CN102057901A - Preparation method of magnetic antibacterial zeolite for processing wastewater containing bacteria - Google Patents
Preparation method of magnetic antibacterial zeolite for processing wastewater containing bacteria Download PDFInfo
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- CN102057901A CN102057901A CN2010105454977A CN201010545497A CN102057901A CN 102057901 A CN102057901 A CN 102057901A CN 2010105454977 A CN2010105454977 A CN 2010105454977A CN 201010545497 A CN201010545497 A CN 201010545497A CN 102057901 A CN102057901 A CN 102057901A
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Abstract
The invention discloses a preparation method of a magnetic antibacterial zeolite for processing wastewater containing bacteria. The method is characterized in that the antibacterial performance of the antibacterial zeolite is integrated with the magnetism of a ferrite organically, and the method comprises the following steps: adhering ferrite magnetic particles with spinel structures to the surface of the zeolite serving as a carrier by a chemical coprepcipitation method, thus obtaining a magnetic zeolite; and using the liquid-phase ion exchange method to adhere antibacterial metal ions in the magnetic zeolite. By utilizing the method, the magnetic antibacterial zeolite capable of being widely applied in the treatment of the wastewater containing bacteria can be prepared; and in the magnetic antibacterial zeolite, magnetic particles account for 10-15wt% of the whole magnetic antibacterial zeolite, so that the problems of the antibacterial zeolite, such as long-time suspension in water and inconvenience for fast recovery and recycle after treatment of the wastewater containing bacteria, are solved.
Description
(1) technical field the present invention relates to a kind of preparation method who is used to handle the magnetic antibacterial zeolite particles that contains bacterium waste water.
(2) background technology contains bacterium waste water threat human health, directly influence normal life and activity in production, could discharge after should adopting certain method to handle, as biological treatment, chemical treatment, thermal treatment, catalytic oxidation, phase transfer and photodissociation etc., but these methods all exist the high or generation secondary pollution problem of processing cost.
Some metal ions are as Ag
+, Cu
2+, Zn
2+Have good antibacterial performance, by certain technology with these metal ion appendix in having the big carrier of ion exchange absorption performance or specific surface area, can be widely used in containing the bacterium field of waste water treatment.Zeolite (comprising artificial synthetic zeolite and natural zeolite) is that a class has hole link, is the hydrous alumino silicates micropore mineral of frame columnar structure, has good ion-exchange performance, and excellent performances such as acidproof, heat-resisting, radiation hardness are suitable for doing the carrier of antibacterial metal ions.Adopt the ionic liquid phase exchange process with Ag
+, Cu
2+, Zn
2+Deng the antibacterial zeolite particles that the metal ion appendix forms, has the good anti-microbial property that antibiotic rate height, anti-microbial property are lasting, can reuse in zeolite.In the antibacterial zeolite particles preparation process, in order to improve exchange velocity and the exchange capacity of zeolite to metal ion, generally all need earlier zeolite to be processed into impalpable powder powder (general tens of microns), when processing contained bacterium waste water, the tiny antibacterial zeolite particles of granularity suspended in water for a long time to be difficult to separate fast from contain bacterium waste water and reclaims.Can solve the quick separation problem of solid-liquid though make particle with certain intensity and shape by adding adhesive in zeolite powder, but the anti-microbial property that adds the corresponding reduction zeolite of joining of adhesive, so this has also restricted antibacterial zeolite particles in the extensive use that contains the bacterium field of waste water treatment.
Since the magnetisable material that suspends in water can be fast under the effect of externally-applied magnetic field and moisture from, therefore, make magnetic zeolite as adhering to a certain amount of magnetic particle at zeolite surface earlier, adopt the ionic liquid phase exchange process that the antibacterial metal ions appendix is made the magnetic antibacterial zeolite particles again in magnetic zeolite, can after processing contains bacterium waste water, utilize magnetic separation technique to carry out solid-liquid and separate fast.And the spinel type ferrite of making by iron family element and other one or more proper metal elements, have characteristics such as kind is many, application is wide, the preparation method is simple, spinel type ferrite particularly, the superparamagnetism that tool is good, easy magnetization, also easily demagnetization is suitable as the magnetic particle in the magnetic antibacterial zeolite particles, and as adopting the chemical coprecipitation preparation, its preparation process is simple, cost is low.
