KR101938850B1 - Method of manufacturing filtering meterials - Google Patents

Abstract

A method for producing a filter material is provided. A method of manufacturing a filter material according to an embodiment of the present invention includes the steps of preparing a porous support having a plurality of pores and using a weightless mixer to form a metal catalyst layer on the outer surface of the porous support and the surface exposed in the pores . According to this, the filtration efficiency, the adsorption efficiency, and the chemical impregnation efficiency can be improved, and the process can be simplified.

Description

Method of manufacturing filtering meterials < RTI ID = 0.0 >

The present invention relates to a method for producing a functional material, and more particularly, to a method for producing a filter material.

Since the porous material exhibits various properties such as molecular sieve, shape selectivity, adsorption property, stability and durability due to high specific surface area, high porosity, fluid permeability, regularity, uniform pore structure to volume, the filter material, the adsorption material, , Or chemical impregnation. In addition, porous materials have been recognized as key technologies for the development of materials and are recognized as important technologies of high added value.

A lot of research has been conducted on a technique for producing a pore-forming material for manufacturing such a porous material, and Korean Patent Publication No. 2000-0064574 is known as a prior art related to such a technique.

In the case of the above-mentioned patent documents, the carbonized carbon obtained by dry distillation is subjected to halogen treatment to produce a porous carbon material. The porous material manufacturing method of the patent document has a complicated process and a long process time. In addition, the porous carbon material has a disadvantage in that the filtration efficiency, the adsorption efficiency, and the chemical impregnation efficiency are low when applied to the filter material.

Patent Document: Korean Patent Publication No. 2000-0064574

SUMMARY OF THE INVENTION It is an object of the present invention to provide a method of manufacturing a filter material capable of improving filtration efficiency, adsorption efficiency, and chemical impregnation efficiency and simplifying the process .

In order to solve the above-described problems, the present invention provides a method for manufacturing a filter material. The method comprises: preparing a porous support having a plurality of pores; And forming a metal catalyst layer on the outer surface of the porous support and the surface exposed in the pores using a zero-gravity mixer.

The forming of the metal catalyst layer may include: spraying the metal catalyst layer forming solution on the porous support in the weightless mixer, and mixing the solution; And drying the porous support on which the metal catalyst layer-forming solution is sprayed.

The solution for forming a metal catalyst layer may include a solution for forming a first metal catalyst layer containing copper nitrate and manganese nitrate, a solution for forming a second metal catalyst layer containing sodium hydroxide (NaOH) And a third metal catalyst layer-forming solution containing potassium (K ₂ MnO ₄ ).

Also, the metal catalyst layer forming solution may be injected at a rate of 1 to 5 L / min.

The drying of the porous support on which the metal catalyst layer-forming solution is sprayed may be performed at a temperature of 100 to 200 ° C for 1 to 5 hours.

According to the production method of the filter material of the present invention, filtration efficiency, adsorption efficiency, chemical impregnation efficiency can be improved, and the process can be simplified.

1 is a flowchart showing a method of manufacturing a filter material according to an embodiment of the present invention.
2A to 2C are graphs showing the concentrations of acetaldehyde (a), toluene concentration (b), and formaldehyde (c) in Experimental Example 1 and Comparative Experimental Example 1 of the present invention.
3A and 3B are graphs showing changes in the concentrations of ammonia (a) and trimethylamine (b) in Experimental Example 2 and Comparative Experimental Example 2 of the present invention.
4 is a graph showing changes in hydrogen sulfide concentration in Experimental Example 3 and Comparative Experimental Example 3 of the present invention.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings, which will be readily apparent to those skilled in the art to which the present invention pertains. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. In order to clearly illustrate the present invention, parts not related to the description are omitted, and the same reference numerals are assigned to the same or similar components throughout the specification.

1 is a flowchart showing a method of manufacturing a filter material according to an embodiment of the present invention.

Referring to FIG. 1, a method of manufacturing a filter material according to an exemplary embodiment of the present invention includes preparing a porous support having a plurality of pores (S100), and applying a weightless mixer to the outer surface of the porous support and the pores And forming a metal catalyst layer on the exposed surface (S200).

The step of preparing the porous support (S100) will be described.

