CN106881059B - A kind of preparation method of iron/carbon composite - Google Patents
A kind of preparation method of iron/carbon composite Download PDFInfo
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- CN106881059B CN106881059B CN201710064168.2A CN201710064168A CN106881059B CN 106881059 B CN106881059 B CN 106881059B CN 201710064168 A CN201710064168 A CN 201710064168A CN 106881059 B CN106881059 B CN 106881059B
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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- 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
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
The present invention relates to field of material technology, specifically disclose a kind of preparation method of iron/carbon composite, and the present invention prepares iron/carbon composite using the method that hydro-thermal method-co-precipitation-galvanoplastic combine for the first time.Synthesis process can be analyzed to two steps: firstly, the organic matter raw material added with molysite is carbonized using hydro-thermal method；Second, product after carbonization is restored using reducing agent appropriate, to obtain required iron/carbon composite.Mainly with the fixed surface and inside for being present in porous carbon materials of zeroth order Iron activiation, carbon material serves not only as the substrate of load Zero-valent Iron but also plays a certain protective role to Zero-valent Iron ferro element in the iron/carbon material obtained using this method.Therefore, the composite material of synthesis had both had the good reducing power of Zero-valent Iron, it may have carbon material is to the good adsorption capacity of organic pollutant, to realize the more efficient removal of organic pollutants.
Description
Technical field
The present invention relates to field of material technology, are to be related to a kind of iron/carbon composite more specifically.
Background technique
Iron/carbon composite is a kind of widely used, new material for haveing excellent performance, is widely used in photocatalysis material
The fields such as material, electrode material, sensor, sewage treatment.Currently, the synthetic method of the material mainly have arc process, ion beam method,
Laser method, chemical vapour deposition technique, high-temperature heat treatment method and Low Temperature Thermal solution.Difference can be synthesized using these preparation methods
Iron/carbon composite of particle size, different shape.But these generally existing costs of iron/carbon composite synthetic method
The disadvantages of high, complicated for operation.Such as: arc process needs special arc discharge device and pure raw material, but the production obtained
Produce amount is seldom；Chemical vapour deposition technique needs to use special experimental provision and synthesis takes a long time；High-temperature heat treatment method
At least 1500 DEG C or more of high temperature is needed, therefore not only energy consumption is high, time-consuming but also more demanding to laboratory apparatus.
In order to solve the above technical problems, the present invention comes therefrom.
Summary of the invention
Invention to be designed to provide a kind of raw material sources extensive, it is at low cost, be suitble to iron/carbon composite wood of large-scale promotion
Material and preparation method thereof, iron/carbon composite of synthesis can be used for removing environmental contaminants.
In order to solve these problems in currently available technology, the technical solution that first aspect present invention provides is a kind of
Iron/carbon composite preparation method comprising following steps:
(1) hydro-thermal method carbonization raw material
It chooses organic carbon source and dissolubility trivalent iron salt is source of iron, after organic carbon source cleaning pretreatment, by carbon ferro element
Organic carbon source and source of iron are added in reaction kettle than the ratio for 10:1-20:1, and suitable water is added by organic carbon source and iron
Source is sufficiently mixed, and under certain temperature and time, obtains carbonized product；
(2) co-precipitation-galvanoplastic reduction step (1) product
Carbonized product obtained in step (1) is cleaned with water, and is scattered in water phase, then addition and ferro element
The reducing agent of the amount of equal substances, stands a period of time；
(3) separation of iron/carbon composite and post-processing
Product obtained in step (2) is separated by solid-liquid separation, solid product is washed with water, is then dried in vacuo, finally
Obtain iron/carbon composite.
Preferably, organic carbon source is selected from carbohydrate, and further, organic carbon source is selected from monosaccharide or polysaccharide, further, described to have
Machine carbon source is selected from glucose or rice husk agricultural organic waste or its mixing.
Preferably, the dissolubility trivalent iron salt is selected from ferric nitrate, ferric sulfate, iron chloride.
Preferably, in step (1), reaction kettle is placed in steel kettle, heating reaction is carried out.
Preferably, in step (1), well-mixed organic carbon source and source of iron are in 160-220 DEG C of temperature, reaction time 8-18
Under the conditions of hour, carbonized product is finally obtained.
Preferably, the reducing agent in step (2) is selected from sodium borohydride.
Preferably, in step (2) at room temperature, the reduction with the amount of the substances such as ferro element is slowly added dropwise while stirring
Agent.
Preferably, vacuum drying is 8-24 hours dry at 60 DEG C of vacuum oven in the step (3).
