CN107185501A - The preparation method of graphene oxide/nano titanium oxide/sodium alginate composite and application - Google Patents
The preparation method of graphene oxide/nano titanium oxide/sodium alginate composite and application Download PDFInfo
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- 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
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- 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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Abstract
The present invention relates to the preparation method of graphene oxide/nano titanium oxide/sodium alginate composite, add graphene oxide into deionized water, obtain graphene oxide solution；Nano titanium oxide is added in graphene oxide solution, reaction solution is obtained；Reaction solution is made by graphene oxide/nano titanium oxide mixed reactant using hydro-thermal method or microwave method；Sodium alginate soln is added in graphene oxide/nano titanium oxide mixed reactant, is placed in water-bath and reacts, then naturally cool to room temperature；Reactant is washed for several times using deionized water and absolute ethyl alcohol respectively, and finished product is obtained after drying.Composite prepared by the present invention considerably improves its dispersiveness and stability, and with specific surface area is big, stability is good, good dispersion, absorption property is strong and absorption specificity is good, to heavy metal ions in sewage Pb2+Removal efficiency it is high, have good application prospect in sewage treatment area.
Description
Technical field
Heavy metal ions in sewage Pb is removed the present invention relates to one kind2+Medicament, more particularly to graphene oxide/nanometer two
The preparation method of titanium oxide/sodium alginate composite and application.
Background technology
Graphene oxide is the oxide of graphene, compared with graphene, graphene oxide have abundant oxy radical,
Good chemical modifiability and hydrophily, has relatively broad as a kind of excellent sorbing material in pollution control field
Application prospect.But, have that absorption specificity is relatively low during Adsorption, antijamming capability is weaker in analysis applications,
Powder is easily reunited simultaneously, stability is poor and causes secondary pollution problems.Nano titanium oxide has that specific surface area is big, absorption
By force, conductibility is high, band gap can reconcile chemical stability it is good the advantages of, in photocatalysis, water process, sensing and the dye sensitization sun
The fields such as energy battery have a extensive future.Sodium alginate, is called sodium alginate, is extracted from the sea-tangle or sargassum of brown algae
A kind of natural polysaccharide carbohydrate, the characteristics of with nontoxic, good hydrophily, biocompatibility and non-secondary pollution,
And sodium alginate heavy metal ion has stronger chelating removal ability.
Publication No. CN106423272A Chinese invention patent application discloses a kind of load type titania/oxidation stone
Black alkene bead and preparation method and application, technical scheme advantage is：Raw material sources are extensive, preparation technology is simple
Singly, industrialized production etc. is easily achieved, while this product has good photo catalytic reduction energy to the hexavalent chromium in waste water
Power；But there is also problem, preparation process is more complicated, the bead of preparation is used to handle the chromium ion in waste water, can not locate
Manage heavy metal in waste water lead ion.
The A of Chinese invention patent application publication number CN 105561963 disclose a kind of nano titanium oxide/graphene oxide
Composite and preparation method and application, the composite specific surface area is big, and photocatalysis efficiency is high, to the absorption property of dyestuff
Improve a lot；But operating procedure is cumbersome, it is unfavorable for realizing industrialized production, is not also applied to remove heavy metal in waste water
Ion.Therefore, develop a kind of preparation method it is simple, can the composite of effectively Adsorption heavy metal ions in sewage have very much
Practical application meaning.
The content of the invention
It is multiple that the technical problems to be solved by the invention are to provide a kind of graphene oxide/nano titanium oxide/sodium alginate
The preparation method of condensation material, the composite is removal heavy metal ions in sewage Pb2+Medicament, with larger ratio surface
Good and dispersed, the stronger absorption property of long-pending, preferable stability and preferable absorption specificity.