The porous support includes a plurality of pores and can be used without limitation in thermal or chemically stable materials, and can be activated carbon, clay, alumina, aluminosilicate, glass, or silica. The porous support may have any one of a pellet form and a granular form. The porous support has antibacterial properties as it contains activated carbon. In addition, by including a plurality of pores, foreign matter in the fluid can be filtered when the fluid to be filtered passes.

At this time, when the porous support is in the form of a pellet, it may have a spherical or cylindrical shape with a diameter ranging from 3 to 4 mm. If the diameter of the porous support pellet is less than 3 mm, formation of pores may be difficult. If it exceeds 4 mm, improvement in filtration efficiency, adsorption efficiency, and chemical impregnation efficiency may be limited when used as a filter material.

In addition, when the porous support is in a granular form, the size of the particles may be 20 to 40 mesh. When the size of the porous support granules is less than 20 mesh, improvement in filtration efficiency, adsorption efficiency, and chemical impregnation efficiency may be limited when used as a filter material, and formation of pores may be difficult if the size exceeds 40 mesh.

Also, the porous support may include 20 to 50% by volume of pores having an average diameter of 10 to 50 nm with respect to the total volume of the porous support. If the pores having a bacterial diameter of 10 to 50 nm are contained in an amount of less than 20% by volume based on the total volume of the porous support, permeability of fluid such as a gas or a liquid to be filtered may be lowered. If the pore size exceeds 50% When used as a filter material, improvement in filtration efficiency, adsorption efficiency, and chemical impregnation efficiency may be limited.

The porous support may be washed and dried before the metal catalyst layer is formed on the surface of the porous support. Washing and drying processes can be performed to improve the specific surface area due to the pore formation of the porous support. The washing may be performed using distilled water, and the drying process may be performed at a temperature of 100 to 150 ° C for 1 to 5 hours.

Next, a step S200 of forming a metal catalyst layer will be described.

First, a solution for forming a metal catalyst layer is sprayed on the porous support in a zero-gravity mixer and mixed. The non-gravity mixer can be used to form a non-gravity fluidized bed so that the metal catalyst layer can be uniformly coated to the outer surface of the porous support as well as to the surface exposed to the pores difficult to coat, Is maintained uniformly. Accordingly, it is possible to uniformly coat the surface of the pores to a surface of the pores in a shorter time than the conventional dip-coating and spray coating processes, and to suppress cracking of the coating layer by the drying process.

At this time, the metal catalyst layer forming solution may be a metal catalyst layer forming solution for inhibiting the generation of volatile organic compounds (VOCs) gas including copper nitrate and manganese nitrate, sodium hydroxide (NaOH) And a third metal catalyst layer-forming solution containing potassium manganate (K ₂ MnO ₄ ). Accordingly, it is possible to suppress the generation of various odor gases in the atmosphere, and to improve the filtration efficiency, the adsorption efficiency, and the chemical impregnation efficiency.

The first metal catalyst layer forming solution includes copper nitrate and manganese nitrate having a function capable of suppressing a volatile organic compound gas such as styrene, toluene, xylene, methyl ethyl ketone, or methyl isobutyl ketone. In this case, 0.1 to 1 part by weight of copper nitrate and 0.1 to 1 part by weight of nitric acid can be added to 100 parts by weight of the solvent. If the amount of copper nitrate is less than 0.1 part by weight based on 100 parts by weight of the solvent, the effect of inhibiting the generation of volatile organic compound gas may be limited. If the amount of copper nitrate is more than 1 part by weight, May be limited. If the amount of the manganese nitrate is less than 0.1 part by weight based on 100 parts by weight of the solvent, the effect of inhibiting the generation of volatile organic compounds may be limited. If the amount of the manganese nitrate is more than 1 part by weight, The rise may be limited.

The solvent used in the solution for forming a volatile organic compound gas generation-inhibiting metal catalyst layer may be any solvent that can dissolve copper nitrate and manganese nitrate, and may be water, for example, water.

