CN102730801A - Preparation method and application of ordered mesoporous carbon-activated carbon fibrofelt composite material - Google Patents
Preparation method and application of ordered mesoporous carbon-activated carbon fibrofelt composite material Download PDFInfo
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- CN102730801A CN102730801A CN2012102364747A CN201210236474A CN102730801A CN 102730801 A CN102730801 A CN 102730801A CN 2012102364747 A CN2012102364747 A CN 2012102364747A CN 201210236474 A CN201210236474 A CN 201210236474A CN 102730801 A CN102730801 A CN 102730801A
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Abstract
The invention relates to the technical fields of preparation and application of a novel massive carbon material with an ordered mesoporous structure, and particularly discloses a preparation method and application of an ordered mesoporous carbon-activated carbon fibrofelt composite material. The ordered mesoporous carbon-activated carbon fibrofelt (OMC-ACF) composite material disclosed by the invention is a novel massive carbon material with an ordered mesoporous structure, and is prepared by taking phenolic resin as a carbon source and F127 as a structure directing agent, coating the phenolic resin and the F127 on the surface of an ACF at the same time according to a certain proportion, and performing intermolecular self-assembly, thermal polymerization and calcination under the protection of an inert gas; and the composite material is large in specific area, high in pore volume and large in bore diameter, so that the composite material can be used as a novel electrode material. The novel massive carbon material prepared by the method has the advantages of high catalytic degradation activity, high stability and the like in a test of cathode diffusion oxygen degradation dye wastewater through electro-Fenton reaction; and the novel massive carbon material is simple in production process and low in cost, and can be easily industrialized.
Description
Technical field
The present invention relates to a kind of preparation and applied technical field, be specifically related to the preparation method of a kind of novel ordered mesopore carbon-activated carbon fiber felt composite material and be applied to the application that electricity-Fenton reacts degradation of dye waste water as cathode material with novel block carbon material of order mesoporous structure.
Background technology
Ordered mesopore carbon is one type of novel non-silicon-based mesoporous material, and having huge specific surface area (can be up to 2500m
2/ g), regular pore passage structure, big aperture (2-50nm) and pore volume (can be up to 2.25cm
3/ g), thereby obtained important application at aspects such as support of the catalyst, hydrogen storage material, electrode materialss, therefore receive people's great attention.In recent years, the mesoporous material science has become one of hot research field of subject crossing such as striding chemistry, physics, material, biology in the world, more becomes an important milestone of Materials science development.But be applied to the research of electricity-Fenton system as a kind of oxygen diffusion cathode degradation of dye waste water to ordered mesopore carbon, Shang Weijian has report.
Electricity-Fenton reacts as a kind of high-level oxidation technology, mainly is with O through electrochemical method
2Be converted into H
2O
2, further being converted into strong oxidizing property active specy OH, OH can very handle organic waste water efficiently, and concrete reaction mechanism is as follows:
O
2+2H
++2e
-→H
2O
2 (1)
Fe
2++H
2O
2+H
+→Fe
3++H
2O+·OH (2)
·OH+RH→R·+H
2O (3)
Dissolving O
2Pass through to generate Fenton reagent H at cathode compartment at different cathode surface generation electronic reduction reactions
2O
2, under slightly acidic (pH≤3) condition and Fe
2+Generation Fenton reaction, the OH of generation strong oxidizing property, the rapid and three kinds of forms reactions of aromatic organic compounds generation in non-selectivity ground: the addition reaction and the electron-transfer reaction of dehydrogenation reaction, destruction C=C unsaturated link(age) make it that chemical degradation take place.Fe in the reaction
3+Can become Fe in cathodic reduction
2+, continue and H
2O
2The Fenton reaction takes place, so Fe
2+In reaction, play the effect of catalyzer, promptly so-called electricity-Fenton process.
