CN103785475A - Preparation method of cobalt ferrite conductive imprinting compound photocatalyst - Google Patents

Preparation method of cobalt ferrite conductive imprinting compound photocatalyst Download PDF

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CN103785475A
CN103785475A CN201410006613.6A CN201410006613A CN103785475A CN 103785475 A CN103785475 A CN 103785475A CN 201410006613 A CN201410006613 A CN 201410006613A CN 103785475 A CN103785475 A CN 103785475A
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CN103785475B (en
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逯子扬
罗莹莹
杨丽丽
蒋银花
霍鹏伟
邢伟男
王丹丹
闫永胜
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Jiangsu University
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Abstract

The invention belongs to the technical field of the preparation of environmental materials, and particularly relates to a preparation method of a cobalt ferrite conductive imprinting compound photocatalyst. The preparation method comprises the following steps: pretreating MWCNTs (Multiwalled Carbon Nanotubes) to obtain acidified MWCNTs; dispersing Co(NO3)2.6H2O and Fe(NO3)3.9H2O into water for ultraphonic, then adding activated MWCNTs for the ultrasonic, and finally adding alkali, stirring and then carrying out hydro-thermal synthesis to obtain CoFe2O4/MWCNTs; adding 2-mercaptobenzothiazole to pyrrole-containing trichloromethane, adding a cross-linking agent and an initiating agent, adding a mixed solution to a CoFe2O4/MWCNTs solution with activated polyethylene glycol 4000, stirring for a period of time under an N2 atmosphere, and washing and drying to obtain a PPy/CoFe2O4/MWCNTs magnetic molecule imprinting photocatalyst.

