CN106984277A - Positively charged composite and its preparation method and application - Google Patents
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Abstract
The present invention relates to field of nanocomposite materials, and more particularly to a kind of positively charged composite and its preparation method and application.The preparation method is by positively charged SURFACTANT ADSORPTION to graphene oxide and CNT using electrostatic adsorption.This method operating procedure is simple, operating condition is gentle, it is easy to accomplish, can large-scale application in industrial production.The composite quickly, efficiently and specifically to high polyanionic compound can carry out Electrochemical Detection.
Description
Technical field
The present invention relates to field of nanocomposite materials, and more particularly to a kind of positively charged composite and its preparation side
Method and application.
Background technology
Lauryl sodium sulfate (SDS) is commonly called as " industrial monosodium glutamate glutamic acid ", is a kind of anion table being most widely used
Face activating agent.Meanwhile, it is also main component in the detergent and detergent that much cleaning, decontamination industry are used, and is also biochemical
With protein denaturant conventional in terms of immune detection.Zoopery, which has proven to SDS, direct toxic action to animal body.Grind
Study carefully and also show that the SDS of foamed can be ultimately resulted under dissolved oxygen concentration with normal oxygen exchange in larger intervention water body
Drop and cause water quality deterioration, and then water ecosystem is done great damage.Before development based on the mankind and the ecosystem
Scape, it is very important to find SDS contents in a kind of detection method detection water body of rapid sensitive.Carbon material is with its excellent electricity
Chemical property and topographical property, make it obtain relatively broad application in fields such as bio-sensing, cell catalyst and environmental analyses,
Its appearance is expected to trigger new round revolution in nanometer material science field, and application prospect is boundless.
The content of the invention
It is an object of the invention to provide a kind of preparation method of positively charged composite, its can quickly by band just
The SURFACTANT ADSORPTION of electric charge is to outside graphene oxide and CNT, this method is simple to operate, mild condition, be easy to real
Now, with wide industrial prospect.
Another object of the present invention is to provide a kind of positively charged composite, the composite is conducive to extension electricity
Application of the chemical technology in environment measuring, solves the high polyanionic polymer electrochemistry to no electro-chemical activity
This technical barrier is detected, the high poly- zwitterion compound of the detection that it can be selective.
Another object of the present invention is to provide a kind of application of positively charged composite in detection SDS, in fact
Now to the high-sensitivity detection of high electronegative surfactant.
The present invention is solved its technical problem and realized using following technical scheme：
The present invention proposes a kind of preparation method of positively charged composite, comprises the following steps：Utilize Electrostatic Absorption
Effect is by positively charged SURFACTANT ADSORPTION to graphene oxide and CNT.
The present invention proposes a kind of positively charged composite, and it is prepared by above-mentioned preparation method.
The present invention provides a kind of application of positively charged composite in detection SDS.
The beneficial effect of the positively charged composite of the present invention and its preparation method and application is：The composite material surface
The positive charge carried can electroactive cloudy anion in adsorbent solution, then can with it is specific with high polyanion by the moon from
Sub- switching technology is replaced, and then is enabled the composite prepared quick, efficient and specifically carried out electrification
Learn detection.And it can realize and Electrochemical Detection is carried out to the high polyanion surfactant of no electro-chemical activity, expand
Its application.And the method operating procedure for preparing the composite is brief, operating condition is gentle, it is easy to accomplish, it can advise greatly
Mould is applied to industrial production.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to institute in embodiment
The accompanying drawing needed to use is briefly described.
Fig. 1 is the electron-microscope scanning figure for the PDDA/GO/SWCNTs composites that the embodiment of the present invention 1 is provided；
Fig. 2 is the testing result collection of illustrative plates of the cyclic voltammetry of experimental example 1 of the present invention；
Fig. 3 is the testing result collection of illustrative plates of the differential pulse voltammetry technology of experimental example 1 of the present invention；
Fig. 4 is the selective enumeration method result figure of the differential pulse voltammetry technology of experimental example 2 of the present invention.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional production that can be obtained by commercially available purchase
Product.