In electricity-Fenton reaction system, negative electrode plays important effect, because carbon material has good electrical conductivity; Thermostability; Erosion resistance, advantages such as resistance to acids and bases, present cathode material is generally selected carbon material (like graphite, reticulated vitreous carbon, thomel etc.) for use.At present do not see its report as the research that negative electrode is applied to electricity-Fenton system relevant for ordered mesopore carbon.Reason is that the preparation method of mesoporous carbon is prepared into powder with it at present, and the mesoporous carbon of this form is difficult to use as electrode materials.The domestic and international research report mainly is the mesoporous carbon powder to be mixed the back compressing tablet use as electrode with the PTFE emulsion at present; This method complex operation; And PTFE is prone to stop up the duct of mesoporous carbon; Reduce the electroconductibility of entire electrode material, and there is unstable in this combining method, particularly in the environment for use of complicacy.Therefore it is very necessary preparing a kind of blocky carbon material with order mesoporous structure.
Summary of the invention
To the deficiency that exists in the prior art, a kind of preparation method and application of novel ordered mesopore carbon-active carbon fiber felt (OMC-ACF) matrix material have been the object of the present invention is to provide.
OMC-ACF matrix material provided by the present invention is the surface that a kind of carbon source with ordered mesopore carbon (OMC) (resol) and template (nonionogenic tenside F127) are coated on active carbon fiber felt (ACF) simultaneously; Through under protection of inert gas, carrying out high-temperature calcination with the carbon source carbonization and make novel block carbon material with mesoporous carbon and active carbon fiber felt are compound simultaneously with order mesoporous structure; This material has high specific surface area, high pore volume, roomy aperture, can be applied to electricity-Fenton system as a kind of oxygen diffusion cathode degradation of dye waste water.
In order to realize above-mentioned technical purpose, the present invention has taked following technical measures:
A kind of ordered mesopore carbon-active carbon fiber felt (OMC-ACF) matrix material, the step of its preparation method is following:
(1) preparation of resol carbon source:
0.61g phenol is put into round-bottomed flask, under 40 ~ 42 ℃ of water bath condition, stirring and dissolving; The NaOH solution that adds 0.13g 20wt% again behind the stirring 10min, dropwise adds 37wt% formaldehyde solution 1.05g; Stirring reaction 1h is cooled to room temperature after being warming up to 78 ~ 80 ℃ then, and the HCl that splashes into 0.6mol/L then transfers to 7.0 with the pH value of reaction system; Remove at 50 ℃ of following rotary evaporations again and anhydrate, the yellow oil product that obtains is subsequent use with the resol ethanolic soln that absolute ethyl alcohol is diluted to 20wt%;
(2) preparation of OMC-ACF matrix material:
The 20g absolute ethyl alcohol is added round-bottomed flask, under 40 ℃ of water bath condition, add 1.0g nonionogenic tenside F127 stirring and dissolving; After treating the solution clarification, splash into the 20wt% resol ethanolic soln that 5.0g step (1) obtains, behind the stirring 10min; Mixing solutions is poured in the petridish that is equipped with the active carbon fiber felt (ACF) of quality (1.0g) such as resol, and volatilization ethanol 8h changes petridish over to 100 ℃ of baking ovens then naturally; Thermopolymerization 24h scrapes the product that obtains, and under the nitrogen protection condition, is fired to target temperature x ℃ through certain heating schedule; Keep 3h, and the resulting sample of mark is OMC-ACF-x, the scope of x is 700-900.
Said heating schedule is: set 20 ℃ of initial temperatures, rise to 350 ℃ and keep 5h with the speed of 1 ℃/min, the speed with 2 ℃/min rises to target temperature x ℃ again.
Compared with prior art, advantage of the present invention and beneficial effect are following:
The preparation method of New O MC-ACF matrix material of the present invention is simple, and needed reaction reagent kind and consumption are all less, and cost is relatively low.In the process that is applied to electricity-Fenton reaction degradation of dye waste water as a kind of novel oxygen diffusion cathode, shown good catalyzed degradation activity and degradation speed, its efficient is far above its matrix active carbon fiber felt.
OMC-ACF elution process after degraded is used is very simple; The OMC-ACF negative electrode has still shown good catalyzed degradation activity behind deionized water washing by soaking natural air drying, reuses 6 times, and degradation rate is all more than 78%; Explain that its regenerability is good, can reuse.
