WO2022071019A1 - 吸着フィルター - Google Patents

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Publication number
WO2022071019A1
WO2022071019A1 PCT/JP2021/034551 JP2021034551W WO2022071019A1 WO 2022071019 A1 WO2022071019 A1 WO 2022071019A1 JP 2021034551 W JP2021034551 W JP 2021034551W WO 2022071019 A1 WO2022071019 A1 WO 2022071019A1
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WO
WIPO (PCT)
Prior art keywords
adsorption filter
volume
activated carbon
adsorption
pore volume
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2021/034551
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English (en)
French (fr)
Japanese (ja)
Inventor
啓太 高橋
哲也 花本
寛枝 吉延
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kuraray Co Ltd
Original Assignee
Kuraray Co Ltd
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Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=80950349&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=WO2022071019(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Kuraray Co Ltd filed Critical Kuraray Co Ltd
Priority to US17/912,929 priority Critical patent/US20230149901A1/en
Priority to CN202180024815.1A priority patent/CN115335143B/zh
Priority to KR1020227032970A priority patent/KR20230078947A/ko
Priority to JP2022530282A priority patent/JP7180036B2/ja
Publication of WO2022071019A1 publication Critical patent/WO2022071019A1/ja
Priority to JP2022152814A priority patent/JP2022188136A/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2055—Carbonaceous material
    • B01D39/2058—Carbonaceous material the material being particulate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2055—Carbonaceous material
    • B01D39/2058—Carbonaceous material the material being particulate
    • B01D39/2062—Bonded, e.g. activated carbon blocks
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B01J20/28071—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being less than 0.5 ml/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials

Definitions

  • the present invention relates to an adsorption filter made of a molded body containing activated carbon and a binder.
  • an adsorption filter made of an activated carbon molded body is generally used.
  • Patent Document 1 discloses a method for manufacturing a turbidity-reducing filter body that can be used for a longer period of time by adjusting the hardness difference between the inflow filter material portion and the outflow filter medium portion of the activated carbon molded body.
  • Patent Document 2 discloses a water purification cartridge provided with an activated carbon molded body and a non-woven fabric, which can achieve both high turbidity removing performance and a sufficiently long clogging life.
  • Patent Document 3 describes the powdered activated carbon (a) and the fibrous binder (b) having a central particle size of 80 ⁇ m to 120 ⁇ m and a standard deviation ⁇ g of 1.3 to 1.9 in the particle size distribution.
  • the activated carbon molded product obtained by molding a mixture containing the above is disclosed. According to the activated carbon molded product of Patent Document 3, it is described that it is excellent in the ability to remove free residual chlorine, volatile organic compounds, CAT and 2-MIB, and is also excellent in turbidity filtration ability.
  • An object of the present invention is to provide an adsorption filter having excellent ultrafine particle removing performance while maintaining good water permeability.
  • the present inventors have reached the present invention as a result of diligent studies to solve the above problems.
  • the adsorption filter according to the aspect of the present invention is an adsorption filter made of a molded body containing activated carbon and a binder.
  • the pore volume having a pore diameter of 10 ⁇ m or more based on the volume of the adsorption filter measured by the mercury intrusion method is 0.10 cm 3 / cc to 0.39 cm 3 / cc.
  • the adsorption filter according to a further aspect of the present invention is an adsorption filter made of a molded body containing activated carbon and a binder.
  • the pore volume with a pore diameter of 7 ⁇ m or less based on the volume of the adsorption filter measured by the mercury intrusion method is 0.15 cm 3 / cc or more, and
  • the total pore volume of the adsorption filter measured by the mercury intrusion method on a volume basis is 0.50 cm 3 / cc to 0.73 cm 3 / cc.
  • FIG. 1 shows a perspective view showing an example of a mold for preparing an adsorption filter according to the present embodiment.
  • FIG. 2 is a perspective view showing an example of an adsorption filter in the present embodiment obtained by using the mold of FIG. 1.
  • FIG. 3 is a diagram illustrating a method of cutting a sample when measuring the pore volume and the pore mode diameter of the adsorption filter.
  • FIG. 4 is a diagram illustrating a method of cutting a measurement sample at the time of measuring the particle size distribution of activated carbon (carbide after heat treatment) in the adsorption filter.
  • FIG. 5 is a perspective view showing an example of an automatic grinder for manufacturing an adsorption filter.
  • FIG. 1 shows a perspective view showing an example of a mold for preparing an adsorption filter according to the present embodiment.
  • FIG. 2 is a perspective view showing an example of an adsorption filter in the present embodiment obtained by using the mold of FIG. 1.
  • FIG. 3 is a diagram illustrating
  • FIG. 6 is a graph showing the pore mode diameter of the adsorption filter and the section pore volume thereof.
  • FIG. 7 is a diagram showing the correlation between the pore volume of the adsorption filter having a pore diameter of 10 ⁇ m or more and the ultrafine particle removing performance.
  • FIG. 8 is a diagram showing the correlation between the pore volume of the adsorption filter having a pore diameter of 7 ⁇ m or less and the ultrafine particle removing performance.
  • the activated carbon molded bodies of Patent Document 1, Patent Document 2 and Patent Document 3 described above have been evaluated for their turbidity removing performance.
  • the turbidity removal performance test performed on the filter of the activated carbon molded body is specified by, for example, JIS S3201: 2019, and in the test, kaolin of about 1 ⁇ m to 20 ⁇ m is turbid component (particulate matter). ), And evaluate its removal performance.
  • the turbidity removing performance is evaluated based on the test.
  • the adsorption filter made of an activated carbon molded body is required to have the ability to remove fine particles (generally, a particle size of 1 ⁇ m to 20 ⁇ m) and ultrafine particles having a particle size of 1 ⁇ m or less. I'm starting.
  • the activated carbon molded body includes a wet molded body and a dry molded body depending on the manufacturing method thereof.
  • the wet molded body tends to have a relatively low density and low water flow resistance, and is also excellent in removing organic compounds and the like, which are generally considered to be harmful. However, due to its low density and low water flow resistance, it is expected that it will be difficult to have the ability to remove even ultrafine particles.
  • the dry molded body has a higher density than the wet molded body. Therefore, although it can be expected to have ultrafine particle removing performance, it becomes unsuitable for applications such as a water purification filter because the water flow resistance becomes high. Therefore, there is a demand for an adsorption filter made of an activated carbon molded body that can achieve both low water flow resistance and ultrafine particle removal performance.
  • the adsorption filter in the present embodiment is an adsorption filter made of a molded body containing activated carbon and a binder, and has a pore volume of 10 ⁇ m or more based on the volume of the adsorption filter measured by the mercury intrusion method. It is 10 cm 3 / cc to 0.39 cm 3 / cc.
  • the adsorption filter in the other embodiment is an adsorption filter made of a molded body containing activated carbon and a binder, and has a fine pore diameter of 7 ⁇ m or less based on the volume of the adsorption filter measured by the mercury intrusion method.
  • the pore volume is 0.15 cm 3 / cc or more, and the total pore volume of the adsorption filter measured by the mercury intrusion method based on the volume is 0.50 cm 3 / cc to 0.73 cm 3 / cc. ..
