CN107262044A - It is a kind of to Congo red magnetic coupling functional material with efficient clearance and preparation method thereof in water - Google Patents
It is a kind of to Congo red magnetic coupling functional material with efficient clearance and preparation method thereof in water Download PDFInfo
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
There is provided a kind of absorption and flocculation of having concurrently to Congo red magnetic coupling functional material with efficient clearance and preparation method thereof in water, belong to dye wastewater treatment technology field.The magnetic coupling functional material is by sepiolite, ferroso-ferric oxide and cetyl trimethylammonium bromide（CTAB）Tri compound is formed.Its preparation method is as follows：The mixed solution progress magnetic modification that divalence and ferric ion are added after sepiolite progress heat modification will be purified, add cetyl trimethylammonium bromide（CTAB）Solution carries out organically-modified, obtained organically-modified magnetic meerschaum, the i.e. signified magnetic coupling functional material of the present invention.The preparation method that the present invention is provided is with low cost, simple and easy to apply, workable.The magnetic coupling function material is applied to the processing of Congo red simulated wastewater, its concentration range is 100 4500mg/L, with optimal conditions, to the Congo red maximum capacity that removes up to 4478.92mg/g, clearance is 96.49% 99.92%.
Description
Technical field
The present invention relates to a kind of to Congo red magnetic coupling functional material and its preparation side with efficient clearance in water
Method, and in particular to a kind of to the Congo red organically-modified magnetic meerschaum composite functional material with efficient clearance in water, be
A kind of novel magnetic composite functional material for having absorption and flocculation concurrently, belongs to dye wastewater treatment technology field.
Background technology
Organic matter used and the intermediate produced are various in printing and dyeing industry production, and waste water from dyestuff organic principle is complicated, poison
Evil property is big, and difficulty is biodegradable, and effect is caused with three；Other colourity is high and is influenceed color-variable by pH value；Due to its chemistry knot
Structure is complicated and aromatic rings isomeric forms are various so that many dyestuffs have toxicity and biological non-biodegradable, are directly discharged to
Serious influence can be caused in environment.Congo red is a kind of anionic dye of typical diphenyl amine azo direct, in production
Easily enter factory's surrounding body with using spent process water, there is destruction to ecological environment.Congo red waste water also has
Change of water quality is big, colourity and the features such as COD high, is one of typical waste water from dyestuff.
Common dye waste water treatment method has Fenton oxidation method, absorption method, catalytic oxidation, Ozonation and life
Thing method.Different processing methods is different to the treatment effect of waste water from dyestuff, but still lacks energy efficient process high concentration dyestuff at present
The practical technique of waste water.And absorption method due to processing more thoroughly, the reaction time is shorter, nonhazardous material generation, be ideal
Wastewater decoloring method.At present, adsorption bleaching technology is to remove dye molecule by the suction-operated of adsorbent.Adsorbent
Including regenerable sorbent such as activated carbon, sepiolite, ion-exchange fibre etc. and for example various natural minerals of non-renewable adsorbent
（Bentonite, diatomite）, industrial waste（Iron filings, cinder, flyash）And natural wastes（Charcoal, sawdust）Deng.
Sepiolite is a kind of magnesium silicate clay mineral of aqueous fibre shape, and its standard chemical formula is Mg8Si12O30(OH)4
(OH2)4·8H2O.Its construction unit is made up of two layers of silicon-oxy tetrahedron and middle one layer of magnesia octahedron, and tetrahedral top layer is
Continuously, therefore every 6 silicon-oxy tetrahedron drift angles on the contrary, form 2：1 layered structure unit, levels are spaced to put down with key
Capable duct.Because this special structure makes sepiolite have very big specific surface area and very strong adsorption capacity, and because of sea
The special construction of afrodite makes it have preferable adsorptivity, rheological characteristic and catalytic.
