CN100482316C - Microbe filter made from micropore ceramics - Google Patents

Microbe filter made from micropore ceramics Download PDF

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CN100482316C
CN100482316C CN 200510085530 CN200510085530A CN100482316C CN 100482316 C CN100482316 C CN 100482316C CN 200510085530 CN200510085530 CN 200510085530 CN 200510085530 A CN200510085530 A CN 200510085530A CN 100482316 C CN100482316 C CN 100482316C
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filter
ceramic
calcium phosphate
porous
porous ceramic
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CN1727032A (en )
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周和平
宁晓山
磊 杨
肖群芳
陈克新
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清华大学
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Abstract

本发明公开了属于医用和生活用过滤材料领域的涉及用于处理含有细菌和病毒的气体或液体的一种微孔陶瓷微生物过滤器。 The present invention discloses a microporous ceramic filters microorganism belonging to the field of medical and life of the filter material relates to a process for a gas or a liquid containing the bacteria and viruses. 该微孔陶瓷微生物过滤器是以磷酸钙盐微孔陶瓷为过滤媒介的。 The microbial filter is a porous ceramic calcium phosphate is a microporous ceramic filter media. 并可以在作为过滤媒介的磷酸钙盐微孔陶瓷中复合抗生剂。 Biocides and can be composited in a calcium phosphate porous ceramic filter media in. 本发明的微孔陶瓷微生物过滤器以具有亚微米孔隙结构的磷酸钙盐微孔陶瓷作为过滤媒介,能够有效地过滤流体中含有的细菌和病毒等微生物,复合抗生剂进一步提升产品对微生物的杀灭和抑制细菌和病毒效果。 Porous ceramic filter according to the present invention the microorganism to calcium phosphate ceramics having a microporous structure of submicron pores as a filter medium can be efficiently filtered fluid contained microorganisms like bacteria and viruses, to further enhance the composite biocide product to kill microorganisms destroy and inhibit bacterial and viral effect.

Description

微孔陶瓷微生物过滤器 Porous ceramic microbial filter

技术领域 FIELD

本发明属于医用和生活用过滤材料领域,特别涉及用于处理含有细菌和病毒的气体或液体的一种微孔陶瓷微生物过滤器。 The present invention belongs to the field of medical and life of the filter material, and particularly relates to a microporous ceramic microbial filter for processing a gas or a liquid containing the bacteria and viruses. 背景技术 Background technique

目前报道的细菌或病毒过滤器主要有: Currently reported bacteria or virus filters are:

(1) S •布林克-赛菲尔斯、R •普拉斯发明的"从水中物理地清除细菌悬浮物质和固体颗粒的过滤器装置"(中国专利第1196518号)。 (1) S • Brink - "remove bacteria and suspended solids from the solids filter means water physically" Saifeiersi, R • Plath invention (Chinese Patent No. 1196518). 该发明采用紧密排列的空心纤维组成的膜板作为过滤件,空心纤维膜壁之间具有在0.00广1.0um 之间的缝隙(width),能够从水中过滤细菌和固相颗粒。 The invention employs a diaphragm closely spaced hollow fibers as a filter element, a gap of between 0.00 1.0um wide (width) between the wall of the hollow fiber membranes, capable of filtering bacteria from water and solid particles.

(2) 王晓宁等人发明的"一种对人体血浆病毒进行过滤的方法和装置"(中国专利CN1531978A)。 "A method and apparatus for filtering human plasma virus" (2) Xiaoning invention et al (China patent CN1531978A). 该装置采用有机高分子多孔膜或对病毒有亲和性的过滤膜相结合的方法,来分离血浆中的病毒。 The device uses a porous organic polymer membrane or membrane filtration affinity method of combining the virus, the virus is isolated plasma.

(3) 由Tsuru Sumiaki等人申请的"filter sheet"的欧洲专利EP0673667 (1995年9月27日)中的过滤材料。 (3) the application by Tsuru Sumiaki et al "filter sheet" European patent EP0673667 (1995 September 27) filter material. 该过滤材料将磷酸钙化合物的粉末或多孔 The filter material or porous calcium phosphate compound powder

颗粒分散于有机高分子材料中作为过滤媒介,用于过滤有害气体和病毒。 Particles are dispersed in an organic polymer material as a filter media for filtering the harmful gases and viruses.