  • the void volume in the filter is appropriately controlled, and the pore volume at a predetermined pore diameter or more is specified. Adjust so that it is within the range. As a result, both water permeability and ultrafine particle removing performance can be achieved at the same time.
  • the adsorption filter in the present embodiment has a pore volume of 10 ⁇ m or more based on the volume of the adsorption filter measured by the mercury intrusion method (hereinafter, also simply referred to as “pore volume of 10 ⁇ m or more”). It is 0.10 cm 3 / cc to 0.39 cm 3 / cc.
  • pore volume of 10 ⁇ m or more By setting the pore volume of the pore diameter of 10 ⁇ m or more to 0.10 cm 3 / cc or more, good water permeability can be maintained in the adsorption filter of the present embodiment.
  • the adsorption filter in the present embodiment is remarkably excellent in the ultrafine particle removing performance.
  • the pore volume having a pore diameter of 10 ⁇ m or more is preferably 0.37 cm 3 / cc or less, more preferably 0.35 cm 3 / cc or less, and further preferably 0.33 cm 3 / cc or less.
  • the pore volume having a pore diameter of 10 ⁇ m or more is preferably 0.12 cm 3 / cc or more, and more preferably 0.15 cm 3 / cc or more.
  • the adsorption filter in the present embodiment preferably has a total pore volume (hereinafter, also simply referred to as “total pore volume”) of 0.50 cm 3 / based on the volume of the adsorption filter measured by the mercury intrusion method. It is cc to 0.73 cm 3 / cc.
  • total pore volume By setting the total pore volume to 0.50 cm 3 / cc or more, the adsorption filter can obtain more excellent water permeability, and can be suitably used for applications such as a water purification filter.
  • the total pore volume By setting the total pore volume to 0.73 cm 3 / cc or less, a sufficient amount of activated carbon can be retained, and the adsorption performance as a general filter can be improved.
  • the total pore volume is more preferably 0.53 cm 3 / cc or more, still more preferably 0.56 cm 3 / cc or more.
  • the total pore volume is more preferably 0.70 cm 3 / cc or less, still more preferably 0.67 cm 3 / cc or less.
  • the adsorption filter in the other embodiment is a pore volume having a pore diameter of 7 ⁇ m or less based on the volume of the adsorption filter measured by the mercury intrusion method (hereinafter, simply “pore volume having a pore diameter of 7 ⁇ m or less”.
  • pore volume having a pore diameter of 7 ⁇ m or less (Also referred to as) is 0.15 cm 3 / cc or more, and the total pore volume is 0.50 cm 3 / cc to 0.73 cm 3 / cc.
  • the adsorption filter can maintain good water permeability and is adsorbed as a general filter. Performance can be improved.
  • the pore volume having a pore diameter of 7 ⁇ m or less is preferably 0.16 cm 3 / cc or more, more preferably 0.17 cm 3 / cc or more, and further preferably 0.18 cm 3 / cc or more.
  • the upper limit of the pore volume having a pore diameter of 7 ⁇ m or less is not particularly limited, but for example, the pore volume having a pore diameter of 7 ⁇ m or less is preferably 0.30 cm 3 / cc or less, more preferably 0.28 cm 3 /. It is cc or less.
  • the preferable upper limit value and lower limit value of the total pore volume in the adsorption filter of the other embodiment are the same as those of the adsorption filter in the above-described embodiment.
  • the adsorption filter has a pore volume of 0.10 cm 3 / cc to 0.39 cm 3 / cc having a pore diameter of 10 ⁇ m or more, and in addition, the adsorption filter has a pore diameter of 7 ⁇ m or less. It is preferable that the pore volume is 0.15 cm 3 / cc or more and the total pore volume is 0.50 cm 3 / cc to 0.73 cm 3 / cc. In other words, it is preferable that the adsorption filter satisfies both conditions defined in the above two embodiments.
  • the ratio of the pore volume having a pore diameter of 10 ⁇ m or more to the total pore volume is preferably 12% or more.
  • the ratio of the pore volume having a pore diameter of 10 ⁇ m or more is more preferably 15% or more, still more preferably 20% or more, particularly preferably 25% or more, and most preferably 30% or more.
  • the ratio of the pore volume having a pore diameter of 10 ⁇ m or more is preferably 80% or less, more preferably 65% or less, and further preferably 60% or less.
  • the ratio of the pore volume having a pore diameter of 7 ⁇ m or less to the total pore volume is preferably 22% or more.
  • the adsorption filter can obtain more excellent ultrafine particle removing performance.
  • the ratio of the pore volume having a pore diameter of 7 ⁇ m or less is more preferably 25% or more.
  • the ratio of the pore volume having a pore diameter of 7 ⁇ m or less is preferably 48% or less, more preferably 45% or less.
  • the adsorption filter in the present embodiment preferably has a pore mode diameter (hereinafter, also simply referred to as “pore mode diameter”) measured by the mercury intrusion method of 15 ⁇ m or less.
  • pore mode diameter measured by the mercury intrusion method
  • the pore mode diameter is more preferably 13 ⁇ m or less, still more preferably 11 ⁇ m or less.
  • the lower limit of the pore mode diameter is not particularly limited, but it is sufficient that the pore mode diameter becomes extremely small and does not significantly affect the water permeability of the filter.
  • the pore mode diameter is preferably 6 ⁇ m or more, more preferably 7 ⁇ m or more.
  • the pore volume having a pore diameter of 10 ⁇ m or more, the pore volume having a pore diameter of 7 ⁇ m or less, the total pore volume, and the pore mode diameter measured by the mercury intrusion method will be described in later examples.
  • the measurement can be performed using a mercury intrusion method pore volume measuring device (“MicroActive AutoPore V 9620” manufactured by Micromeritics Co., Ltd.). Further, from the measured values of these pore volumes, the ratio (%) of the pore volume having a pore diameter of 10 ⁇ m or more to the total pore volume and the ratio (%) of the pore volume having a pore diameter of 7 ⁇ m or less to the total pore volume. ) Can be obtained.
  • the molded layer of the filter is a measurement sample having a size of about 1 cm square, but it is preferable that the size of this measurement sample is appropriately changed depending on the filter size. For example, in the case of a spout-in type filter, it is desirable to measure with a measurement sample of about 5 mm square.
  • the pore volume having a pore diameter of 10 ⁇ m or more, the pore volume having a pore diameter of 7 ⁇ m or less, the total pore volume, and the pore mode diameter have their values by various methods. Can be controlled. By controlling the value of the pore volume, at the same time, the ratio of the pore volume having a pore diameter of 10 ⁇ m or more to the total pore volume and the ratio of the pore volume having a pore diameter of 7 ⁇ m or less to the total pore volume are also controlled. can do.
  • the physical properties of the raw material activated carbon and its blending amount when two or more types of activated carbon with different physical properties are used, their blending ratio, the type of raw material binder and its blending amount, the blending amount of any component of the raw material, the adsorption filter.
  • the value can be controlled by appropriately selecting and appropriately adjusting the treatment conditions (suction pressure, drying time, etc.) and the like in the production of the above.
  • a pore volume having a pore diameter of 10 ⁇ m or more, a pore volume having a pore diameter of 7 ⁇ m or less, a total pore volume and fineness can be used. It is preferable to control the value of the hole mode diameter.
