CN110102262A - A kind of magnetic active carbon composite material and its preparation method and application - Google Patents
A kind of magnetic active carbon composite material and its preparation method and application Download PDFInfo
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- CN110102262A CN110102262A CN201910541144.0A CN201910541144A CN110102262A CN 110102262 A CN110102262 A CN 110102262A CN 201910541144 A CN201910541144 A CN 201910541144A CN 110102262 A CN110102262 A CN 110102262A
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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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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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 belongs to environment functional material technical fields more particularly to a kind of magnetic active carbon composite material and its preparation method and application.The present invention uses sulfhydryl modified magnetic active carbon, the adsorption capacity for the sulfhydryl modified magnetic active carbon composite material being prepared is high, to mercuric adsorption capacity up to 298.8mg/g, good removal effect is shown to common heavy metal ion (dimercurion and trivalent chromic ion) and organic pollutant (methylene blue and phenol) etc.；Magnetic active carbon composite material prepared by the present invention has strong anti-interference ability and stronger selective absorption, stronger affinity especially is shown to heavy metal ion, with good application prospect to the removal of heavy metals in industrial wastewater ion and organic pollutant；Magnetic active carbon composite material prepared by the present invention has good recycling and power of regeneration, and use cost is lower.
Description
Technical field
The present invention relates to environment functional material technical field more particularly to a kind of magnetic active carbon composite material and its preparations
Methods and applications.
Background technique
Mercury metal and mercury compound are widely used in the industries such as chemical industry, medical treatment, electric appliance, and then result in a large amount of mercurous dirts
Contaminate the generation of object.The toxicity of mercury is very strong, and has migration and enriching, these contain, and mercury contaminants are unprocessed to be just discharged
Into natural environment, serious destruction is caused to ecological environment and human health.The existence form of mercury in the natural environment is more
Kind multiplicity, and be largely present in atmosphere, soil and water body.Since water is Source of life, so the mercury solved in water body is dirty
Dye problem is extremely urgent.Mercury mainly exists in water body with ionic forms, is broadly divided into monovalence mercury and bivalent mercury.It defends in the world
The mercury content of raw tissue (WHO) regulation drinking water must not exceed 0.001mg/L.Currently, the side of common mercury pollution wastewater treatment
Method has chemical precipitation method, electrochemical process, ion-exchange, microbial method and absorption method.Wherein, absorption method as it is a kind of it is easy,
Economic and efficient process for treating heavy-metal waste water, has been obtained and is widely applied.
Active carbon is a kind of black solid charcoal containing pore structure.The source of active carbon is very extensive, at present using most
More active carbons is to be prepared by wood-fibred, coconut husk and peach-pit by high-temperature calcination.C atom in active carbon has a variety of miscellaneous
Change mode, and the no regularity of assembled arrangement of C atom, therefore active carbon has many pore and gap structure.Active carbon
In containing the elements such as a small amount of nitrogen, oxygen, hydrogen, chlorine, these elements form the functions such as hydroxyl abundant, carboxyl in activated carbon surface
Group, with heavy metal ion complex reaction can occur for these functional groups, so that active carbon can be removed effectively in waste water
Heavy metal ion.In addition, active carbon has sizable specific surface area, this makes the adsorption efficiency of active carbon higher, also facilitates
It is further modified.Moreover, active carbon has advantage that is efficient, economic, renewable, not generating secondary pollution, so that active
Charcoal is widely used in processing heavy metal wastewater thereby.
However, existing absorbent charcoal material is to be improved to the absorption property of heavy metal and organic pollutant.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of magnetic active carbon composite material, the magnetism of this method preparation
Absorbent charcoal composite material is to heavy metal and organic pollutant adsorption capacity with higher and removal rate.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of magnetic active carbon composite material, comprising the following steps:
Nickel source, source of iron, active carbon, water and ammonium hydroxide are mixed, coprecipitation reaction is carried out, obtains magnetic active carbon；
Thioacetic acid, acetic anhydride and the concentrated sulfuric acid are added into the magnetic active carbon, carries out esterification, obtains magnetic work
Property carbon composite.
