CN108557927A - A kind of multifunction magnetic water purification agent and its preparation method and application - Google Patents
A kind of multifunction magnetic water purification agent and its preparation method and application Download PDFInfo
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- CN108557927A CN108557927A CN201810721469.2A CN201810721469A CN108557927A CN 108557927 A CN108557927 A CN 108557927A CN 201810721469 A CN201810721469 A CN 201810721469A CN 108557927 A CN108557927 A CN 108557927A
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- 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
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- 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
Abstract
The invention discloses a kind of multifunction magnetic water purification agents and its preparation method and application, belong to field of waste water treatment.The material is to disperse magnetic phosphate nano or Micron-nano composites in a solvent, AgNO to be added later3Aqueous solution, ultrasound to being uniformly dispersed, obtain mixed liquor；Later under the action of stirring or ultrasound, the aqueous solution of reducing agent is rapidly added in the mixed liquor of the first step, continue stirring after after separation and washing dry to get loaded Ag composite magnetic phosphate.Magnetic water purification agent in the present invention can remove the multiple pollutant in waste water, can multiple pollutants such as Escherichia coli, organic dyestuff, metal ion in purified water simultaneously.
Description
Technical field
The invention belongs to technical field of waste water processing, and in particular to a kind of multifunction magnetic water purification agent and preparation method thereof and
Using.
Background technology
Nano material is used for the removal of Escherichia coli in solution, is the skill in research and development in biological solution processing technology field
Art.Magnetic Nano material has the characteristics that easily to recycle, reusable, cost-effective, reduces the residual of water scavengine agent to water body
Caused by secondary pollution, therefore magnetic composite nano water scavengine agent has received widespread attention in scientific research and practical application.
Currently, the bacterium, organic dyestuff and heavy metal contaminants in water body constitute serious environmental threat to human health and safety.
Therefore, there is an urgent need to develop the preferably technologies of purified water from various pollutants.It can be effective using a kind of simple material
Multiple pollutant in processing waste water is a challenge.
It has been reported and shows to contain Fe3O4Water scavengine agent due to its using it is easy, be easy to detach from solution, in dirt
Secondary pollution is avoided in water process, makes it have good advantage.This material is usually grouped as by different groups, therefore same
The property of different component can be shown in one nanostructure.However, seldom having been reported that magnetic nanometer composite material is used for while going
Except bacterium and other kinds of pollutant.In most cases, these are used for the material of pollutant removal by Fe3O4With graphene,
Nano silver, chitosan or other organisms etc. are combined.For example, magnetic graphene is used to heavy metal in control water and thin
Bacterium；Silver-ferric oxide nano particles of fine coal gray surface are used for removing bacterium and Pb2+；Chitosan magnetic-graphene oxide composite wood
Material is for the removal of antimicrobial and dyestuff.However, some material preparation processes are complicated, cost is higher, such as graphite alkenes material, has
Organic principle in a little materials may cause secondary pollution during preparation or use to environment.In addition, these materials pair
The removal efficiency of bacterium, dyestuff and metal ion is limited in sewage, to being up to 108The bacterium solution of CFU/mL is more than
The metal ion of 100mg/L high concentrations or the clean-up effect of organic dyestuff are rarely reported.Current report is as contained 50,24 and
0.4mg/mL Fe3O4Embedding ZnO magnetic Nano materials can purify respectively 15-45mg/L metal ions, 10mg/L dyestuffs andStaphylococcus aureus (J.Mater.Chem.A, 2013,1,3325-3333)；0.05mg/mL Ag modifications
Magnetic core shell nanosphere can purify a concentration of 1.6 × 107Bacterial solution (Colloids the and Surfaces, B of CFU/mL:
Biointerfaces.2015,133:58-65)；6.25μg/mL Ag-CoFe2O4- GO nano materials pair 105CFU/mL bacteriums are molten
The removal rate of liquid is 98.8%, Pb2+Removal rate be 60.8mg/g (ACS Applied Materials＆
Interfaces.2015,7:10576-10586).Nano-cellulose and silver nanoparticle insertion cobble show 99% removal of bacteria rate
(C0=105CFU/mL), to methylene blue, Pb2+And Cr3+Adsorbance be respectively 38mg/g, 9.42mg/g and 8.93mg/g
(Environmental Technology,2015,16:706-714)。
Though above-mentioned material is successfully used for complicated pollutant in processing water, material preparation is complicated, and cost is higher, can locate
The pollutant concentration of reason is limited, and lacks compliance test result to the clean-up effect of the lower or different mixed pollutants of high salinity interference.
