CN108636370A - A kind of nano-magnetic powder body material preparation method and application based on oyster shell - Google Patents
A kind of nano-magnetic powder body material preparation method and application based on oyster shell Download PDFInfo
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- CN108636370A CN108636370A CN201810506202.1A CN201810506202A CN108636370A CN 108636370 A CN108636370 A CN 108636370A CN 201810506202 A CN201810506202 A CN 201810506202A CN 108636370 A CN108636370 A CN 108636370A
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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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- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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
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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
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Abstract
The nano-magnetic powder body material preparation method and application based on oyster shell that the invention discloses a kind of belonging to the technical field of nano material preparation and environmental pollution improvement.It is characterized in that the step of preparing is：By the FeCl of certain mass3·6H2O is dissolved in the distilled water for filling certain volume, is separately added into the citric acid of certain mass, the ethylenediamine of certain volume, is stirred until being completely dissolved.The sodium hydroxide that certain mass is added into above-mentioned solution stirs evenly, and finally adds a certain amount of oyster shell powder.Above-mentioned suspension is transferred in autoclave, then reaction kettle is placed in baking oven under certain temperature and is kept for certain time.End product is detached through magnet, is washed with distilled water and ethyl alcohol, and products therefrom is transferred to vacuum drying oven drying to get to the oyster shell base nano-magnetic powder.The raw materials used in the present invention is cheap and easy to get, and preparation condition is simple and practicable, can be obtained sample by one step hydro thermal method, versatile, is conducive to large-scale industrial production, has significant economic and social benefit.The nano magnetic composite materials show the performance for efficiently adsorbing organic dyestuff in wastewater.
Description
Technical field
The invention belongs to new material preparation and the technical fields of environmental pollution improvement, and in particular to one kind being based on oyster shell
Nano-magnetic powder body material preparation method and environmental wastewater processing application.
Background technology
Dyestuff is a kind of important fine chemical product closely bound up with us in daily life.Due to dyestuff work
Industry is constantly developed in China, and the discharge capacity of waste water from dyestuff is also being continuously increased.Wherein, some chemical dyestuffs not just
It is left about when using and disorderly arranging, body eutrophication is caused to pollute.In addition, the organic pollutant category contained in waste water from dyestuff is numerous
It is more, it is difficult to carry out subsequent processing.In traditional chemical process production, the method master of most common removal Wastewater Dyes
To include ozonisation, flocculation, oxidation etc., but the cost is relatively high for these traditional technologies, removal efficiency is poor.Therefore, exploitation and
New and effective sorbing material, the especially waste of some industry and agricultural are explored as sorbing material, to ensureing citizen's
The sustainable development of health and society has very profound significance.
Oyster shell is a kind of shell that some coastal areas are usually arbitrarily abandoned, and wherein chemical composition calcium carbonate accounts for
About 95% or more.In addition to this, also 17 kinds of amino acid, 24 kinds of trace elements and some polysaccharide.According to statistics, China is annual
The shell being dropped is at least at 10,000,000 tons or more, these oyster shells arbitrarily abandoned are because remaining a small amount of organic matter, in length
It is constantly corrupt smelly during phase stacks, a large amount of land resource is not only taken up, and causes to seriously endanger to environment.
Therefore, how these discarded oyster shells are turned waste into wealth, is of great significance to the development of society.Fe3O4Magnetic Nano
Material is widely used in various fields due to larger specific surface area and smaller grain size.But it is if long-term
It is exposed in air, since the unstability of itself is easy to be reunited at di-iron trioxide by the dioxygen oxidation in air
Phenomenon, so as to cause dispersion degree and magnetic reduction.If by Fe3O4Magnetic Nano material is carried on oyster shell, on the one hand
Solves Fe3O4On the other hand the problem of reuniting and easily being aoxidized can make full use of waste oyster shell, to a certain degree
Upper solution problem of environmental pollution.
Therefore, processing of the efficient novel nano-material for organic dyestuff in environmental wastewater is studied with particularly significant
Meaning.In the present invention, we prepare the ferroso-ferric oxide based on oyster shell using waste oyster shell as complex carrier
The composite nano-powder material of load, the adsorption treatment for organic pollution in environmental wastewater.Through consulting literatures, Wo Menfa
Now there is presently no relevant reports.
Invention content
The purpose of the present invention is to provide a kind of, and the nano-magnetic powder body material and preparation method thereof based on oyster shell is used for
The processing of environmental wastewater, intends to solve of high cost in conventional composite materials, the problems such as waste water treatment efficiency is low, while using discarded
Object oyster shell, turns waste into wealth, and solves problem of environmental pollution to a certain extent.This method is simple to operation, using oyster shell powder
It is mixed with reaction raw materials, can be obtained sample using one step hydro thermal method.Nanocomposite prepared by the present invention can be efficient
Adsorb the organic dyestuff in waste water.Preparation method reaction condition of the present invention is simple, raw material is cheap and easy to get, is conducive to large-scale
Industrial production has significant economic and social benefit.
