CN106824076A - A kind of shaddock peel activated carbon and its application - Google Patents
A kind of shaddock peel activated carbon and its application Download PDFInfo
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- CN106824076A CN106824076A CN201710098639.1A CN201710098639A CN106824076A CN 106824076 A CN106824076 A CN 106824076A CN 201710098639 A CN201710098639 A CN 201710098639A CN 106824076 A CN106824076 A CN 106824076A
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- 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
- B01J20/02—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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- 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
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a kind of shaddock peel activated carbon and its application, the shaddock peel activated carbon is prepared from by following methods:1)Pomelo peel is taken, crushed after being dried crosses the sieve that aperture is 200 mesh, obtains powder standby;2)Powder is taken, absolute ethyl alcohol and NaOH solution is added thereto to, MgCl is added after mixing2Solution, mixing immersion, subsequent suction filtration and be washed with distilled water to pH for neutrality, dry for standby;3)Pomelo peel powder after drying is put into Muffle furnace, in N2450 DEG C are warmed up to the speed program of 5 DEG C/min to calcine 3 hours, shaddock peel activated carbon is obtained after cooling under atmosphere.When the charcoal absorption time prepared by the present invention is 90 min, absorption basically reaches balance, and, all to being adsorbed with considerable influence, optimal adsorption temperature is 30 DEG C, and optimal pH is 7 for adsorption temp and solution ph.Shaddock peel activated carbon is to Cu in water2+With preferable absorption property, maximal absorptive capacity is 117.6 mg/g.
Description
Technical field
The invention belongs to sorbing material technical field, and in particular to a kind of shaddock peel activated carbon and its application.
Background technology
Heavy metal can be converted into the stronger organic compound of toxicity because having under microbial action, can be rich long-pending in organism
Interior, it is impossible to degrade, the harm characteristic such as the duration is long causes greatly harm to ecological environment.It is presently used in removal sewage
The method that efficiently separates of heavy metal ion has precipitation, ion exchange, electrochemical treatments, membrane technology, evaporation coagulation, counter-infiltration, electricity
Dialysis and absorption etc., wherein absorption method receive pass extensively as a kind of effective method of heavy metal in removal polluted-water
Note.And develop the study hotspot that new and effective cheap adsorbent is then the field.
Because its specific surface area is big, efficiency is high etc., property turns into one of conventional adsorbent of heavy-metal ion removal to activated carbon.
And it is easy to regeneration after absorption, and repeat and utilize, it is the superior adsorbent for removing water intermediate ion state heavy metal.Farming is utilized in recent years
Activated carbon prepared by the thing discarded object heavy metal ions research in water removal is gone gradually obtains people and pays close attention to.Agricultural wastes amount
Greatly, its stacking can cause environment to be subject to heavy damage.Meanwhile, agricultural wastes are cheap, and ash content is low, and hardness is moderate,
It is the affluent resources of activated carbon preparation.Therefore, agricultural wastes prepare activated carbon and can solve environmental problem, can also reduce activity
Charcoal preparation cost.Conventional agricultural waste material has stalk, cocoanut shell, rice husk, peanut shell, chestnut shell etc. at present.
Chen Cheng etc. with chestnut shell as raw material, using ZnCl2Activated carbon average pore size prepared by activation method is 2~6nm, pore volume
It is 0.04~0.14cm3/ g, specific surface area reaches 1500m2/ g, and have studied under different preparation conditions, Chestnut shell active carbon counterweight
Metal ion Cu2+And Cd2+Static Adsorptive capacity, while having investigated adsorption temp, solution ph etc. to Cd2+And Cu2+Absorption
[Chen Cheng, appoints and celebrates victory, Xu Qingrui etc. Chestnut shell active carbon heavy metal ionic adsorption performance study [J] ions for the influence of performance
Exchange and absorption, 2014,30 (1):029~038.].Yao's book is identical with rice husk as raw material, and zinc chloride is activator, with microwave
Electrical heating is double mode to prepare activated carbon, and have studied heavy metal (sexavalence) chromium ion in active carbon purifying water mechanism [Yao Shuheng,
Jiang little Xiang, Shen Dekui, wait rice hull active carbons to the mechanism Southeast China University journal (natural science of Cr (VI) ionic adsorption process
Version) [J], 2015,45 (3):515-520.].The specific surface area of the rice hull active carbon prepared by them has reached 1719.32m2/
G, total pore volume 1.05cm3/g.At pH=2.0~3.0, the activated carbon prepared under optimum condition has maximal absorptive capacity, and
Adsorption equilibrium is reached in 90min.Wilson K etc. are prepared for activated carbon with peanut shell, with steam activation, to Pb (II), Zn
(II), the adsorbance such as Ni (II), Cd (II) and Cu (II) respectively reaches 159.39,56.55,26.36,48.67 and 47.30mg
g-1, adsorption isotherm line model is Langmuir [Wilson K, H Yang.Select metal adsorption by
activated carbon made from peanut shells[J].Bioresource Technology,2006,97
(18):2266-2270.]。
Pomelo peel is a kind of common agricultural wastes, and yield is big, and utilization rate is low, causes very big waste, at present, with shaddock
Sub- leather goes the research of heavy metal ion in water removal little for activated carbon and with this.
