CN109012578A - A kind of methods and applications of chemical ion exchange-roasting method preparation Activated Carbon with Cu - Google Patents

A kind of methods and applications of chemical ion exchange-roasting method preparation Activated Carbon with Cu Download PDF

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Publication number
CN109012578A
CN109012578A CN201810705696.6A CN201810705696A CN109012578A CN 109012578 A CN109012578 A CN 109012578A CN 201810705696 A CN201810705696 A CN 201810705696A CN 109012578 A CN109012578 A CN 109012578A
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active carbon
discarded
activated carbon
solution
ion exchange
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Inventor
夏洪应
蒋鑫
张利波
彭金辉
王仕兴
程松
舒建华
陈权
胡文海
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72Copper
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/40Organic compounds containing sulfur

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
  • Analytical Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The present invention relates to a kind of chemical ion exchange-roasting method preparation Activated Carbon with Cu methods and applications, belong to photocatalysis technology field.Discarded active carbon is placed in distilled water first, is cleaned at room temperature in ultrasonic wave, filter and is dried to obtain the active carbon discarded after cleaning;The active carbon discarded after cleaning is added to Cu (NO according to solid-to-liquid ratio for 10:30 g/mL3)2It in solution, is handled at room temperature in ultrasonic wave, is then that 160 ~ 220 r/min stir 1 ~ 2h in revolving speed;NaHCO is added3Solution, stirring, filtering, filtrate distilled water and ethyl alcohol wash repeatedly, and drying obtains material drying;By obtained material drying according to amount of substance and microwave power ratio is dried as 1:15 ~ 25g/W, 10 ~ 30min of roasting obtains Activated Carbon with Cu under the conditions of maturing temperature is 300 ~ 500 DEG C.The present invention reduces discharge and the environmental pollution of waste, realizes the comprehensive utilization of resources of waste using discarded active carbon as raw material.