(4) 由S. Masmoudi, R. Ben Amar, A. Larbot, H. El Feki, A. Ben Salah, L. Cot发表在《Jo固al of Membrane Science》上(2005年,Vol.247: 1 -9) 题为"Elaboration of inorganic microfiltration membranes with hydroxyapatite applied to the treatment of wastewater from sea product indiistir"中的陶瓷过滤器。 (4) published by S. Masmoudi, R. Ben Amar, A. Larbot, H. El Feki, A. Ben Salah, L. Cot on "Jo solid al of Membrane Science" (in 2005, Vol.247: 1 -9) entitled "Elaboration of inorganic microfiltration membranes with hydroxyapatite applied to the treatment of wastewater from sea product indiistir" ceramic filter. 作者将羟基磷灰石陶瓷颗粒涂敷在多孔堇青石支撑体表面,经干燥和600。 The ceramic particles of the hydroxyapatite coated porous cordierite support surface, dried and 600. C烧结后在多孔堇青石支撑体上形成了一层厚度约32. 5 um, 平均孔径为0.5"m,气孔率为48%的过滤膜。此陶瓷过滤器可用于过滤海产生 After C is formed on the porous sintered cordierite support having a thickness of about 32. 5 um, an average pore diameter of 0.5 "m, a porosity of 48% of the filter membrane. This may be a ceramic filter for filtering sea produce

产污水中的有机物成分、细菌和盐分。 Production of organic component in water, bacteria and salt.

(5) Syguru Suzuki, Kenji Itoh, Masako 0hgaki, Masaya 0htani, Masakuni 0zawa发表在《Ceramics International》1999年,第25巻第287-291页上的题为"Preparation of sintered fi丄ter for ion exchange by a doctor blade method with aqueous slurries of needlelike hydroxy即atite,,中的陶瓷过滤器。该陶瓷过滤器利用溶胶凝胶法合成的具有针状晶形的羟基磷灰石陶瓷粉体作为原料,经刮刀流延工艺成型、在高温烧结而成。该多孔陶瓷的孔径分布从数微米到十几微米不等,被试验用于过滤含有重金属Pb2 +离子的溶液(0.025mol7U,结果显示一次过滤能够去除59%的Pb2+, 5次过滤就能完全去除溶液中的Pb2+。最近他们发现这种过滤器对蛋白质有很好的吸附效果(0. Takagi, N. Kuramoto, M. 0zawa, S. Suzuki发表在《Ceramics Interaational》 2004年第30巻第139-143页上的题为"Adsorption/desorption of acidic and basic proteins on needle-like hydroxy邻atite filter pre (5) Syguru Suzuki, Kenji Itoh, Masako 0hgaki, Masaya 0htani, Masakuni 0zawa published in "Ceramics International" in 1999, entitled "on Volume 25, page 287-291 Preparation of sintered fi Shang ter for ion exchange by a doctor blade method with aqueous slurries of needlelike hydroxy ,, i.e. atite the ceramic filter. the ceramic filter synthesis using a sol-gel hydroxyapatite ceramic powder having a needle crystal form as the starting material, by a doctor blade casting process molding, sintering at a high temperature. the pore size distribution from porous ceramics several microns to tens of microns range, being used to filter the test solution containing heavy metal ions Pb2 + (0.025mol7U, the results show a filter capable of removing 59% of Pb2 + , five times filtered able to completely remove the solution Pb2 +. recently, they found that the filter has a good protein adsorption (0. Takagi, N. Kuramoto, M. 0zawa, S. Suzuki, published in "Ceramics Interaational" entitled the 2004 Volume 30, pp. 139-143 "Adsorption / desorption of acidic and basic proteins on needle-like hydroxy neighbor atite filter pre pared by slip casting")。 pared by slip casting ").

