CN109261121A - Fe is prepared by one step of solid sintering technology using discarded peanut shell and iron rust3O4The method of/C magnetic composite - Google Patents
Fe is prepared by one step of solid sintering technology using discarded peanut shell and iron rust3O4The method of/C magnetic composite Download PDFInfo
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- CN109261121A CN109261121A CN201811083962.2A CN201811083962A CN109261121A CN 109261121 A CN109261121 A CN 109261121A CN 201811083962 A CN201811083962 A CN 201811083962A CN 109261121 A CN109261121 A CN 109261121A
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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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- 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
- B01J20/28009—Magnetic properties
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3021—Milling, crushing or grinding
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3071—Washing or leaching
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
Fe is prepared by one step of solid sintering technology using discarded peanut shell and iron rust the invention discloses a kind of3O4The method of/C magnetic composite, belongs to the synthesis technical field of composite functional material.Technical solution of the present invention main points are as follows: grind peanut shell and iron rust after over cleaning, drying process respectively, again by the ratio mixed grinding 1-2h of peanut shell powder and iron rust powder 1:2 in mass ratio after grinding, it is 3%H that the mixed powder after taking grinding, which is placed in the percentage by volume that flow is 10mL/min,2In the sintering furnace of/97%Ar reducing atmosphere, 550 DEG C are warming up to the heating rate of 5 DEG C/min and keeps the temperature 30min, then cools to room temperature to obtain Fe3O4/ C magnetic composite.Fe obtained by the present invention3O4The excellent significant effect in terms of Dye Adsorption of/C magnetic composite structure, and separation can be facilitated under magnetic field, it is reusable.On the other hand the condition and instrument needed for testing are simple and easy to get, it can be achieved that big batch metaplasia produces.
Description
Technical field
The invention belongs to the synthesis technical fields of composite functional material, and in particular to a kind of to utilize discarded peanut shell and iron rust
Fe is prepared by one step of solid sintering technology3O4The method of/C magnetic composite.
Background technique
With technologically developing, level of agricultural production is more and more flourishing, and agricultural wastes are used as fuel and fertilizer side by people
Face is fewer and fewer, if agricultural wastes will serious ground contamination environment without appropriate processing.On the other hand, iron is still the world
Upper production and the most metal of usage amount, but iron gets rusty easily in a humidity environment, there is a few kiloton daily in the world
Steel becomes scrap iron, and iron rust usually simply uses chemical formula Fe2O3·xH2O is indicated.Discarded biomaterial flower is used in the present invention
Rawhide passes through solid sintering technology one-step synthesis Fe together as raw material as carbon source and iron rust3O4/ C magnetic composite, no
But the recycling of resource is realized, or a kind of environmentally protective method.
Fe3O4/ C magnetic composite has very big potential in numerous sciemtifec and technical spheres such as chemistry, material, physics, in lithium electricity
Pond, pharmaceutical carrier, microwave absorption and Dye Adsorption etc. are studied more and more, and important role is play[1-8].In addition,
Fe3O4/ C magnetic composite is nano-scale, there is the diffusion length more shorter than solid and a bigger surface area materials, and magnetic
Property is conveniently separated it by the magnetic field of application, shows good recuperability, may be implemented to reuse,
Application effect in terms of Dye Adsorption is significant.Conventional preparation Fe at present3O4The method of/C magnetic composite mainly uses hydro-thermal
Synthetic method, the catalytic pyrolysis of polymer synthesize Fe3O4/ C magnetic composite, these preparation methods can also obtain target
Fe3O4/ C magnetic composite, but since step is more, period longer hinder amplifies production and large-scale application.Therefore,
A kind of method that raw material is environmentally friendly, production line is simple and effective how is developed, preparation Fe is become3O4/ C magnetic composite it is main
Target, at the same accomplish save cost of material, guarantee drug purity, it is green non-poisonous be research direction of the invention.
Bibliography:
[1] J H Zhang, B Yan, S Wan, et al. Converting Polyethylene Waste into
Large Scale One-Dimensional Fe3O4@C Composites by a Facile One-Pot Process
[J]. ACS Publications, 2013, 52:5708-5712。
[2] C G Han, N Sheng, C Y Zhu, et al. Cotton-assisted combustion
synthesis of Fe3O4/C composites as excellent anode materials for lithium-ion
batteries [J]. Materials Today Energy, 2017, 5:187-195。
[3] X Y Fan, S H Li, H H Zhou, et al. One-pot high temperature
hydrothermal synthesis of Fe3O4@C/graphene nanocomposite as anode for high
rate lithium ion battery [J]. Electrochimica Acta, 2015, 180:1041-1049。
[4] Z Yang, D Y Su, J P Yang, et al. Fe3O4/C composite with hollow
spheres in porous 3D-nanostructure as anode material for the lithium-ion
batteries [J]. Journal of Power Sources, 2017, 363:161-167。
[5] L Cheng, W M Ruan, B F Zou, et al. Chemical template-assisted
synthesis of monodisperse rattle-type Fe3O4@C hollow microspheres as drug
carrier [J]. Acta Biomaterialia, 2017, 58:432-441。
[6] L Liang, Q C Zhu, T B Wang, et al. The synthesis of core–shell Fe
3 O 4 @mesoporous carbon in acidic medium and its efficient removal of dye
[J]. Microporous and Mesoporous Materials, 2014, 197:221-228。
[7] Zhang Yanqi carbon-coated magnetic material Fe3O4The synthesis of/C/Pd (0) and its catalytic performance study the Anhui [J]
Technical college journal, 2013,27 (6): 48-56.
