CN106518006A - In-situ composite antibacterial filtering ceramic as well as preparation method and application thereof - Google Patents
In-situ composite antibacterial filtering ceramic as well as preparation method and application thereof Download PDFInfo
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- CN106518006A CN106518006A CN201610994399.9A CN201610994399A CN106518006A CN 106518006 A CN106518006 A CN 106518006A CN 201610994399 A CN201610994399 A CN 201610994399A CN 106518006 A CN106518006 A CN 106518006A
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- silver
- diatomite
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- 239000000919 ceramic Substances 0.000 title claims abstract description 58
- 238000001914 filtration Methods 0.000 title claims abstract description 40
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 29
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 16
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052709 silver Inorganic materials 0.000 claims abstract description 33
- 239000004332 silver Substances 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 19
- 244000005700 microbiome Species 0.000 claims abstract description 17
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 15
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 29
- 230000000845 anti-microbial effect Effects 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 229910019142 PO4 Inorganic materials 0.000 claims description 8
- 159000000007 calcium salts Chemical class 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 8
- 239000010452 phosphate Substances 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical group [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 230000002147 killing effect Effects 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 4
- -1 boccaro Chemical compound 0.000 claims description 4
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000004254 Ammonium phosphate Substances 0.000 claims description 3
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 3
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 2
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000005909 Kieselgur Substances 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims 1
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims 1
- 238000007493 shaping process Methods 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 12
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000004576 sand Substances 0.000 abstract 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 29
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 230000001954 sterilising effect Effects 0.000 description 10
- 241000894006 Bacteria Species 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000003651 drinking water Substances 0.000 description 5
- 235000020188 drinking water Nutrition 0.000 description 5
- 238000004659 sterilization and disinfection Methods 0.000 description 5
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical group [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 4
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 3
- 201000010099 disease Diseases 0.000 description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000012736 aqueous medium Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910000397 disodium phosphate Inorganic materials 0.000 description 2
- 235000019800 disodium phosphate Nutrition 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 238000006385 ozonation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- VWDWKYIASSYTQR-YTBWXGASSA-N sodium;dioxido(oxo)azanium Chemical compound [Na+].[O-][15N+]([O-])=O VWDWKYIASSYTQR-YTBWXGASSA-N 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 208000035473 Communicable disease Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- SXDBWCPKPHAZSM-UHFFFAOYSA-M bromate Inorganic materials [O-]Br(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-M 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000003113 dilution method Methods 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 208000001130 gallstones Diseases 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 229940100890 silver compound Drugs 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 208000017520 skin disease Diseases 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 241001515965 unidentified phage Species 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/131—Inorganic additives
-
- 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
- B01D39/2068—Other inorganic materials, e.g. ceramics
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/1305—Organic additives
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
- C04B38/085—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances of micro- or nanosize
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0442—Antimicrobial, antibacterial, antifungal additives
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/40—Metallic constituents or additives not added as binding phase
- C04B2235/408—Noble metals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/447—Phosphates or phosphites, e.g. orthophosphate or hypophosphite
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Structural Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Filtering Materials (AREA)
Abstract
The invention relates to antibacterial filtering ceramic, in particular to in-situ composite antibacterial filtering ceramic as well as a preparation method and application thereof. The composite antibacterial filtering ceramic is prepared from the following components in percentage by mass: 60 to 75 percent of kieselguhr, 10 to 20 percent of hydroxyapatite, 10 to 30 percent of purple sand, 0.1 to 2 percent of silver and 1 to 5 percent of an adhesive, and the mass percentage sum of the five components is 100 percent. The diameter of the silver is 3 to 20 nm, and the silver is located on the surface and in gaps of the kieselguhr. According to the in-situ composite antibacterial filtering ceramic, combination of nano silveer and porous kieselguhr, combination of the silver and the hydroxyapatite and combination of silver-carried hydroxyapatite and the porous kieselguhr are realized under a hydrothermal condition, so that the dispersivity of the silver and the binding force of the silver and a material are improved. The material is high in filtering performance, antibacterial property and antibacterial endurance, can effectively filter out microorganisms, impurity particles and organic matters from water, and can be widely applied to the field of water treatment and relevant industries.
