CN107715848B - A kind of modified Nano material and its application in stibium-containing wastewater processing - Google Patents
A kind of modified Nano material and its application in stibium-containing wastewater processing Download PDFInfo
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- CN107715848B CN107715848B CN201711128281.9A CN201711128281A CN107715848B CN 107715848 B CN107715848 B CN 107715848B CN 201711128281 A CN201711128281 A CN 201711128281A CN 107715848 B CN107715848 B CN 107715848B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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Abstract
The processing method of stibium-containing wastewater of the present invention, and in particular to a kind of modified Nano material, preparation process, which is included in titania nanotube suspension, is added humic acid.Stibium-containing wastewater is handled the present invention also provides the titania nanotube using humic acid modification.The present invention modifies humic acid to titania nanotube surface, for adsorbing Sb in water environment3+Or Sb5+, antimony removal efficiency is significantly improved, removal cost is reduced, and the material non-toxic used is harmless, environmental-friendly.
Description
Technical field
A kind of processing method of stibium-containing wastewater of the present invention, and in particular to modified Nano material and its in stibium-containing wastewater processing
Application.
Background technology
Antimony has certain carcinogenicity, the presence of antimony in water environment, greatly threatens the safety of aquatile and the mankind, and mesh
The removal effect of antimony is undesirable in preceding water environment, it is difficult to efficiently simultaneously remove Sb3+And Sb5+It is set to meet the water standard of antimony
It is required that being used simultaneously for engineering has good application prospect.
Currently, being mainly the following method for the processing of antimony in water environment both at home and abroad：The precipitation method, absorption method, adjusting
PH value, Coagulation Method, electrochemical method.Wherein the precipitation method, Coagulation Method need that a large amount of precipitations are added during carrying out water process
Agent will produce antimony waste residue in reaction process, and reaction is made to generate secondary pollution, further need exist for by quinquevalence antimony be reduced into trivalent antimony it
It is just obvious to post-process effect；And use to adjust and antimony and be not thorough in pH, electrochemical method removal aqueous solution, in solution there are
Micro residue；Therefore at present more generally using absorption method, but due to the difference of adsorbing medium, going for antimony in water body is caused
Except amount difference is bigger.It is shown according to data of literatures, the active charcoal of common antimony adsorbent, silica gel, montmorillonite, red iron
Mine, rice husk ash, chitosan and cellulosic polymer etc..Inorganic mineral adsorbent, activated carbon, organic can be substantially divided by type
Adsorbent three categories, and these types of adsorbent is all there is certain limitation, mainly adsorption capacity are relatively low, hot environment
Under, pollutant can be parsed from adsorbent surface, cause secondary pollution, adsorbent requirement larger, cost is increased.
Chinese patent application 201611120116.4 discloses a kind of preparation method of heavy metal-polluted water treatment agent, uses
Miniflow Wan technologies in conjunction with emulsification and cross-linking reaction, and add nano-titanium dioxide and γ-ferric oxide, micro- after crosslinking curing
Ball is filtered with petroleum ether, and deionized water is used in combination to clean repeatedly, then bagasse cellulose xanthan vinegar microsphere adsorbing agent is made in drying.
The inorganic agent of this application has stronger suction-operated to the heavy metal ion in heavy metal-containing polluted water, while going back decomposable asymmetric choice net sewage
In organic matter, however the inorganic agent is difficult to realize recycle, and its preparation process is complex, in preparation process also
The organic matters such as glutaraldehyde, toluene are used, harm is brought to environment.
In recent years, the application that nano material is removed in water environment pollution object receives the concern of people, and nano material has
The high specific surface area of nano material and remarkable absorption property, become the ideal adsorbent of water treatment field.Numerous
In metal nano oxide, nano-TiO2It is high-efficiency activated with extraordinary chemical stability and nontoxic, of low cost.
However, traditional nano-TiO2Isoelectric point between pH 4.5-6.5, isoelectric point is relatively low, thus its adsorption capacity is weaker, because
And reduce its treatment effeciency to pollutant.
Invention content
In order to overcome problems of the prior art, it is an object of the present invention to provide one kind at stibium-containing wastewater
The titania nanotube of the humic acid modification of reason.
It is a further object to provide a kind of method for treating water for removing antimony.
The technical scheme is that：A kind of titania nanotube of humic acid modification for stibium-containing wastewater processing,
It is characterized in that, its preparation process, which is included in titania nanotube suspension, is added humic acid.