A kind of preparation method of iron/carbon composite provided by the invention comprising following steps:
(1) hydro-thermal method carbonization raw material
Suitable carbon source and source of iron are selected first.It can use the agriculture organic waste such as the Organic Ingredients such as glucose or rice husk
Object is carbon material, is source of iron with dissolubility trivalent iron salt.After carbon source cleaning pretreatment, (carbon is mixed with source of iron according to a certain percentage
Ferro element ratio is 10:1-20:1), it then feeds the mixture into reaction kettle, and suitable water is added and is sufficiently mixed, it will be anti-
Answer temperature control at 180 DEG C or so, the reaction time is 8-18 hours；
(2) co-precipitation-galvanoplastic reduction step (1) product
Carbonized product obtained in step (1) is cleaned with water and is scattered in water phase, side is stirred at room temperature
Mix side be slowly added to the reducing agent of the amount of the substances such as ferro element (sodium borohydride, NaBH4), be then allowed to stand about 0.5-2 hours；
(3) separation of iron/carbon composite and post-processing
Product obtained in step (2) is separated by solid-liquid separation, solid product is cleaned multiple times with water remaining to remove
Reactant is then placed in vacuum oven, at least 8 hours dry at a temperature of 60 DEG C, and iron/carbon composite can be obtained.
The present invention prepares iron/carbon composite using the method that hydro-thermal method-co-precipitation-galvanoplastic combine for the first time.It closes
It can be analyzed to two steps at process: firstly, the organic matter raw material added with molysite is carbonized using hydro-thermal method；Second,
Product after carbonization is restored using reducing agent appropriate, to obtain required material.
Present invention mainly discloses a kind of inexpensive, simple and practical and environmentally friendly iron/carbon composite preparation methods.
Compared with traditional one-step method for synthesizing, the present invention in preparation method be divided into two steps progress, the reaction temperature needed it is lower and
It is easy to operate.The first step uses hydrothermal synthesis method, and reaction temperature is only about 180 DEG C.Co-precipitation-electroplating reaction in second step exists
It carries out at room temperature, therefore not only reduces operation energy consumption and reduce the risk of operation.In addition, this method can be adapted for
Starch, carbohydrate, cellulose and the gas chromatography raw material (including abandoned biomass) containing these substances, can significantly reduce original
Material cost even may be implemented to turn waste into wealth, these all significantly improve the economic and technical feasibility of large-scale industrial production, ring
Border friendly and sustainability.
Ferro element is mainly present in porous carbon with the fixation of zeroth order Iron activiation in the iron/carbon material obtained using this method
The surface and inside of material, carbon material serve not only as the substrate of load Zero-valent Iron but also play certain protection work to Zero-valent Iron
With.Therefore, the composite material of synthesis had both had the good reducing power of Zero-valent Iron, it may have carbon material is good to organic pollutant
Adsorption capacity, to realize the more efficient removal of organic pollutants.While ferro element of its load is during the reaction
It can be released slowly, therefore not will cause the waste of ferro element and form a large amount of iron cements.Finally, the method for the present invention will be utilized
Iron/carbon composite of synthesis is applied in Fenton advanced oxidation system, to achieve the purpose that efficiently to remove pollutant in water body.
Detailed description of the invention
Fig. 1 is the flow chart of preparation method of the present invention.
Fig. 2 is iron/carbon composite of preparation method of the present invention synthesis.Fig. 2 (a) is the material synthesized with rice husk as carbon source
Material, Fig. 2 (b) are the material that carbon source synthesis is made of glucose.
Fig. 3 (a, b) is shown using glucose as iron/carbon composite scanning electron microscope (SEM) phenogram of carbon source.
Fig. 4 shows the iron/carbon composite synthesized using different carbon source ferrous ion (Fe at different pH2+) dissolution feelings
Condition.
Fig. 5 shows the effect based on iron/carbon composite Fenton process removal sulfamethazine.
Specific embodiment
Above scheme is described further below in conjunction with specific embodiment.It should be understood that these embodiments are for illustrating
The present invention and be not limited to limit the scope of the invention.Implementation condition used in the examples can be done according to the condition of specific producer
Further adjustment, the implementation condition being not specified is usually the condition in routine experiment.
It introduces and summarizes
The present invention by way of example rather than provide the mode of limitation to be illustrated.It should be noted that in present disclosure
" one " or "an" embodiment is not necessarily referring to same specific embodiment, and refers at least a kind of.
