CN108160025A - A kind of preparation method and application of oyster shell powder ferric oxide nano composite material - Google Patents
A kind of preparation method and application of oyster shell powder ferric oxide nano composite material Download PDFInfo
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- CN108160025A CN108160025A CN201711018557.8A CN201711018557A CN108160025A CN 108160025 A CN108160025 A CN 108160025A CN 201711018557 A CN201711018557 A CN 201711018557A CN 108160025 A CN108160025 A CN 108160025A
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- oyster shell
- shell powder
- composite material
- nano composite
- ferric oxide
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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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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
- B01J20/06—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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- 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
- B01J20/28002—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
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
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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
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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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2101/38—Organic compounds containing nitrogen
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a kind of preparation method of oyster shell powder ferric oxide nano composite material, step is：First, discarded oyster shell dilute hydrochloric acid is impregnated certain time, pickling removal surface is organic and inorganic impurity, is put into oven drying after being cleaned with distilled water, smashes it through 80 300 mesh sieve, obtain oyster shell powder；2nd, shell powder is placed in a concentration of 0.01 1.00 mol L, 1 iron nitrate solutions, it stirs after impregnating 3 24 h, filtration drying, 2 10 h is calcined at 800-1100 DEG C, oyster shell powder ferric oxide nano composite material is obtained, material preparation method is stable, reliable, simple and practicable；Oyster shell powder ferric oxide nano composite material is used for the processing of azo dye wastewater, azo dyes to have good Adsorption ability.
Description
Technical field
The present invention relates to the preparation method for preparing a kind of nanocomposite and its for handling azo dye wastewater application
Technical field, specially a kind of preparation method and application of oyster shell powder ferric oxide nano composite material.
Background technology
Dyestuff is widely used in the industries such as printing and dyeing, foods and cosmetics, according to statistics result, and the dyes of commercial use is
More than 100,000 kinds, China is DYE PRODUCTION big country, and textile dyestuff industry is fast-developing in recent years, at present the various dyestuff productions in China
For amount up to 900,000 tons, dyestuff yield accounts for 60% of the world or so.The production of azo dyes and usage amount are maximum in all dyestuffs
, certain azo dyes are it is verified that can result in cancer, and particularly in the degradation process of azo dyes, the mechanism of degradation is very
Be likely to be and be first broken azo group, generate the toxicity bigger of aniline category matter and the substance, thus azo dyes in production and
It can be discharged into environment during use, very serious pollution caused to environment, difficulty of governance is very big.
At present, absorption method is to handle a kind of method being most widely used in waste water from dyestuff method.Industrial common suction
Attached dose of active charcoal, activated silica diatomaceous earth, flyash etc..But due to waiting various factors there are of high cost, them are constrained in work
Application in the production of industry metaplasia.
China's shellfish culture yield accounts for sea-farming total output nearly 80%, and in shellfish culture based on oyster culture,
Therefore oyster culture yield is very big.Since oyster shell added value is low, the overwhelming majority is discarded in seabeach, roadside, causes oyster
Shell pollutes.The nanocomposite that oyster shell is made of calcium carbonate and large biological molecule, organic matter is waved after high-temperature calcination
Hair is so as to form porous structure, it shows organic matter certain adsorption capacity, but this suction-operated is essentially from Ca
(II) to Electrostatic Absorption of the organic matter containing groups such as N or O, adsorption capacity is weaker, limits its processing in waste water etc.
Using.Therefore, performance improvement is carried out to it, improves its absorption property and be of great significance and value.
By adding in transition metal before oyster shell powder high-temperature calcination, it can not only change the shape of calcined product calcium oxide
Looks, and metal oxide composite can be formed, change binding ability of the material to organic matter, so as to improve material to having
The absorption property of machine object can be used for the adsorption treatment agent of waste water from dyestuff as a kind of more excellent adsorbent.
Invention content
It is obtained it is an object of the present invention to provide a kind of preparation method of oyster shell powder ferric oxide nano composite material and by this method
Material be applied to the processing of azo dye wastewater, the material preparation method is stable, reliable, simple and practicable.
The specific preparation method of oyster shell powder ferric oxide nano composite material is as follows:
First, the preparation of composite material precursor powder is received:
Discarded oyster shell dilute hydrochloric acid is impregnated certain time, pickling removal surface is organic and inorganic impurity, is washed with distillation
Oven drying is put into after net, 80-300 mesh sieve is smashed it through, obtains oyster shell powder.
2nd, the preparation of oyster shell powder ferric oxide nano composite material:
Shell powder is placed in a concentration of 0.01-1.00 mol L-1In iron nitrate solution, after 3-24 h are impregnated in stirring, filtration drying,
2-10 h are calcined at 800-1100 DEG C, obtain oyster shell powder ferric oxide nano composite material.