In the description of the invention, it is necessary to which explanation, term " first ", " second " etc. are only used for distinguishing description, without
It is understood that to indicate or imply relative importance.
Positively charged composite of the embodiment of the present invention and its preparation method and application is specifically described below.
A kind of preparation method of positively charged composite provided in an embodiment of the present invention：
S1, by outside positively charged SURFACTANT ADSORPTION to graphene oxide and CNT；
Graphene oxide (GO) and carbon nano tube surface are main with-COOH and the presence of-OH groups, and they can contain to surface
The polymer for having a large amount of positive charges produces specific electrostatic adsorption, and then enables the composite to pass through anion
Switching technology realizes the high-sensitivity detection of high polyanionic compound, effectively extends the application model of electrochemical techniques detection
Enclose.
The raw material used is graphene oxide and CNT rather than single graphene oxide or CNT are
Because the composite cavity using single graphene oxide or CNT formation is small, the space of adsorpting anion is small,
Anion is difficult to replace with cation, and then influences its detection to anion superpolymer.And co-oxidation graphene and
The cavity of the composite of CNT formation is larger, can quickly accommodate more anion superpolymer, and then lifted multiple
Condensation material detects the speed and efficiency of anion superpolymer.
It is further preferred that will be by oxygen outside positively charged SURFACTANT ADSORPTION to graphene oxide and CNT
Graphite alkene is mixed after being mixed with CNT with positively charged surfactant.Graphene and CNT are carried out first
Mixing, is that, in order to ensure subsequently to add after positively charged surfactant, positively charged surfactant can be inhaled simultaneously
It is attached to outside graphene oxide and CNT.If first graphene oxide and positively charged surfactant are mixed either
Can not surfactant be realized while being adsorbed onto graphite oxide by first mixing CNT and positively charged surfactant
On alkene and CNT, surfactant is only adsorbed onto on graphene oxide or CNT, and then influences what is prepared
The performance of composite and the sensitivity for detecting anion.
Mixed it is further preferred that graphene oxide is mixed with CNT using ultrasound, the time of ultrasonic mixing
For 1-2 hours.Ultrasound can act on molecule so that graphene oxide and CNT are mixed evenly, more conducively positively charged
The surfactant of lotus acts on graphene oxide and CNT simultaneously.It is further preferred that being lived with positively charged surface
Property agent mixing also using ultrasound mixed, incorporation time be 2-3 hours.
It is further preferred that the mass ratio of graphene oxide and CNT is 0.8-1.2:1.Mixed using the ratio
Close and ensure that follow-up positively charged surfactant can be while act on graphene oxide and CNT.
It is further preferred that it is that graphene oxide and CNT are dispersed in into chlorine that graphene oxide is mixed with CNT
Change in sodium solution.The present invention using neutral sodium chloride solution rather than using the aqueous solution be in order to strengthen solution ion strength,
Effectively it can be adsorbed onto beneficial to follow-up positively charged surfactant on graphene oxide and CNT.According to water-soluble
Liquid, effects of ion intensity is not enough, it is impossible to provides absorption environment well and absorption power, influences the generation of composite.Enter
Preferably, the molar concentration of sodium chloride solution is 0.8-1.2M to one step.
It is further preferred that CNT is single-walled carbon nanotube (SWCNTs).Had using single-walled carbon nanotube excellent
The performance such as electronics, machinery, mechanics, especially all there is the mobility of superelevation to electronics and hole, therefore, received using single wall carbon
Mitron can be further ensured that subsequent anion is smoothed out exchanging with cation, improve the detection sensitivity of composite.
It is further preferred that positively charged surfactant is positively charged high polymer, it is due to using high polymer
It can form multiple Electrostatic Absorption with graphene oxide and CNT so that the structure of composite more they tends to stable and shape
Cheng Geng great Substitution Spaces.
