CN101142923A - Tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder and its preparation method - Google Patents
Tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder and its preparation method Download PDFInfo
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- CN101142923A CN101142923A CNA2007100727637A CN200710072763A CN101142923A CN 101142923 A CN101142923 A CN 101142923A CN A2007100727637 A CNA2007100727637 A CN A2007100727637A CN 200710072763 A CN200710072763 A CN 200710072763A CN 101142923 A CN101142923 A CN 101142923A
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Abstract
The invention provides an inorganic tourmaline powder containing nano zinc oxide for suppression of sulfate reducing bacteria and a preparation method, which relates to an antibacterial agent and a preparation method. The invention solves the problem that that the prior organic antibacterial agent has poor security, poor heat-resistant property, easy decomposition and short service life. According to quality percentage, the invention is made of the tourmaline of 50-99.99 percent and the nano zinc oxide solid of 0.01-50 percent. The preparation method is as follows: 1. Preparation of the nano zinc oxide; 2. Mixing and stirring; 3. Extraction filtration, washing and drying; 4. Grinding, calcinations and grinding; therefore, the inorganic tourmaline powder containing nano zinc oxide for suppression of sulfate reducing bacteria can be prepared well. With solid-phase synthesis, the invention adopts the nano or submicron tourmaline, not only effectively increasing the amount of the loaded nano zinc oxide, but also improving the antimicrobial effect of the antimicrobial agent.
Description
Technical field
The present invention relates to antibacterial pulvis and preparation method thereof, especially crude tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting bacteria powder and preparation method thereof.
Background technology
In recent years, along with the accelerated development of national economy, the industrial wastewater particularly pollution of sulfate wastewater is quite serious.A lot of big cities underground water of China has been subjected to sulfate contamination in various degree.Sulfur acid salt acidic waste water directly enters water body without processing will make the receiving water body acidifying, reduce water pH value, the harm aquatile, and produce potential corrosion; This class acidic waste water also can destroy soil structure, reduces crop yield.The sulfate wastewater latency period is long, though the activity of nature reduction bacterium is arranged, has become a problem that is subjected to very much concern of field produces.At present, it is 3 big classes that the kind of antibacterial agent can be divided into inorganic system, organic system and natural biological substantially: one, inorganic antiseptic combines by high efficiency, the broad spectrum activity of stability that inorganic material is intrinsic and antimicrobial component, has successfully overcome the shortcoming of organic antibacterial agent; Inorganic bacteriostatic agent and bactericide then be meant with inorganic material most of for material such as natural or artificial mineral's material as carrier, be loaded with a kind of novel inorganic antiseptic that the metallic element that possesses certain antibacterial ability and metal ion and the antibacterial material of nanometer are developed.Two, when selecting organic antibacterial agent for use, except that considering its safety, also there is poor heat resistance in the existing quite long history of the application of organic antibacterial agent, easily decomposes and problem such as service life is short; Three, natural antibacterial agent mainly is extract with the natural plants, and serious waste of resources has been applied certain difficulty.
Summary of the invention
The present invention is in order to solve the poor stability of existing organic antibacterial agent, also exist poor heat resistance, easily decompose and service life short; Natural antibacterial agent mainly is extract with the natural plants, wastes resource, applies the problem of certain difficulty.And provide a kind of tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder and preparation method thereof.The concrete technical scheme that addresses the above problem is as follows: tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder of the present invention is by tourmaline and nano zine oxide solid, by mass percentage tourmaline be 50～99.99%, the nano zine oxide solid be 0.01～50% through mix, clean, oven dry, grind, calcining and grind again and make.
