CN108499542A - A kind of composite material and preparation method based on egg shell of efficient process environmental wastewater - Google Patents
A kind of composite material and preparation method based on egg shell of efficient process environmental wastewater Download PDFInfo
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- CN108499542A CN108499542A CN201810413580.5A CN201810413580A CN108499542A CN 108499542 A CN108499542 A CN 108499542A CN 201810413580 A CN201810413580 A CN 201810413580A CN 108499542 A CN108499542 A CN 108499542A
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
- C02F2101/40—Organic compounds containing sulfur
Abstract
The composite material and preparation method and application that the invention discloses a kind of efficient process environmental wastewaters based on egg shell, belong to material preparation and the technical field of environmental pollution improvement.It is characterized in that the step of preparing is:1) by 0.5g FeSO4·7H2O is dissolved in the conical flask for filling 60mL distilled water, and 1g egg shell powders are added.Then conical flask is placed in magnetic stirrer 0.5h.2) 10mL 0.1mol/L NaBH are slowly added to by dropper4Solution, and it is continually fed into nitrogen reaction 1h.Most dried afterwards to get to the Fe Eggshell composite materials through suction filtration, washing and vacuum drying oven.The present invention is mixed with reaction raw materials using waste egg shell powder without prolonged reaction, can be obtained sample using the method for reduction in aqueous solution at room temperature.Reaction condition is mild, raw material is cheap and easy to get, versatile, is conducive to large-scale industrial production, has significant economic and social benefit.The composite material has the performance for efficiently adsorbing organic dyestuff in wastewater.
Description
Technical field
The invention belongs to material preparation and the technical fields of environmental pollution improvement, and in particular to a kind of efficient process environment is useless
The Fe-Eggshell composite material and preparation methods of the Zero-valent Iron load based on egg shell of water and application.
Technical background
Organic dyestuff has many advantages, such as that bright in colour, good water solubility and application technology are simple and be widely used in printing
In the production of ink, coating, textile fabric, construction material and plastics etc..In water a small amount of dyestuff will stimulate skin cause it is acute in
Poison, or biological chronic injury.In addition, the dyestuff in water can also interfere sunlight to enter in water and the dissolved oxygen amount of air, directly
The photosynthesis for influencing water plant, destroys the balance of aquatic ecosystem.Therefore, how environmental wastewater is effectively treated, to protecting
The health of barrier citizen has extensive social effect.
Currently, processing method includes mainly biological treatment, chemical oxidization method, flocculent precipitation, extraction in dyeing waste water
It follows the example of, electrolysis, photocatalytic method and absorption method etc..Wherein, absorption method uses no or little organic solvent, operation letter due to having
Just the advantages that, safety, production process pH variation are small, insensitive to toxic pollutant and do not generate secondary pollution, becomes current
A kind of effective ways of difficult for biological degradation pollutant in extremely potential processing waste water.Nano zero valence iron is because with larger
Specific surface area and stronger adsorption capacity, can be to be widely used in earth's surface the features such as various pollutants in fast degradation environment
Water and groundwater remediation field.But due to its special physicochemical property, it is made to there are problems that in practical applications, such as easily
Reunite, be difficult to recycle and easily by organic matter absorption etc. in environment.Therefore, the modification of nano zero valence iron is mainly collected in recent years
In be carried on solid carrier such as silicon, activated carbon, resin etc., to increase the specific surface area of nano iron particles, inhibit to reunite
Occur, transfer ability of the enhancing nano zero-valence iron particle in surrounding medium.
Therefore, studying simple, the excellent processing environment waste water of efficient new method processability composite material has ten
Divide important meaning.In the present invention, we prepare the Zero-valent Iron based on egg shell using waste egg shell as bio-carrier
The Fe-Eggshell composite materials of load, the adsorption treatment for organic pollution in environmental wastewater.Through consulting literatures, we
It was found that there is presently no the relevant reports for using liquid phase reduction to prepare Fe-Eggshell composite materials.
Invention content
The purpose of the present invention is to provide the composite materials and its system based on egg shell of a kind of efficient process environmental wastewater
Preparation Method and application intend to solve the problems such as activity is low, and nano particle is easily reunited in conventional composite materials, while utilizing waste chicken
Eggshell is turned waste into wealth.This method is mixed with reaction raw materials using egg shell powder without prolonged reaction, utilizes room temperature liquid phase
The method of reduction can be obtained sample.Composite material prepared by the present invention can be in efficient absorption waste water organic dyestuff.This
Invention preparation method reaction condition is mild, raw material is cheap and easy to get, is conducive to large-scale industrial production, have it is significant economical and
Social benefit.
The present invention is achieved by the following technical solutions, and a kind of composite material of efficient process environmental wastewater is a kind of base
In the composite material of waste egg shell, the ability for efficiently handling waste water is shown by the modification of zeroth order iron nano-particle.
Protein and nanometer Fe interact so that nano particle can be very good to be dispersed in egg shell in egg shell in composite material
Surface improves the adsorption capacity of gained sample without agglomeration occurs.It is characterized by comprising following procedure:
1) Fresh Egg shell is soaked in water and removes egg film, after drying, pulverized.
