CN1724138A - Porous carbon adsorbing agent containing nano zinc oxide micropartical and its preparation process and application - Google Patents

Porous carbon adsorbing agent containing nano zinc oxide micropartical and its preparation process and application Download PDF

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Publication number
CN1724138A
CN1724138A CN 200510035312 CN200510035312A CN1724138A CN 1724138 A CN1724138 A CN 1724138A CN 200510035312 CN200510035312 CN 200510035312 CN 200510035312 A CN200510035312 A CN 200510035312A CN 1724138 A CN1724138 A CN 1724138A
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porous carbon
zine oxide
nano zine
carbon adsorbent
oxide particulate
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CN100336587C (en
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陈水挟
冯飞月
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Sun Yat Sen University
National Sun Yat Sen University
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National Sun Yat Sen University
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Abstract

A porous charcoal adsorbent for cleaning environment is composed of porous charcoal as carrier and zinc oxide nano-particles as active component. Its preparing process includes such steps as reaction between zinc nitrate micro-emulsion and sodium hydroxide to obtain zinc oxide nano-particles, carrying them by porous charcoal and heat treating. Its advantages are high absorptive power and high photo-catalytic and antibacterial activities.

Description

Contain porous carbon adsorbent of nano zine oxide particulate and its production and use
Technical field
The present invention relates to a kind of porous carbon adsorbent that contains the nano zine oxide particulate and preparation method thereof, and this porous carbon adsorbent is used for the purifying volatile organic pollution and as the purposes of anti-biotic material.
Background technology
Nano material has crucial application prospect because of character such as its distinctive particle size and surface characteristic and the distinctive photochemical catalyst character of nano material thereof and antibiotic, deodorizing thereof, sterilizations in the environmental protection field.Nano-ZnO is a kind of novel high function fine inorganic material, and its particle diameter is between 1~100nm.Because the granular of particle size, make nano-ZnO produce the not available skin effect of its body bulk material, small-size effect, quantum effect and macro quanta tunnel effect etc., thereby make nano-ZnO have some special performances at aspects such as magnetic, light, electricity, sensitivities.Nano-ZnO has the effect of catalyst and photochemical catalyst under the irradiation of ultraviolet light, and energy decomposing organic matter matter can be antibiotic, deodorizing and sterilization, protection and environment purification.
Porous carbon material has abundant microporous and high specific area, and its adsorption capacity is higher than other porous adsorbing materials such as polymeric adsorbent, zeolite, silica gel etc. far away; Also more much better than its like product active carbon.Porous carbon adsorbent is bigger several times even tens times than granular activated charcoal to the adsorbance of organic steam; And because NACF and the strong active force of adsorbate, its micropore directly contacts with adsorbate, has reduced the distance of diffusion.The absorption of porous carbon adsorbent and gas can reach balance in tens of seconds to several minutes; NACF has very strong interaction force to organic matter, can adsorb the organic pollution (VOC) of removing ppm, ppb level and even lower concentration.At present, this class material has been applied to the purified treatment to VOC.But, the complexity of technological design and the complexity of use have been increased owing to after the saturated absorption of porous carbon adsorbent, must carry out desorption and regeneration and could continue to use.By the structural change to sorbing material, the realization original position is regenerated in real time, is to improve material to the processing of VOC and the effective way of transformation efficiency.In addition, because carbon surface is easy to breed bacteria, aspect purifying of drinking water, may cause the microorganism secondary pollution especially.
Summary of the invention
The object of the present invention is to provide a kind of porous carbon adsorbent that contains the nano zine oxide particulate and preparation method thereof, and this porous carbon adsorbent is used for the purifying volatile organic pollution and as the purposes of anti-biotic material.
The present invention utilizes the high-specific surface area and the abundant nano-pore structure of porous carbon material, ZnO superfine nano particle is compounded in the surface of porous carbon material by microemulsion method, prepare porous charcoal-nano-ZnO composite---contain the porous carbon adsorbent of nano zine oxide particulate, the good adsorption performance that had both kept porous carbon material has been brought into play the photocatalysis performance and the anti-microbial property of ZnO superfine nano particle again.
The porous carbon adsorbent that contains the nano zine oxide particulate of the present invention is to be formed by nano zine oxide particulate in the porous carbon material load, and wherein nano zine oxide accounts for 5~70% of gross mass.
Described porous carbon material is generally NACF or active carbon.
Described NACF is normally formed through the high temperature cabonization activation by sisal fiber, pitch fibers, phenolic fibre, viscose rayon, PVA fiber or PAN fiber.
Nano zine oxide particulate in the porous carbon adsorbent that contains the nano zine oxide particulate of the present invention can and load on the porous carbon material through the microemulsion method preparation.
The porous carbon adsorbent that contains the nano zine oxide particulate of the present invention can prepare by the following method:
Ethanol, water and zinc nitrate are mixed, add surfactant, be made into microemulsion, add porous carbon material then; Ethanol: water: zinc nitrate: surfactant=(20~30) ml: (60~120) ml: (2~8) g: (15~20) g, the mass ratio of zinc nitrate and porous carbon material are controlled between 0.01: 1~0.5: 1; Stir and to add sodium hydroxide solution down, make to form the zinc hydroxide precipitation, the mol ratio of zinc nitrate and NaOH is 5: 1~1: 3 (mass ratio be about 25: 1~1.5: 1); Elimination solution, washing, drying; The gained solid mixture promptly obtains the required porous carbon adsorbent that contains the nano zine oxide particulate in 300~600 ℃ of calcination 1~2h.Used surfactant is generally dodecyl sodium sulfate, neopelex or softex kw.
The present invention through generating nano zine oxide with the NaOH reaction and being carried on the carrier porous carbon material, makes the porous carbon adsorbent composite of supported nano zinc oxide particulate by the zinc nitrate microemulsion by adopting microemulsion method through heat treatment.Gained porous carbon adsorbent composite has kept porous charcoal to inhale the porous of material, thereby has kept the strong adsorption capacity of material; Simultaneously, the photocatalytic activity and the antibacterial activity of zinc oxide fine particles have superposeed in this material again, make this composite both can be used for catalytic decomposition light-concentration volatile organic pollution, can prevent that again microorganism from the growing of carbon surface, having prevented the secondary pollution of microorganism; Also can be used as the antibacterial bacteriostatic material.Aspect the depollution of environment, has important application prospects.
Test shows:
The porous carbon adsorbent that the present invention contains the nano zine oxide particulate can reach more than the 500mg/g the adsorption capacity of volatile organic contaminant, can reach 20% to the photocatalysis Decomposition rate of volatile organic contaminant.
It is 10 that the porous carbon adsorbent that the present invention contains the nano zine oxide particulate can be killed concentration fully 7The Escherichia coli of cfu/mL or staphylococcus aureus.
Therefore, the porous carbon adsorbent that the present invention contains the nano zine oxide particulate can be used for the material as the airborne low concentration volatile organic matter of photocatalysis Decomposition (VOC), or as anti-biotic material.
When the porous carbon adsorbent that contains the nano zine oxide particulate of the present invention is used to adsorb the decomposing volatile organic pollution, the gas that normally will contain VOC is by the above-described porous carbon adsorbent fixed bed that contains the nano zine oxide particulate, and under ultra violet lamp, the gas that contains VOC is fully contacted with the porous carbon adsorbent that contains the nano zine oxide particulate, can be with the VOC catalytic decomposition.
When the porous carbon adsorbent that contains the nano zine oxide particulate of the present invention is used as the antibacterial bacteriostatic material, the solution that normally will contain Escherichia coli or staphylococcus aureus directly contacts 0.5~2h with the porous carbon adsorbent of above-described supported nano zinc oxide particulate, can kill the bacterium in the solution.
The porous carbon adsorbent of supported nano zinc oxide particulate of the present invention carries out under dynamic condition the adsorption capacity of volatile organic contaminant and the mensuration of photocatalysis Decomposition efficient.The gas that contains volatile organic matter that makes certain humidity according to exit concentration, is estimated adsorption capacity or the decomposition efficiency of porous carbon adsorbent to volatile organic matter by above-mentioned porous carbon adsorbent fixed bed.
Description of drawings
Fig. 1 is the sem photograph that contains the acticarbon sample of nano zine oxide particulate.Show the zinc-oxide nano sized particles of activated carbon surface dense distribution, particle is long column shape, and diameter is about about 30nm, and draw ratio is about 3: 1.
Fig. 2 is the sem photograph that contains the activated carbon fiber adsorbing substance sample of nano zine oxide particulate.Show the equally distributed Zinc oxide nanoparticle in NACF surface, size is about about 10~20nm.
Fig. 3 is the X-ray diffracting spectrum that contains the porous carbon adsorbent of nano zine oxide particulate.With database look into standard diagram contrast, be highly purified hexagonal crystal system zinc oxide.XRD material phase analysis result shows that active carbon or the adsorbate above the charcoal fiber mainly are nano-ZnOs, and particle diameter is hexagonal wurtzite structure between 11~24nm.
The specific embodiment
Embodiment 1
In ethanol: the ratio of water: zinc nitrate: surfactant: NACF=30ml: 100ml: 5g: 15g: 5g, ethanol, water and zinc nitrate are mixed, add the surfactant neopelex again, be made into microemulsion; Add NACF then; Stir and press zinc nitrate down: the mol ratio of NaOH=1: 1 adds sodium hydroxide solution (concentration 1 mol), makes to form zinc hydroxide and precipitate.Elimination solution, washing, drying; The gained solid mixture promptly obtains the NACF that product contains the nano zine oxide particulate in 600 ℃ of calcination 1h.The load capacity of zinc oxide is 40%wt in the product.Product is through scanning electron microscope analysis, and the particle that its area load is intensive, particle are the reunion attitude, about aggregation size 1 μ m.Aggregate is made up of many more tiny nano-scale particles.This particle proves the hexagonal crystal system zincite crystal through the X-ray diffraction analysis.
Embodiment 2