Titania nanotube surface, titania nanotube surface are arrived in humic acid fully modification under electrostatic attraction effect
The negatively charged density of institute increases, and forms the functional groups such as more more aromatic groups.
Further, the addition of the humic acid is more than maximal absorptive capacity of the titania nanotube for humic acid.
Further, the titania nanotube is q for the theoretical maximum adsorbance of humic acidm=56mg/g.
Further, the caliber of prepared titania nanotube is 12-15nm, internal diameter 11-12nm.
Further, the titania nanotube preparation process of the humic acid modification includes the following steps：
(1) it takes titania nanotube to be added in deionized water, so that it is formed stabilization in the solution by supersound process
Titania nanotube suspension；
(2) humic acid is added in the titania nanotube suspension, is put into shaking table processing, obtain humic acid modification
Titania nanotube.
Further, the obtained titania nanotube suspension of step (1), pH value control are 6.5-7.8.
Further, the temperature of the shaking table is 20-25 degrees Celsius, rotating speed 150-200r/min, using the place of shaking table
The reason time is 1-3h.
Further, the titania nanotube is obtained by concentrated base hydro-thermal legal system.
Further, the preparation method of the titania nanotube includes the following steps：Take titanium dioxide granule point
It is dispersed in NaOH solution, is dispersed with stirring, be transferred in the autoclave of polytetrafluoroethylene (PTFE), heating reaction；Obtained white production
Object is washed with deionized to neutrality, impregnates the sodium ion in removal lattice with hydrochloric acid solution, is cleaned to neutrality with deionized water,
Drying, obtains titania nanotube.
Further, a diameter of 40-50nm of the titanium dioxide nanoparticle, surface area 12-16m2/g。
Further, the heating reaction is 120-140 DEG C of heating 24-28h.
Further, prepared titania nanotube is q for the theoretical maximum adsorbance of humic acidm=56mg/
g。
The present invention passes through the reaction condition of control titania nanotube preparation process, obtained titania nanotube
Specific surface area with bigger and meso-hole structure, the electrically charged amount bigger of unit area institute, adsorption capacity are stronger.
Further, the isoelectric point of the titania nanotube is between pH6~7.
A kind of method for treating water for removing antimony, this method includes the titanium dioxide for making water Yu being modified with above-mentioned humic acid
Nanotube is in contact.
Further, the antimony in the stibium-containing wastewater is Sb3+And/or Sb5+。
Further, the method further includes：Sb is adsorbed3+And/or Sb5+Humic acid modification nano titania
The elution process of pipe.Realize the recycling of the titania nanotube of humic acid modification.
The elution process is：Sb will have been adsorbed3+And/or Sb5+Humic acid modification titania nanotube carry out from
Heart processing, centrifugation obtained solid are eluted using ethyl alcohol, and removal is adsorbed on the titania nanotube of humic acid modification
Antimony.
Sb is adsorbed3+And/or Sb5+Humic acid modification titania nanotube, since its surface charge is neutralized,
It more easily settles, is separated by solid-liquid separation by centrifugation in the solution, through ethanol elution, the rate of recovery can reach 90% or more, realize
The purpose of the titania nanotube recycling of humic acid modification.
Further, the one kind or more for the humic acid that the humic acid extracts in soil, water body, aerosol and frond
Kind.
Absorption between titania nanotube surface and humic acid is mainly handed over by hydrophobic effect, electrostatic interaction and ligand
The effect of changing codetermines.The isoelectric point of traditional titanium dioxide nanoparticle is between pH4~5, and prepared by the present invention
The isoelectric point of titania nanotube is between pH6~7, than the isoelectric point higher of Conventional nano titanium dioxide granule, table
Face is carried compared with multi-charge, under the conditions of neutral aqueous solution, can adsorb a large amount of humic acid.In addition to this, titania nanotube table
Face is with functional groups such as more hydroxyls, carboxyls so that humic acid is more easy to be adsorbed in nano-material surface, compared to nano-silica
Change titanium particle, the surface modification efficiency of titania nanotube is obviously improved, and reduces the cost of surface modification, is a kind of
Environmentally friendly, economical sorbing material.