Invention content
That the present invention be directed to existing magnetic Nano water scavengine agents is of high cost, prepare complicated, easy secondary pollution, can not a variety of dirts
Dye type purify simultaneously, be low to target contaminant purifying rate in high interference ion and highrank fuel salinity water etc. the problems such as insufficient provide it is a kind of
Multifunction magnetic water purification agent and its preparation method and application.
A kind of multifunction magnetic water purification agent, the material are prepared via a method which to obtain：
The first step disperses magnetic phosphate nano or Micron-nano composites in a solvent, AgNO to be added later3's
Aqueous solution, ultrasound obtain mixed liquor to being uniformly dispersed；
Second step is rapidly added the aqueous solution of reducing agent under the action of stirring or ultrasound in the mixed liquor of the first step,
Continue stirring 15~40 minutes, stand 1~5 hour, after after separation and washing dry to get loaded Ag composite magnetic phosphorus
Hydrochlorate.
A kind of preparation method of multifunction magnetic water purification agent, this approach includes the following steps：
The first step disperses magnetic phosphate nano or Micron-nano composites in a solvent, AgNO to be added later3's
Aqueous solution, ultrasound obtain mixed liquor to being uniformly dispersed；
Second step is rapidly added the aqueous solution of reducing agent under the action of stirring or ultrasound in the mixed liquor of the first step,
Continue stirring 15~40 minutes, stand 1~5 hour, after after separation and washing dry to get loaded Ag composite magnetic phosphorus
Hydrochlorate.
In technical solution of the present invention：Solvent described in the first step is water, methanol or ethyl alcohol；As preferred：First step institute
The solvent stated is water.
In technical solution of the present invention：The reducing agent described in two step of reducing agent described in second step is NaBH4, sodium sulfite,
Azanol NH2OH, hydrazine N2H4, glycine, glucose, ascorbic acid, common water-soluble inorganic or the organic reducing agent such as ethylene glycol；It is excellent
Select NaBH4。
In technical solution of the present invention：Reducing agent and AgNO3Molar ratio be preferably 0.01-100：1.
In technical solution of the present invention：The load capacity of Ag is 1~15%. in the composite magnetic phosphate of loaded Ag
Multifunction magnetic water purification agent described in the technical solution of the present invention heavy metal ion and/or organic in removing solution
Pollutant and/or the application for adsorbing Escherichia coli.
Heavy metal ion described in technical solution of the present invention is preferably lead ion；The organic pollution is preferably the Congo
One or more of red, malachite green, methyl blue, acid fuchsin.
In some specific technical solutions：Weight in a kind of composite magnetic phosphate removal solution using above-mentioned loaded Ag
Metal ion and/or organic dyestuff and/or the method for adsorbing Escherichia coli, this method are that adjusting solution ph is 4~9, will be born
The even dispersion of composite magnetic phosphate for carrying Ag in the solution, is stirred to react 10-60 minutes at 5 DEG C~40 DEG C.After the completion of stirring
Make the water purification agent aggregation for being attached with pollutant under magneticaction, realizes and be separated by solid-liquid separation.
Wherein the dosage of multifunction magnetic water purification agent is every liter of dirt containing Escherichia coli or lead ion or organic dyestuff
2-10 grams is added in water；
In above-mentioned processing method：A concentration of 10-1000mg/L of the heavy metal ion, the organic pollution
A concentration of 10-1000mg/L, a concentration of the 10 of the Escherichia coli5-109CFU/mL。
Magnetic phosphate nano or Micron-nano composites described in technical solution of the present invention be using application No. is
Technical solution disclosed in 2017103461997 is prepared.
In some specific technical solutions：The preparation side of the magnetic phosphate nano or Micron-nano composites
Method includes the following steps：
(1) soluble ferric iron salt is dissolved in common organic alcohols solvent, it is poly- that sodium acetate, surfactant and solid is added
Ethylene glycol reacts 1~48 hour in being fitted into reaction kettle at 85~300 DEG C, product after reaction by centrifugation, filtering or
Person's Magnetic Isolation, washing, drying to obtain ferriferrous oxide nano/micro materials；
(2) soluble metallic salt is dissolved in the water, ferriferrous oxide nanometer material is added, surfactant, mixing are equal
It is even to obtain solution；
(3) soluble-salt of phosphorous acid group is dissolved in the water, obtains the soluble-salt aqueous solution of phosphorous acid group, thinks step
(1) it is gradually added dropwise in the solution obtained, until the two is thoroughly mixed, is reloaded into reaction kettle, it is small that 1~48 is reacted at 5~300 DEG C
When, the product after reaction is by centrifuging, filtering either Magnetic Isolation, washing, drying to obtain magnetism phosphate nano or micro-
Nanocomposite.
