CN104525119B - A kind of g-C3n4functional charcoal sorbing material of/ZnO/ activated carbon and preparation method thereof - Google Patents
A kind of g-C3n4functional charcoal sorbing material of/ZnO/ activated carbon and preparation method thereof Download PDFInfo
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- CN104525119B CN104525119B CN201510000963.6A CN201510000963A CN104525119B CN 104525119 B CN104525119 B CN 104525119B CN 201510000963 A CN201510000963 A CN 201510000963A CN 104525119 B CN104525119 B CN 104525119B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
- 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
- B01J20/02—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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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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
- B01J20/34—Regenerating or reactivating
- B01J20/3441—Regeneration or reactivation by electric current, ultrasound or irradiation, e.g. electromagnetic radiation such as X-rays, UV, light, microwaves
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention discloses a kind of g C3N4Functional charcoal sorbing material of/ZnO/ activated carbon and preparation method thereof, with living beings (wood or bamboo), melamine, zinc acetate as primary raw material, by carbonize, impregnates, activate, high-temperature polycondensation etc. react, prepared g C3N4The functional charcoal sorbing material of/ZnO/ activated carbon.The present invention uses activated carbon precursor and g C3N4Presoma and ZnO precursor are combined, and with zinc acetate for preparing the activator of activated carbon, prepared g C3N4The functional charcoal sorbing material of/ZnO/ activated carbon is firmly combined with not easily runing off, and service life is long, and can original position Photocatalytic Regeneration.
Description
Technical field
The invention belongs to the preparation field of functional charcoal sorbing material, be specifically related to a kind of g-C3N4Functional charcoal sorbing material of/ZnO/ activated carbon and preparation method thereof.
Background technology
Activated carbon, because of advantages such as its pore structure flourishing, absorption affinity is strong, surface functional group is abundant, mechanical strength is high, chemical inertnesses, is widely used in the fields such as food industry, chemical industry, environmental protection.But owing to activated carbon variety is few, with low content of technology, lack functionalization high-quality special-purpose activated charcoal, restriction China activated carbon industry is marched toward higher level application.By activated carbon modified process, develop pollutant can be carried out efficiently, the functional activity charcoal of deep purifying, be to reduce activated carbon use cost, expand its range, improve the effective way of its utilization ratio, be the important directions of activated carbon industry future development.
Due to activated carbon to the absorption of pollutant mainly based on micropore filling, adsorbance is limited, and i.e. saturated up to absorption and lose adsorption capacity in the short time, adsorbing saturated activated carbon becomes secondary pollution source, and it must be carried out regeneration processes can be again with.Regeneration method of active carbon can be divided into two classes generally at present: one is to manage to make adsorbate be desorbed, i.e. by creating the condition (introduce material or energy make reaction force attenuation adsorption molecule and activated carbon between or disappearance) corresponding with underload, remove adsorbate；Two structures being dependent on thermal decomposition or redox reaction destruction adsorbate, remove adsorbate.Traditional renovation process mainly has the regeneration of hot recycling, chemicals, solvent reclamation, bio-regeneration etc., but owing to it exists, efficiency is low, expend the defects such as height, operating condition harshness, complex process, and conventional regeneration method can not meet the demand of present industrial development.Therefore a kind of focus becoming research the most both at home and abroad at normal temperature, normal pressure, low cost, high efficiency, the simple renovation process of operating procedure is developed.
2009, China scientist was found that the conjugated polymer graphite phase carbon nitride (g-C of not metallic components with Germany, Japanese Scientists cooperation3N4) visible-light photocatalysis material, and utilize density of states Functional Theory (DFT) and electrochemical method, have studied the band structure of carbonitride, find g-C3N4There is typical semiconductor energy band structure,sp 2The N of hydridization2 pTrack constitutes g-C3N4Highest occupied molecular orbital (HOMO), and C2 pHybridized orbit then forms its lowest unoccupied molecular orbital (LUMO), and band gap is about 2.7eV, and specific surface area is 10 m2/ g,λ> under 387 nm visible light-inducings, can catalytic oxidation-reduction reaction.But, g-C3N4Polymer there is also some problems as photochemical catalyst, exciton binding energy as little in specific surface area, generation photo-generated carrier is high, quantum efficiency is low and energy gap is bigger than normal (λ＜ 460 nm) and can not effectively utilize sunshine etc..For these problems, scientists is around g-C3N4Carry out substantial amounts of research work to improve g-C3N4The specific surface area of catalyst, the absorption region to spectrum, the separative efficiency etc. of photo-generated carrier.
