CN107262033A - The preparation and application of a kind of attapulgite/Fe3O4/ carbon composites - Google Patents

The preparation and application of a kind of attapulgite/Fe3O4/ carbon composites Download PDF

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Publication number
CN107262033A
CN107262033A CN201710522989.6A CN201710522989A CN107262033A CN 107262033 A CN107262033 A CN 107262033A CN 201710522989 A CN201710522989 A CN 201710522989A CN 107262033 A CN107262033 A CN 107262033A
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China
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attapulgite
composite
magnetic
carbon
carbon nano
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CN201710522989.6A
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Chinese (zh)
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王诗生
盛广宏
戴波
于冬冬
练建军
王萍
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安徽工业大学
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Priority to CN201710522989.6A priority Critical patent/CN107262033A/en
Publication of CN107262033A publication Critical patent/CN107262033A/en

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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
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • 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
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid 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
    • B01J20/28009Magnetic 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
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • C02F2101/22Chromium or chromium compounds, e.g. chromates

Abstract

The invention discloses a kind of attapulgite/Fe3O4The preparation and application of/carbon composite, belong to technical field of heavy metal wastewater treatment.The present invention is prepared using one step hydro thermal method, using attapulgite, molysite and chitosan as raw material, and reproducibility solvent ethylene glycol is by part ferric iron back into ferrous iron in hydrothermal reaction kettle, and reaction in the basic conditions generates magnetic Fe3O4In attapulgite surface nucleation and growth, chitosan carbonization is supported on attapulgite surface for agraphitic carbon, ultimately forms magnetic nanometer composite material.The nano composite material surface is rich in hydroxyl, carboxyl and amino isoreactivity group, available for Cr in water body (VI) Adsorption, under conditions of pH=2 and 298K to water in the maximal absorptive capacity of Cr VI be 250mg/g;With certain magnetic, quick separating can be achieved under conditions of externally-applied magnetic field, the problem of being difficult to separation after attapulgite/carbon nano-composite material absorption is solved.