The content of the invention
Goal of the invention:For the deficiencies in the prior art, it is an object of the invention to provide a kind of shaddock peel activated carbon,
It is raw material using discarded pomelo peel, prepares the big activated carbon of adsorbance.It is a further object of the present invention to provide a kind of above-mentioned shaddock
The application of sub- leather activated char Adsorption of Heavy Metals ion in water.
Technical scheme:In order to realize foregoing invention purpose, the technical solution adopted by the present invention is:
A kind of shaddock peel activated carbon, is prepared from by following methods:
1) pomelo peel is taken, crushed after being dried crosses the sieve that aperture is 80-200 mesh, obtains powder standby;
2) powder is taken, absolute ethyl alcohol and NaOH solution is added thereto to, MgCl is added after mixing2Solution, mixing
Immersion, subsequent suction filtration and be washed with distilled water to pH for neutrality, dry for standby;
3) the pomelo peel powder after drying is put into Muffle furnace, in N2With the speed program liter of 2-5 DEG C/min under atmosphere
Temperature is calcined 2-4 hours to 400-500 DEG C, and shaddock peel activated carbon is obtained after cooling.
Step 2) in, the concentration of NaOH solution is 0.5-1.5mol/L.
Step 2) in, MgCl2The concentration of solution is 1.0-2.0mol/L.
Step 2) in, powder is 1 with the g/mL of absolute ethyl alcohol:4-6.
Step 2) in, absolute ethyl alcohol is 1 with the volume ratio of NaOH solution:0.5-1.
Step 2) in, mix more than 30min.
Step 2) in, NaOH solution and MgCl2The volume ratio of solution is 1:1.
Step 2) in, mixing immersion more than 24h.
Application of the described shaddock peel activated carbon in adsorbing heavy metal in water.
Beneficial effect:Compared with prior art, shaddock peel activated carbon of the invention and its application, with advantages below:
1) shaddock peel activated carbon is to Cu in water2+With larger adsorption capacity, saturated extent of adsorption is 117.6mg/g, far
Much larger than disclosed result in the prior art, (Wilson K etc. are prepared for activated carbon with peanut shell, to Pb (II), Zn (II), Ni
(II), the adsorbance such as Cd (II) and Cu (II) respectively reaches 159.39,56.55,26.36,48.67 and 47.30mgg-1
[Wilson K,H Yang.Select metal adsorption by activated carbon made from peanut
shells[J].Bioresource Technology,2006,97(18):2266-2270.];Bouhamed F et al. are with fruit stone
Activated carbon is prepared to Cu2+Adsorbance reaches 31.25mgg-1[Bouhamed F,Elouear Z,Bouzid
J.Adsorptive removal of copper(Ⅱ)from aqueous solutions on activated carbon
prepared from Tunisiandate stones:Equilibrium,kinetics and thermodynamics[J]
.Journal of the Taiwan Institute of Chemical Engineers, 2012,43 (5):741-749.];
Atul V Maldhure et al. are with Preparation of Activated Carbon with Lignin to Cu2+Adsorbance reaches 98.62mgg-1[Atul V
Maldhure,Ekhe J D.Preparation and characterizations of microwave assisted
activated carbons from industrial waste lignin for Cu(Ⅱ)sorption[J].Chemical
Engineering Journal,2011,168(3):1103-1111.];Chen Liping etc. prepares activated carbon pair with sunflower straw
Cu2+Adsorbance reaches 41.03mgg-1[Chen Liping, department is elegant flourish, and Li Lingyun phosphoric acid activation activated carbons are to Cu2+Adsorpting characteristic
Research ecological environment journals, 2011,20 (2):353-358]).
2) raw material pomelo peel is common agricultural wastes, and source is wide, is easy to get.