The preparation method's of tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder of the present invention step is as follows: one, adopt direct precipitation method to prepare nano zine oxide: be the ZnCl of 0.75mol/L with deionized water preparation molar concentration respectively
22H
2O solution and molar concentration are the (NH of 0.03mol/L
4)
2CO
3Solution, the ratio that according to volume ratio is 1: 1 is mixed two kinds of solution, under 90～100 ℃ condition, vibrated 12～20 minutes with the supersonic oscillations instrument, carry out suction filtration then, solid formation spends after the deionised water 1～3 time under 100～115 ℃ condition the oven dry back and grinds, calcined under 200～350 ℃ condition 2～3 hours then, grinding the Zinc oxide powder particle diameter then is 20～35nm; Two, be the tourmaline of 50～800nm with particle diameter, get tourmaline by mass percentage and be 50～99.99%, the nano zine oxide of step 1 preparation is surplus, puts into deionized water, under magnetic stirring apparatus, stir; Three, the liquid to step 2 carries out suction filtration, and uses washed with de-ionized water, dries under 90～110 ℃ condition obtaining powder after cleaning; Four, the powder to oven dry grinds, and the powder after the grinding grinds calcining the back powder once more 200～800 ℃ of calcinings 2～4 hours; Promptly obtain the inorganic inhibiting sulfate reducing bacteria powder of tourmaline carried zinc oxide.
The chemical composition of tourmaline mineral is very complicated, after the 1950's its crystal structure being determined, just proposes relatively rational structure general formula, and its general formula is expressed as: XY
3Z
6Si
6O
18 (BO
3)
3W
4, X is mainly by Na, Ca or comprise K in the formula, and perhaps the part room occupies; Y is mainly by Fe
2+(or) Mg
2+, Al
+ 3± Li
+Or Fe
3+, usually also by Mn
2+And Mn
3+Occupy; Z is mainly by Al
3+, Fe
3+Or Cr
3+Occupy, also may comprise Mg
2+And V
3+W is by OH, F-, O
-2Occupy.X, Y, the atom of 3 positions of Z or ionic species can not influence the color of tourmaline simultaneously.The tourmaline crystal structure belongs to trigonal system, C
5 3v-R3m group is so tourmaline is the heteropolarity mineral.Tourmaline is with a wide range of applications as a kind of novel environment friendly material.
Nano zine oxide especially under ultraviolet irradiation, in water and air or oxygen, can decomposite the electronegative electronics (e that moves freely at sunlight voluntarily
-), stay the hole (h of positively charged simultaneously
+).This hole can be activated airborne oxygen and become active oxygen, and extremely strong chemism is arranged, can with multiple organic matter generation oxidation reaction (comprise bacterium in organic matter), thereby most of germs and virus are killed.When the mass fraction of nano zine oxide is 1%, to golden yellow colibacillary sterilizing rate 98.86%, staphylococcic sterilizing rate is 99.93% in 5min.
It is the tourmaline of nanometer or the sub-micron of 50～800nm that the present invention has adopted particle diameter, nanometer-zinc-oxide-loaded with solid-phase synthesis, not only effectively raises nanometer-zinc-oxide-loaded amount, and has improved the sulfate reducing bacteria sterilization effects.This inorganic bacteriostatic agent has tourmaline itself can produce anion, electric polarity, spontaneous polarization effect, piezoelectricity and far infrared radiation characteristic, has improved the surface area of contact; Has the bacteria resistance function that other bacteriostatic agents do not have simultaneously, to Escherichia coli fungistatic effect 100%; Can effectively improve redox potential, suppress the activity of sulfate reducing bacteria, make it no longer to carry out sulfate reduction, no longer produce hydrogen sulfide gas and sulphide; 100%, this antibacterial pulvis adds in the fibrous woven goods to the inhibiting rate of sulfate reducing bacteria, also is widely used in improvement and water body reparation that water pollutes.There is not warm tolerance in antibacterial pulvis safety of the present invention, easily decomposes and problem that service life is short; And saving resource.For reducing sulfate reducing bacteria, has crucial meaning to field produces and economic benefit aspect.