In above-mentioned preparation method：The soluble ferric iron salt be iron chloride, ferric nitrate, one or both of ferric sulfate with
On；It is preferred that the soluble ferric iron salt is iron chloride.
In above-mentioned preparation method：The organic alcohols solvent be ethylene glycol, ethyl alcohol, isopropanol, one kind in methanol or
It is two or more.
The dosage of the soluble metallic salt and the soluble-salt of phosphorous acid group, generally according to the phosphate of required preparation
The mol ratio of metal cation and phosphate radical calculates the use of the soluble-salt of soluble metallic salt and phosphorous acid group in material
Amount or a certain raw material are excessive, ensure that product generates completely, the soluble metallic salt, surfactant and phosphorous acid group
Soluble-salt mass ratio be 1: 0.1: 0.5-10.
The soluble metallic salt is made of metal cation and anion, the metal cation and phosphate material
Sr can be selected in metal cation meaning having the same in material2+、Ba2+、Ca2+One or both of, soluble metallic salt
In anion is not required particularly, it is only necessary to meet and Sr2+、Ba2+、Ca2+In conjunction with rear for soluble salt.
The anion can be selected one or two kinds of in organic acid anions, inorganic acid radical ion.
It is one or more kinds of in the preferred chlorion of inorganic acid radical ion, nitrate ion.
Sodium phosphate, sodium dihydrogen phosphate, disodium-hydrogen, ammonium phosphate, phosphorus can be selected in the soluble-salt of the phosphorous acid group
One or more of acid dihydride ammonium, monoammonium phosphate, potassium phosphate, potassium dihydrogen phosphate, potassium phosphate,monobasic.
The surfactant can play the role of soft template, and co-product forms regular pattern, and ability can be selected
The common surfactant in domain, preferably neopelex, diethylenetriamine, quaternary ammonium compound, stearic acid, glycine betaine,
One or more of amino acid, fatty glyceride, lecithin, fatty acid sorbitan, polysorbate.
The soluble-salt concentration of the phosphorous acid group, the concentration of the soluble metallic salt can influence product phosphoric acid
The pattern of salt, under the conditions of concentration is higher, product regularity is deteriorated, and size becomes smaller, to influence the performance of product.It is terrible
Soluble-salt concentration to more regular product, the phosphorous acid group is preferably 0.02-1.2mol/L, the solubility gold
The concentration for belonging to salt is preferably 0.03-0.8mol/L.
In step (1), pH to 6-7 is preferably adjusted after mixing.It is too sour to prevent ferroso-ferric oxide by chemical attack, too alkali
Prevent metal ion strontium or barium from generating strontium hydroxide or the follow-up phosphatic generation of barium hydroxide interference.The common acid of generally use
Property pH adjusting agent is adjusted, such as dilute hydrochloric acid, dust technology.
In step (2), reaction condition is preferentially selected as：It is reacted 2-8 hours at 100 DEG C -200 DEG C.Temperature it is too low or when
Between it is too short, product morphology is bad.The too high easy sintering of temperature, product specific surface area is small, and effective active site is reduced, being unfavorable for property
Energy.Time can be appropriately extended, and product morphology does not have too big variation, but it is uneconomical to consume energy, and a large amount of to extend the time, solvent can
It can slowly volatilize, product sinters.
Wash conditions are preferentially selected as：The solvent of washing is one or both of water or alcohol, is washed 3-7 times.Usually
Before this wash 3-5 times, then alcohol wash 3-5 times, to reduce follow-up drying time.
Drying condition is preferentially selected as：Dry 1-24 hours at 30 DEG C -60 DEG C, vacuum is ferroso-ferric oxide in order to prevent
Middle ferrous iron is aoxidized.
In some preferred technical solutions, the magnetic phosphate nano or Micron-nano composites are to use Shen
Please number be 2017103461997, composite material is prepared in any one of Examples 1 to 6 described in specification method.
