CN102417220B - Application of tantalum-doped zinc oxide nanometer powder photocatalyst in water treatment antisepsis - Google Patents
Application of tantalum-doped zinc oxide nanometer powder photocatalyst in water treatment antisepsis Download PDFInfo
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- 238000006555 catalytic reaction Methods 0.000 description 11
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- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention discloses application of a tantalum-doped zinc oxide nanometer powder photocatalyst to water treatment antisepsis. A strain comprises Gram-positive bacterium bacillus subtilis, staphylococcus aureus, Gram-negative bacterium escherichia coli and pseudomonas aeruginosa. According to the invention, tantalum-doped zinc oxide nanometer powder can be used for restraining the growth of bacteria in dark environments and under visible light, and has superior bacterinertness to pure zinc oxide nanometer powder. The MIC (Minimal Inhibitory Concentration) can be effectively lowered in dark environments by performing photocatalysis, and a higher bacteriostatic effect can be achieved with a smaller adding amount.
Description
Technical field
The present invention relates to the application of a kind of novel tantalum-doped zinc oxide nano-photocatalyst in water treatment, specifically is the application of the sterilizing and purifying of water being handled and suppressed bacterial growth.
Background technology
Tellurian water resources is limited, and along with the rapid expansion of global total population, the shortage of water resources shows that day by day the tap water of cleaning is more and more important.Although the human method of having grasped chlorine or ozonization processing water, in many developing countries or low developed area, the disease that causes because of unclean water purification still is unequal to act, for example typhoid fever, hepatitis, gray nucleus inflammation, dysentery etc. more.The antiseptic-germicide of therefore efficient, the easy use of development, safety, more and more important and urgent.And the nano material photocatalyst recently as a kind of advanced person's oxidation technology, becomes a focus of water treatment research.It can be used for degradation of organic substances, reduces harmful metal ion content, and water is carried out sterilization and disinfection.
Antiseptic-germicide mainly can be divided into two big classifications: organic materials and inorganic materials.Most organic antibacterial agent is relatively more responsive to temperature and pressure, easily loses efficacy.Inorganic materials such as metal and metal oxide then can bear the treatment condition of comparison harshness.So inorganic materials shows bigger advantage in antimicrobial treatment.
Zinc oxide since characteristics such as its excellent photoelectricity, piezoelectricity, pressure-sensitive and semi-conductor obtained paying close attention to widely, but the antibiotic behavioral study about zinc oxide is less, the zinc oxide of having reported that has is better than intestinal bacteria to the anti-microbial effect of subtilis, to the minimal inhibitory concentration (MIC) of subtilis with particle do not coexist 2000 and 12500ppm between, and to colibacillary MIC 50000 and 100000ppm between, only for subtilis, the zinc oxide antibacterial effect is better than silicon-dioxide and titanium dioxide.Yet about photocatalysis antibacterial effect research under the visible light of zinc oxide seldom.This is because the band gap of zinc oxide is 3.3ev, can only wavelength absorption less than the UV-light of 385nm, in order to improve zinc oxide to the absorption of visible light, can change, narrow the band gap of zinc oxide by other ion of doping vario-property, increase surface imperfection simultaneously, improve the photocatalytic activity of zinc oxide, and then strengthen antibacterial ability.
Summary of the invention
Technical problem to be solved by this invention provides the tantalum-doped zinc oxide nano-photocatalyst to multiple common pathogen, comprises the application that gram-positive microorganism subtilis, streptococcus aureus and Gram-negative bacteria intestinal bacteria, pseudomonas aeruginosa table have excellent germ resistance.
The invention provides the application of tantalum-doped zinc oxide nano powder photocatalyst agent in water treatment is antibiotic.
Above-mentioned bacterial classification comprises gram-positive microorganism subtilis, streptococcus aureus, Gram-negative bacteria intestinal bacteria and pseudomonas aeruginosa.
The present invention is with 1～5%(atomic percent) tantalum-doped zinc oxide nano powder is applied in the water treatment, under the concentration and radiation of visible light of every milliliter of 160-200 microgram, multiple common pathogen (gram-positive microorganism subtilis, streptococcus aureus and Gram-negative bacteria intestinal bacteria, pseudomonas aeruginosa) is shown excellent germ resistance, and this antiseptic-germicide is under dark situation, also have germ resistance preferably, to subtilis, streptococcus aureus and intestinal bacteria minimal inhibitory concentration about about every milliliter of 200 microgram.Compare with unadulterated pure zinc oxide powder, anti-microbial property is significantly improved, and particularly the antibacterial effect to subtilis is best under the visible light.Tantalum-doped zinc oxide nano powder and have characteristics such as easy to operate, highly effective and safe can be applicable to environmental improvement and water treatment.