Now, sepiolite is mainly for the treatment of heavy metal, organic wastewater, due to the hydrophily and interlayer on sepiolite surface
A large amount of exchangeable cations hydrolysis, adsorption capacity is poor when it is used to handle Organic Pollutants in Wastewater.Asked to solve this
Topic, common improved method is organically-modified sepiolite, sepiolite surface is become lipophile by hydrophily, while increasing newly
Organo-functional group, improves the absorption property of sepiolite.Conventional organic modifiers have：Surfactant, silane coupler, pyridine
Class, organic acid etc..
At present, mainly there are biological treatment, absorption, flocculation and photocatalysis etc. to Congo red minimizing technology, and wherein, inhale
Attached is the main methods used at present.Such as Qiao Nan（A kind of processing method Tohoku Electric Powers of congo red waste water are big
Learn .2013）The Congo red of 20-40mg/L is have studied to be dissolved in the restricted culture medium of 1L white rot bacteria liquids, using 120h as a circulation,
It is repeated 5 times, 75.1%-95.2% is remained to the clearance of Dye Wastewater Decolorization；Chen Yi is loyal（It is Congo red in a kind of processing printing and dyeing
Method Changzhou University .2014）It has studied having by modifying agent of sodium pyrophosphate, sodium polyphosphate and neopelex
Congo red concentration range is in 200-300mg/L in machine modified alta-mud, raw wastewater, to its clearance up to more than 98%；Dong Yanmin
（Congo red decolorising agent Changzhou University .2015 in one kind processing textile printing and dyeing wastewater）Have studied with butyl titanate, aluminium chloride,
Activated carbon etc. be raw material, prepare Congo red Photocatalytic Decoloration agent, to concentration range 1000-1800mg/L Congo red printing and dyeing
After waste water, stirring 1-3h, to Congo red clearance up to more than 99.5%.It can be seen that, existing biological, absorption and photocatalysis technology are remote
Being not reaching to the actual production waste water to high concentration range has very strong disposal ability.
The invention provides a kind of to Congo red magnetic coupling functional material and its preparation with efficient clearance in water
Method, washing purifying and thermally-denatured pretreatment, then composite ferroferric oxide and hexadecane successively are carried out by sepiolite original soil
Base trimethylammonium bromide（CTAB）, under conditions of pH=7, compared to single composite ferroferric oxide or cetyl trimethyl bromine
Change ammonium（CTAB）Material, the clearance of this pair of composite is significantly improved；Further, under conditions of pH=1-3.5,
The clearance of this pair of composite has further bigger lifting again, and now it does not only have suction-operated, more generates flocculation
Effect.And have concurrently absorption and the flocculation that this material has at home and abroad have no report, it has efficiently to Congo red in addition
The advantage of clearance, compared to other prior arts, the material is not only found that new mechanism, also possesses stronger market competition
Power.
The content of the invention
The invention provides a kind of to Congo red magnetic coupling functional material and its preparation with efficient clearance in water
Method, solves the strong acidic condition that biological method is difficult to be applicable Congo red production waste water, such as tune raw wastewater pH value to neutrality is again
Biological method processing then increases handling process complexity and its cost burden；Also solve existing modified adsorbent and be unable to reach height
The problem of effect processing high concentration Congo red actual production waste water.