3) activated carbon can be at a lower temperature prepared, calcining heat is 400-500 DEG C
4) to Pb2+、Ni2+、Cd2+Also there is preferable absorption property Deng other heavy metal ion.
Brief description of the drawings
Fig. 1 is activated carbon N2Adsorption-desorption curve map;
Fig. 2 is influence result figure of the adsorption time to adsorption rate;
Fig. 3 is influence result figure of the adsorption temp to adsorption rate;
Fig. 4 is influence result figure of the solution ph to adsorption rate;
Fig. 5 is adsorption isotherm line chart;
Fig. 6 is ce~ce/qeGraph of a relation.
Specific embodiment
With reference to specific embodiment, the present invention is described further.
Embodiment 1
1st, the preparation of shaddock peel activated carbon
Pomelo peel dries 24h in 70 DEG C of drying boxes, crushes, and crosses the sieve that aperture is 200 mesh, then takes 40g and is placed in
In the conical flask of 500mL, it is the NaOH of 0.5mol/L to be added thereto to 200mL absolute ethyl alcohols and 100mL concentration, is mixed
It is the MgCl of 1.5mol/L that 100mL concentration is added after 30min2Solution, mixing immersion 24h, subsequent suction filtration and with distill water washing
It is neutrality to pH, 24h is dried in 80 DEG C of air dry ovens.Pomelo peel after drying is put into Muffle furnace as in N2Under atmosphere
450 DEG C are warmed up to the speed program of 5 DEG C/min to calcine 3 hours, shaddock peel activated carbon sample is obtained after cooling.
The specific surface of sample and the measure of pore structure are carried out on Micromertics ASAP 2020HD physical adsorption appearances.
Sample vacuumizes activation, -196 DEG C of measure N at 350 DEG C2Adsorbance, BET method calculates the specific surface area of sample, and BJH methods are determined
The pore volume of catalyst and pore size distribution.
By N2Adsorption/desorption is tested, and surveys the BET specific surface area and pore volume of prepared activated carbon, as a result sees Fig. 1.From figure
In can obtain, prepared activated carbon specific surface area is 1167.9m2/ g, pore volume is 1.34cm3/ g, there is micropore, and average pore size is
4.6nm。
2nd, the application of the shaddock peel activated carbon for preparing
Cu in water2+Concentration mensuration:With Cu in Atomic Absorption Spectrometer (Agilent AAS240) measure water2+(by Cu
(NO3)2Prepare) concentration.
The measure of the equilibrium adsorption capacity of activated carbon heavy metal ion:The accurate m g activated carbons that weigh in tool plug Erlenmeyer flask,
It is separately added into the Cu of V mL various concentrations2+In solution, in 25 DEG C, 24h is vibrated, the balance for measuring different equilibrium concentration activated carbons is inhaled
Attached amount qe(represented with mg/g, i.e., every gram charcoal absorption Cu2+Or Ni2+Milligram number)
In formula:c0, c be respectively absorption before and after solution concentration (mg/L);V is addition Cu2+Liquor capacity;M inhales for solid
Attached dose of quality (g)
1) influence of adsorption time
Take 100mL Cu2+Concentration be 0.100mg/L solution in conical flask, add 0.100g activated carbons, in 25 DEG C of constant temperature
Vibrate, at regular intervals sampling analysis Cu2+Concentration, calculates its adsorption rate, as a result sees Fig. 2.From figure 2 it can be seen that when suction
When the attached time reaches 90 minutes, absorption basically reaches balance.
2) influence of adsorption temp
Take 50mL Cu2+Concentration be 0.100mg/L solution in conical flask, add 0.050g activated carbons, it is permanent in different temperatures
Temperature vibration 3 hours, sampling analysis Cu2+Concentration, calculates its adsorption rate, as a result sees Fig. 3.As can be seen from Fig. 3, adsorption temp is to absorption
Rate has considerable influence, and adsorption rate is maximum when adsorption temp is 30 DEG C.
3) influence of solution ph
Take 50mL Cu2+Concentration be 0.100mg/L different pH values in conical flask, add 0.050g activated carbons, in 25
DEG C constant temperature oscillation 3 hours, sampling analysis Cu2+Concentration, calculates its adsorption rate, as a result sees Fig. 4.As can be seen from Fig. 4, the pH value of solution
There is large effect to adsorption rate, adsorption rate is maximum when solution ph is 7.