Various aspects of the invention are described below.However, as will be readily apparent to one of skill in the art, it can
Only some or all of aspects according to the present invention implement the present invention.For purposes of illustration, provide herein specific number, material and
Configuration, enables one to thoroughly understand the present invention.However, those of skill in the art are evident that,
The present invention is without concrete details, that is, implementable.In other examples, many institutes have been omitted or simplified not make the present invention obscure
Known feature.
Various operations are successively described as multiple discrete steps, and with the side of the invention most helpful in understanding
Formula illustrates；However, in-order description should not be construed as to imply that these operations are necessarily dependent on sequence.
It will illustrate various embodiments according to the reactant of type species.Those of skill in the art will be shown and
It is clear to, any number of different types of reactant can be used to implement for the present invention, and be more than those for the purpose of illustration
And the reactant provided herein.In addition, also it is evident that, the invention is not limited to any specific mixing to show
Example.
1 iron of embodiment/carbon composite preparation method
(1), hydro-thermal method carbonization organic matter
The rice husk for taking 2g carries out the impurity that removal surface is cleaned multiple times with water, then dries at 60 DEG C or so；It will be by pre-
The raw material of processing is added in the polytetrafluoroethylene (PTFE) autoclave that dischargeable capacity is 25mL, while the nitric acid of 0.005mol is added
Iron (Fe (NO3)3·9H2O) solid is added 15mL deionized water, is then sufficiently stirred, is sufficiently mixed reactant, due to
The density of rice husk is small, it is easy to it floats on above solution, therefore rice husk should be thoroughly impregnated in clear water before the reaction, it can be abundant
Dispersion in the liquid phase, will install the autoclave of reactant additional steel kettle again, which is put into electric drying oven with forced convection
In, 180 DEG C are set by reaction temperature, controls the reaction time appropriate: 8 hours when rice husk is carbon source.
(2), product obtained in co-precipitation-galvanoplastic reduction step 1
Product obtained in step 1 is filtered, obtained solid matter is cleaned three times with deionized water, then will
Solid product is put into vacuum oven at 80 DEG C 6 hours dry.Solid product 1.5g after taking out drying is added to reaction
In device, and the deionized water of 200mL is added, ultrasound 5 minutes keeps solid particle fully dispersed in water, same what is be stirred continuously
When, by the sodium borohydride (NaBH of 100mL 0.6mol/L4) solution is added dropwise in reactor, after being added dropwise to complete, stops stirring
It mixes and stands 1 hour.
(3), the collection of iron/carbon composite and characterization
After the completion of step 2, reaction product is filtered rapidly, and three are cleaned to obtained solid with deionized water
Time, then by the solid product cleaned up be put into vacuum oven 60 DEG C dry 8 hours or more, can be obtained desired
Material.
Embodiment 2
The step only uses 0.01mol glucose as carbon source with embodiment 1, and hydro-thermal method carbonization organic matter walks
Suddenly in (1), the reaction time is 12 hours.
As it is clear from fig. 2 that iron/the carbon material synthesized by carbon source of rice husk is shiny black color, the basic primary morphology for keeping rice husk；
It is then in black powder using iron/carbon material that glucose is synthesized as carbon source.
One, scanning electron microscope (SEM) and power spectrum (EDS) characterization of material.
Iron/the carbon composite synthesized using glucose as carbon source is taken, material is pre-processed before characterization.It takes a small amount of
It lightly, is equably sprinkled upon on the conducting resinl for being used for testing, then blows the conducting resinl with stream of nitrogen gas by synthetic product
The extra material not with conducting resinl contact is blown away on surface.Material characterization result after pretreatment is as shown in Figure 3.
SEM figure shows that some iron is grown with spherical shape in carbon-based bottom surface, some iron is longer than in carbon substrate with spherical shape
Portion, EDS chart confirm the presence of iron and carbon into one.Table 1 is shown using glucose as iron/carbon composite of carbon source
EDAX results.Mainly it is demonstrated by the element contained in it and shared ratio.
Table 1
| Element | Wt% | At% |
| C | 03.21 | 07.98 |
| O | 03.52 | 06.56 |
| S | 89.31 | 83.01 |
| Ti | 03.96 | 02.46 |
Two, ferrous ion (Fe2+) dissolution experiment.
