CN110420619A - A method of recycling graphene-based adsorbent material processing pesticide sewage - Google Patents
A method of recycling graphene-based adsorbent material processing pesticide sewage Download PDFInfo
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- CN110420619A CN110420619A CN201910622471.9A CN201910622471A CN110420619A CN 110420619 A CN110420619 A CN 110420619A CN 201910622471 A CN201910622471 A CN 201910622471A CN 110420619 A CN110420619 A CN 110420619A
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- graphene
- adsorbent material
- based adsorbent
- pesticide
- sewage
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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
- B01J20/02—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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- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F2101/30—Organic compounds
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The present invention relates to a kind of methods for recycling graphene-based adsorbent material processing pesticide sewage.The characteristics of using a large amount of transportable pi-electron and large specific surface area is contained in graphene and its derivative, corresponding adsorbent material is prepared, relevant insecticide pollution is adsorbed, and realizes recycling for graphene-based material.Cleaning, efficient novel absorption material are brought for the sewage treatment of pesticide pollutant.
Description
Technical field
The present invention relates to carbon nanomaterial fields, and in particular to the graphene oxide of recycling and carbon-based adsorbent material
The method of preparation and processing pesticide organic sewage.
Background technique
Pesticide also relies to the mankind while promoting the well-being of mankind brings harm according to the environment of existence, and pesticide utilization rate is generally 10
%, the residual of about 90 % is in the environment.Largely lost pesticide is evaporate into air, is flowed into water body, and sedimentation is gathered in soil
In, remaining insecticide pollution reaches rivers,lakes and seas and stratum depths by rain drop erosion and osmosis, so that contaminant water provides
Source.It is shown according to data survey, the pollution rate of China's river,lake and reservior substrate is more than 80 %.Insecticide pollution in waters is to agriculture
Crop and aquatile have great harm, pollute farming animals fishing fruit product, by bioconcentration, and the richness for passing through food chain
Collection effect is transferred to human body.Living environment and health to people constitute great threat.
The processing of sewage has many Treatment process, and some of which technology is developed and promotes.These technologies include
Biologic treating technique (activated sludge, biomembrane, oxidation pond etc.), physico-chemical process (absorption method, Coagulation Method, extraction) and chemical treatment
Method (neutralisation, oxidation-reduction method, chemical precipitation method).Absorption method in these processing methods, because it is with adsorption capacity
Greatly, the advantages that reaction rate is fast, easy to operate, energy consumption is lower becomes most important method for treating water in actual sewage treatment
One of.It is to develop the reusable high-performance adsorbent material of green in the Main way of absorption research.
Graphene (including graphene oxide) composite material is research hotspot in recent years, and the structure of graphene is by a large amount of
Carbon atom formed by the pi-conjugated combination of π-, so containing a large amount of transportable pi-electron, Ke Yitong in graphene
π-π effect effectively absorption aromatic pollution is crossed, to realize the removal of this pollutant.And graphene oxide is because of surface
Oxygen-containing functional group rich in, such as carboxyl, hydroxyl, carbonyl, epoxy group and excellent specific surface area have good
Hydrophily and very strong adsorptivity can have good adsorption effect to insecticide pollution in aqueous solution.Graphene-based absorption
Material is also widely used in the absorption of the organic pollutants such as dyestuff, polycyclic aromatic hydrocarbon, hydrocarbon and gasoline.
Summary of the invention
The problem to be solved in the present invention is to handle pesticide sewage using graphene-based adsorbent material and can be recycled stone
Mertenyl adsorbent material, is reused, and an experimental program is devised, and realizes graphene-based adsorbent material to sewage middle peasant
The Adsorption of medicine pollutant improves the utilization efficiency of adsorbent, reduces cost.
Purpose to realize the present invention, technical solution of the present invention the following steps are included:
Step 1
The preparation of graphene-based adsorbent: graphite is added in the concentrated sulfuric acid, under the conditions of being stirred for, potassium permanganate is sequentially added, goes
Ionized water, hydrogen peroxide.Then it after being washed with dilute hydrochloric acid, is centrifuged with deionized water to neutrality, freeze-drying obtains graphene
The continuous poriferous block materials of oxide, it is cleavable, to obtain the adsorbent of different quality.
Step 2
The pesticide sewage contains one kind of organic agricultural chemicals.(such as insecticide chlorpyrifos and herbicide hydroquinone).By organic agriculture
The adsorbent of different quality is added in the solution of medicine respective concentration.