Description

A kind of attapulgite/Fe3O4The preparation and application of/carbon composite
Technical field
The invention belongs to technical field of heavy metal wastewater treatment, and in particular to a kind of attapulgite/Fe3O4/ carbon is nano combined The preparation method of material, the invention further relates to attapulgite/Fe using above-mentioned preparation3O4/ carbon nano-composite material Adsorption Cr (VI) application in water.
Background technology
Heavy metal chromium is one of pollutant of China's priority acccess control, is mainly derived from plating, metallurgy, process hides, printing and dyeing and changes The three wastes of the industries such as work discharge.Chromium is main in water body to be existed with Cr (III) and two kinds of forms, and wherein Cr (VI) is a kind of acute Carcinogen, migration and toxicity are far above Cr (III), and more easily absorbed by the body and accumulate in vivo.At present, chromate waste water Main methods have chemical precipitation method, solvent extraction method, hyperfiltration, reducing process and absorption method etc..Due to absorption method tool Have the advantages that simple to operate, cost is relatively low, high treating effect, have been widely used for processing waste water containing chrome.
Attapulgite is a kind of clay mineral of the magnesium silicate containing Shuifu County with chain layer structure, with larger ratio table Area, chemism and good absorption property, have been applied to water treatment field.But it is due to the design feature of attapulgite Cause poor to Cr in water (VI) absorption property.Accordingly, it would be desirable to be modified to improve to Cr's in water (VI) to attapulgite Adsorption capacity.At present, the method for modifying of attapulgite has high temperature modified, sour modification, organically-modified etc..These method of modifying are present The shortcomings of method is cumbersome, cost is higher, absorption property is still smaller.
There is scholar to be carried out using hydrothermal carbonization method to attapulgite in recent years organically-modified, so as to improve the suction of attapulgite Attached performance.Using glucose as biomass carbon source, it is organically-modified after attapulgite surface rich in abundant hydroxyl, carboxyl, ketone group, Ester group isoreactivity group, has stronger absorption property (Langmui, 2011,27,8998-9004) to Cr in water (VI);Shell gathers Sugar is as a kind of resourceful natural polymerses, the features such as with bio-intermiscibility, environment friendly, and molecule Containing abundant hydroxyl, amino etc. on chain, there is scholar to be carried out by biomass carbon source of chitosan to attapulgite organically-modified, it is modified Product is to Cr in water (VI) absorption property higher than glucose carbonization modified product.But it is difficult to solid-liquid after above-mentioned all presence absorption Separation, its application in terms of industrialization of limit value.
Magnetic separation method because simple to operate, energy consumption is low, the advantages of be not likely to produce secondary pollution receive much concern.If will have magnetic γ-the Fe of property2O3Or Fe3O4It is incorporated into attapulgite/carbon nano-composite material, then can solves after adsorbent absorption Separation problem.There is scholar using cheap natural nano-material attapulgite clay and useless atlapulgite as raw material, pass through molysite Temperature programming calcining makes the method that organic matter thermal cracking is carbonized in useless atlapulgite under hydrolysis and hydrogen atmosphere, in attapulgite table Face load nanometer magnetic iron oxide (γ-Fe2O3) and carbon, prepare cheap attapulgite/γ-Fe2O3The nano combined material of/carbon Expect (silicate journal, 2009,34 (4):548-553).Although attapulgite/γ-Fe2O3/ carbon nano-composite material has certain Magnetic, but the preparation process of the composite is complex, and experiment condition requires higher.
Using iron ammonium sulfate, glucose and attapulgite as raw material, using one step hydro thermal method be prepared for attapulgite/ Fe3O4/ carbon nano-composite material (carbon technique, 2014,33 (1):23-38).Reaction equation is as follows:
Fe2++2OH-→Fe(OH)2 (1)
3Fe(OH)2+0.5O2→Fe(OH)2+2FeOOH+2H2O (2)
Fe(OH)2+FeOOH→Fe3O4+H2O (3)
When adding ammoniacal liquor, generating polynomial (1) reaction.Before starting due to reaction, raw material is stirred under air, so hair Raw formula (2) reaction.When being transferred in autoclave, generating polynomial (3) reaction generates Fe3O4Particulate load is in attapulgite table Face.The advantage of this method is that preparation process is less, but formula (2) reaction is difficult to control to, and this is due to that ferrous hydroxide is easily empty Gas is oxidized to ferric hydroxide precipitate, is that can not generate Fe in hydrothermal reaction kettle3O4Particle.
The content of the invention
To overcome the deficiencies in the prior art, the technical problem to be solved in the present invention is to provide a kind of preparation process is simple, energy The relatively low and easily controllable attapulgite/Fe of consumption3O4The preparation method of/carbon nano-composite material, to utilize receiving that this is prepared Nano composite material realizes the Adsorption to Cr in water (VI).