[8] Ben Xiaodong, neat pioneer, Liu Chengmao wait the hud typed Fe of3O4The solvent-thermal method of/C nano particle is prepared and its micro-
Wave absorbent properties [J] Materials Science and Engineering journal, 2014,32 (3): 436-464.
Summary of the invention
Be easy to get the technical problem to be solved by the present invention is to provide a kind of raw material and it is low-cost using discarded peanut shell and
Iron rust prepares Fe by one step of solid sintering technology3O4The method of/C magnetic composite, this method is with obsolete material peanut shell and iron
Rust is used as raw material, and the powder after the two is ground respectively remixes grinding, the method that mixed-powder is then passed through solid-phase sintering
Fe can simply and easily be made3O4/ C magnetic composite, Fe made from this method3O4/ C magnetic composite epigranular
And structure is excellent.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, passes through solid phase using discarded peanut shell and iron rust
One step of sintering process prepares Fe3O4The method of/C magnetic composite, it is characterised in that specific steps are as follows: by peanut shell and iron rust point
Do not ground after over cleaning, drying process, then by after grinding peanut shell powder and the iron rust powder ratio of 1:2 in mass ratio mix
Grinding 1-2h is closed, it is 3%H that the mixed powder after taking grinding, which is placed in the percentage by volume that flow is 10mL/min,2/ 97%Ar reduction
In the sintering furnace of atmosphere, 550 DEG C are warming up to the heating rate of 5 DEG C/min and keeps the temperature 30min, then cools to room temperature to obtain
Fe3O4/ C magnetic composite.
Fe of the present invention3O4Application of/C the magnetic composite in the organic congo red waste water of adsorption cleaning.
Compared with the prior art, the invention has the following beneficial effects:
1, operation of the present invention process is simply environmentally protective, and the raw material used is obsolete material, and raw material has at low cost, easy acquisition
The advantages that；
2, experiment condition of the invention is easy to be made, and core operation is the raw material after mixed grinding carrying out solid-phase sintering,
Fe can be quickly and easily made in one step3O4/ C magnetic composite, preparation flow are simple, it can be achieved that the production of big batch metaplasia, system
The Fe obtained3O4/ C magnetic composite has magnetic and epigranular, and has very big specific surface area；
3, Fe produced by the present invention3O4/ C magnetic composite significant effect in terms of Dye Adsorption, adsorption rate are higher and almost
It is degradable, Fe can be realized by externally-applied magnetic field3O4The separation of/C magnetic composite has good recuperability and is easy to
Repetitive cycling uses.
Detailed description of the invention
Fig. 1 is that Fe is made in embodiment3O4The XRD diagram of/C magnetic composite；
A, b, c and d are that Fe is made in embodiment respectively in Fig. 23O4/ C magnetic composite SEM figure, TEM figure, HR-TEM figure and
SAED figure；
(a) and (b) is that Fe is made in embodiment respectively in Fig. 33O4/ C magnetic composite adsorbs the UV, visible light of Congo red solution
Spectrum and adsorption rate curve, wherein illustration is the comparison of absorption front and back in (a).
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment
Peanut shell is cleaned by ultrasonic clean and dry be placed in mortar and grinds 1h, iron rust is successively used into ethyl alcohol and distilled water
It cleans up and dries to be placed in mortar and grind 1h, then by the peanut shell powder and iron rust powder 1:2 in mass ratio after grinding
Ratio mixed grinding 1-2h, to be placed in the percentage by volume that flow is 10mL/min be 3%H to the mixed powder after taking grinding2/
In the sintering furnace of 97%Ar reducing atmosphere, 550 DEG C are warming up to the heating rate of 5 DEG C/min and keeps the temperature 30min, is subsequently cooled to
Room temperature obtains black powder Fe3O4/ C magnetic composite.
The corresponding XRD spectrum of black powder obtained above is as shown in Figure 1, all diffraction maximums in figure can refer to well
To Fe3O4Spinelle shape structure (PDF#65-3107), show to successfully synthesize Fe3O4, strong diffraction maximum shows Fe3O4Mutually have
Good crystallinity.However, the diffraction maximum of C is not detected in XRD spectrum, probably due to C layers of crystallinity is bad.