Description

A kind of preparation method of Conjugate ferrite conduction trace composite photo-catalyst
Technical field
The invention belongs to material and environment preparing technical field, be specially the method for utilizing Hydrothermal Synthesis and suspension polymerisation to combine and prepare PPY@CoFe 20 4the magnetic molecularly imprinted photochemical catalyst of/MWCNTs.
Background technology
2-mercaptobenzothiazole, as the one of mercaptan, commonly uses and does corrosion inhibiter, antimycotic medicine, and agriculture chemicals fungicide and thiofide, it is extensively present in waste water, and river, in sewage treatment plant and surface water.Because 2-mercaptobenzothiazole is poisonous, can induced tumor, allergy, poisonous and hinder wastewater treatment to aquatile, the 2-mercaptobenzothiazole of removing in environment is necessary.At present, adopted multiple technologies as absorption, photochemical catalytic oxidation, biodegradation, hydrodesulfurization and electric reactor process disposal of mercaptans.Because photocatalysis technology can be by many poisonous and not biodegradable organic matter permineralizations, its application has caused extensive concern.
CNT can prevent the gathering of nano particle and improve the avtive spot of catalyst, can show excellent catalytic activity as catalyst carrier.Meanwhile, carry out secondary utilization in order to reclaim catalyst, magnetic carbon material is synthesized and for photocatalysis.In magnetic nano-particle, due to Conjugate ferrite (CoFe 20 4) there is unique physics, electronics and magnetic properties, be widely used.In recent years, by hydrothermal synthesis method, electrostatic spinning, the synthetic CoFe of in-situ high temperature hydrolysis and chemical vapour deposition technique 2o 4/ MWCNTs, and for the pollutant of the environment of degrading.
Molecularly imprinted polymer is easy to preparation, and low consumption, has stability, can reuse and carry out specific recognition.By introducing conducting polymer polypyrrole, can further improve photocatalytic activity and selective.Molecular imprinting utilizes the covalently or non-covalently effect between template molecule and monomer, prepares the polymer with specific structure by cross-linked polymeric and wash-out.Current molecular imprinting comprises sol-gel process, heating using microwave, precipitation polymerization and emulsion polymerisation etc.Consider the formation of recognition site, avoid particle to assemble and simplify experimental procedure, adopted suspension polymerization herein.
Summary of the invention
The method that the present invention adopts hydro-thermal method and suspension polymerisation to combine, prepares PPY/CoFe 2o 4/ MWCNTs magnetic conductive trace photochemical catalyst.Its advantage is to build a cyclic process in system, realizes light induced electron effective separate right with hole; Can effectively utilize light source to reach the object of mercaptan waste water in effective degraded environment.
The technical solution used in the present invention is:
(1) CoFe 2o 4the preparation of/MWCNTs: multi-walled carbon nano-tubes (MWCNTs) is joined to red fuming nitric acid (RFNA) and the concentrated sulfuric acid mixed solution that volume ratio is 1:3 ain, stir 6h at 60 ℃, washing 40～60 ℃ of vacuum drying, so acidification obtains the MWCNTs of activation; By Co (NO 3) 26H 2o and Fe (NO 3) 39H 2o is scattered in water, ultrasonic 10min, then by the MWCNT of activation sadd in the above-mentioned aqueous solution and ultrasonic 10min, finally add N aoH solid also stirs 30min.The solution of gained proceeds in autoclave, 100～200 ℃ of Hydrothermal Synthesis 4～16h, and water and ethanol washing respectively, 40～60 ℃ of vacuum drying, obtain CoFe 2o 4/ MWCNTs.
(2) CoFe 2o 4the activation of/MWCNTs: the CoFe that step (1) is made 2o 4/ MWCNTs and Macrogol 4000 are added to the water, and ultrasonic dispersion obtains the CoFe activating 2o 4/ MWCNTs suspension.
(3) preparation of Conjugate ferrite conduction trace composite photo-catalyst: the 2-mercaptobenzothiazole and the pyrroles that are 1: 1～24 by mol ratio join in chloroform, then add crosslinking agent and initator, and ultrasonic venting one's spleen, obtains mixed solution b.Then mixed solution b is joined to the CoFe of activation 2o 4in/MWCNTs suspension, under 40 ℃ of nitrogen atmospheres, stir 6～36h.After water, methyl alcohol and ethanol washing, be placed in 40～60 ℃ of vacuum drying chambers and dry respectively, obtain magnetic blotting molecule photochemical catalyst PPy/CoFe 2o 4/ MWCNTs.
(4) Conjugate ferrite conducts electricity the preparation of non-trace photochemical catalyst: pyrroles is joined in chloroform, then add crosslinking agent and initator, ultrasonic venting one's spleen, obtains mixed solution c.Then by mixed solution cjoin the CoFe of activation 2o 4in/MWCNTs suspension, under 40 ℃ of nitrogen atmospheres, stir 24h.After water, methyl alcohol and ethanol washing several times, be placed in 40～60 ℃ of vacuum drying chambers and dry respectively, obtain the non-microsphere photochemical catalyst of magnetic PPy/CoFe2O4/MWCNTs.
