CN110514712A - A kind of polymeric ionic liquid modification MXene nanocomposite and its preparation method and application - Google Patents
A kind of polymeric ionic liquid modification MXene nanocomposite and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of polymeric ionic liquids to modify MXene (Ti3C2Tx) nanocomposite and its preparation method and application.The technical solution adopted is that: the MXene nanocomposite of poly- 1- vinyl -3- ethyl imidazol(e) bromide (PILs) modification is prepared for by noncovalent interaction, and it is its is immobilized in glass carbon (GCE) electrode surface, the modified electrode of glucose oxidase (GOx) and PILs-MXene is constructed, enzyme and interelectrode Direct electron transfer are successfully realized.Composite material of the invention can be used for the detection of glucose, have good detection performance.
Description
Technical field
The invention belongs to field of compound material more particularly to a kind of polymeric ionic liquid to modify MXene nanocomposite
Preparation method and application.
Background technique
It is a variety of to can lead to blindness, nerve retrograde affection and renal failure etc. for the exception of glucose level in blood of human body
Disease.Diabetes are to lead to one of dead and disabled Etiological in the world, and there are about 300,000,000 people to suffer from diabetes in the whole world.Glycosuria
The diagnosis and supervision of patient needs accurate measurements and controls intracorporal blood glucose level.Therefore, researchers develop big measurement
Determine the method for blood glucose, such as spectrophotometry, chromatography and electrochemical method.However, there are pre-treatment steps for many methods
The limitations such as complexity, equipment cost height, cost of labor height.Quickly, simply, reliably blood sugar monitoring is examined in biotechnology, clinic
It is disconnected that fields is waited to be of great significance.Compared with traditional glucose sensing approach, electrochemical method have higher selectivity and
Sensitivity, response speed are faster, more simply, more reliable, it is possible to provide the advantages that continuous real-time detection.Therefore, design, processability
Better electrode material seems outstanding for glucose sensing detection for constructing sensitive, stable glucose oxidase modified electrode
It is important.
Two-dimentional transition metal carbon/nitride is one of the New Two Dimensional stratified material quickly grown in recent years, due to having
Higher hydrophily, metallic conductivity, low diffusion barrier, macroion transport performance, biocompatibility, high surface area and it is easy to function
The features such as capable of changing, has attracted the concern from different scientific domain researchers.Such material includes early transition metal carbide, nitrogen
Compound and carbonitride, they are made by selective detachment MAX phase, in catalysis, clean energy resource, electronics, fuel cell, super
There is potentially large number of application value in the fields such as capacitor.In the recent period, it has been found that can effectively promote MXene as electrode material
Electron-transport between protein and the redox center and electrode surface of enzyme.The nanocomposite of MXene can be in electricity
The immobilized electroactive enzyme of pole surface, constructs the electrochemica biological sensor of medialess body, not only enables immobilized enzyme well
It keeps the bioactivity of its own and has effectively facilitated enzyme and interelectrode electron-transport.
Summary of the invention
The present invention consolidates polymeric ionic liquid by π-π interaction, by polymeric ionic liquid by electrostatic adsorption
It is downloaded to MXene material surface, it is therefore an objective to obtain one kind and have both polymeric ionic liquid highly dissoluble, satisfactory electrical conductivity and MXene material
Expect the nanocomposite (PILs-MXene) of high-specific surface area characteristic.The method for synthesizing composite material is simple, has in water
Good stability, obtained detector is sensitive, is having good application prospect using electrochemical method detection glucose field.
To achieve the above object, the technical solution adopted by the present invention is that: a kind of polymeric ionic liquid is modified MXene nanometer and is answered
Condensation material, preparation method include the following steps: to disperse MXene in deionized water, ultrasonic 3-4h, form suspension；To shape
At suspension in be added polymeric ionic liquid, after ultrasonic 5-6h, 10000rpm is centrifuged 5min, be washed with water remove it is unmodified
Polymeric ionic liquid on MXene, products therefrom are dried in vacuo at 60 DEG C, are obtained polymeric ionic liquid and are modified MXene nanometers again
Condensation material.
Further, the MXene is by utilizing hf etching Ti3AlC2Method preparation, include the following steps: by
The hydrofluoric acid that mass percentage concentration is 40% is placed in oil bath, is slowly added to Ti3AlC2And be stirred continuously, 72h is reacted at 25 DEG C
Afterwards, it is centrifuged 5min through 3500rpm, is washed with water to pH=6.0, products therefrom is dried in vacuo in 60 DEG C, obtains target product
MXene。
Further, the polymeric ionic liquid is made by 1- vinyl -3- imidazole-butyl bromide salt monomer.
