CN104971778A - Preparation method and applications of ferriferrous oxide-polyaniline-gold nano composite material - Google Patents

Preparation method and applications of ferriferrous oxide-polyaniline-gold nano composite material Download PDF

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CN104971778A
CN104971778A CN201510374440.8A CN201510374440A CN104971778A CN 104971778 A CN104971778 A CN 104971778A CN 201510374440 A CN201510374440 A CN 201510374440A CN 104971778 A CN104971778 A CN 104971778A
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composite material
gold
pani
polyaniline
volume ratio
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李方
陈东升
薛涛
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Tianjin University
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Tianjin University
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Abstract

The invention discloses a preparation method a ferriferrous oxide-polyaniline-gold nano composite material. According to the preparation method, nano Fe3O4 is synthesized via solvothermal method, and is taken as the core of the composite material; Fe3O4 is uniformly dispersed into a PVP aqueous solution; aniline monomer, citric acid, and initiator ammonium peroxydisulfate are added respectively under ice bath and continuous stirring so as to form polyaniline on the surface of nano Fe3O4 from aniline via polymerization, and obtain a Fe3O4-PANI core-shell structure composite material; assembling of prepared gold nanosol with Fe3O4-PANI is realized via electrostatic attraction; and finally seed-mediated growth is adopted, and gold shell is prepared from gold seed with methanol and a reductive gold salt solution so as to obtain the ferriferrous oxide-polyaniline-gold nano composite material. The preparation method of ferriferrous oxide-polyaniline-gold nano composite material is low in cost, simple in technology, and excellent in performance; and the ferriferrous oxide-polyaniline-gold nano composite material is sensitive and rapid, and can be recycled in catalyzing pollutant p-nitrophenol.

Description

A kind of preparation method of tri-iron tetroxide-polyaniline-gold nano composite and application thereof
Technical field
The present invention relates to a kind of preparation method and application of nano composite material of quick catalysis p-nitrophenol
Background technology
In recent years, phenol and the pollution of phenol compound to water body cause to be paid close attention to widely, and China is classified as one of pollutant needing priority acccess control in water.Wherein, p-nitrophenol (4-NP) is a class high toxicity, difficult degradation, be difficult to the compounds administered most, is therefore the technical barrier in China and even the world containing the water purification of giving up of phenol and compound fragrant hydrocarbon.And the toxicity of the reduzate para-aminophenol (4-AP) of 4-NP is relatively much lower, be important chemical industry and medicine intermediate simultaneously.The conversion of 4-NP to 4-AP, can realize the degraded of 4-NP, also effectively can produce 4-AP.At present, the minimizing technology of conventional 4-NP has: absorption method, microbial degradation method, photocatalytic degradation method, electrocoagulation and electrochemical treatment etc.Although the removal of said method to 4-NP has certain effect, there is limitation, as can not be effectively degraded, the slow and secondary pollution of degradation speed etc.In addition, running cost, reaction condition, equipment etc. are also had higher requirements.Therefore, how proposing practical, efficient, quick and eco-friendly solution and strategy is this field bottleneck problem urgently to be resolved hurrily.
Along with the rapid emergence of nanometer technology, nanogold particle (AuNPs) is used widely in optics, catalysis, electrochemistry, biology sensor and the field such as antibacterial.Wherein, as the powerful that catalysis 4-NP reduces, nano gold catalysis material is subject to extensive concern day by day.This route have mild condition, efficient, fast and the advantage such as environmental friendliness, there is outstanding feature in phenol wastewater purification, become the Some Questions To Be Researched in this direction.
Nano gold grain catalytic activity and its size, distribution and morphologic correlation.How obtaining that size is little, homogeneous, high degree of dispersion, nano catalyst that is stable and that be easy to separation and recovery be important research target, is also the bottleneck that its actual application surface faces.In order to improve stability and the catalytic activity of nanogold particle, better solved by immobilized obtained nm of gold compound catalyze material that nano-metal particle is easily reunited, the drawback of separation and recovery difficulty, the structures and characteristics of carrier and the interaction of gold and carrier interface simultaneously may play facilitation to its performance.
