CN101708457B - Preparation method and application of activated carbon loaded nano-iron material - Google Patents
Preparation method and application of activated carbon loaded nano-iron material Download PDFInfo
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- CN101708457B CN101708457B CN2009100906161A CN200910090616A CN101708457B CN 101708457 B CN101708457 B CN 101708457B CN 2009100906161 A CN2009100906161 A CN 2009100906161A CN 200910090616 A CN200910090616 A CN 200910090616A CN 101708457 B CN101708457 B CN 101708457B
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- pentachlorophenol
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Abstract
The invention relates to a preparation method and an application of an activated carbon loaded nano-iron material. The material is prepared by using potassium borohydride as a reducing agent for reducing ferrous ions into nonvalent nano-iron. The grain diameter of the nano-iron grains formed by reaction is ensured to be below 100 nanometers through controlling reactant concentration and dropwise adding speed. In the reaction process, preprocessed activated carbon is used as a load material, and the nonvalent nano-iron grains generated through the reaction are fully dispersed and loaded on the activated carbon by utilizing the porous characteristic of the activated carbon. Meanwhile, argon is led in and an ultrasonoscope is used for assisting dispersion so as to enhance the dispersive action of the nano-iron grains, and the activated carbon loaded nano-iron material is obtained. The preparation method of the material is simple, the used raw materials are low in price and easy to obtain, has no special requirements for external environmental conditions and occupies small space. The nano-iron loaded on the activated carbon has good dispersive property and more uniform grain diameter distribution; and the activated carbon loaded nano-iron material is applied to the degradation processing of pentachlorophenol, integrates the good absorption performance and the strong reducing property of the nano-iron and has good processing effect.
Description
Technical field
The invention belongs to the nano material preparation technical field, be specifically related to a kind of preparation method and application thereof of activated carbon loaded nano-iron material.
Background technology
Activated carbon has apolar surfaces, is hydrophobicity and close organic adsorbent, and it has stable performance, cancer resistance, adsorption capacity big with advantages such as desorb is easy, warp repeatedly cycling still can keep original absorption property.Activated carbon mainly is made up of C, H, three kinds of elements of O.Carbon atom exists with class graphitic carbon form.The physical arrangement of activated carbon is by macropore, and mesopore (being transitional pore) and micropore are formed, and pore structure accounts for 80～90% of cumulative volume.General big bore dia is greater than 100nm, and the transitional pore diameter is between 4～100nm, and micro-pore diameter is less than 4nm.In the process of absorption, bigger Molecular Adsorption is in macropore, and more a little bit smaller molecule gets into micropore through transitional pore.Exactly because activated carbon has flourishing microcellular structure, so have huge specific area.In addition, because the existence of carbon surface of solids atom unsaturation, they will combine atom and atomic radical beyond the carbon component with chemical species, form various surface functional groups, thereby make activated carbon produce various characterization of adsorptions.These functional groups mainly are oxygen-containing functional groups, and like hydroxyl, carbonyl, carboxyl, lactone group etc., hydroxyl, ether account for 25%, and carbonyl, carboxyl, ester group account for 10%.
The nano-level iron particle is reunited owing to receive the actings in conjunction such as magnetostatic power and surface tension between telluric magnetic force, granule easily.The introducing of activated carbon can play peptizaiton to the nanometer iron that generates in the solution, reduces the probability that reunion takes place for it.Simultaneously; Because activated carbon has the good adsorption performance; Activated carbon loaded nano-iron material can be brought into play the suction-operated of activated carbon and the reduction of nanometer iron simultaneously, can more effectively be used for organic pollution and handle, especially the lower zone of pollutant levels.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and application thereof of activated carbon loaded nano-iron material,
The objective of the invention is to realize like this: with the potassium borohydride is that reducing agent is reduced into Zero-valent Iron with ferrous salt.Guarantee that through control reactant concentration and rate of addition the iron particle grain size is below 100nm.In course of reaction, adopt pretreated activated carbon as support materials, the Zero-valent Iron of utilizing the mushy characteristic of activated carbon that reaction is produced is fully disperseed and is loaded on the activated carbon.Make reactor keep anaerobic state on the one hand to stop the oxidation of Zero-valent Iron through argon gas simultaneously, the micro-bubble of aeration head generation also can be brought into play the effect of dispersion on the one hand.And through the ultrasonoscope aid dispersion.
After the activated carbon loaded nano-iron material preparation is accomplished, adopt vacuum drying chamber at room temperature dry, dried sample is used to handle pentachlorophenol.