Further, the preparation method of the polymeric ionic liquid includes the following steps: 1- vinyl -3- butyl miaow
Azoles bromide monomer and azodiisobutyronitrile are dissolved in chloroform, are passed through nitrogen, and flow back 3h under 70 DEG C of oil baths, products therefrom chloroform
Washing, vacuum drying, obtains target product polymeric ionic liquid PILs.
Further, the polymeric ionic liquid modification MXene nanocomposite PILs-MXene is multilayer chip knot
Structure.
Application of the above-mentioned polymeric ionic liquid modification MXene nanocomposite in detection glucose.
Further, the method is as follows:
1) preparation of Nafion-GOx-PILs-MXene/GCE modified electrode: 1:1:1 by volume takes the concentration to be respectively
Aqueous solution, the quality percentage of the PBS solution of the glucose oxidase (GOx) of 5mg/mL, the PILs-Mxene that concentration is 2mg/mL
The Nafion aqueous solution that concentration is 5%, shakes up after mixing；By gained mixing drop in the glassy carbon electrode surface pre-processed, 4 DEG C
Lower dry 6h forms one layer of Nafion-GOx-PILs-MXene film in glassy carbon electrode surface, Nafion-GOx-PILs- is made
MXene/GCE modified electrode；
2) using Ag/AgCl electrode as reference electrode, platinum electrode is auxiliary electrode, Nafion-GOx-PILs-MXene/GCE
Modified electrode is working electrode, three-electrode system is placed in the PBS solution of the pH=7.0 containing glucose, is lied prostrate by circulation
The chemical property of peace method (CV) and differential pulse voltametry (DPV) measurement glucose.
The beneficial effects of the present invention are:
1, the present invention has obtained a kind of polymeric ionic liquid modification MXene nanocomposite PILs-MXene.
2, the composite material PILs-MXene prepared by the present invention has both that water stability is good, large specific surface area, good conductivity
Etc. characteristics.
3, the composite material PILs-MXene prepared by the present invention can be used for glucose detection, have highly selective, detection
The features such as facilitating has good application prospect in glucose detection field.
Detailed description of the invention
Fig. 1 is Ti3AlC2(a), the SEM of MXene (b), PILs-MXene (c) scheme.
Fig. 2 is Ti3AlC2(a), the XRD diagram of MXene (b), PILs-MXene (c).
Fig. 3 is the Zeta potential figure of MXene (a), PILs (b), PILs-MXene (c).
Fig. 4 is PILs-MXene/GCE (a), GOx-PILs-MXene/GCE (b) molten in the potassium ferricyanide and potassium ferrocyanide
CV figure in liquid.
Fig. 5 is PILs-MXene/GCE (a), Nafion-GOx-PILs-MXene/GCE (b), Nafion-GOx-Mxene/
CV of the GCE (c) in 0.1mol/L PBS (pH=7.0) solution of saturation nitrogen schemes (sweeping speed: 200mV/s).
Fig. 6 is Nafion-GOx-PILs-MXene/GCE modified electrode various concentration (a-l 0.5- in the case where being saturated oxygen
8.0mmol/L) the DPV curve graph of glucose.
Fig. 7 is different concentration of glucose (Cglucose) and current-responsive difference (Δ Ip)Relational graph (lower right corner illustration:
Cglucose/ΔIp-CglucoseLinear calibration curve).
Specific embodiment
1 polymeric ionic liquid of embodiment modifies MXene nanocomposite (PILs-MXene)
(1) preparation method
1, the preparation of MXene
MXene(Ti3C2Tx) by utilizing hf etching Ti3AlC2Method preparation.120mL is added into plastic beaker
The hydrofluoric acid that mass percentage concentration is 40%, then places it in oil bath, is slow added into the Ti of 1g3AlC2And be stirred continuously,
After 25 DEG C of reaction 72h, 3500rpm is centrifuged 5min, centrifugation is washed with water, repeatedly until pH=6.0, products therefrom is 60
DEG C vacuum drying 12h, obtain target product MXene.