Preferably, before nickel source, source of iron, active carbon, water and ammonium hydroxide being mixed, the active carbon is mixed with acid solution, into
Row acid processing；The temperature of the acid processing is 90 DEG C, and the time of the acid processing is 6~9h.
Preferably, the acid solution is nitric acid solution, and the concentration of the acid solution is 1~2mol/L.
Preferably, the temperature of the acid processing is 60~90 DEG C, and the time of the acid processing is 6~9h.
Preferably, the mass ratio of the nickel source, source of iron and active carbon is 1.2~2.4:2.7~5.4:1~2；The activity
The amount ratio of charcoal and ammonium hydroxide is 1~2g:6~12mL；The mass concentration of the ammonium hydroxide is 25%~28%.
Preferably, the temperature of the coprecipitation reaction is 150~250 DEG C, time of the coprecipitation reaction is 12~
16h。
Preferably, the magnetic active carbon and the amount ratio of thioacetic acid are 0.5~1g:1.7~3.5mL；The sulfydryl
The amount ratio of acetic acid, acetic anhydride and the concentrated sulfuric acid is the μ of 1.7~3.5mL:1.2~2.5mL:13~25 L.
Preferably, the temperature of the esterification is 50~90 DEG C, and the time of the esterification is 6~10h.
The present invention provides the magnetic active carbon composite materials that preparation method described in above-mentioned technical proposal is prepared.
The present invention provides magnetic active carbon composite materials described in above-mentioned technical proposal in absorption heavy metal ion and to have
Application in machine pollutant.
The present invention provides a kind of preparation method of magnetic active carbon composite material, by nickel source, source of iron, active carbon, water and
Ammonium hydroxide mixing, carries out coprecipitation reaction, obtains magnetic active carbon；Thioacetic acid, acetic anhydride are added into the magnetic active carbon
And the concentrated sulfuric acid, esterification is carried out, magnetic active carbon composite material is obtained.Sulfydryl is grafted on magnetic active carbon by the present invention,
Magnetic active carbon is modified, magnetic active carbon composite material is prepared.
The present invention provides application of the magnetic active carbon composite material in absorption heavy metal ion and organic pollutant.
Magnetic active carbon composite material prepared by the present invention adsorbs heavy metal ion process, environmentally protective without secondary pollution, used
Medicament totally nontoxic；
The adsorption capacity of magnetic active carbon composite material prepared by the present invention is high, reachable to mercuric adsorption capacity
298.8mg/g, to common heavy metal ion (dimercurion and trivalent chromic ion) and organic pollutant (methylene blue and
Phenol) etc. show good removal effect；
Magnetic active carbon composite material prepared by the present invention have strong anti-interference ability with stronger selective absorption,
Stronger affinity especially is shown to heavy metal ion, is had to the removal of heavy metals in industrial wastewater ion and organic pollutant
There is preferable application prospect；
Magnetic active carbon composite material prepared by the present invention has good recycling and power of regeneration, and use cost is lower；
Preparation method of the invention is simple, easy to operate, and experimental cost is low, and experiment condition requirement is lower, and aggregate velocity is fast.
Detailed description of the invention
Fig. 1 is NiFe prepared by embodiment 12O4The SEM of-PAC-SH schemes；
Fig. 2 is PAC, NiFe prepared by embodiment 12O4- PAC and NiFe2O4The FTIR of-PAC-SH schemes；
Fig. 3 is NiFe prepared by embodiment 12O4- PAC and NiFe2O4The hysteresis loop figure of-PAC-SH；
Fig. 4 is PAC, NiFe prepared by embodiment 12O4- PAC and NiFe2O4- PAC-SH removes mercuric effect picture；
Fig. 5 is NiFe prepared by embodiment 12O4The regenerability figure of-PAC-SH；
Fig. 6 is the coexisting ion of various concentration to NiFe2O4- PAC-SH removes mercuric influence situation schematic diagram.