Summary of the invention
It is an object of the invention to provide a kind of g-C3N4Functional charcoal sorbing material of/ZnO/ activated carbon and preparation method thereof, the g-C prepared3N4The functional charcoal sorbing material of/ZnO/ activated carbon, removes pollutant ability high, and easy in inactivation, service life is not long, and can Photocatalytic Regeneration in situ.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of g-C3N4In the functional charcoal sorbing material of/ZnO/ activated carbon, the content of ZnO is 2 ~ 5wt.%, g-C3N4Content be 3 ~ 8wt.%.
Preparation method comprises the following steps:
(1) carry out pulverizing, sieve and drying by wooden or bamboo raw material；
(2) take the raw material after 10g is dried under high pure nitrogen is protected with the ramp of 5 DEG C/min to 400 ~ 450 DEG C, and be incubated 1-2h, naturally cool to room temperature；
(3) under agitation toward addition 1g ~ 3g zinc acetate in 50 mL distilled water, after reaction 20min, add 1.5 ~ 5g melamine, continue stirring reaction 30min, after the material prepared with step (2) is sufficiently mixed, impregnate 24h, dry at 80 DEG C；
(4) material that step (3) prepares is risen to 500 DEG C with the speed of 10 DEG C/min by room temperature under high pure nitrogen is protected, constant temperature 2 h, then rise to 530 DEG C, and constant temperature 5h with the speed of 0.2 DEG C/min, naturally cool to room temperature, obtain described g-C3N4The functional charcoal sorbing material of/ZnO/ activated carbon.
The remarkable advantage of the present invention is: the g-C that the present invention prepares3N4The functional charcoal sorbing material of/ZnO/ activated carbon, removes pollutant ability high, and easy in inactivation, service life is not long, and can Photocatalytic Regeneration in situ.It has the biggest potential using value in deep treatment organic pollution aquifer.
Accompanying drawing explanation
Fig. 1 is g-C3N4The XRD spectrum of/ZnO/AC.
Fig. 2 is g-C3N4The N of/ZnO/AC and AC2Adsorption-desorption curve map.
Fig. 3 is g-C under illumination and dark adsorption conditions3N4The removal situation of/ZnO/AC and AC Pyrogentisinic Acid.
Fig. 4 is g-C under illumination condition3N4/ ZnO/AC and AC reuses the removal effect of 6 Pyrogentisinic Acids.
Fig. 5 is g-C3N4/ ZnO/AC, g-C3N4/ AC and AC Photocatalytic Regeneration effect.1、g-C3N4/ ZnO/AC, 2, g-C3N4/ AC, 3, AC.
Detailed description of the invention
Embodiment
1
A kind of g-C3N4The preparation method of the functional charcoal sorbing material of/ZnO/ activated carbon comprises the following steps:
(1) carry out pulverizing, sieve and drying by wooden or bamboo raw material；
(2) take the raw material after 10g is dried under high pure nitrogen is protected with the ramp of 5 DEG C/min to 400 DEG C, and be incubated 2h, naturally cool to room temperature；
(3) under agitation toward addition 1g zinc acetate in 50 mL distilled water, after reaction 20min, add 1.5g melamine, continue stirring reaction 30min, after the material prepared with step (2) is sufficiently mixed, impregnate 24h, dry at 80 DEG C；
(4) material that step (3) prepares is risen to 500 DEG C with the speed of 10 DEG C/min by room temperature under high pure nitrogen is protected, constant temperature 2 h, then rise to 530 DEG C, and constant temperature 5h with the speed of 0.2 DEG C/min, naturally cool to room temperature, obtain described g-C3N4The functional charcoal sorbing material of/ZnO/ activated carbon, in functional charcoal sorbing material, the content of ZnO is 2wt.%, g-C3N4Content be 3wt.%.
Embodiment
2
A kind of g-C3N4The preparation method of the functional charcoal sorbing material of/ZnO/ activated carbon comprises the following steps:
(1) carry out pulverizing, sieve and drying by wooden or bamboo raw material；
(2) take the raw material after 10g is dried under high pure nitrogen is protected with the ramp of 5 DEG C/min to 420 DEG C, and be incubated 1h, naturally cool to room temperature；
(3) under agitation toward addition 3g zinc acetate in 50 mL distilled water, after reaction 20min, add 5g melamine, continue stirring reaction 30min, after the material prepared with step (2) is sufficiently mixed, impregnate 24h, dry at 80 DEG C；
(4) material that step (3) prepares is risen to 500 DEG C with the speed of 10 DEG C/min by room temperature under high pure nitrogen is protected, constant temperature 2 h, then rise to 530 DEG C, and constant temperature 5h with the speed of 0.2 DEG C/min, naturally cool to room temperature, obtain described g-C3N4The functional charcoal sorbing material of/ZnO/ activated carbon, in functional charcoal sorbing material, the content of ZnO is 5wt.%, g-C3N4Content be 8wt.%.
