CN109827954A - A kind of decorated by nano-gold poly-dopamine nanotube, preparation method and application - Google Patents
A kind of decorated by nano-gold poly-dopamine nanotube, preparation method and application Download PDFInfo
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Abstract
The invention discloses poly-dopamine nanotube, preparation method and the applications of a kind of decorated by nano-gold, preparation process is as follows: (1) using zinc oxide nano rod as template, zinc oxide nano rod Tris-HCl buffer solution, then Dopamine hydrochloride room temperature anti-0.5 ~ for 24 hours is added, precipitating is dispersed in water to obtain poly-dopamine zinc oxide nano rod aqueous solution after centrifuge washing, the mass ratio of zinc oxide nano rod and Dopamine hydrochloride is 1:1,55 ~ 65 DEG C of ammonium chloride are added in backward solution to react 50 ~ 70 minutes, obtain poly-dopamine nanotube after centrifugation, washing；(2) chlorauric acid solution is added in the solution of poly-dopamine nanotube, room temperature reaction 20 ~ after forty minutes, centrifuge washing obtains decorated by nano-gold poly-dopamine nanotube.Material prepared by the present invention has absorption and reducing power well to potassium bichromate, and the material is environmentally protective, there is good cyclicity, and reduction efficiency is high, will not pollute.
Description
Technical field
The invention belongs to environment functional material and heavy metal process fields, specifically disclose a kind of poly- DOPA of decorated by nano-gold
Amine nanotube, preparation method and application, the nanocomposite are having good absorption and reduction to Cr (VI).
Background technique
Heavy metal chromium and compound be in industrial development it is essential, be widely used in plating, dye, battery
The industries such as manufacture and mining.However, the heavy metal chromium in industrial wastewater would seriously pollute the environment, and human health can be caused sternly
It damages again.In numerous heavy metal pollution, due to its virulent property and generality, chromium becomes a kind of typical pollutant.Chromium
Ion is in the natural environment there are mainly two types of form [trivalent chromium Cr(III) and Cr VI Cr(VI)], and Cr(VI) toxicity want
Than Cr(III) it is hundreds times high, and be easily absorbed by the body and give rise to diseases.It is limited in the discharge standard of China, industrial chrome
0.1 mg·L-1Below.Therefore, the Cr(VI in sewage) is reduced to level of security is problem in the urgent need to address at present, is drawn
The extensive concern of domestic and foreign scholars is played.Nowadays, various technologies, including ion exchange, reverse osmosis, absorption, flocculation and film filtering
Etc. the Cr VI having been used in processing sewage.Wherein, absorption method is since with high efficiency, simplification, low cost has been obtained
It is widely applied.But currently used adsorbent, such as active carbon, resin and chitosan etc., active site is few, adsorptive selectivity
It is weak, and can only be by Cr(VI) Cong Yixiang is transferred to another phase, it is not removed, it is still necessary to subsequent processing.It therefore, if can be
Adsorb Cr(VI) while, highly toxic Cr(VI) is reduced to the Cr(III of hypotoxicity), so that it may effectively reduce pollution and
Treatment cost.Therefore, Cr(VI can be adsorbed and restore simultaneously by studying one kind) material be of great significance.
Poly-dopamine (PDA) be it is a kind of by mussel secrete viscous protein structure inspire obtained from polymer, its conduct
Multi-purpose function material, in biology, the relevant field such as environment and the energy causes people's extensive concern.PDA contains largely
Phenols, quinones and amidine functional group, it can be with Cr(VI) ion is combined strongly, while in-situ deposition nanogold can be effectively catalyzed
Reduction removes Cr(VI).
Summary of the invention
The purpose of the present invention is to provide a kind of decorated by nano-gold poly-dopamine nanotube, preparation method and applications.Pass through mould
Plate method is prepared for poly-dopamine nanotube, and has obtained the poly-dopamine of decorated by nano-gold by the in-situ deposition of gold nano grain
Bionical composite nano materials are managed, poly-dopamine provides the immobilized active point of gold nanoparticle, makes the dispersibility of nanoparticle
Improve.Meanwhile the big specific surface area of poly-dopamine pipe is also beneficial to the active point that test substance is diffused into interface.