  • the density of the adsorption filter (hereinafter, also simply referred to as “filter density”) in the present embodiment is preferably 0.59 g / cm 3 or less.
  • the filter density is 0.59 g / cm 3 or less, the water flow resistance can be kept better, and for example, it can be suitably used for a water purification filter or the like. In addition, clogging of the filter can be suppressed.
  • the filter density is preferably 0.35 g / cm 3 or more. When the filter density is 0.35 g / cm 3 or more, the total amount of activated carbon becomes a suitable amount, and the removal performance of ultrafine particles and other ordinary harmful substances can be kept good.
  • the filter density is more preferably 0.38 g / cm 3 or more, further preferably 0.40 g / cm 3 or more, and particularly preferably 0.42 g / cm 3 or more.
  • the filter density is more preferably 0.57 g / cm 3 or less, further preferably 0.55 g / cm 3 or less, and particularly preferably 0.53 g / cm 3 or less.
  • the filter density can be measured by the methods described in detail in later examples.
  • the value of the filter density can be controlled by various methods. For example, the physical properties of the raw material activated carbon and its blending amount, when two or more types of activated carbon with different physical properties are used, their blending ratio, the type of raw material binder and its blending amount, the blending amount of any component of the raw material, the adsorption filter.
  • the value can be controlled by appropriately selecting and appropriately adjusting the treatment conditions (suction pressure, drying time, etc.) and the like in the production of the above.
  • the adsorption filter in this embodiment preferably has a benzene saturated adsorption amount of 18% to 35%.
  • the benzene saturated adsorption amount of the adsorption filter conforms to the activated carbon test method of JIS K 1474: 2014, and at 25 ° C., the mass is passed through air containing solvent vapor which is 1/10 of the solvent saturation concentration. It can be obtained from the increase (%) of the sample when it becomes constant.
  • the benzene saturated adsorption amount is 18% or more, sufficient removal performance especially for organic substances can be obtained.
  • the benzene saturated adsorption amount is 35% or less, it is possible to prevent the pore diameter from increasing in the overactivated state, and it is possible to suppress the possibility that the adsorption retention capacity of harmful substances is reduced.
  • the benzene saturated adsorption amount is more preferably 20% or more, still more preferably 22% or more.
  • the saturated benzene adsorption amount is more preferably 33% or less, still more preferably 30% or less.
  • the benzene saturated adsorption amount of the adsorption filter in the present embodiment for example, the physical properties of the activated carbon as a raw material and the blending amount thereof, and when two or more kinds of activated carbons having different physical properties are used, the blending ratio thereof and the like are appropriately selected and appropriately adjusted. By doing so, the value can be controlled.
  • the carbide obtained by heat-treating the adsorption filter in the present embodiment at 900 ° C. for 20 minutes has a particle size of 10 ⁇ m or less.
  • the particle content is preferably 2% by volume or more.
  • the adsorption filter by subjecting the adsorption filter to such a heat treatment, components such as a binder are removed from the adsorption filter, and activated carbon in the adsorption filter remains as carbide.
  • the adsorption filter in the present embodiment before the heat treatment is more excellent. It has the ability to remove ultrafine particles.
  • the particle content of activated carbon (carbide after heat treatment) in the adsorption filter having a particle diameter of 10 ⁇ m or less is more preferably 4% by volume or more, still more preferably 6% by volume or more.
  • the upper limit of the particle content of the activated carbon having a particle diameter of 10 ⁇ m or less in the adsorption filter is not limited, but the particle size may not significantly affect the water permeability of the adsorption filter in the present embodiment before the heat treatment because the particle size is extremely small. .. For example, it may be 10% by volume or less.
  • the particle content of activated carbon (carbide after heat treatment) in the adsorption filter with a particle size of 10 ⁇ m or less mainly depends on the physical properties of the raw material activated carbon and the blending ratio of two or more types of activated carbon with different physical properties. It is a value that changes. Therefore, their values can be controlled by appropriately selecting and adjusting them appropriately.
  • the adsorption filter in the present embodiment has a 0% particle size (hereinafter, also simply referred to as “D0”) of 7 ⁇ m or less in the volume-based cumulative particle size distribution of the activated carbon (carbide after heat treatment) in the adsorption filter. preferable.
  • D0 0% particle size
  • the adsorption filter in the present embodiment before the heat treatment has more excellent ultrafine particle removing performance.
  • the D0 of activated carbon (carbide after heat treatment) in the adsorption filter is more preferably 5 ⁇ m or less, still more preferably 3 ⁇ m or less.
  • the lower limit of D0 is not limited, but it does not have a great influence on the water permeability of the adsorption filter before the heat treatment. For example, it may be 1 ⁇ m or more.
  • D0 of the activated carbon (carbide after heat treatment) in the adsorption filter is also a value that mainly changes according to the compounding ratio of the activated carbon as a raw material and when two or more types of activated carbon having different physical characteristics are used. Therefore, their values can be controlled by appropriately selecting and adjusting them appropriately.
  • the particle content of the activated carbon (carbonized material after heat treatment) in the adsorption filter having a particle diameter of 10 ⁇ m or less and the D0 of the activated carbon (carbonized material after heat treatment) in the adsorption filter are as described in the later examples. Similar to activated carbon as a normal raw material, it can be measured by a laser diffraction / scattering method using, for example, a wet particle size distribution measuring device (“Microtrac MT3300EX-II” manufactured by Microtrac Bell).
  • the adsorption filter in this embodiment is made of a molded body containing activated carbon and a binder.
  • the activated carbon (preferably granular activated carbon) as a raw material used for the adsorption filter in the present embodiment is not particularly limited, and can be used alone or in combination of two or more types of activated carbon having different physical characteristics.
  • the physical properties of the active charcoal as a raw material include, for example, the packing density of the activated charcoal (g / cm 3 ), the 10% particle size in the volume-based cumulative particle size distribution (hereinafter, also simply referred to as “D10”), and the volume-based cumulative particle size distribution.
  • D10 the 10% particle size in the volume-based cumulative particle size distribution
  • D90 90% particle size in the volume-based cumulative particle size distribution
  • the voids can be controlled when the adsorption filter is molded by adjusting the blending ratio of activated carbon having different physical characteristics, and the pore volume (and / or the pore diameter of 7 ⁇ m or less) having a pore diameter of 10 ⁇ m or more can be controlled. This is because the pore volume and the total pore volume) can be easily adjusted to be within the specific range defined in the present embodiment.
  • the activated carbon having different physical characteristics examples include powdered activated carbon X having smaller D10, D50 and / or D90 and containing a large amount of fine powder, and powdered activated carbon Y having larger D10, D50 and / or D90. It is preferable to use it in combination.
  • the activated carbon Y is formed by the activated carbon Y when molding the adsorption filter by using the activated carbon Y in combination with the activated carbon X at a mass ratio larger than the same level. Voids that are too large are properly filled with fine powder of activated carbon X.
  • the voids of the molded body are appropriately controlled, and the pore volume having a pore diameter of 10 ⁇ m or more (and / or the pore volume having a pore diameter of 7 ⁇ m or less and the total pore volume) is specified in the present embodiment. It is adjusted within the range of.