2, the preparation of polymeric ionic liquid
5g 1- vinyl -3- imidazole-butyl bromide salt monomer and 0.1g azodiisobutyronitrile are dissolved in 50mL chloroform, are passed through
Nitrogen, flow back 3h under 70 DEG C of oil baths, products therefrom chloroform, and vacuum drying obtains target product polymeric ionic liquid
PILs。
3, the preparation of PILs-MXene
The MXene of 50mg is taken to be scattered in 100mL deionized water, ultrasonic 3h forms the suspension of stable dispersion.Again to outstanding
In turbid after addition 140mg polymeric ionic liquid PILs, ultrasonic 5h, 10000rpm is centrifuged 5min, with water centrifuge washing 5 times, with
Remove the unmodified polymeric ionic liquid on MXene.Centrifugation product is dried in vacuo 12h at 60 DEG C, obtains polymerization plasma liquid
Body modifies MXene nanocomposite (PILs-MXene).
(2) structure and property representation of PILs-MXene
Fig. 1 is Ti3AlC2(a), the SEM shape appearance figure of MXene (b), PILs-MXene (c) can be seen that MAX by a in Fig. 1
(Ti3AlC2) mutually accordion like MXene material representative configuration is showed (in Fig. 1 after HF acid etch in stacking block structure
b).After MXene and PILs are compound, by c in Fig. 1 it is observed that made PILs-MXene is the slightly harsh multilayer in surface
Laminated structure, the MXene structure of this multilayer, so that the specific surface area of material increases, while the modification of PILs increases MXene
The water dispersible of material.
Fig. 2 is Ti3AlC2(a), the XRD diagram of MXene (b), PILs-MXene (c).Figure it is seen that Ti3AlC2's
39.2 ° (104) characteristic peak almost disappears, and and Ti3AlC2Position before etching is compared, and (002), (004) peak broaden,
It loses intensity and is moved to lower angle, show that MXene is successfully prepared.The XRD's and MXene of PILs-MXene
XRD has almost no change, and shows that the PILs modified on MXene does not destroy the orderly crystalline structure of MXene.
Fig. 3 is the Zeta potential figure of MXene (a), PILs (b), PILs-MXene (c).Zeta potential characterization can from figure
With see the Zeta value of MXene (a) for -9.8mV, the Zeta value 31.1mV of PILs (b), and the PILs-MXene (c) of modificationization
Zeta value is 14.5mV, it can be seen that the surface charge property of MXene changes before and after modification, is become just from negative
's.The reason is that, it is possible thereby to illustrate, the present invention exists as caused by introducing the imidazole ring containing positive charge on MXene
Modification introduces imidazolium ionic liquid in MXene nanometer sheet.The introducing of its surface charge plays electrostatic repulsion, prevents
The irreversible reunion of MXene nanometer sheet, maintains its stable dispersion in water.
2 polymeric ionic liquid of embodiment modifies MXene nanocomposite PILs-MXene answering in detection glucose
With the preparation of (one) modified electrode
1) pretreatment of glass-carbon electrode: successively with 0.1 μm, 0.3 μm, 0.05 μm of A12O3Glass-carbon electrode (GCE) is thrown
Light.Then, ultrapure water is cleaned by ultrasonic 1min.Using glass-carbon electrode as working electrode, Ag/AgCl electrode is reference electrode, and platinum filament is
To electrode, contain l × 10 in 1mol/L-3mol/L K3Fe(CN)6KCl solution in carry out electrochemistry cyclic voltammetric (CV) survey
Examination, scanning range are -0.8~-0.2V (vs.Ag/AgCl), sweep speed 200mV/s.It is after test that electrode ultrapure water is clear
It washes, high pure nitrogen drying is spare.
2) preparation of Nafion-GOx-PILs-MXene/GCE modified electrode: taking concentration respectively is the glucose of 5mg/mL
The aqueous solution of PILs-Mxene prepared by PBS (pH=7.0) solution of oxidizing ferment (GOx), the embodiment 1 that concentration is 2mg/mL,
The Nafion aqueous solution that mass percentage concentration is 5%, each 300 μ L shake up after mixing.5 μ L drop of gained mixed liquor is being pre-processed
Good glassy carbon electrode surface, on the electrode beaker on mask, dry 6h at 4 DEG C form one layer of Nafion- in glassy carbon electrode surface
Nafion-GOx-PILs-MXene/GCE modified electrode is made in GOx-PILs-MXene film
(2) experimental result
Electrochemistry experiment method: this experiment is tested under different pH respectively and is followed using 0.1mol/L PBS as supporting electrolyte
Ring volt-ampere (CV), analyzing optimal conditions by contrast is pH=7.0.Experiment uses three-electrode system, and Ag/AgCl electrode is reference electricity
Pole, platinum electrode are auxiliary electrode, and Nafion-GOx-PILs-MXene/GCE modified electrode is working electrode.
