CN101700499A - Super-fine fly ash silver-loaded antimicrobial and preparation method - Google Patents
Super-fine fly ash silver-loaded antimicrobial and preparation method Download PDFInfo
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- CN101700499A CN101700499A CN200910177165A CN200910177165A CN101700499A CN 101700499 A CN101700499 A CN 101700499A CN 200910177165 A CN200910177165 A CN 200910177165A CN 200910177165 A CN200910177165 A CN 200910177165A CN 101700499 A CN101700499 A CN 101700499A
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- 239000010881 fly ash Substances 0.000 title claims abstract description 45
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 230000000845 anti-microbial effect Effects 0.000 title claims abstract description 18
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 17
- 239000004332 silver Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000004599 antimicrobial Substances 0.000 claims abstract 3
- 239000003245 coal Substances 0.000 claims abstract 3
- 230000000844 anti-bacterial effect Effects 0.000 claims description 15
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 230000003115 biocidal effect Effects 0.000 claims description 6
- 239000003242 anti bacterial agent Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002086 nanomaterial Substances 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 claims description 3
- 238000007146 photocatalysis Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 230000001143 conditioned effect Effects 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 238000013401 experimental design Methods 0.000 claims description 2
- 239000006210 lotion Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000004448 titration Methods 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 1
- 230000002776 aggregation Effects 0.000 claims 1
- 238000004220 aggregation Methods 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 claims 1
- CBOQJANXLMLOSS-UHFFFAOYSA-N ethyl vanillin Chemical class CCOC1=CC(C=O)=CC=C1O CBOQJANXLMLOSS-UHFFFAOYSA-N 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 238000011068 loading method Methods 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000000969 carrier Substances 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 230000002421 anti-septic effect Effects 0.000 description 13
- 230000005764 inhibitory process Effects 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 3
- 239000001963 growth medium Substances 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000010883 coal ash Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- 244000063299 Bacillus subtilis Species 0.000 description 1
- 239000001888 Peptone Substances 0.000 description 1
- 108010080698 Peptones Proteins 0.000 description 1
- 241001635574 Sabatia angularis Species 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 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
- 239000012153 distilled water Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000019319 peptone Nutrition 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- -1 pottery Substances 0.000 description 1
- 239000003642 reactive oxygen metabolite Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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Abstract
Antimicrobials are extensively used in human production and living, wherein the cost of the antimicrobials is directly decided by the selection of antimicrobial carriers. At present, coal is used as the main energy source for generating power in China, and fly ashes become important pollutants produced by a power plant. If the fly ashes can be more finely used as the carriers by fully using the advantages of porosity and large specific surface areas, the fly ashes can bring greater economic benefit. The invention discloses a superfine fly ash silver-loaded antimicrobial and a preparation method. The fly ashes are pulverized to be about 0.5 microns by an airflow pulverizer, and the pulverized fly ashes are combined with AgNO-3 under a series of processing conditions to prepare the silver-loaded antimicrobial. The prepared antimicrobial has simple preparation, antimicrobial durability, weather resistance, security, high temperature resistance, broad spectrum and good antimicrobial effect.
Description
One, technical field
The present invention relates to a kind of superfined flyash load photocatalysis nano material technology, be specifically related to a kind of antiseptic based on superfined flyash and preparation method thereof.
Two, background technology
Antiseptic is that a class has antibacterial and New-type adjuvant bactericidal property, be widely used in commodity and tame electrical article,, be harmless to the health because its security is good, do not cause pollution, expand to fields such as construction material, pottery, fibre in recent years rapidly environment.Antiseptic generally is divided into organic antibacterial agent and inorganic antibacterial two big classes.
Metal ion support type inorganic antiseptic is that the metal ion that will have antibacterial functions is loaded on the various inorganic carriers, discharges antibacterial metal ions or reactive oxygen species during use, makes material have antibiotic and bactericidal effect.Metal ion commonly used have Ag, Cu, Zn, etc.Because characteristics such as that inorganic carrier requires to have is safe, good heat resistance, long service life, no volatilization, so correctly selecting for use of inorganic carrier is an importance of current inorganic antiseptic exploitation.Inorganic antiseptic and organic antibacterial agent available support are a lot, require that carrier has porous, specific area is big, absorption property good, nontoxic, the stable lasting characteristics such as sustained release performance of having of antimicrobial component of not destroying of chemical property.Antiseptic will be applied widely, and at first the problem that will solve reduces cost exactly.Under the situation that active component is determined, reduction inorganic or the organic antibacterial agent cost mainly depends on the reduction of carrier cost.Inorganic antibacterial agent carriers such as at present used zeolite, montmorillonite all are artificial synthetic product usually, and are too high because of product cost though that they have purity height, fine size and ion-exchange capacity is big etc. a bit, limited its scope of application.
Physicochemical properties, microstructure according to flyash, flyash after air-flow is pulverized can reach the fundamental characteristics as antibiotic filler on color and characteristic, this is the exploration to the high meticulous utilization of flyash, and the preparation cost that reduces inorganic antiseptic is also had certain value.Studies show that superfined flyash can reach the fundamental characteristics as antibiotic filler.