Step 3
Using static adsorption method, after the adsorbent of different weight devotes the pollutant solution of respective concentration, ultrasonic 1-10 points
Clock is stood.
Step 4
All detection absorbance tests are detected on spectrophotometer.Because the pollutant of selection has ultraviolet characteristic absorption
Peak, using ultraviolet specrophotometer to pollutant solution adsorb front and back carry out absorbance test, reference solution be deionized water or
One kind of petroleum ether.According to standard testing.
Step 5
Graphene oxide adsorbent is recycled, circulation detergent selects deionized water, one kind of petroleum ethyl alcohol.
Detailed description of the invention
Adsorbent after the circular treatment that Fig. 1 provides for the embodiment of the present application 2 handles the adsorption efficiency to herbicide sewage
Figure；
Fig. 2 is the infrared spectrogram of graphene-based adsorbent provided by the embodiments of the present application.
Specific embodiment
Technical solution of the present invention is described further below in conjunction with specific embodiment
Embodiment 1
The preparation of 1 graphene-based adsorbent:
0.6 g crystalline flake graphite and 1.0 g sodium nitrate are added in the 35 ml concentrated sulfuric acids.It is slowly added to 3.0 under constant agitation
G potassium permanganate, reactant stir 2 hours at 5 DEG C of water-bath.Then 150 ml deionized waters are slowly added into reactant, are added
After adding, temperature is raised to 98 DEG C.Reaction solution is slowly added in 200 ml deionized waters of preheating, in stirring condition
The lower hydrogen peroxide that 10 ml, 30 % is added.Dispersion liquid by black transitions glassy yellow during have bubble generation.Use centrifuge
Centrifugation, removes removal of residue, obtains the dispersion liquid of graphene oxide.Dispersion liquid pH is set to reach 7.Freeze-drying, makes graphene oxide
It is dried to solid.
2 sewage are pesticide, chlopyrifos.
The graphene oxide that 0.005 g-0.5 g is respectively implanted in the solution of various concentration chlopyrifos is being added 10-20
Ml petroleum ether adds 0.2 g-0.5 g sodium chloride, 1-10 minutes ultrasonic.
3 stand 30-60 minutes, reach adsorption equilibrium.
4 carry out ultraviolet spectrometry detection, carry out length scanning in 190-1100 nm, have at 293 nm of specific peaks or so place
Particular peaks.As shown in Table 1 and Table 2, with the adsorption efficiency of the adsorbent absorption organophosphorus insecticide sewage of different quality, maximum value
It can reach 54.55 %, illustrate that graphene-based adsorbent has good adsorption capacity to organophosphorus insecticide sewage.
Table 1 is adsorption efficiency table of the graphene-based adsorbent of 0.005 g that provides of the embodiment of the present application 1 to insecticide chlorpyrifos
| Concentration/mgL-1 | 20 | 30 | 40 | 50 | 60 |
| Adsorption efficiency | 45.70% | 43.88% | 38.70% | 16.30% | 15.55% |
Table 2 is adsorption efficiency table of the graphene-based adsorbent of 0.010 g that provides of the embodiment of the present application 1 to insecticide chlorpyrifos
| Concentration/mgL-1 | 20 | 30 | 40 | 50 | 60 |
| Adsorption efficiency | 54.55% | 50.21% | 50.21% | 40.67% | 22.75% |
5 recycling graphene oxide adsorbents are detected with a kind of repeated flushing 3 times of petroleum ether or deionized water
After be freeze-dried.
Embodiment 2
The preparation of 1 graphene-based adsorbent:
0.6 g crystalline flake graphite and 1.0 g sodium nitrate are added in the 35 ml concentrated sulfuric acids.It is slowly added to 3.0 under constant agitation
G potassium permanganate, reactant stir 2 hours at 5 DEG C of water-bath.Then 150 ml deionized waters are slowly added into reactant, are added
After adding, temperature is raised to 98 DEG C.Reaction solution is slowly added in 200 ml deionized waters of preheating, in stirring condition
The lower hydrogen peroxide that 10 ml, 30 % is added.Dispersion liquid by black transitions glassy yellow during have bubble generation.Use centrifuge
Centrifugation, removes removal of residue, obtains the dispersion liquid of graphene oxide.Dispersion liquid pH is set to reach 7.Freeze-drying, makes graphene oxide
It is dried to solid.
2 sewage are herbicide pesticide, hydroquinone.
