KR960011045B1 - Manufacturing method of antibiotic ultrafiltration - Google Patents
Manufacturing method of antibiotic ultrafiltration Download PDFInfo
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- KR960011045B1 KR960011045B1 KR1019930020131A KR930020131A KR960011045B1 KR 960011045 B1 KR960011045 B1 KR 960011045B1 KR 1019930020131 A KR1019930020131 A KR 1019930020131A KR 930020131 A KR930020131 A KR 930020131A KR 960011045 B1 KR960011045 B1 KR 960011045B1
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- antimicrobial
- polypropylene
- ultrafiltration membrane
- weight
- nonwoven fabric
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- 238000000108 ultra-filtration Methods 0.000 title claims description 19
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 230000003115 biocidal effect Effects 0.000 title abstract 2
- 239000000919 ceramic Substances 0.000 claims abstract description 27
- 239000012528 membrane Substances 0.000 claims abstract description 21
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 8
- 229920002492 poly(sulfone) Polymers 0.000 claims abstract description 8
- 239000004417 polycarbonate Substances 0.000 claims abstract description 5
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 5
- -1 polypropylene Polymers 0.000 claims description 21
- 239000004743 Polypropylene Substances 0.000 claims description 19
- 239000004745 nonwoven fabric Substances 0.000 claims description 19
- 229920001155 polypropylene Polymers 0.000 claims description 19
- 230000000845 anti-microbial effect Effects 0.000 claims description 18
- 239000004599 antimicrobial Substances 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 150000003755 zirconium compounds Chemical class 0.000 claims description 3
- 239000004695 Polyether sulfone Substances 0.000 claims description 2
- 229920006393 polyether sulfone Polymers 0.000 claims description 2
- 229940100890 silver compound Drugs 0.000 claims description 2
- 150000003379 silver compounds Chemical class 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 13
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 3
- 150000002736 metal compounds Chemical class 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 abstract description 3
- 239000004744 fabric Substances 0.000 abstract 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 241000894006 Bacteria Species 0.000 description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 229910021645 metal ion Inorganic materials 0.000 description 6
- 239000008213 purified water Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920001817 Agar Polymers 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 235000008708 Morus alba Nutrition 0.000 description 1
- 240000000249 Morus alba Species 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000002070 germicidal effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009966 trimming Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
- B01D67/00793—Dispersing a component, e.g. as particles or powder, in another component
-
- 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
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/107—Organic support material
- B01D69/1071—Woven, non-woven or net mesh
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/1213—Laminated layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—Metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/26—Polyalkenes
- B01D71/262—Polypropylene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/50—Polycarbonates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/12—Specific ratios of components used
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
Description
본 발명은 두기계 항균체를 함유하는 항균성이 우수한 폴리프로필렌 장섬유 부직포위에 미세다공층을 코팅시킨 한외여과막의 제조방법에 관한 것으로, 좀더 상세하게는 폴리프로필렌, 수지에 은화합물과 지르코늄 화합물 등의 살균성 금속화합물이 무기세라믹에 대하여 2~50% 함유된 비다공성 무기세라믹을 첨가하여 마스터배치를 만든 후 최종 부직포 섬유에 대하여 무기 세라믹이 0.1~5중량% 되도록 폴리프로필렌 수지를 방사, 제직한 후 그 위에 폴리설폰, 폴리에테르설폰, 폴리카보네이트 등으로 구성된 군으로부터 선택된 1종으로 미세다공층을 코팅함을 특징으로 하는 항균성이 우수한 한외여과막의 제조방법에 관한 것이다.The present invention relates to a method for producing an ultrafiltration membrane coated with a microporous layer on a polypropylene long fiber nonwoven fabric having excellent antimicrobial properties including bimachined antimicrobial agents, and more particularly, to a polypropylene, a resin, a zirconium compound, and the like. After adding a non-porous inorganic ceramic containing 2 to 50% of inorganic ceramics to the sterilizing metal compound to make a masterbatch, spinning and weaving the polypropylene resin so that the inorganic ceramic is 0.1 to 5% by weight based on the final nonwoven fabric. The present invention relates to a method for producing an ultrafiltration membrane having excellent antimicrobial characteristics, characterized in that the microporous layer is coated with one selected from the group consisting of polysulfone, polyethersulfone, polycarbonate, and the like.