Specific embodiment
The present invention provides a kind of preparation methods of magnetic active carbon composite material, comprising the following steps:
Nickel source, source of iron, active carbon, water and ammonium hydroxide are mixed, coprecipitation reaction is carried out, obtains magnetic active carbon；
Thioacetic acid, acetic anhydride and the concentrated sulfuric acid are added into the magnetic active carbon, carries out esterification, obtains magnetic work
Property carbon composite.
In the present invention, if without specified otherwise, the required raw material for preparing is commercial goods well known to those skilled in the art.
The present invention mixes nickel source, source of iron, active carbon, water and ammonium hydroxide, carries out coprecipitation reaction, obtains magnetic active carbon.
Before nickel source, source of iron, active carbon, water and ammonium hydroxide are mixed, the present invention preferably mixes the active carbon with acid solution, carries out at acid
Reason.In the present invention, the acid solution is preferably nitric acid solution, and the concentration of the acid solution is preferably 1~2mol/L；The work
The amount ratio of property charcoal and acid solution is preferably 1~5g:500mL；The temperature of the acid processing is preferably 60~90 DEG C, preferably 80
DEG C, the time of the acid processing is preferably 6~9h, more preferably 7~8h.In the present invention, the active carbon is preferably wooden
Active carbon, the partial size of the active carbon are preferably 300 mesh.After completing the acid processing, the present invention successively carries out products therefrom
Washing and drying, obtain pretreated active carbon.The present invention does not have special restriction to the mode of the washing and drying, selects
Mode well known to those skilled in the art is washed and is dried.The present invention leads to peracid treatment and activated carbon surface is filled
Divide oxidation, the quantity of the hydroxyl and carboxyl that make activated carbon surface increases, moreover, acid processing can increase the aperture of active carbon.
In the present invention, the nickel source preferably includes six hydration Nickel Chlorides or ferrous sulfate；The source of iron preferably includes
Iron(III) chloride hexahydrate or ferrous sulfate, the mass ratio of the nickel source, source of iron and active carbon be preferably 1.2~2.4:2.7~
5.4:1~2, more preferably 1.5~2.0:3.0~5.0:1.2~1.8, most preferably 1.6~1.8:3.5~4.5:1.4~
1.6；The amount ratio of the active carbon and ammonium hydroxide is preferably 1~2g:6~12mL, more preferably 1.2~1.8g:8~10mL, most
Preferably 1.4~1.6g:9mL；The mass concentration of the ammonium hydroxide is preferably 25~28%, and more preferably 26%；The nickel source, iron
The amount ratio of source and water is preferably 1.2~2.4g:2.7~5.4g:50~80mL, more preferably 1.5~2.0g:3.0~5.0g:
55~70mL, most preferably 1.6~1.8g:3.5~4.5g:60~65mL.
In the present invention, nickel source and source of iron are preferably first dissolved in the water by the mixing, and ammonia is added into acquired solution
Water is dispersed, and ammonium hydroxide then is added into gained dispersion liquid, is stirred, obtains mixed liquor.In the present invention, described point
It dissipates and is preferably carried out under ultrasound condition, the power of the ultrasound is preferably 600W；The time of the ultrasound is preferably 30min；Institute
The revolving speed for stating stirring is preferably 200r/min, and the time of the stirring is preferably 20min.
In the present invention, the temperature of the coprecipitation reaction is preferably 150~250 DEG C, more preferably 220 DEG C, described total
The time of precipitation reaction is preferably 12~16h, more preferably 13~15h, most preferably 14h.The present invention is preferably in a kettle
Carry out the coprecipitation reaction.In coprecipitation process, nickel source and source of iron generate iron hydroxide and hydroxide under ammonium hydroxide effect
Nickel precipitating, then at high temperature, the two is co-precipitated, and obtains NiFe2O4.The present invention utilizes the crystal structure of Ni, enhancing
NiFe2O4Chemical stability and capacity antacid.