To achieve the above object, the present invention is realized using following technical scheme：
The preparation method of graphene oxide/nano titanium oxide/sodium alginate composite, is completed in the steps below：
Step one：Add graphene oxide into deionized water, low whipping speed is under 180r/min~500r/min
15min~45min is stirred, the graphene oxide solution that concentration is 0.5mg/mL~5mg/mL is obtained；By nano titanium oxide plus
Enter into graphene oxide solution, the mass ratio of nano titanium oxide and graphene oxide is 1~5:1；Low whipping speed is
0.5h~1h is stirred under 180r/min~500r/min, reaction solution is obtained；
Step 2：Graphene oxide/nano-silica is made in the reaction solution for being obtained step one using hydro-thermal method or microwave method
Change titanium mixed reactant；
Step 3：Sodium alginate is added in deionized water, low whipping speed be 180r/min~500r/min under stir
0.5h~2h is mixed, the sodium alginate soln that concentration is 5mg/mL~15mg/mL is obtained；Sodium alginate soln is added to step 2
In obtained graphene oxide/nano titanium oxide mixed reactant, it is placed in water-bath, is 40 DEG C~80 DEG C, stirs in temperature
Mix speed to stir 0.5h~1h under the conditions of 180r/min~500r/min, then naturally cool to room temperature；Sodium alginate and oxidation
The mass ratio of graphene/nanometer titanium dioxide mixed reactant is 0.75~3:1；
Step 4：Step 3 is made into reactant to wash for several times, then in temperature using deionized water and absolute ethyl alcohol respectively
12h~24h is dried at 40 DEG C~80 DEG C of degree, graphene oxide/nano titanium oxide/sodium alginate composite is obtained.
Graphene oxide described in step one is prepared by Hummers methods.
Hydro-thermal method described in step 2 is reaction solution is under conditions of 100 DEG C~180 DEG C in temperature, hydro-thermal reaction 5h~
20h, then reactor is naturally cooled into room temperature, graphene oxide/nano titanium oxide mixed reactant is made.
Microwave method described in step 2 is reaction solution under conditions of microwave intensity is 2.0KW~10KW, microwave reaction
5min~40min；Reactor is naturally cooled into room temperature again, graphene oxide/nano titanium oxide mixed reactant is obtained.
The application of graphene oxide/nano titanium oxide/sodium alginate composite：
Take a certain amount of containing Pb2+Waste water, it is described to contain Pb2+The concentration of waste water is 1~400mg/L, by a certain amount of oxidation stone
Black alkene/nano titanium oxide/sodium alginate composite is added to containing Pb2+Add 0.1~50g's in waste water, in every liter of waste water
Graphene oxide/nano titanium oxide/sodium alginate composite, is 5~8 with the HCl and NaOH pH value for adjusting solution, reaction
Temperature control is at 15~30 DEG C, 3~18h of magnetic agitation, then static 30min, and Pb in waste water is completed through membrane filtration2+Removal.
Above-mentioned composite removes heavy metal ions in sewage Pb2+Principle：
By the structure of graphene oxide/nano titanium oxide/sodium alginate composite, be first graphene oxide and
The combination of inorganic nano material premium properties, not only substantially increases the specific surface area of material, and in neutral and faintly acid ring
Under border, due to electrostatic interaction, nano titanium oxide and the electronegative functional group of surface of graphene oxide are by the heavy metal of positively charged
Ion Pb2+Neutralize, with Pb2+Complex compound is formed, makes Pb2+Almost all is aggregated and precipitated；Again by graphene oxide/receive
Addition sodium alginate prepares composite in rice titania solution, and sodium alginate both plays fixed effect as binding agent,
Simultaneously again to Pb2+Absorption serve cooperative effect, the composite can be promoted to heavy metal ions in sewage Pb2+Suction
Attached performance.
Compared with prior art, the beneficial effects of the invention are as follows：
1. composite prepared by the present invention considerably improves its dispersiveness and stability, adsorbent is not only overcome
The shortcoming of secondary pollution can be caused by easily reuniting and remaining in water, and it is more beneficial for the solid-liquid point after absorption as macroscopic body
From.The composite has that specific surface area is big, stability is good, good dispersion, absorption property is strong and absorption specificity is good, to sewage
Middle heavy metal ion Pb2+Removal efficiency it is high, have good application prospect in sewage treatment area.