At present based on the energy mode of thermoelectricity, flyash becomes the important pollutant of power plant output for China.If the utilization that flyash can be become more meticulous is more regarded it as " through the mineral resources of high-temperature calcination " and is treated, make full use of the big advantage of its porous and specific area, just can make it produce bigger economic benefit.
Three, summary of the invention
Technical scheme of the present invention comprises superfined flyash load photocatalysis nano material technology, and main is example with the technical scheme of super-fine fly ash silver-loaded antimicrobial and the technical scheme of its preparation method.
This antiseptic of the present invention is based on silver, adopts immersion process for preparing silver-carrying nano complex.
The preparation method of this super-fine fly ash silver-loaded antimicrobial of the present invention is as follows:
1) with the flyash high temperature sintering to remove remaining char in the flyash, with airslide disintegrating mill flyash is crushed to 0.5 micron then, the particle diameter after flyash is pulverized should be approximately about 2 microns.Can a metachromatism occur by flyash in this process, both flyash was Dark grey before pulverizing, even change in color is also little after 500 ℃ of calcinations.And after air-flow was pulverized, flyash was after 500 ℃ of calcinations, and color becomes rose pink.
2) take by weighing an amount of superfined flyash powder, put into the 100ml deionized water, disperse a few minutes, put into an amount of AgNO3 in the ratio of experimental design then with the sonic oscillation instrument, come the pH value of conditioned reaction liquid by the interpolation of dilute nitric acid solution, in 60 ℃ of waters bath with thermostatic control, stir and (after 200~300r/min) a period of times, take out and filter, then spend deionised water, washing lotion is checked with the HCl titration, washing is not to producing till the white precipitate, and oven dry, roasting then taken out sample and ground.
It is simple that the antiseptic that the present invention prepares has preparation, antibiotic persistence, weather resisteant, security, heat-resisting quantity, broad spectrum activity and have good antibacterial effect.Be characterized in: the culture dish that 1. will be placed with super-fine fly ash silver-loaded complex test specimen was placed respectively 3 months under 37 ℃ incubator and room temperature environment, and test specimen still shows strong anti-microbial property.This be because, after bacterial body lost activity, the Ag+ that combines with it can dissociate out from thalline again, contacted with other bacterium colony again, that goes round and begins again carries out said process.2. Wei Liang silver is safe, nontoxic to human body, and superfined flyash also is nontoxic.3. with super-fine fly ash silver-loaded complex after carrying out high-temperature heat treatment under 600 ℃, carry out anti-microbial property experiment again, super-fine fly ash silver-loaded nano complex still shows strong anti-microbial property.4. the bacterial classification of this research experiment test introducing is the mixed bacteria that comprises staphylococcus aureus, Escherichia coli and Bacillus subtillis, and this is three kinds of representative bacterial classifications.According to biological general knowledge,, just can think that this antiseptic has had broad-spectrum antimicrobial effect if certain antiseptic all has antibacterial action to above three kinds of cells.
Four, description of drawings
Preparation technology's flow process of the super-fine fly ash silver-loaded nano complex of Fig. 1
Ultra-fine year silver powder coal ash of Fig. 2 antibacterial effect figure
Ultra-fine year silver powder coal ash of Fig. 3 can spectrogram
Five, the specific embodiment
The super-fine fly ash silver-loaded antimicrobial that comes out produced according to the present invention illustrates its anti-microbial property by routine example down.In antibacterial experiment, at first be the preparation of culture medium, beef-protein medium is adopted in experiment.Peptone 10g, beef extract 5g, sodium chloride 5g, agar 5g are added in the 950ml distilled water, on electric furnace, carefully be heated to and dissolve, with NaOH adjust pH to 7.0~7.6, adding distil water is to 1L, be sub-packed in conical flask then, put under the HTHP sterilization, pour into after being cooled to 50 ℃ and be cooled to room temperature in the culture dish again as culture medium.
The ratio of super-fine fly ash silver-loaded complex with 1: 100 is dispersed in the deionized water, puts into wherein with treated round carrier then, through fully taking out oven dry after the contact.Sterile working injection Escherichia coli and Staphylococcus aureus bacterium liquid are on culture medium and scrape even, the sample that is loaded with inorganic antiseptic is placed in the culture dish, place insulating box (37 ℃) to cultivate 24 hours, take out back slide measure working sample inhibition zone size on every side.
For guaranteeing the accuracy of data, the inhibition zone width of each sample respectively to be measured 6 times in different directions every 60 °, the inhibition zone size is the mean value of each sample inhibition zone width.Adopt ordinary camera to take the inhibition zone sheet at last.
At flyash and silver nitrate mol ratio is 15: 1, and the pH value of solution value is 6, and the reaction time is 10 hours, and reaction temperature is 60) ℃, sintering temperature is under 550 ℃ the process conditions, the silver-colored complex of preparing that carries has good antibacterial performance.Its result is shown in Fig. 2,3.