Realize that the technology used in the present invention solution is：A kind of magnetic coupling functional material provided is by Hai Pao
Stone, ferroso-ferric oxide and cetyl trimethylammonium bromide（CTAB）Composition, wherein ferroso-ferric oxide and CTAB all passes through
Hydro-thermal method is loaded on sepiolite successively, forms three-component compound system.Carry out according to the following steps：
（1）Sepiolite original soil obtains purifying sepiolite through washing drying, takes a certain amount of ground purifying sea for crossing 50-200 mesh sieves
Afrodite is placed in crucible, then is placed in Muffle furnace heat modification sepiolite is obtained after 200-300 DEG C of heat modification 1-4h, cooling；
（2）Weigh 8-15g heat modifications sepiolite and be added in 150mL conical flask, using FeCl3·6H2O prepares 250mL
Concentration is 0.05-0.2mol/L Fe3+Solution, using FeSO4·7H2O prepares the Fe that 250mL concentration is 0.025-0.1mol/L2 +Solution, and by prepared Fe3+And Fe2+Solution respectively takes 50mL, and the mixed solution of common 100mL iron is added to above-mentioned conical flask in the lump
In, it is placed in after vibration 1-2h in thermostatic control oscillator vibration be heated to 50-80 DEG C at room temperature, then by the way that 1mol/L NaOH is added dropwise
Solution adjusts the pH value of mixed solution in bottle to 8-11, then is placed in 50-80 DEG C of thermostatic control oscillator vibration and vibrates 1-2h, so
The still aging 1-2h at 50-80 DEG C afterwards, after carrying out suction filtration separation after solution cooling, with deionized water by resulting solid material
Material washing is 7 or so to pH, and finally the solid material on filter paper is placed in 80-120 DEG C of drying box and dried, through grinding after cooling
Cross 50-200 mesh sieves and obtain magnetic meerschaum；
（3）Weigh 8-15g magnetic meerschaums and be added in 150mL conical flask, then by 150-300mL initial concentrations be 25-
30mmol/L cetyl trimethylammonium bromide（CTAB）Solution is added in above-mentioned conical flask, by mixed solution in 20-50
DEG C thermostatic control oscillator vibration reaction 18-36h, mixed solution is centrifuged after terminating for question response, using absolute ethyl alcohol
Cyclic washing being carried out to the solid material of gained with the mixed liquor of deionized water, being up to can't detect bromide ion with silver nitrate
Only, then by the solid material of gained 50-80 DEG C of drying in oven is placed in, organic change is obtained through ground 50-200 mesh sieves after cooling
Property magnetic meerschaum.
The advantageous effects of the present invention are：
Present invention also offers a kind of application to the Congo red magnetic coupling functional material with efficient clearance in water, specifically
For：Under identical adsorption conditionses, relatively obtained organically-modified magnetic meerschaum, organic sepiolite, magnetic meerschaum and
Sepiolite original soil is applied to handle Congo red simulated wastewater（The Congo red solution of series of identical initial concentration）Effect.
By the comparison of adsorption effect, organically-modified magnetic meerschaum is to unit adsorbance Congo red in water respectively than having
Organic sepiolite, magnetic meerschaum and sepiolite original soil improve 0.69 times, 8.86 times, 8.08 times.
In addition, the organically-modified magnetic meerschaum prepared by described method is in acid condition（PH value is 1-3.5）Under,
Centering low concentration（100-2000mg/L）Congo red waste water is based on suction-operated, supplemented by flocculation, and to high concentration
（2000-4500mg/L）Congo red waste water is then based on flocculation, supplemented by suction-operated；And be conducive to it in acid condition
To Congo red flocculation, and with the increase of Congo red waste water initial concentration, flocculation is stronger.
Congo red concentration range is 100-4500mg/L in simulated wastewater, is 1-3.5 in pH value（As azo waste water
The pH value range of actual production waste water）Under conditions of, organically-modified magnetic meerschaum is reachable to Congo red maximum removal capacity
4478.92mg/g, clearance is 96.488%-99.923%.
Using sepiolite as matrix, ferroso-ferric oxide and cetyl trimethylammonium bromide（CTAB）Prepared for modifying agent organic
The method of modified magnetic sepiolite, with low cost, simple and easy to apply, workable, preparation process non-secondary pollution, with industry
The application prospect of change.
Brief description of the drawings
Fig. 1 schemes for the SEM and TEM of the magnetic coupling functional material of the embodiment of the present invention 1.
Fig. 2 is applied to compare the adsorption isotherm line chart for the treatment of effect for the magnetic coupling functional material of the embodiment of the present invention 1.
Fig. 3 is applied to the FTIR figures of processing for the magnetic coupling functional material of the embodiment of the present invention 1.
Fig. 4 for the embodiment of the present invention 2 magnetic coupling functional material checking flocculation centrifugation after solution displaying figure.
Fig. 5 verifies the datagram of flocculation for the magnetic coupling functional material of the embodiment of the present invention 2.