Oyster shell powder ferric oxide nano composite material prepared by the present invention is used for the processing of azo dye wastewater, to azo
Dyestuff has good Adsorption ability.
Advantageous effect of the present invention：
(1) oyster shell is prepared into oyster shell powder, is stirred for being immersed in certain density iron nitrate solution, oyster shell powder surface
Iron ion that can be more effectively in adsorbent solution, by selecting the concentration of appropriate iron nitrate solution and oyster shell whiting and iron nitrate solution
Ratio and calcination temperature, can control oyster shell powder absorption iron ion number, obtain Fe, Ca two oxides ratio difference
Nanocomposite..
(2) oyster shell powder nanocomposite preparation method of the present invention is simple, easily controllable, suitable for industrialized production and
Using.
(3) the oyster shell powder ferric oxide nano composite material prepared has excellent absorption property, available for handling
The waste water of azo dyes.
Description of the drawings
Fig. 1 is the X-ray diffractogram of nanocomposite prepared by embodiment 1
Fig. 2 is the scanning electron microscope (SEM) photograph of nanocomposite prepared by embodiment 1.
Fig. 3 is the oyster shell powder ferric oxide nano composite material absorption methyl orange activity figure of embodiment 5.
Fig. 4 is the Congo red activity figure of oyster shell powder ferric oxide nano composite material absorption of embodiment 6.
Specific embodiment
Embodiment 1
First, the preparation of composite material precursor powder is received：
The oyster shell powder for crossing 100 mesh is soaked in 0.15 mol L-1Iron nitrate solution（The solid-liquid ratio of powder and solution（g:
mL）It is 1:4）In, it is stirred at room temperature and impregnates 12 h, filtering drying obtains nanocomposite precursor powder.
2nd, the preparation of composite material：
Above-mentioned nanocomposite precursor powder is put into crucible to be placed in high temperature furnace, 900 are warming up to the speed of 300 DEG C/h
DEG C heat preservation 6 h carry out calcination reaction, after the completion of reaction, taken out after cooled to room temperature, obtain oyster shell powder ferric oxide nano
Composite material.
Embodiment 2
First, the preparation of nanocomposite precursor powder：
The oyster shell powder for crossing 100 mesh is soaked in 0.10 mol L-1Iron nitrate solution（The solid-liquid ratio of powder and solution（g:
mL）To be 1:4）In, it is stirred at room temperature and impregnates 12 h, filtering drying obtains nanocomposite precursor powder.
2nd, the preparation of nanocomposite：
Above-mentioned nanocomposite precursor powder is put into crucible to be placed in high temperature furnace, 900 are warming up to the speed of 300 DEG C/h
DEG C heat preservation 6 h carry out calcination reaction, after the completion of reaction, taken out after cooled to room temperature, obtain oyster shell powder ferric oxide nano
Composite material.
Embodiment 3
First, the preparation of nano composite material precursor powder：
The oyster shell powder for crossing 100 mesh is soaked in 0.05 mol L-1Iron nitrate solution（The solid-liquid ratio of powder and solution（g:
mL）To be 1:4）In, it is stirred at room temperature and impregnates 12 h, filtering drying obtains nanocomposite precursor powder.
2nd, the preparation of nano composite material：
Above-mentioned nanocomposite precursor powder is put into crucible to be placed in high temperature furnace, 900 are warming up to the speed of 300 DEG C/h
DEG C heat preservation 6h carry out calcination reaction, after the completion of reaction, taken out after cooled to room temperature, obtain oyster shell powder ferric oxide nano and answer
Condensation material.
Embodiment 4
First, the preparation of nano composite material precursor powder：
The oyster shell powder for crossing 100 mesh is soaked in 0.01 mol L-1Iron nitrate solution（The solid-liquid ratio of powder and solution（g:
mL）To be 1:4）In, it is stirred at room temperature and impregnates 12 h, filtering drying obtains nanocomposite precursor powder.
2nd, the preparation of nano composite material：
Above-mentioned nanocomposite precursor powder is put into crucible to be placed in high temperature furnace, 900 are warming up to the speed of 300 DEG C/h
DEG C heat preservation 6h carry out calcination reaction, after the completion of reaction, taken out after cooled to room temperature, obtain oyster shell powder ferric oxide nano and answer
Condensation material.
Embodiment 5：
With 30 mgL-125 mL of methyl orange simulated wastewater is dye wastewater treatment object, is made with 0.01-0.06g embodiments 1
Standby nanocomposite is inorganic agent, and the stir process Methyl Orange in Wastewater at 30 DEG C takes methyl orange solution to carry out ultraviolet ~ visible
Spectrum analysis determines that MO concentration changes in degradation process, by 2 h stirrings, the static suctions of 2h according to light absorption value at sample 464nm
Attached processing, the removal rate of methyl orange is 96.5% during 0.05g inorganic agent dosages.