Compared with prior art, the method for the present invention has the following advantages that：
1. silver nano-grain is newly added in the magnetic material of the present invention, the bactericidal properties of composite material can be promoted
2. the magnetic material of the present invention can be used for removing Escherichia coli, organic pollution or one kind in metal ion or two
Kind or more,
3. the magnetic material of the present invention can be in the presence of the salinity of high concentration and interfering ion to the target stains in waste water
Object efficiently quickly removes.
4. the magnetic material recycling of the present invention is convenient, fast, the secondary pollution to water body, the saturated magnetization of material can avoid
Intensity about 1-50emu/g, with magnet or calutron.
It effectively reduces cost, recycles 1-5 times 5. the magnetic material of the present invention can be recycled for multiple times, a variety of dirts in waste water
Dye object removal rate may remain in 70%-99%.
Description of the drawings
Fig. 1 is the material of comparative example 1, embodiment 1, embodiment 2 and embodiment 3 being killed to Escherichia coli in ten minutes
Bacterium rate comparison diagram.
Fig. 2 is that (NaCl is dense in different salinity for the magnetic barium phosphate material that is obtained after 2 grams of 2 silver nano-grains of embodiment are compound
Degree) sterilizing rate comparison diagram in lower ten minutes.
Fig. 3 be the material of comparative example 1, embodiment 1, embodiment 2 and embodiment 3 to the lead ion containing 500mg/L and
The removal rate comparison diagram of lead ion and malachite green in the malachite green mixed solution of 500mg/L.
Fig. 4 is that the material of comparative example 1, embodiment 1, embodiment 2 and embodiment 3 purifies 5 × 10 respectively8The large intestine of CFU/mL
Bacillus liquid, the lead ion aqueous solution (pH is adjusted to 5) of 100mg/L, the purifying rate of malachite green aqueous solution of 100mg/L and right
Contain 5 × 10 in mixed liquor8The Escherichia coli of CFU/mL, the lead ion of 100mg/L, 100mg/L malachite green purifying rate.
Specific implementation mode
Present invention is further described in detail with reference to embodiments, and but the scope of the present invention is not limited thereto：
Embodiment 1
The preparation method of magnetic phosphate nano or Micron-nano composites used in the present embodiment is as follows：
0.03mol strontium nitrates are added in 40 milliliters of deionized water and are dissolved, four standby oxidations three of 0.06 restraint are added
Ferrum nano material is stirred well to evenly dispersed, as solution 1,0.01mol sodium phosphates is added in 20 milliliters of deionized water
Dissolving, as solution 2, solution 2 are slowly dropped into solution 1, and the mixed solution is placed in 40 DEG C of water-baths, are sufficiently stirred
30 minutes, which is poured into 100 milliliters of pyroreaction kettles, is reacted 12 hours at 180 DEG C, be cooled to room temperature, spend
Ionized water cleans 3-5 times, then cleans vacuum drying 4 hours at 3 times, 60 DEG C with ethyl alcohol, obtains the magnetic di of pale pink
Strontium nano material.
A kind of preparation method of multifunction magnetic water purification agent, is as follows：
The first step, 1 gram of magnetic di strontium nano material are dispersed in 10 grams of water, and a concentration of 0.1mol/L is added later
AgNO30.93 milliliter of aqueous solution, ultrasonic disperse 10 minutes, obtains mixed liquor；
Second step is rapidly added 1 milliliter, 0.01mol/L under the action of stirring or ultrasound in the mixed liquor of the first step
NaBH4Aqueous solution continues stirring after twenty minutes, stands 2 hours, and precipitation is washed with water with the method for centrifugation or magnet adsorption
2 times, then ethyl alcohol washing, 50-60 DEG C of drying in an oven is put later to get the composite magnetic strontium phosphate of load 1%Ag.
Embodiment 2
The preparation method of magnetic phosphate nano or Micron-nano composites used in the present embodiment is as follows：
0.03mol barium nitrates are added in 40 milliliters of deionized water and are dissolved, four standby oxidations three of 0.06 restraint are added
Ferrum nano material is stirred well to evenly dispersed, as solution 1,0.01mol sodium phosphates is added in 20 milliliters of deionized water
Dissolving, as solution 2, solution 2 are slowly dropped into solution 1, and the mixed solution is placed in 40 DEG C of water-baths, are sufficiently stirred
30 minutes, which is poured into 100 milliliters of pyroreaction kettles, is reacted 12 hours at 180 DEG C, be cooled to room temperature, spend
Ionized water cleans 3-5 times, then cleans vacuum drying 4 hours at 3 times, 60 DEG C with ethyl alcohol, and the magnetic barium phosphate for obtaining pale pink is received
Rice material.