Due to titania nanotube, its isoelectric point is different compared with ordinary titanium dioxide nano material, in aqueous solution property
Under the conditions of, titania nanotube surface, that is, positively charged, negatively charged humic acid can preferably modify titanium dioxide
Nanotube surface, and then make the titania nanotube after modification that there is preferably suspension, dispersion effect in water environment, simultaneously
The humic acid to surface is modified rich in more polyfunctional group, makes Sb3+Or Sb5+Adsorbance significantly increase, removal rate substantially increases in turn
Add；
The nanometer titanic oxide material of unadsorbed humic acid is only capable of removing the Sb in water body by electrostatic adsorption3+With
Sb5+, and the titania nanotube of surface modification humic acid, the functional group containing there are many, electrostatic attraction and hydrophobic work can be passed through
With the Sb in synergistic sorption aqueous solution3+And Sb5+, make it for Sb3+And Sb5+Removal efficiency be substantially improved, adsorbance is notable
Increase.Conventional nano titanic oxide material only has 60%-75% for the removal rate of antimony, and theoretical maximum adsorbance is qm=6-
22mg/g, and the titania nanotube of the humic acid modification of the present invention can reach 100% for the removal rate of antimony, for Sb3+
And Sb5+Theoretical maximum adsorbance is respectively qm=145mg/g, qm=113mg/g.
Traditional sorbing material, the suspension, settling property in water environment are unstable, need to be stirred in adsorption process
Increase suspension, generally require the supplementary means such as centrifugal filtration in separation of solid and liquid process, the consuming time is longer, and institute of the present invention
The titania nanotube of the humic acid modification of use, since surface charge is neutralized by humic acid, without using nondominant hands such as stirrings
Section can well suspended dispersed in aqueous solution, Sb3+Or Sb5+It is fully connect with the titania nanotube of humic acid modification
It touches, convenient for the Sb in adsorption aqueous solution3+Or Sb5+, adsorption equilibrium can be reached faster, to remove the antimony in water body faster.
Adsorb Sb3+Or Sb5+After reaching balance, due to the reduction of electrostatic repulsion between particle, can rapid subsidence, reach
The purpose of quick separating from solution.Both adsorption efficiency is increased, while reducing the cost and energy consumption of separation of solid and liquid.
The present invention modifies humic acid to titania nanotube surface, for adsorbing Sb in water environment3+Or Sb5+, significantly
Antimony removal efficiency is improved, removal cost is reduced, and the material non-toxic used is harmless, environmental-friendly.
Description of the drawings
The titania nanotube of Fig. 1 humic acid modifications of the present invention removes Sb in water removal3+And/or Sb5+Process.
Specific implementation mode
Embodiment 1
A kind of titania nanotube of humic acid modification for stibium-containing wastewater processing, preparation method includes following step
Suddenly：
(1) it is 12-15nm to take caliber, and 50ml deionized waters are added in the titania nanotube 20mg that internal diameter is 11-12nm
In, so that it is formed stable titania nanotube in the solution by supersound process and suspend, and is 6.8- by pH value control
7.2。
(2) humic acid is added in titania nanotube suspension, a concentration of 50ppm of humic acid is put at shaking table
2h is managed, the temperature of shaking table is 20 degrees Celsius, rotating speed 150r/min, obtains the titania nanotube of humic acid modification.Humic
Fully titania nanotube surface is arrived in modification to acid under electrostatic attraction effect, and titania nanotube surface institute is negatively charged close
Degree increases, and forms the functional groups such as more more aromatic groups.
Wherein, the humic acid that humic acid extracts in soil, water body, aerosol and frond it is one or more.
The preparation method of titania nanotube includes the following steps：Take a diameter of 40-50nm, surface area 12-16m2/
The titanium dioxide granule of g is dispersed in NaOH solution, is dispersed with stirring, and is transferred in the autoclave of polytetrafluoroethylene (PTFE), 130 DEG C
Heating is for 24 hours；Obtained white product is washed with deionized to neutrality, impregnates the sodium ion in removal lattice with hydrochloric acid solution,
It is cleaned to neutrality with deionized water, drying obtains titania nanotube.
Adsorbance of the present embodiment humic acid on titania nanotube is 38.6mg/g (humic acid/titanium dioxide).
The isoelectric point of the present embodiment titania nanotube is between pH6~7.Sb is adsorbed3+And/or Sb5+Humic
The titania nanotube of acid modification, since its surface charge is neutralized, it is easier to settle, be consolidated by centrifugation in the solution
Liquid detaches, and through ethanol elution, the rate of recovery reaches 95%, realizes the titania nanotube recycling of humic acid modification
Purpose.