Therefore, the present invention organically combines the magnetic of anti-microbial property that antibacterial zeolite particles had and ferrite institute tool, is carrier with the zeolite earlier promptly, adopts chemical coprecipitation, with the ferrite (MeFe of spinel structure
2O
4, Me is Fe
2+, Mn
2+, Zn
2+, Cu
2+, Ni
2+, Mg
2+, Co
2+A kind of in the bivalent metal ion) magnetic particle is attached to zeolite surface and makes magnetic zeolite, with the ionic liquid phase exchange process antibacterial metal ions appendix is prepared in magnetic zeolite again and can be widely used in the magnetic antibacterial zeolite particles that contains the bacterium wastewater treatment, to solve antibacterial zeolite particles suspended in water, was difficult to quick recovery for a long time, repeats to utilize again after processing contains bacterium waste water a difficult problem.
(3) summary of the invention
1, goal of the invention; The purpose of this invention is to provide the preparation method that a kind of processing contains the magnetic antibacterial zeolite particles of bacterium waste water.
2, technical scheme: technical scheme of the present invention is: a kind ofly be used to handle the magnetic antibacterial zeolite particles preparation method who contains bacterium waste water, it is to be carrier with the zeolite, make magnetic zeolite after adopting chemical coprecipitation that magnetic particle is attached to zeolite surface earlier, utilize again the ionic liquid phase exchange process with metal antibacterial ion appendix in magnetic zeolite, preparation has anti-microbial property and magnetic property, can be widely used in containing the magnetic antibacterial zeolite particles of bacterium wastewater treatment.Its concrete operations step is:
1) be 1 by solid-to-liquid ratio: (10～30) will join through the zeolite powder that the 100-200 mesh sieve is crossed in fragmentation, grinding, dry back and make the zeolite suspension in the deionized water, again according to MeFe in the magnetic zeolite for preparing
2O
4The magnetic particle mass fraction is 10～50%, takes by weighing the needed Fe of containing
2+, Mn
2+, Zn
2+, Cu
2+, Ni
2+, Mg
2+, Co
2+In a kind of bivalent metal ion Me
2+Hydrochloride or nitrate or sulphate and contain Fe
3+Hydrochloride or nitrate or sulphate, and join in the zeolite suspension, fully stir 15～30 minutes after, ultrasonic dispersion made and contains zeolite, Me in 30～60 minutes
2+And Fe
3+Suspension, with this suspension stir be warming up to 50～80 ℃ after, when continuing stirring, with mass fraction is that 15～25% ammoniacal liquor or the NaOH drips of solution of 1.0～2.0mol/L add in the suspension, after the adjusting pH of suspension is 11～13, under stirring it was fully reacted 30～90 minutes, crystallization after 1～2 hour in 60～80 ℃ of following waters bath with thermostatic control again, filter and the washing filter residue, filter residue successively in 105 ℃ of vacuum dryings 1～3 hour, 300～500 ℃ the calcining 1～2 hour after, grind 200 mesh sieves again, promptly made MeFe
2O
4The magnetic particle mass fraction is 10～50% magnetic zeolite;
2) configuration concentration is the Ag that contains of 0.1～0.5mol/L
+, Cu
2+, Zn
2+In the nitrate solution or the mixed solution of one or more metal ions, be 1 with solid-to-liquid ratio again: (10～30) add magnetic zeolite, after fully stirring 60～120 minutes under 30～80 ℃, utilizing externally-applied magnetic field to carry out solid-liquid separates fast, and after adopting deionized water washing magnetisable material 2～4 times, magnetisable material in 105 ℃ of following vacuum dryings 1～3 hour, is promptly made the magnetic antibacterial zeolite particles.