Fig. 6 verifies the datagram of flocculation for the magnetic coupling functional material of the embodiment of the present invention 2.
Embodiment
With reference to specific embodiment, the present invention is further illustrated, but these embodiments are not intended to limit the guarantor of the present invention
Protect scope.
Embodiment 1
1. the preparation of magnetic coupling functional material：
（1）Sepiolite original soil obtains purifying sepiolite through washing drying, takes a certain amount of ground purifying sea for crossing 50-200 mesh sieves
Afrodite is placed in crucible, then is placed in Muffle furnace heat modification sepiolite is obtained after 200-300 DEG C of heat modification 1-4h, cooling；
（2）Weigh 8-15g heat modifications sepiolite and be added in 150mL conical flask, using FeCl3·6H2O prepares 250mL
Concentration is 0.05-0.2mol/L Fe3+Solution, using FeSO4·7H2O prepares the Fe that 250mL concentration is 0.025-0.1mol/L2 +Solution, and by prepared Fe3+And Fe2+Solution respectively takes 50mL, and the mixed solution of common 100mL iron is added to above-mentioned conical flask in the lump
In, it is placed in after vibration 1-2h in thermostatic control oscillator vibration be heated to 50-80 DEG C at room temperature, then by the way that 1mol/L NaOH is added dropwise
Solution adjusts the pH value of mixed solution in bottle to 8-11, then is placed in 50-80 DEG C of thermostatic control oscillator vibration and vibrates 1-2h, so
The still aging 1-2h at 50-80 DEG C afterwards, after carrying out suction filtration separation after solution cooling, with deionized water by resulting solid material
Material washing is 7 or so to pH, and finally the solid material on filter paper is placed in 80-120 DEG C of drying box and dried, through grinding after cooling
Cross 50-200 mesh sieves and obtain magnetic meerschaum；
（3）Weigh 8-15g magnetic meerschaums and be added in 150mL conical flask, then by 150-300mL initial concentrations be 25-
30mmol/L cetyl trimethylammonium bromide（CTAB）Solution is added in above-mentioned conical flask, by mixed solution in 20-50
DEG C thermostatic control oscillator vibration reaction 18-36h, mixed solution is centrifuged after terminating for question response, using absolute ethyl alcohol
Cyclic washing being carried out to the solid material of gained with the mixed liquor of deionized water, being up to can't detect bromide ion with silver nitrate
Only, then by the solid material of gained 50-80 DEG C of drying in oven is placed in, organic change is obtained through ground 50-200 mesh sieves after cooling
Property magnetic meerschaum.
Its surface can be observed by scheming a as shown in a in Fig. 1 and b in SEM the and TEM characterization results of magnetic coupling functional material
In fiber migrated first dopant；It can be observed by scheming b, ferroso-ferric oxide and cetyl trimethylammonium bromide（CTAB）From inside to outside according to
It is secondary to be carried on sepiolite surface, form three-component compound system.
2. the application of magnetic coupling functional material is compared：By sepiolite original soil, magnetic meerschaum, organic sepiolite and
Organically-modified magnetic meerschaum is applied to handle Congo red simulated wastewater：To evaluate the quality of each material absorption property, therefore do and inhale
Attached thermoisopleth experiment.In neutral conditions, 100mg/L, 200mg/L, 300mg/L, 400mg/L, 500mg/L are configured successively,
600mg/L, 700mg/L, 800mg/L, 900mg/L, 1000mg/L, 1100mg/L, 1200mg/L, 1300mg/L's is Congo red molten
Liquid, above-mentioned each material, Congo red solution are added in conical flask by 1g/L dosage, in the constant water bath box for being placed in 30 DEG C,
Through adsorb 5.0h it is to be adsorbed it is in a basic balance after, residual concentration is surveyed by ultraviolet-visible spectrophotometer（Dilution suitable multiple makes residue
Concentration is in 0-50mg/L concentration ranges）, then unit adsorbance obtained by standard curve.Finally, it can obtain as shown in Figure 2 comment
The adsorption isotherm line chart of each material absorption property quality of valency.
