CN106881059A - 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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- CN106881059A CN106881059A CN201710064168.2A CN201710064168A CN106881059A CN 106881059 A CN106881059 A CN 106881059A CN 201710064168 A CN201710064168 A CN 201710064168A CN 106881059 A CN106881059 A CN 106881059A
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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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- 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
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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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- 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
-
- 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
-
- 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
Abstract
The present invention relates to field of material technology, a kind of preparation method of iron/carbon composite is specifically disclosed, method that the present invention is combined using hydro-thermal method co-precipitation galvanoplastic first prepares iron/carbon composite.Building-up process can be analyzed to two steps：First, the organic matter raw material that will be added with molysite using hydro-thermal method is carbonized；Second, the product after carbonization is reduced using appropriate reducing agent, so as to obtain required iron/carbon composite.Using the main surface and inside for being present in porous carbon materials with the fixation of zeroth order Iron activiation of ferro element in iron/carbon material that the method is obtained, carbon material serves not only as loading the substrate of Zero-valent Iron but also playing Zero-valent Iron certain protective effect.Therefore, the composite of synthesis had both had the good reducing power of Zero-valent Iron, it may have the carbon material adsorption capacity good to organic pollution, the removal more efficient so as to realize organic pollutants.
Description
Technical field
It is to be related to a kind of iron/carbon composite more specifically the present invention relates to field of material technology.
Background technology
Iron/carbon composite is a kind of widely used, excellent performance new material, is widely used in photocatalysis material
The fields such as material, electrode material, sensor, sewage disposal.At present, 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.Can synthesize difference using these preparation methods
Iron/the carbon composite of grain size, different shape.But, the synthetic method generally existing cost of these iron/carbon composites
The shortcomings of height, complex operation.Such as：Arc process needs special arc discharge device and pure raw material, but the product for obtaining
Produce amount is little；Chemical vapour deposition technique needs to use special experimental provision and synthesis is time-consuming more long；High-temperature heat treatment method
Need at least more than 1500 DEG C of high temperature, thus not only high energy consumption, time-consuming but also laboratory apparatus is required higher.
In order to solve the above technical problems, the present invention comes therefrom.
The content of the invention
The purpose of invention is to provide a kind of raw material sources extensively, and low cost is adapted to the iron/carbon composite wood of large-scale promotion
Material and preparation method thereof, the iron/carbon composite of synthesis can be used to remove environmental contaminants.
In order to solve these problems in currently available technology, the technical scheme that first aspect present invention is provided is a kind of
The preparation method of iron/carbon composite, it comprises the following steps：
(1) hydro-thermal method carbonization raw material
It is source of iron to choose organic carbon source and dissolubility trivalent iron salt, after organic carbon source cleaning is pre-processed, by carbon ferro element
Than being 10:1-20:1 ratio adds organic carbon source and source of iron in reactor, and adds appropriate water by organic carbon source and iron
Source is sufficiently mixed, and under uniform temperature and time, obtains carbonized product；
(2) product of co-precipitation-galvanoplastic reduction step (1)
The carbonized product obtained in step (1) is cleaned with water, and is scattered in water phase, be subsequently adding and ferro element
Deng the reducing agent of the amount of material, a period of time is stood；
(3) separation and post processing of iron/carbon composite
The product obtained in step (2) is carried out into separation of solid and liquid, solid product is cleaned with water, be then vacuum dried, finally
Obtain iron/carbon composite.
Preferably, organic carbon source is selected from carbohydrate, and further, organic carbon source is selected from monose 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), reactor is positioned in steel kettle, carries out heating response.
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 ambient temperature, the reduction with the amount of the material such as ferro element is slowly added dropwise while stirring
Agent.
Preferably, vacuum drying is to be dried 8-24 hours at 60 DEG C of vacuum drying chamber in the step (3).