2) by FeSO4·7H2O is added in 60 milliliters of distilled water, stirring to dissolving.
3) a certain amount of egg shell powder is added in the step 2) solution, stirs 0.5~1h.
4) NaBH of a certain concentration certain volume is slowly dropped into suspension obtained by step 3)4, one section of maintaining nitrogen purge
Time.
5) suspension obtained by step 4) is filtered, washed and is transferred to vacuum drying oven drying.
By said program, the FeSO described in step 2)4·7H2O is 0.1~5.0mmol.
By said program, the amount of the egg shell powder described in step 3) is 1.0~10g.
By said program, the step 4) NaBH4Volume be 0.1~120mL, 0.1~2.0mmol/L of concentration.
The present invention proposes at room temperature, using egg shell as carrier, to utilize NaBH4Liquid-phase reduction is carried out, using in egg shell
The interaction of protein and iron makes Zero-valent Iron may be uniformly dispersed on egg shell carrier.
The Fe-Eggshell composite materials prepared using the present invention are applied to Congo red in absorption waste water.Experiment
Process is as follows:The Fe-Eggshell of a concentration of 0.1~0.6g/L is dispersed in the Congo red solution for being loaded with 300mL50mg/L
Conical flask in, with salt acid for adjusting pH value to 3~7, temperature is controlled at 25~45 DEG C, and conical flask is sufficiently stirred in the place of being protected from light.
Timing takes a certain amount of reaction solution centrifugation, filtering, and supernatant is taken to measure its absorbent properties with ultraviolet specrophotometer.
The physical property characterizing method of Fe-Eggshell composite materials:With X-ray diffraction (XRD) spectrum analysis product object
Matter forms and structure situation, and the pattern of product is observed with field emission scanning electron microscope (FE-SEM), uses ultraviolet-uisible spectrophotometer
Analyze the light absorption situation of product.
The beneficial effects of the present invention are:
(1) preparation method of Fe-Eggshell composite materials of the present invention is simple and easy to do, passes through a step liquid-phase reduction
Method, preparation flow is simple, is conducive to large-scale industrial production.
(2) on the one hand the present invention is turned waste into wealth using waste egg shell as carrier, on the other hand, utilizes egg shell
The interaction of middle protein and Fe allow nano zero valence iron to be uniformly dispersed in egg shell surface, improve its absorption property.
(3) Fe-Eggshell composite materials of the present invention can efficiently adsorb the congo red in waste water,
Separation and recovery processing can be easily carried out in absorption system, composite material is Ke Xunhuanliyong, has very high practical value
And application prospect.
Description of the drawings
Fig. 1 is the XRD spectra of product obtained by example 1.
Fig. 2 is the SEM spectrograms of product obtained by example 1.
Influence of the different dosages that Fig. 3 is Fe-Eggshell obtained by example 1 to the absorption property of Congo red solution.
Fig. 4 is Fe-Eggshell and zeroth order Fe and egg shell powder obtained by example 1 to the ratio of Congo red solution absorption property
Compared with figure.
Shadow of the different initial concentrations that Fig. 5 is Fe-Eggshell obtained by example 1 to the absorption property of Congo red solution
It rings.
Fig. 6 is Fe-Eggshell obtained by example 1 at different temperatures to the absorption property of Congo red solution.
Fig. 7 is for Fe-Eggshell obtained by example 1 to the absorption property of Congo red solution at different pH.
Specific implementation mode
It is further illustrated the present invention with reference to embodiment, which is served only for illustrating the present invention, is not intended to limit the present invention.
Embodiment 1
By 0.5g FeSO4·7H2O is dissolved in the conical flask for filling 60mL distilled water, and 1g egg shell powders are added.Then cone
Shape bottle is placed in magnetic stirrer 0.5h, then is slowly added to 10mL 0.1mol/L NaBH by dropper4Solution, and persistently lead to
Enter nitrogen reaction 1h.The distillation washing 3 times of gained sample is finally filtered, absolute ethyl alcohol is washed 1 time, and acetone is washed 3 times, is finally placed true
The drying of empty drying box is to get to the Fe-Eggshell composite materials.Fig. 1 is the XRD spectrum of products therefrom, it can be seen that chicken
The main component of eggshell is calcium carbonate, occurs the diffraction maximum of Fe on the XRD spectra of composite material, shows gained composite material
Middle Zero-valent Iron accounts for major part.Wherein, also occurs a small amount of FeOOH during synthesis.Fig. 2 is the SEM figures of products therefrom
Spectrum, what can be apparent from sees, nano zero valence iron is uniformly dispersed in the surface of egg shell so that nano particle easily reunites this
Problem is greatly improved.
Application examples 1
The application of absorption property is carried out to above-mentioned gained Fe-Eggshell composite materials:
The Fe-Eggshell of a concentration of 0.1~0.6g/L is dispersed in the cone for the Congo red solution for being loaded with 300mL 50mg/L
In shape bottle, with salt acid for adjusting pH value to 3~7, temperature is controlled at 25~45 DEG C.Conical flask is sufficiently stirred in the place of being protected from light.Periodically
A certain amount of reaction solution centrifugation, filtering are pipetted, supernatant ultraviolet specrophotometer is taken to measure absorbent properties.The present invention investigates
Different materials (Fig. 4), composite material dosage (Fig. 3), composite material initial concentration (Fig. 5), temperature (Fig. 6) and pH value (Fig. 7) etc.