Core-shell type nano Au catalysis material a kind ofly constructs novelty, higher level ordered composite nanometer package assembly.Especially Fe 3o 4/ shell/Au magnetic nanometer composite material has many advantages.The kernel of magnetic can make catalysis material efficiently be separated by externally-applied magnetic field, reduces running cost, can control the process of reacting easily.And shell can not only suppress Fe in nucleocapsid compound 3o 4reunion, improve its stability, meanwhile, shell can provide modify space, be conducive to the immobilized of AuNPs.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of with low cost, technique is simple, the preparation method of the tri-iron tetroxide-polyaniline-gold nano composite of function admirable and have the sensitive advantage that fast, can to reuse in the application process of catalysis pollutant p-nitrophenol.
In order to solve the problems of the technologies described above, the preparation method of a kind of tri-iron tetroxide-polyaniline-gold nano composite that the present invention proposes, comprises the following steps:
Step one: obtain the Fe that particle diameter is 200 ~ 350nm with solvent-thermal method 3o 4nano particle;
Step 2: take the Fe that step one is obtained 3o 4nano particle is soluble in water, Fe 3o 4quality-the volume ratio of nano particle and water is 1 ~ 2mg/mL, stirs, and is that 1 ~ 2mg/mL adds PVP according to the quality-volume ratio of PVP and water, stirs and ultrasonic 30 minutes obtained mixed solution A, mixed solution A is at room temperature stirred 3 hours; Then aniline monomer and citric acid is added successively, aniline, citric acid, Fe 3o 4the mass ratio of nano particle is 1 ~ 4:10:2, stirs and ultrasonic 15min; 10 minutes are stirred again according to APS and Fe under condition of ice bath 3o 4the mass ratio of nano particle is that 5:2 adds APS, stirs 7 ~ 9 hours, product distilled water and absolute ethyl alcohol are repeatedly cleaned under the condition of ice bath; Thus at Fe 3o 4nano grain surface wraps up one deck polyaniline, prepares Fe 3o 4-PANI composite material of core-shell structure;
Step 3: according to the HAuCl of volume ratio 1:100 by 1wt% 4the aqueous solution is soluble in water, magnetic agitation 10min; Be the trisodium citrate that 1:100 adds 1wt% according to the volume ratio of trisodium citrate and water, then add the HAuCl doubling 1wt% simultaneously 4the 1wt% trisodium citrate of aqueous solution volume and 0.08wt% sodium borohydride; Magnetic agitation reaction 30 ~ 60min, prepares nm of gold seed solution;
Step 4: be 0.5 ~ 2mg/mL according to quality-volume ratio, the Fe obtained by step 2 3o 4-PANI composite material of core-shell structure joins the obtained nm of gold seed solution of step 3, mechanical agitation ultrasonic 10min, mechanical agitation 3 ~ 5h under room temperature, with magnet by product separation, product distilled water and absolute ethyl alcohol is respectively cleaned 3 times, prepares Fe 3o 4-PANI-Au inano composite material;
Step 5: be that 0.3mg/ml adds sodium carbonate in distilled water according to quality-volume ratio, after mechanical agitation 15min, add 1wt% aqueous solution of chloraurate, the volume ratio of 1wt% aqueous solution of chloraurate and distilled water is 3:200, mechanical agitation 9 ~ 12h under lucifuge condition, obtain reducing golden salting liquid, for subsequent use;
Step 6: be 2 ~ 5mg/mL according to quality-volume ratio, the Fe obtained by step 4 3o 4-PANI-Au inano composite material joins the obtained reduction gold salting liquid of step 5, stirs, then is that 400:1 adds formaldehyde according to the volume ratio of the golden salting liquid of reduction and formaldehyde, reaction 10min;
Step 7: be that 2 ~ 3mg/mL continues to add the golden salting liquid of reduction according to quality-volume ratio, stirs, then is that 400:1 adds formaldehyde according to the volume ratio of the golden salting liquid of reduction and formaldehyde, reaction 10min;
Step 8: step 7 is repeated N time, wherein N is 1 ~ 5 time; By distilled water and ethanol repeatedly washed product, prepare Fe 3o 4-PANI-Au iInano composite material.
