the pores 17 to the outside of the porous tube 12 if a pressure difference is generated between the inside of the porous tube 12 and the outside of the porous tube 12. Due to the pressure difference generated between the porous tube 12 and the inside thereof, the gas is extracted to the outside from the pores 17 formed in the porous tube 12. At this time, since the pore diameter r is as small as about 0.8 μm and the pore path is formed in a complicated manner, impurities contained in the liquid component (water) are also removed during the permeation. It can be used as disinfecting water.

As described above, the water extracted on the outer surface of each of the porous tubes 12 falls toward the receiving tray 13 a formed at the bottom of the liquid recovery casing 13 and is collected.
The water collected in the tray 13a in this manner is sent to the next device through the discharge pipe 23 through the discharge port 22 as a treatment liquid.

In this embodiment, the gas-liquid separation section S is composed of four porous tubes 12 (12a, 12b, 12c, 12d). A liquid separation operation has been performed. Therefore, the hydrogen peroxide in the hydrogen peroxide water decreases as the first and second tubes flow, and almost no hydrogen peroxide remains in the terminal end porous tube 12d, and the desired gas component And only enough water to wet the porous tube 12 remains. Further, by providing the plurality of porous tubes 12 in this manner, the separation accuracy is improved, and the gas component and the liquid component can be separated with an extremely high separation rate.

Next, the gas-liquid separation performance using the gas-liquid separation device D according to the present invention will be described with reference to experimental results. This experiment was conducted using the gas-liquid separation device D shown in FIG. 1, using 1% aqueous hydrogen peroxide as the liquid to be treated, and applying the flow rate by the pump 11 under the condition of a pressure of 1 kg / cm ^2. Of 12 ml / min. The experiment was performed as follows. The concentration of the hydrogen peroxide solution in the processing solution obtained by the experiment is reduced to 0.01%, and the concentration of the hydrogen peroxide solution is reduced to about 1/100 by using the gas-liquid separation device D according to the present invention. Means lowering

In this embodiment, manganese dioxide is used as a catalyst as a means for evaporating oxygen from the hydrogen peroxide solution. However, an enzyme (catalase) may also be used to convert oxygen from the hydrogen peroxide solution. Can be vaporized.

The present invention has been described based on the embodiments. However, the present invention is not limited to the above embodiments.
It can be easily inferred that various modifications and improvements can be made without departing from the spirit of the present invention. That is,
In this embodiment, a case is described in which oxygen gas is generated from hydrogen peroxide water using a catalyst (manganese dioxide) as a gas generating means. It may be used as a generating means to remove ozone (O ₃ ), and a catalyst or an enzyme capable of gasifying and removing a desired gas component from a liquid to be treated may be used as a means for generating gas. It is.

In this embodiment, a porous tube is used for gas-liquid separation and recovery. However, the present invention is not limited to this as long as it has a space structure having a porous wall. It may be a rectangular tube provided with. Further, the raw material of the porous tubular body may be porous silica or zeolite in addition to alumina as long as the raw material is adjusted so as to obtain a desired pore diameter, and is limited to the raw material used in the present embodiment. There is no. Also, the molding method is not limited to the molding method used in the embodiment as long as a molding method according to the raw material is adopted.

The method of supporting the catalyst and the enzyme on the porous tubular body differs depending on the catalyst and the enzyme to be used. It is sufficient to adopt an optimum supporting method for each catalyst and enzyme. The method is not limited. Further, in the present embodiment, a case where a catalyst or the like for gas generation is placed inside the porous tube and the liquid to be treated flows inside the tube is described. The same result can be obtained by placing the catalyst or the like on the substrate so that the liquid to be treated flows around the porous tube, and collecting the extract after gas separation in the tube.

[0040]

As is apparent from the above description, according to the gas-liquid separation device of the present invention, the liquid to be treated supplied to the space partitioned by the porous wall through which the liquid can pass is chemically treated. A gas is generated by the reaction with the reaction medium, and only the liquid portion excluding the generated gas is separated and recovered through the porous wall, so that it depends on the boiling point of the liquid to be treated or its solute. Gas-liquid separation can be performed without any need, and gas-liquid separation with high gas-liquid separation accuracy can be performed. In addition, since it is not necessary to use a power unit for generating gas, energy for operating such a power unit is unnecessary, and there is no generation of noise and vibration due to the power unit, and further, space saving is achieved. It has many advantages such as continuous gas-liquid separation operation.

[Brief description of the drawings]

FIG. 1 is an overall view showing a schematic configuration of a gas-liquid separation device according to the present invention.

FIG. 2 is a view schematically showing a cross section of a porous tube body containing a catalyst or an enzyme in the gas-liquid separation device shown in FIG.

[Explanation of symbols]

 Reference Signs List 12 porous tube 17 pore 18 manganese dioxide powder layer 19 manganese dioxide carrier D gas-liquid separator

──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. ⁷ , DB name) B01D 19/00 C02F 1/20

Claims (6)

(57) [Claims] 1. A chemical reaction medium, which chemically reacts with a liquid to be treated fed into the space to generate a gas, is provided in a space partitioned by a porous wall through which a liquid can pass. A gas-liquid separator characterized in that a separated liquid after removing gas generated by a medium is extracted and separated through the porous wall. 2. The gas-liquid separation device according to claim 1, wherein the chemical reaction medium is a catalyst. 3. The gas-liquid separation device according to claim 1, wherein the chemical reaction medium is an enzyme. 4. A process according to claim 1, wherein a porous wall partitioning said space is formed by a porous tubular body, and said chemical reaction medium is provided in said porous tubular body, and said processing object is fed into said porous tubular body. 2. The method according to claim 1, wherein a separated liquid obtained by removing a gas generated by the chemical reaction medium from the liquid is extracted to the outside of the porous tube through the porous wall of the porous tube. Gas-liquid separator. 5. A porous wall partitioning said space is formed by a porous tube, and said chemical reaction medium is provided around said porous tube, and is fed around said porous tube.
2. The method according to claim 1, wherein a separated liquid obtained by removing the gas generated by the chemical reaction medium from the liquid to be treated is extracted into the porous tube through the porous wall of the porous tube. The gas-liquid separation device described in the above item. 6. The gas-liquid separation apparatus according to claim 1, wherein a pressure at which the liquid to be treated is supplied is lower than a bubble point pressure of the porous wall.