After completing the coprecipitation reaction, the present invention preferably separates gained precipitated product with solution, and by obtained solid
Object is successively washed, is dried, and magnetic active carbon is obtained, and is denoted as NiFe2O4-PAC.In magnetic active carbon, NiFe2O4It is attached to
On the surface of active carbon, the NiFe2O4Magnetism is only provided, does not influence the absorption property of active carbon.
In the present invention, the isolated mode is preferably magnet separation, and the washing is preferably deionization washing, this hair
The bright number to the washing does not have special restriction, washing to neutrality.The present invention carries out preferably in thermostatic drying chamber
The drying, the temperature of the drying are preferably 60 DEG C.
After obtaining magnetic active carbon, thioacetic acid, acetic anhydride and the concentrated sulfuric acid are added into the magnetic active carbon by the present invention,
Esterification is carried out, magnetic active carbon composite material is obtained.In the present invention, the dosage of the magnetic active carbon and thioacetic acid
Than being preferably 0.5~1g:1.7~3.5mL, more preferably 0.6~0.8g:2.0~3.0mL, most preferably 0.7g:2.5mL；Institute
The amount ratio for stating thioacetic acid, acetic anhydride and the concentrated sulfuric acid is preferably the μ L of 1.7~3.5mL:1.2~2.5mL:13~25, more preferably
For the μ L of 2.0~3.0mL:1.5~2.0mL:15~20, most preferably 2.5mL:1.8mL:18 μ L.In the present invention, the dense sulphur
The mass concentration of acid is preferably 98%.
The present invention requirement not special to the sequence of the addition thioacetic acid, acetic anhydride and the concentrated sulfuric acid, selects ability
Sequence known to field technique personnel is added.
In the present invention, the temperature of the esterification is preferably 50~90 DEG C, and more preferably 80 DEG C, the esterification
Time be preferably 6~10h, more preferably 7~9h, most preferably 8h.The present invention is preferably in brown reaction flask, air-proof condition
It is lower to carry out the esterification.Using acetic anhydride as dehydrating agent, the water that esterification is generated absorbs the present invention, so that esterification
Reaction is carried out towards positive direction.The present invention plays dehydration and catalytic action using the concentrated sulfuric acid.In esterification reaction process, active carbon
Esterification occurs for the hydroxyl and thioacetic acid on surface, and sulfydryl is grafted on magnetic active carbon, and it is living to obtain sulfhydryl modified magnetism
Property charcoal.
After completing the esterification, the present invention preferably separates obtained solid product with solution, and by obtained solid object
It successively washed, dried, obtain magnetic active carbon composite material, be denoted as NiFe2O4-PAC-SH。
In the present invention, the isolated mode is preferably magnet separation, and the washing is preferably deionization washing, this hair
The bright number to the washing does not have special restriction, washing to neutrality.The present invention carries out preferably in thermostatic drying chamber
The drying, the temperature of the drying are preferably 60 DEG C.
The present invention provides the magnetic active carbon composite materials that preparation method described in above-mentioned technical proposal is prepared.
The present invention provides magnetic active carbon composite materials described in above-mentioned technical proposal in absorption heavy metal ion and to have
Application in machine pollutant.
In the present invention, the magnetic active carbon composite material is used to adsorb heavy metal ion as adsorbent and had
The method of machine pollutant, preferably includes following steps:
By containing in the solution of heavy metal ion or organic pollutant merging conical flask, arrived by NaOH and HCl solution adjusting
Adsorbent, is then distributed in acquired solution by pH value needed for testing, and concussion reaction is to guarantee that absorption reaches balance；Lead to later
It crosses Clod Vapour Atomic Absorption tester and ICP-OES and measures after reaction remaining heavy metal ion and organic pollutant in solution respectively
Concentration.By the additive amount of the heavy metal ion of comparison absorption front and back or the concentration of organic pollutant and adsorbent, pass through public affairs
Formula (1) and formula (2) can calculate adsorbent to the adsorption capacity q of heavy metal ion or organic pollutanteWith removal rate E.