Description of drawings
Fig. 1 schemes for the transmission electron microscope (TEM) of the OMC-ACF that calcining under the differing temps of ACF matrix and embodiment 1 preparation obtains;
Wherein a1, a2 represent ACF, and b1, b2 represent OMC-ACF-900, and c1, c2 represent OMC-ACF-800, and d1, d2 represent OMC-ACF-700;
From Fig. 1, the sample surfaces after 700 ℃, 800 ℃, 900 ℃ calcinings all has one deck to have the meso-porous carbon material in orderly duct.These results show, when calcining temperature during greater than 700 ℃, the carbon source of mesoporous carbon is carbonization and compound with active carbon fiber felt generation carbon carbon, forms matrix material.
Fig. 2 is the OMC-ACF-x of embodiment 1 preparation and the nitrogen physisorption desorption curve of ACF matrix;
Wherein, a represents ACF, and b represents OMC-ACF-700, and c represents OMC-ACF-800, and d represents OMC-ACF-900.
Fig. 3 is the BJH graph of pore diameter distribution (the mainly pore size distribution of the mesoporous and macropore of exosyndrome material) of the OMC-ACF-x and the ACF matrix of embodiment 1 preparation.
Fig. 4 is the palliating degradation degree time history plot of the OMC-ACF of ACF matrix and embodiment 1 preparation as the cathode material degradation of dye waste water X3B of electricity-Fenton system;
Degradation rate (amount of the dyestuff that is decomposed accounts for the ratio of original bulk) is by X3B starting point concentration c
0With X3B terminal point concentration c
tDifference divided by X3B starting point concentration c
0Calculating gets.
As can be seen from the figure ACF matrix, OMC-ACF-700, OMC-ACF-800, OMC-ACF-900 degradation rate behind reaction beginning 120min is respectively 83.2%, 87.1%, 97.7%, 90.1%, and the degradation rate of OMC-ACF-800 is the highest, is 1.2 times of ACF.
Fig. 5 recycles degradation of dye waste water X3B figure for the OMC-ACF-800 of embodiment 1 preparation as the cathode material of electricity-Fenton system.
Embodiment
Following applicant will combine concrete embodiment that the preparation process and the application process of product of the present invention are elaborated, and be convenient to understand the present invention with those skilled in the art know that.But should be appreciated that following examples should not be interpreted as the restriction of scope that the application's claims are asked for protection by any way.
Experimental raw related in following examples is all available from Chemical Reagent Co., Ltd., Sinopharm Group, and (performance index: specific surface area is 1200-1500m to active carbon fiber felt (ACF matrix) available from Shandong Xuesheng Technology Co., Ltd.
2/ g; Micropore volume 0.7-0.8mL/g; Benzene adsorptive capacity 35-50%; Iodine sorption value 800-1200mg/g.), all reagent and material are before use without any purification process.
Embodiment 1 product prepn embodiment:
1, a kind of novel ordered mesopore carbon-active carbon fiber felt (OMC-ACF) matrix material, its preparation process is following:
(1) preparation of resol carbon source:
0.61g phenol is put into round-bottomed flask, under 40 ~ 42 ℃ of water bath condition, stirring and dissolving; The NaOH solution that adds 0.13g 20wt% again behind the stirring 10min, dropwise adds 37wt% formaldehyde solution 1.05g; Stirring reaction 1h is cooled to room temperature after being warming up to 78 ~ 80 ℃ then, and the HCl that splashes into 0.6mol/L then transfers to 7.0 with the pH value of reaction system; Remove at 50 ℃ of following rotary evaporations again and anhydrate, the yellow oil product that obtains is subsequent use with the resol ethanolic soln that absolute ethyl alcohol is diluted to 20wt%;
(2) preparation of mesoporous carbon-activated carbon fiber felt composite material (OMC-ACF):
The 20g absolute ethyl alcohol is added round-bottomed flask, under 40 ℃ of water bath condition, add 1.0g nonionogenic tenside F127 (sigma, EO
106PO
70EO
106) stirring and dissolving, treat solution clarification after, splash into the 20wt% resol ethanolic soln that 5.0g step (1) obtains; After stirring 10min, mixing solutions is poured in the petridish that 1.0g active carbon fiber felt (ACF has been cut into about 3cm * 6cm size) is housed, naturally volatilization ethanol 8h; Change petridish over to 100 ℃ of baking ovens then, thermopolymerization 24h scrapes the product that obtains; Under the nitrogen protection condition, be fired to target temperature x ℃ (700-900 ℃) through certain heating schedule, keep 3h, take out the cooling back; And the resulting sample of mark is OMC-ACF-x, and the scope of x is 700-900.