A kind of preparation method of multifunction magnetic water purification agent, is as follows：
The first step, 1 gram of magnetic di barium nano material are dispersed in 10 grams of water, and a concentration of 0.6mol/L is added later
AgNO30.93 milliliter of aqueous solution, ultrasonic disperse 10 minutes, obtains mixed liquor；
Second step is rapidly added 1 milliliter, 0.06mol/L under the action of stirring or ultrasound in the mixed liquor of the first step
NaBH4Aqueous solution continues stirring after twenty minutes, stands 2 hours, and precipitation is washed with water with the method for centrifugation or magnet adsorption
2 times, then ethyl alcohol washing, 50-60 DEG C of drying in an oven is put later to get the composite magnetic barium phosphate of load 6%Ag.
Embodiment 3
0.015mol barium nitrates and 0.015mol strontium nitrates are dissolved in 40 milliliters of deionized water, add 0.06 gram
The ferriferrous oxide nanometer material of preparation is stirred well to evenly dispersed, as solution 1, and 20 millis are added in 0.01mol sodium phosphates
It dissolves, as solution 2, solution 2 is slowly dropped into solution 1, and the mixed solution is placed in 40 DEG C of water in the deionized water risen
It in bath, is sufficiently stirred 30 minutes, which is poured into 100 milliliters of pyroreaction kettles, reacted 12 hours at 180 DEG C,
It is cooled to room temperature, is cleaned 3-5 times with deionized water, then vacuum drying 4 hours at 3 times, 60 DEG C are cleaned with ethyl alcohol, obtain pale pink
Magnetic strontium phosphate barium composite nano materials.
A kind of preparation method of multifunction magnetic water purification agent, is as follows：
The first step, 1 gram of magnetic di strontium barium nano material are dispersed in 10 grams of water, and a concentration of 1mol/L is added later
AgNO30.93 milliliter of aqueous solution, ultrasonic disperse 10 minutes, obtains mixed liquor；
Second step is rapidly added 1 milliliter, 0.15mol/L under the action of stirring or ultrasound in the mixed liquor of the first step
NaBH4Aqueous solution continues stirring after twenty minutes, stands 2 hours, and precipitation is washed with water with the method for centrifugation or magnet adsorption
2 times, then ethyl alcohol washing, 50-60 DEG C of drying in an oven is put later to get the composite magnetic strontium phosphate barium of load 10%Ag.
Comparative example 1
0.015mol barium nitrates and 0.015mol strontium nitrates are dissolved in 40 milliliters of deionized water, add 0.06 gram
The ferriferrous oxide nanometer material of preparation is stirred well to evenly dispersed, as solution 1, and 20 millis are added in 0.01mol sodium phosphates
It dissolves, as solution 2, solution 2 is slowly dropped into solution 1, and the mixed solution is placed in 40 DEG C of water in the deionized water risen
It in bath, is sufficiently stirred 30 minutes, which is poured into 100 milliliters of pyroreaction kettles, reacted 12 hours at 180 DEG C,
It is cooled to room temperature, is cleaned 3-5 times with deionized water, then vacuum drying 4 hours at 3 times, 60 DEG C are cleaned with ethyl alcohol, obtain pale pink
Magnetic strontium phosphate barium composite nano materials.
Performance detection：
The removal effect of 1- Escherichia coli
Such as Fig. 1, prepares 1 liter and contain about 5 × 108The Escherichia coli aqueous solution of CFU/mL, respectively by the magnetism of 2 grams of comparative examples 1
Strontium phosphate barium composite nano materials, the composite magnetic strontium phosphate of loaded Ag of embodiment 1, embodiment 2 loaded Ag compound magnetic
Property barium phosphate and the composite magnetic strontium phosphate barium of Ag that loads of embodiment 3 be added to 5 × 108The Escherichia coli aqueous solution of CFU/mL
In, it stirs ten minutes, obtains as shown in Figure 1 to the sterilizing rate of Escherichia coli.The result shows that being containing 1% silver in composite material
It is remarkably improved bactericidal properties.