Description
Technical field
The present invention relates to a kind of antimicrobial filtering ceramics, more particularly to a kind of In-situ reaction antimicrobial filtering ceramics and its preparation side
Method and application.
Background technology
With the increasingly raising of people's living standard, improve drinking water quality, ensure drinking water safety, have become full people
The topic of class concern.WHO investigation results show：Drinking contaminated water can cause disease of digestive tract, skin disease, infectious disease, sugar
More than the 50 kinds of diseases such as urine disease, cancer, gall stone.At present, China's urban waters more than 90% are polluted by different degrees of, wherein
78% water quality of river does not meet sanitary standard, 75% lake eutrophication, 50% city zone groundwater serious pollution.Therefore
Purified treatment is carried out to drinking water to be of great immediate significance.
At present, China's city tap-water factory is mostly using conventional water treatment processes such as coagulation, precipitation, filtration, sterilizations.Its
In, at water source, the conventional sterilization method of head has cholorination, ozonization, disinfection by ultraviolet light, and water terminal commonly uses membrane filtration, absorption
Technology, ceramic foam filter etc..Although these technologies have certain sterilised filtration effect, but the drawbacks of all have obvious.It is conventional
Cholorination be also easy to produce harmful side product and to the clearance of Organic substance in water generally only 20～30%, ozonization cost
Big and be also easy to produce the harmful side products such as formaldehyde, bromate ion, the water of Jing ultraviolet disinfections is easily grown in pipe network course of conveying again
Raw microorganism.Although membrane filtration can obtain excellent water quality, there are problems that film blocking, fouling membrane with.Adsorption material
Activated carbon is the most common are in material, the suspended particulate that effectively can go in eliminating water, organic matter etc., but due to its good bio-compatible
Property and chemical compatibility, in water microorganism easily absorption organic matter activated carbon on breed, become microbial reproduction " temperature
Bed ", and activated carbon recycles high cost.Although porous ceramics can effective filter out microorganism, impurity particle, and produce and
Recycling low cost, it is but the same with activated carbon, can only retain microorganism and can not be by its thorough killing, microorganism easily assembles shape
Into biomembrane, secondary pollution is caused.
The bactericidal property that silver-colored porous ceramics combines the strainability and silver of porous ceramics is carried, becomes water process neck in recent years
The study hotspot in domain.Silver-colored porous ceramics is carried to including common cause in 15 kinds of water including E.Coli, S.aureus and MS2 bacteriophage
The average rejection rate of sick microorganism is more than 99%.Spraying process and infusion process are to carry the most frequently used preparation method of silver-colored porous ceramics.So
And spraying process has the shortcomings of silver ion adhesion is weak, release is fast, after one month, the silver ion burst size in material is accounted for always
The 20-22% of silver carrying amount.Silver of the infusion process inside drying stage is easily enriched with the evaporation of moisture and segregates to ceramic surface,
So that it is uneven to carry silver.Some documents are directly incorporated into silver nano-grain in ceramic raw material, obtain carrying silver-colored many Jing after high temperature sintering
Hole ceramics.Although the method can strengthen the adhesion of silver, under high temperature, silver nano-grain is easily reunited and loses nano effect.
Diatomite has performances such as bigger serface, high porosity, strong adsorptivity, and rich reserves, cheap, fits
Porous filter material is done in conjunction.Nano-Ag particles size is little, specific surface area big, activity is high, has extremely strong killing effect to microorganism.Hydroxyl
Ca in base apatite2+Easily be substituted with metal ions, be adapted to do the carrier of silver, in addition hydroxyapatite Organic substance in water is had compared with
Strong adsorption capacity.Boccaro has good plasticity, is conducive to ceramic body to be molded, and its double multi-hole structure and water-quality activating are made
With significant to water process.