In addition, its FTIR characterization result sees Fig. 3, analyzed by Fig. 3 and demonstrate organically-modified magnetic meerschaum surface
Ferroso-ferric oxide and Congo red sulfonic acid group between there occurs coordination, so the coordination of magnetic is also its absorption
One of Congo red effect.
Embodiment 2
Magnetic coupling functional material verifies the experiment of flocculation：Demonstrating the material according to mechanism experiment is made with electrostatic attraction
Based on, therefore pH value plays a leading role to treatment effect.
Under conditions of pH=1-3.5,200mg/L, 400mg/L, 600mg/L, 800mg/L, 1000mg/L are configured successively,
1200mg/L, 1400mg/L, 1600mg/L, 2000mg/L, 2500mg/L, 3000mg/L, 3500mg/L, 4000mg/L,
4500mg/L Congo red solution, above-mentioned organically-modified magnetic meerschaum, Congo red solution are added in cone by 1g/L dosage
Shape bottle in, in the constant water bath box for being placed in 30 DEG C, through handle 5.0h question responses it is in a basic balance after, by spectrophotometry
Measure residual concentration（Dilution suitable multiple makes residual concentration in 0-50mg/L concentration ranges）, then unit obtained by standard curve
Adsorbance.Finally, the magnetic coupling functional material that can be respectively obtained as shown in Figure 5 and Figure 6 verifies the datagram of flocculation, and
Fig. 4 be then magnetic coupling functional material checking flocculation centrifugation after solution displaying figure.
Congo red is a kind of acid-base indicator in itself, and it shows rufous in neutral conditions, and royal purple is shown in acid condition
Color.It can be observed by Fig. 4, in Congo red 2500-4500mg/L high concentration range, after 5.0h reacts, do not add
The conical flask of any medicament（Blank group）, bluish violet is always maintained at, and add the conical flask of organically-modified magnetic meerschaum（Experiment
Group）, then light red brown is become.In addition, with the increase of Congo red initial concentration, the reacted color of experimental group is more shallow, just
The clearance of arnotto is also bigger, and this is runed counter to Adsorption Model, it is understood that there may be another removal mechanism of action；Optimize pH before contact
The experimental phenomena of value：There is bluish violet flocculent deposit generation under conditions of pH=1-3.5, after adsorption reaction, therefore speculate and there may be
Flocculation.
In order to verify whether there is flocculation, under Congo red 2500mg/L initial concentration, in pH=1-3.5 bar
Under part, contrast experiment has been（Other conditions are identical, and simply adding of agent situation is different）, as a result as shown in Figure 6.Pass through analysis chart
6 can obtain, headpin（Any medicament is not added）In to it is Congo red have certain removal effect be due to its own there occurs flocculation make
With；No. 2 bottles（Add sepiolite original soil）Lifted compared to the Congo red treatment effect of headpin be due to sepiolite original soil absorption
Effect；No. 3 bottles（Add organically-modified magnetic meerschaum）Compared to No. 2 Congo red treatment effects of bottle obtain further lifting
Organically-modified magnetic meerschaum is more preferable than the suction-operated of sepiolite original soil；No. 4 bottles（Add a kind of common flocculant PAM）Phase
The removal effect Congo redder than headpin more preferably further improves the Congo red flocculation work of itself due to adding flocculant PAM
With；Further, in 2500-4500mg/L high concentration range, with the rise of Congo red initial concentration, the removal effect of blank group
Step up, namely the Congo red flocculation of itself constantly strengthens；And add the experimental group absorption of magnetic coupling functional material
Removal effect（Total removal amount-correspondence blank group removal amount）But progressively decline, namely flocculation is competing compared to suction-operated
Strive power stronger；It can be obtained with reference to Fig. 5 analyses, the low initial concentration of centering（100-2000mg/L）Congo red waste water using Adsorption as
It is main, supplemented by flocculation removal, and to high concentration（2000-4500mg/L）Based on Congo red waste water is then removed with flocculating, Adsorption
Supplemented by, the reason for its is possible is：In pH=1-3.5, Congo red as flocculation core, its initial concentration is bigger, touching between molecule
Hit probability more, flocculation is stronger.