Fe3O4The characterization of/C magnetic composite: Fig. 2 (a) is that the SEM of gained black powder schemes, and shows the Fe of synthesis3O4/
C sample form is the spherical particle of uniform particle sizes' distribution, has coarse surface, average diameter is about 30nm.In order to observe sample
The microstructure of product carries out TEM characterization to sample, and Fig. 2 (b) is that the TEM of gained black powder schemes, can from figure in conjunction with Fig. 2 (a)
To find out Fe3O4/ C nano particle coated structure, the deeper part of color are Fe3O4, shallower part is amorphous C, Fe3O4?
Grain outer layer is wrapped up by a large amount of C.Fig. 3 (a) is that the HR-TEM of gained black powder schemes, and having the visible interplanar distance of figure is about 0.498
Nm, corresponding PDF card are (111) crystal face；Fig. 3 (b) is the SAED photo of gained black powder, and it is more that SAED pattern shows characteristic
Brilliant diffraction ring, again with face-centered cubic Fe3O4Phase matched well.These results show there are many Fe wherein3O4/ C receives
Rice compound particle.
With Fe obtained3O4/ C magnetic composite carries out adsorption experiment: Fe to Congo red solution3O4/ C magnetic coupling material
The usage amount of material is 2.3g/L, is carried out in ultrasonic cleaner, adsorbs the Congo red solution of 50mg/L within a certain period of time, right
The solution at 0min, 1min, 3min, 6min, 10min, 20min, 25min moment carries out uv-spectrogram analysis, adsorbs in 25min
For rate up to 97.57%, adsorption effect is shown in Fig. 3 (a), Fig. 3 (b).After experiment, Fe is recycled by the method for externally-applied magnetic field3O4/ C magnetic
Property composite material, and realize Fe3O4The repetitive cycling of/C magnetic composite uses.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. preparing Fe by one step of solid sintering technology using discarded peanut shell and iron rust3O4The method of/C magnetic composite, it is special
Sign is specific steps are as follows: grinds peanut shell and iron rust after over cleaning, drying process respectively, then by the peanut shell after grinding
The ratio mixed grinding 1-2h of powder and iron rust powder 1:2 in mass ratio, it is 10mL/ that the mixed powder after taking grinding, which is placed in flow,
The percentage by volume of min is 3%H2In the sintering furnace of/97%Ar reducing atmosphere, 550 DEG C are warming up to the heating rate of 5 DEG C/min
And 30min is kept the temperature, it then cools to room temperature to obtain Fe3O4/ C magnetic composite.
2. Fe made from the method according to claim 113O4/ C magnetic composite is in the organic congo red of adsorption cleaning
Application in waste water.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811083962.2A CN109261121A (en) | 2018-09-17 | 2018-09-17 | Fe is prepared by one step of solid sintering technology using discarded peanut shell and iron rust3O4The method of/C magnetic composite |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811083962.2A CN109261121A (en) | 2018-09-17 | 2018-09-17 | Fe is prepared by one step of solid sintering technology using discarded peanut shell and iron rust3O4The method of/C magnetic composite |
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| CN109261121A true CN109261121A (en) | 2019-01-25 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102623693A (en) * | 2012-04-13 | 2012-08-01 | 山东大学 | High specific capacity spindle-shaped ferroferric oxide/carbon nano composite material for negative electrode of lithium ion battery |
| CN102800858A (en) * | 2012-08-03 | 2012-11-28 | 浙江大学 | Preparation method and purpose for iron oxide-based anode material for lithium ion battery |
| CN104645330A (en) * | 2014-12-11 | 2015-05-27 | 高占虎 | Method for preparing iron-carbon composite magnetic carrier |
| CN106799208A (en) * | 2017-02-23 | 2017-06-06 | 黄淮学院 | A kind of biomass carbon carried magnetic material composite adsorbing material and preparation method thereof, application process |
-
2018
- 2018-09-17 CN CN201811083962.2A patent/CN109261121A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102623693A (en) * | 2012-04-13 | 2012-08-01 | 山东大学 | High specific capacity spindle-shaped ferroferric oxide/carbon nano composite material for negative electrode of lithium ion battery |
| CN102800858A (en) * | 2012-08-03 | 2012-11-28 | 浙江大学 | Preparation method and purpose for iron oxide-based anode material for lithium ion battery |
| CN104645330A (en) * | 2014-12-11 | 2015-05-27 | 高占虎 | Method for preparing iron-carbon composite magnetic carrier |
| CN106799208A (en) * | 2017-02-23 | 2017-06-06 | 黄淮学院 | A kind of biomass carbon carried magnetic material composite adsorbing material and preparation method thereof, application process |
Non-Patent Citations (2)
| Title |
|---|
| CHUN WANG ET AL.: "Magnetic Biomass Activated Carbon-Based Solid-Phase Extraction Coupled with High Performance Liquid Chromatography for the Determination of Phenylurea Herbicides in Bottled Rose Juice and Water Samples", 《FOOD ANAL. METHODS》 * |
| 九三学社江苏省委员会编: "《科技创新与促进江苏绿色制造发展》", 30 June 2016, 东南大学出版社 * |
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