4) adsorption isotherm
The accurate 0.050g activated carbons that weigh in tool plug Erlenmeyer flask, be separately added into 50ml initial concentrations be respectively 20,40,
60th, 100,150, the 200, Cu of 300mg/L2+Solution, in 25 DEG C, pH=7 vibrates 24h, surveys activated carbon to Cu2+Adsorption isotherm
Line is shown in Fig. 5.
Langmuir adsorption isotherms are:
Q in formulamIt is saturated extent of adsorption, mg/g;KbIt is constant;ceIt is equilibrium concentration, mg/L.
With ceTo ce/qmMapping, can obtain a straight line, see Fig. 6.As can be seen from Figure 6, linear correlation coefficient R2=
0.9961, illustrate preferably be retouched by the good relationship of Langmuir equation models gained straight line, therefore Langmuir equations
Activated carbon is stated to Cu2+Absorption behavior.Saturated extent of adsorption q can be obtained by the slope of straight linemIt is 117.6mg/g.
To Pb under the same terms2+、Ni2+And Cd2+Deng maximal absorptive capacity be respectively 328.8mg/g, 96.7mg/g and
175.4mg/g。
Embodiment 2
1st, the preparation of shaddock peel activated carbon
Pomelo peel dries 24h in 70 DEG C of drying boxes, crushes, and crosses the sieve that aperture is 200 mesh, then takes 40g and is placed in
In the conical flask of 500mL, it is the NaOH of 0.5mol/L to be added thereto to 200mL absolute ethyl alcohols and 100mL concentration, is mixed
It is the MgCl of 1.5mol/L that 100mL concentration is added after 30min2Solution, mixing immersion 24h, subsequent suction filtration and with distill water washing
It is neutrality to pH, 24h is dried in 80 DEG C of air dry ovens.Pomelo peel after drying is put into Muffle furnace as in N2Under atmosphere
400 DEG C are warmed up to the speed program of 5 DEG C/min to calcine 3 hours, shaddock peel activated carbon sample is obtained after cooling.
2nd, the application of shaddock peel activated carbon
The accurate 0.050g activated carbons that weigh in tool plug Erlenmeyer flask, be separately added into 50ml initial concentrations be respectively 20,40,
60th, 100,150, the 200, Cu of 300mg/L2+Solution, in 25 DEG C, pH=7 vibrates 24h, to Cu2+Maximal absorptive capacity be
113.6mg/g。
Embodiment 3
1st, the preparation of shaddock peel activated carbon
Pomelo peel dries 24h in 70 DEG C of drying boxes, crushes, and crosses the sieve that aperture is 200 mesh, then takes 40g and is placed in
In the conical flask of 500mL, it is the NaOH of 0.5mol/L to be added thereto to 200mL absolute ethyl alcohols and 100mL concentration, is mixed
It is the MgCl of 1.5mol/L that 100mL concentration is added after 30min2Solution, mixing immersion 24h, subsequent suction filtration and with distill water washing
It is neutrality to pH, 24h is dried in 80 DEG C of air dry ovens.Pomelo peel after drying is put into Muffle furnace as in N2Under atmosphere
500 DEG C are warmed up to the speed program of 5 DEG C/min to calcine 3 hours, shaddock peel activated carbon sample is obtained after cooling.
2nd, the application of shaddock peel activated carbon
The accurate 0.050g activated carbons that weigh in tool plug Erlenmeyer flask, be separately added into 50ml initial concentrations be respectively 20,40,
60th, 100,150, the 200, Cu of 300mg/L2+Solution, in 25 DEG C, pH=7 vibrates 24h, and the maximal absorptive capacity to copper is
110.3mg/g。
Embodiment 4
1st, the preparation of shaddock peel activated carbon
Pomelo peel dries 24h in 70 DEG C of drying boxes, crushes, and crosses the sieve that aperture is 200 mesh, then takes 40g and is placed in
In the conical flask of 500mL, it is the NaOH of 0.5mol/L to be added thereto to 200mL absolute ethyl alcohols and 100mL concentration, is mixed
It is the MgCl of 1.0mol/L that 100mL concentration is added after 30min2Solution, mixing immersion 24h, subsequent suction filtration and with distill water washing
It is neutrality to pH, 24h is dried in 80 DEG C of air dry ovens.Pomelo peel after drying is put into Muffle furnace as in N2Under atmosphere
450 DEG C are warmed up to the speed program of 5 DEG C/min to calcine 3 hours, shaddock peel activated carbon sample is obtained after cooling.