Above-mentioned Fe 3o 4-PANI-Au iInano composite material may be used for the catalysis of p-nitrophenol in catalysis pollutant.
Compared with prior art, the invention has the beneficial effects as follows:
1, the present invention avoids loaded down with trivial details centrifugal process in preparation process, simplifies preparation process, without the need to professional equipment in application process, greatly reduces running cost;
Compared with the minimizing technology of 2, the 4-NP such as the present invention and existing absorption method, microbial degradation method, not only degradation speed is fast, and catalyst can recycle and reuse simultaneously, not only saves cost, also avoid secondary pollution;
3, the present invention selects polyaniline to be intermediate layer, with non-metallic layer as SiO 2layer is compared, the Fe of positively charged 3o 4-PANI composite material of core-shell structure and electronegative nm of gold can directly by together with electrostatic attraction assemblings, and do not need to intermediate layer carry out base group modification could and nm of gold assemble, and polyaniline and nm of gold combine more tight;
4, the present invention uses seed mediated growth method trapping gold shell on the basis of ADSORPTION OF GOLD seed, and the existence of golden shell effectively can reduce the loss that comes off of nm of gold in application process, substantially increases recycling ability;
5, product stability of the present invention is good, recyclability is good, catalytic performance is good, good in anti-interference performance.
Accompanying drawing explanation
Fig. 1 is Fe prepared by the embodiment of the present invention 1 3o 4sEM figure;
Fig. 2 is the TEM figure of nanometer Au seed prepared by the embodiment of the present invention 1;
Fig. 3 is Fe prepared by the embodiment of the present invention 1 3o 4the TEM figure of-PANI;
Fig. 4 is Fe prepared by the embodiment of the present invention 1 3o 4-PANI partial enlargement TEM schemes;
Fig. 5 is Fe prepared by the embodiment of the present invention 2 3o 4-PANI partial enlargement TEM schemes;
Fig. 6 is Fe prepared by the embodiment of the present invention 1 3o 4-PANI-Au ithe TEM figure of nano composite material;
Fig. 7 is Fe prepared by the embodiment of the present invention 1 3o 4-PANI-Au iIthe TEM figure of nano composite material;
Fig. 8 is Fe prepared by the embodiment of the present invention 3 3o 4-PANI-Au iIthe TEM figure of nano composite material;
Fig. 9 is the UV-vis figure of the catalysis p-nitrophenol that the embodiment of the present invention 3 obtains;
Figure 10 is the Fe that the embodiment of the present invention 3 obtains 3o 4-PANI-Au iI(black) and Fe 3o 4-PANI-Au ithe recycling number of times figure of (twill).
Detailed description of the invention
Be described in further detail technical solution of the present invention below in conjunction with the drawings and specific embodiments, described specific embodiment only explains the present invention, not in order to limit the present invention.
Embodiment 1
Step one: solvent-thermal method prepares the Fe that particle diameter is 200 ~ 350nm 3o 4nano particle, step is as follows: by 1gFeCl 36H 2o and 0.4g trisodium citrate joins in 30mL ethylene glycol, dissolves completely, under agitation adds 2.4g anhydrous sodium acetate, is transferred in 50mL polytetrafluoroethylene (PTFE) autoclave by mixed solution after continuing to stir 30min.Reactor is reacted 9h in the insulating box of 200 DEG C.After reaction terminates, naturally cool to room temperature, be separated with magnet and obtain black Fe 3o 4nano particle, respectively clean 3 times with distilled water and absolute ethyl alcohol, vacuum drying is stand-by;
Step 2: preparation Fe 3o 4-PANI composite material of core-shell structure: take the Fe that step one is obtained 3o 4nano particle 0.2g is dissolved in 200mL water, stirs, and adds 0.2gPVP, stirs and ultrasonic 30 minutes obtained mixed solutions, this mixed solution is at room temperature stirred 3 hours.Then add 0.1g aniline monomer and 1g citric acid successively, stir and ultrasonic 15min.Stir under condition of ice bath and within 10 minutes, add 0.5g ammonium peroxydisulfate (APS) again, stir 9 hours under the condition of ice bath, product distilled water and absolute ethyl alcohol are cleaned repeatedly; Thus at Fe 3o 4nano grain surface wraps up one deck polyaniline, prepares Fe 3o 4-PANI composite material of core-shell structure;