The present invention is achieved by the following technical solutions, and a kind of nanocomposite of efficient process environmental wastewater is
A kind of composite material based on waste oyster shell, is shown efficiently by the modification of ferroferric oxide magnetic nano-material
Adsorb the ability of organic dyestuff in wastewater.In nanocomposite, Fe with a smaller size3O4Nano particle can be very good
The surface of oyster shell is dispersed in without agglomeration occurs, improves the adsorption capacity of gained sample.It is characterized by comprising
Following procedure：
1) by a certain amount of FeCl3·6H2O is added in the water of 20mL, stirring to dissolving；
2) a certain amount of citric acid and ethylenediamine are added in step 1) acquired solution, stirring to dissolving；
3) a certain amount of sodium hydroxide is added in step 2) acquired solution, is stirred evenly；
4) a certain amount of oyster shell powder is added into step 3) acquired solution；
5) suspension obtained by step 4) is transferred in autoclave, is then transferred to reaction kettle in baking oven centainly
At a temperature of kept for 12 hours；
6) suspension obtained after step 5) hydro-thermal is detached by magnet, is washed through a certain amount of distilled water and ethyl alcohol,
Finally it is transferred to vacuum drying oven drying.
By said program, the FeCl described in step 1)3·6H2O is 0.1~5.0g.
By said program, the citric acid quality described in step 2) is 0.1~10g, and ethylenediamine volume is 0.1~10mL.
By said program, step 3) the NaOH mass is 0.1~2.0g.
By said program, step 4) the oyster shell powder quality is 0.01~0.5g.
By said program, the step 5) hydrothermal temperature is 80~200 DEG C.
The present invention proposes to pass through one step hydro thermal method, using oyster shell as carrier, by magnetic material Fe3O4It is evenly dispersed in male
On oyster shell surface.
The Fe prepared using the present invention3O4Oyster shell nanocomposite, the Congo being applied in absorption waste water
It is red.Experimentation is as follows：Precise is Congo red to be dissolved in distilled water, and volumetric flask is used to prepare 1g/L mother liquors as storing solution.It takes out
A certain amount of storing solution, it is respectively 25mg/L that Congo red initial mass concentration is prepared after being diluted with distilled water, using liquid-transfering gun
The Congo red solution of 10mL is taken out, is put into vial, precise 50mg Fe3O4Oyster shell nanocomposite is put into dress
In the vial for having Congo red solution, tested in different time at 200~600nm of wavelength with ultraviolet-visible spectrophotometer
And the absorbance under different wave length, determine adsorption curve figure.
Fe3O4The physical property characterizing method of oyster shell nanocomposite：It is produced with X-ray diffraction (XRD) spectrum analysis
Object material composition and structure situation observe the pattern of product with field emission scanning electron microscope (FE-SEM), and light is divided with UV, visible light
The light absorption situation and drafting kinetic curve of degree score division object.
The beneficial effects of the present invention are：
(1) Fe of the present invention3O4The preparation method of oyster shell nanocomposite is simple and easy to do, passes through a step water
Hot method can be obtained, and preparation flow is simple, be conducive to large-scale industrial production.
(2) on the one hand the present invention turns waste into wealth using waste oyster shell as carrier, solves oyster shell to environment
Pollution problem；On the other hand, by the Fe with large specific surface area and smaller particle size3O4Magnetic material uniformly disperses
On oyster shell surface, the absorption property of composite material is improved.
(3) Fe of the present invention3O4Oyster shell nanocomposite can efficiently adsorb the Congo in environmental wastewater
Red dye, and composite material is easy to be recycled, and recycling, is of very high actual application value and application prospect.
Description of the drawings
Fig. 1 is X-ray diffraction (XRD) spectrogram of product obtained by example 1.
Fig. 2 is Fe obtained by example 13O4Scanning electron microscope (SEM) spectrogram of oyster shell.
Fig. 3 is Fe obtained by example 13O4The magnetic snapback figure of oyster shell.
Fig. 4 is Fe obtained by example 13O4Oyster shell and Fe3O4Nano particle and oyster shell powder are identical to initial concentration
The control collection of illustrative plates that Congo red solution absorption property changes over time.
