WO2018062705A1 - Membrane de filtration à membrane de distillation et son procédé de fabrication - Google Patents

Membrane de filtration à membrane de distillation et son procédé de fabrication Download PDF

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Publication number
WO2018062705A1
WO2018062705A1 PCT/KR2017/009630 KR2017009630W WO2018062705A1 WO 2018062705 A1 WO2018062705 A1 WO 2018062705A1 KR 2017009630 W KR2017009630 W KR 2017009630W WO 2018062705 A1 WO2018062705 A1 WO 2018062705A1
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Prior art keywords
membrane
filtration
porous body
pore diameter
nominal pore
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PCT/KR2017/009630
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English (en)
Korean (ko)
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이광진
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코오롱인더스트리 주식회사
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Publication of WO2018062705A1 publication Critical patent/WO2018062705A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
    • B01D61/364—Membrane distillation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/447—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by membrane distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/24—Quality control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/02—Details relating to pores or porosity of the membranes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/08—Seawater, e.g. for desalination
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A20/00—Water conservation; Efficient water supply; Efficient water use
    • Y02A20/124—Water desalination
    • Y02A20/131—Reverse-osmosis

Definitions

  • the present invention relates to a membrane distillation filtration membrane and a method for producing the same, and more particularly, to a membrane distillation filtration membrane having excellent non-wetting property and a method for producing the same.
  • Seawater desalination is largely divided into evaporation and reverse osmosis.
  • Seawater desalination technology using the evaporation method has been actively spread around the Middle East where water shortages are serious, but as the concern about rising energy costs increases, the attractiveness of future seawater desalination technology is decreasing. For this reason, the adoption of reverse osmosis seawater desalination technology is increasing.
  • reverse osmosis has many problems. For example, since high pressure raw water is supplied to the reverse osmosis membrane, it is vulnerable to membrane contamination, and it requires difficulty in operation and management because several steps of pretreatment are required to prevent contamination of the reverse osmosis membrane. And a lot of energy is consumed because it must be operated at a higher pressure than the osmotic pressure.
  • Membrane distillation is a method of separating pure water from the raw water using a temperature difference between feed water and clean water located on opposite sides of the filter membrane.
  • Phase change (liquid-> gas) of raw water which is relatively hot, occurs at the surface of the filtration membrane, and steam generated by the phase change penetrates the micropores of the filtration membrane and loses heat to the fresh water to condense.
  • the pores get wet with water from the largest pore to the smallest pore, and water as well as water passes through the wet pores of the filtration membrane. That is, the wet pores become a leak point, and as the number of wet pores increases, the rejection rate decreases, thereby losing the filtration membrane performance.
  • the existing filtration membranes contain many relatively small pore pores, so that sufficient permeate flux (e.g., the temperature difference between the raw water and the filtrate is 20 ° C in standard conditions) is suitable for commercialization of the membrane distillation method. Filtration flow rates above LMH) were very difficult to achieve.
  • the present invention relates to a membrane distillation filtration membrane and a method of manufacturing the same that can prevent problems caused by the above limitations and disadvantages of the related art.
  • One aspect of the present invention is to provide a membrane distillation filtration membrane having excellent wet resistance.
  • Another aspect of the present invention is to provide a method for producing a membrane distillation filter membrane having excellent wet resistance.
  • a membrane distillation filter membrane including a porous member (porous member) having a nominal pore diameter of 0.1 ⁇ m or more, 99% or more of the pores of the porous body is less than 120% of the nominal pore diameter
  • a membrane distillation filtration membrane having a pore size, a contact angle with respect to pure water of the filtration membrane is 60 ° or more, and a thermal conductivity of the filtration membrane is 0.6 W / mK or less.
  • the nominal pore diameter may be 0.1 ⁇ m to 0.2 ⁇ m.
  • the contact angle may be 100 ° or more.
  • the thermal conductivity may be 0.2 W / mK or less.
  • the porous body may have a porosity of 60% to 80%.
  • the nominal pore diameter may be 0.13 ⁇ m to 0.2 ⁇ m, and at least 99% of the pores of the porous body may have a pore diameter of 115% or less of the nominal pore diameter.
  • the nominal pore diameter may be 0.13 ⁇ m to 0.16 ⁇ m.
  • the porous body may include at least one of polytetrafluoroethylene, polyethylene, polypropylene, and polyvinylidene fluoride.
  • the porous body may include polytetrafluoroethylene or polypropylene.