Step 3: preparation nm of gold seed solution: the HAuCl at room temperature adding 2ml 1wt% in 200ml distilled water 4solution, magnetic agitation 10min.Backward solution in add the trisodium citrate of 2ml 1wt%, then add 2ml 1wt% trisodium citrate and 2mL 0.08wt% sodium borohydride simultaneously; Magnetic agitation reaction 60min, prepares nm of gold seed solution, stand-by;
Step 4: preparation Fe 3o 4-PANI-Au inano composite material: get the Fe that 0.1g step 2 is obtained 3o 4-PANI composite material of core-shell structure joins the obtained nm of gold seed solution of 150mL step 3, mechanical agitation ultrasonic 10min, mechanical agitation 3h under room temperature, with magnet by product separation, product distilled water and absolute ethyl alcohol is respectively cleaned 3 times, prepares Fe 3o 4-PANI-Au inano composite material;
Step 5: the golden salting liquid of configuration reduction: add 60mg sodium carbonate in 200ml deionized water, after mechanical agitation 15min, add the chlorauric acid solution of 3ml 1wt%, lucifuge magnetic agitation 12h, obtain reducing golden salting liquid, for subsequent use;
Step 6: the Fe obtained by step 4 3o 4-PANI-Au inano composite material joins the obtained reduction gold salting liquid of 40mL step 5, stirs, then adds 0.1mL formaldehyde, reaction 10min;
Step 7: continue to add 40mL and reduce golden salting liquid, add 0.1mL formaldehyde again after stirring, reaction 10min;
Step 8: step 7 is repeated 1 time, by distilled water and ethanol repeatedly washed product, prepares Fe 3o 4-PANI-Au iInano composite material.
Fig. 1 is the Fe that in embodiment 1, step one prepares 3o 4nano particle, this Fe 3o 4nano particle globulate, particle diameter is 200 ~ 300nm; Fig. 2 is the nm of gold seed that in embodiment 1, step 3 prepares, and shape is that class is spherical, and particle diameter is about 5nm; Fig. 3 is the Fe that in embodiment 1, step 2 prepares 3o 4-PANI composite material of core-shell structure, significantly can find out the nucleocapsid structure of composite, and the complete continuous print of polyaniline wraps Fe 3o 4nano particle; Fig. 4 is the Fe that in embodiment 1 prepared by step 2 3o 4the partial enlarged drawing of-PANI, as can be seen from the figure the polyaniline of surface parcel is about 10nm; Fig. 6 is the Fe that embodiment 1 step 4 prepares 3o 4-PANI-Au inano composite material, significantly can see polyaniline adsorption one deck nm of gold seed; The Fe that Fig. 7 embodiment 1 finally prepares 3o 4-PANI-Au iInano composite material, can find out that there is reduction reaction in the golden salting liquid of reduction after, gold seeds is grown up, and adjacent gold seeds contact forms the shell of gold gradually.
Embodiment 2
Compared with embodiment 1, difference is only that step 2 prepares Fe 3o 4-PANI composite material of core-shell structure, that is: take the Fe that step one is obtained 3o 4nano particle 0.2g is dissolved in 200mL water, stirs, and adds 0.2gPVP, stirs and ultrasonic 30 minutes, mixed solution is at room temperature stirred 3 hours.Then add 0.2g aniline monomer and 1g citric acid successively, stir and ultrasonic 15min.Stir under condition of ice bath and within 10 minutes, add 0.5g ammonium peroxydisulfate (APS) again, stir 9 hours under the condition of ice bath, product distilled water and absolute ethyl alcohol are cleaned repeatedly.
Due to, embodiment 2, compared with embodiment 1, adds the amount of aniline monomer, makes the surface coated polyaniline of tri-iron tetroxide thickening, and this point can comparison diagram 4 and Fig. 5 Fe 3o 4the partial enlarged drawing of-PANI draws, can significantly find out Fe in embodiment 2 by figure 3o 4the polyaniline of-PANI composite material of core-shell structure thickens than embodiment 1.Namely Fe can be regulated and controled by the mass ratio of regulation and control aniline monomer and tri-iron tetroxide 3o 4-PANI composite material of core-shell structure shell thickness.