2. preparation method of the present invention is simple and easy to apply, mild condition, reproducible, raw material are easy to get, it is with low cost to prepare.
Brief description of the drawings
Fig. 1 is sweeping for graphene oxide/nano titanium oxide/sodium alginate composite prepared by the embodiment of the present invention 3
Retouch electron microscope picture.
Fig. 2 is graphene oxide/nano titanium oxide/sodium alginate composite of the preparation of the embodiment of the present invention 3 to Pb2+
Removal effect figure.
Embodiment
The embodiment to the present invention is further illustrated below in conjunction with the accompanying drawings：
Embodiment 1
The preparation method of present embodiment graphene oxide/nano titanium oxide/sodium alginate composite is by following
What step was completed：
Step one：Add graphene oxide into deionized water, the concentration that stirring obtains graphene oxide solution is
0.5mg/mL；Then nano titanium oxide is added in 50mL 0.5mg/mL graphene oxide solutions, nano titanium oxide
Mass ratio with graphene oxide is 5:1, stirring obtains reaction solution；
Step 2：Reaction solution is poured into hydrothermal reaction kettle, under conditions of temperature is 120 DEG C, hydro-thermal reaction 8h, then will
Reactor naturally cools to room temperature, and graphene oxide/nano titanium oxide mixed reactant is made；
Step 3：Sodium alginate is added in deionized water, mixing speed is 180r/min~200r/min, stirring
0.5h, stirring obtains concentration 15mg/mL sodium alginate soln；30mL 15mg/mL sodium alginate solns are added to oxidation
In graphene/nanometer titanium dioxide mixed reactant, it is placed in after being reacted in water-bath, is 50 DEG C in temperature, mixing speed is
30min is stirred under the conditions of 180r/min~200r/min, room temperature is cooled to；Sodium alginate and graphene oxide/nano-silica
The mass ratio for changing titanium mixed reactant is 3:1；
Step 4：Step 3 is made into reactant to wash 3 times using deionized water and absolute ethyl alcohol respectively, then in temperature
14h is dried at 60 DEG C, graphene oxide/nano titanium oxide/sodium alginate composite is made.
Embodiment 2
The preparation method of present embodiment graphene oxide/nano titanium oxide/sodium alginate composite is by following
What step was completed：
Step one：Add graphene oxide into deionized water, the concentration that stirring obtains graphene oxide solution is
5mg/mL；Then nano titanium oxide is added in 50mL 5mg/mL graphene oxide solutions, nano titanium oxide and oxygen
The mass ratio of graphite alkene is 1:1, stirring obtains reaction solution；；
Step 2：Reaction solution is poured into reactor, under conditions of microwave intensity is 5KW, microwave reaction 10min；Again
Reactor is naturally cooled into room temperature, graphene oxide/nano titanium oxide mixed reactant is obtained；
Step 3：Sodium alginate is added in deionized water, low whipping speed be 300r/min~330r/min under stir
0.5h is mixed, stirring obtains concentration 10mg/mL sodium alginate soln；75mL 10mg/mL sodium alginate solns are added to oxygen
In graphite alkene/nano titanium oxide mixed reactant, be placed in after being reacted in water-bath, temperature be 60 DEG C, mixing speed be
1h is stirred under the conditions of 260r/min~300r/min, room temperature is cooled to；Sodium alginate and graphene oxide/nano titanium oxide
The mass ratio of mixed reactant is 1.5:1；
Step 4：Step 3 is made into reactant to wash 4 times using deionized water and absolute ethyl alcohol respectively, then in temperature
12h is dried at 70 DEG C, graphene oxide/nano titanium oxide/sodium alginate composite is made.