Wherein, equilibrium adsorption capacities qe(mg/g) calculation formula is as follows:
In formula: C0For pollutant initial concentration (mg/L) in solution；
CeFor concentration (mg/L) when pollutant equilibrium in solution；
V is sample solution volume (L)；
W is adsorbent mass (g)；
The calculation formula of removal rate E (%) is as follows:
In formula: C0For pollutant initial concentration (mg/L) in solution；
CeFor concentration (mg/L) when pollutant equilibrium in solution.
In the present invention, the mass concentration of the solution containing heavy metal ion or organic pollutant be preferably 30~
100mg/L；The mass concentration of the adsorbent is preferably 0.05~1.5g/L；It is described containing heavy metal ion or organic pollutant
The amount ratio of solution and adsorbent is preferably 100mL:0.05g；The concentration of the NaOH solution is preferably 0.1mol/L, described
The concentration of HCl solution is preferably 1mol/L；PH value needed for testing is preferably 2~9；The time of the concussion reaction is preferably 2~
8h。
Magnetic active carbon composite material provided by the invention and its preparation method and application is carried out below with reference to embodiment
Detailed description, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
3g active carbon powder is miscible in the nitric acid solution of 500mL 2mol/L, and 90 DEG C are heated to, 6h is persistently stirred,
It will be dried after products therefrom washes clean, obtain the active carbon powder of nitric acid pretreatment, be denoted as PAC；
Weigh 2.38gNiCl2·6H2O and 5.41g FeCl3·6H2O is dissolved in 70mL deionized water, into acquired solution
Be added 2g nitric acid pretreatment active carbon powder, by gained mixture in Ultrasound Instrument ultrasound 30min；After ultrasound, to institute
It obtains and 11mL ammonium hydroxide is added in dispersion liquid, and continue to stir 20min；Finally gained mixed liquor is moved into reaction kettle, at 220 DEG C
Under the conditions of carry out coprecipitation reaction 14h.After reaction, obtained material is separated with magnet with solution, and uses deionized water
After washing for several times, it is put into thermostatic drying chamber and is dried under the conditions of 60 DEG C, obtain magnetic active carbon, be denoted as NiFe2O4-PAC；
Weigh 0.5g NiFe2O4- PAC is placed in brown reaction flask, then successively measures 2.5mL thioacetic acid, 1.5mL second
Acid anhydrides and the 15 μ L concentrated sulfuric acids are simultaneously moved into brown reaction flask respectively, by bottle sealing, carry out esterification under the conditions of 80 DEG C
8h；After reaction, obtained material is separated with magnet, and after being washed with deionized for several times with solution, it is dry is put into constant temperature
It is dried under the conditions of 60 DEG C in dry case, obtains magnetic active carbon composite material, be denoted as NiFe2O4-PAC-SH。
Fig. 1 is NiFe prepared by embodiment 12O4The SEM of-PAC-SH schemes；As shown in Figure 1, magnetic nano-particle NiFe2O4
Uniformly it is attached to activated carbon surface.
Fig. 2 is PAC, NiFe prepared by embodiment 12O4- PAC and NiFe2O4The FTIR of-PAC-SH schemes；As shown in Fig. 2,
2363cm-1And 607cm-1The new peak at place, respectively due to-SH and NiFe in thioacetic acid2O4In Ni-O, this illustrates sulfydryl
Successfully it is connected in magnetic active carbon.
Fig. 3 is NiFe prepared by embodiment 12O4- PAC and NiFe2O4The hysteresis loop figure of-PAC-SH；As shown in figure 3,
NiFe2O4- PAC and NiFe2O4- PAC-SH all has stronger magnetic ability.