A kind of preparation method of iron/carbon composite that the present invention is provided, it comprises the following steps：
(1) hydro-thermal method carbonization raw material
Suitable carbon source and source of iron are selected first.Can be using the Organic Ingredients or rice husk etc. such as glucose agricultural organic waste
Thing is carbon material, is source of iron with dissolubility trivalent iron salt.After by carbon source cleaning pretreatment, mix (carbon with source of iron according to a certain percentage
Ferro element ratio is 10:1-20:1) in, then feeding the mixture into reactor, and appropriate water is added to be sufficiently mixed, will be anti-
Answer temperature control at 180 DEG C or so, the reaction time is 8-18 hours；
(2) product of co-precipitation-galvanoplastic reduction step (1)
The carbonized product obtained in step (1) is cleaned and be scattered in water phase with water, side is stirred at ambient temperature
The reducing agent (sodium borohydride, NaBH4) that side is slowly added to the amount of the material such as ferro element is mixed, about 0.5-2 hours is then stood；
(3) separation and post processing of iron/carbon composite
The product obtained in step (2) is carried out into separation of solid and liquid, solid product water is cleaned multiple times to remove residual
Reactant, is then placed in vacuum drying chamber, is dried at least 8 hours at a temperature of 60 DEG C, you can obtain iron/carbon composite.
Method that the present invention is combined using hydro-thermal method-co-precipitation-galvanoplastic first prepares iron/carbon composite.Close
Two steps are can be analyzed into process：First, the organic matter raw material that will be added with molysite using hydro-thermal method is carbonized；Second,
The product after carbonization is reduced using appropriate reducing agent, so as to obtain required material.
Present invention mainly discloses a kind of preparation method of inexpensive, simple and practical and environmental protection iron/carbon composite.
Compared with traditional one-step method for synthesizing, the present invention in preparation method be divided into two steps carry out, it is necessary to reaction temperature it is relatively low and
It is simple 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
Carry out at room temperature, therefore not only reduce operation energy consumption and reduce the danger of operation.In addition, the method goes for
Starch, carbohydrate, cellulose and the gas chromatography raw material (including abandoned biomass) containing these materials, can significantly reduce original
Material cost even can be realized turning waste into wealth, and these all significantly improve the economic and technical feasibility of large-scale industrial production, ring
Border friendly and sustainability.
It is present in porous carbon using main the fixation with zeroth order Iron activiation of ferro element in iron/carbon material that the method is obtained
The surface and inside of material, carbon material serve not only as loading the substrate of Zero-valent Iron but also certain protection work are played to Zero-valent Iron
With.Therefore, the composite of synthesis had both had the good reducing power of Zero-valent Iron, it may have carbon material is good to organic pollution
Adsorption capacity, the removal more efficient so as to realize organic pollutants.The ferro element that it is loaded simultaneously is during the course of the reaction
Can be released slowly, therefore not result in the waste of ferro element and form a large amount of iron cements.Finally, will be using the inventive method
Iron/the carbon composite of synthesis is applied in Fenton advanced oxidation system, to reach the purpose of pollutant in efficiently removal water body.
Brief description of the drawings
Fig. 1 is the flow chart of preparation method of the present invention.
Fig. 2 is the iron/carbon composite of preparation method synthesis of the present invention.Fig. 2 (a) is the material synthesized as carbon source with rice husk
Material, Fig. 2 (b) is to do the material that carbon source synthesizes with glucose.
Fig. 3 (a, b) shows ESEM (SEM) phenogram of the iron/carbon composite with glucose as carbon source.
Fig. 4 displays ferrous ion (Fe under different pH using the iron/carbon composite of different carbon source synthesis2+) dissolution feelings
Condition.
Fig. 5 shows that the Fenton process based on iron/carbon composite removes the effect of sulfamethazine.
Specific embodiment
Such 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 present invention.The implementation condition used in embodiment can be done according to the condition of specific producer
Further adjustment, unreceipted implementation condition is usually the condition in normal experiment.
Introduce and summarize
The present invention by way of example rather than provides the mode of limitation and illustrates.It should be noted that in present disclosure
Described " one " or " one kind " implementation method 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, can
Only some or all of aspects of the invention implement the present invention.For purposes of illustration, be given herein specific numbering, material and
Configuration, enables one to thoroughly understand the present invention.However, be evident that for those of skill in the art,
The present invention can be implemented without concrete details.In other examples, not make, the present invention is obscure to be omitted or simplified many institutes
Known feature.