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
0.1g ferric chloride hexahydrates are added in 20mL water and are stirred, 0.1g citric acids, 1mL ethylenediamines is separately added into, stirs
It mixes until being completely dissolved, adds 0.5g sodium hydroxides and stir evenly, finally add 0.1g oyster shell powders.Above-mentioned suspension is turned
It moves in autoclave, reaction kettle is then placed in 100 DEG C of holding 12h in baking oven.Product after hydro-thermal passes through magnet point
From being washed using distilled water and ethyl alcohol.Vacuum drying oven drying is finally placed to get to the Fe3O4Oyster shell nanometer is multiple
Condensation material.Fe3O4The preparation method of nano particle is similar with the above flow, is only added without oyster shell powder in reaction process.Fig. 1
For the XRD spectrum of products therefrom, it can be seen that the main component of oyster shell is calcium carbonate, is gone out on the XRD spectra of composite material
Fe is showed3O4Diffraction maximum.Fig. 2 is gained Fe respectively3O4Nano particle and Fe3O4The SEM spectrum of oyster shell can be apparent from
See, Fe with a smaller size3O4Nano particle is uniformly dispersed in the surface of oyster shell so that nano particle is easily reunited
This problem is greatly improved.Fig. 3 is the magnetization curve figure of composite material, which has apparent hysteresis,
Belong to typical ferromagnetic behavior.Saturation magnetization is 26.9emu/g, is conducive to the recycling after absorption.
Application examples 1
To above-mentioned gained Fe3O4Oyster shell nanocomposite carries out the application of absorption property：
After the Congo red solution of a concentration of 1g/L is diluted with distilled water, preparing Congo red initial mass concentration is respectively
25mg/L takes out the Congo red solution of 10mL using liquid-transfering gun, is put into vial.Precise 50mg Fe3O4Oyster shell
Nanocomposite is put into the vial equipped with Congo red solution, with ultraviolet-visible spectrophotometer wavelength 200~
Absorbance of the test under different time and different wave length, determines adsorption curve figure at 600nm.The present invention has investigated different materials
Expect (Fig. 4) comparison in difference and Fe to Congo red solution absorption property3O4Oyster shell nanocomposite inhales Congo red solution
Attached kinetic model.The result shows that nanocomposite of the invention has efficient absorption property.
Embodiment 2
0.5g ferric chloride hexahydrates are added in 20mL water and are stirred, 0.1g citric acids, 1mL ethylenediamines is separately added into, stirs
It mixes until being completely dissolved, adds 0.5g sodium hydroxides and stir evenly, finally add 0.1g oyster shell powders.Above-mentioned suspension is turned
It moves in autoclave, reaction kettle is then placed in 100 DEG C of holding 12h in baking oven.Product after hydro-thermal passes through magnet point
From being washed using distilled water and ethyl alcohol.Vacuum drying oven drying is finally placed to get to the Fe3O4Oyster shell nanometer is multiple
Condensation material.
Embodiment 3
1.0g ferric chloride hexahydrates are added in 20mL water and are stirred, 0.1g citric acids, 1mL ethylenediamines is separately added into, stirs
It mixes until being completely dissolved, adds 0.5g sodium hydroxides and stir evenly, finally add 0.1g oyster shell powders.Above-mentioned suspension is turned
It moves in autoclave, reaction kettle is then placed in 100 DEG C of holding 12h in baking oven.Product after hydro-thermal passes through magnet point
From being washed using distilled water and ethyl alcohol.Vacuum drying oven drying is finally placed to get to the Fe3O4Oyster shell nanometer is multiple
Condensation material.
Embodiment 4
1.5g ferric chloride hexahydrates are added in 20mL water and are stirred, 0.1g citric acids, 1mL ethylenediamines is separately added into, stirs
It mixes until being completely dissolved, adds 0.5g sodium hydroxides and stir evenly, finally add 0.1g oyster shell powders.Above-mentioned suspension is turned
It moves in autoclave, reaction kettle is then placed in 100 DEG C of holding 12h in baking oven.Product after hydro-thermal passes through magnet point
From being washed using distilled water and ethyl alcohol.Vacuum drying oven drying is finally placed to get to the Fe3O4Oyster shell nanometer is multiple
Condensation material.
Embodiment 5
1.5g ferric chloride hexahydrates are added in 20mL water and are stirred, 0.1g citric acids, 1mL ethylenediamines is separately added into, stirs
It mixes until being completely dissolved, adds 0.5g sodium hydroxides and stir evenly, finally add 0.1g oyster shell powders.Above-mentioned suspension is turned
It moves in autoclave, reaction kettle is then placed in 150 DEG C of holding 12h in baking oven.Product after hydro-thermal passes through magnet point
From being washed using distilled water and ethyl alcohol.Vacuum drying oven drying is finally placed to get to the Fe3O4Oyster shell nanometer is multiple
Condensation material.