Said heating schedule is: set 20 ℃ of initial temperatures, rise to 350 ℃ and keep 5h with the speed of 1 ℃/min, the speed with 2 ℃/min rises to target temperature x ℃ again.
The result of Fig. 2, Fig. 3 and table 1 shows that the mesoporous number of OMC-ACF-x is higher than without the ACF (ACF matrix) that modifies far away; Show that ordered mesopore carbon is successfully through the surface growth of compound mode at ACF; This result is consistent with the result of transmission electron microscope (TEM); But because the difference of calcining temperature causes the mesoporous number of the OMC-ACF that calcining obtains under the differing temps to differ greatly, reason is when calcining temperature is higher; Mesoporous aperture can be because the skeleton of resol shrinks expansion, and still too high temperature can cause that caving in of skeleton causes mesoporous obstruction.
Table 1 OMC-ACF-x and relatively without ACF (ACF matrix) physical parameter of modifying
Embodiment 2 application implementations example: the OMC-ACF-x of embodiment 1 preparation is applied to electricity-Fenton system tests as oxygen diffusion cathode degradation of dye waste water X3B
1. the preparation of electrode:
The OMC-ACF-x that accurately takes by weighing 0.1g (is about on the pure titanium sheet that the single face of 3cm * 3cm) is wrapped in 3cm * 3cm as negative electrode, and the ACF single face of equal quality is wrapped on the pure titanium sheet of 3cm * 3cm and contrasts as negative electrode.(3cm * 3cm) make up with ACF, OMC-ACF-x negative electrode respectively forms different electrode pairs to graphite cake anode GE after the activation, and that one side that is surrounded by OMC-ACF-x or ACF is relative with GE, and this electrode pair is applied to electricity-Fenton system.
2. degradation step:
In electricity-Fenton degraded X3B experimentation, X3B waste water is simulated by the X3B aqueous solution.To keep in the solution oxygen saturated, is that the starting point concentration that contains of the pH=3.0 of 200mL is 1.0 * 10 at cathode surface bubbling air (flow velocity 0.6L/min) with volume
-4The X3B solution of mol/L is injected in the reactor drum, Na in the system
2SO
4The concentration of supporting electrolyte solution is 0.1mol/L, the Fe in the system
2+Concentration is 1 * 10
-3Mol/L at the uniform velocity stirs 3-5h and reaches adsorption equilibrium.Regulating D.C. regulated power supply (PS-605D type numeral shows DC stable power supply (the happy exhibition in Shenzhen instrument company)) makes electrochemical reaction equal to carry out under the 6.2V condition in potential difference.After the degraded beginning; 3mL at set intervals takes a sample; Carry out the omnidistance scanning of UV-Vis absorption spectrum (UV2450 type ultraviolet-visible spectrophotometer (Tianjin, island company; Japan) maximum absorption wavelength 530nm) measure, refund reaction tank after each detection finishes to eliminate because of liquor capacity reduces the error that causes, the result sees Fig. 4.
Embodiment 3: the regenerability test of the OMC-ACF-x of embodiment 1 preparation
Each OMC-ACF-800 electrode later that in embodiment 2, uses is soaked in deionized water 3 times, soak 1h at every turn after, natural air drying, 2 operation steps again repeats to implement to grin.This electrode is reused altogether 6 times, and the degradation capability when using for the 6th time still keeps 84.0% (the seeing table 2) that use first, explains that the regenerability of this cathode material is good, can reuse.