1, the electrochemical behavior research of Nafion-GOx-PILs-MXene/GCE modified electrode
Fig. 4 is that PILs-MXene/GCE (a), GOx-PILs-MXene/GCE (b) are molten in the potassium ferricyanide and potassium ferrocyanide
CV figure in liquid, Fig. 4 are Fe [(CN) of the electrode in 0.1mol/L of different materials modification6]3-/4-CV curve graph in solution.From
As can be seen that the redox current intensity of PILs-MXene/GCE electrode is higher than electrode GOx-PILs-MXene/GCE in figure
Current strength, this shows when GOx is modified on GOx-PILs-MXene/GCE electrode, under the current strength of electrode slightly has
Drop, this is because the enzyme as large biological molecule usually has huge space structure, redox center is by polypeptide chain packet
It encloses, surface charge is in asymmetric distribution, this will hinder enzyme that Direct electron transfer occurs in electrode surface, leads to the conductive energy of electrode
Power decline.
Fig. 5 is PILs-MXene/GCE (a), Nafion-GOx-PILs-MXene/GCE (b), Nafion-GOx-MXene/
CV of the GCE (c) in 0.1mol/L PBS (pH=7.0) solution of saturation nitrogen schemes (sweeping speed: 200mV/s).By can be in figure
Find out that curve a non-oxidation reduction peak in -0.7V~-0.2V voltage range occurs, shows on PILs-MXene/GCE electrode
Electroactive material exists.And shown in curve b, c, near current potential -0.42V, there is a pair of apparent redox in electrode
Peak, this is because GOx realizes characteristic peak caused by Direct Electrochemistry on this electrode, furtherly can be carried out can for prescribed electrode
Inverse Direct Electrochemistry reaction, the above results show that GOx has excellent electrocatalysis characteristic.And the redox peaks of b curve are bright
It is aobvious to be higher than c curve, it can thus be concluded that PILs-MXene material conductivity is more preferable out.
2, research of the Nafion-GOx-PILs-MXene/GCE modified electrode to glucose catalytic performance
Electrochemistry experiment method: this experiment is electrolysed using 0.1mol/L PBS (pH=7.0) as supporting electrolyte in support
Glucose, test loop volt-ampere (CV) and differential scanning volt-ampere (DPV) figure are added in matter.Experiment uses three-electrode system, Ag/
AgCl electrode is reference electrode, and platinum electrode is auxiliary electrode, and Nafion-GOx-PILs-MXene/GCE modified electrode is work electricity
Pole.Scanning range is -0.5~-0.2V (vs.Ag/AgCl), sweep speed 200mV/s.
Fig. 6 be Nafion-GOx-PILs-MXene/GCE modified electrode in the case where being saturated oxygen various concentration (0.5~
8.0mmol/L) the DPV curve graph of glucose.As seen from the figure, when adding small amount glucose, occur one it is stronger also
Parent peak shows that GOx remains high biology catalytic activity to glucose.In addition, with the increase of glucose in solutions content, it should
The reduction peak intensity continuous of electrode reduces.This is because directly reacting, making with GOx (FAD) when glucose content is more
GOx (FAD) is converted into GOx (FADH2).Which results in GOx (FAD) reductions for participating in electrochemical reaction, so that reduction peak intensity
Degree gradually weakens with the increase of glucose additional amount.
Fig. 7 is different concentration of glucose (Cglucose) and current-responsive difference (Δ Ip)Relational graph (lower right corner illustration:
Cglucose-Cglucose/ΔIpLinear calibration curve) as seen from the figure, concentration of glucose increases, and the current difference of peak value is also therewith
Increase.Between 0.5~8.0mmol/L of concentration range, Δ IpWith CglucoseIt is in a linear relationship, linear equation: Cglucose/ΔIp
=0.6624Cglucose+ 1.0285, coefficient R2It is 0.9962, detection is limited to 0.03mmol/L.This shows glucose oxidase
There are good bioactivity and enzyme kinetics response on Nafion-GOx-PILs-MXene/GCE electrode, it may also be said to bright
Glucose oxidase has good catalytic capability and stronger biological affinity on the modified electrode, this should be attributed to
The preferable bio-compatibility of PILs-MXene nano material, biggish specific surface area, higher conductivity and good chemistry
Stability.These characteristics not only increase the electric conductivity of electrode, while also accelerating the speed of the electron transmission between GOx and electrode
Rate.