Description

A kind of methods and applications of chemical ion exchange-roasting method preparation Activated Carbon with Cu
Technical field
The present invention relates to a kind of chemical ion exchange-roasting method preparation Activated Carbon with Cu methods and applications, belong to light and urge Change technical field.
Background technique
Active carbon is that have pore structure abundant made of a kind of six ring objects accumulation consisting of carbon and huge compare table Area is a kind of excellent adsorbent.Meanwhile active carbon is stablized with chemical property, mechanical strength is high, can be from farm-forestry crop The advantages that middle preparation, so using relatively broad.However as being widely used for active carbon, more and more discarded work are produced Property charcoal.Discarded active carbon is not used, and easily causes environmental pollution to surrounding enviroment.Currently, can only using regeneration method Restore part of it absorption property, so the loaded modified active carbon of common metal, to improve its absorption property.
In recent years, environmental protection ideas and the crisis of resource consciousness of deeply implementing with the Scientific Outlook on Development, people are more and more stronger. Scientific and technical research personnel plan as a whole two aspect of environmental protection and economic benefit, to realize the research of waste material comprehensive utilization by society The increasing concern of meeting.
Currently, the method for common carried metal has impregnation-calcination method, baking mixed method, admixture activation method, chemical gaseous phase The precipitation method, sol-gal process etc..However, these are loaded, the sample dispersion that regeneration methods prepare is poor, load capacity is small, restricts The development and application of new material have great importance so preparing a kind of physical and chemical performance good material.Meanwhile the present invention Using discarded active carbon as the carrier of catalyst, accomplish to turn waste into wealth, waste is recycled.
To disclose in the patent application of 106937647 A of CN, " a kind of novel load silver is living in patent publication No. by applicant Property charcoal Rheological Phase Method ", which is to add water to be tuned into rheology state levigate Tetrasilver tetroxide and active carbon, be mixed evenly, then Potassium peroxydisulfate or sodium peroxydisulfate, sodium hydroxide or potassium hydroxide is added, is tuned into rheology state and vacuumizes reaction, finally use distilled water It rinses 2 ~ 4 times.A variety of auxiliary reagents are added in above method preparation process, and experimental implementation is not only made to have become complicated but also are made Entire process costs increase.
Applicant is to disclose a kind of " magnesium oxide-based work in the patent application of 105771900 A of CN in patent publication No. The preparation method of property charcoal ", this method is that magnesium salts-Mixture of Activated Carbon is obtained after mixing active carbon with magnesium salt solution, then Progress precipitation reaction is mixed with alkaline aqueous solution and obtains magnesium hydroxide-Mixture of Activated Carbon, is then roasted and is aoxidized through anaerobic Magnesium-based active carbon.Only with simple dipping and roasting in above method preparation process, so that the hydrogen-oxygen of attachment on the activated carbon It is less to change magnesium precipitate.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provide a kind of chemical ion exchange-roast legal system The methods and applications of standby Activated Carbon with Cu.The present invention reduces the discharge of waste and to ring using discarded active carbon as raw material Border pollution, realizes the comprehensive utilization of resources of waste.The invention is realized by the following technical scheme.
A kind of method of chemical ion exchange-roasting method preparation Activated Carbon with Cu, the specific steps of which are as follows:
Discarded active carbon is placed in distilled water by step 1 first, in the ultrasonic wave that power is 500 ~ 1200W, is at room temperature cleaned 1 ~ 3h is filtered and is dried to obtain the active carbon discarded after cleaning;
Step 2, by the active carbon discarded after step 1 cleaning according to solid-to-liquid ratio be 10:30 g/mL be added to concentration be 0.04 ~ Cu (the NO of 0.08mmol/mL3)2In solution, 40 ~ 80 min are handled in the ultrasonic wave that power is 500 ~ 1200W, are then being turned Speed is that 160 ~ 220 r/min stir 1 ~ 2h;Then according to Cu (NO3)2Solution and NaHCO3Liquor capacity ratio is that concentration is added in 1:1 For the NaHCO of 0.04 ~ 0.1mmol/mL3Solution stirs 1h, filtering, filtering in the case where revolving speed is the magnetic stirring apparatus of 160r/min Object distilled water and ethyl alcohol wash repeatedly, and drying obtains material drying;
Step 3, the material drying for obtaining step 2 are 1:15 ~ 25g/W according to drying amount of substance and microwave power ratio, are being roasted 10 ~ 30min of roasting obtains Activated Carbon with Cu under the conditions of temperature is 300 ~ 500 DEG C.
The discarded active carbon of the step 1 is 150 ~ 300 mesh, and methylene blue value is 30 ~ 60mg/g.
A kind of Activated Carbon with Cu, can apply the adsorption process in waste water from dyestuff.
The beneficial effects of the present invention are:
(1) present invention reduces discharge and the environmental pollution of waste, realizes waste using discarded active carbon as raw material Comprehensive utilization of resources.
(2) the method for the present invention is easy to operate, low in cost and pollution-free.
(3) present invention uses microwave heating and ultrasonication, preparation time is shortened, not merely with the selectivity of microwave Heating, low energy consumption, and heating speed is fast, and decomposition rate is fast, also uses the cavitation of ultrasonic wave, is conducive to improve industrialized Production efficiency.
(4) Activated Carbon with Cu of the method for the present invention preparation can apply the processing in azo dye wastewater.
Detailed description of the invention
Fig. 1 is Activated Carbon with Cu nitrogen adsorption-desorption isotherm figure that the embodiment of the present invention 3 is prepared;
Fig. 2 is the discarded active carbon SEM figure that the embodiment of the present invention 3 uses;
Fig. 3 is the Activated Carbon with Cu SEM figure that the embodiment of the present invention 3 is prepared;
Fig. 4 is the Activated Carbon with Cu EDS figure that the embodiment of the present invention 3 is prepared;
Fig. 5 is the SEM figure after the Activated Carbon with Cu absorption methylene blue dyestuff that the embodiment of the present invention 3 is prepared.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment methylene blue value is measured according to standard GB/T/T12496.10-1999.
Embodiment 1
The chemical ion exchange-roasting method preparation Activated Carbon with Cu method, the specific steps of which are as follows:
Step 1, the active carbon for first discarding 50 g (discarded active carbon is 150 mesh, and methylene blue value is 30 mg/g) are placed in In 100 mL distilled water, in the ultrasonic wave that power is 500W, 1h is cleaned at room temperature, filters and is cleaned in 105 DEG C of dry 12h Discarded active carbon afterwards;