  • the porous body may include polypropylene.
  • a method for producing a membrane for filtration membranes is provided.
  • the porous body may be manufactured by a 3D printer, and the nominal pore size of the porous body may be 0.1 ⁇ m to 0.2 ⁇ m.
  • the polymer resin may include at least one of polytetrafluoroethylene, polyethylene, polypropylene, and polyvinylidene fluoride.
  • the polymer resin may include polytetrafluoroethylene or polypropylene.
  • the polymer resin may include polypropylene.
  • the porous body may have a porosity of 60% to 80%.
  • the nominal pore size of the porous body may be 0.13 ⁇ m to 0.2 ⁇ m.
  • the nominal pore size of the porous body may be 0.13 ⁇ m 0.16 ⁇ m.
  • the filtration performance of the membrane distillation filtration membrane can be maintained for a long time by significantly delaying the wet phenomenon during operation of the membrane distillation filtration membrane.
  • the present invention enables the commercialization of the seawater desalination system using the membrane distillation method, thereby significantly reducing the energy consumption required for seawater desalination.
  • FIG. 1 schematically shows a membrane distillation system according to an embodiment of the present invention.
  • FIG. 1 illustrates a direct contact membrane distillation system.
  • Membrane distillation system 100 of the present invention the filtration module 110 for performing a water treatment, the raw water storage tank 120, the feed water (for example seawater) to be treated, and the filtration module And a filtrate storage tank 130 for storing filtrate produced by 110.
  • the filtration module 110 includes a housing 111 and a filtration membrane 112.
  • the filtration membrane 112 is installed in the housing 111 and divides the internal space of the housing 111 into a first flow path FP1 and a second flow path FP2.
  • the first flow path FP1 constitutes a part of the circulation path of raw water
  • the second flow path FP2 constitutes a part of the circulation path of the filtered water.
  • the filtration module 110 illustrated in FIG. 1 includes a flat sheet membrane as the filtration membrane 112, but the filtration membrane 112 of the present invention is not limited to the flat membrane, and various types of filtration membranes, for example, hollow It may be a hollow fiber membrane.
  • the filtration membrane is a hollow fiber membrane
  • the space in the housing ie, the space between the housing and the hollow fiber membrane
  • the lumen of the hollow fiber membrane provides a second flow path for filtered water. .
  • Raw water stored in the raw water storage tank 120 is provided to the filtration module 110 by the first pump (P1).
  • the first pump P1
  • seawater may be directly provided to the filtration module 110 from the sea by the first pump P1 without passing through the raw water storage tank 120.
  • the raw water may be heated by the heating unit 140 immediately before being provided to the filtration membrane module 110 for the phase change on the surface of the filtration membrane 112.
  • the temperature of the raw water to be treated is sufficiently high, such as seawater in the Middle East, raw water heating by the heating unit 140 may be omitted.
  • the heating unit 140 is a heat exchanger for transmitting waste heat of a power plant to the raw water (that is, heat exchange is performed between the hot steam and hot water discharged after rotating the turbine of the power plant). Heat exchanger).
  • the raw water passing through the first flow path FP1 may be discharged directly into the sea instead of returning to the raw water storage tank 120.
  • Clean water is stored in the filtrate storage tank 130 before the filtration operation starts, but as the filtration operation proceeds, the fresh water is gradually replaced by the filtered water.
  • fresh water is referred to as filtered water.
  • Filtrate stored in the filtrate storage tank 130 is provided to the filtration module 110 by a second pump (P2).
  • the filtered water may be cooled by the cooling unit 150 immediately before being provided to the filtration membrane module 110 for the phase change of raw water on the surface of the filtration membrane 112.
  • the relatively low temperature filtered water provided to the filtration module 110 passes through the second flow path FP2 of the filtration module 100, a part of the relatively high temperature raw water passing through the first flow path FP1, that is, the The raw water in contact with the filtration membrane 112 is converted into steam by causing a phase change due to a temperature difference.
  • the vapor penetrates through the filtration membrane 112 and moves to the low temperature filtered water, and then condenses, and moves to the filtered water storage tank 130 together with the original filtered water.
  • the membrane distillation process described above is an example of a direct contact membrane distillation process, and instead of inducing a low temperature fresh water flow to the filtration side, the vapor is passed through the membrane pores to form a vacuum space, and then the condensation unit after the vacuum space.
  • Other membrane distillation processes known to date such as the vacuum membrane distillation process, which is phase-separated into separate water by air, and the air-gap membrane distillation process, which places an air layer between the membrane and the filtration fresh water stream
  • the filter membrane of the present invention can be applied to obtain the effects of the present invention.