上述微'生物过滤器的基本原理是机械阻挡,所选用的过滤媒介的孔径必须小于所过滤的微生物的尺寸。 Micro above 'basic principle of the biological filter is a mechanical barrier, the pore size of the filter medium is selected to be smaller than the size of the filtered microbes. 这些过滤器虽然能够过滤直径为0.5-5ym的细菌, 但很难过滤直径为10 —500nm的病毒。 Although these filters capable of filtering bacteria 0.5-5ym diameter, it is difficult to filter viruses having a diameter of 10 -500nm. 这是因为一方面现有技术很难制造出具有纳米量级的微孔材料,而另一方面即使能够制备出纳米孔隙,过滤时所需要的压力将非常大,而且被截留的微生物会迅速地堵塞滤膜,造成过滤压力剧增和过滤器失效。 This is because on the one hand the prior art is difficult to manufacture a microporous material having a nano-order, on the other hand can be prepared even if the nanopores, the pressure required for filtration will be very large, and entrapped microorganisms rapidly clogging the membrane, causing pressure surge filtered and the filter failure. 上述有些过滤器虽然也利用了吸附效应,但由于它们一般采用薄膜结构或者孔径较大,吸附效果有限。 Although some of the above filter is also used adsorption effects, but because they are generally thin-film structure or a larger pore size, suction effect is limited.

发明内容 SUMMARY

本发明的目的是提供一种能够有效过滤细菌和病毒的,对人体和环境完全无 Object of the present invention is to provide an effective filtration of bacteria and viruses, humans and the environment completely

毒无害的微孔陶瓷微生物过滤器,其特征在于:所述微孔陶瓷微生物过滤器是以 Porous ceramic filters toxic harmless microorganism, wherein: said porous ceramic is a microbial filter

磷酸钙盐微孔陶瓷作为过滤媒介; Calcium phosphate porous ceramic as a filter medium;

所述磷酸钙盐微孔陶瓷的气孔率范围为10%〜75%。 The calcium phosphate porous ceramic porosity in the range of 10% ~ 75%. 所述磷酸钙盐微孔陶瓷中的孔隙直径范围为0. 1 um〜200 um。 Pore ​​diameter of said porous calcium phosphate ceramic is 0. 1 um~200 um. 所述的微孔陶瓷微生物过滤器的另一种过滤媒介为采用复合有抗生剂的磷 Another porous ceramic filter according microbial filter medium for use with a phosphorus compound biocide

酸钙盐微孔陶瓷。 Calcium salt of porous ceramics.

本发明的有益效果是以微孔磷酸钙盐生物陶瓷作为微生物过滤的主要媒介,对人体完全无害且与生物机体有良好的相容性。 Advantageous effects of the present invention is primarily a microporous calcium phosphate bioceramics medium microorganisms filtration, and completely harmless to humans and living organisms have good compatibility. 微孔陶瓷具有大量的亚微米孔隙,能够有效的吸附和阻挡尺寸很小的病毒和细菌,同时在微孔陶瓷中引入一定体积的大孔径连通孔隙,使过滤器在保持过滤效果的同时具有良好的渗透性能且不容易被堵塞,进而提高了过滤效率和过滤器的使用寿命。 A large number of porous ceramic having submicron pores, can effectively block adsorption and very small size of viruses and bacteria, while introducing a volume of large pore size in the porous ceramic communicating pores, the filter having a good filtering effect while maintaining penetration properties not easily clogged, thereby increasing the life of the filter and filtration efficiency. 还通过在过滤媒介中复合抗生剂进一步提升产品对微生物的杀灭和抑制效果。 Further enhance the killing of microorganisms and the products inhibiting effect of the composite filter media in the biocides. 具体实施方式 detailed description

本发明提供一种微孔陶瓷微生物过滤器。 The present invention provides a microporous ceramic microbial filter. 该微孔陶瓷微生物过滤器是以磷酸钙盐微孔陶瓷作为过滤媒介。 The microbial filter is a porous ceramic porous calcium phosphate ceramics as a filter medium. 并在作为过滤媒介的磷酸钙盐微孔陶瓷中复合抗生剂进一步提升产品对微生物的杀灭和抑制效果。 Biocides and compounded in a calcium phosphate porous ceramic filter medium to further enhance the killing of microorganisms and the product inhibitory effect. 下面例举实施例予以说明。 The following example embodiment will be described.

实施例1 Example 1

将磷酸,丐盐陶瓷粉体与作为造孔剂的水溶性淀粉和不可溶淀粉按体积比4: 3: 3在去离f水中充分混合,所得到的浆料经干燥、研磨,过筛后,干压成型。 After thorough mixing from 3 to f in water, the resulting slurry was dried, ground and screened to: phosphoric acid, a salt cai ceramic powder soluble starch as a pore former and insoluble starch by volume ratio 4: 3 , dry pressing.

