CN105148995B - Application of PAMAM carboxylated graphene Co nano-composite material in 4-nitroaniline degradation and catalysis - Google Patents
Application of PAMAM carboxylated graphene Co nano-composite material in 4-nitroaniline degradation and catalysis Download PDFInfo
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- CN105148995B CN105148995B CN201510607953.9A CN201510607953A CN105148995B CN 105148995 B CN105148995 B CN 105148995B CN 201510607953 A CN201510607953 A CN 201510607953A CN 105148995 B CN105148995 B CN 105148995B
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Abstract
The invention discloses application of a PAMAM carboxylated graphene Co nano-composite material in 4-nitroaniline degradation and catalysis. A preparation method comprises the steps of 1 synthesizing PAMAM/GO-COOH and 2 synthesizing a PAMAM/GO-COOH/Co nano-composite material. A chemical crosslinking method and polyamidoamine dendrimer modified carboxylated graphene are adopted to successfully obtain the PAMAM/carboxylated graphene/Co nano-composite material with PAMAM carboxylated graphene as a template and sodium borohydride as a reducing agent. The PAMAM/carboxylated graphene/Co nano-composite material is a catalytic carrier material having unique performance and has high catalytic activity on the 4-nitroaniline water solution degradation effect only in the presence of air and water under the normal-temperature condition, and a new way is provided for degradation of environmental pollutants in our actual life.
Description
Technical field
The present invention relates to a kind of carboxylated Graphene Co nano composite materials of PAMAM are in the degraded catalysis of 4- nitroanilines
Using.
Background technology
Graphene (Graphene) has caused all circles' research worker as a kind of material since being found from 2004
Extensive concern.Graphene due to its two-dimentional monoatomic layer crystal structure, big specific surface area, capacitor, sensor, catalysis and
The fields such as nano composite material show excellent application prospect.Graphene/dendrimer composite is with the knot of its uniqueness
Structure and performance advantage become one new study hotspot of field of nanometer material technology.
Polyamidoamine Dendrimers (PAMAM) are class three-dimensional, the macromolecule of height cladodification, with controllable phase
To molecular mass, there is cavity, the symmetry of height in substantial amounts of surface functional group, intramolecular, and the end group of densification can
So that with reference to more active substances, these construction featuress make it have the property of uniqueness.Use Polyamidoamine Dendrimers function
Changing the Graphene of modification, to be not only due to the sterically hindered reunion for reducing interlayer that dendrimer produces between graphene layer existing
As while its dispersibility and dissolubility are also improved, it is often more important that due to dendrimer, its controllable prepares little chi
It is very little, the finely dispersed metal nanoparticle and algebraically using dendrimer adjusts the size of its internal cavities so as to control
Contact of the catalyst with reactant, can be preparation as the good catalyst carrier of organic functional molecular and inorganic nano-particle
Multifunctional high-performance material has constructed a wide platform.
As dye industry develops, main organic poison is the aromatic compound of nitro or amido functional group in waste water
Thing, these high temperature resistant Organic substances are difficult to be decomposed using traditional chemical precipitation method.Therefore, the PAMAM carboxyl graphites of preparation
If alkene Co nano composite materials can have remarkable effect to the degraded catalysis of 4- nitroanilines, with important practical value,
Also there is important Eco-environmental Significance.
The content of the invention
To promote scientific and technological progress, the present inventor to invent a kind of carboxylated Graphene Co nanometers of PAMAM through lot of experiments
Composite and preparation method thereof, and probed into the carboxylated Graphene Co nano composite materials of PAMAM（PAMAM/GO-COOH/
Co）Degraded catalytic action to 4- nitroanilines.
The preparation of the carboxylated Graphene Co nano composite materials of PAMAM includes following step：
（1）The synthesis of PAMAM/GO-COOH：The g of carboxylated Graphene 0.42 is weighed, 40 mL deionized waters, ultrasound is added
4 g EDC and 4.2 g NHS, the h of magnetic agitation 4 at 40 DEG C are added after dispersion, product is filtered, is centrifuged, deionized water cleaning
Afterwards the ultrasonic disperse in 40 mL deionized waters, adds 10 mL PAMAM (g/mL of 4.0 G concentration 0.1) aqueous solution, at 35 DEG C
The lower h of stirring reaction 12, product is vacuum dried Jing after centrifugation, deionized water cleaning and obtains final product；
（2）The synthesis of PAMAM/GO-COOH/Co nano composite materials：The mg of PAMAM/GO-COOH/Co 100 are weighed, plus
Enter 20 mL deionized waters, ultrasonic disperse adds 10 mL CoCl2Solution (0.5 mol/L), stirs 1 h, is subsequently adding 0.5 g
NaBH4, the h of magnetic agitation 4 at 50 DEG C, product is collected in beaker Jing after centrifugation, deionized water cleaning, then ultrasonic again to divide
Dissipate, remove unnecessary Co2+, end product Jing centrifugations, deionized water cleaning are vacuum dried after filtration and obtain final product.