The present invention has hollow tubular structures by the nano composite structure that transmission electron microscope demonstrates, and nanogold exists
Uniform deposition on pipe has good dispersibility and homogeneity.Pass through the crystal structure of XRD characterization composite material.Lead to simultaneously
Cross uv-visible absorption spectra and demonstrate composite material to Cr(VI) absorption and reduction.
Based on above-mentioned purpose, the technical solution adopted by the present invention is as follows:
A kind of preparation method of decorated by nano-gold poly-dopamine nanotube, includes the following steps:
(1) preparation of poly-dopamine nanotube
Using zinc oxide nano rod as template, then hydrochloric acid DOPA is added in zinc oxide nano rod Tris-HCl buffer solution
Amine room temperature reaction 0.5 ~ for 24 hours, precipitating is dispersed in water to obtain poly-dopamine zinc oxide nano rod aqueous solution after centrifuge washing, then
55 ~ 65 DEG C of ammonium chloride are added into solution to react 50 ~ 70 minutes, obtains poly-dopamine nanotube after centrifugation, washing, is distributed to
Poly-dopamine nanotube solution is obtained in ionized water, wherein the mass ratio of zinc oxide nano rod, Dopamine hydrochloride and ammonium chloride is
(2 ~ 1): (1 ~ 2): 320；
(2) preparation of decorated by nano-gold poly-dopamine nanotube
Chlorauric acid solution is added in poly-dopamine nanotube aqueous solution, the mass ratio of gold chloride and poly-dopamine nanotube is
(0.206 ~ 0.5): 1, room temperature reaction 20 ~ after forty minutes, centrifuge washing obtains decorated by nano-gold poly-dopamine nanotube.
Further, the dosage of zinc oxide nano rod and Dopamine hydrochloride is 10mg, Tris-HCl in the step (1)
Buffer concentration is 10mM, pH 8.5, dosage 20mL, and the concentration of ammonium chloride is 2mol/L, dosage 30mL.
Further, the concentration of gold chloride is 0.01mol/L in the step (2), and dosage is 100 ~ 250 μ L, poly- DOPA
The concentration of amine nanotube aqueous solution is 0.2mg/mL, dosage 10mL.
Further, the preparation process of the zinc oxide nano rod is as follows: by zinc nitrate and sodium hydroxide be dissolved into from
In sub- water, ethyl alcohol is then sequentially added, mixed solution is ultrasonically formed uniform solution by ethylenediamine, and it is anti-that solution is poured into high pressure
It answers in kettle, 170 ~ 190 DEG C are reacted 18 ~ 25 hours, and washing obtains template zinc oxide nano rod after dry, wherein zinc nitrate, hydrogen
The volume ratio of the molar ratio 3:5:20 of sodium oxide molybdena and ethylenediamine, deionized water and ethyl alcohol is 6:5, and the zinc nitrate is in deionized water
In concentration be 0.1 ~ 1mol/L.
Further, the volume of the deionized water is 30mL, the concentration of zinc nitrate and sodium hydroxide in deionized water
Respectively 0.5M, 10M.
Decorated by nano-gold poly-dopamine nanotube made from above-mentioned preparation method.
Above-mentioned decorated by nano-gold poly-dopamine nanotube is adsorbing and is restoring the application in 6 valence chromium ions.