In ethanol: the ratio of water: zinc nitrate: surfactant: NACF=20ml: 120ml: 5g: 20g: 5g, ethanol, water and zinc nitrate are mixed, add the surfactant neopelex again, be made into microemulsion; Add NACF then; Stir and press zinc nitrate down: the mol ratio of NaOH=1: 3 adds sodium hydroxide solution (concentration 2 mol), makes to form zinc hydroxide and precipitate.Elimination solution, washing, drying; The gained solid mixture promptly obtains the NACF that product contains the nano zine oxide particulate in 600 ℃ of calcination 1h.The load capacity of zinc oxide is 20% in the product.Product is through scanning electron microscope analysis, and its area load dispersed particle is about particle particle diameter 10~20nm.This particle proves the hexagonal crystal system zincite crystal through the X-ray diffraction analysis.The size of microcrystal that calculates according to X-ray diffraction is 10nm.
Embodiment 3
In ethanol: the ratio of water: zinc nitrate: surfactant: active carbon=30ml: 100ml: 8g: 20g: 5g, ethanol, water and zinc nitrate are mixed, add the surfactant dodecyl sodium sulfate again, be made into microemulsion; Add active carbon then; Stir and press zinc nitrate down: the mol ratio of NaOH=1: 1 adds sodium hydroxide solution (concentration 1 mol), makes to form zinc hydroxide and precipitate.Elimination solution, washing, drying; The gained solid mixture promptly obtains the active carbon that product contains the nano zine oxide particulate in 600 ℃ of calcination 1h.The load capacity of zinc oxide is 65%wt in the product.Product is through scanning electron microscope analysis, the intensive strip hexagonal columnar of its area load crystal, the about 20nm of crystal diameter, the about 300nm of length.This particle proves the hexagonal crystal system zincite crystal through the X-ray diffraction analysis.
Embodiment 4
In ethanol: the ratio of water: zinc nitrate: surfactant: active carbon=30ml: 120ml: 2g: 10g: 30g, ethanol, water and zinc nitrate are mixed, add the surfactant softex kw again, be made into microemulsion; Add active carbon then; Stir and press zinc nitrate down: the mol ratio of NaOH=1: 0.2 adds sodium hydroxide solution (concentration 1 mol), makes to form zinc hydroxide and precipitate.Elimination solution, washing, drying; The gained solid mixture promptly obtains the active carbon that product contains the nano zine oxide particulate in 600 ℃ of calcination 2h.The load capacity of zinc oxide is 10%wt in the product.Product is through scanning electron microscope analysis, the intensive granular crystal of its area load, the about 20nm of particle diameter.This particle proves the hexagonal crystal system zincite crystal through the X-ray diffraction analysis.
Embodiment 5
In ethanol: the ratio of water: zinc nitrate: surfactant: active carbon=30ml: 100ml: 2g: 10g: 50g, ethanol, water and zinc nitrate are mixed, add the surfactant neopelex again, be made into microemulsion; Add active carbon then; Stir and press zinc nitrate down: the mol ratio of NaOH=1: 3 adds sodium hydroxide solution (concentration 0.1 mol), makes to form zinc hydroxide and precipitate.Elimination solution, washing, drying; The gained solid mixture promptly obtains the active carbon that product contains the nano zine oxide particulate in 600 ℃ of calcination 1h.The load capacity of zinc oxide is 5%wt in the product.Product is through scanning electron microscope analysis, its area load dispersed particle, the about 20nm of particle particle diameter.This particle proves the hexagonal crystal system zincite crystal through the X-ray diffraction analysis.Particle is through transmission electron microscope analysis, and the visible particles size evenly has reunion slightly, and particle diameter is between 10~24nm, and the shape of particle has hexagonal prism type and trend ball-type.
Embodiment 6
In ethanol: the ratio of water: zinc nitrate: surfactant: active carbon=30ml: 100ml: 5g: 10g: 2.5g, ethanol, water and zinc nitrate are mixed, add the surfactant neopelex again, be made into microemulsion; Add active carbon then; Stir and press zinc nitrate down: the mol ratio of NaOH=1: 1 adds sodium hydroxide solution (concentration 1 mol), makes to form zinc hydroxide and precipitate.Elimination solution, washing, drying; The gained solid mixture promptly obtains the NACF that product contains the nano zine oxide particulate in 300 ℃ of calcination 1h.The load capacity of zinc oxide is 70%wt in the product.Product is through scanning electron microscope analysis, the blocky-shaped particle thing that its area load is intensive, and particle is the reunion attitude, about aggregation size 1 μ m.Aggregate is made up of many more tiny nano-scale particles.This particle proves the hexagonal crystal system zincite crystal through the X-ray diffraction analysis.
Embodiment 7
To contain the fixed bed of the gas of VOC toluene vapor by the porous carbon adsorbent of load zinc-oxide nano particulate.Gas flow rate is 300mL/min, and the inlet toluene concentration is 2mg/L, relative humidity 85%.Absorption is carried out at ambient temperature.When exit concentration was identical with entrance concentration, the porous charcoal of computational load zinc-oxide nano particulate was 500mg/g to the absorption total amount of toluene.
Embodiment 8
To contain the fixed bed of the gas of VOC toluene vapor by the porous carbon adsorbent of load zinc-oxide nano particulate.Gas flow rate is 300mL/min, and the inlet toluene concentration is 2mg/L, relative humidity 85%.Absorption is carried out at ambient temperature.Do not having under the light conditions, the outlet toluene concentration is 0.2mg/L; Under the UV-irradiation situation, the outlet toluene concentration is 0.16mg/L.Show that this material has strong catalytic decomposition ability to toluene, the photocatalysis Decomposition rate of toluene is 20% under this condition.
Embodiment 9
Containing the Escherichia coli counting at 20 milliliters is 4 * 10 6It is 4 * 10 that the solution neutralization of cfu/ml contains the staphylococcus aureus counting 6In the solution of cfu/ml, the NACF that adds 50mg load Zinc oxide nanoparticle respectively, contact after 2 hours, the detection of Escherichia coli in the solution and staphylococcus aureus is shown that it is 4 * 10 that the NACF of load zinc-oxide nano particulate can contain 20ml bacterial concentration 6Escherichia coli or the staphylococcus aureus of cfu/ml are killed fully.