Advantage of the present invention is that the magnetic of anti-microbial property that antibacterial zeolite particles is had and ferrite institute tool organically combines preparation magnetic antibacterial zeolite particles.Because the good ion-exchange performance that zeolite itself is had, the antibacterial metal ions of appendix can slowly discharge when actual treatment contains bacterium waste water in the zeolite, promptly has good antibiotic persistence; And magnetic particle is attached to zeolite surface and have stronger magnetic.In containing the bacterium wastewater treatment process, the magnetic antibacterial zeolite particles can adopt magnetic separation technique to carry out solid-liquid and separate fast, utilizes after containing bacterium waste water and handling.Descend as its anti-microbial property in magnetic antibacterial zeolite particles repeated use process, also can by the ionic liquid phase exchange process metal antibacterial ion appendix be separated in the regenerant to magnetic once more, thereby regenerate its anti-microbial property, realize that it repeatedly reuses.Therefore, magnetic antibacterial zeolite particles of the present invention can be after processing contains bacterium waste water can be under the externally-applied magnetic field effect Separation of Solid and Liquid fast, and can reuse, have stronger practical value.The magnetic antibacterial zeolite particles that obtains all reaches more than 99% the antibiotic rate of Escherichia coli and staphylococcus aureus.
(4) description of drawings
Fig. 1 is the preparation flow of magnetic antibacterial zeolite particles; Fig. 2 is the hysteresis curve of MAZ1 of the present invention, MAZ2, MAZ3.
(5) embodiment
Embodiment 1
By solid-to-liquid ratio is 1: 10, and the 5A zeolite 20.88g that will cross 100 mesh sieves after fragmentation, grinding, drying joins the suspension that makes the 5A zeolite in the 100mL deionized water, again according to FeFe in the magnetic 5A zeolite of preparation
2O
4(Fe
3O
4) the magnetic particle mass fraction is 10%, takes by weighing FeSO respectively
47H
2O, FeCl
36H
2Each 2.78g of O, 5.41g join in the 5A zeolite suspension, fully stir 30 minutes after, made in 30 minutes in ultrasonic dispersion again and contain 5A zeolite, Fe
2+And Fe
3+Suspension, with this suspension stir be warming up to 80 ℃ after, when continue stirring be after pH that 25% ammoniacal liquor drops to suspension is 13 with mass fraction, be allowed to condition at and stir down fully reaction 90 minutes, crystallization after 1 hour in 80 ℃ water bath with thermostatic control is filtered also washing filter residue again, and filter residue is successively in 105 ℃ of vacuum dryings 2 hours, 300 ℃ of calcinings after 1 hour, be ground to-200 orders again, promptly make Fe
3O
4The magnetic particle mass fraction is 10% magnetic 5A zeolite.
Configuration concentration is the AgNO of 0.1mol/L
3Solution 100mL, be 1: 10 adding magnetic 5A zeolite 10g with solid-to-liquid ratio again, after fully stirring 120 minutes under 50 ℃, utilize the quick Separation of Solid and Liquid of externally-applied magnetic field, and after adopting deionized water washing magnetisable material 2 times, magnetisable material is made the antibiotic 5A zeolite of magnetic (MAZ1) in 105 ℃ of following vacuum dryings after 2 hours, the antibiotic 5A zeolite of the magnetic that obtains is respectively 99.9%, 99.9% to the antibiotic rate of Escherichia coli and staphylococcus aureus.
Embodiment 2
By solid-to-liquid ratio is 1: 10, will cross the clinoptilolite 9.28g of 100 mesh sieves after fragmentation, grinding, drying, adds among the deionized water 100mL to make the clinoptilolite suspension, again according to FeFe in the magnetic clinoptilolite of preparation
2O
4(Fe
3O
4) the magnetic particle mass fraction is 20%, takes by weighing FeSO respectively
47H
2O, FeCl
36H
2Each 2.78g of O, 5.41g join in the clinoptilolite suspension, fully stir 30 minutes after, made in 30 minutes in ultrasonic dispersion again and contain clinoptilolite, Fe
2+And Fe
3+Suspension, with this suspension stir be warming up to 80 ℃ after, the NaOH that with concentration is 2.0mol/L when continue stirring drops in the suspension, regulate after pH of suspension is 12, it was fully reacted 90 minutes, again crystallization after 1 hour in 80 ℃ water bath with thermostatic control, filter and the washing filter residue, filter residue after 1 hour, is ground to-200 orders in 105 ℃ of vacuum dryings 2 hours, 300 ℃ of calcinings successively again, promptly makes Fe
3O
4The magnetic particle mass fraction is 20% magnetic clinoptilolite.