In described step (1), the amount ratio of MWCNTs and red fuming nitric acid (RFNA) concentrated sulfuric acid mixed liquor a is 25mg:3mL.
In described step (1), Co (NO 3) 26H 2o, Fe (NO 3) 39H 2the ratio of the consumption of O, water is 1mmo1:2mmo1:30mL.
In described step (1), Co (NO 3) 26H 2the ratio of the MWCNTs of O, activation and the consumption of NaOH is 1mmo1:60mg:4.5g.
In described step (2), CoFe 2o 4the ratio of the consumption of/MWCNTs, Macrogol 4000 and water is 1g:10g:150mL.
In described step (3) and (4), crosslinking agent is trimethylol-propane trimethacrylate TRIM, and initator is ABVN ABVN.
In described step (3), 2-mercaptobenzothiazole in mixed solution b: chloroform: TRIM:ABVN=2mmo1:15mL:1mL:1.2mmo1.
In described step (3), the CoFe of mixed solution b and activation 2o 4the volume ratio of/MWCNTs solution is 10～13:100.
In described step (4), pyrroles in mixed solution c: chloroform: TRIM:ABVN=2～48mmo1:15 ml:1 ml:12 mmo1.
In described step (4), the CoFe of mixed solution c and activation 2o 4the volume ratio of/MWCNTs solution is 10～13:100.
The present invention adopts Hydrothermal Synthesis technology to prepare CoFe 2o 4/ MWCNTs, then prepare PPy/CoFe by suspension polymerisation molecular imprinting 2o 4/ MWCNTs magnetic conductive trace photochemical catalyst.
Photocatalytic activity is evaluated: in GHX-2 type photochemical reaction instrument (purchased from Educational Instrument Factory of Yangzhou University), carry out, ultraviolet lamp irradiates, 50mL2-mercaptobenzothiazoler simulated wastewater is added in reaction bulb and adds composite photo-catalyst, magnetic agitation and open aerator pass into air make catalyst in suspend or afloat, dark absorption a period of time is measured initial concentration, then carry out illumination, 10min sample analysis in interval in During Illumination, magnetic is got liquid at ultraviolet specrophotometer λ after separating max=321nm place measures absorbance, and passes through C/C 0judge degradation efficiency, wherein C 0the initial concentration of 2-mercaptobenzothiazole solution during for beginning light degradation, C is the concentration of the 2-mercaptobenzothiazole solution of timing sampling mensuration.
Technological merit of the present invention: conductive light catalyst system can effectively improve the right separative efficiency of light induced electron and hole; Magnetic photocatalyst contributes to improve the rate of recovery of catalyst; Selective disposal of mercaptans class waste water preferably.
Accompanying drawing explanation
Fig. 1 CoFe 2o 4/ MWCNTs (a), PPy/CoFe 2o 4/ MWCNTs conduction trace photochemical catalyst (b) and PPy/CoFe 2o 4the ultraviolet degradation rate collection of illustrative plates of the 2-mercaptobenzothiazole simulated wastewater of the 20mg/L of the non-trace photochemical catalyst of/MWCNTs (c) to 50mL.
Fig. 2 CoFe 2o 4/ MWCNTs (a) and PPy/CoFe 2o 4the X-ray diffractogram of/MWCNTs conduction trace photochemical catalyst (b).
Fig. 3 CoFe 2o 4/ MWCNTs (a) and PPy/CoFe 2o 4the TEM figure of/MWCNTs conduction trace photochemical catalyst (b).
Fig. 4 CoFe 2o 4/ MWCNTs (a) and PPy/CoFe 2o 4the FT-IR spectrogram of/MWCNTs conduction trace photochemical catalyst (b).
Fig. 5 CoFe 2o 4/ MWCNTs (a) and PPy/CoFe 2o 4the UV-vis DRS figure of/MWCNTs conduction trace photochemical catalyst (b).
The specific embodiment
Below in conjunction with concrete embodiment, the present invention will be further described.
Embodiment 1:(1) (red fuming nitric acid (RFNA) and the concentrated sulfuric acid are respectively 15mL for the red fuming nitric acid (RFNA) that is 1:3 by effective 0.5g multi-wall carbon nano-tube volume ratio and concentrated sulfuric acid mixed solution 60mL, 45mL) at 60 ℃, stir 6h, washing 40 ℃ of one nights of vacuum drying, so acidification obtains the MWCNTs of activation; By 0.291gCo (NO 3) 26H 2o and 0.808gFe (NO 3) 39H 2o is scattered in 30mL water and ultrasonic 10min, then the MWCNTs of 60mg activation is added in above-mentioned solution and ultrasonic 10min, finally adds 4.5 gnaOH the solution that stirs 30min. gained proceed in autoclave, 180 ℃ of Hydrothermal Synthesis 12h, and water and ethanol washing respectively, at 40 ℃ of one nights of vacuum drying, obtains CoFe 2o 4/ MWCNTs.
(2) preparation of magnetic molecularly imprinted photochemical catalyst: by the 1g CoFe making in above-mentioned steps (1) 2o 4/ MWCNTs and 10g polyethylene glycol (4000) join in 150mL water, and ultrasonic dispersion obtains the CoFe activating 2o 4/ MWCNTs; 2mmo12-mercaptobenzothiazoler and 8mmo1 pyrroles are joined in 15mL chloroform, add 1.0mL TRIM and 1.2mmo1ABVN, ultrasonic venting one's spleen.Again above-mentioned solution is joined to the CoFe of activation 2o 4in/MWCNTs solution, under 40 ℃ of nitrogen atmospheres, stir 24h.After water, methyl alcohol and ethanol washing several times, be placed in 40 ℃ of vacuum drying chambers and dry respectively, obtain PPy/CoFe 2o 4/ MWCNTs conduction trace photochemical catalyst.Under similarity condition, do not add 2-mercaptobenzothiazole template molecule and make non-molecular engram photochemical catalyst.