将压片置于箱式电阻炉中在120(TC烧结得到多孔陶瓷。烧结成的多孔陶瓷外观规整,经XRD测试其主要成份仍是磷酸钙盐。该陶瓷的气孔率为50%, SEM观察显示陶瓷同时含有亚微米孔隙和孔径较大的连通气孔,亚微米孔隙的孔径分布范围在0.l!xm〜lum之间,连通气孔的孔径分布范围从数微米到几十微米不等,连通气孔的体积占陶瓷总体积的38%。 The pellet was placed under observation (TC sintered to obtain a porous ceramics sintered porous ceramic neat appearance, by the XRD measurement is still the main ingredient calcium salt of the ceramic porosity of 50%, SEM Box resistance furnace at 120 ceramics containing both display a greater porosity and pore size of submicron communication pore, the pore size distribution of pores in the submicron range 0.l! between xm~lum, intercommunicating pores of pore size distribution from several microns to tens of microns, communication 38% of the volume of the pores of the total volume of the ceramic.

将此陶瓷过滤器用于过滤浓度大于105个/ml的大肠杆菌悬液,结果显示100 %的大肠杆菌能够被此陶瓷过滤器所过滤。 This ceramic filter for filtering a concentration of greater than 105 / ml suspension of E. coli, the results showed 100% of E. coli can be filtered by the ceramic filter. SEM观察显示大肠杆菌被吸附在磷酸钙微孔陶瓷„中,其中一定数量的大肠杆菌被亚微米孔隙直接阻挡。说明该陶瓷过滤器对细菌有明显的过滤效果。 SEM observations indicate that the E. coli is adsorbed calcium phosphate porous ceramic ", where a certain number of E. coli is directly blocked submicron pores. Description The ceramic filter bacteria significant filtering effect.

将此陶瓷过滤器用于过滤滴度为100TCID5。 This ceramic filter for filtering titer 100TCID5. /ml的呼肠病毒(3型)悬液,将过滤后的病毒悬液接种于HeLa细胞以观察病毒的感染能力。 / Ml of reovirus (type 3) suspension, the filtered virus suspension was inoculated into HeLa cells infected observation. 结果显示,经过过滤的样品两天后没有可察的细胞病变,而此时作为对照的未过滤样品中已经有部分细胞发生病变;五天后,未经过滤的样品中的全部细胞发生病变,而经过过滤样品只有25〜50%的细胞发生病变,说明该陶瓷过滤器对病毒有过滤或抑制效果。 The results showed that, after the filtered samples can be observed two days without cytopathic, at a time when the unfiltered sample as a control part already diseased cells; After five days, all of the unfiltered sample cell lesions occur, but after filtering the sample cell only 25~50% of lesions, indicating that the virus ceramic filter with a filter or inhibitory effect. 实施例2 Example 2

将实施例1中所述的陶瓷过滤器置于浓度为0. 2mol/L的AgN(V溶液中浸泡1 小时后取出、在6CTC干燥。XRD测试显示该陶瓷的主要成分磷酸钙盐外,还有Ag3P04,说明银离子抗生剂已经通过置换反应复合到了陶瓷过滤器中。 The ceramic filter in Example 1 was placed in a concentration of 0. 2mol / L after 1 hour of extraction AgN (V soaking solution, show a main component of the ceramic dried .XRD 6CTC calcium phosphate in the test, but also there Ag3P04, biocides described silver ions have complexed to the ceramic filter through a displacement reaction.

将此陶瓷过滤器置于浓度大于10'5个/ml的大肠杆菌悬液中,经摇瓶法测试其杀灭细菌的效果。 This ceramic filter is placed E. coli suspension concentration greater than 10'5 cells / ml, the shake-flask method was tested for its effect of killing bacteria. 结果显示,100%的大肠杆菌被杀灭或抑制,说明复合了银离子抗生剂可以进一步提高的陶瓷过滤器的抗菌效果。 The results showed that 100% of E. coli killing or inhibiting the described antibacterial effect of silver ions complexed antibiotic agents may be further improved ceramic filter.