The poly-dopamine pipe that the present invention is prepared by template, while realizing that in-situ deposition nanogold obtains composite material,
The material has apparent absorption and reduction to Cr (VI), avoids secondary pollution, material has good cyclicity, for containing chromium
The processing of waste water provides the effective method of green.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture for the decorated by nano-gold poly-dopamine nanotube that embodiment 3 obtains；
Fig. 2 is the XRD diagram for the decorated by nano-gold poly-dopamine nanotube that embodiment 3 obtains；What JCPDS04-0784 was represented is vertical
The standard card product of square phase Au；
Fig. 3 is that the obtained decorated by nano-gold poly-dopamine nanotube of embodiment 3 restores Cr(VI) time change ultraviolet-visible
Spectrogram；
Fig. 4 be implement 1 ~ 3 preparation material reduction Cr(VI) residual concentration with the reaction time variation diagram, wherein C0Table
Show that the initial concentration of potassium bichromate, C indicate the concentration of potassium bichromate.
Specific embodiment
Embodiment of the present invention is described in detail below, but should not be used as the limit to technical solution of the present invention
System.
Embodiment 1
A kind of preparation method of decorated by nano-gold poly-dopamine nanotube, includes the following steps:
(1) preparation of template
By zinc nitrate ((Zn (NO3)2) and sodium hydroxide (NaOH) be dissolved into 30 mL deionized waters so that deionization
Zn (NO in water3)2Concentration is 0.50M, NaOH concentration 10.0M, then sequentially adds 25 mL ethyl alcohol (C2H5OH)、5 mL
Ethylenediamine (C2H4(NH2)2), mixed solution ultrasound is formed into uniform solution in 30 minutes, solution is poured into autoclave
In, 180 DEG C are reacted 20 hours, and obtaining zinc oxide nano rod (being denoted as ZnO NRs) after washing, drying can be used as template.
(2) preparation of poly-dopamine nanotube
20 mL Tris-HCl buffer (10 mM, pH of (ZnO NRs) 10 mg of zinc oxide nano rod made from step (1)
8.5) it dissolves, 10 mg Dopamine hydrochlorides is then added and react at room temperature 4 hours.Precipitating is dispersed in 1mL water after centrifuge washing
In obtain poly-dopamine zinc oxide nano rod (ZnO@PDA NRs) aqueous solution.Then 30mL ammonium chloride solution is added into solution
Liquid (NH4Cl, 2 M), 60 DEG C are reacted 60 minutes, are distributed to after centrifuge washing and are obtained poly-dopamine in 100mL deionized water and receive
Mitron solution (concentration is about 0.2mg/mL).
(3) preparation of decorated by nano-gold poly-dopamine nanotube
The chlorauric acid solution of 100 μ L 0.01mol/L is added in the solution of 10mL poly-dopamine nanotube (0.2mg/mL),
Centrifugation, washing after room temperature reaction 30 minutes, precipitating, which is distributed in 10mL water, obtains decorated by nano-gold poly-dopamine pipe solution (concentration
About 0.25mg/mL is denoted as Au-PDA-1).
(4) absorption and reduction of Cr (VI)
1mL sample, which is added to 10mL concentration that three groups prepare, is in 106 mg/mL potassium bichromate solutions, purple at regular intervals
The reducing degree of outer detection Cr (VI), concrete outcome are detailed in Fig. 4.
Embodiment 2
A kind of preparation method of decorated by nano-gold poly-dopamine nanotube, includes the following steps:
(1) preparation of template
By zinc nitrate ((Zn (NO3)2) and sodium hydroxide (NaOH) be dissolved into 30 mL deionized waters so that deionization
Zn (NO in water3)2Concentration is 0.50M, NaOH concentration 10.0M, then sequentially adds 25 mL ethyl alcohol (C2H5OH), 5 mL
Ethylenediamine (C2H4(NH2)2), mixed solution ultrasound is formed into uniform solution in 30 minutes, solution is poured into autoclave
In, 180 DEG C are reacted 20 hours.Washing, obtaining zinc oxide nano rod (ZnO NRs) after dry can be used as template.