The Escherichia coli removal effect of 2- difference salinity
Such as Fig. 2, prepares 1 liter and contain about 5 × 108CFU/ milliliters of Escherichia coli aqueous solution, puts into different amounts of sodium chloride
(NaCl) so that in solution salinity (NaCl concentration) be respectively 1,10,20,50,100mg/L, by the loaded Ag of 2 grams of embodiments 2
Composite magnetic barium phosphate be added to 5 × 108In the Escherichia coli aqueous solution of CFU/mL, stirs ten minutes, obtain to large intestine bar
The sterilizing rate of bacterium is as shown in Figure 2.The result shows that material is higher than 90% when concentration is less than 20mg/L to the sterilizing rate of Escherichia coli,
To also can reach 82% sterilizing rate in the presence of 100mg/L NaCl.Illustrate that material can effectively remove in highrank fuel salinity water solution
Escherichia coli.
3- heavy metals from and removal effect while organic pollution
Such as Fig. 3, the malachite green mixed solution of 1 liter of lead ion and 500mg/L containing about 500mg/L is prepared, pH is adjusted to 5,
By the magnetic strontium phosphate barium composite nano materials of 4 grams of comparative examples 1, the loaded Ag of embodiment 1 composite magnetic barium phosphate it is compound
Magnetic strontium phosphate, embodiment 2 loaded Ag composite magnetic barium phosphate and embodiment 3 loaded Ag composite magnetic strontium phosphate barium
Composite material is added in mixed solution, is stirred 30 minutes, as shown in Figure 3 to the removal rate of lead ion and malachite green.Knot
Fruit shows that the removal rate to lead ion and malachite green can be improved in the silver in composite material, because silver nano-grain surface carries
Negative electrical charge so that entire composite material surface is negatively charged, is conducive to adsorb positively charged metal ion and the dye of positive ion.
4- handles heavy metal ion, organic pollution and the effect data of Escherichia coli simultaneously
Such as Fig. 4,1 liter is prepared respectively and contains about 5 × 108The Escherichia coli liquid of CFU/mL, the lead ion aqueous solution of 100mg/L
The malachite green aqueous solution of (pH is adjusted to 5), 100mg/L, then prepare 1 liter and contain about 5 × 108The Escherichia coli liquid of CFU/mL,
The mixed aqueous solution of the lead ion of 100mg/L, the malachite green of 100mg/L, pH are adjusted to 5.By the material difference of 2 grams of comparative examples 1
It is added in aforementioned four beaker, stirs 30 minutes, obtain to the removal rate of three kinds of pollutants purified respectively and to three kinds
The purifying rate of mixed pollutants solution is as shown in Figure 4.Separately change the material of above-mentioned comparative example 1 into 2 grams of embodiments 1 and embodiment
2 material repeats above-mentioned experiment, the results showed that the clean-up effect of mixed liquor when two kinds of composite materials pair, three kinds of pollutants coexist
Only than slightly being reduced when individually purification, because one timing of adsorption site of material surface, different pollutants exist in material surface
Competitive Adsorption relationship.The silver content in composite material is improved the difference purifying rate to three kinds of pollutants can be improved and mix purification
Rate, therefore compound silver nanometer particle can effectively improve clean-up effect of the material to different pollutants in water.
Claims (10)
1. a kind of multifunction magnetic water purification agent, it is characterised in that：The material is prepared via a method which to obtain：
The first step disperses magnetic phosphate nano or Micron-nano composites in a solvent, AgNO to be added later3It is water-soluble
Liquid, ultrasound obtain mixed liquor to being uniformly dispersed；
Second step is rapidly added the aqueous solution of reducing agent under the action of stirring or ultrasound in the mixed liquor of the first step, continues
Stirring 15~40 minutes, stand 1~5 hour, after after separation and washing dry to get loaded Ag composite magnetic phosphoric acid
Salt.
2. multifunction magnetic water purification agent according to claim 1, it is characterised in that：Solvent described in the first step is water, first
Alcohol or ethyl alcohol；It is preferred that the solvent described in the first step is water；The magnetic phosphate nano or Micron-nano composites with
The mass ratio of solvent is 1~20：100.