Claims (7)
1. a kind of polymeric ionic liquid modifies MXene nanocomposite, it is characterised in that: preparation method includes the following steps:
It disperses MXene in deionized water, ultrasonic 3-4h, forms suspension；Polymeric ionic liquid is added into the suspension of formation,
After ultrasonic 5-6h, 10000rpm is centrifuged 5min, is washed with water and removes the unmodified polymeric ionic liquid on MXene, and gained produces
Object is dried in vacuo at 60 DEG C, obtains polymeric ionic liquid modification MXene nanocomposite.
2. a kind of polymeric ionic liquid according to claim 1 modifies MXene nanocomposite, which is characterized in that institute
The preparation method for stating MXene includes the following steps: that the hydrofluoric acid for being 40% by mass percentage concentration is placed in oil bath, is slowly added to
Ti3AlC2And be stirred continuously, after reacting 72h at 25 DEG C, it is centrifuged 5min through 3500rpm, is washed with water to pH=6.0, gained produces
Object is dried in vacuo in 60 DEG C, obtains target product MXene.
3. a kind of polymeric ionic liquid according to claim 1 modifies MXene nanocomposite, it is characterised in that: institute
Polymeric ionic liquid is stated to be made by 1- vinyl -3- imidazole-butyl bromide salt monomer.
4. a kind of polymeric ionic liquid according to claim 3 modifies MXene nanocomposite, it is characterised in that: institute
State polymeric ionic liquid preparation method include the following steps: 1- vinyl -3- imidazole-butyl bromide salt monomer and azo two is different
Butyronitrile is dissolved in chloroform, is passed through nitrogen, and flow back 3h under 70 DEG C of oil baths, products therefrom chloroform, and vacuum drying obtains target
Product polymeric ionic liquid PILs.
5. a kind of polymeric ionic liquid according to claim 3 or 4 modifies MXene nanocomposite, it is characterised in that:
The polymeric ionic liquid modification MXene nanocomposite PILs-MXene is multilayer chip structure.
6. the described in any item polymeric ionic liquid modification MXene nanocomposites of claim 1-5 are in detection glucose
Application.
7. application according to claim 6, which is characterized in that method is as follows:
1) preparation of Nafion-GOx-PILs-MXene/GCE modified electrode: 1:1:1 by volume, taking concentration respectively is 5mg/
The PBS solution of the glucose oxidase (GOx) of mL, the aqueous solution for the PILs-Mxene that concentration is 2mg/mL, mass percentage concentration
For 5% Nafion aqueous solution, shaken up after mixing；Gained mixing drop is done at the glassy carbon electrode surface pre-processed, 4 DEG C
Dry 6h forms one layer of Nafion-GOx-PILs-MXene film in glassy carbon electrode surface, Nafion-GOx-PILs- is made
MXene/GCE modified electrode；
2) using Ag/AgCl electrode as reference electrode, platinum electrode is auxiliary electrode, Nafion-GOx-PILs-MXene/GCE modification
Electrode is working electrode, three-electrode system is placed in the PBS solution of the pH=7.0 containing glucose, passes through cyclic voltammetry
(CV) and differential pulse voltametry (DPV) measurement glucose chemical property.
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| CN111785534A (en) * | 2020-06-08 | 2020-10-16 | 华中科技大学 | Method for immobilizing MXene by ionic liquid covalent bonding and product thereof |
| CN113552196A (en) * | 2021-08-20 | 2021-10-26 | 辽宁大学 | Few-layer MXene-ionic liquid droplet modified electrode, preparation method thereof and application thereof in detection of Sudan red |
| CN114854157A (en) * | 2022-05-18 | 2022-08-05 | 中国科学院大学 | Multifunctional MXene/polyion liquid composite material |
| CN115055172A (en) * | 2022-07-11 | 2022-09-16 | 东莞理工学院 | Preparation method and application of polyion liquid modified MXene adsorbent |
| CN115055172B (en) * | 2022-07-11 | 2024-03-12 | 东莞理工学院 | Preparation method and application of polyion liquid modified MXene adsorbent |
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