최근 환경오염의 악화 및 건강의식의 향상으로 가정용 정수기가 각 가정에 널리 보급되어 있으나, 정화수에서 세균이 검출되는 문제점이 있었다. 산업의 발달과 함께 수반되는 각종 오염물질이 양적 증가로 인하여 상수원의 오염이 가속화되어 소독제로 쓰여지는 염소가 대량으로 투여되고 또한, 급수관의 노후화로 인한 유기물, 녹찌꺼기, 전염성균, 미생물 등에 의하여 2차 오염이 심화되어 한외여과막이나 활성탄 흑인 이온 교환수지를 이용한 정수시스템이 널리 쓰이고 있는데, 각 시스템 공히 장시간 사용하거나 오염수의 오염정도가 심한 경우에는 분리능이 저하되어 2차 오염과 세균번식의 문제점이 있다.Recently, household water purifiers have been widely used in households due to deterioration of environmental pollution and improvement of health awareness, but there has been a problem in that bacteria are detected in purified water. Due to the quantitative increase in the amount of various pollutants accompanied by the development of the industry, the pollution of the water supply is accelerated, and chlorine, which is used as a disinfectant, is administered in large quantities.In addition, due to the aging of water pipes As the secondary pollution is intensified, water purification systems using ultrafiltration membranes or activated carbon black ion exchange resins are widely used.In case of using the system for a long time or when the pollution degree of the contaminated water is severe, the resolution decreases and the problems of secondary pollution and bacterial propagation are reduced. have.
특히, 수용액에 포함되어 있는 세균의 제거측면에서 보면 이론상으로는 한외여과막의 미세공의 크기는 10옹스트롱~1000옹스트롱으로 세균의 크기인 10,000옹스트롱보다 1/100배로 작아 세균이 통과할 수 없으나 실제공정에서는 일정시간 사용한 후의 한외여과막으로 생산된 용액에서 오염수는 한외역과막의 다공성 지지층을 지나 부직포를 통과하여 정화수로 생산되는데 이 한외여과막을 일정시간 이상 사용하게 되면 미세다공층 또는 부직표에서 세균이 번식하여 실제로는 전처리 필터에서 세균을 제거하여도 한외여과막을 통과한 정화수에서 세균이 검출되는 것이다. 또한, 각종 세균들이 다공성 지지층보다 부직포에서 잘 번식함을 발견하였다.In particular, in terms of the removal of bacteria contained in the aqueous solution, in theory, the size of the micropores of the ultrafiltration membrane is 10 angstroms to 1000 angstroms, which is 1/100 times smaller than the size of 10,000 angstroms, which prevents bacteria from passing through. In the actual process, the contaminated water from the solution produced by the ultrafiltration membrane after using for a certain time is passed through the porous support layer of the ultrafiltration membrane and passed through the nonwoven fabric to produce purified water.If the ultrafiltration membrane is used for a certain time, the bacteria in the microporous layer or nonwoven table By breeding and actually removing bacteria from the pretreatment filter, bacteria are detected in the purified water that has passed through the ultrafiltration membrane. In addition, it was found that various bacteria propagate better in nonwoven fabrics than porous support layers.
따라서, 본 발명의 목적은 세균번식억제 및 살균효과가 있는 항균성 한외여과막의 제조방법을 제공함에 있다.Accordingly, an object of the present invention is to provide a method for producing an antimicrobial ultrafiltration membrane having bacteriostatic and bactericidal effects.