  • the particle size distribution of the raw material activated carbon is not particularly limited, but it is preferable that the content of particles having a particle diameter of 10 ⁇ m or less is more than 2% by volume. Specifically, in the particle size distribution of the activated carbon as a raw material, since the content of particles having a particle size of 10 ⁇ m or less is more than 2% by volume, the amount of fine powder contained in the activated carbon in the adsorption filter increases. The filter exhibits better ultrafine particle removal performance. When two or more types of activated carbon are used in combination, the particle content of the raw material activated carbon having a particle diameter of 10 ⁇ m or less varies depending on the physical characteristics of each activated carbon and the blending ratio of each activated carbon. Therefore, their values can be controlled by appropriately selecting and adjusting them appropriately.
  • the particle content of the activated carbon as a raw material having a particle diameter of 10 ⁇ m or less is more preferably 3% by volume or more, further preferably 4% by volume or more, still more preferably 5% by volume or more.
  • the upper limit of the particle content of the activated carbon as a raw material having a particle diameter of 10 ⁇ m or less is not limited, but the fine powder contained in the activated carbon in the adsorption filter becomes excessive, which should not greatly affect the water permeability of the molded adsorption filter. Just do it. For example, it may be 15% by volume or less.
  • the filling densities of the activated carbon as raw materials, D10, D50 and D90 are, for example, the types of carbonaceous materials used as raw materials for activated carbon described later, and the activation treatment method and treatment of the carbonic material in the production of activated carbon.
  • the values can be controlled by appropriately selecting and appropriately selecting the conditions (heating temperature and time, etc.), pulverization conditions and classification conditions.
  • the particle content of D10, D50 and D90, and the activated carbon as a raw material having a particle diameter of 10 ⁇ m or less as described in later examples, for example, a wet particle size distribution measuring device (manufactured by Microtrac Bell, Inc., “Microtrac”). It can be analyzed and measured by a laser diffraction / scattering method using MT3300EX-II ”) or the like.
  • activated carbon obtained by carbonizing a carbonaceous material that is a raw material of activated carbon as necessary, then activating it, and if necessary, performing a washing treatment, a drying treatment, and a crushing treatment. It can also be used.
  • the carbonaceous material used as a raw material is not particularly limited, but for example, a plant-based carbonaceous material (for example, wood, shavings, coal, fruit husks such as coconut husks and walnut husks, fruit seeds, pulp production by-products, lignin, etc.
  • a plant-based carbonaceous material for example, wood, shavings, coal, fruit husks such as coconut husks and walnut husks, fruit seeds, pulp production by-products, lignin, etc.
  • Plant-derived materials such as waste sugar honey), mineral-based carbonaceous materials (eg, mineral-derived materials such as peat, sub-charcoal, brown charcoal, bituminous charcoal, smokeless charcoal, coke, coal tar, coal pitch, petroleum distillation residue, petroleum pitch), Synthetic resin-based carbonaceous materials (for example, materials derived from synthetic resins such as phenol resin, polyvinylidene chloride, acrylic resin), natural fiber-based carbonaceous materials (for example, natural fibers such as cellulose, recycled fibers such as rayon, etc.) Material derived from fiber) and the like. These carbonaceous materials may be used alone or in combination of two or more.
  • mineral-based carbonaceous materials eg, mineral-derived materials such as peat, sub-charcoal, brown charcoal, bituminous charcoal, smokeless charcoal, coke, coal tar, coal pitch, petroleum distillation residue, petroleum pitch
  • Synthetic resin-based carbonaceous materials for example, materials derived from synthetic resins such as phenol resin, polyvinylidene chlor
  • coconut shells or phenolic resins are preferable from the viewpoint that micropores involved in the volatile organic compound removal performance specified in JIS S3201: 2019 are likely to develop.
  • these carbonaceous materials are usually subjected to, for example, 400 ° C. to 800 ° C., preferably 500 ° C. to 800 ° C., and more preferably 550 ° C. in an environment where oxygen or air is shielded.
  • the carbonization treatment can be performed at about 750 ° C. After that, the particle size may be adjusted if necessary.
  • the activation treatment is a treatment in which pores are formed on the surface of a carbonaceous material and converted into activated carbon which is a porous body.
  • the activation treatment can be carried out by a method general in the art, and is not particularly limited, and mainly includes two types of treatment methods, gas activation treatment and drug activation treatment. Of these, when used for water purification treatment, gas activation treatment is preferable from the viewpoint of residual impurities.
  • the gas activation treatment is a treatment for heating a carbonaceous material in the presence of, for example, water vapor, carbon dioxide, air, oxygen, combustion gas, or a mixed gas thereof.
  • the heating temperature is not particularly limited, but is, for example, 700 ° C. to 1100 ° C., preferably 800 ° C. to 980 ° C., and more preferably 850 ° C. to 950 ° C.
  • the activation time and the rate of temperature rise are not particularly limited, and may be appropriately adjusted according to the type, shape, and size of the carbonaceous material to be selected. Considering safety and reactivity, it is preferable to use a water vapor-containing gas containing 10% by volume to 40% by volume of water vapor.
  • an activator such as zinc chloride, calcium chloride, phosphoric acid, sulfuric acid, sodium hydroxide, potassium hydroxide, magnesium hydroxide, calcium hydroxide is mixed with a carbonaceous material to create an inert gas atmosphere. It may be carried out by a known method of heating below.
  • Activated carbon after activation treatment is washed and dried as necessary.
  • a plant-based carbonaceous material such as coconut shell or a mineral-based carbonaceous material containing impurities such as alkali metal, alkaline earth metal and transition metal is used as a raw material for activated carbon, ash and chemicals are removed. Clean as needed. Mineral acid or water is used for cleaning, and hydrochloric acid having high cleaning efficiency is preferable as the mineral acid.
  • the activated carbon after the activation treatment is pulverized and / or classified as necessary.
  • the crushing treatment is performed using a crushing device generally used for crushing activated carbon, for example, a high-speed rotary mill such as an erotic fall mill, a rod mill, a roller mill, a hammer mill, a blade mill, a pin mill, a ball mill, a jet mill, or the like.
  • a crushing device generally used for crushing activated carbon
  • a high-speed rotary mill such as an erotic fall mill, a rod mill, a roller mill, a hammer mill, a blade mill, a pin mill, a ball mill, a jet mill, or the like.
  • the classification treatment include methods generally used for classification of activated carbon, for example, classification using a sieve, wet classification, and dry classification.
  • the wet classifier include classifiers that utilize principles such as gravity classification, inertial classification, hydraulic classification, and centrifugal classification.
  • the dry classifier include classifiers
  • the shape of the activated carbon obtained through such treatment or the commercially available activated carbon may be any of powder, particle, fibrous (thread-like, woven cloth (cloth) -like, felt-like) and the like, and may be appropriately used depending on the intended use. You can choose. Of these shapes, a powder with high adsorption performance per volume is preferable.
  • the binder used for the adsorption filter in the present embodiment is not particularly limited, and a binder having a powdery or fibrous shape can be used alone or in combination of two or more. Of these, it is preferable to include a fibrous binder from the viewpoint of excellent water permeability when the adsorption filter is molded.