Various operations are described successively as multiple discrete steps, and with most helpful in understanding side of the invention
Formula is illustrated；However, in-order description should not be construed as to imply that into these operations are necessarily dependent on order.
Various implementation methods will be illustrated according to the reactant of type species.To show for those of skill in the art and
It is clear to, the present invention can be used any number of different types of reactant to implement, and is more than those for the purpose of illustration
And the reactant for being given herein.Additionally, be also evident that, the invention is not limited in any specific mixing is shown
Example.
The preparation method of 1 iron of embodiment/carbon composite
(1), hydro-thermal method carbonization organic matter
The rice husk of 2g is taken, carries out being cleaned multiple times the impurity on removal surface with water, then in 60 DEG C or so drying；Will be by pre-
The raw material for the treatment of is added in the polytetrafluoroethylene (PTFE) autoclave that dischargeable capacity is 25mL, while adding the nitric acid of 0.005mol
Iron (Fe (NO3)3·9H2O) solid, adds 15mL deionized waters, is then sufficiently stirred for, and is sufficiently mixed reactant, due to
The density of rice husk is small, it is easy to float over above solution, therefore rice husk should be thoroughly impregnated in clear water before the reaction, can be abundant
Dispersion in the liquid phase, will install the autoclave of reactant additional steel kettle again, and the steel kettle is put into electric drying oven with forced convection
In, reaction temperature is set to 180 DEG C, control the appropriate reaction time：8 hours when rice husk is carbon source.
(2), the product obtained in co-precipitation-galvanoplastic reduction step 1
The product that will be obtained in step 1 carries out suction filtration, and the solid matter that will be obtained is cleaned three times with deionized water, then will
Solid product is dried 6 hours in being put into vacuum drying chamber at 80 DEG C.Take out the solid product 1.5g after drying and be added to reaction
In device, and the deionized water of 200mL is added, ultrasound 5 minutes makes solid particle be well 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
Mix and stand 1 hour.
(3), the collection of iron/carbon composite and sign
Treat after the completion of step 2, product is carried out into suction filtration rapidly, and three are cleaned to the solid for obtaining with deionized water
Time, the solid product that then will be cleaned up is put into vacuum drying chamber in 60 DEG C of dryings more than 8 hours, you can obtain desired
Material.
Embodiment 2
Described step is simply walked with 0.01mol glucose with embodiment 1 as carbon source, and hydro-thermal method carbonization organic matter
Suddenly in (1), the reaction time is 12 hours.
As it is clear from fig. 2 that iron/the carbon material synthesized as carbon source with rice husk is shiny black color, the primary morphology of basic holding rice husk；
It is in then black powder with iron/carbon material that glucose synthesizes as carbon source.
First, the ESEM (SEM) of material and power spectrum (EDS) are characterized.
Iron/the carbon composite synthesized as carbon source with glucose is taken, material is pre-processed before sign.Take a small amount of
Synthetic product, it lightly, is equably sprinkled upon on the conducting resinl for testing, and then blows the conducting resinl with stream of nitrogen gas
Surface, the unnecessary material not contacted with conducting resinl is blown away.Material characterization result after pretreatment is as shown in Figure 3.
SEM figures show some iron with spherical length in carbon-based basal surface, some iron is longer than in carbon substrate with spherical
Portion, EDS charts enter a presence for confirming iron and carbon.Table 1 shows the iron/carbon composite with glucose as carbon source
EDAX results.Mainly it is demonstrated by element and shared ratio that it is contained within.
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 |
2nd, ferrous ion (Fe2+) dissolution experiment.
Iron/carbon composite the 20mg obtained using different carbon source (glucose or rice husk) synthesis is taken, its is dispersed
In the solution of pH=3, pH=7, pH=10 of 50mL, the pH value of solution is adjusted using watery hydrochloric acid or diluted sodium hydroxide solution
Section.Sampled after reacting 0 minute, 30 minutes, 60 minutes and 120 minutes respectively.Per sub-sampling 1mL, then test 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 basal surface becomes ferrous ion in being largely dissolved in water body, progressively weakens later and tends towards stability within 30 minutes, illustrates point
The cloth gradually dissolution of the iron inside carbon substrate.Iron/the carbon composite of result explanation synthesis can in the range of pH very wide
Enough slow release ferrous ions, so as to constantly provide ferrous ion to ensure the height of pollutant for follow-up Fenton's reaction process
Effect stabilization degraded.