The active carbon discarded after the cleaning of 10g step 1 according to solid-to-liquid ratio is that be added to concentration be 0.04 to 10:30 g/mL by step 2 Cu (the NO of mmol/mL3)2In solution, 40min is handled at room temperature in the ultrasonic wave that power is 500W, is then 160r/ in revolving speed Min stirs 1h;According to Cu (NO after stirring 1h3)2Solution and NaHCO3Liquor capacity ratio is that 1:1 addition concentration is 0.04mmol/ mLNaHCO3Solution then stirs 1h, filtering, filtrate distilled water and second in the case where revolving speed is the magnetic stirring apparatus of 160r/min Alcohol washs repeatedly, and 12h is dried at 105 DEG C and dries to obtain material drying;
Step 3, the material drying for obtaining step 2 are 1:15g/W according to drying amount of substance and microwave power ratio, in maturing temperature 20min is roasted under the conditions of being 500 DEG C obtains Activated Carbon with Cu.
The absorption methylene blue value of Activated Carbon with Cu through above-mentioned steps preparation is 150mg/g.
Embodiment 2
The chemical ion exchange-roasting method preparation Activated Carbon with Cu method, the specific steps of which are as follows:
Step 1, the active carbon for first discarding 20 g (discarded active carbon is 200 mesh, and methylene blue value is 45mg/g) are placed in In 100 mL distilled water, in the ultrasonic wave that power is 600W, 2h is cleaned at room temperature, filters and is cleaned in 105 DEG C of dry 12h Discarded active carbon afterwards;
The active carbon discarded after the cleaning of 10g step 1 according to solid-to-liquid ratio is that 10:30 g/mL is added to concentration and is by step 2 Cu (the NO of 0.05mmol/mL3)2In solution, 40min is handled at room temperature in the ultrasonic wave that power is 600W, is then in revolving speed 160r/min stirs 2h;According to Cu (NO after stirring 2h3)2Solution and NaHCO3Liquor capacity ratio is that 1:1 addition concentration is 0.04mmol/mLNaHCO3Solution, then stirs 1h in the case where revolving speed is the magnetic stirring apparatus of 160r/min, and filtering, filtrate are used Distilled water and ethyl alcohol wash repeatedly, and 12h is dried at 105 DEG C and dries to obtain material drying;
Step 3, the material drying for obtaining step 2 are 1:20g/W according to drying amount of substance and microwave power ratio, in maturing temperature 20min is roasted under the conditions of being 300 DEG C obtains Activated Carbon with Cu.
The absorption methylene blue value of Activated Carbon with Cu through above-mentioned steps preparation is 105mg/g.
Embodiment 3
The chemical ion exchange-roasting method preparation Activated Carbon with Cu method, the specific steps of which are as follows:
Step 1, the active carbon for first discarding 50 g (discarded active carbon is 200 mesh, and methylene blue value is 45mg/g) are placed in In 200 mL distilled water, in the ultrasonic wave that power is 1000W, 3h is cleaned at room temperature, filters and obtains clearly in 105 DEG C of dry 12h The active carbon discarded after washing;
The active carbon discarded after the cleaning of 10g step 1 according to solid-to-liquid ratio is that be added to concentration be 0.07 to 10:30g/mL by step 2 Cu (the NO of mmol/mL3)2In solution, 60 min are handled at room temperature in the ultrasonic wave that power is 1000 W, are then 180 in revolving speed R/min stirs 2 h;It stirs after 2 h according to Cu (NO3)2Solution and NaHCO3Liquor capacity ratio is that 1:1 addition concentration is 0.06 mmol/mLNaHCO3Solution then stirs 1h, filtering, filtrate distillation in the case where revolving speed is the magnetic stirring apparatus of 160r/min Water and ethyl alcohol wash repeatedly, and 12h is dried at 105 DEG C and dries to obtain material drying;
Step 3, the material drying for obtaining step 2 are 1:20g/W according to drying amount of substance and microwave power ratio, in maturing temperature 30min is roasted under the conditions of being 500 DEG C obtains Activated Carbon with Cu.
The absorption methylene blue value of Activated Carbon with Cu through above-mentioned steps preparation is 195mg/g.
Nitrogen adsorption-desorption isotherm of discarded active carbon and the Activated Carbon with Cu being prepared that the present embodiment uses is such as Shown in Fig. 1, the Activated Carbon with Cu adsorbance being prepared as can be seen from Figure 1 using the method is apparently higher than discarded active carbon, Illustrate the pore structure that can improve active carbon using chemical ion exchange-roasting method.The active carbon discarded used in this example As shown in Fig. 2, waste active carbon surface is rougher as can be seen from Figure 2, hole absorbate blocks SEM.What is be prepared is copper-loaded Active carbon SEM produces tissue defects, favorably as shown in figure 3, carbon irregular arrangement in structure as can be seen from Figure 3 It is spherical in shape in the copper particle of the load of Cu and its oxides, activated carbon surface and have apparent pore structure, illustrate that regeneration duties are imitated Fruit is obvious.Fig. 4 is the EDS figure for the Activated Carbon with Cu being prepared, it can be seen that contains Cu element in Activated Carbon with Cu, illustrates this Kind method successfully loads to copper on active carbon.
The Activated Carbon with Cu that the present embodiment is prepared adsorbs methylene blue dye, and obtained SEM figure is as shown in Figure 5. There is the dyestuff as petal on Activated Carbon with Cu surface as can be seen from Figure 5, illustrates that Activated Carbon with Cu has one to methylene blue Fixed adsorption capacity.
Embodiment 4
The chemical ion exchange-roasting method preparation Activated Carbon with Cu method, the specific steps of which are as follows:
Step 1, the active carbon for first discarding 50 g (discarded active carbon is 300 mesh, and methylene blue value is 60mg/g) are placed in In 100 mL distilled water, in the ultrasonic wave that power is 1200W, 3h is cleaned at room temperature, filters and obtains clearly in 105 DEG C of dry 12h The active carbon discarded after washing;
The active carbon discarded after the cleaning of 10g step 1 according to solid-to-liquid ratio is that be added to concentration be 0.08 to 10:30 g/mL by step 2 Cu (the NO of mmol/mL3)2In solution, power be 1200W ultrasonic wave handle 80min at room temperature, then proceed to be in revolving speed 220 r/min stir 1.5 h;According to Cu (NO after stirring 1.5h3)2Solution and NaHCO3Liquor capacity ratio is that 1:1 addition concentration is The NaHCO of 0.1mmol/mL3Solution, then stirs 1h in the case where revolving speed is the magnetic stirring apparatus of 160r/min, and filtering, filtrate are used Distilled water and ethyl alcohol wash repeatedly, and 12h is dried at 105 DEG C and dries to obtain material drying;
Step 3, the material drying for obtaining step 2 are 1:25g/W according to drying amount of substance and microwave power ratio, in maturing temperature 10min is roasted under the conditions of being 400 DEG C obtains Activated Carbon with Cu.
The absorption methylene blue value of Activated Carbon with Cu through above-mentioned steps preparation is 150 mg/g.
In conjunction with attached drawing, the embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept Put that various changes can be made.