Preparation process of the present invention comprises the steps:
(1) get the 100g activated carbon in the 500mL there-necked flask, add about 200mL deionized water, place and stir the constant temperature electric heating cover, boil 3h, cooling final vacuum suction filtration is collected filter residue, 110 ℃ of oven dry down, is stored in the drier subsequent use;
(2) take by weighing activated carbon 50g that step (1) obtains in the 500mL there-necked flask, the FeSO of preparation 0.02mol/L-0.10mol/L
4Solution 100mL pours there-necked flask into, under the situation of logical argon gas, makes FeSO
4Solution fully mixes with activated carbon, in flask, drips the KBH of 0.1mol/L-0.5mol/L behind the stirring 1h
4Solution 100mL; Whole process continues logical argon gas and forms vigorous stirring; And through the ultrasonoscope aid dispersion, question response finishes, leave standstill after continuing to stir 5-15min, and the rapid vacuum filtration of the solid after staticly settling, and be transferred to 110 ℃ of dryings of vacuum drying chamber immediately.
Said whole process continues logical argon gas and forms the argon flow amount 0.5-1L/min of vigorous stirring.
And the material of the method preparation is used for the degraded of pentachlorophenol.
The present invention compared with prior art has the following advantages:
1. material preparation method is simple, and entire reaction course can be accomplished under temperate condition, and raw materials used cheap and easy to get, environmental condition does not have specific (special) requirements to external world, and it is little to take up room.
2. with respect to nanometer iron powder, activated carbon loaded nanometer iron good dispersion, particle diameter distributes more even;
3. with respect to the existing treatment technology of pentachlorophenol, the prepared collection of material of the present invention good adsorption properties and the strong reducing property of nanometer iron of activated carbon, treatment effect is good.
Description of drawings
Fig. 1 is SEM figure for prepared activated carbon loaded nano-iron material: a in the embodiment of the invention 1, and b is the EDS analysis result.
Fig. 2 is the ESEM figure of prepared nanometer iron in the embodiment of the invention 2.
The Cl of Fig. 3 for discharging in the system
-Testing result.
The specific embodiment
Below in conjunction with embodiment technical scheme of the present invention is further specified:
The preparation of embodiment 1 activated carbon loaded nano-iron material,
(1) get the 100g activated carbon in the 500mL there-necked flask, add about 200mL deionized water, place and stir the constant temperature electric heating cover, boil 3h, cooling final vacuum suction filtration is collected filter residue, 110 ℃ of oven dry down, is stored in the drier subsequent use;
(2) take by weighing activated carbon activated carbon 50g that step (1) obtains in the 500mL there-necked flask, the FeSO of preparation 0.02mol/L-0.10mol/L
4Solution 100mL pours there-necked flask into, under the situation of logical argon gas, makes FeSO
4Solution fully mixes with activated carbon, in flask, drips the KBH of 0.2mol./L behind the stirring 1h
4Solution 100mL; Whole process continues logical argon gas and vigorous stirring; And through 250W ultrasonoscope aid dispersion, question response finishes, leave standstill after continuing to stir a period of time 5-15min, and the rapid vacuum filtration of the solid after staticly settling, and be transferred to 110 ℃ of dryings of vacuum drying chamber immediately.Dried sample is observed through ESEM, SEM photo that obtains (shown in Fig. 1 a) and EDS analysis result (shown in Fig. 1 b).
(1) the preparation initial concentration is the pentachlorophenol aqueous solution of 50mg/L-500mg/L; With 18mL reagent bottle (band plug) is reactor; Add the 10-15mL pentachlorophenol aqueous solution and the prepared activated carbon loaded nano-iron material of 10-15mg in each reaction bulb; Be placed in the desk-top constant-temperature shaking culture case with plug sealing and react, vibration oven temperature, degree is made as 30 ℃, and rotating speed is made as 100-150rpm.With the active carbon material of loaded with nano-iron not as control samples.
(2) in the different time sampling, adopt ultraviolet-visible spectrophotometer to analyze pentachlorophenol and organic product thereof, adopt the chlorion that produces in the ion chromatography system.The degradation process of the quantitative detecting analysis pentachlorophenol through organic matter and chlorion.
The activated carbon loaded nano-iron material concentration of treatment that accompanying drawing 2 has provided iron theoretical negative carrying capacity 10% is the UV spectrogram behind the pentachlorophenol 0.5h of 50mg/L; As can be seen from the figure; Solution behind the reaction 0.5h has not had the peak to occur between 200-400nm, explains that the pentachlorophenol in the solution is removed fully.
Accompanying drawing 3 has provided the Cl that discharges in the system
-Testing result.The active carbon material of loaded with nano-iron not though also can within a certain period of time pentachlorophenol be removed, fails to detect Cl in system
-The suction-operated that activated carbon is described mainly is with the pentachlorophenol enrichment.Nano iron particles can be with the pentachlorophenol dechlorination.