Embodiment 3
Compared with embodiment 1, difference is only in step 8, repeats step 73 times.
Because embodiment 3 is compared with embodiment 1, add the number of repetition of step 7, make repeatedly reduction reaction to occur, the Fe therefore finally obtained 3o 4-PANI-Au iIthe load capacity of the gold on nano composite material surface increases, and the shell of gold becomes fine and close.The comparison diagram of Fig. 8 with Fig. 7 conforms to result.
Fig. 9 is the UV-vis figure of the catalysis p-nitrophenol that the embodiment of the present invention 3 obtains.As seen from the figure, the composite that prepared by the present invention has sensitive feature fast on catalysis p-nitrophenol.
Figure 10 is the Fe that the embodiment of the present invention 3 obtains 3o 4-PANI-Au iI(black) and Fe 3o 4-PANI-Au ithe recycling number of times figure of (twill).This figure illustrates, trapping gold shell considerably increases the recycling ability of catalyst.
Although invention has been described by reference to the accompanying drawings above; but the present invention is not limited to above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is only schematic; instead of it is restrictive; those of ordinary skill in the art is under enlightenment of the present invention; when not departing from present inventive concept, can also make a lot of distortion, these all belong within protection of the present invention.

Claims (2)

1. a preparation method for tri-iron tetroxide-polyaniline-gold nano composite, comprises the following steps:
Step one: obtain the Fe that particle diameter is 200 ~ 350nm with solvent-thermal method 3o 4nano particle;
Step 2: take the Fe that step one is obtained 3o 4nano particle is soluble in water, Fe 3o 4quality-the volume ratio of nano particle and water is 1 ~ 2mg/mL, stirs, and is that 1 ~ 2mg/mL adds PVP according to the quality-volume ratio of PVP and water, stirs and ultrasonic 30 minutes obtained mixed solution A, mixed solution A is at room temperature stirred 3 hours; Then aniline monomer and citric acid is added successively, aniline, citric acid, Fe 3o 4the mass ratio of nano particle is 1 ~ 4:10:2, stirs and ultrasonic 15min; 10 minutes are stirred again according to APS and Fe under condition of ice bath 3o 4the mass ratio of nano particle is that 5:2 adds APS, stirs 7 ~ 9 hours, product distilled water and absolute ethyl alcohol are repeatedly cleaned under the condition of ice bath; Thus at Fe 3o 4nano grain surface wraps up one deck PANI, prepares Fe 3o 4-PANI composite material of core-shell structure;
Step 3: according to the HAuCl of volume ratio 1:100 by 1wt% 4the aqueous solution is soluble in water, magnetic agitation 10min; Be the trisodium citrate that 1:100 adds 1wt% according to the volume ratio of trisodium citrate and water, then add the HAuCl doubling 1wt% simultaneously 4the 1wt% trisodium citrate of aqueous solution volume and 0.08wt% sodium borohydride; Magnetic agitation reaction 30 ~ 60min, prepares nm of gold seed solution;
Step 4: be 0.5 ~ 2mg/mL according to quality-volume ratio, the Fe obtained by step 2 3o 4-PANI composite material of core-shell structure joins the obtained nm of gold seed solution of step 3, mechanical agitation ultrasonic 10min, mechanical agitation 3 ~ 5h under room temperature, with magnet by product separation, product distilled water and absolute ethyl alcohol is respectively cleaned 3 times, prepares Fe 3o 4-PANI-Au inano composite material;
Step 5: be that 0.3mg/ml adds sodium carbonate in distilled water according to quality-volume ratio, after mechanical agitation 15min, add 1wt% aqueous solution of chloraurate, the volume ratio of 1wt% aqueous solution of chloraurate and distilled water is 3:200, mechanical agitation 9 ~ 12h under lucifuge condition, obtain reducing golden salting liquid, for subsequent use;
Step 6: be 2 ~ 5mg/mL according to quality-volume ratio, the Fe obtained by step 4 3o 4-PANI-Au inano composite material joins the obtained reduction gold salting liquid of step 5, stirs, then is that 400:1 adds formaldehyde according to the volume ratio of the golden salting liquid of reduction and formaldehyde, reaction 10min;
Step 7: be that 2 ~ 3mg/mL continues to add the golden salting liquid of reduction according to quality-volume ratio, stirs, then is that 400:1 adds formaldehyde according to the volume ratio of the golden salting liquid of reduction and formaldehyde, reaction 10min;
Step 8: step 7 is repeated N time, wherein N is 1 ~ 5 time; By distilled water and ethanol repeatedly washed product, prepare Fe 3o 4-PANI-Au iInano composite material.