  • the fibrous binder is not particularly limited as long as it can be shaped by entwining activated carbon, and can be widely used regardless of whether it is a synthetic product or a natural product.
  • a binder include acrylic fiber, polyethylene fiber, polypropylene fiber, polyacrylonitrile fiber, cellulose fiber, nylon fiber, aramid fiber, pulp and the like.
  • the fiber length of the fibrous binder is preferably 4 mm or less.
  • the fibrous binder contains an acrylic fibrous binder. Further, it is more preferable that the fibrous binder contains a cellulosic fibrous binder. Further, these fibrous binders may be used in combination of two or more. For example, it is more preferable to use both an acrylic fibrous binder and a cellulosic fibrous binder in combination. By using a cellulosic fibrous binder in combination, it is possible to reduce the outflow of fine powder from the adsorption filter in the present embodiment.
  • the blending ratio of the acrylic fibrous binder and the cellulose-based fibrous binder is such that the cellulose-based fibrous binder is preferably 30 parts by mass to 70 parts by mass, more preferably 40 parts by mass with respect to 100 parts by mass of the acrylic fibrous binder. It is a mass part to 60 parts by mass.
  • the water permeability of the fibrous binder is preferably about 1 mL to 200 mL in terms of CSF value.
  • the CSF value is more preferably 10 mL to 150 mL.
  • the CSF value is a value measured with reference to the "Pulp drainage test method" Canadian standard freeness method specified in JIS P 8121: 2012. Specifically, in the measurement, the value is set to be evaluated using tap water having a conductivity of about 100 ⁇ s / cm. The CSF value can be adjusted, for example, by making the binder fibril.
  • the CSF value of the fibrous binder is 1 mL or more, sufficient water permeability can be maintained, a decrease in the strength of the molded body can be suppressed, and a risk of pressure loss can be prevented. Further, when the CSF value is 200 mL or less, the powdered activated carbon can be sufficiently retained, the decrease in the strength of the molded body can be suppressed, and the possibility that the adsorption performance can be deteriorated can be prevented.
  • two or more kinds of fibrous binders are used in combination, it is preferable that the CSF value in a state where two or more kinds of fibrous binders are mixed satisfies the above range.
  • the CSF value of the acrylic fibrous binder is preferably 20 mL or more, more preferably 50 mL or more.
  • the CSF value of the acrylic fibrous binder is preferably 200 mL or less, more preferably 150 mL or less.
  • the cellulosic fibrous binder is the cellulose fibrous binder with respect to 100 parts by mass of the acrylic fibrous binder.
  • the CSF value in the state of blending 50 parts by mass is preferably 1 mL or more, and more preferably 10 mL or more.
  • the cellulose-based fibrous binder preferably has a CSF value of 50 mL or less, preferably 40 mL or less, in a state where 50 parts by mass of the cellulose-based fibrous binder is blended with 100 parts by mass of the acrylic fibrous binder. Is more preferable.
  • the blending ratio of the activated carbon and the binder is not particularly limited, and when the adsorption filter is molded, the pore volume having a pore diameter of 10 ⁇ m or more (and / or the pore volume having a pore diameter of 7 ⁇ m or less and the total pore volume) is not particularly limited. ) May be appropriately set so as to be within the specific range specified in the present embodiment.
  • the amount is preferably about 3 parts by mass to 8 parts by mass of the binder with respect to 100 parts by mass of activated carbon.
  • a molded body of an adsorption filter having sufficient strength can be obtained.
  • the amount of the binder By setting the amount of the binder to 8 parts by mass or less, it is possible to suppress the deterioration of the adsorption performance of the activated carbon in the adsorption filter.
  • the mixing ratio of the binder to 100 parts by mass of activated carbon is more preferably 4 parts by mass or more, and further preferably 5 parts by mass or more.
  • the mixing ratio of the binder to 100 parts by mass of activated carbon is more preferably 7 parts by mass or less, still more preferably 6 parts by mass or less.
  • the adsorption filter in the present embodiment may contain any other functional component as long as the effect of the present invention is not impaired.
  • a zeolite powder lead adsorbent
  • ion exchange resin a chelate resin and the like
  • various adsorbents containing silver ions or silver compounds may be contained alone or in combination of two or more.
  • silver-impregnated activated carbon added in an amount that does not affect the physical properties of the adsorption filter in the present embodiment can be mentioned.
  • the blending amount of these other optional components is not particularly limited, but when the adsorption filter is molded, the pore volume having a pore diameter of 10 ⁇ m or more (and / or the pore volume having a pore diameter of 7 ⁇ m or less) and the total fineness.
  • the hole volume may be appropriately set so as to be within the specific range specified in the present embodiment. For example, 1 part by mass to 20 parts by mass can be blended with respect to 100 parts by mass of the entire adsorption filter.
  • the adsorption filter made of a molded body containing activated carbon and a binder in the present embodiment further contains a core, and may be a cylindrical adsorption filter.
  • the cylindrical shape can reduce the water flow resistance. Further, when the cartridge is used as a cartridge by filling the housing as described later, there is an advantage that the cartridge can be easily loaded and replaced in the water purifier.
  • the core is not particularly limited as long as it is inserted into the hollow portion of the cylindrical adsorption filter and can reinforce the cylindrical adsorption filter.
  • a trical pipe, a netron pipe, a ceramic filter and the like can be mentioned.
  • a non-woven fabric or the like can be wrapped around the outer circumference of the core for use.
  • the method for producing the adsorption filter in the present embodiment may be performed by any method known to those skilled in the art, and is not particularly limited.
  • the slurry suction method is preferable from the viewpoint of efficient production.
  • the manufacturing method is not limited to the manufacturing method.
  • the cylindrical adsorption filter (molded body) in the present embodiment has a slurry preparation step, a suction filtration step, a rolling step if necessary, a drying step, and a grinding step if necessary. It can be manufactured by a method including.
  • a slurry preparation step powdered activated carbon and a fibrous binder are dispersed in water to prepare a slurry.
  • the suction filtration step the prepared slurry is suctioned and filtered to obtain a preformed body.
  • the shape of the outer surface is adjusted as necessary by compressing the preformed body after suction filtration on a shaping table.
  • the drying step the preformed body having been shaped is dried to obtain a dried molded body.
  • the outer surface of the dried molded body is ground as needed.
  • the powdered activated carbon and the fibrous binder are used, for example, the fibrous binder is 4 parts by mass to 8 parts by mass with respect to 100 parts by mass of the powdered activated carbon, and the solid content concentration is 0.1.
  • a slurry dispersed in a solvent is prepared so as to be in an amount of 10% by mass to 10% by mass, preferably 1% by mass to 5% by mass.
  • the solvent is not particularly limited, but it is preferable to use water or the like.
  • the molding time can be shortened and the productivity can be improved. Further, it is possible to prevent the density of the molded body from becoming too high, and to maintain good water permeability.
  • each reference numeral represents a mold 1, a core body 2, a suction hole 3, flanges 4, 4', and a filtrate discharge port 5.
  • a large number of suction holes 3 are provided on the surface of the core body 2, flanges 4 and 4'are attached to both ends, and a filtrate discharge port 5 is provided.
  • the mold 1 for the cylindrical molded body is used.