Iron/carbon composite the 20mg obtained using different carbon source (glucose or rice husk) synthesis is taken, its is evenly dispersed
In the solution of pH=3, pH=7, pH=10 of 50mL, the pH value of solution is adjusted using dilute hydrochloric acid or diluted sodium hydroxide solution
Section.It is sampled after reaction 0 minute, 30 minutes, 60 minutes and 120 minutes respectively.Then every sub-sampling 1mL tests the solution Central Asia
Iron ion (Fe2+) concentration.Experimental result is as shown in Figure 4.In 30 minutes quickly, explanation is carried on the burst size of ferrous ion
The iron of carbon-based bottom surface, which is largely dissolved in water body, becomes ferrous ion, gradually weakens and tends towards stability after 30 minutes, illustrates point
Iron of the cloth inside carbon substrate gradually dissolves out.The result illustrates that iron/carbon composite of synthesis can within the scope of very wide pH
Enough slow release ferrous ions, so as to the height for providing ferrous ion constantly for subsequent Fenton's reaction process to guarantee pollutant
Effect stablizes degradation.
Three, the organic pollutant in water removal is removed using iron/carbon composite that embodiment 1,2 synthesizes
The composite material of 20mg synthesis is added into the aqueous solution containing 20mg/L sulfamethazine, and is added 20
μ L hydrogen peroxide constitutes Fenton's reaction system.Monitoring reactor reacts the pollutant removal situation after 2h under condition of different pH.
Organic matter removal effect is as shown in Figure 5.The removal rate of sulfamethazine is 60%-80%, illustrates that iron/carbon of synthesis is compound
Material can be applied to Fenton's reaction system within the scope of very wide pH and obtain preferable contaminant degradation effect, but in acidity
Under the conditions of effect it is more preferable.In addition, comparison can be seen that with iron/carbon composite that different carbon source obtains, using rice husk as the iron of carbon source/
Carbon composite generally has higher removal efficiency.This explanation is synthesized using agricultural solid residues such as rice husks as carbon source
Iron/carbon composite has wide development and application prospect
Specific embodiment described above is only the preferred embodiment of the present invention, it is noted that for the art
For those of ordinary skill, without departing from the principle of the present invention, several improvement or replacement can also be made, these improvement
Or replacement should also be as being considered as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of iron/carbon composite comprising following steps:
(1) hydro-thermal method carbonization raw material
It chooses organic carbon source and dissolubility trivalent iron salt is source of iron, after organic carbon source cleaning pretreatment, be by carbon ferro element ratio
Organic carbon source and source of iron are added in reaction kettle the ratio of 10:1-20:1, and suitable water is added and fills organic carbon source and source of iron
Divide mixing, reaction kettle is placed in steel kettle, heating reaction is carried out；Well-mixed organic carbon source and source of iron are in temperature 160-
220 DEG C, under the conditions of reaction time 8-18 hour, finally obtain carbonized product；The organic carbon source is selected from rice husk agricultural organic waste
Gurry；
(2) co-precipitation-galvanoplastic reduction step (1) product
Carbonized product obtained in step (1) is cleaned with water, and is scattered in water phase, is then added and the objects such as ferro element
The reducing agent of the amount of matter stands a period of time；
(3) separation of iron/carbon composite and post-processing
Product obtained in step (2) is separated by solid-liquid separation, solid product is washed with water, is then dried in vacuo, finally to obtain the final product
To iron/carbon composite.
2. preparation method according to claim 1, which is characterized in that the dissolubility trivalent iron salt is selected from ferric nitrate, sulphur
Sour iron, iron chloride.
3. preparation method according to claim 1, which is characterized in that the reducing agent in step (2) is selected from sodium borohydride.
4. preparation method according to claim 1, which is characterized in that in step (2), at room temperature, while stirring
The reducing agent with the amount of the substances such as ferro element is slowly added dropwise.
5. preparation method according to claim 1, which is characterized in that vacuum drying is in vacuum oven in step (3)
It is 8-24 hours dry at 60 DEG C.
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| CN108326323A (en) * | 2018-03-29 | 2018-07-27 | 洛阳理工学院 | A kind of preparation method of rice husk carbon load nanometer nulvalent iron particle |
| CN108936194A (en) * | 2018-07-24 | 2018-12-07 | 武汉轻工大学 | Colloid carbon ball/nano zero-valence iron composite material preparation method, food deoxidant and preparation method thereof |
| CN109065310A (en) * | 2018-08-27 | 2018-12-21 | 合肥学院 | A kind of magnetic carbon composite material preparation process |
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| CN109939680B (en) * | 2019-03-28 | 2021-01-01 | 南开大学 | Biochar-loaded zero-valent iron composite material and preparation method thereof |
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| CN115703058A (en) * | 2021-08-04 | 2023-02-17 | 中国石油天然气股份有限公司 | Iron-carbon nano composite and preparation method and application thereof |
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| CN102784913A (en) * | 2012-07-26 | 2012-11-21 | 天津大学 | Hydrothermal preparation method of carbon-coated iron nanoparticles |
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