Claims (3)
1. the preparation method of an activated carbon loaded nano iron is characterized in that the preparation method comprises the steps:
(1) get the 100g activated carbon in the 500mL there-necked flask, add the 200mL deionized water, place and stir the constant temperature electric heating cover, boil 3h, cooling final vacuum suction filtration is collected filter residue, 110 ℃ of oven dry down, is stored in the drier subsequent use;
(2) take by weighing activated carbon 50g that step (1) obtains in the 500mL there-necked flask, the FeSO of preparation 0.02mol/L-0.10mol/L
4Solution 100mL pours there-necked flask into, under the situation of logical argon gas, makes FeSO
4Solution fully mixes with activated carbon, in flask, drips the KBH of 0.1mol/L-0.5mol/L behind the stirring 1h
4Solution 100mL; Whole process continues logical argon gas and vigorous stirring; And through the ultrasonoscope aid dispersion, question response finishes, leave standstill after continuing to stir 5-15min, and the rapid vacuum filtration of the solid after staticly settling, and be transferred to 110 ℃ of dryings of vacuum drying chamber immediately.
2. the preparation method of a kind of activated carbon loaded nano iron according to claim 1 is characterized in that: the argon flow amount that said whole process continues to lead to argon gas and form vigorous stirring is 0.5-1L/min.
3. the prepared application of activated carbon loaded nano-iron material in the degraded pentachlorophenol of claim 1 is characterized in that experimental procedure is following:
(1) the preparation initial concentration is the pentachlorophenol solution of 50mg/L-500mg/L; With 18mL band plug reagent bottle is reactor; Add the 10-15mL pentachlorophenol aqueous solution and the prepared activated carbon loaded nano-iron material of 10-15mg in each reaction bulb; Be placed in the desk-top constant-temperature shaking culture case with plug sealing and react, vibration oven temperature, degree is made as 20-40 ℃, and rotating speed is made as 100-150rpm.
(2) adopt ultraviolet-visible spectrophotometer to analyze pentachlorophenol and organic product thereof, adopt the chlorion that produces in the ion chromatography system; In different time sampling, the degradation process of the quantitative detecting analysis pentachlorophenol through organic matter and chlorion.
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| CN101862639B (en) * | 2010-06-21 | 2012-07-18 | 黑龙江省农业科学院农村能源研究所 | Preparation method of modified activated carbon fiber loaded metal ion methane desulfurizer |
| CN102266782B (en) * | 2011-06-13 | 2013-04-03 | 清华大学 | Method for producing nano Fe(O)/CeO2 composite material and application in removing chlorophenol pollutant thereof |
| CN103721715B (en) * | 2013-11-28 | 2016-02-03 | 温州大学 | A kind of load type active carbon zero-valent iron material |
| CN105081305B (en) * | 2014-05-04 | 2018-10-09 | 山东碧泉环境工程技术有限公司 | Porous nano Zero-valent Iron and porous nano zero-valent iron composite material |
| CN104084125B (en) * | 2014-06-25 | 2016-08-24 | 华南理工大学 | A kind of sintering activity charcoal loading Nanoscale Iron and its preparation method and application |
| CN104308181B (en) * | 2014-10-17 | 2017-01-11 | 浙江工业大学 | Method for preparing nanoscale zero-valent iron and nanoscale duplex metal Cu/Fe |
| CN105461042A (en) * | 2015-12-22 | 2016-04-06 | 镇江市自来水公司 | Preparation method of carbon based nano-iron alloy water treatment material |
| CN105854797A (en) * | 2016-04-11 | 2016-08-17 | 中国矿业大学 | Preparation method and application of nanometer zero-valence bimetal-supported functional charcoal |
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| CN106964197B (en) * | 2017-04-26 | 2019-11-19 | 吉林师范大学 | A kind of Supported On Granular Activated Carbon Nanoscale Iron composite filter element material and preparation method thereof |
| CN107243358B (en) * | 2017-06-09 | 2020-02-21 | 北京农学院 | Nanoscale zero-valent iron carrier and preparation method and application thereof |
| CN108187623A (en) * | 2018-03-01 | 2018-06-22 | 哈尔滨工业大学 | A kind of preparation method for effectively removing the green composite Nano magnetic material of heavy metal in environment |
| CN108714413A (en) * | 2018-06-08 | 2018-10-30 | 湖南农业大学 | One Yeasts carry nano zero valence iron and application thereof |
| CN110220766B (en) * | 2019-06-21 | 2021-10-22 | 辽宁石油化工大学 | Method for quantitatively collecting phenol in water environment through composite material |
| CN111118075A (en) * | 2019-11-27 | 2020-05-08 | 同济大学 | Method for deodorizing kitchen waste and simultaneously strengthening acid production |
| CN114601066A (en) * | 2022-03-30 | 2022-06-10 | 浙江大飞龙动物保健品股份有限公司 | Anti-diarrhea pig creep feed and preparation method thereof |
| CN116395919B (en) * | 2023-06-09 | 2023-11-14 | 威海蓝创环保设备有限公司 | Nitroimidazole-containing wastewater treatment process |
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| CN101481155A (en) * | 2009-03-03 | 2009-07-15 | 同济大学 | Composite material for water treatment, and preparation and use thereof |
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