2nd, the application of shaddock peel activated carbon
The accurate 0.050g activated carbons that weigh in tool plug Erlenmeyer flask, be separately added into 50ml initial concentrations be respectively 20,40,
60th, 100,150, the 200, Cu of 300mg/L2+Solution, in 25 DEG C, pH=7 vibrates 24h, and the maximal absorptive capacity to copper is
106.3mg/g。
Embodiment 5
1st, the preparation of shaddock peel activated carbon
Pomelo peel dries 24h in 70 DEG C of drying boxes, crushes, and crosses the sieve that aperture is 200 mesh, then takes 40g and is placed in
In the conical flask of 500mL, it is the NaOH of 0.5mol/L to be added thereto to 200mL absolute ethyl alcohols and 100mL concentration, is mixed
It is the MgCl of 2.0mol/L that 100mL concentration is added after 30min2Solution, mixing immersion 24h, subsequent suction filtration and with distill water washing
It is neutrality to pH, 24h is dried in 80 DEG C of air dry ovens.Pomelo peel after drying is put into Muffle furnace as in N2Under atmosphere
450 DEG C are warmed up to the speed program of 5 DEG C/min to calcine 3 hours, shaddock peel activated carbon sample is obtained after cooling.
2nd, the application of shaddock peel activated carbon
The accurate 0.050g activated carbons that weigh in tool plug Erlenmeyer flask, be separately added into 50ml initial concentrations be respectively 20,40,
60th, 100,150, the 200, Cu of 300mg/L2+Solution, in 25 DEG C, pH=7 vibrates 24h, and the maximal absorptive capacity to copper is
115.8mg/g。
Embodiment 6
1st, the preparation of shaddock peel activated carbon
Pomelo peel dries 24h in 70 DEG C of drying boxes, crushes, and crosses the sieve that aperture is 200 mesh, then takes 40g and is placed in
In the conical flask of 500mL, it is the NaOH of 1.5mol/L to be added thereto to 200mL absolute ethyl alcohols and 100mL concentration, is mixed
It is the MgCl of 1.5mol/L that 100mL concentration is added after 30min2Solution, mixing immersion 24h, subsequent suction filtration and with distill water washing
It is neutrality to pH, 24h is dried in 80 DEG C of air dry ovens.Pomelo peel after drying is put into Muffle furnace as in N2Under atmosphere
450 DEG C are warmed up to the speed program of 5 DEG C/min to calcine 3 hours, shaddock peel activated carbon sample is obtained after cooling.
2nd, the application of shaddock peel activated carbon
The accurate 0.050g activated carbons that weigh in tool plug Erlenmeyer flask, be separately added into 50ml initial concentrations be respectively 20,40,
60th, 100,150, the 200, Cu of 300mg/L2+Solution, in 25 DEG C, pH=7 vibrates 24h, and the maximal absorptive capacity to copper is
112.6mg/g。
Claims (9)
1. a kind of shaddock peel activated carbon, it is characterised in that be prepared from by following methods:
1)Pomelo peel is taken, crushed after being dried crosses the sieve that aperture is 80-200 mesh, obtains powder standby;
2)Powder is taken, absolute ethyl alcohol and NaOH solution is added thereto to, MgCl is added after mixing2Solution, mixing immersion,
Subsequent suction filtration and to be washed with distilled water to pH be neutrality, dry for standby;
3)Pomelo peel powder after drying is put into Muffle furnace, in N2It is warmed up to the speed program of 2-5 DEG C/min under atmosphere
400-500 DEG C is calcined 2-4 hours, and shaddock peel activated carbon is obtained after cooling.
2. shaddock peel activated carbon according to claim 1, it is characterised in that step 2)In, the concentration of NaOH solution is
0.5-1.5 mol/L。
3. shaddock peel activated carbon according to claim 1, it is characterised in that step 2)In, MgCl2The concentration of solution is
1.0-2.0mol/L。
4. shaddock peel activated carbon according to claim 1, it is characterised in that step 2)In, the g/ of powder and absolute ethyl alcohol
ML is 1:4-6.
5. shaddock peel activated carbon according to claim 1, it is characterised in that step 2)In, absolute ethyl alcohol and NaOH solution
Volume ratio be 1:0.5-1.
6. shaddock peel activated carbon according to claim 1, it is characterised in that step 2)In, mix more than 30min.
7. shaddock peel activated carbon according to claim 1, it is characterised in that step 2)In, NaOH solution and MgCl2Solution
Volume ratio be 1:1.
8. shaddock peel activated carbon according to claim 1, it is characterised in that step 2)In, mixing immersion more than 24h.
9. application of the shaddock peel activated carbon described in claim 1 in adsorbing heavy metal in water.
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