  • the core as described above is attached to the mold 1, placed in the prepared slurry, and filtered while being sucked from the inside of the mold 1 from the filtrate discharge port 5 to attach the slurry to the mold 1.
  • a conventional method for example, a method of suction using a suction pump or the like can be used. In this way, the premolded body is attached to the mold 1.
  • a rolling step may be performed in order to adjust the outer diameter of the premolded body to a predetermined size, increase the roundness, and reduce the unevenness of the outer peripheral surface. can.
  • the mold 1 with the preformed body obtained in the suction filtration step attached may be placed on a table and moved back and forth while being pressed by a predetermined force.
  • the suction filtration step and the rolling step performed as needed may be performed any number of times in order to obtain a desired pore volume, adsorption filter density, and the like.
  • the drying temperature is, for example, 100 ° C to 150 ° C, particularly 110 ° C to 130 ° C.
  • the drying time is, for example, about 4 to 24 hours, particularly about 8 to 16 hours.
  • a grinding step can be performed to further adjust the outer diameter of the adsorption filter or to reduce the unevenness of the outer peripheral surface.
  • the grinding method is not particularly limited as long as the outer surface of the dried molded body can be ground (or polished), and any grinding method known to those skilled in the art may be used. From the viewpoint of grinding uniformity, a method using a grinder that rotates and grinds the molded body itself is preferable.
  • the grinding process is not limited to the method using a grinder, and for example, a molded body fixed to a rotating shaft may be ground with a fixed flat plate-shaped grindstone.
  • the generated grinding residue is likely to be deposited on the grinding surface, so it is effective to grind while blowing air.
  • the adsorption filter in this embodiment can be used as, for example, a water purification filter, a filter for artificial dialysis, or the like.
  • a water purification filter or a filter for dialysis for example, an adsorption filter can be manufactured by the above-mentioned manufacturing method, shaped and dried, and then cut into a desired size and shape to be used. Further, if necessary, a cap may be attached to the tip portion, or a non-woven fabric may be attached to the surface.
  • the adsorption filter in this embodiment can be filled in a housing and used as a water purification cartridge.
  • the water purification cartridge is loaded into a water purifier and used for water flow, and as the water flow method, a full filtration method or a circulation filtration method in which the entire amount of raw water is filtered can be adopted.
  • a water purification filter adsorption filter in the present embodiment
  • the water purification filter can be used in combination with a known non-woven fabric filter, various adsorbents, mineral additives, ceramic filter materials and the like.
  • the adsorption filter according to the aspect of the present invention is an adsorption filter made of a molded body containing activated carbon and a binder.
  • the pore volume having a pore diameter of 10 ⁇ m or more based on the volume of the adsorption filter measured by the mercury intrusion method is 0.10 cm 3 / cc to 0.39 cm 3 / cc.
  • the density of the adsorption filter is preferably 0.59 g / cm 3 or less.
  • the total pore volume of the adsorption filter measured by the mercury intrusion method on a volume basis is 0.50 cm 3 / cc to 0.73 cm 3 / cc.
  • the pore volume having a pore diameter of 7 ⁇ m or less based on the volume of the adsorption filter measured by the mercury intrusion method is 0.15 cm 3 / cc or more.
  • the adsorption filter according to a further aspect of the present invention is an adsorption filter made of a molded body containing activated carbon and a binder.
  • the pore volume with a pore diameter of 7 ⁇ m or less based on the volume of the adsorption filter measured by the mercury intrusion method is 0.15 cm 3 / cc or more, and
  • the total pore volume of the adsorption filter measured by the mercury intrusion method on a volume basis is 0.50 cm 3 / cc to 0.73 cm 3 / cc.
  • the ratio of is preferably 22% or more.
  • the pore mode diameter measured by the mercury intrusion method is 15 ⁇ m or less.
  • the content of particles having a particle diameter of 10 ⁇ m or less is 2% by volume or more. preferable.
  • the benzene saturation adsorption amount obtained from the increase of the sample when the mass becomes constant by passing air containing solvent vapor which is 1/10 of the solvent saturation concentration at 25 ° C. is 18% to 35%. % Is particularly preferable.
  • the 0% particle size in the cumulative particle size distribution on a volume basis is 7 ⁇ m or less in the carbide obtained by heat-treating the adsorption filter in an inert gas at 900 ° C. for 20 minutes.
  • the binder contains a fibrous binder.
  • the fibrous binder contains an acrylic fibrous binder.
  • the fibrous binder contains a cellulosic fibrous binder.
  • Powdered activated carbon A Carbonized coconut shell charcoal from the Philippines is steam-activated at 900 ° C, the activation time is adjusted to the desired benzene adsorption amount, and the obtained coconut shell activated carbon is washed with dilute hydrochloric acid and desalted with ion-exchanged water.
  • Granular activated carbon JIS K 1474, 18 ⁇ 42 mesh, benzene adsorption amount 29.5 wt%) was obtained.
  • the obtained granular activated carbon was pulverized with a ball mill to obtain powdered activated carbon A having a D50 of 19.5 ⁇ m.
  • Powdered activated carbon B Carbonized coconut shell charcoal from the Philippines is steam-activated at 900 ° C, the activation time is adjusted to the desired benzene adsorption amount, and the obtained coconut shell activated carbon is washed with dilute hydrochloric acid and desalted with ion-exchanged water. Granular activated carbon (JIS K 1474, 18 ⁇ 42 mesh, benzene adsorption amount 30.1 wt%) was obtained. The obtained granular activated carbon was pulverized with a ball mill, and fine powder was removed using a dry classifier to obtain powdered activated carbon B having a D50 of 36.8 ⁇ m.
  • Powdered activated carbon C Carbonized coconut shell charcoal from the Philippines is steam-activated at 900 ° C, the activation time is adjusted to the desired benzene adsorption amount, and the obtained coconut shell activated carbon is washed with dilute hydrochloric acid and desalted with ion-exchanged water.
  • Granular activated carbon JIS K 1474, 18 ⁇ 42 mesh, benzene adsorption amount 27.9 wt%) was obtained.
  • the obtained granular activated carbon was pulverized with a ball mill and fine powder was removed using a dry classifier to obtain powdered activated carbon C having a D50 of 33.2 ⁇ m.
  • Powdered activated carbon D Carbonized coconut shell charcoal from the Philippines is steam-activated at 900 ° C, the activation time is adjusted to the desired benzene adsorption amount, and the obtained coconut shell activated carbon is washed with dilute hydrochloric acid and desalted with ion-exchanged water.
  • Granular activated carbon JIS K 1474, 18 ⁇ 42 mesh, benzene adsorption amount 29.7 wt%) was obtained.
  • the obtained granular activated carbon was pulverized with a ball mill and then classified with a 325 mesh sieve to obtain powdered activated carbon D having a D50 of 145.3 ⁇ m.
  • Powdered activated carbon E Bituminous coal was used as a carbonaceous raw material, and carbonization was carried out at 650 ° C. to obtain a dry distillation product. The obtained dry distillation product is put into a furnace, the activation time is adjusted so that the desired amount of benzene is adsorbed, and the obtained coal-based activated carbon is washed with dilute hydrochloric acid and desalted with ion-exchanged water to obtain acid-washed activated carbon. Obtained.