Description of drawings
The former master drawing of Fig. 1 nano zine oxide, Fig. 2 is the SEM figure of nano zine oxide former state, Fig. 3 is the AFM figure of nano zine oxide former state, Fig. 4 is the former master drawing of tourmaline, Fig. 5 is the SEM figure of tourmaline former state, Fig. 6 is the AFM figure of tourmaline former state, Fig. 7 is tourmaline nanometer-zinc-oxide-loaded sample drawing, Fig. 8 is tourmaline nanometer-zinc-oxide-loaded stereogram, Fig. 9 is tourmaline nanometer-zinc-oxide-loaded plane, Figure 10 is tourmaline nanometer-zinc-oxide-loaded infrared spectrogram, and Figure 11 is the inhibition figure of tourmaline nanometer-zinc-oxide-loaded activity to sulfate reducing bacteria, and Figure 12 is tourmaline nanometer-zinc-oxide-loaded XRD figure.
Embodiment
Embodiment one: the tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder of present embodiment by tourmaline carried molybdenum inorganic inhibiting sulfate reducing bacteria powder by tourmaline and nano zine oxide solid, by mass percentage tourmaline be 50～99.99%, the nano zine oxide solid be 0.01～50% through mix, clean, oven dry, grind, calcining and grind again and make.
Embodiment two: tourmaline is 60% to present embodiment by mass percentage, the nano zine oxide solid is 40% to make.Other identical with embodiment one.
Embodiment three: tourmaline is 80% to present embodiment by mass percentage, the nano zine oxide solid is 20% to make.Other identical with embodiment one.
Embodiment four: tourmaline is 90% to present embodiment by mass percentage, the nano zine oxide solid is 10% to make.Other identical with embodiment one.
Embodiment five: the preparation method's of the inorganic inhibiting sulfate reducing bacteria powder that present embodiment is tourmaline nanometer-zinc-oxide-loaded step is as follows: one, adopt direct precipitation method to prepare nano zine oxide: be the ZnCl of 0.75mol/L with deionized water preparation molar concentration respectively
22H
2O solution and molar concentration are the (NH of 0.03mol/L
4)
2CO
3Solution, the ratio that according to volume ratio is 1: 1 is mixed two kinds of solution, under 90～100 ℃ condition, vibrated 12～20 minutes with the supersonic oscillations instrument, carry out suction filtration then, solid formation spends after the deionised water 1～3 time under 100～115 ℃ condition the oven dry back and grinds, calcined under 200～350 ℃ condition 2～3 hours then, grinding the Zinc oxide powder particle diameter then is 20～35nm; Two, be the tourmaline of 50～800nm with particle diameter, get tourmaline by mass percentage and be 50～99.99%, the nano zine oxide of step 1 preparation is surplus, puts into deionized water, under magnetic stirring apparatus, stir; Three, the liquid to step 2 carries out suction filtration, and uses washed with de-ionized water, dries under 90～110 ℃ condition obtaining powder after cleaning; Four, the powder to oven dry grinds, and the powder after the grinding grinds calcining the back powder once more 200～800 ℃ of calcinings 2～4 hours; Promptly obtain the inorganic inhibiting sulfate reducing bacteria powder of tourmaline carried zinc oxide.
Embodiment six: the difference of present embodiment and embodiment five is: vibrated 15 minutes with the supersonic oscillations instrument under 95 ℃ of parts in the step 1.Other steps and parameter are identical with embodiment five.
Embodiment seven: the difference of present embodiment and embodiment five is: oven dry back grinding under 105 ℃ condition in the step 1, under 280 ℃ condition, calcined 2 hours then, and grinding the Zinc oxide powder particle diameter then is 25nm.Other steps and parameter are identical with embodiment five.
Embodiment eight: the difference of present embodiment and embodiment five is: obtain powder after will cleaning in the step 3 and dry under 105 ℃ condition.Other steps and parameter are identical with embodiment five.