Claims (3)

1. a kind of chemical ion exchange-roasting method preparation Activated Carbon with Cu method, it is characterised in that specific step is as follows:
Discarded active carbon is placed in distilled water by step 1 first, in the ultrasonic wave that power is 500 ~ 1200W, is at room temperature cleaned 1 ~ 3h is filtered and is dried to obtain the active carbon discarded after cleaning;
Step 2, by the active carbon discarded after step 1 cleaning according to solid-to-liquid ratio be 10:30 g/mL be added to concentration be 0.04 ~ Cu (the NO of 0.08mmol/mL3)2In solution, power be 500 ~ 1200W ultrasonic wave in handle, then revolving speed be 160 ~ 220 r/min stir 1 ~ 2h;Then according to Cu (NO3)2Solution and NaHCO3Liquor capacity ratio be 1:1 be added concentration be 0.04 ~ The NaHCO of 0.1mmol/mL3Solution stirs 1h, filtering, filtrate distillation in the case where revolving speed is the magnetic stirring apparatus of 160r/min Water and ethyl alcohol wash repeatedly, and drying obtains material drying;
Step 3, the material drying for obtaining step 2 are 1:15 ~ 25g/W according to drying amount of substance and microwave power ratio, are being roasted 10 ~ 30min of roasting obtains Activated Carbon with Cu under the conditions of temperature is 300 ~ 500 DEG C.
2. chemical ion exchange according to claim 1-roasting method preparation Activated Carbon with Cu method, it is characterised in that: The discarded active carbon of the step 1 is 150 ~ 300 mesh, and methylene blue value is 30 ~ 60mg/g.
3. it is a kind of according to claim 1 or 2 Activated Carbon with Cu that are prepared, the absorption in waste water from dyestuff can be applied Journey.
CN201810705696.6A 2018-07-02 2018-07-02 A kind of methods and applications of chemical ion exchange-roasting method preparation Activated Carbon with Cu Pending CN109012578A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1876232A (en) * 2006-07-04 2006-12-13 北京交通大学 Activated charcoal carried copper oxide catalyst and process for preparing same
CN103143357A (en) * 2013-03-12 2013-06-12 太原理工大学 Catalyst for synthesizing dimethyl carbonate through continuous oxidative carbonylation of liquid phase methanol and preparation method and application of catalyst
CN105032353A (en) * 2015-07-29 2015-11-11 昆明理工大学 Preparation method and application of modified activated carbon
WO2017024420A1 (en) * 2015-08-12 2017-02-16 华北电力大学(保定) Supported solid phase catalyst, and preparation method and use thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1876232A (en) * 2006-07-04 2006-12-13 北京交通大学 Activated charcoal carried copper oxide catalyst and process for preparing same
CN103143357A (en) * 2013-03-12 2013-06-12 太原理工大学 Catalyst for synthesizing dimethyl carbonate through continuous oxidative carbonylation of liquid phase methanol and preparation method and application of catalyst
CN105032353A (en) * 2015-07-29 2015-11-11 昆明理工大学 Preparation method and application of modified activated carbon
WO2017024420A1 (en) * 2015-08-12 2017-02-16 华北电力大学(保定) Supported solid phase catalyst, and preparation method and use thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
饶辉凯等: "活性炭的再生方法", 《创新驱动,加快战略性新兴产业发展——吉林省第七届科学技术学术年会论文集(上)》 *

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Application publication date: 20181218