Embodiment 3
The preparation method of present embodiment graphene oxide/nano titanium oxide/sodium alginate composite is by following
What step was completed：
Step one：Add graphene oxide into deionized water, the concentration that stirring obtains graphene oxide solution is
3mg/mL；Then nano titanium oxide is added in 50mL 3mg/mL graphene oxide solutions, nano titanium oxide and oxygen
The mass ratio of graphite alkene is 3:1, stirring obtains reaction solution；
Step 2：Reaction solution is poured into hydrothermal reaction kettle, under conditions of temperature is 150 DEG C, hydro-thermal reaction 16h, then
Reactor is naturally cooled into room temperature, graphene oxide/nano titanium oxide mixed reactant is made.
Step 3：Sodium alginate is added in deionized water, low whipping speed be 400r/min~420r/min under stir
0.5h is mixed, stirring obtains concentration 5mg/mL sodium alginate soln；90mL 5mg/mL sodium alginate solns are added to oxidation
In graphene/nanometer titanium dioxide mixed reactant, be placed in after being reacted in water-bath, temperature be 70 DEG C, mixing speed be
40min is stirred under the conditions of 230r/min~260r/min, room temperature is cooled to；Sodium alginate and graphene oxide/nano-silica
The mass ratio for changing titanium mixed reactant is 0.75:1；
Step 4：Step 3 is made into reactant to wash 3 times using deionized water and absolute ethyl alcohol respectively, then in temperature
18h is dried at 55 DEG C, graphene oxide/nano titanium oxide/sodium alginate composite is made.
Scanning electron microscope diagram such as Fig. 1 of graphene oxide/nano titanium oxide/sodium alginate composite of preparation
It is shown.
The application examples of the composite of embodiment 3
Compound concentration is 40mg/L Pb2+Solution is separately added into the oxygen of the preparation of 0.05g embodiments 3 in 50mL conical flasks
Graphite alkene/nano titanium oxide/sodium alginate composite, is 6, reaction temperature with the HCl and NaOH pH value for adjusting solution
Control carries out magnetic agitation 0.5h, 1h, 2h, 3h, 4h, 5h, 6h, then static 30min respectively at 25 DEG C, after membrane filtration
Pb in solution is measured using atomic absorption spectrophotometer2+, experimental result is as shown in Figure 2.
As seen from the figure, graphene oxide/nano titanium oxide/sodium alginate composite is to Pb2+Removal effect is with the time
Change.
Graphene oxide/nano titanium oxide/sodium alginate composite and Pb2+When reacting 0.5h, Pb2+Clearance is
39.2%；From 0.5h to 2h, Pb2+Clearance brings up to 93.5%, heavy metal ions in wastewater Pb from 39.2%2+By big portion
Divide and remove；When reaction carries out 3h, clearance reaches 98.9%, continues to increase the reaction time, clearance is basically unchanged, now adsorbed
Reaction reaches balance.
The specific surface area of graphene oxide/nano titanium oxide/sodium alginate composite is big, stability is good, dispersiveness
Well, absorption property is strong and absorption specificity is good, to heavy metal ions in sewage Pb2+Removal efficiency it is high.
Described above is only the general principle of the present invention, and not the present invention is imposed any restrictions, every right according to the present invention
It carries out equivalent variations and modification, within the category of the art of this patent protection scheme.
Claims (5)
1. the preparation method of graphene oxide/nano titanium oxide/sodium alginate composite, it is characterised in that by following steps
It is rapid to complete：
Step one：Add graphene oxide into deionized water, low whipping speed is stirring under 180r/min~500r/min
15min~45min, obtains the graphene oxide solution that concentration is 0.5mg/mL~5mg/mL；Nano titanium oxide is added to
In graphene oxide solution, the mass ratio of nano titanium oxide and graphene oxide is 1~5:1；Low whipping speed is 180r/
0.5h~1h is stirred under min~500r/min, reaction solution is obtained；
Step 2：Graphene oxide/nano titanium oxide is made in the reaction solution for being obtained step one using hydro-thermal method or microwave method
Mixed reactant；
Step 3：Sodium alginate is added in deionized water, low whipping speed is stirring under 180r/min~500r/min
0.5h~2h, obtains the sodium alginate soln that concentration is 5mg/mL~15mg/mL；Sodium alginate soln is added to step 2 system
In the graphene oxide/nano titanium oxide mixed reactant obtained, it is placed in water-bath, is 40 DEG C~80 DEG C, stirring in temperature
Speed is stirring 15min~1h under the conditions of 180r/min~500r/min, then naturally cools to room temperature；Sodium alginate and oxidation stone
The mass ratio of black alkene/nano titanium oxide mixed reactant is 0.75~3:1；
Step 4：Step 3 is made into reactant to wash for several times, then in temperature 40 using deionized water and absolute ethyl alcohol respectively
DEG C~80 DEG C at dry 12h~24h, obtain graphene oxide/nano titanium oxide/sodium alginate composite.