将此陶瓷过滤器用于过滤呼肠病毒(3型)悬液,方法和条件与实施例l相同。 This ceramic filter for filtering reovirus (type 3) suspension, and the method and conditions the same as in Example l embodiment. 结果显^^,经过过滤的样品前三天都没有使细胞发生可察的病变,此结果明显优于实施例l中的结果。 ^^ significant results after three days prior to filtration of the sample may be observed in cells without lesions, this result was significantly better than the results in Example l embodiment. 五天后,经过过滤的样品虽然也有25〜50%的细胞发生了病变,但详细观察表明细胞发生病变的数目明显少于实施例1中的经过过滤样品发生病变的细胞数目。 After five days, the filtered samples, although there 25~50% of diseased cells, but the number of cells observed in detail lesions showed significantly less cytopathic number of embodiments of the filtered sample in Example 1 occurred. 上述结果说明复合了银离子抗生剂可以进一步提高的陶瓷过滤器的抗病毒效果。 These results indicated that the complex of silver ion biocide can be further improved ceramic filter antiviral effect.

比较例1 Comparative Example 1

将磷酸钙盐陶瓷粉体与有机单体和表面活性剂在未离子水中混合,利用搅拌气泡和有机单体的原位聚合成型多孔陶瓷的生坯,经干燥后置于箱式电阻炉中在120(TC烧结。烧结成的多孔陶瓷气孔率为79%, SEM观察其含有孔径很大的连通气孔,孔隙的孔径分布较宽,范围在几个微米到270pm之间,连通气孔的体积占陶瓷总体积的63%,基本不含有亚微米的孔隙结构。 The calcium phosphate ceramic powder with an organic monomer and non-ionic surface active agent in water and mixing, polymerization by in situ molding of the porous ceramic green organic monomer bubbles and stirred, after drying box was placed in a resistance furnace 120 (TC sintered. sintered porous ceramic porosity of 79%, SEM observation of containing intercommunicating pores large, wide pore size distribution of the porosity of the aperture, the range between a few microns to 270pm, by volume of intercommunicating pores of the ceramic 63% of the total volume, containing substantially submicron pore structures.

细菌过滤结果显示,只有66. 7%的大肠杆菌被过滤。 Bacterial filtration showed only 66.7% of E. coli was filtered. 此结果说明该陶瓷过滤器未能有效'地过滤微生物。 This result indicates that the ceramic filter can not effectively 'filtered microbes.

本发明所选用的磷酸钙盐是自然界最重要的生物矿物之一,是天然骨和牙的主要无机成分,其代表是羟基磷灰石,到目前为止,以羟基磷灰石为代表的磷酸钙盐陶瓷已经被证明具有良好的生物适应性、无细胞毒性、且可与骨组织形成良好的键合等优点,因此被广泛地研究与使用于骨组织的替代和移植。 The choice of calcium phosphate of the present invention is one of the most important biological mineral nature, the major inorganic component of natural bone and tooth, which is representative of hydroxyapatite, so far, as represented by hydroxyapatite calcium phosphate ceramic salt has been shown to have good biocompatibility, non-cytotoxic, and can form a good bond with the bone tissue, etc., which is widely studied and used in bone tissue replacement and transplantation. 选用磷酸钙盐生物陶瓷能够保证产品安全无毒。 Selection of calcium phosphate bioceramic to ensure product safety non-toxic.

磷酸钙盐陶瓷复杂的结构使其具有很多的置换或吸附位置,例如羟基磷灰石中包括Ca2+形成的离子置换位或吸附位,(P04)3—形成的离子置换位或吸附位,以及(0H)—形成的氢键等,证明羟基磷灰石对各种阴阳离子,蛋白质和生物大分子有置换或吸附作用。 Calcium phosphate ceramic having a complicated structure so many substitutions or suction position, e.g. hydroxyapatite comprises Ca2 + ion substitution bit or adsorption site formation, (P04) 3- ion substitution position or adsorption site formation, and ( 0H) - hydrogen bond formation, have proved substitution or hydroxyapatite adsorption of various anions and cations, proteins, and biological macromolecules. 发明人通过研究证实了这种磷酸钙盐陶瓷对细菌和病毒有明显的吸附效'果,而且由于多孔的磷酸钙盐陶瓷具有非常大的比表面积,因此非常适合作为微生物的过滤和吸附材料。 The inventors have confirmed this by studying calcium phosphate ceramics have significant adsorption effect 'results against bacteria and viruses, but also since the porous calcium phosphate ceramic having a very large specific surface area, and therefore well suited as a filter and adsorbent of microorganisms. 研究表明合适的连通孔隙尺寸为5〜200um, 连通孔的体积为陶瓷体积的5〜60%。 Studies have shown that a suitable pore size of the communication 5~200um, the volume of communication holes is 5 to 60% by volume of a ceramic. 连通孔隙尺寸过大,数量过多容易使微生物随流体快速通过过滤器而没有被吸附或阻挡,造成过滤器失效。 Communicating pore size is too large, an excessive number of microorganisms with the fluid tends to quickly pass through the filter without being adsorbed or blocked, resulting in failure of the filter. 孔径过小或连通孔体积过小,则难以连通。 Pore ​​volume of the communication hole is too small or too small, it is difficult to communicate.