  • the filtration membrane 112 of the present invention includes a porous member having a plurality of pores.
  • the form of the pores is not particularly limited in the present invention, but may be, for example, a pore P having a prismatic form such as a cylinder or a square pillar or a rectangular pillar.
  • the porous body has a nominal pore diameter of 0.1 ⁇ m or more, preferably 0.1 to 100 ⁇ m, more preferably 0.1 to 0.2 ⁇ m, even more preferably 0.13 to 0.2 ⁇ m, even more preferably 0.13 to 0.16 ⁇ m.
  • the nominal pore means a diameter corresponding to pore cumulative number of 90% in a cumulative distribution of pore diameter in ascending order, and gas-liquid displacement porosimetry Or Liquid-Liquid Displacement Porosimetry (LLDP).
  • the nominal pore size of the porous body is less than 0.1 mu m, a filtration flow rate suitable for commercialization of the membrane distillation method is difficult to be achieved.
  • a liquid containing impurities eg, a salt such as NaCl
  • the rejection rate is lowered to 95% or less.
  • the filtration membrane 112 In order to achieve a sufficient filtration flow rate (for example, a filtration flow rate of 20 LMH or more under standard conditions where the temperature difference between the raw water and the filtered water is 40 ° C.) suitable for commercialization of the membrane distillation method, the filtration membrane 112 according to one embodiment of the present invention
  • the porous body of may have a relatively high porosity of 50% or more, preferably 60% to 80%, in addition to a nominal pore diameter of 0.1 ⁇ m or more.
  • the porosity means the percentage of the total volume of pores relative to the apparent volume of the filtration membrane 112 (ie (total volume of pores / apparent volume of the filtration membrane) ⁇ 100 (%)), and the mercury method is used. Can be obtained through
  • the membrane distillation filtration membrane 112 should have high wetting resistance.
  • the higher hydrophobicity of the filtration membrane 112 generally improves its wettability, but it has been found by the present invention that the most important factor for determining the wettability of the filtration membrane 112 is the pore size distribution of the porous body.
  • the more uniform the pore diameters of the porous body i.e., the fewer pores having pores much larger than the nominal pore size
  • satisfactory medium and long term filtration performance can be ensured. have. This is because the wetting phenomenon is mainly caused by pores of relatively large pore size (eg, a pore exceeding 120% of the nominal pore size).
  • wettability of the filtration membrane 112 may be significantly improved by having 99% or more of the pores of the porous body having a pore size of 120% or less, preferably 115% or less of the pore size of the porous body. .
  • the filtration membrane 112 of the present invention has a contact angle to pure water of 60 ° or more, preferably 100 ° or more.
  • the contact angle refers to a static contact angle that can be obtained by dropping a drop of pure water on the surface of the membrane 112 and measuring the angle between the surface of the membrane and the droplet.
  • the static contact angle should be measured after melting the filtration membrane 112 with heat and resolidifying the nonporous solid. In the case of materials that cannot be melted by heat such as PTFE, the static contact angle can be measured in the solid form of the same material.
  • plasma sputtering increases or increases the surface roughness of the porous body and changes the surface of the porous body to a fluorine-based functional group such as -CF 3 , -CF. 2 H, -CF 2 -, and modified by at least one of the -CH 2 -CF 3, may further enhance the hydrophobicity of the membrane (112).
  • the membrane distillation method utilizes the temperature difference between the raw water and the filtrate which are located opposite to each other with the filtration membrane 112 interposed therebetween, it is necessary to ensure a certain amount of filtration flow rate while performing the filtration through the membrane distillation (that is, the filtration performance In order to maintain the long term, the temperature difference between the raw water and the filtrate must be maintained at a predetermined size or more. For this reason, the filtration membrane 112 applied to membrane distillation should be able to inhibit or prevent heat transfer from relatively hot raw water to relatively cold filtration water. Therefore, according to the present invention, the thermal conductivity of the membrane distillation filtration membrane 112 is 0.6 W / mK or less, preferably 0.2 W / mK or less. The thermal conductivity may be measured after melting the filtration membrane 112 with heat and re-solidifying the non-porous solid.
  • the porous body is made of polytetrafluoroethylene (PTFE), polyethylene (PE), polypropylene (PP), and polyvinylidene fluoride (PVDF).
  • PTFE polytetrafluoroethylene
  • PE polyethylene
  • PP polypropylene
  • PVDF polyvinylidene fluoride
  • the porous body in order to produce a filtration membrane 112 having a contact angle of 100 ° or more and a thermal conductivity of 0.6 W / mK or less, may be polytetrafluoroethylene (PTFE) or polypropylene (PP). It may include.
  • PTFE polytetrafluoroethylene
  • PP polypropylene
  • the porous body may include polypropylene (PP).
  • a polymer resin having a contact angle to pure water of 60 ° or more and a thermal conductivity of 0.6 W / mK or less is prepared.
  • the polymer resin may include at least one of polytetrafluoroethylene (PTFE), polyethylene (PE), polypropylene (PP), and polyvinylidene fluoride (PVDF).