Configuration concentration is the Cu (NO of 0.2mol/L
3)
2Solution 100mL, be 1: 10 adding magnetic clinoptilolite 10g with solid-to-liquid ratio again, after fully stirring 120 minutes under 50 ℃, utilize the quick Separation of Solid and Liquid of externally-applied magnetic field, and after adopting deionized water washing magnetisable material 2 times, magnetisable material is made the antibiotic clinoptilolite of magnetic (MAZ2) in 105 ℃ of following vacuum dryings after 1 hour, the antibiotic clinoptilolite of the magnetic that obtains is respectively 99.9%, 99.5% to the antibiotic rate of Escherichia coli and staphylococcus aureus.
Embodiment 3
By solid-to-liquid ratio is 1: 10, will cross the 4A zeolite 10.83g of 100 mesh sieves after fragmentation, grinding, drying, adds among the deionized water 100mL to make 4A zeolite suspension, again according to FeFe in the magnetic 4A zeolite of preparation
2O
4(Fe
3O
4) the magnetic particle mass fraction is 30%, takes by weighing FeSO respectively
47H
2O, FeCl
36H
2Each 5.56g of O, 10.82g join in the 4A zeolite suspension, fully stir 30 minutes after, made in 30 minutes in ultrasonic dispersion again and contain 4A zeolite, Fe
2+And Fe
3+Suspension, with this suspension stir be warming up to 80 ℃ after, when continue stirring be that 25% ammoniacal liquor drops in the suspension with mass fraction, regulate after pH of suspension is 13, it was fully reacted 90 minutes, again crystallization after 1 hour in 80 ℃ water bath with thermostatic control, filter and the washing filter residue, filter residue after 1 hour, grinds-200 orders in 105 ℃ of vacuum dryings 2 hours, 400 ℃ of calcinings successively again, promptly makes Fe
3O
4The magnetic particle mass fraction is 30% magnetic 4A zeolite.
Configuration concentration is the Zn (NO of 0.2mol/L
3)
2Solution 100mL, be 1: 10 adding magnetic 4A zeolite 10g with solid-to-liquid ratio again, after fully stirring 120 minutes under 50 ℃, utilize the quick Separation of Solid and Liquid of externally-applied magnetic field, and after adopting deionized water washing magnetisable material 2 times, magnetisable material is made the antibiotic 5A zeolite of magnetic (MAZ3) in 105 ℃ of following vacuum dryings after 2 hours, the antibiotic 4A zeolite of the magnetic that obtains is respectively 99.3%, 99.2% to the antibiotic rate of Escherichia coli and staphylococcus aureus.
Can prepare the product that reaches the object of the invention by the foregoing description, the invention is not restricted to these embodiment.
Claims (6)
1. the preparation method of a magnetic antibacterial zeolite particles that is used to handle contain bacterium waste water, it is characterized in that, it is to be carrier with the zeolite, make magnetic zeolite after adopting chemical coprecipitation that magnetic particle is attached to zeolite surface earlier, utilize again the ionic liquid phase exchange process with metal antibacterial ion appendix in magnetic zeolite, preparation has anti-microbial property and magnetic property, can be widely used in handling the magnetic antibacterial zeolite particles that contains bacterium waste water.