The second metal catalyst layer forming solution includes sodium hydroxide (NaOH), which is a metal catalyst having an effect of removing amines such as trimethylamine or ammonia. The sodium hydroxide may include 0.1 to 1 part by weight based on 100 parts by weight of the solvent. If the sodium hydroxide is included in an amount of less than 0.1 part by weight based on 100 parts by weight of the solvent, the effect of removing the amine may be limited. If the amount of the sodium hydroxide is more than 1 part by weight, The solvent used in the second metal catalyst layer-forming solution may be any solvent that can dissolve sodium hydroxide, and may be water, for example, water.

The third metal catalyst layer forming solution includes potassium manganate (K ₂ MnO ₄ ) having an effect capable of removing a sulfide such as hydrogen sulfide, methyl sulfide, methyl disulfide, or methyl mercaptan. At this time, the potassium manganate may include 0.1 to 1 part by weight based on 100 parts by weight of the solvent. When the potassium manganate is contained in an amount of less than 0.1 part by weight based on 100 parts by weight of the solvent, the effect of removing the sulfide may be limited. When the amount of potassium manganate is more than 1 part by weight, the increase of the sulfide removal effect may be limited due to the increase of the potassium manganate content. The solvent used for the third metal catalyst layer-forming solution may be any solvent that can dissolve potassium manganate. For example, the solvent may be water.

The first metal catalyst layer forming solution, the second metal catalyst layer forming solution, and the third metal catalyst layer forming solution may be sequentially injected into the zero-gravity mixer and sprayed onto the porous support.

In this case, the metal catalyst layer forming solution may be injected at a rate of 1 to 5 L / min in the zero-gravity mixer. If the injection speed is less than 1 L / min, the process time may become longer, and if it exceeds 5 L / min, it may be difficult to form a uniform metal catalyst layer.

Also, the coating process time in the zero-gravity mixer may be 1 to 3 hours. If the coating process time is less than 1 hour, it may be difficult to form the metal catalyst layer to the inner surface of the pore, and if it exceeds 3 hours, it may become difficult to form a uniform metal catalyst layer.

Next, a step of drying the porous support on which the metal catalyst layer-forming solution is sprayed will be described.

The step of drying the porous support on which the metal catalyst layer-forming solution is sprayed may be performed at a temperature of 100 to 200 ° C for 1 to 5 hours.

If the drying temperature is less than 100 ° C, the metal catalyst layer is more likely to be damaged when the fluid passes through the produced filter material, and if the drying temperature exceeds 200 ° C, cracks may be generated in the metal catalyst layer. If the drying time is less than 1 hour, the metal catalyst layer is more likely to be damaged when the fluid passes through the manufactured filter material, and if the drying time exceeds 5 hours, the metal catalyst layer may be cracked.

Thus, the filter material produced by the method of manufacturing a filter material according to an embodiment of the present invention is coated with the metal catalyst layer to the surface of the porous support and the exposed pore surface in the porous support using a zero-gravity mixer. Thus, a filter material capable of improving filtration efficiency, adsorption efficiency, and chemical impregnation efficiency can be manufactured by including a metal catalyst layer having antibacterial and foreign matter filtration effect by the porous support and uniformly forming up to the inner surface of the pores . In addition, the process can be simplified.

In addition, the produced filter material can be applied to various filter products by mixing them at an appropriate ratio according to the application.

The present invention will now be described more specifically with reference to the following examples. However, the following examples should not be construed as limiting the scope of the present invention, and should be construed to facilitate understanding of the present invention.

< Preparation Example  1: Porous support>

A water repellency, a crushing strength of 70 N / cm or more, a specific gravity of 0.34 to 0.38 g / ml, a water adsorption of 90% or more, an iodine value of 950 or more, an abrasion of 95 or more, 20 g of pellets or granular porous supports having a pore size of not less than 740 m ² / g, a total pore volume of 0.48 cm ³ / g and an average particle size of 10 to 50 nm of 36% or more were washed with distilled water, Lt; 0 &gt; C for 3 hours.

< Preparation Example  2: Metal The catalyst layer  Forming solution &gt;

First metal catalyst layer forming solution: 5 g of copper nitrate and 5 g of manganese nitrate were mixed with 1 L of water to prepare a solution for forming a metal catalyst layer for inhibiting generation of volatile organic compound gas.