Embodiment
3
A kind of g-C3N4The preparation method of the functional charcoal sorbing material of/ZnO/ activated carbon comprises the following steps:
(1) carry out pulverizing, sieve and drying by wooden or bamboo raw material；
(2) take the raw material after 10g is dried under high pure nitrogen is protected with the ramp of 5 DEG C/min to 450 DEG C, and be incubated 1.5h, naturally cool to room temperature；
(3) under agitation toward addition 2g zinc acetate in 50 mL distilled water, after reaction 20min, add 3g melamine, continue stirring reaction 30min, after the material prepared with step (2) is sufficiently mixed, impregnate 24h, dry at 80 DEG C；
(4) material that step (3) prepares is risen to 500 DEG C with the speed of 10 DEG C/min by room temperature under high pure nitrogen is protected, constant temperature 2 h, then rise to 530 DEG C, and constant temperature 5h with the speed of 0.2 DEG C/min, naturally cool to room temperature, obtain described g-C3N4The functional charcoal sorbing material of/ZnO/ activated carbon, in functional charcoal sorbing material, the content of ZnO is 3.5wt.%, g-C3N4Content be 5wt.%.
Fig. 1 is g-C3N4The XRD spectra of/ZnO/AC, it can be seen that g-C3N4There is g-C in/ZnO/ activated carbon3N4With two phases of ZnO, in spectrogram 13.2oWith 27.6oThe diffraction maximum at place corresponds respectively to g-C3N4(100) crystal face and (002) crystallographic plane diffraction peak.In spectrogram 31.7o、34.4o、36.2o、47.5o、56.5oThe diffraction maximum at place corresponds respectively to (100) crystal face of ZnO, (002) crystal face, (101) crystal face, (102) crystal face, the diffraction maximum of (110) crystal face.
Fig. 2 is g-C3N4The N of/ZnO/AC2Adsorption-desorption curve map.It can be seen that g-C3N4The adsorption isotherm of/ZnO/AC presents IV type (IUPAC classification) adsorption-desorption isothermal and hysteresis loop.When relative pressure is relatively low, adsorbance raises along with relative pressure and is gradually increased, now N2Molecule adsorbs at internal surface of hole with single or multiple lift；Adsorption equilibrium is basically reached when relative pressure is 0.1；Increase adsorbance then as relative pressure is slowly increased, and works as N2When relative pressure is 0.95, adsorbance produces hop, and this is due to N2Mesopore orbit occurs caused by capillary condensation.As can be seen here, g-C3N4Based on micropore in/ZnO/AC, there is part mesopore.
Fig. 3 is g-C under illumination and dark adsorption conditions3N4The removal situation of/ZnO/AC and AC Pyrogentisinic Acid.It can be seen that the g-C prepared with this technique3N4/ ZnO/AC not only has adsorption function, but also has photo-catalysis function.At dark adsorption conditions, g-C3N4The adsorbance of/ZnO/AC is slightly less than AC；But g-C under illumination condition3N4The removal effect of/ZnO/AC Pyrogentisinic Acid is significantly higher than the removal effect of AC Pyrogentisinic Acid.
Fig. 4 is g-C under illumination condition3N4/ ZnO/AC and AC reuses the removal effect experiment of 6 Pyrogentisinic Acids, it can be seen that g-C3N4The removal effect of/ZnO/AC Pyrogentisinic Acid is significantly better than AC, under the same conditions g-C3N4/ ZnO/AC reuses after 6 the clearance of Pyrogentisinic Acid 91.6%.And Pyrogentisinic Acid plays removal effect hardly after AC reuses 3 times.
Being mixed with melamine by activated carbon, and after being fully ground, sample is under high pure nitrogen is protected, and with the ramp of 2 DEG C/min to 480 DEG C, after insulation 2h, then the ramp of 1 DEG C/min is to 520 DEG C, is incubated 2h, naturally cools to room temperature, prepares g-C3N4/AC.Fig. 5 is g-C3N4/ ZnO/AC, g-C3N4/ AC and AC adsorb under lucifuge part saturated after Photocatalytic Regeneration effect experimental (experimental technique: g-C under light illumination3N4/ ZnO/AC, g-C3N4/ AC and AC adsorb under the conditions of lucifuge saturated after, centrifugation goes out g-C3N4/ ZnO/AC, g-C3N4/ AC and AC is separately added in distilled water, regenerates under sunshine illumination, and after regeneration, centrifugation goes out g-C3N4/ ZnO/AC, g-C3N4/ AC and AC is respectively put in the water body of certain pollutant levels again and carries out adsorbing pollutant).It can be seen that g-C under similarity condition3N4/ ZnO/AC effect is best, secondly g-C3N4/ AC, and AC is almost without regeneration effect.