Influence to Congo red solution absorption property.The result shows that composite material of the invention has efficient absorption property.
Embodiment 2
By 1g FeSO4·7H2O is dissolved in the conical flask for filling 60mL distilled water, and 1g egg shell powders are added.Then taper
Bottle is placed in magnetic stirrer 0.5h, then is slowly added to 10mL 0.1mol/L NaBH by dropper4Solution, and be continually fed into
Nitrogen reacts 1h.The distillation washing 3 times of gained sample is finally filtered, absolute ethyl alcohol is washed 1 time, and acetone is washed 3 times, and vacuum is finally placed
Drying box drying is to get to the Fe-Eggshell composite materials.
Embodiment 3
By 2.5g FeSO4·7H2O is dissolved in the conical flask for filling 60mL distilled water, and 1g egg shell powders are added.Then cone
Shape bottle is placed in magnetic stirrer 0.5h, then is slowly added to 10mL 0.1mol/L NaBH by dropper4Solution, and persistently lead to
Enter nitrogen reaction 1h.The distillation washing 3 times of gained sample is finally filtered, absolute ethyl alcohol is washed 1 time, and acetone is washed 3 times, is finally placed true
The drying of empty drying box is to get to the Fe-Eggshell composite materials.
Embodiment 4
By 3.0g FeSO4·7H2O is dissolved in the conical flask for filling 60mL distilled water, and 1g egg shell powders are added.Then cone
Shape bottle is placed in magnetic stirrer 0.5h, then is slowly added to 10mL 0.1mol/L NaBH by dropper4Solution, and persistently lead to
Enter nitrogen reaction 1h.The distillation washing 3 times of gained sample is finally filtered, absolute ethyl alcohol is washed 1 time, and acetone is washed 3 times, is finally placed true
The drying of empty drying box is to get to the Fe-Eggshell composite materials.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (5)
1. a kind of composite material and preparation method based on egg shell of efficient process environmental wastewater, which is characterized in that including
Following steps:
One, Fresh Egg shell is soaked in water and removes egg film, after drying, pulverized.
Two, a certain amount of ferrous sulfate hydrate is added in 60 milliliters of distilled water, stirring to dissolving.
Three, the egg shell powder obtained by a certain amount of step 1 is added in above-mentioned solution.
Four, above-mentioned gained suspension is placed in magnetic stirrer 0.5 hour.
Five, by certain density NaBH4It is slowly dropped into the suspension obtained by step 4, maintaining nitrogen purge is for a period of time.
Six, gained suspension filtration washing in step 5 is finally transferred to vacuum drying oven drying.
2. the composite material and preparation method according to claim 1 based on egg shell, it is characterised in that step 2 institute
State FeSO4·7H2O is 0.1~5.0mmol.
3. the composite material and preparation method according to claim 1 based on egg shell, it is characterised in that step 3 institute
The quality for stating egg shell powder is 1.0~10g.
4. the composite material and preparation method according to claim 1 based on egg shell, it is characterised in that step 5 institute
State NaBH4A concentration of 0.1~2.0mmol/L.
5. a kind of application of the composite material based on egg shell as described in claim 1, it is characterised in that:It is described based on chicken
The composite material of eggshell is used for the adsorption treatment of congo red in waste water.
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Cited By (3)
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CN109809466A (en) * | 2019-03-27 | 2019-05-28 | 泉州师范学院 | A kind of preparation method and application of the copper sulfide nano material based on egg shell template |
CN109847774A (en) * | 2019-03-16 | 2019-06-07 | 泉州师范学院 | It is a kind of for removing the preparation method and application of p-nitrophenol material |
CN110000397A (en) * | 2019-04-19 | 2019-07-12 | 泉州师范学院 | A kind of copper nano material based on egg shell template and preparation method thereof, antibacterial applications |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109847774A (en) * | 2019-03-16 | 2019-06-07 | 泉州师范学院 | It is a kind of for removing the preparation method and application of p-nitrophenol material |
CN109809466A (en) * | 2019-03-27 | 2019-05-28 | 泉州师范学院 | A kind of preparation method and application of the copper sulfide nano material based on egg shell template |
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CN110000397A (en) * | 2019-04-19 | 2019-07-12 | 泉州师范学院 | A kind of copper nano material based on egg shell template and preparation method thereof, antibacterial applications |
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Effective date of registration: 20190123 Address after: 362000 Donghai Street 398, Fengze District, Quanzhou City, Fujian Province Applicant after: QUANZHOU NORMAL University Address before: 362000 Shishi City, Quanzhou City, Fujian Province, Shihugang Industrial Park, Bijiang Town, Building 501, No. 5, 1900, Science and Technology Incubation Base on both sides of the Taiwan Strait Applicant before: SHISHI NATONG NEW MATERIAL TECHNOLOGY CO.,LTD. |
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Application publication date: 20180907 |