Embodiment 2
3g active carbon powder is miscible in the nitric acid solution of 500mL 2mol/L, and 90 DEG C are heated to, 6h is persistently stirred,
It will be dried after products therefrom washes clean, obtain the active carbon powder of nitric acid pretreatment；
Weigh 2.38gNiCl2·6H2O and 5.41g FeCl3·6H2O is dissolved in 70mL deionized water, into acquired solution
Be added 2g nitric acid pretreatment active carbon powder, by gained mixture in Ultrasound Instrument ultrasound 30min；After ultrasound, to institute
It obtains and 11mL ammonium hydroxide is added in dispersion liquid, and continue to stir 20min；Finally gained mixed liquor is moved into reaction kettle, at 220 DEG C
Under the conditions of carry out coprecipitation reaction 14h.After reaction, obtained material is separated with magnet with solution, and uses deionized water
After washing for several times, it is put into thermostatic drying chamber and is dried under the conditions of 60 DEG C, obtain magnetic active carbon, be denoted as NiFe2O4-PAC；
Weigh 0.5g NiFe2O4- PAC is placed in brown reaction flask, then successively measures 2.5mL thioacetic acid, 1.5mL second
Acid anhydrides, the glacial acetic acid of 0.5mL and the 15 μ L concentrated sulfuric acids are simultaneously moved into brown reaction flask respectively, by bottle sealing, in 80 DEG C of conditions
Lower progress esterification 8h；After reaction, obtained material is separated with magnet with solution, and be washed with deionized for several times
Afterwards, it is put into thermostatic drying chamber and is dried under the conditions of 60 DEG C, obtain magnetic active carbon composite material, be denoted as NiFe2O4-PAC-SH。
Application examples 1
NiFe prepared by embodiment 12O4- PAC-SH is for adsorbing dimercurion:
It measures the divalent mercury solution that 100mL concentration is 30mg/L to pour into the conical flask of 250mL, uses NaOH solution
PH value of solution is adjusted to 7 by (0.1mol/L) and HCl solution (1mol/L), and the NiFe that dosage is 0.1g/L is added2O4- PAC-SH, most
Conical flask is put into shaking table afterwards and reacts 3h at room temperature；After reaction, mercuric residual concentration is measured, and is calculated pair
The adsorption capacity and removal rate under pH and dosage are answered, concrete outcome is shown in Fig. 4.It is computed, adsorption capacity 298.8mg/g, removes
Rate is 99.6%.
NiFe2O4The desorption of-PAC-SH:
Mercuric NiFe will have been adsorbed with magnet2O4- PAC-SH is separated from aqueous solution, then with 0.15mol/L's
Hydrochloric acid solution washs 3 times, and each scavenging period is 10min.Extra hydrochloric acid solution is washed away into pure water again after cleaning
Property, continue to repeat to adsorb mercuric experiment after 60 DEG C of drying, carries out five regeneration tests, concrete outcome is shown in Fig. 5.
Fig. 4 is PAC, NiFe prepared by embodiment 12O4- PAC and NiFe2O4- PAC-SH removes mercuric effect picture；Such as
Shown in Fig. 4, it is sulfhydryl modified after magnetic active carbon composite material NiFe2O4- PAC-SH compares the adsorption capacity of dimercurion
In PAC and NiFe2O4- PAC is greatly improved, and maximum value is reached in pH=7, and adsorption capacity at this time is
298.8mg/g。
Fig. 5 is NiFe prepared by embodiment 12O4The regenerability figure of-PAC-SH, wherein qeFor adsorption capacity, E is removal
Rate；As shown in figure 5, NiFe2O4- PAC-SH still has good absorption property after repeatedly regenerating, after the 5th regeneration,
Adsorption capacity still reaches 246.2mg/g, reduced by only 17.3%.
Fig. 6 is the coexisting ion of various concentration to NiFe2O4- PAC-SH removes mercuric influence situation schematic diagram；Such as figure
Shown in 6, in the higher Ca of concentration2+In the presence of, competitive Adsorption can be generated with bivalent mercury, influence NiFe2O4- PAC-SH adsorbs divalent
Mercury ion, but NiFe at this time2O4- PAC-SH still has 188mg/g to the adsorbance of dimercurion；Other five kinds of ion K+、Na+、Cl-、NO3 -、SO4 2-To NiFe2O4- PAC-SH, which adsorbs bivalent mercury, to be influenced less, to illustrate NiFe2O4- PAC-SH has preferable anti-
Interference performance.