The technical problem of the present invention is achieved by the following technical programs.
Attapulgite/the Fe3O4/ carbon nano-composite material is through the following steps that prepared:
1) 1.0g Iron(III) chloride hexahydrates and 0.5g Concave-convex clay rods are added in ethylene glycol, in magnetic agitation condition Lower addition Chitosan powder, obtains light yellow viscous liquid;
Described Iron(III) chloride hexahydrate and the mass ratio of Chitosan powder are 1:0.3~4.5.
2) in step 1) add 3.0g anhydrous sodium acetate powder in obtained faint yellow viscous fluid, and it is stirred continuously 30min, Obtain suspension;
3) by step 2) the obtained suspension of processing be transferred in 100mL ptfe autoclaves (filling degree≤ 80%) 12~48h, is reacted under 180 DEG C of hydrothermal conditions.
4) reaction terminates Magneto separate after natural cooling, with absolute ethyl alcohol and distilled water respectively washing 3~4 times, obtained black Product drying, grinding, sieving, produce attapulgite/Fe3O4/ carbon nano-composite material.
Above-mentioned attapulgite/the Fe prepared3O4/ carbon nano-composite material can be in Adsorption water in Cr (VI) It is applied.
As one kind optimization, the condition of above-mentioned application is:Under 298K, solid-liquid mass ratio is 5:4, pH value of solution is 2~8.
It is used as further optimization, the pH=2 of above-mentioned solution.
The principles of science of the present invention:
The present invention prepares attapulgite/Fe using the step of hydro-thermal method one3O4/ carbon nano-composite material.With attapulgite, iron Salt and chitosan are raw material, in hydrothermal reaction kettle reproducibility solvent ethylene glycol by part ferric iron back into ferrous iron, in alkali Property under the conditions of reaction generation magnetic Fe3O4In attapulgite surface nucleation and growth, chitosan carbonization is supported on recessed for agraphitic carbon Convex rod stone surface, ultimately forms magnetic nanometer composite material.The nano composite material surface is living rich in oxy radical and amino etc. Property group, available for Cr in water body (VI) Adsorption;With certain magnetic, it can be achieved under conditions of externally-applied magnetic field quick Separation, solves the problem of being difficult to separation after attapulgite/carbon nano-composite material absorption.Occur in preparation process of the present invention Specific reaction equation is as follows:
ATP is attapulgite, ATP/Fe in formula (2)3O4/ C is attapulgite/Fe3O4/ C nano composite.
Compared with other similar inventions, the invention has the advantages that:
1) solvent-thermal method is used.The present invention prepares attapulgite/Fe using the step of solvent-thermal method one3O4/ C nano composite wood Material.This method preparation technology is simple, energy consumption is relatively low, easy to control easy to operate.
2) there is excellent magnetic performance.Nano composite material prepared by the present invention has excellent magnetic performance, outside In the presence of portion magnetic field, separation of solid and liquid can be quickly realized in the short period of time.
3) adsorption capacity is big.The adsorbent surface that the present invention is provided is rich in OH, COOH and NH2Isoreactivity group, to sexavalence Chromium has stronger adsorption capacity.Under conditions of 298K, pH=2 and solid-liquid mass ratio=5/4, the theoretical maximum of the adsorbent Adsorbance is 250mg/g.
4) it is cheap, it is widely used.The composite is a kind of new surrounding purifying material, can be widely used in Processing containing heavy metal ion, the sanitary sewage of organic pollution and industrial wastewater.
Brief description of the drawings
Fig. 1 is that (ATP is concave convex rod for infrared spectrum (FTIR) figure of the magnetic attapulgite prepared in the embodiment of the present invention 2 Stone, MATP@C are attapulgite/Fe3O4/ C nano composite).
As shown in Figure 1, not only there is the characteristic absorption peak of attapulgite in MATP@C, separately find several different peaks, 3425cm-1Locate the stretching vibration absworption peak for O-H and N-H, 2929 and 2882cm-1Locate be>C-H's is flexible in CH2 and-CH3 Vibration absorption peak, 1620cm-1The C=C, 1442cm generated after flexural vibrations absworption peak and hydrothermal carbonization that the broad peak at place is N-H-1Locate the C=O absworption peaks that are formed after being carbonized for chitosan, and magnetic iron ore characteristic absorption peak (578cm-1Corresponding Fe-O shakes Dynamic peak).
Fig. 2 be the embodiment of the present invention 2 prepare magnetic attapulgite X-ray diffraction (XRD) figure (ATP is attapulgite, MATP@C are attapulgite/Fe3O4/ C nano composite).
As shown in Figure 2, the characteristic diffraction peak of attapulgite is in 2 θ=8.3 °, 13.6 °, 19.8 °, 27.3 °, this and standard card Piece is completely the same.Attapulgite/Fe3O4/ C nano composite does not only have the characteristic diffraction peak of attapulgite, also magnetic iron ore Characteristic diffraction peak (30.2 °, 35.5,43.2,53.4,57.3).Show attapulgite area load magnetite ore particles.
Fig. 3 is the hysteresis curve figure (VSM) of magnetic attapulgite prepared by the embodiment of the present invention 2.
From the figure 3, it may be seen that magnetic attapulgite of the present invention has certain magnetic, quick separating can be carried out with magnet.