 Second metal catalyst layer forming solution: 5 g of sodium hydroxide was mixed with 1 L of water to prepare a solution for forming a metal catalyst layer for removing amines.

Third metal catalyst layer forming solution: 5 g of potassium manganate was mixed with 1 L of water to prepare a solution for forming a metal catalyst layer for removing sulfide.

< Example  >

The porous supports prepared in Preparation Example 1 were placed in a zero-gravity mixer, and the first metal catalyst layer forming solution prepared in Preparation Example 2 was added thereto, followed by mixing and spraying at a rate of 2 L / min. Thereafter, the second metal catalyst layer-forming solution prepared in Preparation Example 2 was added and mixed and sprayed at a rate of 2 L / min. Then, the third metal catalyst layer-forming solution prepared in Preparation Example 2 was added and mixed and sprayed at a rate of 2 L / min to prepare porous supports coated with the metal catalyst layer-forming solution. Then, the coated porous supports were dried for 3 hours at a temperature of 150 캜 using a hot-air drier to prepare a filter material.

Experimental Example  One : Volatile organic compounds  gassing Inhibition  Experiment

20 g of the filter material prepared in the above example was put into each of three reactors having a volume of 5 L and sealed. Thereafter, the initial concentration of the test gas was injected into a different reactor with acetaldehyde, 50 μmol / mol of toluene and 20 μmol / mol of formaldehyde, and the concentration of the test gas was measured at the initial (0 minute), 30 minute, 60 minute, 90 minute, Respectively. At this time, the concentration of the test gas was measured by a gas detection tube (formerly KS I 2218: 2009), and the gas concentration was measured after maintaining the test temperature at 23.0 ± 5.0 ° C. and the humidity at 50 ± 15% And Figs. 2 (a) to 2 (c).

Comparative Experimental Example  One

For the sake of comparison, experiments were conducted under the same conditions as in Experimental Example 1, except that a filter material was not put in the reactor and experiments for inhibiting the generation of volatile organic compound gases were carried out, and the results are shown in Table 1 and Figs.

At this time, the removal rate of the test gas for each time period was calculated by the following equation.

(Concentration of Comparative Experimental Example 1) - (concentration of Experimental Example 1) / (concentration of Comparative Experimental Example 1)}] 占 100

time
(minute) unit Test result Experimental Example 1 Concentration
(μmol / mol) Comparative Experiment Example 1 Concentration
(μmol / mol) The deodorization rate
(%) division Acetaldehyde
(Detection limit: 0.25 μmol / mol) 0 % 50 50 0 30 % <0.25 49 99.5 60 % <0.25 49 99.5 90 % <0.25 49 99.5 120 % <0.25 49 99.5 toluene
(Detection limit: 0.5 μmol / mol) 0 % 50 50 0 30 % 5 49 89.8 60 % 4 49 91.8 90 % 4 49 91.8 120 % 3 49 93.9 Formaldehyde
(Detection limit: 0.5 μmol / mol) 0 % 20 20 0 30 % 5 20 75 60 % 3 20 85 90 % 3 20 85 120 % 2 20 90

Referring to Table 1 and Figs. 2 (a) to (c) above, the filter material prepared according to one embodiment of the present invention has a maximum of 99.5%, 93.9, and 90% for each of volatile organic compound gases acetaldehyde, toluene, and formaldehyde %, Respectively.

As a result, it can be seen that the filter material according to an embodiment of the present invention is excellent in suppressing the generation of the volatile organic compound gas.

Experimental Example  2: Amines Removability  Experiment

20 g of the filter material prepared in the above example was placed in two reactors each having a volume of 5 L and sealed. Thereafter, the initial concentration of the test gas was injected into the different reactors at 50 μmol / mol of ammonia (NH ₃ ) and 50 μmol / mol of trimethylamine (CH ₃ ) ₃ N, , 60 minutes, 90 minutes and 120 minutes. At this time, the concentration of the test gas was measured by a gas detection tube (formerly KS I 2218: 2009), and the gas concentration was measured after maintaining the test temperature at 23.0 ± 5.0 ° C. and the humidity at 50 ± 15% And Figs. 3 (a) to 3 (b).