Embodiment 6：
With 50 mgL-1Congo red 30 mL of simulated wastewater is dye wastewater treatment object, is made with 0.01-0.06g embodiments 3
Standby nanocomposite is inorganic agent, and the Congo red waste water of stir process at 30 DEG C takes Congo red solution to carry out ultraviolet ~ visible
Spectrum analysis determines that MO concentration changes in degradation process, stirs, the static suctions of 1h by 1h according to light absorption value at sample 498nm
Attached processing, during 0.06g inorganic agent dosages, Congo red removal rate is 97.5%.The substantially former of the present invention has been shown and described above
Reason and main feature and advantages of the present invention, it is obvious to a person skilled in the art that the present invention is not limited to above-mentioned demonstrations
The details of embodiment, and without departing from the spirit or essential characteristics of the present invention, it can be in other specific forms
Realize the present invention.Therefore, in all respects, the present embodiments are to be considered as illustrative and not restrictive,
The scope of the invention being indicated by the appended claims rather than by the foregoing description, it is intended that will fall in the equivalent requirements of the claims
Meaning and scope in all changes be included within the present invention.Any reference numeral in claim should not be considered as limitation
Involved claim.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in each embodiment can also be properly combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (2)
1. a kind of preparation method of oyster shell powder ferric oxide nano composite material, which is characterized in that its step is：
First, the preparation of composite material precursor powder is received:Discarded oyster shell dilute hydrochloric acid is impregnated certain time, pickling removal
Surface is organic and inorganic impurity, is put into oven drying after being cleaned with distilled water, smashes it through 80-300 mesh sieve, obtain oyster shell
Powder；
2nd, the preparation of oyster shell powder ferric oxide nano composite material:Shell powder is placed in a concentration of 0.01-1.00 mol L-1 nitric acid
It in ferrous solution, stirs after impregnating 3-24 h, filtration drying, 2-10 h is calcined at 800-1100 DEG C, obtain oyster shell powder iron oxide
Nanocomposite.
2. by oyster shell powder made from a kind of preparation method of oyster shell powder ferric oxide nano composite material described in claim 1
Ferric oxide nano composite material is used for the processing of azo dye wastewater, and azo dyes have good Adsorption ability.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711018557.8A CN108160025A (en) | 2017-10-27 | 2017-10-27 | A kind of preparation method and application of oyster shell powder ferric oxide nano composite material |
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| CN201711018557.8A CN108160025A (en) | 2017-10-27 | 2017-10-27 | A kind of preparation method and application of oyster shell powder ferric oxide nano composite material |
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| CN108160025A true CN108160025A (en) | 2018-06-15 |
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| CN201711018557.8A Withdrawn CN108160025A (en) | 2017-10-27 | 2017-10-27 | A kind of preparation method and application of oyster shell powder ferric oxide nano composite material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109502815A (en) * | 2018-12-11 | 2019-03-22 | 天津大学 | A kind of environmentally friendly oyster shell water filter of outdoor portable |
| 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 |
| CN111018210A (en) * | 2020-01-16 | 2020-04-17 | 安阳师范学院 | Treatment method of organic dye wastewater |
| CN111607315A (en) * | 2020-06-30 | 2020-09-01 | 江苏达美瑞新材料有限公司 | Production process of high-wear-resistance polyester resin powder coating |
| CN113000012A (en) * | 2021-03-18 | 2021-06-22 | 大连理工大学 | Arsenic removal adsorption material, preparation method thereof and application of arsenic removal adsorption material in removal of As (III) in acidic wastewater |
-
2017
- 2017-10-27 CN CN201711018557.8A patent/CN108160025A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109502815A (en) * | 2018-12-11 | 2019-03-22 | 天津大学 | A kind of environmentally friendly oyster shell water filter of outdoor portable |
| 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 |
| CN111018210A (en) * | 2020-01-16 | 2020-04-17 | 安阳师范学院 | Treatment method of organic dye wastewater |
| CN111607315A (en) * | 2020-06-30 | 2020-09-01 | 江苏达美瑞新材料有限公司 | Production process of high-wear-resistance polyester resin powder coating |
| CN113000012A (en) * | 2021-03-18 | 2021-06-22 | 大连理工大学 | Arsenic removal adsorption material, preparation method thereof and application of arsenic removal adsorption material in removal of As (III) in acidic wastewater |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
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 Nathon new Mstar Technology Ltd |
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| SE01 | Entry into force of request for substantive examination | ||
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| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180615 |