The present invention has following beneficial effect:
1, show first tantalum-doped zinc oxide nano powder can be under dark situation and visible light bacteria growing inhibiting, and germ resistance is better than the pure zinc oxide nanometer powder.Photochemical catalysis can effectively reduce the MIC under the dark situation, and littler add-on just can reach higher fungistatic effect.
2, synthetic method is simple, the antiseptic-germicide easy to operate, and the tantalum-doped zinc oxide photocatalyst after can recycling, reuses after catalysis is antibacterial.
3, catalysis under visible light can utilize sun power as light source, and better effects if under the illumination, has effectively utilized inexhaustible, nexhaustible solar energy resources.
4, the tantalum-doped zinc oxide photocatalyst can carry out sewage disposal, all right cleaning water system, and the control microorganism, range of application is wider.
Description of drawings
The X-ray diffraction of Fig. 1, tantalum-doped zinc oxide nano powder (XRD) figure.
The pattern of Fig. 2, tantalum-doped zinc oxide nano powder, wherein a is pure zinc oxide; B is the zinc oxide that 1% tantalum mixes; C is 3% tantalum-doped zinc oxide; D is 5% tantalum-doped zinc oxide.
Fig. 3, the antibacterial time curve of tantalum-doped zinc oxide photochemical catalysis, wherein (a) is the tantalum-doped zinc oxide photochemical catalysis inhibition pseudomonas aeruginosa of every milliliter of 200 microgram; (b) be the tantalum-doped zinc oxide photochemical catalysis inhibition intestinal bacteria of every milliliter of 200 microgram; (c) be the tantalum-doped zinc oxide photochemical catalysis inhibition streptococcus aureus of every milliliter of 200 microgram; (d) be the tantalum-doped zinc oxide photochemical catalysis inhibition subtilis of every milliliter of 160 microgram.
Bacterium pattern after Fig. 4, the antimicrobial treatment, wherein (a) is the processing of every milliliter of the contrast of positive pseudomonas aeruginosa bacterium and 3% tantalum-doped zinc oxide dark situation, 200 microgram; (b) be the processing of every milliliter of 300 microgram under the contrast of positive intestinal bacteria and the 3% tantalum-doped zinc oxide dark situation; (c) be the processing of every milliliter of positive staphylococcus aureus contrast and 1% tantalum-doped zinc oxide, 200 microgram; (d) be the processing of every milliliter of positive subtilis contrast and 1% tantalum-doped zinc oxide dark situation, 160 microgram.
Embodiment
The tantalum precursor solution that relates among the present invention and tantalum-doped zinc oxide nano powder photocatalyst agent, open through Chinese patent " stable water miscible niobium and preparation method and the application of tantalum precursor " (publication number 1699186) and Chinese patent " a kind of tantalum-doped zinc oxide nano powder photocatalyst agent; its preparation method and application " (publication number 101433833), be prepared from according to its method.Two kinds of processing steps are simple, and good dispersity is convenient to large-scale industrial production.The nano-photocatalyst of preparing has higher specific surface area, shows higher photocatalytic activity and germ resistance under visible light, also has tangible antibacterial surname under dark situation.
1, tantalum-doped zinc oxide nano powder is synthetic
Synthesis material: the water-soluble precursor solution of tantalum (seeing the patent of invention of publication number 1699186), soluble zinc salt (analytical pure), ethylene glycol (analytical pure), nitric acid (analytical pure), citric acid (analytical pure), methyl ethyl diketone (analytical pure), polypropylene pyrrolidone (PVP weight-average molecular weight 100,000), hydroxy propyl cellulose (HPC, molar average molecular weight 100,000), deionized water.
Synthesis path (seeing the patent of invention of publication number 101433833) obtains tantalum-doped zinc oxide nano powder (faint yellow) sample.Productive rate is about 100%.
Embodiment 1:
With 2.98g zinc nitrate hexahydrate Zn (NO
3)
26H
2O places the 100mL beaker, adds the 50mL deionized water, slowly adds an amount of citric acid while stirring, until the solution clarification, forms solution A; Get 2.93g tantalum precursor solution (35.93mol/g) again, add 1g ethylene glycol, form solution B.Again above-mentioned two kinds of solution are mixed, add 1g PVP, 0.55ml nitric acid, continue to stir 0.5 hour.Evaporating solvent adds 1g HPC and 1g methyl ethyl diketone again to 70% of proper mass under 50 ° of C, is placed on after the stirring in the air, wears out after 24 hours, under 140 ° of C, dries by the fire 12 hours again, obtains precursor powder.Carry out 400 ° of C annealing 2 hours again, 700 ° of C annealed 1 hour again, obtained 1% tantalum-doped zinc oxide nano powder sample.