Therefore, the advantage of above-mentioned material is combined, prepares a kind of new In-situ reaction antimicrobial filtering ceramics, make silver
Can be securely joined with ceramics and be uniformly distributed with nano-scale, will be a significant technological progress.
The content of the invention
An object of the present invention is to provide a kind of In-situ reaction antimicrobial filtering ceramics, by diatomite, hydroxyapatite,
Boccaro, silver and binding agent composition, the mass percent of each component are followed successively by 60～75wt%, 10～20wt%, 10～30wt%,
The mass percent sum of kind of the component of 0.1～2wt%, 1～5wt%, five is 100wt%.
Wherein, the diatomite purity is food-grade, and size controlling was the powder of 100 mesh sieves；The boccaro is broken for Jing
Broken, removal of impurities simultaneously crosses the boccaro powder that 100 mesh sieves are obtained.The hydroxyapatite particle size range is 30～300nm.It is described silver it is straight
Footpath is 3～20nm, in diatomite surface and hole.The binding agent is sodium carboxymethylcellulose, hydroxypropyl methyl fiber
One or more in element, hydroxymethyl cellulose, polyvinyl alcohol, polyethylene glycol.
The second object of the present invention is to provide the In-situ reaction antimicrobial filtering ceramic preparation method, and concrete grammar is
The compound and silver carrying hydroxyapatite of Nano Silver compound, silver diatomaceous with porous and hydroxyapatite is realized under hydrothermal conditions
Stone is diatomaceous with porous compound, improves the dispersiveness of silver, strengthens silver with the adhesion of material.
The present invention is employed the following technical solutions：
(1) according to Ca/P stoichiometric proportions be 1.67/1, configuration 0.1～0.5mol/L phosphate solutions, 0.1～
0.5mol/L calcium salt solns, and phosphate solution pH=8～12 are adjusted with ammoniacal liquor；
(2) by a certain amount of AgNO3Solid is dissolved in adding calcium salt soln, and adds a certain amount of diatomite to stir,
Obtain diatomite mixed solution；
(3), after phosphate solution being added dropwise in diatomite mixed solution and is stirred continuously, pouring in reactor is carried out
Hydro-thermal reaction；
(4) reactant liquor that step (3) is obtained is filtered and deionized water and ethanol is washed in filtrate being in substantially
Property (pH=6～8), drying obtain dry powder；
(5) by dry powder with boccaro by certain mass is than dispensing and adds a certain amount of binder solution, be fully uniformly mixed so as to obtain
Compound；
(6) compound is put into into compressing in mould or injection forming, drying, high-temperature calcination, after along with the furnace cooling
To In-situ reaction antimicrobial filtering ceramics.Further, step (1) phosphate is diammonium hydrogen phosphate, disodium hydrogen phosphate or phosphorus
Sour ammonium, the calcium salt are calcium nitrate or calcium chloride.
Further, in step (2), AgNO3Solid, diatomite, the amount ratio of calcium salt soln are (0.2～1g):(20～
50g):(200～500mL)；Step (5) dry powder is (70 with the mass ratio of boccaro:30)～(90:10).
Further, realization silver, hydroxyapatite and diatom under the conditions of 100～240 DEG C of hydrothermal temperature, pH=8～12
Native In-situ reaction.
Further, the concentration of binder solution described in step (5) is 10g/L～30g/L.
Further, in step (6), it 8～12MPa, dwell time is 20～60s that briquetting pressure is, baking temperature 60～
100 DEG C, 900～1200 DEG C of calcining heat, 4～6h of calcination time.
The third object of the present invention is the application for providing the In-situ reaction antimicrobial filtering ceramics in terms of water process：Institute
State In-situ reaction antimicrobial filtering ceramics to can be used to filtering and killing the microorganism in water.Preferably, the microorganism is E.Coli
And S.aureus.