Embodiment
Below by example, the present invention is described in further detail, but the present invention is not limited to following embodiments.
Embodiment 1
1) 1.0g Iron(III) chloride hexahydrates and 0.5g attapulgites are added in 70mL ethylene glycol, added after strong agitation Light yellow viscous liquid is obtained after 0.3g Chitosan powders, ultrasonic disperse 30min;
2) in step 1) addition 3.0g anhydrous sodium acetate powder in obtained thick liquid is handled, and it is stirred continuously 30min;
3) by step 2) the obtained aaerosol solution of processing be transferred in 100mL ptfe autoclaves (filling degree≤ 80%), 24h is reacted under 180 DEG C of hydrothermal conditions;
4) Magneto separate after natural cooling, with absolute ethyl alcohol and distilled water respectively washing 3~4 times, obtained black product is put into Into electric drying oven with forced convection, 60 DEG C of drying, grinding sievings, produce attapulgite/Fe3O4/ C nano composite;
5) magnetic nanometer composite material prepared in 0.05g examples 1 is weighed, 40mLK is added to2Cr2O7(pH=in solution 2,300mg/L), vibrated in 298K to adsorption equilibrium, Cr (VI) concentration in supernatant is determined after Magneto separate, calculating obtains Cr (VI) clearance is 25.4%.
Embodiment 2
1) be the same as Example 1, except that the chitosan added in magnetic nanometer composite material preparation process is 1.5g;
2) 0.05g steps 1 are weighed) the middle adsorbent prepared, it is added to 40mLK2Cr2O7(pH=2,300mg/ in solution L), vibrated in 298K to adsorption equilibrium, Cr (VI) concentration in supernatant is determined after Magneto separate, calculating obtains Cr (VI) clearance For 82.9%.
Embodiment 3
1) be the same as Example 1, except that the chitosan added in magnetic nanometer composite material preparation process is 3.0g;
2) 0.05g steps 1 are weighed) the middle adsorbent prepared, it is added to 40mLK2Cr2O7(pH=2,300mg/ in solution L), vibrated in 298K to adsorption equilibrium, Cr (VI) concentration in supernatant is determined after Magneto separate, calculating obtains Cr (VI) clearance For 93.4%.
Embodiment 4
1) be the same as Example 1, except that the chitosan added in magnetic carbosphere preparation process is 4.5g;
2) 0.05g steps 1 are weighed) the middle adsorbent prepared, it is added to 40mLK2Cr2O7(pH=2,300mg/ in solution L), vibrated in 298K to adsorption equilibrium, Cr (VI) concentration in supernatant is determined after Magneto separate, calculating obtains Cr (VI) clearance For 95.0%.
Embodiment 5
1) be the same as Example 3, except that the hydro-thermal reaction time is 12h;
2) 0.05g steps 1 are weighed) the middle adsorbent prepared, it is added to 40mLK2Cr2O7(pH=2,300mg/ in solution L), vibrated in 298K to adsorption equilibrium, Cr (VI) concentration in supernatant is determined after Magneto separate, calculating obtains Cr (VI) clearance For 85.6%.
Embodiment 6
1) be the same as Example 3, except that the hydro-thermal reaction time is 48h;
2) 0.05g steps 1 are weighed) the middle adsorbent prepared, it is added to 40mLK2Cr2O7(pH=2,300mg/ in solution L), vibrated in 298K to adsorption equilibrium, Cr (VI) concentration in supernatant is determined after Magneto separate, calculating obtains Cr (VI) clearance For 94.8%.
Embodiment 7
The adsorbent prepared in 0.05g embodiments 3 is weighed, 40mLK is added to2Cr2O7In solution (300mg/L), in 298K When vibrate to adsorption equilibrium, Cr (VI) concentration in supernatant is determined after Magneto separate.As adsorbent solution pH=2, Cr (VI) clearance For 93.4%;As adsorbent solution pH=3, Cr (VI) clearance is 21.5%;Adsorbent solution pH=4, Cr (VI) clearance is 16.4%;Adsorbent solution pH=5, Cr (VI) clearance is 14.7%;Adsorbent solution pH=6, Cr (VI) clearance is 13.6%.
It follows that embodiment 3 prepare magnetic nanometer composite material to Cr in water body (VI) adsorbance with pH's Raise and be gradually reduced.
Embodiment 8
The adsorbent prepared in several pieces 0.050g embodiments 3 is weighed, (pH in 20mL potassium bichromate solutions is added separately to =2,300mg/L), vibrated in 298K, Cr (VI) is remaining in supernatant is determined after presetting point in time sampling, Magneto separate Concentration, result of calculation is listed in Table 1 below.
The adsorption dynamics adsorption kinetics of table 1
As shown in Table 1, the adsorbent that the present invention is provided is very fast to Cr (VI) rate of adsorption, and clearance is approached after absorption 1h 90%.
Embodiment 9
Weigh the adsorbent prepared in several pieces 0.050g embodiments 3, be added separately to 40mL various concentrations (100~ 600mg/L) (pH=2) in potassium bichromate solution, vibrated in 298K to adsorption equilibrium, Cr in supernatant is determined after Magneto separate (VI) residual concentration, result of calculation is listed in Table 2 below.
The adsorption isotherm of table 2
F and L-type linear fit are carried out to the data of table 2, as a result meet L-type absorption.Theoretical maximum suction is calculated according to L-type equation Attached amount is 250mg/g.
Described above is the preferred embodiments of the invention, it is noted that for those skilled in the art For, without departing from the technical principles of the invention, some improvements and modifications can also be made, these improvements and modifications Also it should be regarded as protection scope of the present invention.