Degraded catalysis of the carboxylated Graphene Co nano composite materials of PAMAM to 4- nitroanilines is probed into：Obtain 10 mg's
PAMAM/GO-COOH/Co ultrasonic disperses are in 30 mL 5.8 × 10-5In the aqueous solution of mol/L 4- nitroanilines, mixture is in sky
Room temperature (25 DEG C) is stirred in gas, is determined with ultraviolet-visual spectrometer at set intervals.The ultraviolet absorption peak of 4- nitroanilines is
378 nm, by absworption peak peak intensity degraded catalytic capability of the composite to 4- nitroanilines is illustrated.
Compared with prior art, the beneficial effects of the present invention is：
Polyamidoamine Dendrimers (PAMAM 4.0G) are modified carboxyl graphite by the present invention using chemical crosslink technique
Alkene, successfully obtains the carboxylated Graphenes of PAMAM for template, using sodium borohydride as the carboxylated Graphenes of the PAMAM/ of reducing agent/
Co nano composite materials.Jing is determined, and Co nano-particles size is uniform in size to be dispersed in the carboxylated graphenic surfaces of PAMAM/.
The carboxylated Graphenes of PAMAM//Co nano composite materials prepared by the present invention are a kind of catalysis of unique energy
Carrier material, under normal temperature condition, as long as the aqueous solution with the presence of air and water PAMAM/GO-COOH/Co to 4- nitroanilines
Degradation shows high catalysis activity, and this degraded in our real lifes to environmental pollutants provides a kind of new road
Footpath.
Description of the drawings
Fig. 1 be PAMAM/GO-COOH/Co in room temperature room to the aqueous solution Degradation figure of 4- nitroanilines.
Specific embodiment
In conjunction with accompanying drawing 1, to the carboxylated Graphene Co nano composite materials of PAMAM in the degraded catalysis of 4- nitroanilines
Using being described in detail.
The preparation of the carboxylated Graphene Co nano composite materials of PAMAM includes following step：
（1）The synthesis of PAMAM/GO-COOH：The g of carboxylated Graphene 0.42 is weighed, 40 mL deionized waters, ultrasound is added
4 g EDC and 4.2 g NHS, the h of magnetic agitation 4 at 40 DEG C are added after dispersion, product is filtered, is centrifuged, deionized water cleaning
Afterwards the ultrasonic disperse in 40 mL deionized waters, adds 10 mL PAMAM (g/mL of 4.0 G concentration 0.1) aqueous solution, at 35 DEG C
The lower h of stirring reaction 12, product is vacuum dried Jing after centrifugation, deionized water cleaning and obtains final product；
（2）The synthesis of PAMAM/GO-COOH/Co nano composite materials：The mg of PAMAM/GO-COOH/Co 100 are weighed, plus
Enter 20 mL deionized waters, ultrasonic disperse adds 10 mL CoCl2Solution (0.5 mol/L), stirs 1 h, is subsequently adding 0.5 g
NaBH4, the h of magnetic agitation 4 at 50 DEG C, product is collected in beaker Jing after centrifugation, deionized water cleaning, then ultrasonic again to divide
Dissipate, remove unnecessary Co2+, end product Jing centrifugations, deionized water cleaning are vacuum dried after filtration and obtain final product.
Degraded catalysis of the carboxylated Graphene Co nano composite materials of PAMAM to 4- nitroanilines is probed into：Obtain 10 mg's
PAMAM/GO-COOH/Co ultrasonic disperses are in 30 mL 5.8 × 10-5In the aqueous solution of mol/L 4- nitroanilines, mixture is in sky
Room temperature (25 DEG C) is stirred in gas, is determined with ultraviolet-visual spectrometer at set intervals.The ultraviolet absorption peak of 4- nitroanilines is
378 nm, by absworption peak peak intensity degraded catalytic capability of the composite to 4- nitroanilines is illustrated.