Embodiment nine: the difference of present embodiment and embodiment five is: the powder after grinding in the step 4 was 300～700 ℃ of calcinings 3 hours.Other steps and parameter are identical with embodiment five.
Embodiment ten: the difference of present embodiment and embodiment five is: the powder after grinding in the step 4 is 500 ℃ of calcinings.Other steps and parameter are identical with embodiment five.
Claims (10)
1. tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder, it is characterized in that by tourmaline carried molybdenum inorganic inhibiting sulfate reducing bacteria powder by tourmaline and nano zine oxide solid, by mass percentage tourmaline be 50～99.99%, the zinc oxide solid be 0.01～50% through mix, clean, oven dry, grind, calcining and grind again and make.
2. tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder according to claim 1 is characterized in that by mass percentage that tourmaline is 60%, the nano zine oxide solid is 40% to make.
3. tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder according to claim 1 is characterized in that by mass percentage that tourmaline is 80%, the nano zine oxide solid is 20% to make.
4. tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder according to claim 1 is characterized in that by mass percentage that tourmaline is 90%, the nano zine oxide solid is 10% to make.
5. the preparation method of tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder is characterized in that preparation method's the step of tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder is as follows:
One, adopt direct precipitation method to prepare nano zine oxide: to be the ZnCl of 0.75mol/L with deionized water preparation molar concentration respectively
22H
2O solution and molar concentration are the (NH of 0.03mol/L
4)
2CO
3Solution, the ratio that according to volume ratio is 1: 1 is mixed two kinds of solution, under 90～100 ℃ condition, vibrated 12～20 minutes with the supersonic oscillations instrument, carry out suction filtration then, solid formation spends after the deionised water 1～3 time under 100～115 ℃ condition the oven dry back and grinds, calcined under 200～350 ℃ condition 2～3 hours then, grinding the Zinc oxide powder particle diameter then is 20～35nm; Two, be the tourmaline of 50～800nm with particle diameter, get tourmaline by mass percentage and be 50～99.99%, the nano zine oxide of step 1 preparation is surplus, puts into deionized water, under magnetic stirring apparatus, stir; Three, the liquid to step 2 carries out suction filtration, and uses washed with de-ionized water, dries under 90～110 ℃ condition obtaining powder after cleaning; Four, the powder to oven dry grinds, and the powder after the grinding grinds calcining the back powder once more 200～800 ℃ of calcinings 2～4 hours; Promptly obtain the inorganic inhibiting sulfate reducing bacteria powder of tourmaline carried zinc oxide.
6. the preparation method of tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder according to claim 5 is characterized in that vibrating 15 minutes with the supersonic oscillations instrument under 95 ℃ of parts in the step 1.
7. the preparation method of tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder according to claim 5, it is characterized in that oven dry back grinding under 105 ℃ condition in the step 1, calcined 2 hours under 280 ℃ condition then, grinding the Zinc oxide powder particle diameter then is 25nm.
8. the preparation method of tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder according to claim 5 obtains powder after it is characterized in that will cleaning in the step 3 and dries under 105 ℃ condition.
9. the preparation method of tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder according to claim 5, the powder after it is characterized in that grinding in the step 4 was 300～700 ℃ of calcinings 3 hours.
10. the preparation method of tourmaline nanometer-zinc-oxide-loaded inorganic inhibiting sulfate reducing bacteria powder according to claim 5, the powder after it is characterized in that grinding in the step 4 is 500 ℃ of calcinings.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010136792A3 (en) * | 2009-05-26 | 2011-06-16 | Intrinsiq Materials Limited | Antibacterial composition comprising metal oxide nanoparticles |
-
2007
- 2007-09-06 CN CNA2007100727637A patent/CN101142923A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010136792A3 (en) * | 2009-05-26 | 2011-06-16 | Intrinsiq Materials Limited | Antibacterial composition comprising metal oxide nanoparticles |
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Open date: 20080319 |