Claims (10)

1. a porous carbon adsorbent that contains the nano zine oxide particulate is characterized in that this porous carbon adsorbent is to be formed by nano zine oxide particulate in the porous carbon material load, and wherein nano zine oxide accounts for 5~70% of gross mass.
2. a porous carbon adsorbent as claimed in claim 1 is characterized in that described porous carbon material is NACF or active carbon.
3. a porous carbon adsorbent as claimed in claim 2 is characterized in that described NACF is formed through the high temperature cabonization activation by sisal fiber, pitch fibers, phenolic fibre, viscose rayon, PVA fiber or PAN fiber.
4. one kind as the described porous carbon adsorbent of claim 1,2 or 3, it is characterized in that described nano zine oxide particulate is through the microemulsion method preparation and load on the porous carbon material.
5. a preparation method who contains the porous carbon adsorbent of nano zine oxide particulate is characterized in that ethanol, water and zinc nitrate are mixed, and adds surfactant, is made into microemulsion, adds porous carbon material then; Ethanol: water: zinc nitrate: surfactant=(20~30) ml: (60~120) ml: (2~8) g: (15~20) g, the mass ratio of zinc nitrate and porous carbon material are controlled between 0.01: 1~0.5: 1; Stir adding sodium hydroxide solution down, make to form the zinc hydroxide precipitation, the mol ratio of zinc nitrate and NaOH is 5: 1~1: 3; Elimination solution, washing, drying; The gained solid mixture promptly obtains the required porous carbon adsorbent that contains the nano zine oxide particulate in 300~600 ℃ of calcination 1~2h.
6. method as claimed in claim 5 is characterized in that described surfactant is dodecyl sodium sulfate, neopelex or softex kw.
7. the described application that contains the porous carbon adsorbent of nano zine oxide particulate as the material of the airborne low concentration volatile organic matter of photocatalysis Decomposition of one of claim 1~4.
8. according to the described application of claim 7, it is characterized in that to contain the gas of low concentration volatile organic matter by the described porous carbon adsorbent fixed bed that contains the nano zine oxide particulate, and under ultra violet lamp, the gas that contains low concentration volatile organic matter is fully contacted with the porous carbon adsorbent that contains the nano zine oxide particulate, can be with the low concentration volatile organic matter catalytic decomposition.
9. the described application that contains the porous carbon adsorbent of nano zine oxide particulate as anti-biotic material of one of claim 1~4.
10. according to the described application of claim 9, it is characterized in that the solution that will contain Escherichia coli or staphylococcus aureus directly contacts 0.5~2h with the described porous carbon adsorbent that contains the nano zine oxide particulate, can kill the bacterium in the solution.
CNB2005100353127A 2005-06-22 2005-06-22 Porous carbon adsorbing agent containing nano zinc oxide micropartical and its preparation process and application Expired - Fee Related CN100336587C (en)

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