气孔率是影响陶瓷过滤器过滤效率和过滤压力的一个重要参数。 The porosity is an important parameter of the ceramic filter and the filtration efficiency of the filtration pressure. 气孔率低于10%的陶瓷^已经不透气,而气孔率高于75%的陶瓷在过滤时会发生破坏或已经不能有效的过滤微生物。 Less than 10% porosity has a ceramic airtight ^, whereas 75% of the high porosity ceramic or destruction of microorganisms by filtration can not effectively occur during filtration.

研究还发现在上述磷酸钙盐微孔陶瓷过滤器上复合抗生剂可以进一步提高过滤器对微生物的杀灭和抑制效果。 The study also found that calcium salts on said porous ceramic filter composite biocide killing the filter can be further improved and the effect of suppressing microorganisms. 所采用的银离子抗生剂具有抗菌抗病毒效果明显,效用持久等优点,已经被广泛的应用于医疗器械、卫生洁具和生活用品, 而且,载银羟基磷灰石的安全性己经被世界卫生组织所接受。 Silver ion biocide used having antibacterial and antiviral effect is obvious, lasting effectiveness, etc., has been widely used in medical equipment, sanitary and household goods, and, silver hydroxyapatite have been security WHO organization accepted.

本发明通过进一步在上述过滤媒介上复合抗生剂得到具有明显杀灭细菌和病毒效果的过滤器产品。 The present invention has significant effects kill bacteria and viruses filters the composite product obtained by further biocide on the filter medium. 所选用的抗生剂对人体也是安全无害的,从而保证了整个产品的安全和无害。 The choice of antibiotic agents is safe and harmless to the human body, thus ensuring the safe and sound the entire product.

Claims (4)

  1. 1. 一种微孔陶瓷微生物过滤器,其特征在于:该微生物过滤器是一种微生物病毒过滤器,所述微生物病毒过滤器是以具有0.1μm<孔隙直径≤1μm微孔的磷酸钙盐多孔陶瓷作为过滤媒介。 1. A microporous ceramic microbial filter, wherein: the microorganism is a microbial filter virus filters, the microorganism is a virus filter having a porous calcium phosphate <micropores of pore diameter 0.1μm ≤1μm ceramics as a filtration medium.
  2. 2. 根据权利要求1所述微孔陶瓷微生物过滤器,其特征在于,所述磷酸钙盐微孔陶瓷的孔隙直径范围为0.1 ii m〈孔隙直径《200u m, 气孔率范围为10%-75%。 1 2. The porous ceramic filter as claimed in claim microorganism, wherein said calcium phosphate porous ceramic pore diameter in the range 0.1 ii m <pore diameter "200u m, a porosity in the range 10% to 75 %.
  3. 3. 根据权利要求1或2所述微孔陶瓷微生物过滤器,其特征在于, 磷酸钙盐微孔陶瓷还含有抗生剂。 3. The porous ceramic of claim 2 or a microbial filter, wherein the porous calcium phosphate ceramic further contains antibiotic agents.
  4. 4. 根据权利要求3所述微孔陶瓷微生物过滤器,其特征在于,所述抗生剂为银离子抗生剂。 4. The microbial filter 3 Porous ceramic claim, wherein the biocide is a silver-ion biocide.
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US5310548A (en) 1989-04-21 1994-05-10 Asahi Kogaku Kogyo Kabushiki Kaisha Deodorants, deodorant sheets, filter sheets and functional papers as well as filtering mediums for exhaust gas

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