(2) preparation of poly-dopamine nanotube
20 mL Tris-HCl Tris-HCl buffer (10 mM, pH of zinc oxide nano rod (ZnO NRs, 10 mg)
8.5) it dissolves, 10 mg Dopamine hydrochlorides is then added and react at room temperature 4 hours.Precipitating is dispersed in 1mL water after centrifuge washing
In obtain poly-dopamine zinc oxide nano rod (ZnO@PDA NRs) aqueous solution.Then 30mL ammonium chloride solution is added in the solution
Liquid (NH4Cl, 2 M), 60 DEG C are reacted 60 minutes, are distributed to after centrifuge washing and are obtained poly-dopamine in 100mL deionized water and receive
Mitron solution (concentration is about 0.2mg/mL).
(3) preparation of decorated by nano-gold poly-dopamine nanotube
The chlorauric acid solution of 250 μ L 0.01mol/L is added in the solution of 10mL poly-dopamine nanotube (0.2mg/mL),
After room temperature reaction 30 minutes, centrifuge washing, precipitating, which is distributed in 10mL water, obtains decorated by nano-gold poly-dopamine pipe solution (concentration
About 0.25mg/mL is denoted as Au-PDA-2).
(4) absorption and reduction of Cr (VI)
1mL sample, which is added to 10mL concentration that three groups prepare, is in 106 mg/mL potassium bichromate solutions, purple at regular intervals
The reducing degree of outer detection Cr (VI), concrete outcome are detailed in Fig. 4.
Embodiment 3
A kind of preparation method of decorated by nano-gold poly-dopamine nanotube, includes the following steps:
(1) preparation of template
By zinc nitrate ((Zn (NO3)2) and sodium hydroxide (NaOH) be dissolved into 30 mL deionized waters so that deionization
Zn (NO in water3)2Concentration is 0.50M, NaOH concentration 10.0M, then sequentially adds 25 mL ethyl alcohol (C2H5OH), 5 mL
Ethylenediamine (C2H4(NH2)2), mixed solution ultrasound is formed into uniform solution in 30 minutes, solution is poured into autoclave
In, 180 DEG C are reacted 20 hours.Washing, obtaining zinc oxide nano rod (ZnO NRs) after dry can be used as template.
(2) preparation of poly-dopamine nanotube
20 mL Tris-HCl Tris-HCl buffers (10 mM, pH 8.5) of zinc oxide nano rod (ZnO NRs, 10 mg)
Then dissolution is added 10 mg Dopamine hydrochlorides and reacts at room temperature 4 hours.Precipitating, which is dispersed in 1mL water, after centrifuge washing obtains
Poly-dopamine zinc oxide nano rod (ZnO@PDA NRs) aqueous solution.Then 30mL aqueous ammonium chloride solution is added in the solution
(NH4Cl, 2 M), 60 DEG C are reacted 60 minutes, are distributed in 100mL deionized water after centrifuge washing and are obtained poly-dopamine nanometer
Pipe solution (concentration is about 0.2mg/mL).
(3) preparation of decorated by nano-gold poly-dopamine nanotube
The chlorauric acid solution of 200 μ L 0.01mol/L is added in the solution of 10mL poly-dopamine nanotube (0.2mg/mL),
Centrifuge washing after room temperature reaction 30 minutes carries out SEM spectrum to precipitating and XRD spectrum detects, is detailed in Fig. 1 and Fig. 2, can by Fig. 1
Know, obtained poly-dopamine pipe has apparent hollow structure, and nanogold is uniformly deposited on poly-dopamine pipe；As shown in Figure 2,
The nanogold deposited on poly-dopamine pipe is corresponding with the standard card JCPDS04-0784 of gold of cubic, illustrates deposition
Nanogold has good crystal form.
Precipitating, which is distributed in 10mL water, to be obtained decorated by nano-gold poly-dopamine pipe solution (concentration is about 0.25mg/mL, is denoted as
Au-PDA-3)。
(4) absorption and reduction of Cr (VI)
It is 106 mg/mL that 1mL0.25mg/mL decorated by nano-gold poly-dopamine pipe solution, which is added to the 10mL concentration that three groups prepare,
In potassium bichromate solution, the reducing degree of ultraviolet detection Cr (VI), concrete outcome are detailed in Fig. 3 and Fig. 4 at regular intervals；Fig. 3
In, the corresponding peak of 350nm or so is Cr(VI) ultraviolet absorption peak, nanocomposite is to Cr(VI as we know from the figure) have it is fast
The absorption of speed and reducing catalysis action, the interior almost fully reacting in 3min.