Embodiment 2
The method that the titania nanotube for the humic acid modification prepared using embodiment 1 removes antimony in water, including such as
Lower step：
(1) titania nanotube that 20mg humic acid is modified is added to 50ml 30ppm Sb3+Or Sb5+Solution
In, adsorb 60min；
(2) elution process of the titania nanotube of the humic acid modification of antimony has been adsorbed：The humic acid of antimony will have been adsorbed
The titania nanotube of modification carries out centrifugal treating, and centrifugation obtained solid is eluted using ethyl alcohol, and removal is adsorbed on humic
Antimony on the titania nanotube of acid modification.
The adsorbance to antimony of the titania nanotube of the present embodiment humic acid modification is 75.4mg/g, the removal rate of antimony
It can reach 100%.
Embodiment 3
A kind of titania nanotube of humic acid modification for stibium-containing wastewater processing, preparation method includes following step
Suddenly：(1) it is 12-15nm to take caliber, and the titania nanotube 20mg that internal diameter is 11-12nm is added in 50ml deionized waters, warp
Crossing to be ultrasonically treated makes it form stable titania nanotube suspension in the solution, and is 6.5-7.8 by pH value control.
(2) humic acid is added in titania nanotube suspension, a concentration of 55ppm of humic acid is put at shaking table
1h is managed, the temperature of shaking table is 25 degrees Celsius, rotating speed 200r/min, obtains the titania nanotube of humic acid modification.Humic
Fully titania nanotube surface is arrived in modification to acid under electrostatic attraction effect, and titania nanotube surface institute is negatively charged close
Degree increases, and forms the functional groups such as more more aromatic groups.
Wherein, the humic acid that humic acid extracts in soil, water body, aerosol and frond it is one or more.
The preparation method of titania nanotube includes the following steps：Take a diameter of 40-50nm, surface area 12-16m2/
The titanium dioxide granule of g is dispersed in NaOH solution, is dispersed with stirring, and is transferred in the autoclave of polytetrafluoroethylene (PTFE), 120 DEG C
Heat 26h；Obtained white product is washed with deionized to neutrality, impregnates the sodium ion in removal lattice with hydrochloric acid solution,
It is cleaned to neutrality with deionized water, drying obtains titania nanotube.
The present embodiment humic acid maximal absorptive capacity on titania nanotube is 31.2mg/g (humic acid/titanium dioxide
Titanium).
The isoelectric point of the present embodiment titania nanotube is between pH6~7.Sb is adsorbed3+And/or Sb5+Humic
The titania nanotube of acid modification, since its surface charge is neutralized, it is easier to settle, be consolidated by centrifugation in the solution
Liquid detaches, and through ethanol elution, the rate of recovery reaches 94%, realizes the titania nanotube recycling of humic acid modification
Purpose.
Embodiment 4
The method that the titania nanotube for the humic acid modification prepared using embodiment 3 removes antimony in water, including such as
Lower step：
(1) titania nanotube that 20mg humic acid is modified is added to 50ml 25ppm Sb3+Or Sb5+Solution
In, adsorb 75min；
(2) elution process of the titania nanotube of the humic acid modification of antimony has been adsorbed：The humic acid of antimony will have been adsorbed
The titania nanotube of modification carries out centrifugal treating, and centrifugation obtained solid is eluted using ethyl alcohol, and removal is adsorbed on humic
Antimony on the titania nanotube of acid modification.
The adsorbance to antimony of the titania nanotube of the present embodiment humic acid modification is 68.5mg/g, the removal rate of antimony
It can reach 100%.
Embodiment 5
A kind of titania nanotube of humic acid modification for stibium-containing wastewater processing, preparation method includes following step
Suddenly：(1) it is 12-15nm to take caliber, and the titania nanotube 20mg that internal diameter is 11-12nm is added in 50ml deionized waters, warp
Crossing to be ultrasonically treated makes it form stable titania nanotube suspension in the solution, and is 6.5-7.5 by pH value control.
(2) humic acid is added in titania nanotube suspension, a concentration of 50ppm of humic acid is put at shaking table
3h is managed, the temperature of shaking table is 20 degrees Celsius, rotating speed 175r/min, obtains the titania nanotube of humic acid modification.Humic
Fully titania nanotube surface is arrived in modification to acid under electrostatic attraction effect, and titania nanotube surface institute is negatively charged close
Degree increases, and forms the functional groups such as more more aromatic groups.
Wherein, the humic acid that humic acid extracts in soil, water body, aerosol and frond it is one or more.