  • the obtained acid-washed activated carbon was put into the furnace again, and the activation time was adjusted so as to obtain the desired benzene adsorption amount to obtain granular activated carbon (JIS K 1474, 10 ⁇ 32 mesh, benzene adsorption amount 42.1 wt%). rice field.
  • the obtained granular activated carbon was pulverized with a ball mill to obtain powdered activated carbon E having a D50 of 36.8 ⁇ m.
  • the phenol resin fiber was oxidized at 300 ° C. for 1 hour, and the obtained oxidized product was carbonized at 700 ° C. for 1 hour.
  • the obtained phenol resin fiber after carbonization treatment was activated at an activation temperature of 950 ° C. to obtain a phenol resin-based fibrous activated carbon having a BET specific surface area of 1850 m 2 / g.
  • binder (binder) -Acrylic fiber binder: manufactured by Japan Exlan Co., Ltd., "Acrylic fiber Bi-PUL / F", CSF value 83 mL Cellulose-based fibrous binder (The CSF value is 28 mL when 50 parts by mass of the cellulosic fibrous binder is blended with 100 parts by mass of the acrylic fibrous binder (CSF value 83 mL)).
  • -Powder binder high-density polyethylene powder binder: "Miperon MX-220" manufactured by Mitsui Chemicals, Inc.
  • the adsorption filter density (g / cm 3 ) was calculated according to the following formula after the obtained adsorption filter was dried at 120 ° C. for 2 hours.
  • the adsorption filter density refers to the density of only the molded layer of activated carbon.
  • Adsorption filter density (mass of adsorption filter activated carbon molded layer) / (volume of adsorption filter activated carbon molded layer)
  • the pore volume of the adsorption filter was measured using a mercury intrusion method pore volume measuring device (“MicroActive AutoPore V 9620” manufactured by Micromeritics Co., Ltd.). The measured pressure was 0.7 kPa-420 MPa. After cutting the molded layer composed of activated carbon and the binder of the cylindrical adsorption filter as shown in FIG. 3, the cut pieces were further cut into a size of about 1 cm square.
  • the pore volume (cm 3 / g) was calculated. Then, by multiplying these values by the adsorption filter density obtained above, the pore volume (cm 3 / cc) having a pore diameter of 10 ⁇ m or more and the pore diameter of 7 ⁇ m or less based on the volume of the adsorption filter is obtained.
  • the pore mode diameter ( ⁇ m) of the adsorption filter was the pore diameter showing the peak value of the obtained pore distribution.
  • the obtained charcoal was used as a sample for measuring the particle size distribution of the activated charcoal in the adsorption filter, and 0% in the cumulative particle size distribution based on the volume of the activated charcoal in the adsorption filter by the same method as the method for measuring the particle size distribution of the activated charcoal as the raw material described above.
  • the particle size (D0) ( ⁇ m) and the particle content (% by volume) having a particle size of 10 ⁇ m or less were measured.
  • benzene adsorption performance of adsorption filter For the benzene adsorption performance of the adsorption filter, refer to the activated carbon test method (JIS K 1474: 1991) in the Japanese Industrial Standards, and pass air containing solvent vapor, which is 1/10 of the solvent saturation concentration, at 25 ° C. to the mass. The benzene saturated adsorption amount (%) was obtained from the increase in the amount of the sample when the value became constant. As the measurement sample, a sample obtained by cutting out a part of the adsorption filter and pulverizing it was used, and the adsorption performance of the sample after pulverization was evaluated.
  • sample waters are filtered through a 0.2 ⁇ m membrane filter (ADVANTEC, MEMBRANE FILTER A020B025A WHITE (cellulose mixed ester, 0.2 ⁇ m, 25 mm, with black ruled lines)), and the membrane filter is dried at 60 ° C. rice field.
  • ADVANTEC MEMBRANE FILTER A020B025A WHITE (cellulose mixed ester, 0.2 ⁇ m, 25 mm, with black ruled lines)
  • BX51-34-FL manufactured by OLYMPUS
  • the removal rate (%) by processing the particles was calculated.
  • the fluorescent particle removal rate when 10940 L of water was passed was evaluated, and a removal rate of 95% or more was used as a pass criterion for ultrafine particle removal performance.
  • Example 1 The powdered activated carbon A, the powdered activated carbon B, the acrylic fibrous binder, the cellulosic fibrous binder and the titanosilicate-based lead adsorbent were prepared so as to have a total of 1.055 kg in the blending ratio shown in Table 2 below. , Added tap water. The amount of slurry after the addition was 20 L. In Table 2, the particle content (% by volume) of the activated carbon as a raw material measured by the above method and having a particle diameter of 10 ⁇ m or less is also shown.
  • the core was attached to the above-mentioned mold for cylindrical molding (outer diameter 60 mm ⁇ , center pole diameter 30 mm ⁇ , and outer diameter flange spacing 84.9 mmH) shown in FIG. 1, and the obtained slurry was slightly smaller than the outer diameter of the mold. It was molded by suction only at 450 mmHg up to a large diameter of 62 mm ⁇ , and then dried.
  • the obtained molded body was mounted on the automatic grinder shown in FIG. 5, and the molded body rotation speed was 360 rotations / minute, the grindstone rotation speed was 2535 rotations / minute, and the grindstone moving speed was 300 mm / 10 seconds (3 cm / sec).
  • the outer surface of the molded body was ground to obtain a cylindrical adsorption filter having an outer diameter of 60 mm ⁇ , an inner diameter of 30 mm ⁇ , and a height of 84.9 mmH.
  • the density of the adsorption filter, the pore volume and the pore mode diameter in the mercury porosimeter, the particle size distribution of the activated carbon (carbide after heat treatment) in the adsorption filter, and the particle size distribution of the activated carbon (carbide after heat treatment) in the adsorption filter are obtained by the above-mentioned method.
  • the benzene adsorption performance was measured. The results of measuring the physical properties of these adsorption filters are summarized in Table 3 below.
  • the non-woven fabric was wrapped in a single layer around the outer circumference of the obtained adsorption filter. Further, a donut-shaped packing formed of a foamed polyethylene sheet having a thickness of 2 mm and having an outer diameter of 60 mm ⁇ and an inner diameter of 30 mm ⁇ was bonded to both ends of the adsorption filter with a hot melt adhesive.
  • Example 2 As shown in Table 2 below, in Example 2, a cylindrical adsorption filter was obtained by the same method as in Example 1 except that the cellulosic fibrous binder was not blended in the raw material.
  • the physical property measurement results and performance evaluation results of the adsorption filter in Example 2 are summarized in Table 3 below.
  • Example 3 As shown in Table 2 below, in Example 3, the amount of powdered activated carbon A was slightly increased and the amount of powdered activated carbon B was slightly decreased as compared with Example 1. A cylindrical adsorption filter was obtained in the same manner as in Example 1 except for the above. The physical property measurement results and performance evaluation results of the adsorption filter in Example 3 are summarized in Table 3 below.