The present invention compared with prior art, has the advantage that and beneficial effect：
In In-situ reaction antimicrobial filtering ceramics prepared by the present invention, argentum-carried hydroxylapatite is former on diatomite surface and hole
Position nucleation simultaneously grows, and silver is uniformly distributed in whole material with nano-grade size.In-situ reaction prepares method, on the one hand improves and receives
The dispersiveness of meter Yin and nano silver-carrying hydroxyapatite, it is to avoid agglomeration, on the other hand enhances the adhesion of silver and material,
Make material that there is efficient, stable, permanent anti-microbial property.Silver-colored release experiment shows, releases of this material 24h in aqueous medium
Amount only 0.43 μ g/L, are less than the requirement of 50 μ g/L far below health ministry to silver in drinking water content.Antibacterial experiment shows, this
Plant material 3h and 3h and 100% is to the sterilizing rate of E.Coli and S.aureus later.By 106The bacterium solution of cfu/mL is by ceramics
Piece, and in filtrate, inspection does not measure bacterium colony group, shows that this material has good filtration result to microorganism.
Between the diatomite particle in ceramics, micron order hole can retain the larger microorganism of body and impurity particle, make current
Pass through, so as to improve filtering rate；What the hole of diatomite 200-400nm itself and nano-hydroapatite particles were formed
Less microorganism, impurity particle and organic matter etc. in the adsorbable water in gap, so as to ensure filtering accuracy.By micron order hole and
The microorganism of nanoscale hole retention can be killed by the Nano Silver in diatomite and argentum-carried hydroxylapatite quickly, reach antibacterial effect
Really.Additionally, as current take away the silver of denier by ceramic dielectric, the silver in filtrate can play certain suppression to microorganism
System, killing action are so as to ensureing filtrate not microbial contamination.
In-situ reaction antimicrobial filtering ceramics disclosed by the invention are a kind of novel antibacterial filtering materials, with excellent suction
It is attached, filter, activated water function, and good antibiotic property, antimicrobial sustained-release and persistence, and preparation method is simple, raw material
Inexpensively, water treatment field and relevant industries be can be widely applied to.
Description of the drawings
Fig. 1 is In-situ reaction antimicrobial filtering ceramics ESEM (SEM) photo prepared by the embodiment of the present invention 1.
In the In-situ reaction antimicrobial filtering ceramics that Fig. 2 is prepared for the embodiment of the present invention 1, diatomite particle nano surface silver is saturating
Radio mirror (TEM) photo.
Fig. 3 is In-situ reaction antimicrobial filtering ceramics antibacterial experiment photo prepared by the embodiment of the present invention 1, wherein (a) is
E.Coli blanks, are (b) S.aureus blanks, (c) be composite ceramics to E.Coli bactericidal effect figures, (d) be combined
Ceramics are to S.aureus bactericidal effect figures.
Specific embodiment
Embodiment 1
(1) 11.81gCa (NO are weighed3)2·4H2O, uses 200mL deionized water dissolvings, obtains the calcium nitrate of 0.25mol/L
Solution；Weigh 3.96g (NH4)2HPO4, 100mL deionized water dissolvings are used, the ammonium dibasic phosphate solution of 0.3mol/L are obtained, is used in combination
Ammoniacal liquor adjusts its pH for 10；
(2) by 0.3gAgNO3Dissolve in adding calcium nitrate solution, and add 22.5g diatomite, obtain diatomite mixing molten
Liquid；
(3), after ammonium dibasic phosphate solution being added dropwise in diatomite mixed solution and is stirred continuously, pour in reactor
Carry out hydro-thermal reaction, 120 DEG C of reaction temperature, pH=10, the reaction time is 4h；
(4) supernatant is outwelled after reactant liquor precipitation 12h for obtaining step (3), and deionized water and ethanol washing, mistake
Filter 3 times, be in neutrality (pH=6～8) to filtrate substantially, and 70 DEG C of dryings obtain dry powder；
(5) by dry powder and boccaro in mass ratio 90:10 dispensings simultaneously add 3mL sodium carboxymethylcellulose binding agent solution, fill
Divide and be uniformly mixed so as to obtain compound；
(6) compound is put into compressing in mould, briquetting pressure 10MPa, dwell time 30s；Resistance is put into afterwards
1000 DEG C of calcining 5h in stove, obtain In-situ reaction antimicrobial filtering ceramics after along with the furnace cooling.