Embodiment 2:
With 1.43g zinc nitrate hexahydrate Zn (NO
3)
26H
2O places the 100mL beaker, adds the 50mL deionized water, slowly adds an amount of citric acid while stirring, until the solution clarification, forms solution A; Get 2.89g tantalum precursor solution (35.93mol/g) again, add 1g ethylene glycol, form solution B.Again above-mentioned two kinds of solution are mixed, add 1g PVP, 0.55mL nitric acid, continue to stir 1 hour.Evaporating solvent adds 1g HPC and 1g methyl ethyl diketone again to 70% of proper mass under 50 ° of C, is placed on after the stirring in the air, wears out after 24 hours, under 140 ° of C, dries by the fire 12 hours again, obtains precursor powder.Carry out 400 ° of C annealing 2 hours again, 700 ° of C annealed 1 hour again, obtained 1% tantalum-doped zinc oxide nano powder sample.
Embodiment 3:
With 1.49g zinc nitrate hexahydrate Zn (NO
3)
26H
2O places the 100mL beaker, adds the 50mL deionized water, slowly adds an amount of citric acid while stirring, until the solution clarification, forms solution A; Get 7.34g tantalum precursor solution (35.93mol/g) again, add 1g ethylene glycol, form solution B.Again above-mentioned two kinds of solution are mixed, add 1g PVP, 0.55mL nitric acid, continue to stir 1 hour.Evaporating solvent adds 1g HPC and 1g methyl ethyl diketone again to 75% of proper mass under 50 ° of C, is placed on after the stirring in the air, wears out after 24 hours, under 140 ° of C, dries by the fire 12 hours again, obtains precursor powder.Carry out 400 ° of C annealing 2 hours again, 700 ° of C annealed 1 hour again, obtained 1% tantalum-doped zinc oxide nano powder sample.
Fig. 1 is X-ray diffraction (XRD) figure of tantalum-doped zinc oxide nano powder, and as seen, the tantalum doping is less than 5% o'clock, and the diffraction peak on the XRD figure is the peak of corresponding and zinc oxide all, and the little tantalum doping does not change the crystalline structure of zinc oxide; The tantalum doping was more than or equal to 5% o'clock, and tantalum pentoxide occurs mutually.
Fig. 2 is the pattern of tantalum-doped zinc oxide nano powder, and wherein a is pure zinc oxide; B is the zinc oxide that 1% tantalum mixes; C is 3% tantalum-doped zinc oxide; D is 5% tantalum-doped zinc oxide.
2, the antibacterial effect of tantalum-doped zinc oxide nano powder
Tantalum-doped zinc oxide nano powder shown in the present can be used for dark situation and photocatalysis antibacterial.The constant temperature shaking table is cultivated under the dark situation, and clarification is minimal inhibitory concentration to occur obviously; Photochemical catalysis with visible light (or sunlight) as light source, being placed on the constant temperature shaking table in illumination cultivates, add a certain amount of catalyzer, within a certain period of time, degrade subtilis, streptococcus aureus, intestinal bacteria, the pseudomonas aeruginosa of certain integrated group unit (CFU) come the variation of bacterial detection concentration with the spectrophotometric determination solution absorbency.
Under the dark situation, mensuration (seeing Table one) by minimal inhibitory concentration, discovery is to subtilis, streptococcus aureus and intestinal bacteria, mixing tantalum zinc oxide compares pure zinc oxide significantly antibacterial effect is arranged, 5% tantalum doping effect is the most remarkable, minimal inhibitory concentration to above-mentioned three kinds of bacteriums is respectively every milliliter of 180,200,160 microgram, and the minimal inhibitory concentration of pure zinc oxide is respectively〉1000, every milliliter of 1000,350 microgram.
The minimal inhibitory concentration of table 1, zinc oxide, tantalum-doped zinc oxide, tantalum pentoxide (unit: mcg/ml)
Under photocatalysis, the nanometer powder concentration that inhibitory effect takes place under the visible light is effectively reduced (see figure 3).Under the concentration of every milliliter of 160-200 microgram, subtilis, streptococcus aureus, intestinal bacteria, pseudomonas aeruginosa, the zinc oxide that uses lower concentration to mix tantalum amount (1% and 3%) equally also shows excellent anti-microbial property, particularly to subtilis, compare with pure zinc oxide, the photocatalysis antibacterial advantage of mixing tantalum zinc oxide is more obvious.The photocatalysis antibacterial effect that 1% tantalum mixes reaches the effect of 5% tantalum-doped zinc oxide of isodose under the dark situation, and tantalum-doped zinc oxide is more serious to the destruction of bacterium, tears cytolemma and cell walls, causes the dead (see figure 4) of bacterial metabolism.