(3) get the CoFe making in step (1) 2o 4/ MWCNTs0.1g, the PPy/CoFe making in step (2) 2o 4/ MWCNTs conduction trace photochemical catalyst 0.1g and non-trace sample 0.1g carry out photocatalytic degradation test in photochemical reaction instrument, record each sample to 2-mercaptobenzothiazole the efficiency that removes at 60min, as Fig. 1, PPy/CoFe 2o 4/ MWCNTs conduction trace photochemical catalyst has stronger photocatalytic activity and selective.
Embodiment 2: undertaken by the same step of embodiment 1 preparation technology, the Hydrothermal Synthesis temperature that different is in step (1) is respectively 100 ℃, 140 ℃, 200 ℃; By preparing different CoFe 2o 4/ MWCNTs investigates the impact of different temperatures on synthetic photochemical catalyst, and result shows that the photochemical catalyst effect making in the time that synthesis temperature is 180 ℃ is best.
Embodiment 3: undertaken by the same step of embodiment 1 preparation technology, the Hydrothermal Synthesis time that different is in step (1) is respectively 4h, 8h, 16h; By preparing different CoFe 2o 4/ MWCNTs investigates the impact of different reaction time on photochemical catalyst, and result shows that the photochemical catalyst effect making in the time that generated time is 12h is best.
Embodiment 4: undertaken by the same step of embodiment 1 preparation technology, different is that in step (2), pyrroles's amount is respectively 2mmo1,24mmo1,48mmo1; Investigate the impact of the different function monomers of measuring on trace photocatalyst activity by preparing different trace catalyst.Press the activity of (3) step investigation light degradation 2-mercaptobenzothiazole waste water in embodiment 1.Result shows, when pyrroles's amount is during for 8mmo1, light degradation effect is best.
Embodiment 5: undertaken by the same step of embodiment 1 preparation technology, different is that in step (2), polymerization reaction time is respectively 6h, 12h, 36h.Investigate the impact of polymerization reaction time on trace photocatalyst activity by preparing different trace catalyst.Press the activity of (3) step investigation light degradation 2-mercaptobenzothiazole waste water in embodiment 1.Result shows, in the time that polymerization reaction time is 24h, light degradation effect is best.
As can be seen from Figure 1, CoFe 2o 4/ MWCNTs (a), PPy/CoFe 2o 4/ MWCNTs conduction trace photochemical catalyst (b) and PPy/CoFe 2o 4the ultraviolet degradation rate of the 2-mercaptobenzothiazole simulated wastewater of the 20mg/L of the non-trace photochemical catalyst of/MWCNTs (c) to 50mL, shows that the photochemical catalyst making has good photocatalytic activity and selective.
From Fig. 2, CoFe 2o 4/ MWCNTs and PPy/CoFe 20 4in the X-ray diffractogram of/MWCNTs conduction trace photochemical catalyst, can find out CoFe in conduction trace photochemical catalyst 2o 4 diffractive features peak 20=30.1.，35.5。，43.2。，53.5。，57.0。With 62.6., this shows that PPY does not change CoFe 2o 4crystal formation.Calculate CoFe according to Scherrer equation 2o 4at CoFe 2o 4/ MWCNTs and PPy/CoFe 2o 4size in/MWCNTs is respectively 19.0nm and 17.7nm.In addition, the broad peak of PPY shows that PPY is unbodied.
From Fig. 3, CoFe 2o 4/ MWCNTs and PPy/CoFe 2o 4in the TEM figure of/MWCNTs conduction trace photochemical catalyst, can find out CoFe 2o 4on MWCNTs, build up.Can draw CoFe by statistical method 2o 4at CoFe 2o 4/ MWCNTs and PPY/CoFe 2o 4size in/MWCNTs is respectively 19.1nm and 17.2nm, and this is consistent with X-ray diffraction result.
From Fig. 4, CoFe 2o 4/ MWCNTs and PPY/CoFe 2o 4in the FT-IR spectrogram of/MWCNTs, 582cm -1belong to metal-O, 1387cm -1for the O-H key chattering of adsorption particle, 2974cm -1belong to C-H and PPy/CoFe 2o 4in/MWCNTs, peak strengthens.PPY/CoFe 2o 4/ MWCNTs is at 1635cm, 1457cm, 1264cm -1, 1150cm -1and 1050cm -1be respectively N-H flexural vibrations, pyrrole ring is flexible, C-N flexible and=C-H in-plane deformation.Due to PPY and CoFe 2o 4the interaction of/MWCNTs, these peaks produce peak value and move.In addition 1733em, -1the absworption peak of (-C=Ogroup) is likely due to the existence of crosslinking agent or the peroxidating of PPY.This shows that PPY well implants in imprinted layer.
From Fig. 5, can find out, and CoFe 2o 4/ MWCNTs compares, PPy/CoFe 2o 4in the UV-vis DRS spectrum of/MWCNTs conduction trace photochemical catalyst, absworption peak generation blue shift.But PPY/CoFe 2o 4/ MWCNTs magnetic conductive trace photochemical catalyst has very high absorption intensity in UV, visible light region, shows that it has good Uv and visible light absorbability.
Shown in table 1, CoFe 2o 4/ MWCNTs and PPY/CoFe 2o 4the specific area of/MWCNTs is respectively 9.627m 2/ g and 35.531m 2/ g, illustrates that trace process can produce more recognition site, thereby increases specific area and the adsorptivity of catalyst.They are all meso-hole structure for the pore size explanations of catalyst.
Table 1
[0041]