본 발명의 목적뿐 아니라 용이하게 표출되는 또 다른 목적을 달성하기 위하여 본 발명에서는 은화합물과 지르코늄 화합물등의 살균성 금속화합물이 무기세라믹에 대하여 2~50% 함유된 비다공성 무기세라믹을 첨가한 폴리프로필렌 마스터배치를 제조하여 최종 부직포섬유에 대하여 살균성 금속함유 비다공성 무기세라믹 0.1~5중량% 되도록 폴리프로필렌 부직포를 제지한 후 그 표면에 폴리설폰, 폴리에스테르설폰, 폴리카보네이트 등으로 구성된 군으로부터 선택된 1종으로 미세다공층을 코팅한다.In order to achieve not only the object of the present invention but also another object that is easily expressed, in the present invention, a polypropylene containing a non-porous inorganic ceramic containing 2 to 50% of a bactericidal metal compound such as a silver compound and a zirconium compound in an inorganic ceramic 1 batch of polysulfone, polyestersulfone, polycarbonate, etc., made of polysulfone, polyestersulfone, polycarbonate, etc. to make a masterbatch and to make a polypropylene nonwoven fabric of 0.1-5% by weight of a non-porous inorganic ceramic containing germicidal metal to the final nonwoven fabric The microporous layer is coated with.
본 발명의 무기미립자 세라믹의 항균작용은 세라믹내에 함유된 항균금속 이온의 촉매작용에 의해 접촉하는 공기중의 산소를 이온화시키므로서 활성산소에 의한 미생물 세포의 호흡계, 전자전달계 등의 기본 대사계의 효소저해 혹은 세포막의 물질이동 저해로 설명될 수 있다.The antimicrobial action of the inorganic fine particle ceramic of the present invention ionizes oxygen in the air in contact with the catalytic action of the antimicrobial metal ions contained in the ceramic, thereby enzymatically acting on the basic metabolic system such as the respiratory system and the electron transfer system of microbial cells by active oxygen. Inhibition can be explained by inhibition of mass transfer of the cell membrane.
본 발명은 좀 더 상세하게 설명하면 다음과 같다.The present invention will be described in more detail as follows.
본 발명의 요지는 한외여과막의 보강지지체로서 사용되어져 왔던 폴리프로필렌 부직포를 항균성 재질로 사용함으로써 분리막을 이용하여 물을 정수할 때 정화수측에 세균이 검출되지 않도록 하는 것이다.The gist of the present invention uses polypropylene nonwoven fabric which has been used as a reinforcing supporter of an ultrafiltration membrane as an antimicrobial material so that bacteria are not detected on the purified water side when water is purified using a separation membrane.
종래에는 부직포에 항균성을 부여하기 위하여 항균제를 후처리하는 방법이 이용되었으나, 항균제 탈락에 의한 내구성 및 인체안정성 등의 문제가 있고, 또한 항균제로는 종래 제4급 암모늄염계(일본특개소 62-42715)나 키틴의 탈아세틸화물(일본특개평 4-272273)과 같은 유기계 항균제가 사용되었으나, 열에 대해 분해 및 증발을 일으키기 쉬워 내열성, 인체안정성 및 항균성 면에서 불리한 단점을 갖고 있으며 무기계 항균체의 경우도 다공성 물질인 제올라이트를 사용한 경우 다량의 수분을 흡수하여 부직포 제조시 방사공정 등에서 수분에 의한 폴리머 분해 등으로 인한 사절 및 강도저하 등의 악영향을 끼칠 수 있다.Conventionally, post-treatment of antimicrobial agents has been used to impart antimicrobial properties to nonwoven fabrics, but there are problems such as durability and human stability due to the removal of antimicrobial agents. Organic antibacterial agents, such as deacetylate of chitin and Japanese Patent Application Laid-Open No. 4-272273, have the disadvantages of heat resistance, human stability and antimicrobial properties because they are easily decomposed and evaporated against heat. In the case of using a zeolite, which is a porous material, it may absorb a large amount of moisture and may adversely affect trimming and strength reduction due to polymer decomposition by moisture in a spinning process, etc., in the manufacturing of a nonwoven fabric.