Claims (4)

1. a kind of attapulgite/Fe3O4The preparation method of/carbon composite, it is characterised in that comprise the following steps:
(1) 1.0g Iron(III) chloride hexahydrates and 0.5g attapulgites are added in 70mL ethylene glycol, shell is added after strong agitation Glycan powder, ultrasonic disperse 30min, obtains light yellow viscous liquid;
The Iron(III) chloride hexahydrate and the mass ratio of Chitosan powder are 1:0.3~4.5;
(2) 3.0g anhydrous sodium acetate powder is added in the thick liquid that step (1) processing is obtained, and is stirred continuously 30min, obtained Aaerosol solution;
(3) aaerosol solution for obtaining step (2) processing is transferred in 100mL ptfe autoclaves, 180 DEG C of hydrothermal conditions 12~48h of lower reaction, filling degree≤80% of the reactor;
(4) Magneto separate after natural cooling, with absolute ethyl alcohol and distilled water respectively washing 3~4 times, obtained black product is put into electricity 60 DEG C of drying, grinding sievings, produce attapulgite/Fe in hot blast drying box3O4/ carbon nano-composite material.
2. such as attapulgite/Fe obtained by claim 1 preparation method3O4/ carbon nano-composite material Cr in Adsorption water (VI) application in.
3. attapulgite/Fe as claimed in claim 23O4/ carbon nano-composite material answering in Cr (VI) in Adsorption water With, it is characterised in that under 298K, solid-liquid mass ratio is 5:4, pH value of solution is 2~8.
4. attapulgite/Fe as claimed in claim 33O4/ carbon nano-composite material answering in Cr (VI) in Adsorption water With, it is characterised in that pH value of solution=2.
CN201710522989.6A 2017-06-30 2017-06-30 The preparation and application of a kind of attapulgite/Fe3O4/ carbon composites CN107262033A (en)

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