Under illumination and dark condition, the purification effect to pollutant is tested:
Light-catalyzed reaction is carried out in homemade quartz/glass clamp shell type reactor (250 ml), the built-in 350 W xenon short-arc lamp (λ of quartz/glass tubeML=450 nm, filter off λ with glass optical filtering pipeMLThe light of ＜ 400 nm) be visible light source, to reactor outer layer chuck be passed through cooling water so that reaction temperature maintains (25 ± 1) DEG C, reactor outer layer with aluminium foil be coated with, to avoid other light to disturb.Lucifuge magnetic agitation 120 min before light-catalyzed reaction, makes catalyst surface absorption reach balance, and is passed through 60 ml/min air, be used for stirring and complement lysis oxygen, and catalyst amount is 1.0 g/L.Sample after reaction certain time, by the concentration of chromatogram detection test substance.
Under sunshine, the clean-up effect to pollutant is tested:
Claim 0.1 g catalyst to pour the plate of a diameter of 15 cm into, add pollutant solution 100 ml to be measured of 0.05 g/L, adsorb 120 min under magnetic stirring, then seal plate mouth with preservative film, be placed under sunshine irradiation.After illumination terminates, sampling, by the concentration of chromatogram detection test substance.
Application examples 1
Table 1 is g-C under sunshine3N4/ZnO/AC、g-C3N4/ AC and AC is to nitrobenzene-containing purification of waste water effect experimental.By table it can be seen that g-C3N4/ ZnO/AC p-nitrophenyl clean-up effect is significantly better than g-C3N4/ AC and AC p-nitrophenyl clean-up effect.
Table 1 g-C3N4/ZnO/AC、g-C3N4/ AC and AC is to nitrobenzene-containing purification of waste water effect
Application examples 2
Table 2 is g-C under sunshine3N4/ZnO/AC、g-C3N4/ AC and AC is to containing ortho-chlorotolu'ene purification of waste water effect experimental.By table it can be seen that g-C3N4/ ZnO/AC is significantly better than g-C to ortho-chlorotolu'ene clean-up effect3N4/ AC and AC is to ortho-chlorotolu'ene clean-up effect.
Table 2 g-C3N4/ZnO/AC、g-C3N4/ AC and AC is to containing ortho-chlorotolu'ene purification of waste water effect
Application examples 3
Table 3 is g-C under sunshine3N4/ZnO/AC、g-C3N4/ AC and AC tests containing aniline waste water clean-up effect.By table it can be seen that g-C3N4/ ZnO/AC is significantly better than g-C to aniline clean-up effect3N4/ AC and AC is to containing aniline clean-up effect.
Table 3 g-C3N4/ZnO/AC、g-C3N4/ AC and AC is to containing aniline waste water clean-up effect
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent and modification, all should belong to the covering scope of the present invention.
Claims (2)
1. a g-C3N4The preparation method of the functional charcoal sorbing material of/ZnO/ activated carbon, it is characterised in that: in functional charcoal sorbing material, the content of ZnO is 2 ~ 5wt.%, g-C3N4Content be 3 ~ 8wt.%；Its preparation method comprises the following steps:
(1) carry out pulverizing, sieve and drying by wooden or bamboo raw material；
(2) take the raw material after 10g is dried under high pure nitrogen is protected with the ramp of 5 DEG C/min to 400 ~ 450 DEG C, and be incubated 1 ~ 2h, naturally cool to room temperature；
(3) under agitation toward addition 1g ~ 3g zinc acetate in 50 mL distilled water, after reaction 20min, add 1.5 ~ 5g melamine, continue stirring reaction 30min, after the material prepared with step (2) is sufficiently mixed, impregnate 24h, dry at 80 DEG C；
(4) material that step (3) prepares is risen to 500 DEG C with the speed of 10 DEG C/min by room temperature under high pure nitrogen is protected, constant temperature 2 h, then rise to 530 DEG C, and constant temperature 5h with the speed of 0.2 DEG C/min, naturally cool to room temperature, obtain described g-C3N4The functional charcoal sorbing material of/ZnO/ activated carbon.
2. the g-C that a preparation method as claimed in claim 1 prepares3N4The application of the functional charcoal sorbing material of/ZnO/ activated carbon, it is characterised in that: described g-C3N4/ ZnO/ activated carbon is used for administering organic pollution aquifer.
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