따라서, 본 발명에서는 무기미립자 세라믹을 폴리프로필렌, 장섬유 부직포 제조시 첨가하여 섬유내부에 존재되도록 하여 항균성을 부여한 폴리프로필렌 부직포를 제조하고 여기에 다공성 지지층인 폴리설폰을 코팅시켜 항균성 한외여과막을 제조하였다.Therefore, in the present invention, an inorganic particulate ceramic was added during the production of polypropylene and a long fiber nonwoven fabric to prepare a polypropylene nonwoven fabric having an antimicrobial property by being present in the fiber, and coated with a polysulfone, a porous support layer, to prepare an antimicrobial ultrafiltration membrane. .
본 발명에 있어서, 금속이온을 함유하는 무기세라믹의 첨가량은 최종 폴리프로필렌 부직포에 대하여 0.1~5중량%가 적당하여 가장 좋게는 0.2~2중량%가 바람직하다. 본 발명에 있어서 사용된 금속이온 함유 무기 세라믹의 경우에 있어서 항균성능의 효과는 무리세라믹 표면에 존재하는 금속이온의 양에 크게 의존한다. 본 발명에 있어서, 항균성을 효과적으로 발휘하기 위해서 무기세라믹에 함유된 금속의 종류는 은과 지르코늄으로서 함유량은 무기세라믹에 대하여 2~50중량%되게 하였으며 바람직하게는 5~40중량%되게 하였다.In the present invention, the addition amount of the inorganic ceramic containing metal ions is preferably 0.1 to 5% by weight relative to the final polypropylene nonwoven fabric, and most preferably 0.2 to 2% by weight. In the case of the metal ion-containing inorganic ceramic used in the present invention, the effect of the antimicrobial performance is largely dependent on the amount of metal ions present on the surface of the mulberry ceramic. In the present invention, in order to effectively exhibit antimicrobial properties, the metals contained in the inorganic ceramics are silver and zirconium, and the content is 2 to 50% by weight with respect to the inorganic ceramics, preferably 5 to 40% by weight.
무기세라믹의 첨가량이 0.1중량%미만이면 항균효과가 저하되고, 5중량%를 초과하면 폴리프로필렌사의 물성이 저하된다. 또한, 무기세라믹에 함유된 항균성 금속의 양이 2중량%미만이면 항균효과가 저하되고 50중량%를 초과하면 항균성의 증진효과가 없어 비경제적이다.If the amount of the inorganic ceramic added is less than 0.1% by weight, the antimicrobial effect is lowered. In addition, when the amount of the antimicrobial metal contained in the inorganic ceramic is less than 2% by weight, the antimicrobial effect is lowered.
본 발명에 있어서, 금속이온을 포함하는 무기세라믹을 부직포 섬유에 첨가하고 한외여과막을 만드는 방법을 폴리프로필렌 수지와 무기세라믹을 혼련기로 혼련하여 마스터배치 칩을 만들고 일반 부직포용 폴리프로필렌 수지와 적정비율로 혼합방사한 후 통상의 방법으로 부직포를 제조후 압착하여 막제조에 적합토록 한 후 폴리설폰 수지를 디메틸포름아마이드 용매에 20중량%로 녹여 50미크론 두께로 코팅하여 수응고시켜 한외여과막을 제조하였다.In the present invention, a method of adding an inorganic ceramic containing metal ions to a nonwoven fabric and making an ultrafiltration membrane is kneaded with a polypropylene resin and an inorganic ceramic with a kneader to make a masterbatch chip, and a suitable ratio with a polypropylene resin for general nonwoven fabric. After mixing and spinning, a nonwoven fabric was prepared by conventional methods and then pressed to make it suitable for the preparation of a membrane. The polysulfone resin was dissolved in 20% by weight of a dimethylformamide solvent, coated to a thickness of 50 microns, and coagulated with water to prepare an ultrafiltration membrane.