3. multifunction magnetic water purification agent according to claim 1, it is characterised in that：The magnetic phosphate nano or
The preparation method of Micron-nano composites includes the following steps：
(1) soluble ferric iron salt is dissolved in common organic alcohols solvent, sodium acetate, surfactant and the poly- second of solid two is added
Alcohol is fitted into reaction kettle, is reacted 1~48 hour at 85~300 DEG C, and the product after reaction is by centrifugation, filtering or magnetism
Separation, washing, drying to obtain ferriferrous oxide nanometer material；
(2) soluble metallic salt is dissolved in the water, ferriferrous oxide nanometer material, surfactant is added, be uniformly mixed
To solution；
(3) soluble-salt of phosphorous acid group is dissolved in the water, obtains the soluble-salt aqueous solution of phosphorous acid group, to step (2)
It is gradually added dropwise in obtained solution, until the two is thoroughly mixed, is reloaded into reaction kettle, it is small that 1~48 is reacted at 85~300 DEG C
When, the product after reaction is by centrifuging, filtering either Magnetic Isolation, washing, drying to obtain magnetism phosphate nano or micro-
Nanocomposite.
4. multifunction magnetic water purification agent according to claim 1, it is characterised in that：Reducing agent described in second step is
NaBH4, sodium sulfite, azanol NH2OH, hydrazine N2H4, glycine, glucose or ascorbic acid；It is preferred that NaBH4：
The reducing agent and AgNO3Molar ratio be 0.01-100：1.
5. multifunction magnetic water purification agent according to claim 1, it is characterised in that：In the composite magnetic phosphate of loaded Ag
The load capacity of Ag is 1~15%.
6. a kind of preparation method of multifunction magnetic water purification agent, it is characterised in that：This approach includes the following steps：
The first step disperses magnetic phosphate nano or Micron-nano composites in a solvent, AgNO to be added later3It is water-soluble
Liquid is uniformly dispersed, and obtains mixed liquor；
Second step is rapidly added the aqueous solution of reducing agent under the action of stirring or ultrasound in the mixed liquor of the first step, continues
Stirring 15~40 minutes, stand 1~5 hour, after after separation and washing dry to get loaded Ag composite magnetic phosphoric acid
Salt.
7. the preparation method of multifunction magnetic water purification agent according to claim 6, it is characterised in that：It is molten described in the first step
Agent is water, methanol or ethyl alcohol；It is preferred that the solvent described in the first step is water；The magnetic phosphate nano or micro-nano multiple
The mass ratio of condensation material and solvent is 1~20：100.
8. the preparation method of multifunction magnetic water purification agent according to claim 6, it is characterised in that：Going back described in second step
Former agent is NaBH4, sodium sulfite, azanol NH2OH, hydrazine N2H4, glycine, glucose or ascorbic acid；It is preferred that NaBH4：
The reducing agent and AgNO3Molar ratio be 0.01-100：1.
9. multifunction magnetic water purification agent described in claim 1 in removing solution heavy metal ion and/or organic pollution and/
Or the application of absorption Escherichia coli.
10. the application described in claim 9, the heavy metal ion is lead ion；The organic pollution is Congo red, hole
One or more of sparrow malachite green, methyl blue, acid fuchsin.
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Cited By (1)
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| US20210387875A1 (en) * | 2020-06-12 | 2021-12-16 | University Of Florida Research Foundation, Inc. | Methods of separating ultrafine pollutant particles from aqueous suspension |
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|---|---|---|---|---|
| CN106946310A (en) * | 2017-05-17 | 2017-07-14 | 南京农业大学 | Magnetic Nano material adsorbs the application of Escherichia coli in the solution |
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2018
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| CN106946310A (en) * | 2017-05-17 | 2017-07-14 | 南京农业大学 | Magnetic Nano material adsorbs the application of Escherichia coli in the solution |
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| SARIKA SINGH, D. BAHADUR: "Catalytic and antibacterial activity of Ag decorated magnetic core shell nanosphere", 《COLLOIDS AND SURFACES B: BIOINTERFACES》 * |
| 何晓文等编著: "《水体污染处理新技术》", 31 March 2013, 中国科学技术大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210387875A1 (en) * | 2020-06-12 | 2021-12-16 | University Of Florida Research Foundation, Inc. | Methods of separating ultrafine pollutant particles from aqueous suspension |
| US11866353B2 (en) * | 2020-06-12 | 2024-01-09 | University Of Florida Research Foundation, Inc. | Methods of separating ultrafine pollutant particles from aqueous suspension |
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