Silver-colored release experiment：Take 1g composite ceramics samples to be put in 500mL deionized waters, constantly rock at 25 DEG C, use
ICP-MS detects silver ion total burst size of the composite ceramics in 1h, 3h, 6h, 12h and 24h.As a result show, 1h, 3h, 6h, 12h and
After 24h, composite ceramics silver total volume is respectively 0.12 μ g/L, 0.21 μ g/L, 0.35 μ g/L, 0.37 μ g/L and 0.43 μ g/L；Can
To find out, the only 0.43 μ g/L of the total volume after this material 24h in aqueous medium, far below health ministry in drinking water
Requirement of the silver content less than 50 μ g/L.
Sterilizing rate is tested：0.5g composite ceramics samples are put into into 10mL bacterial concentrations for 106In cfu/mL bacteria suspensions, vibration
37 DEG C of constant temperature and humidity cultures after uniform.Plate count is applied with 10 times of dilution methods and the sterilization of 1h, 3h, 6h, 12h, 24h sample is calculated
Rate.Its sterilizing rate computing formula：
Wherein, X is sterilizing rate, and A is blank control group average colony number, and B is test specimen average colony number.
Sterilizing rate experimental result shows that the sterilizing rate of composite ceramics sample reaches composite ceramic after 99%, 3h and 3h after 1h
Porcelain sample is 100% to the sterilizing rate of E.Coli and S.aureus.
Bacterium rejection rate is tested：To cultivate after 24h, with normal saline dilution to 10 in bacterium liquid medium within6cfu/
ML, obtains experimental bacteria, and experimental bacteria is passed through composite ceramic ceramics in superclean bench, collects filtrate and applies flat board calculating bacterium colony
Number.As a result show, in the filtrate through composite ceramic ceramics, do not detect E.Coli or S.aureus bacterium colony groups.
Fig. 1 shows that Nano Silver, nano silver-carrying hydroapatite particles are dispersed in diatomite particle surface and hole
In, and having part argentum-carried hydroxylapatite to be to be scattered in surface to melt the form of inlaying, this result can strengthen silver with ceramics
The adhesion of material, improves the Durability of antimicrobial effect of material.Fig. 2 shows that the Nano Silver size in diatomite particle is substantially distributed in 3
～20nm scopes, without obvious agglomeration.It is good that Fig. 3 shows that In-situ reaction antimicrobial filtering ceramics have to E.Coli and S.aureus
Good bactericidal effect.
Embodiment 2
(1) weigh 11.1gCaCl2, 300mL deionized water dissolvings are used, the calcium chloride solution of 0.33mol/L is obtained；Weigh
21.5gNa2HPO4·12H2O, uses 200mL deionized water dissolvings, obtains the disodium phosphate soln of 0.3mol/L, and uses ammoniacal liquor
Its pH is adjusted for 11；
(2) by 0.5gAgNO3Dissolve in being added to calcium chloride solution, and add 50g diatomite, obtain diatomite mixing molten
Liquid；
(3), after disodium phosphate soln being added dropwise in diatomite mixed solution and is stirred continuously, pour in reactor
Carry out hydro-thermal reaction, 160 DEG C of reaction temperature, pH=11, the reaction time is 6h；
(4) supernatant is outwelled after reactant liquor precipitation 12h for obtaining step (3), and deionized water and ethanol washing, mistake
Filter 3 times, be in neutrality (pH=6～8) to filtrate substantially, and 70 DEG C of dryings obtain dry powder；
(5) by dry powder and boccaro in mass ratio 80:20 dispensings simultaneously add 5mL sodium carboxymethylcellulose binding agent solution, fill
Divide and be uniformly mixed so as to obtain compound；
(6) compound is put into compressing in mould, briquetting pressure 10MPa, dwell time 50s；Resistance is put into afterwards
1100 DEG C of calcining 6h in stove, obtain In-situ reaction antimicrobial filtering ceramics after along with the furnace cooling.