The result of table 2O MC-ACF-800 regenerability test
Claims (2)
1. ordered mesopore carbon-activated carbon fiber felt composite material, the step of its preparation method is following:
(1) preparation of resol carbon source:
0.61g phenol is put into round-bottomed flask, under 40 ~ 42 ℃ of water bath condition, stirring and dissolving; The NaOH solution that adds 0.13 g 20wt% again behind the stirring 10min, dropwise adds 37wt% formaldehyde solution 1.05g; Stirring reaction 1h is cooled to room temperature after being warming up to 78 ~ 80 ℃ then, and the HCl that splashes into 0.6mol/L then transfers to 7.0 with the pH value of reaction system; Remove at 50 ℃ of following rotary evaporations again and anhydrate, the yellow oil product that obtains is subsequent use with the resol ethanolic soln that absolute ethyl alcohol is diluted to 20wt%;
(2) preparation of ordered mesopore carbon-activated carbon fiber felt composite material:
20 g absolute ethyl alcohols are added round-bottomed flask, under 40 ℃ of water bath condition, add 1.0 g nonionogenic tenside F127 stirring and dissolving; After treating the solution clarification, splash into the 20wt% resol ethanolic soln that 5.0g step (1) obtains, behind the stirring 10min; Mixing solutions is poured in the petridish that is equipped with the active carbon fiber felt of quality such as resol, and volatilization ethanol 8h changes petridish over to 100 ℃ of baking ovens then naturally; Thermopolymerization 24h scrapes the product that obtains, and under the nitrogen protection condition, is fired to target temperature x ℃ through certain heating schedule; Keep 3h, and the resulting sample of mark is OMC-ACF-x, the scope of x is 700-900;
Said heating schedule is: set 20 ℃ of initial temperatures, rise to 350 ℃ and keep 5h with the speed of 1 ℃/min, the speed with 2 ℃/min rises to target temperature x ℃ again.
2. the described ordered mesopore carbon of claim 1-activated carbon fiber felt composite material is as the application of negative electrode in the diffusion of oxygen degradation of dye waste water of electricity-Fenton reaction.
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Cited By (6)
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| CN103225132A (en) * | 2013-02-28 | 2013-07-31 | 江苏竹溪活性炭有限公司 | Bioactive carbon fiber preparation method |
| CN103225133A (en) * | 2013-02-28 | 2013-07-31 | 江苏竹溪活性炭有限公司 | Active carbon fiber and preparation method thereof |
| CN103641212A (en) * | 2013-12-13 | 2014-03-19 | 南开大学 | Method for preparing graphite felt cathode material for treating organic wastewater |
| CN105036250A (en) * | 2015-06-15 | 2015-11-11 | 中南民族大学 | Preparation method and application of activated-carbon-fiber-supported ordered mesoporous carbon-graphene composite material |
| CN110258123A (en) * | 2019-06-27 | 2019-09-20 | 山东大学 | The hydrogen storage active carbon fiber felt and its preparation method and application of one specific admixture hollow glass microballoon |
| CN113477699A (en) * | 2021-07-21 | 2021-10-08 | 中国科学院南京土壤研究所 | Electric Fenton method for repairing polycyclic aromatic hydrocarbon in soil by in-situ self-production of oxidant |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103225132A (en) * | 2013-02-28 | 2013-07-31 | 江苏竹溪活性炭有限公司 | Bioactive carbon fiber preparation method |
| CN103225133A (en) * | 2013-02-28 | 2013-07-31 | 江苏竹溪活性炭有限公司 | Active carbon fiber and preparation method thereof |
| CN103641212A (en) * | 2013-12-13 | 2014-03-19 | 南开大学 | Method for preparing graphite felt cathode material for treating organic wastewater |
| CN105036250A (en) * | 2015-06-15 | 2015-11-11 | 中南民族大学 | Preparation method and application of activated-carbon-fiber-supported ordered mesoporous carbon-graphene composite material |
| CN105036250B (en) * | 2015-06-15 | 2017-03-08 | 中南民族大学 | A kind of preparation method and application of activated carbon fiber-loaded ordered mesopore carbon graphene composite material |
| CN110258123A (en) * | 2019-06-27 | 2019-09-20 | 山东大学 | The hydrogen storage active carbon fiber felt and its preparation method and application of one specific admixture hollow glass microballoon |
| CN110258123B (en) * | 2019-06-27 | 2024-02-23 | 山东大学 | Active carbon fiber felt for hydrogen storage of hybrid hollow glass microspheres and preparation method and application thereof |
| CN113477699A (en) * | 2021-07-21 | 2021-10-08 | 中国科学院南京土壤研究所 | Electric Fenton method for repairing polycyclic aromatic hydrocarbon in soil by in-situ self-production of oxidant |
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