Concrete antibacterial experiment
Embodiment 1:
Synthesis condition obtains 1%, 3%, 5% tantalum-doped zinc oxide nano powder with concrete synthetic enforcement.Carry out the dark situation antibacterial experiment with this pale yellow powder.Join by prescription and to get broth culture 2.5ml, phosphate buffer solution 2.5ml mixes and adds in the test tube, adds 10 respectively
7The bacterial load that integrated group unit is every milliliter, and positive control (do not contain catalyzer, but inoculated bacteria) and recessive contrast (having only mixing solutions) are set.Catalyzer adds in the test tube by the gradient amount.Test tube 37 ℃ of constant temperature on shaking table, the 120r/min concussion was cultivated 48 hours, obvious defecator's minimal inhibitory concentration (MIC) occurred even compare with contrast afterwards.The result shows: 5% tantalum-doped zinc oxide consumption is minimum, and effect is best relatively, and consumption is about half of zinc oxide, and particularly remarkable to subtilis, consumption is minimum.
Embodiment 2:
Synthesis condition obtains 1%, 3%, 5% faint yellow tantalum dopen Nano powder with specific embodiment one.Every milliliter of 1% tantalum-doped zinc oxide, 160 microgram, 3%, in the test tube of every milliliter of adding of 5% tantalum-doped zinc oxide, 200 micrograms with the inoculation of example one, 300w xenon lamp (＞425nm) following photo-irradiation treatment, the constant temperature shaking table of equivalent time is cultivated after the illumination, afterwards the absorbancy under the spectrophotometer measurement 600nm.The result shows: do not have every milliliter of add-on of 200 micrograms of fungistatic effect to show stronger restraining effect under the dark situation in the following short period of time of photochemical catalysis, and every milliliter of add-on of 160 micrograms finds that relatively 1% tantalum-doped zinc oxide has showed high photocatalysis antibacterial performance under more a spot of situation, and antibacterial effect reaches the effect of 5% tantalum-doped zinc oxide of isodose under the dark situation.
Embodiment 3:
Measure the MIC of tantalum pentoxide under the dark situation, actual conditions adds the tantalum pentoxide powder with embodiment one in the test tube, determine MIC after cultivating.Measure the photocatalysis antibacterial effect of tantalum pentoxide simultaneously, actual conditions adds the tantalum pentoxide powder of every milliliter of 200 microgram with example two in the inoculated bacteria test tube, after illumination cultivation is handled, and the absorbancy of spectrophotometer measurement 600nm.The result shows: no matter at dark situation or under photochemical catalysis, to streptococcus aureus, intestinal bacteria, pseudomonas aeruginosa, the tantalum pentoxide powder does not have germ resistance.The tantalum pentoxide powder has the subtilis germ resistance at dark situation or under visible light (concentration is every milliliter of 200 microgram) to subtilis.This experiment shows that the tantalum pentoxide powder does not have photocatalytic.
Above-mentioned these embodiments only are used for explanation the present invention, but do not limit the scope of the invention, and after having read the present invention, those skilled in the art all fall within the application's claims institute restricted portion to the modification of the various equivalent form of values of the present invention.
Claims (1)
1. the application of tantalum-doped zinc oxide nano powder photocatalyst agent in water treatment is antibiotic, it is characterized in that atomic percent 1～5% tantalum-doped zinc oxide nano powder is applied in the water treatment, under the concentration and radiation of visible light of every milliliter of 160-200 microgram, gram-positive microorganism subtilis, streptococcus aureus and Gram-negative bacteria intestinal bacteria, pseudomonas aeruginosa had anti-microbial effect.
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| CN107779493A (en) * | 2017-10-25 | 2018-03-09 | 安徽古尔特科技有限公司 | ZnO nano particle suppresses the New function of Escherichia coli Growth |
| CN107771856A (en) * | 2017-10-25 | 2018-03-09 | 安徽古尔特科技有限公司 | ZnO nano particle suppresses the New function of bacillus subtilis bacteria growing |
| CN107455388A (en) * | 2017-11-09 | 2017-12-12 | 中国海洋大学 | A kind of ZnO/V of light and shade field sterilization2O5Composite and preparation method thereof |
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