3rd, using embodiment 1, it is 2-in-1 into iron/carbon composite go water removal in organic pollution
The composite of 20mg synthesis is added toward the aqueous solution containing 20mg/L sulfamethazines, and adds 20
μ L hydrogen peroxide, constitutes Fenton's reaction system.Pollutant removal situation of the monitoring reactor after reaction 2h under condition of different pH.
Organic matter removal effect is as shown in Figure 5.The clearance of sulfamethazine is 60%-80%, illustrates that the iron/carbon of synthesis is combined
Material can be applied to Fenton's reaction system in the range of pH very wide and obtain preferable contaminant degradation effect, but in acidity
Under the conditions of effect it is more preferable.In addition, iron/carbon composite that contrast is obtained with different carbon source can be seen that, the iron with rice husk as carbon source/
Carbon composite generally has removal efficiency higher.This explanation is synthesized by the use of agricultural solid residues such as rice husks as carbon source
Iron/carbon composite has wide development and application prospect
The above specific embodiment is only the preferred embodiment of the present invention, it is noted that for the art
For those of ordinary skill, under the premise without departing from the principles of the invention, some 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 (10)
1. a kind of preparation method of iron/carbon composite, it comprises the following steps：
(1) hydro-thermal method carbonization raw material
It is source of iron to choose organic carbon source and dissolubility trivalent iron salt, after organic carbon source cleaning is pre-processed, is by carbon ferro element ratio
10:1-20:1 ratio adds organic carbon source and source of iron in reactor, and adds appropriate water to fill organic carbon source and source of iron
Divide mixing, under uniform temperature and time, obtain carbonized product；
(2) product of co-precipitation-galvanoplastic reduction step (1)
The carbonized product obtained in step (1) is cleaned with water, and is scattered in water phase, be subsequently adding and the thing such as ferro element
The reducing agent of the amount of matter, stands a period of time；
(3) separation and post processing of iron/carbon composite
The product obtained in step (2) is carried out into separation of solid and liquid, solid product is cleaned with water, be then vacuum dried, finally obtained final product
To iron/carbon composite.
2. preparation method according to claim 1, it is characterised in that the organic carbon source is selected from carbohydrate.
3. preparation method according to claim 1, it is characterised in that the organic carbon source is selected from monose or polysaccharide.
4. preparation method according to claim 1, it is characterised in that the organic carbon source is selected from glucose or rice husk agricultural
Organic waste or its mixing.
5. preparation method according to claim 1, it is characterised in that the dissolubility trivalent iron salt is selected from ferric nitrate, sulphur
Sour iron, iron chloride.
6. preparation method according to claim 1, it is characterised in that in step (1), reactor is positioned in steel kettle,
Carry out heating response.
7. preparation method according to claim 1, it is characterised in that in step (1), well-mixed organic carbon source and iron
Source finally obtains carbonized product in 160-220 DEG C of temperature, under the conditions of reaction time 8-18 hours.
8. preparation method according to claim 1, it is characterised in that the reducing agent in step (2) is selected from sodium borohydride.
9. preparation method according to claim 1, it is characterised in that in step (2), at ambient temperature, while stirring
It is slowly added dropwise the reducing agent with the amount of the material such as ferro element.
10. preparation method according to claim 1, it is characterised in that vacuum drying is in vacuum drying chamber in step (3)
Dried at 60 DEG C 8-24 hours.
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| CN106861623A (en) * | 2017-04-07 | 2017-06-20 | 郑州大学 | A kind of carbon material of load C o Fe alloys and its preparation method and application |
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| CN106861623A (en) * | 2017-04-07 | 2017-06-20 | 郑州大学 | A kind of carbon material of load C o Fe alloys and its preparation method and application |
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