2. the preparation method of graphene oxide/nano titanium oxide/sodium alginate composite according to claim 1,
Characterized in that, the graphene oxide described in described step one is prepared by Hummers methods.
3. the preparation method of graphene oxide/nano titanium oxide/sodium alginate composite according to claim 1,
Characterized in that, it is water under conditions of 100 DEG C~180 DEG C that the hydro-thermal method described in described step two, which is reaction solution in temperature,
Thermal response 5h~20h, then reactor is naturally cooled into room temperature, graphene oxide/nano titanium oxide mixed reactant is made.
4. the preparation method of graphene oxide/nano titanium oxide/sodium alginate composite according to claim 1,
Characterized in that, the microwave method described in described step two is reaction solution under conditions of microwave intensity is 2.0KW~10KW,
Microwave reaction 5min~40min；Reactor is naturally cooled into room temperature again, graphene oxide/nano titanium oxide mixing is obtained
Reactant.
5. the application of graphene oxide/nano titanium oxide/sodium alginate composite according to claim 1：It is special
Levy and be, comprise the following steps that：
Graphene oxide/nano titanium oxide/sodium alginate composite is added to containing Pb2+In waste water, containing Pb2+Waste water it is dense
Spend for 1~400mg/L, every liter contains Pb2+0.1~50g graphene oxide/nano titanium oxide/sodium alginate is added in waste water
Composite, is 5~8 with HCl and the NaOH pH value for adjusting solution, reaction temperature control at 15~30 DEG C, magnetic agitation 3~
18h, then static 30min, Pb in waste water is completed through membrane filtration2+Removal.
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| CN107469772A (en) * | 2017-10-13 | 2017-12-15 | 山东理工大学 | A kind of method of heavy metal classes incretion interferent in removal reverse osmosis concentrated water |
| CN107761195A (en) * | 2017-10-26 | 2018-03-06 | 青岛大学 | A kind of lignin-base nano carbon fibre preparation method for electrode of super capacitor |
| CN109126647A (en) * | 2018-09-08 | 2019-01-04 | 佛山市森昂生物科技有限公司 | A kind of preparation method of graphene oxide-sodium alginate gel ball |
| CN109651860A (en) * | 2018-12-24 | 2019-04-19 | 湖北航天化学技术研究所 | A kind of graphene/nanometer titanium dioxide composite material and preparation method and application |
| CN109651860B (en) * | 2018-12-24 | 2021-06-11 | 湖北航天化学技术研究所 | Graphene/nano titanium dioxide composite material and preparation method and application thereof |
| CN111054395A (en) * | 2019-12-10 | 2020-04-24 | 中国环境科学研究院 | Visible-light-driven photocatalyst, and preparation method and application thereof |
| CN116386928A (en) * | 2023-06-02 | 2023-07-04 | 山东科技大学 | Sodium alginate/titanium dioxide composite porous electrode material and preparation method thereof |
| CN116386928B (en) * | 2023-06-02 | 2023-08-04 | 山东科技大学 | Sodium alginate/titanium dioxide composite porous electrode material and preparation method thereof |
| CN118329785A (en) * | 2024-06-14 | 2024-07-12 | 东北师范大学 | Detection bottle for simultaneously detecting glucose, uric acid and lactic acid in whole blood and application thereof |
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