The preparation method of titania nanotube includes the following steps：Take a diameter of 40-50nm, surface area 12-16m2/
The titanium dioxide granule of g is dispersed in NaOH solution, is dispersed with stirring, and is transferred in the autoclave of polytetrafluoroethylene (PTFE), 140 DEG C
Heat 28h；Obtained white product is washed with deionized to neutrality, impregnates the sodium ion in removal lattice with hydrochloric acid solution,
It is cleaned to neutrality with deionized water, drying obtains titania nanotube.
Adsorbance of the present embodiment humic acid on titania nanotube is 41.6mg/g (humic acid/titanium dioxide
Titanium).
The isoelectric point of the present embodiment titania nanotube is between pH6~7.Sb is adsorbed3+And/or Sb5+Humic
The titania nanotube of acid modification, since its surface charge is neutralized, it is easier to settle, be consolidated by centrifugation in the solution
Liquid detaches, and through ethanol elution, the rate of recovery reaches 91%, realizes the titania nanotube recycling of humic acid modification
Purpose.
Embodiment 6
The method that the titania nanotube for the humic acid modification prepared using embodiment 5 removes antimony in water, including such as
Lower step：
(1) titania nanotube that 20mg humic acid is modified is added to 50ml 35ppm Sb3+Or Sb5+Solution
In, adsorb 45min；
(2) elution process of the titania nanotube of the humic acid modification of antimony has been adsorbed：The humic acid of antimony will have been adsorbed
The titania nanotube of modification carries out centrifugal treating, and centrifugation obtained solid is eluted using ethyl alcohol, and removal is adsorbed on humic
Antimony on the titania nanotube of acid modification.
The adsorbance to antimony of the titania nanotube of the present embodiment humic acid modification is 72.1mg/g, the removal rate of antimony
It can reach 100%.
Above-mentioned detailed description is illustrating for one of them possible embodiments of the present invention, the embodiment not to
The scope of the claims of the present invention is limited, all equivalence enforcements or change without departing from carried out by the present invention are intended to be limited solely by the technology of the present invention
In the range of scheme.
Claims (10)
1. a kind of titania nanotube of humic acid modification for stibium-containing wastewater processing, which is characterized in that its preparation process
It is included in titania nanotube suspension and humic acid is added.
2. the titania nanotube of humic acid modification according to claim 1, which is characterized in that the humic acid adds
Enter maximal absorptive capacity of the amount more than titania nanotube for humic acid.
3. the titania nanotube of humic acid modification according to claim 1, which is characterized in that the titanium dioxide
The caliber of nanotube is 12-15nm, internal diameter 11-12nm.
4. the titania nanotube of humic acid modification according to claim 1, which is characterized in that the preparation process packet
Include following steps：
（1）It takes titania nanotube to be added in deionized water, so that it is formed stable dioxy in the solution by supersound process
Change titanium nanotube suspension；
（2）Humic acid is added in the titania nanotube suspension, shaking table processing is put into, obtains the dioxy of humic acid modification
Change titanium nanotube.
5. the titania nanotube of humic acid modification according to claim 4, which is characterized in that step（1）It is acquired
Titania nanotube suspension, pH value control be 6.5-7.8.
6. the titania nanotube of humic acid modification according to claim 4, which is characterized in that the temperature of the shaking table
It it is 20-25 degrees Celsius, rotating speed 150-200r/min uses the processing time of shaking table for 1-3h.
7. a kind of method for treating water for removing antimony, which is characterized in that this method includes making water and using the claims 1-6
The titania nanotube for the humic acid modification that middle any claim is prepared is in contact.
8. the method according to the description of claim 7 is characterized in that the antimony in the stibium-containing wastewater is Sb3+And/or Sb5+。
9. according to the method described in claim 8, it is characterized in that, the method further includes：The dioxy of the humic acid modification
Change titanium nanotube and adsorbs Sb3+And/or Sb5+Elution process afterwards.
10. according to the method described in claim 9, it is characterized in that, the elution process is：The dioxy of the humic acid modification
Change titanium nanotube and adsorbs Sb3+And/or Sb5+Afterwards, centrifugal treating is carried out, centrifugation obtained solid is eluted using ethyl alcohol, and removal is inhaled
The antimony being attached on the titania nanotube of humic acid modification.
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| CN109019748A (en) * | 2018-09-10 | 2018-12-18 | 芜湖新达园林绿化集团有限公司 | The preparation and application of a kind of flocculation adsorption complex microsphere and flocculation adsorption agent |
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