  • a polymer resin having a contact angle of 100 ° or more and a thermal conductivity of 0.6 W / mK or less for example, polytetrafluoroethylene (PTFE) or polypropylene (PP)
  • Polymer resin containing may be used.
  • a polymer resin containing polypropylene (PP) having a contact angle with respect to pure water of 100 ° or more and a thermal conductivity of 0.2 W / mK or less may be used.
  • a nominal of 0.1 ⁇ m or more preferably 0.1 to 100 ⁇ m, more preferably 0.1 to 0.2 ⁇ m, still more preferably 0.13 to 0.2 ⁇ m, even more preferably 0.13 to 0.16 ⁇ m
  • a porous body having a pore diameter is produced.
  • the porous body of the present invention can be formed using a 3D printer.
  • porous body of the filtration membrane 112 may have a relatively high porosity of 50% or more, preferably 60% to 80%.
  • a plasma sputtering process for increasing the surface roughness of the porous body, and / or ii) the surface of the porous body is fluorine-based, for example -CF 3 ,-
  • the process of modifying to at least one of CF 2 H, —CF 2 —, and —CH 2 —CF 3 may be further performed.
  • the plasma sputtering process may be performed using an RF power source in a vacuum.
  • the surface modification process may be performed by etching the porous surface with plasma to form a rough surface, and then generating a plasma in a fluorine-based gas environment.
  • the filtration membrane 112 of the present invention may have a high hydrophobicity such that the contact angle with pure water is 130 ° or more.
  • the nominal pore diameter, 99% pore range, porosity, contact angle, thermal conductivity, filtration flow rate, rejection rate, and wetting time of the filtration membrane were measured by the following methods, respectively.
  • the nominal pore means a pore corresponding to a total of 90% pore in the ascending cumulative distribution of pore size, and was obtained from a pore distribution graph obtained through Liquid-Liquid Displacement Porosimetry (LLDP) after taking a sample from the center portion of the entire filtration membrane.
  • LLDP Liquid-Liquid Displacement Porosimetry
  • the 99% nominal pore is similar to the nominal pore but refers to the pore diameter corresponding to the 99% pore accumulation in the ascending cumulative distribution of the pore sizes.
  • Samples were taken from the central portion of the entire filtration membrane and then obtained from a pore distribution graph obtained through LLDP.
  • Porosity means the percentage of the total volume of pores relative to the apparent volume of the filtration membrane (ie, (total volume of pores / apparent volume of the filtration membrane) ⁇ 100 (%)), which was obtained by mercury method.
  • the contact angle means a static contact angle
  • a drop of pure water was dropped on the surface of the filtration membrane to measure the angle between the membrane surface and the droplets.
  • the filter membrane is melted with heat and re-solidified to make a nonporous solid, and then the static contact angle is measured.
  • the static contact angle is measured in the form of a solid of the same material. do.
  • the exclusion rate was measured 10 minutes after the start of the operation, and the wetting time was the time taken until the exclusion rate was reduced by 10% after the time was measured 10 minutes after the operation in which the initial exclusion rate was measured.
  • Porous filtration membranes were made of the same materials as that of Comparative Examples 1 to 4, that is, PTFE, PE, PP and PVDF, respectively, using a 3D printer. At this time, the nominal pore size of the porous filtration membranes were unified to 0.1 ⁇ m, and had the same porosity as the filtration membranes of Comparative Examples 1 to 4, respectively. The 99% nominal pore size, filtration flow rate, rejection rate, and wetting time of the porous filtration membranes were measured, respectively, and are shown in Table 1 below.
  • PP porous filtration membranes were prepared in the same manner as in Example 3 except that the porosities were 60%, 70%, and 80%, respectively. 99% nominal pore size, filtration flow rate, rejection rate, and wetting time of the PP porous filtration membranes were measured, respectively, and are shown in Table 1 below.
  • PP porous filter membranes were prepared in the same manner as in Example 7, except that the nominal pore sizes were 0.13 ⁇ m, 0.16 ⁇ m, and 0.2 ⁇ m, respectively. 99% nominal pore size, filtration flow rate, rejection rate, and wetting time of the PP porous filtration membranes were measured, respectively, and are shown in Table 1 below.
  • the filtration membranes of Examples 5 to 10 are filtration membranes manufactured using polypropylene (PP), which is the most advantageous material in consideration of hydrophobicity and thermal conductivity.
  • PP polypropylene
  • the filtration membranes of Examples 3 and 5-7 were made to have the same nominal pore diameter (0.1 ⁇ m) of the same material (PP), with porosities of 50% to 60%, 70% and 80% When increased to each, it was confirmed that the filtration flow rate is increased while the wettability and rejection rate of the filtration membrane is maintained.
  • the filtration membranes of Examples 7 to 10 are manufactured to have the same porosity (80%) with the same material (PP), but have a nominal pore diameter of 0.13 ⁇ m, 0.16 ⁇ m, and 0.2 ⁇ m. When increased to each, while the wettability and rejection rate of the filtration membrane was maintained well it was confirmed that the filtration flow rate is rapidly increased.