2. the preparation method who is used to handle the magnetic antibacterial zeolite particles that contains bacterium waste water according to claim 1 is characterized in that preparation method's step is as follows:
1) be will through fragmentation, grinding, dry back cross 100-200 purpose zeolite at 1: 10 to add in the deionized water and make the zeolite suspension by solid-to-liquid ratio, again according to MeFe in the magnetic zeolite for preparing
2O
4The magnetic particle mass fraction is 10～25%, takes by weighing the needed Fe of containing
2+, Mn
2+, Zn
2+, Cu
2+, Ni
2+, Mg
2+, Co
2+In a kind of bivalent metal ion Me
2+Hydrochloride or nitrate or sulphate and contain Fe
3+Hydrochloride or nitrate or sulphate, join in the lump in the zeolite suspension, fully stir 15～30 minutes after, made in 30～60 minutes in ultrasonic dispersion again and contain zeolite, Me
2+And Fe
3+Suspension, with this suspension stir be warming up to 50～80 ℃ after, when continue stirring be that 15～25% ammoniacal liquor or the NaOH drips of solution of 1.0～2.0mol/L add in the suspension with mass fraction, after the adjusting pH of suspension is 11～13, stir fully reaction 30～90 minutes, again in 60～80 ℃ of following water bath with thermostatic control crystallization after 1～2 hour, filter and the washing filter residue, filter residue successively in 105 ℃ of vacuum dryings 1～3 hour, 300～500 ℃ the calcining 1～2 hour after, grind 200 mesh sieves again, promptly made MeFe
2O
4The magnetic particle mass fraction is 10～50% magnetic zeolite;
2) configuration concentration is the Ag that contains of 0.1～0.5mol/L
+, Cu
2+, Zn
2+In the nitrate solution of a metal ion species, be 1: 10～1: 50 adding magnetic zeolite with solid-to-liquid ratio again, after fully stirring 60～120 minutes under 30～80 ℃, utilize the quick Separation of Solid and Liquid of externally-applied magnetic field, and after adopting deionized water washing magnetisable material 2～4 times, magnetisable material is made the magnetic antibacterial zeolite particles in 105 ℃ of following vacuum dryings after 1～3 hour.
3. the preparation method who is used to handle the magnetic antibacterial zeolite particles that contains bacterium waste water according to claim 1 and 2 is characterized in that described zeolite is artificial synthetic zeolite or natural zeolite.
4. the preparation method who is used to handle the magnetic antibacterial zeolite particles that contains bacterium waste water according to claim 1 and 2 is characterized in that described magnetic particle is spinel-type MeFe
2O
4Magnetic particle, wherein bivalent metal ion Me
2+Be Fe
2+, Mn
2+, Zn
2+, Cu
2+, Ni
2+, Mg
2+, Co
2+In a kind of.
5. the preparation method who is used to handle the magnetic antibacterial zeolite particles that contains bacterium waste water according to claim 1 and 2 is characterized in that the mass fraction of magnetic particle is 10～50% in the described magnetic zeolite.
6. the preparation method who is used to handle the magnetic antibacterial zeolite particles that contains bacterium waste water according to claim 1 and 2 is characterized in that described metal antibacterial ion is Ag
+, Cu
2+, Zn
2+In one or more.
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Cited By (6)
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| CN102578149A (en) * | 2012-01-14 | 2012-07-18 | 哈尔滨工程大学 | Magnetic sterilizing material as well as preparation method and application method thereof |
| CN103109864A (en) * | 2013-01-30 | 2013-05-22 | 黑龙江大学 | Preparation method of recyclable silver-embedded magnetic compound bacteriostat |
| WO2015028818A1 (en) * | 2013-08-29 | 2015-03-05 | University Of Central Lancashire | Antimicrobial nanocomposites |
| CN106734129A (en) * | 2016-12-22 | 2017-05-31 | 胡自田 | A kind of sulfide modifier maize straw soil remediation conditioner and preparation method thereof |
| CN106734162A (en) * | 2016-12-22 | 2017-05-31 | 胡自田 | A kind of inexpensive soil-repairing agent doped with activated sludge and preparation method thereof |
| CN106734130A (en) * | 2016-12-22 | 2017-05-31 | 胡自田 | A kind of improving salinization soil red mud base modified soil renovation agent and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102578149A (en) * | 2012-01-14 | 2012-07-18 | 哈尔滨工程大学 | Magnetic sterilizing material as well as preparation method and application method thereof |
| CN103109864A (en) * | 2013-01-30 | 2013-05-22 | 黑龙江大学 | Preparation method of recyclable silver-embedded magnetic compound bacteriostat |
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| CN106734129A (en) * | 2016-12-22 | 2017-05-31 | 胡自田 | A kind of sulfide modifier maize straw soil remediation conditioner and preparation method thereof |
| CN106734162A (en) * | 2016-12-22 | 2017-05-31 | 胡自田 | A kind of inexpensive soil-repairing agent doped with activated sludge and preparation method thereof |
| CN106734130A (en) * | 2016-12-22 | 2017-05-31 | 胡自田 | A kind of improving salinization soil red mud base modified soil renovation agent and preparation method thereof |
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Application publication date: 20110518 |