Embodiment 3
(1) 23.6gCa (NO are weighed3)2·4H2O, uses 200mL deionized water dissolvings, and the calcium nitrate for obtaining 0.5mol/L is molten
Liquid；Weigh 12.18g (NH4)3PO4, 200mL deionized water dissolvings are used, the ammonium phosphate solution of 0.3mol/L are obtained, and is adjusted with ammoniacal liquor
Its pH is saved for 11；
(2) by 0.9gAgNO3Dissolve in being added to calcium nitrate solution, and add 35g diatomite, obtain diatomite mixing molten
Liquid；
(3), after ammonium phosphate solution being added dropwise in diatomite mixed solution and is stirred continuously, pouring in reactor is carried out
Hydro-thermal reaction, 160 DEG C of reaction temperature, pH=11, the reaction time is 4h；
(4) supernatant is outwelled after reactant liquor precipitation 12h for obtaining step (3), and deionized water and ethanol washing, mistake
Filter 3 times, be in neutrality (pH=6～8) to filtrate substantially, and 80 DEG C of dryings obtain dry powder；
(5) by dry powder and boccaro in mass ratio 70:30 dispensings simultaneously add 4mL sodium carboxymethylcellulose binding agent solution, fill
Divide and be uniformly mixed so as to obtain compound；
(6) compound is put into compressing in mould, briquetting pressure 8MPa, dwell time 60s；Resistance furnace is put into afterwards
In 1050 DEG C calcining 5h, obtain after along with the furnace cooling In-situ reaction antimicrobial filtering ceramics.
Although having been presented for some embodiments of the present invention herein, it will be appreciated by those of skill in the art that
Without departing from the spirit of the invention, the embodiments herein can be changed.Above-described embodiment be it is exemplary, no
Should be using the embodiments herein as the restriction of interest field of the present invention.
Claims (10)
1. a kind of In-situ reaction antimicrobial filtering is ceramic, it is characterised in that by diatomite, hydroxyapatite, boccaro, silver and binding agent
Composition, the mass percent of each component be followed successively by 60～75wt%, 10～20wt%, 10～30wt%, 0.1～2wt%, 1～
5wt%, the mass percent sum of five kinds of components is 100wt%.
2. a kind of In-situ reaction antimicrobial filtering ceramics according to claim 1, it is characterised in that the diatomite purity is
Food-grade, size controlling were the powder of 100 mesh sieves；The boccaro is Jing broken, removal of impurities and crosses the boccaro powder that 100 mesh sieves are obtained
Body.
3. a kind of In-situ reaction antimicrobial filtering according to claim 1 is ceramic, it is characterised in that the hydroxyapatite grain
Footpath scope is 30～300nm；A diameter of 3～20nm of the silver, in diatomite surface and hole.
4. a kind of In-situ reaction antimicrobial filtering according to claim 1 is ceramic, it is characterised in that the binding agent is carboxylic first
One or more in base sodium cellulosate, hydroxypropyl methyl cellulose, hydroxymethyl cellulose, polyvinyl alcohol, polyethylene glycol.