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  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L'invention concerne une membrane de filtration à membrane de distillation ayant une excellente propriété de non-mouillage, et son procédé de fabrication. La membrane de filtration à membrane de distillation de la présente invention comprend un élément poreux ayant une taille de pore nominale de 0,1 µm ou plus, dans lequel 99 % ou plus de tous les pores de l'élément poreux ont une taille de pore de 120 % ou moins de la taille de pore nominale de l'élément poreux.
PCT/KR2017/009630 2016-09-28 2017-09-04 Membrane de filtration à membrane de distillation et son procédé de fabrication WO2018062705A1 (fr)

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KR10-2016-0124798 2016-09-28
KR20160124798 2016-09-28

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113412147A (zh) * 2019-02-12 2021-09-17 昭和电工材料株式会社 层叠物

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KR20120126213A (ko) * 2011-05-11 2012-11-21 단국대학교 산학협력단 경화 가능한 초소수성 코팅을 위한 조성물 및 이를 이용한 초소수성 막을 구비한 기판의 제조방법
KR20130089494A (ko) * 2012-02-02 2013-08-12 한국과학기술연구원 막 증류용 분리막 모듈 장치
WO2016006670A1 (fr) * 2014-07-10 2016-01-14 旭化成株式会社 Appareil de distillation à membrane et membrane poreuse hydrophobe

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KR20120126213A (ko) * 2011-05-11 2012-11-21 단국대학교 산학협력단 경화 가능한 초소수성 코팅을 위한 조성물 및 이를 이용한 초소수성 막을 구비한 기판의 제조방법
KR20130089494A (ko) * 2012-02-02 2013-08-12 한국과학기술연구원 막 증류용 분리막 모듈 장치
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113412147A (zh) * 2019-02-12 2021-09-17 昭和电工材料株式会社 层叠物

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