2. an application for tri-iron tetroxide-polyaniline-gold nano composite, is characterized in that, by the Fe prepared according to the preparation method of tri-iron tetroxide-polyaniline-gold nano composite described in claim 1 3o 4-PANI-Au iIthe catalytic applications of nano composite material p-nitrophenol in catalysis pollutant.
CN201510374440.8A 2015-06-30 2015-06-30 Preparation method and applications of ferriferrous oxide-polyaniline-gold nano composite material Pending CN104971778A (en)

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CN111215152A (en) * 2020-03-13 2020-06-02 烟台大学 Preparation of magnetic core-shell conductive polymer supported nano gold catalyst and application of magnetic core-shell conductive polymer supported nano gold catalyst in p-nitrophenol hydrogenation
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CN106449139A (en) * 2016-09-21 2017-02-22 浙江大学 Co3O4@PEDOT porous nanorod material with core-shell structure and preparation method of Co3O4@PEDOT porous nanorod material
CN107030295A (en) * 2017-03-24 2017-08-11 同济大学 A kind of preparation method of magnetic/gold nanocomposite particle
CN109534481A (en) * 2018-12-17 2019-03-29 安徽环境科技股份有限公司 A kind of processing method of phenol wastewater
CN111855635A (en) * 2019-04-26 2020-10-30 天津大学 MXenes-gold nano composite material, preparation method thereof and application of MXenes-gold nano composite material as Raman substrate
CN111855635B (en) * 2019-04-26 2023-03-21 天津大学 MXenes-gold nano composite material, preparation method thereof and application of MXenes-gold nano composite material as Raman substrate
CN110579521B (en) * 2019-07-31 2022-08-30 安徽环境科技集团股份有限公司 Modified electrode for nitrobenzene detection and preparation method and application thereof
CN110579521A (en) * 2019-07-31 2019-12-17 安徽环境科技集团股份有限公司 Modified electrode for nitrobenzene detection and preparation method and application thereof
CN110898854A (en) * 2019-11-08 2020-03-24 同济大学 Magnetic nano hollow material loaded with gold particles and preparation method and application thereof
CN111215152A (en) * 2020-03-13 2020-06-02 烟台大学 Preparation of magnetic core-shell conductive polymer supported nano gold catalyst and application of magnetic core-shell conductive polymer supported nano gold catalyst in p-nitrophenol hydrogenation
CN111215152B (en) * 2020-03-13 2022-11-18 烟台大学 Preparation of magnetic core-shell conductive polymer supported nano gold catalyst and application of magnetic core-shell conductive polymer supported nano gold catalyst in p-nitrophenol hydrogenation
CN112326749B (en) * 2020-10-26 2022-10-11 中国科学院重庆绿色智能技术研究院 Preparation method of novel coronavirus kit for electrochemical immunodetection, product and use method of novel coronavirus kit
CN112326749A (en) * 2020-10-26 2021-02-05 中国科学院重庆绿色智能技术研究院 Preparation method of novel coronavirus electrochemical immunoassay kit, product and use method of novel coronavirus electrochemical immunoassay kit
CN112557383A (en) * 2020-12-10 2021-03-26 贵州大学 Based on MnO2Copper ion colorimetric detection method of complex enzyme analogue
CN112557383B (en) * 2020-12-10 2024-01-26 贵州大学 MnO-based 2 Copper ion colorimetric detection method of complex enzyme simulant

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