Embodiment 6
1.5g ferric chloride hexahydrates are added in 20mL water and are stirred, 0.1g citric acids, 1mL ethylenediamines is separately added into, stirs
It mixes until being completely dissolved, adds 0.5g sodium hydroxides and stir evenly, finally add 0.1g oyster shell powders.Above-mentioned suspension is turned
It moves in autoclave, reaction kettle is then placed in 180 DEG C of holding 12h in baking oven.Product after hydro-thermal passes through magnet point
From being washed using distilled water and ethyl alcohol.Vacuum drying oven drying is finally placed to get to the Fe3O4Oyster shell nanometer is multiple
Condensation material.
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, it should all belong to the covering scope of the present invention.
Claims (6)
1. a kind of nano-magnetic powder body material preparation method and application based on oyster shell, which is characterized in that include the following steps：
(1) by a certain amount of FeCl3·6H2O is added in the deionized water of 20mL, stirring to dissolving；
(2) a certain amount of citric acid and ethylenediamine are added in step (1) acquired solution, stirring is to being completely dissolved；
(3) a certain amount of sodium hydroxide is added in step (2) acquired solution, is stirred evenly, is eventually adding a certain amount of male
Oyster shells；
(4) above-mentioned gained suspension is transferred in autoclave, then reaction kettle is transferred in baking oven under certain temperature
It is kept for 12 hours；
(5) products therefrom is detached by magnet, is washed through a certain amount of distilled water and ethyl alcohol, be finally transferred to vacuum drying oven drying
Obtain powder sample.A certain amount of powder sample is taken to handle waste water.
2. a kind of nano-magnetic powder body material preparation method and application based on oyster shell according to claim 1, special
Sign is step (1) described FeCl3·6H2The quality of O is 0.1~5.0g.
3. a kind of nano-magnetic powder body material preparation method and application based on oyster shell according to claim 1, special
Sign is that step (2) the citric acid quality is 0.1~10g, and ethylenediamine volume is 0.1~10mL.
4. a kind of nano-magnetic powder body material preparation method and application based on oyster shell according to claim 1, special
Sign is that the quality of step (3) described sodium hydroxide is 0.1~2.0g, and the quality of oyster shell powder is 0.01~0.5g.
5. a kind of nano-magnetic powder body material preparation method and application based on oyster shell according to claim 1, special
Sign is that step (4) described hydrothermal temperature is 80~200 DEG C.
6. a kind of a kind of nano-magnetic powder body material preparation method and application based on oyster shell as described in claim 1,
It is characterized in that the nano-magnetic powder concentration described in step (5) is 1-50mg/mL, waste water is congo red, a concentration of 50-
150mg/L。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN109999752A (en) * | 2019-03-12 | 2019-07-12 | 农业部沼气科学研究所 | A kind of preparation method and application of the multifunctional material of efficient absorption and degradable organic pollutant |
| CN110013834A (en) * | 2019-04-30 | 2019-07-16 | 广东海洋大学 | A kind of chemical modification oyster shell adsorbent and its method for removing Mercury in Water Body ion |
| CN111018210A (en) * | 2020-01-16 | 2020-04-17 | 安阳师范学院 | Treatment method of organic dye wastewater |
| CN111821951A (en) * | 2020-07-06 | 2020-10-27 | 杭州电子科技大学 | Recyclable nitrogen and phosphorus synchronous adsorbent and preparation method and application thereof |
| CN114849663A (en) * | 2022-03-30 | 2022-08-05 | 天津万象恒远科技有限公司 | Oyster shell powder and preparation method and application thereof |
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|---|---|---|---|---|
| CN109999752A (en) * | 2019-03-12 | 2019-07-12 | 农业部沼气科学研究所 | A kind of preparation method and application of the multifunctional material of efficient absorption and degradable organic pollutant |
| CN109999752B (en) * | 2019-03-12 | 2022-05-27 | 农业部沼气科学研究所 | Preparation method and application of multifunctional material for efficiently adsorbing and degrading organic pollutants |
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| CN110013834A (en) * | 2019-04-30 | 2019-07-16 | 广东海洋大学 | A kind of chemical modification oyster shell adsorbent and its method for removing Mercury in Water Body ion |
| CN111018210A (en) * | 2020-01-16 | 2020-04-17 | 安阳师范学院 | Treatment method of organic dye wastewater |
| CN111821951A (en) * | 2020-07-06 | 2020-10-27 | 杭州电子科技大学 | Recyclable nitrogen and phosphorus synchronous adsorbent and preparation method and application thereof |
| CN111821951B (en) * | 2020-07-06 | 2023-04-28 | 杭州电子科技大学 | Recoverable nitrogen-phosphorus synchronous adsorbent and preparation method and application thereof |
| CN114849663A (en) * | 2022-03-30 | 2022-08-05 | 天津万象恒远科技有限公司 | Oyster shell powder and preparation method and application thereof |
| CN114849663B (en) * | 2022-03-30 | 2024-05-28 | 天津万象恒远科技有限公司 | Oyster shell powder and preparation method and application thereof |
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