Comparative Experimental Example  2

For comparison, the experiment was carried out under the same conditions as in Experimental Example 2, except that the filter material was not put in the reactor, and an amine removal ability test was carried out, and the results are shown in Table 2 and Figs.

At this time, the removal rate of the test gas for each time period was calculated by the following equation.

(Concentration of Comparative Experiment 2) - (concentration of Experimental Example 2) / (concentration of Comparative Experiment 2)}] 占 100

time
(minute) unit
Test result
Experimental Example 2 Concentration
(μmol / mol) Comparative Experimental Example 2 Concentration
(μmol / mol) The deodorization rate
(%) division
ammonia
(Detection limit: 0.2 μmol / mol) 0 % 50 50 0 30 % 3 49 93.9 60 % 3 49 93.9 90 % 3 49 93.9 120 % 2 49 95.9 Trimethylamine
(Detection limit: 0.2 μmol / mol) 0 % 50 50 0 30 % 0.2 49 99.6 60 % 0.2 49 99.6 90 % 0.2 49 99.6 120 % 0.2 49 99.6

Referring to Table 2 and FIGS. 3 a to 3 b, it can be seen that the filter material prepared according to one embodiment of the present invention shows maximum deodorization rates of 95.9% and 99.6, respectively, with respect to amines ammonia and trimethylamine.

As a result, it can be seen that the filter material according to one embodiment of the present invention is excellent in removing effects on amines.

Experimental Example  3: Sulfide Removability  Experiment

20 g of the filter material prepared in the above example was placed in a reactor having a volume of 5 L and sealed. Then, the initial concentration of the test gas was injected into the different reactors at a concentration of 50 μmol / mo ℓ of hydrogen sulfide (H ₂ S) and the concentration of the test gas was measured at the initial (0 minute), 30 minute, 60 minute, 90 minute and 120 minute did. At this time, the concentration of the test gas was measured by a gas detection tube (formerly KS I 2218: 2009), and the gas concentration was measured after maintaining the test temperature at 23.0 ± 5.0 ° C. and the humidity at 50 ± 15% And FIG. 4, respectively.

Comparative Experimental Example  3

For comparison, the experiment was carried out under the same conditions as in Experimental Example 3, except that the filter material was not put in the reactor and the experiment for removing the sulfide was carried out, and the results are shown in Table 3 and FIG.

At this time, the removal rate of the test gas for each time period was calculated by the following equation.

(Concentration of Comparative Experiment 3) - (concentration of Experimental Example 3) / (concentration of Comparative Experiment 3)}] 占 100

time
(minute) unit Test result Experimental Example 3 Concentration
(μmol / mol) Comparative Experiment Example 3 Concentration
(μmol / mol) The deodorization rate
(%) Hydrogen sulfide (H ₂ S)
(Detection limit: 0.1 μmol / mol) 0 % 50 50 0 30 % 0.1 49 99.8 60 % 0.1 49 99.8 90 % 0.1 49 99.8 120 % 0.1 49 99.8

Referring to Table 3 and FIG. 4, it can be seen that the filter material prepared according to one embodiment of the present invention exhibits a deodorization rate of up to 99.8 with respect to hydrogen sulfide as a sulfide.

As a result, it can be seen that the filter material according to one embodiment of the present invention is excellent in the removal effect on the sulfide.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (5)

Preparing a porous support having a plurality of pores; And
Forming a metal catalyst layer on an outer surface of the porous support and a surface exposed in the pores using a zero-gravity mixer,
The forming of the metal catalyst layer may include: spraying and mixing the metal catalyst layer forming solution on the porous support in the zero-gravity mixer; And drying the porous support on which the metal catalyst layer forming solution is sprayed,
The solution for forming a metal catalyst layer may include a first metal catalyst layer forming solution including Cu-Nitrate and Mn-nitrate, a second metal catalyst layer forming solution including sodium hydroxide (NaOH) K ₂ MnO ₄ ) in the first metal catalyst layer forming solution. delete delete The method according to claim 1,
Wherein the metal catalyst layer forming solution is injected at a rate of 1 to 5 L / min. The method according to claim 1,
Wherein the step of drying the porous support on which the metal catalyst layer-forming solution is sprayed is performed at a temperature of 100 to 200 ° C for 1 to 5 hours.

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