Embodiment 1 is to Cr(VI as can be seen from Figure 4) absorption with reduction removal rate be 46%, embodiment 2 is to Cr(VI) absorption and also
Former removal rate be 62%, embodiment 3 is to Cr(VI) absorption with reduction removal rate be 95%.
Claims (7)
1. a kind of preparation method of decorated by nano-gold poly-dopamine nanotube, which comprises the steps of:
(1) preparation of poly-dopamine nanotube
Using zinc oxide nano rod as template, then hydrochloric acid DOPA is added in zinc oxide nano rod Tris-HCl buffer solution
Amine room temperature reaction 0.5 ~ for 24 hours, precipitating is dispersed in water to obtain poly-dopamine zinc oxide nano rod aqueous solution after centrifuge washing, then
55 ~ 65 DEG C of ammonium chloride are added into solution to react 50 ~ 70 minutes, obtains poly-dopamine nanotube after centrifugation, washing, is distributed to
Poly-dopamine nanotube solution is obtained in ionized water, wherein the mass ratio of zinc oxide nano rod, Dopamine hydrochloride and ammonium chloride is
(2 ~ 1): (1 ~ 2): 320；
(2) preparation of decorated by nano-gold poly-dopamine nanotube
Chlorauric acid solution is added in poly-dopamine nanotube aqueous solution, the mass ratio of gold chloride and poly-dopamine nanotube is
(0.206 ~ 0.5): 1, room temperature reaction 20 ~ after forty minutes, centrifuge washing obtains decorated by nano-gold poly-dopamine nanotube.
2. the preparation method of decorated by nano-gold poly-dopamine nanotube according to claim 1, which is characterized in that the step
(1) dosage of zinc oxide nano rod and Dopamine hydrochloride is 10mg in, and Tris-HCl buffer concentration is 10mM, pH 8.5,
Dosage is 20mL, and the concentration of ammonium chloride is 2mol/L, dosage 30mL.
3. the preparation method of decorated by nano-gold poly-dopamine nanotube according to claim 1, which is characterized in that the step
(2) concentration of gold chloride is 0.01mol/L in, and dosage is 100 ~ 250 μ L, and the concentration of poly-dopamine nanotube aqueous solution is
0.2mg/mL, dosage 10mL.
4. the preparation method of decorated by nano-gold poly-dopamine nanotube according to claim 1, which is characterized in that the oxidation
The preparation process of zinc nanometer rods is as follows: zinc nitrate and sodium hydroxide being dissolved into deionized water, ethyl alcohol, second are then sequentially added
Mixed solution is ultrasonically formed uniform solution, solution is poured into autoclave by diamines, 170 ~ 190 DEG C of reactions 18 ~ 25
Hour, washing obtains template zinc oxide nano rod after dry, wherein the molar ratio 3:5 of zinc nitrate, sodium hydroxide and ethylenediamine:
20, the volume ratio of deionized water and ethyl alcohol is 6:5, and the concentration of the zinc nitrate in deionized water is 0.1 ~ 1mol/L.
5. the preparation method of decorated by nano-gold poly-dopamine nanotube according to claim 4, which is characterized in that it is described go from
The volume of sub- water is 30mL, and the concentration of zinc nitrate and sodium hydroxide in deionized water is respectively 0.5M, 10M.
6. decorated by nano-gold poly-dopamine nanotube made from any preparation method of claim 1 to 5.
7. decorated by nano-gold poly-dopamine nanotube described in claim 6 is adsorbing and is restoring the application in 6 valence chromium ions.
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