  • Example 4 As shown in Table 2 below, in Example 4, the amount of powdered activated carbon A was further increased and the amount of powdered activated carbon B was further decreased as compared with Example 3. A cylindrical adsorption filter was obtained in the same manner as in Example 3 except for the above. The physical property measurement results and performance evaluation results of the adsorption filter in Example 4 are summarized in Table 3 below.
  • Example 5 As shown in Table 2 below, in Example 5, the cylindrical adsorption filter was provided in the same manner as in Example 1 except that the powdered activated carbon A was changed to the powdered activated carbon E and the blending amount was changed. Obtained.
  • the physical property measurement results and performance evaluation results of the adsorption filter in Example 5 are summarized in Table 3 below.
  • Example 6 As shown in Table 2 below, in Example 6, the same compounding conditions as in Example 1 were used. In Example 6, when molding the adsorption filter, the obtained slurry is sucked and molded at 450 mmHg up to 70 mm ⁇ , which is larger than the outer diameter of the mold, and then the rolling step is sandwiched until the outer diameter becomes 63 mm ⁇ . A cylindrical adsorption filter was obtained in the same manner as in Example 1 except that the surface was molded and then dried. The physical property measurement results and performance evaluation results of the adsorption filter in Example 6 are summarized in Table 3 below.
  • Example 7 As shown in Table 2 below, in Example 7, a cylindrical adsorption filter was obtained by the same method as in Example 1 except that the titanosilicate-based lead adsorbent was not blended. The physical property measurement results and performance evaluation results of the adsorption filter in Example 7 are summarized in Table 3 below.
  • Comparative Example 1 As shown in Table 2 below, in Comparative Example 1, the same method as in Example 1 was used except that the powdered activated carbon A was not contained and only the powdered activated carbon B was used in the blending of the powdered activated carbon. A cylindrical adsorption filter was obtained. The physical property measurement results and performance evaluation results of the adsorption filter in Comparative Example 1 are summarized in Table 3 below.
  • the obtained mixture was filled into a tubular stainless steel mold having an inner diameter of 65 mm ⁇ , a core diameter of 30 mm ⁇ , and a height of 90 mm with a lid on one side while gradually vibrating with a mallet, and the lid was placed on the open side. And fixed the contents.
  • the mold filled with the mixture was put into a dryer at 160 ° C., heated for 120 minutes, and then allowed to cool to 50 ° C. or lower. After that, the lid was removed and the molded product was taken out from the mold so as not to damage the molded product.
  • the obtained molded product was cut to prepare a dry molded body having an outer diameter of 65 mm ⁇ , an inner diameter of 30 mm ⁇ , and a height of 84 mm. Finally, both ends of the obtained molded body were cut with a saw to prepare an adsorption filter having a height of 64 mm.
  • Table 3 The physical property measurement results and performance evaluation results of the adsorption filter in Comparative Example 2 are summarized in Table 3 below.
  • ⁇ Comparative Example 3> In a 100 L small beater, 1.5 kg of fibrous activated carbon was added to 100 L of tap water by dry weight, and then 0.075 kg of acrylic fibrous binder was added by dry weight to beat the mixture. .. Specifically, the fibrous activated carbon was subdivided by dispersing and mixing the fibrous activated carbon and the binder, and further narrowing the gap between the fixed teeth and the rotating teeth of the beater. When the fiber length of the fibrous activated carbon is shortened due to subdivision, the filling property is improved when molded into a specific shape, so that the weight per unit volume increases. This weight per unit volume was called the beating density and was used as a measure of the shortness of the fibrous activated carbon.
  • the following molded body was prepared. Specifically, a 300-mesh wire mesh is wound around a central shaft with a small hole diameter of 3 mm ⁇ for suction and a pitch of 5 mm, and a mold with a central shaft diameter of 18 mm ⁇ , an outer diameter of 40 mm ⁇ , and an outer diameter flange spacing of 50 mmH is prepared, and the slurry is sucked from the center. By doing so, a molded body of a cylindrical suction filter was produced.
  • the beating density was calculated from the dimensions and weight of the dried product of this molded product and found to be 0.183 g / ml. In Comparative Example 3, this slurry having a beating density of 0.183 g / ml was used as a standard slurry.
  • Comparative Example 3 the same method as in Example 1 was used except that a predetermined amount of powdered activated carbon C was added to the standard slurry in the blending of the raw materials so as to have the blending ratio shown in Table 2 below. A cylindrical adsorption filter was obtained. The physical property measurement results and performance evaluation results of the adsorption filter in Comparative Example 3 are summarized in Table 3 below.
  • Comparative Example 4 is the same as Comparative Example 2 except that the powdered activated carbon D, the titanosilicate-based lead adsorbent, and the high-density polyethylene powder binder were used in the blending ratios shown in Table 2 below.
  • a cylindrical adsorption filter was obtained by the above method.
  • the physical property measurement results and performance evaluation results of the adsorption filter in Comparative Example 4 are summarized in Table 4 below.
  • FIG. 6 shows a graph of the pore mode diameter and the section pore volume of the adsorption filter in Examples 1 to 7 and Comparative Examples 1 to 3 measured by a mercury porosimeter.
  • FIG. 7 the pore volume (cm 3 / cc) and ultrafine particle removal of the adsorption filters having a pore diameter of 10 ⁇ m or more in Examples 1 to 7 and Comparative Examples 1 and 3 measured with a mercury porosimeter are shown. The correlation with the performance (%) is shown. Further, in FIG. 8, the pore volume (cm 3 / cc) having a pore diameter of 7 ⁇ m or less and the removal of ultrafine particles in Examples 1 to 7 and Comparative Examples 1 and 3 to 4 measured by a mercury porosimeter are shown. The correlation with the performance (%) is shown. Comparative Example 2 is not shown because it stopped halfway as shown in Table 3 above.
  • the adsorption filters of Examples 1 to 7 had excellent ultrafine particle removing performance and maintained good water permeability.
  • the adsorption filter of Comparative Example 1 did not satisfy the acceptance criteria of the ultrafine particle removing performance, and the adsorption filter of Comparative Example 2 did not satisfy the acceptance criteria of the initial water flow resistance.
  • Comparing Example 1 and Comparative Example 1 although the total pore volume and the pore mode diameter are about the same values, the adsorption filter of Comparative Example 1 has a pore diameter of 10 ⁇ m or more in this embodiment. It did not meet both the specified range of pore volume and the specified range of pore volume with a pore diameter of 7 ⁇ m or less. Specifically, as shown in FIG.
  • the pore distribution of Comparative Example 1 has a pore diameter of 10 ⁇ m or more in a direction in which the pore diameter is larger than that of Example 1. It can be seen that there are more in the range. Further, the pore distribution of Comparative Example 1 is smaller than that of Example 1 in the direction in which the pore diameter is smaller, specifically in the range of the pore diameter of 7 ⁇ m or less. I understand. Therefore, it is assumed that there is a difference in the effect of the ultrafine particle removal performance. As described above, it is considered that in the adsorption filters of Examples 1 to 7, the pore volume of the adsorption filter having a pore diameter of 10 ⁇ m or more and the pore volume of the pore diameter of 7 ⁇ m or less are suitably controlled.
  • the adsorption filter of the present invention for example, by using it as a water purification filter or the like, it is possible to exhibit excellent ultrafine particle removing performance while maintaining good water permeability.

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