항균효과는 황색포도상 구균(ATTCC6538. Staphylococcus aureus)을 사용하여 한천배지에 배양균을 접종하여 37℃에서 24시간 배양한 균을 접종원으로 하여 시험편에 접종한 후 일정량의 액체를 가하여 시험편으로 부터 세균을 액중에 추출시킨다. 그 다음 처리 한외여과막과 미처리 한외여과막의 액중에 잔존하는 세균의 수를 측정하여 금속이온이 함유된 무기미립자 세라믹의 첨가로 인한 세균의 감소백분율을 계산하여 평가하였다.The antimicrobial effect was obtained by inoculating the agar medium with Staphylococcus aureus (ATTCC6538. Staphylococcus aureus), inoculating the test specimen with the incubator for 24 hours at 37 ° C, and adding a certain amount of liquid to the bacteria. Extract in liquid. Then, the number of bacteria remaining in the liquid of the treated ultrafiltration membrane and the untreated ultrafiltration membrane was measured and evaluated by calculating the percentage reduction of the bacteria due to the addition of inorganic fine ceramics containing metal ions.
다음의 실시예 및 비교예는 본 발명을 보다 상세히 설명하는 것이지만, 본 발명에 한정하지는 않는다.The following examples and comparative examples further illustrate the present invention in detail, but are not limited to the present invention.
실시예 1Example 1
일반적인 부직포 용도의 폴리프로필렌 수지(용융지수 35, 평균입경 200μ) 940중량부, 3.8중량%의 은과 35중량%의 지르코늄이 함유된 평균입경 0.4㎛의 무기세라믹 60중량부를 혼합기에 넣고 용융혼련기로 혼련한다. 이렇게 제조한 마스터배치 칩을 건조하여 칩표면의 수분을 제거한 후 용융지수 35의 부직포용 폴리르로필렌 칩과 혼합비율 1 : 9로 하여 용융방사하고 웹형성 및 열접착을 거쳐 부직포를 제조하고 일반용도의 폴리설폰을 디메틸 포름아마이드에 20중량%로 녹여 건조후 50미크론 두께가 되도록 코팅후 수응고시켜 한외여과막을 제조한 후 항균성 시험을 하여 표1에 나타내었다.940 parts by weight of polypropylene resin (melt index 35, average particle diameter: 200 μ) for general nonwoven fabrics, 60 parts by weight of an inorganic ceramic having an average particle diameter of 0.4 μm containing 3.8% by weight of silver and 35% by weight of zirconium are placed in a mixer. Knead. The masterbatch chips thus prepared were dried to remove moisture from the surface of the chip, melt spun with a non-woven polylopropylene filter having a melt index of 35 and a mixing ratio of 1: 9, and produced nonwoven fabric through web formation and heat bonding. The polysulfone of the purpose was dissolved in dimethyl formamide at 20% by weight, dried and coated to a thickness of 50 microns, and then coagulated to prepare an ultrafiltration membrane.
실시예 2Example 2
무기 세라믹 함유 마스터배치 칩의 제조에 있어서, 폴리프로필렌 파우더 886중량부, 무기세라믹 40중량부를 투입한 것 이외에는 실시예 1과 동일하게 실시하여 그 결과를 표1에 나타내었다.In the preparation of the inorganic ceramic-containing masterbatch chip, the same procedure as in Example 1 was conducted except that 886 parts by weight of polypropylene powder and 40 parts by weight of inorganic ceramic were added, and the results are shown in Table 1.
비교실시예 1Comparative Example 1
이산화티탄을 20중량% 함유한 폴리프로필렌 마스터배치 칩과 용융지수 35의 부직포용 폴리프로필렌 칩을 혼합비율 1 : 28로 혼합하고 용융방사하여 웨형성 및 열접착을 거친 것 외에는 실시예 1과 동일하게 실시하여 그 결과를 표1에 나타내었다.A polypropylene masterbatch chip containing 20% by weight of titanium dioxide and a polypropylene chip for nonwoven fabric having a melt index of 35 were mixed in a mixing ratio of 1:28, melt-spun and subjected to wetting and heat bonding in the same manner as in Example 1. The results are shown in Table 1.
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