Application examples 2
NiFe prepared by embodiment 12O4- PAC-SH is for adsorbing trivalent chromic ion:
It measures the trivalent chromium solutions that 100mL concentration is 80mg/L to pour into the conical flask of 250mL, uses NaOH solution
PH value of solution is adjusted to 6 by (0.1mol/L) and HCl solution (1mol/L), and the NiFe that dosage is 0.25g/L is added2O4- PAC-SH,
Finally conical flask is put into shaking table and reacts 3h at room temperature；After reaction, the residual concentration of trivalent chromium is measured, calculates and corresponds to
PH and adsorption capacity and removal rate under dosage.It is computed, adsorption capacity 294.4mg/g, removal rate 92.0%.
Application examples 3
NiFe prepared by embodiment 12O4- PAC-SH is for adsorbing methylene blue:
It measures the methylene blue solution that 100mL concentration is 50mg/L to pour into the conical flask of 250mL, uses NaOH solution
PH value of solution is adjusted to 8 by (0.1mol/L) and HCl solution (1mol/L), and the NiFe that dosage is 0.2g/L is added2O4- PAC-SH, most
Conical flask is put into shaking table afterwards and reacts 4h at room temperature；After reaction, the residual concentration of methylene blue is measured, calculates and corresponds to
PH and adsorption capacity and removal rate under dosage.It is computed, adsorption capacity 245.6mg/g, removal rate 98.2%.
Application examples 4
NiFe prepared by embodiment 12O4- PAC-SH is used for adsorbing phenol:
It measures the phenol solution that 100mL concentration is 100mg/L to pour into the conical flask of 250mL, uses NaOH solution
PH value of solution is adjusted to 7 by (0.1mol/L) and HCl solution (1mol/L), and the NiFe that dosage is 0.5g/L is added2O4- PAC-SH, most
Conical flask is put into shaking table afterwards and reacts 5h at room temperature.After reaction, measure the residual concentration of phenol, calculate corresponding pH and
Adsorption capacity and removal rate under dosage.It is computed, adsorption capacity 186.6mg/g, removal rate 93.3%.
As seen from the above embodiment, the present invention provides a kind of magnetic active carbon composite material and preparation method thereof and answer
With according to embodiment it is found that the adsorption capacity of magnetic active carbon composite material prepared by the present invention is high, to mercuric absorption appearance
It measures up to 298.8mg/g, to common heavy metal ion (dimercurion and trivalent chromic ion) and organic pollutant (methylene
Base is blue and phenol) etc. show good removal effect；Magnetic active carbon composite material prepared by the present invention has stronger
Anti-interference ability and stronger selective absorption, especially show stronger affinity to heavy metal ion, in industrial wastewater
The removal of heavy metal ion and organic pollutant is with good application prospect；Magnetic active carbon composite material prepared by the present invention
With good recycling and power of regeneration, use cost is lower.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of magnetic active carbon composite material, which comprises the following steps:
Nickel source, source of iron, active carbon, water and ammonium hydroxide are mixed, coprecipitation reaction is carried out, obtains magnetic active carbon；
Thioacetic acid, acetic anhydride and the concentrated sulfuric acid are added into the magnetic active carbon, carries out esterification, obtains magnetic active carbon
Composite material.
2. preparation method according to claim 1, which is characterized in that mix nickel source, source of iron, active carbon, water and ammonium hydroxide
Before, the active carbon is mixed with acid solution, carries out sour processing.
3. preparation method according to claim 2, which is characterized in that the acid solution is nitric acid solution, the acid solution
Concentration be 1~2mol/L.
4. preparation method according to claim 2 or 3, which is characterized in that the temperature of the acid processing is 60~90 DEG C, institute
The time for stating acid processing is 6~9h.
5. preparation method according to claim 1, which is characterized in that the mass ratio of the nickel source, source of iron and active carbon is
1.2~2.4:2.7~5.4:1~2；The amount ratio of the active carbon and ammonium hydroxide is 1~2g:6~12mL；The quality of the ammonium hydroxide
Concentration is 25%~28%.