Magnetic coupling functional material handles the Congo red front and rear SEM characterization results of 1200mg/L as shown in a in Fig. 1 and c, from
Figure c can be observed, Congo red to be rolled into layer structure by magnetic coupling function material from inside to outside in pH=1-3.5, its particle
Before scale ratio absorption（Scheme a）It is much bigger, therefore figure a need to amplify 5000 times, and need to only be amplified by scheming c by 500 times.
In summary, magnetic coupling functional material is in sour environment, is reacted in the range of low initial concentration in Congo red
Be based on suction-operated, supplemented by flocculation, and in high concentration range reaction be that based on flocculation, suction-operated is
It is auxiliary.
Claims (3)
1. a kind of to Congo red magnetic coupling functional material with efficient clearance and preparation method thereof in water, its feature exists
In：Described composite functional material is by sepiolite, ferroso-ferric oxide and cetyl trimethylammonium bromide（CTAB）Composition, its
Middle ferroso-ferric oxide and CTAB are loaded to successively on sepiolite by hydro-thermal method, form ternary complex, i.e., institute of the present invention
The magnetic coupling functional material of finger.By the materials application in the processing of Congo red waste water, and treatment conditions are optimized.
2. a kind of according to claims 1 to Congo red magnetic coupling functional material with efficient clearance in water and
Its preparation method, it is characterised in that comprise the following steps：
（1）Sepiolite original soil obtains purifying sepiolite through washing drying, takes a certain amount of ground purifying sea for crossing 50-200 mesh sieves
Afrodite is placed in crucible, then is placed in Muffle furnace heat modification sepiolite is obtained after 200-300 DEG C of heat modification 1-4h, cooling；
（2）Weigh 8-15g heat modifications sepiolite and be added in 150mL conical flask, using FeCl3·6H2It is dense that O prepares 250mL
Spend the Fe for 0.05-0.2mol/L3+Solution, using FeSO4·7H2O prepares the Fe that 250mL concentration is 0.025-0.1mol/L2+
Solution, and by prepared Fe3+And Fe2+Solution respectively takes 50mL, and the mixed solution of common 100mL iron is added to above-mentioned conical flask in the lump
In, it is placed in after vibration 1-2h in thermostatic control oscillator vibration be heated to 50-80 DEG C at room temperature, then by the way that 1mol/L NaOH is added dropwise
Solution adjusts the pH value of mixed solution in bottle to 8-11, then is placed in 50-80 DEG C of thermostatic control oscillator vibration and vibrates 1-2h, so
The still aging 1-2h at 50-80 DEG C afterwards, after carrying out suction filtration separation after solution cooling, with deionized water by resulting solid material
Material washing is 7 or so to pH, and finally the solid material on filter paper is placed in 80-120 DEG C of drying box and dried, through grinding after cooling
Cross 50-200 mesh sieves and obtain magnetic meerschaum；
（3）Weigh 8-15g magnetic meerschaums and be added in 150mL conical flask, then by 150-300mL initial concentrations be 25-
30mmol/L cetyl trimethylammonium bromide（CTAB）Solution is added in above-mentioned conical flask, by mixed solution in 20-50
DEG C thermostatic control oscillator vibration reaction 18-36h, mixed solution is centrifuged after terminating for question response, using absolute ethyl alcohol
Cyclic washing being carried out to the solid material of gained with the mixed liquor of deionized water, being up to can't detect bromide ion with silver nitrate
Only, then by the solid material of gained 50-80 DEG C of drying in oven is placed in, organic change is obtained through ground 50-200 mesh sieves after cooling
Property magnetic meerschaum.
3. it is a kind of to the Congo red magnetic coupling functional material with efficient clearance in water according to claims 1
Treatment conditions optimize, it is characterised in that including following optimal conditions：20-40 DEG C of bath temperature, 0.05-1g/L dosage,
4.0-7.0h adsorption time, pH=1-3.5.
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