As shown in figure 1, under normal temperature condition, as long as with the presence of air and water PAMAM/GO-COOH/Co to 4- nitroanilines
Aqueous solution Degradation show high catalysis activity.After 8 h, PAMAM/GO-COOH/Co is to 4- nitroanilines
Aqueous solution catalytic degradation peak value is almost 0, illustrates aqueous solution catalytic degradation tables of the PAMAM/GO-COOH/Co to 4- nitroanilines
Reveal high catalytic performance.This is to provide more steric restrictions by template fabricated in situ cobalt nanometer particle of PAMAM/GO-COOH
The polymerization of cobalt nanometer particle, and pollutant are adsorbed onto surface and carry out catalytic degradation by the huge specific surface energies of PAMAM/GO-COOH.
It is more that PAMAM/GO-COOH/Co catalytic degradation reactions can be carried out in room temperature room, not any increasing
Oxidizer etc. is (such as H2O2)。
Above-mentioned simply presently preferred embodiments of the present invention, not makees any pro forma restriction to the present invention.It is any to be familiar with sheet
The technical staff in field, in the case of without departing from technical solution of the present invention scope, all using the technology contents of the disclosure above
Many possible variations and modification, or the Equivalent embodiments for being revised as equivalent variations are made to technical solution of the present invention.Therefore, it is all
It is the content without departing from technical solution of the present invention, any simply repaiies to made for any of the above embodiments according to the technology of the present invention essence
Change, equivalent variations and modification, all should fall in the range of technical solution of the present invention protection.
Claims (2)
1. the preparation method of the carboxylated Graphene Co nano composite materials of a kind of PAMAM, it is characterised in that including following step
Suddenly：
（1）The synthesis of PAMAM/GO-COOH：The g of carboxylated Graphene 0.42 is weighed, 40 mL deionized waters, ultrasonic disperse is added
After add 4 g EDC and 4.2 g NHS, the h of magnetic agitation 4 at 40 DEG C, product is filtered, centrifugation, after deionized water cleaning
Ultrasonic disperse in 40 mL deionized waters, the 4.0G PAMAM aqueous solutions for adding 10 mL concentration to be 0.1 g/mL, stirs at 35 DEG C
12 h of reaction are mixed, product is vacuum dried Jing after centrifugation, deionized water cleaning and obtains final product；
（2）The synthesis of PAMAM/GO-COOH/Co nano composite materials：The mg of PAMAM/GO-COOH 100 are weighed, 20 mL are added
Deionized water, ultrasonic disperse adds the CoCl that 10 mL concentration are 0.5 mol/L2Solution, stirs 1 h, is subsequently adding 0.5 g
NaBH4, the h of magnetic agitation 4 at 50 DEG C, product is collected in beaker Jing after centrifugation, deionized water cleaning, then ultrasonic again to divide
Dissipate, remove unnecessary Co2+, end product Jing centrifugations, deionized water cleaning are vacuum dried after filtration and obtain final product.
2. the carboxylated Graphene Co nano composite materials of PAMAM that according to claim 1 prepared by method are in 4- nitroanilines
Application in degraded catalysis, it is characterised in that：Degraded catalytic process has water and air to participate in.
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| CN108014132A (en) * | 2016-11-03 | 2018-05-11 | 湖南师范大学 | With selective cytotoxicity graphene complex and preparation method thereof |
| CN107501500B (en) * | 2017-08-16 | 2020-05-19 | 陕西科技大学 | Polyamide-amine functionalized graphene/hyperbranched waterborne polyurethane and preparation method thereof |
| CN110194451A (en) * | 2019-05-15 | 2019-09-03 | 华东理工大学 | There is grapheme material and its preparation method and the application of the macromolecule covalent modification of donor and acceptor groups simultaneously |
| CN110882724B (en) * | 2019-12-09 | 2022-11-08 | 万华化学集团股份有限公司 | Platinum-supported catalyst, preparation method thereof and application thereof in cyclododecanol synthesis |
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| CN101773855A (en) * | 2010-01-19 | 2010-07-14 | 华南理工大学 | Oxygen reduction catalyst prepared from grapheme modified by macrocyclic compound, and preparation method thereof |
| CN104307515A (en) * | 2014-09-11 | 2015-01-28 | 闽南师范大学 | Au-Pd/graphene catalyst and preparation method and application thereof |
| CN104383943A (en) * | 2014-09-16 | 2015-03-04 | 安徽大学 | Preparation method for catalyst efficiently catalyzing hydrogenation reduction of 4-nitrophenol |
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| Reduced graphene oxide/PAMAM–silver nanoparticles nanocomposite modified electrode for direct electrochemistry of glucose oxidase and glucose sensing;Zhimin Luo et al.;《Biosensors and Bioelectronics》;20120420;第36卷(第1期);摘要、第180页右栏第3段 * |
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