6. preparation method according to claim 1, which is characterized in that the temperature of the coprecipitation reaction is 150~250
DEG C, the time of the coprecipitation reaction is 12~16h.
7. preparation method according to claim 1, which is characterized in that the amount ratio of the magnetic active carbon and thioacetic acid
For 0.5~1g:1.7~3.5mL；The amount ratio of the thioacetic acid, acetic anhydride and the concentrated sulfuric acid be 1.7~3.5mL:1.2~
The μ of 2.5mL:13~25 L.
8. preparation method according to claim 1, which is characterized in that the temperature of the esterification is 50~90 DEG C, institute
The time for stating esterification is 6~10h.
9. the magnetic active carbon composite material that any one of claim 1~8 preparation method is prepared.
10. application of the magnetic active carbon composite material described in claim 9 in absorption heavy metal ion and organic pollutant.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111137891A (en) * | 2020-01-10 | 2020-05-12 | 齐鲁工业大学 | Preparation method of nickel-doped magnetic carbon and application of nickel-doped magnetic carbon in hydrogen production by dark fermentation |
| CN114752632A (en) * | 2022-05-26 | 2022-07-15 | 沈阳航空航天大学 | Application method of modified biochar in methane production by anaerobic digestion of kitchen waste |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101502789A (en) * | 2009-01-22 | 2009-08-12 | 上海交通大学 | Method for preparing magnetic active carbon composite material for water processing |
| CN102600794A (en) * | 2012-04-10 | 2012-07-25 | 东北大学 | Two preparation methods of nanometer magnetic adsorbent |
| CN105771902A (en) * | 2016-05-27 | 2016-07-20 | 北京三聚环保新材料股份有限公司 | Preparation method and application of sulfhydryl activated carbon mercury removal agent |
| CN107442085A (en) * | 2017-08-15 | 2017-12-08 | 苏州科技大学 | A kind of sulfhydryl modified silica Conjugate ferrite core-shell structure magnetic nano composite material and its preparation method and application |
| CN108421533A (en) * | 2018-03-22 | 2018-08-21 | 清华大学 | A kind of magnetic nanoparticle of surface modification, preparation method, application and regeneration method |
-
2019
- 2019-06-21 CN CN201910541144.0A patent/CN110102262A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101502789A (en) * | 2009-01-22 | 2009-08-12 | 上海交通大学 | Method for preparing magnetic active carbon composite material for water processing |
| CN102600794A (en) * | 2012-04-10 | 2012-07-25 | 东北大学 | Two preparation methods of nanometer magnetic adsorbent |
| CN105771902A (en) * | 2016-05-27 | 2016-07-20 | 北京三聚环保新材料股份有限公司 | Preparation method and application of sulfhydryl activated carbon mercury removal agent |
| CN107442085A (en) * | 2017-08-15 | 2017-12-08 | 苏州科技大学 | A kind of sulfhydryl modified silica Conjugate ferrite core-shell structure magnetic nano composite material and its preparation method and application |
| CN108421533A (en) * | 2018-03-22 | 2018-08-21 | 清华大学 | A kind of magnetic nanoparticle of surface modification, preparation method, application and regeneration method |
Non-Patent Citations (1)
| Title |
|---|
| KUAN CHEN等: ""Facile Synthesis of Thiol-Functionalized Magnetic Activated Carbon and Application for the Removal of Mercury(II) from Aqueous Solution"", 《OMEGA》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111137891A (en) * | 2020-01-10 | 2020-05-12 | 齐鲁工业大学 | Preparation method of nickel-doped magnetic carbon and application of nickel-doped magnetic carbon in hydrogen production by dark fermentation |
| CN111137891B (en) * | 2020-01-10 | 2021-11-19 | 齐鲁工业大学 | Preparation method of nickel-doped magnetic carbon and application of nickel-doped magnetic carbon in hydrogen production by dark fermentation |
| CN114752632A (en) * | 2022-05-26 | 2022-07-15 | 沈阳航空航天大学 | Application method of modified biochar in methane production by anaerobic digestion of kitchen waste |
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