5. a kind of preparation method of the In-situ reaction antimicrobial filtering ceramics described in any one of claim 1-4, it is characterised in that bag
Include following steps：
(1) 0.1～0.5mol/L phosphate solutions, 0.1～0.5mol/L calcium salt solns are configured, and adjusts phosphate solution pH=
8～12；
(2) by a certain amount of AgNO3Solid is dissolved in adding calcium salt soln, and adds a certain amount of diatomite to stir, and obtains silicon
Diatomaceous earth mixed solution；
(3), after phosphate solution being added dropwise in diatomite mixed solution and is stirred continuously, carry out hydro-thermal reaction；
(4) reactant liquor that step (3) is obtained is filtered and is washed to filtrate pH=6～8, drying is obtained dry powder；
(5) by dry powder with boccaro by certain mass is than dispensing and adds a certain amount of binder solution, be fully uniformly mixed so as to obtain mixing
Material；
(6) compound is put into into compressing in mould or injection forming, drying, high-temperature calcination, obtains original after along with the furnace cooling
Position composite antibacterial ceramic for filtration.
6. preparation method according to claim 1, it is characterised in that step (1) phosphate is diammonium hydrogen phosphate, phosphorus
Sour disodium hydrogen or ammonium phosphate, the calcium salt are calcium nitrate or calcium chloride.
7. preparation method according to claim 5, it is characterised in that in step (2), AgNO3Solid, diatomite, calcium salt are molten
The amount ratio of liquid is (0.2～1g):(20～50g):(200～500mL)；Step (5) dry powder is (70 with the mass ratio of boccaro:
30)～(90:10).
8. preparation method according to claim 5, it is characterised in that the condition of step (3) hydro-thermal reaction is：100
～240 DEG C, pH=8～12；The concentration of binder solution described in step (5) is 10g/L～30g/L；In step (6), shaping
Pressure be 8～12MPa, the dwell time be 20～60s, 60～100 DEG C of baking temperature, 900～1200 DEG C of calcining heat, calcining when
Between 4～6h.
9. application of the In-situ reaction antimicrobial filtering ceramics described in any one of claim 1-4 in terms of water process, its feature exist
In the In-situ reaction antimicrobial filtering ceramics can be used to filtering and killing the microorganism in water.
10. application according to claim 9, it is characterised in that the microorganism is E.Coli and S.aureus.
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| CN107267980A (en) * | 2017-07-11 | 2017-10-20 | 芜湖市宝艺游乐科技设备有限公司 | A kind of ceramic coating with broad spectrum antibiotic activity and preparation method thereof |
| CN108355401A (en) * | 2018-02-09 | 2018-08-03 | 纳琦环保科技有限公司 | A kind of preparation method of novel inorganic porous purification filter core |
| CN108355401B (en) * | 2018-02-09 | 2021-01-08 | 纳琦环保科技有限公司 | Preparation method of inorganic porous purification filter element |
| CN109095886A (en) * | 2018-10-09 | 2018-12-28 | 揭阳市腾晟科技咨询有限公司 | A kind of anti-bacteria ceramic raw material |
| CN109607968A (en) * | 2019-01-11 | 2019-04-12 | 刘恒 | A kind of ecological riverway system of hydraulic engineering |
| CN110372326A (en) * | 2019-06-12 | 2019-10-25 | 魏炎梅 | A kind of preparation method of heatproof and shockproof ceramic filtering material |
| CN110963784A (en) * | 2019-12-31 | 2020-04-07 | 郑州登电科诚新材料有限公司 | Production process for recycling cutting waste of foamed ceramic insulation board |
| CN112919881A (en) * | 2021-03-15 | 2021-06-08 | 同曦集团有限公司 | Antibacterial, mildewproof and antiviral dark-red enameled pottery and preparation method thereof |
| CN113292333A (en) * | 2021-06-24 | 2021-08-24 | 四川三联新材料有限公司 | Preparation method of silver-loaded hydroxyapatite atomization core |
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