The result shows, can clearly find to have the appearance at Ag peak by spectrogram by SEM, and passes through the front and back quality contrast that silver-colored complex is carried in preparation, and its content can reach about 5.5%.This just makes it possess good antibiotic and sterilizing ability.In Fig. 2, can significantly see the existence of inhibition zone, its inhibition zone is between 2mm~2.3mm.
Claims (6)
1. one kind is the photocatalysis nano material technology of carrier with the superfined flyash, it is characterized in that, the flyash high temperature sintering to remove remaining char in the flyash, is pulverized flyash with airslide disintegrating mill then.
2. in pulverizing, air-flow adds certain grinding aid to reduce the formation of hard aggregation according to right 1 described flyash.It is 0.4721um that flyash is pulverized the back average grain diameter, and density is 2.2g/cm3, and specific area is 72.183m2/g.
3. have the nano materials such as nano metal ion A g, Cu, Zn and nano titanium oxide of antibacterial functions according to claim 1,2 described ultra-fine fine coal by loading, to reach antibiotic and bactericidal effect.
4. pass through to load organic antibacterial agents such as vanillic aldehyde or ethyl vanillin compounds according to claim 1,2 described ultra-fine fine coal, play antibacterial action.
5. according to claim 1,2, the preparation method of 3 described super-fine fly ash silver-loaded antimicrobials, its feature comprises and takes by weighing an amount of superfined flyash powder, put into the 100ml deionized water, disperse a few minutes with the sonic oscillation instrument, put into an amount of AgNO3 in the ratio of experimental design then, come the pH value of conditioned reaction liquid by the interpolation of dilute nitric acid solution, in 60 ℃ of waters bath with thermostatic control, stir (after 200~300r/min) a period of times, take out and filter, then spend deionised water, washing lotion with HCl titration check, is washed to not producing till the white precipitate, oven dry then, roasting is taken out sample and is ground.
6. super-fine fly ash silver-loaded antimicrobial according to claim 3 is 15: 1 at flyash and silver nitrate mol ratio, the pH value of solution value is 6, reaction time is 10 hours, reaction temperature is 60 ℃, sintering temperature is under 550 ℃ the process conditions, and the silver-colored complex of preparing that carries has good antibacterial performance.
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104789069A (en) * | 2015-04-24 | 2015-07-22 | 西南科技大学 | Preparation method of ultra-fine coal ash colored paint |
CN109332720A (en) * | 2018-12-05 | 2019-02-15 | 太原理工大学 | High dispersancy nano silver anti-biotic material and preparation method thereof |
CN109874813A (en) * | 2019-03-27 | 2019-06-14 | 中国能源建设集团安徽省电力设计院有限公司 | A kind of method that flyash prepares antibacterial agent through mechanical ball mill |
CN111234140A (en) * | 2019-10-23 | 2020-06-05 | 古乐怡 | High-strength antibacterial PMMA (polymethyl methacrylate) plate and preparation method thereof |
CN111657299A (en) * | 2020-07-10 | 2020-09-15 | 广州佳乐生态科技有限公司 | Composite nano-ion bacteriostatic agent |
CN111841496A (en) * | 2020-07-24 | 2020-10-30 | 泉州南京大学环保产业研究院 | Method for rapidly preparing silver-loaded activated carbon |
CN112021332A (en) * | 2020-09-10 | 2020-12-04 | 安徽理工大学 | Disinfection powder suitable for livestock and poultry farm and preparation method thereof |
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2009
- 2009-09-28 CN CN200910177165A patent/CN101700499A/en active Pending
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104789069A (en) * | 2015-04-24 | 2015-07-22 | 西南科技大学 | Preparation method of ultra-fine coal ash colored paint |
CN109332720A (en) * | 2018-12-05 | 2019-02-15 | 太原理工大学 | High dispersancy nano silver anti-biotic material and preparation method thereof |
CN109332720B (en) * | 2018-12-05 | 2021-08-31 | 太原理工大学 | High-dispersity nano-silver antibacterial material and preparation method thereof |
CN109874813A (en) * | 2019-03-27 | 2019-06-14 | 中国能源建设集团安徽省电力设计院有限公司 | A kind of method that flyash prepares antibacterial agent through mechanical ball mill |
CN111234140A (en) * | 2019-10-23 | 2020-06-05 | 古乐怡 | High-strength antibacterial PMMA (polymethyl methacrylate) plate and preparation method thereof |
CN111657299A (en) * | 2020-07-10 | 2020-09-15 | 广州佳乐生态科技有限公司 | Composite nano-ion bacteriostatic agent |
CN111841496A (en) * | 2020-07-24 | 2020-10-30 | 泉州南京大学环保产业研究院 | Method for rapidly preparing silver-loaded activated carbon |
CN112021332A (en) * | 2020-09-10 | 2020-12-04 | 安徽理工大学 | Disinfection powder suitable for livestock and poultry farm and preparation method thereof |
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Application publication date: 20100505 |