The graphene oxide of 0.002 g-0.005 g, ultrasonic 1- are respectively implanted in the solution of various concentration hydroquinone
It is centrifuged after ten minutes.
3 stand 1-3 hours, reach adsorption equilibrium.
4 carry out ultraviolet spectrometry detection, length scanning are carried out in 190-1100 nm, at 288 .5 nm of specific peaks or so place
There are particular peaks.Table 3 is the adsorption efficiency that graphene-based adsorbent adsorbs herbicide sewage, and adsorption efficiency maximum value can reach
55.02%, provable adsorbent has good adsorptivity to herbicide.
5 recycling graphene oxide adsorbents are freezed dry with ethyl alcohol or deionized water repeated flushing 3 times after being detected
It is dry.Fig. 1 is after different detergent handle graphene-based sorbent circulation, to adsorb again to herbicide sewage.At circulation
Adsorbent after reason can reach 28.78% to the adsorption efficiency of pollutant.
Table 3 is that the graphene-based adsorbent of 0.005 g that the embodiment of the present application 2 provides imitates the absorption for killing herbicide hydroquinone
Rate table
| Concentration/mgL-1 | 10 | 25 | 50 |
| Adsorption efficiency | 55.02% | 15.60% | 5.87% |
Claims (5)
1. a kind of method for recycling graphene-based adsorbent material processing pesticide sewage, is realized: system by following steps
Standby continuous poriferous block materials, the cleavable graphene-based adsorbent for obtaining different quality take static state to pesticide pollutant
Adsorption method recycles adsorbent material, carries out spectrophotometer measurement.
2. according to claim 1 graphene-based adsorbent material the preparation method comprises the following steps: by graphite be added the concentrated sulfuric acid in, be stirred for
Under the conditions of, sequentially add potassium permanganate, deionized water, hydrogen peroxide；Then it after being washed with dilute hydrochloric acid, is centrifuged with deionized water
To neutrality, freeze-drying.
3. pesticide pollutant according to claim 1 is organophosphorus insecticides and organic phenol-derivative herbicide.
4. in Static Adsorption according to claim 1, pH value of solution cannot be greater than 7, strong light is avoided.
5. according to claim 1 recycle one kind that detergent is petroleum ether, second alcohol and water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116037063A (en) * | 2022-12-23 | 2023-05-02 | 北京科技大学 | Graphene-like biochar and preparation method and application thereof |
Citations (2)
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|---|---|---|---|---|
| CN106167285A (en) * | 2016-07-25 | 2016-11-30 | 合众（佛山）化工有限公司 | A kind of chemical modification graphene oxide ion-type sewage-treating agent and preparation method |
| CN109248654A (en) * | 2018-10-15 | 2019-01-22 | 沈阳大学 | A kind of method that iron-based three-dimensional grapheme self-supporting material and its activation persulfate remove water removal middle peasant's chemicals contamination object |
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2019
- 2019-07-11 CN CN201910622471.9A patent/CN110420619A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106167285A (en) * | 2016-07-25 | 2016-11-30 | 合众（佛山）化工有限公司 | A kind of chemical modification graphene oxide ion-type sewage-treating agent and preparation method |
| CN109248654A (en) * | 2018-10-15 | 2019-01-22 | 沈阳大学 | A kind of method that iron-based three-dimensional grapheme self-supporting material and its activation persulfate remove water removal middle peasant's chemicals contamination object |
Non-Patent Citations (8)
| Title |
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| MALIYEKKAL, SM等: "Graphene: A Reusable Substrate for Unprecedented Adsorption of Pesticides", 《SHIHABUDHEEN》 * |
| TAMARA LAZAREVIĆ-PAŠTI等: "The impact of the structure of graphene-based materials on the removal of organophosphorus pesticides from water", 《ENVIRONMENTAL SCIENCE NANO》 * |
| 傅玲等: "Hummers法制备氧化石墨时影响氧化程度的工艺因素研究", 《炭素》 * |
| 孟娜: "《聚合物/氧化石墨烯南无复合膜制备及其分离性能研究》", 30 September 2017 * |
| 朱亚光等: "石墨烯类材料在水处理和地下水修复中的应用", 《中国环境科学》 * |
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| 郑茹等: "石墨烯基吸附材料研究进展", 《化工新型材料》 * |
| 项奇等: "氯酚类废水处理机理研究进展", 《工业水处理》 * |
Cited By (1)
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| CN116037063A (en) * | 2022-12-23 | 2023-05-02 | 北京科技大学 | Graphene-like biochar and preparation method and application thereof |
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