Claims (5)

1. a preparation method for Conjugate ferrite conduction trace composite photo-catalyst, is characterized in that carrying out according to following step:
(1) CoFe 2 o 4 the preparation of/MWCNTs: multi-walled carbon nano-tubes MWCNTs is joined in the red fuming nitric acid (RFNA) and concentrated sulfuric acid mixed solution a that volume ratio is 1:3, stir 6 h at 60 ℃, washing 40 ~ 60 ℃ of vacuum drying, acidification obtains the MWCNTs of activation; By Co (NO 3 ) 2 6H 2 o and Fe (NO 3 ) 3 9H 2 o is scattered in water, ultrasonic 10 min, then the MWCNTs of activation is added in the above-mentioned aqueous solution and ultrasonic 10 min, finally add NaOH solid and stir 30 min; The solution of gained proceeds in autoclave, 100 ~ 200 ℃ of Hydrothermal Synthesis 4 ~ 16h, and water and ethanol washing respectively, 40～60 ℃ of vacuum drying, obtain CoFe 2 o 4 / MWCNTs;
(2) CoFe 2o 4the activation of/MWCNTs: the CoFe that step (1) is made 2o 4/ MWCNTs and Macrogol 4000 are added to the water, and ultrasonic dispersion obtains the CoFe activating 2o 4/ MWCNTs suspension;
(3) preparation of Conjugate ferrite conduction trace composite photo-catalyst: the 2-mercaptobenzothiazole and the pyrroles that are 1:1 ~ 24 by mol ratio join in chloroform, then add crosslinking agent and initator, and ultrasonic venting one's spleen, obtains mixed solution b; Again above-mentioned solution b is joined to the CoFe of activation 2o 4in/MWCNTs suspension, under 40 ℃ of nitrogen atmospheres, stir 6 ~ 36h; After water, methyl alcohol and ethanol washing, be placed in 40～60 ℃ of vacuum drying chambers and dry respectively, obtain magnetic blotting molecule photochemical catalyst PPy/CoFe 2o 4/ MWCNTs.
2. the preparation method of a kind of Conjugate ferrite conduction trace composite photo-catalyst as claimed in claim 1, is characterized in that: in step (1), the amount ratio of described MWCNTs and red fuming nitric acid (RFNA) concentrated sulfuric acid mixed liquor a is 25 mg:3 mL; Described Co (NO 3 ) 2 6H 2 o, Fe (NO 3 ) 3 9H 2 the ratio of O, water three's consumption is 1mmol:2mmol:30mL; Described Co (NO 3 ) 2 6H 2 the ratio of the MWCNTs of O, activation and NaOH three's consumption is 1mmol:60mg:4.5g.
3. the preparation method of a kind of Conjugate ferrite conduction trace composite photo-catalyst as claimed in claim 1, is characterized in that:
In step (2), described CoFe 2o 4the ratio of the consumption of/MWCNTs, Macrogol 4000 and water is 1g:10g:150mL.
4. the preparation method of a kind of Conjugate ferrite conduction trace composite photo-catalyst as claimed in claim 1, is characterized in that:
In step (3), described crosslinking agent is trimethylol-propane trimethacrylate TRIM, and initator is ABVN ABVN.
5. the preparation method of a kind of Conjugate ferrite conduction trace composite photo-catalyst as described in claim 1 or 4, it is characterized in that: in step (3), 2-mercaptobenzothiazole in described mixed solution b: chloroform: TRIM:ABVN=2 mmol:15mL:1mL:1.2mmol; Described mixed solution b and the CoFe of activation 2o 4the volume ratio of/MWCNTs solution is 10 ~ 13:100.
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CN104001173A (en) * 2014-06-09 2014-08-27 上海师范大学 Water-soluble multifunctional CoFe2O4@MnFe2O4@polypyrrole satellite structure nanomaterial and preparation method and application thereof
CN116002842A (en) * 2022-12-22 2023-04-25 昆明理工大学 Method for degrading carbamazepine by activating peroxyacetic acid with carbon nano tube supported catalyst

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104001173A (en) * 2014-06-09 2014-08-27 上海师范大学 Water-soluble multifunctional CoFe2O4@MnFe2O4@polypyrrole satellite structure nanomaterial and preparation method and application thereof
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CN116002842A (en) * 2022-12-22 2023-04-25 昆明理工大学 Method for degrading carbamazepine by activating peroxyacetic acid with carbon nano tube supported catalyst
CN116002842B (en) * 2022-12-22 2024-04-12 昆明理工大学 Method for degrading carbamazepine by activating peroxyacetic acid with carbon nano tube supported catalyst

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