Further, positively charged surfactant is PDDA, PEI and gathered
Any one in acid imide.PDDA (PDDA) is strong cationic polyelectrolytes, and outward appearance is colourless
To light yellow viscous liquid.Safe and nontoxic, soluble in water, nonflammable, cohesiveness is strong, hydrolytic stability is good.PEI
(PEI) there is high intensity, high rigidity, wearability and dimensional stability at high temperature.PEI have excellent mechanical strength,
Electrical insulation capability, radiation resistance, high-low temperature resistant and fatigue performance and molding processibility；Add glass fibre, carbon fiber or its
His filler can reach the modified purpose of enhancing.Polyimides (PI) is one of optimal high-molecular organic material of combination property, resistance to height
Temperature range -200~300 DEG C, no sharp melting point, high insulating property are used for a long time up to more than 400 DEG C in temperature.
S2, centrifugation；
Centrifuged after graphene oxide, CNT are mixed with positively charged surfactant, the rotating speed of centrifugation
For 6500-7500rpm, centrifugation time is 15-25 minutes.It is to remove in the composite material surface prepared to carry out centrifugation
Unnecessary sodium chloride and positively charged surfactant.Using above-mentioned centrifugal rotational speed and centrifugation time, it is ensured that removal of impurities is imitated
Really, while avoiding because excessive centrifugal rotational speed and long centrifugation time destroy positively charged surfactant and oxidation stone
Electrostatic interaction between black alkene and CNT.
A kind of positively charged composite that the embodiment of the present invention is also provided.The composite passes through above-mentioned preparation side
Method is prepared.Simultaneously, it is necessary to which explanation is that the composite can be applied to fast qualitative and quantitatively detect that SDS contains in water
Amount.The preparation method is produced special by the anion on positively charged surfactant and graphene oxide and CNT
The Electrostatic Absorption of property prepares positively charged composite.The composite being capable of specificity and anion formation electrostatic suction
It is attached then to recycle anionexchangetechnique to detect high polyanionic compound, realize the composite quick, high
Imitate, optionally carry out Electrochemical Detection.This method integrated operation is simple, it is only necessary to is mixed and is stirred and need not be added
Heat and other operations, simplify the preparation process of composite, and preparation condition is gentle, it is easy to accomplish, it is more conducive to industry
Using.
The feature and performance to the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of PDDA/GO/SWCNTs composites that the present embodiment is provided, it is mainly received by graphene oxide, single wall carbon
Mitron and PDDA, which are made, to be obtained.Wherein, graphene oxide, single-walled carbon nanotube mass ratio are 1:1.To PDDA/GO/SWCNTs
Composite carries out Electronic Speculum and swept, and specifically sees Fig. 1.
The present embodiment also provides a kind of method for preparing PDDA/GO/SWCNTs composites：
Weigh GO and SWCNTs (mass ratioes 1:1) (1M) is placed in 50mL NaCl solutions, at room temperature ultrasound 1.5h, then
Directly toward addition 80mg PDDA in mixed solution, continuous ultrasound 2.5h, finally unnecessary to remove by product centrifugation at room temperature
NaCl and PDDA.Eccentric cleaning rotating speed is 7000rpm, and centrifugation time is 20min, that is, electrochemical performance is made
PDDA/GO/SWCNTs nano composite materials.
Embodiment 2
A kind of PI/GO/SWCNTs composites that the present embodiment is provided, it is mainly by graphene oxide, single
Pipe and PI are made and obtained.Wherein, graphene oxide and single-walled carbon nanotube mass ratio are 0.8:1.
The present embodiment also provides a kind of method for preparing PI/GO/SWCNTs composites：
Weigh GO and SWCNTs (mass ratioes 0.8:1) (1.2M) is placed in 50mL NaCl solutions, at room temperature ultrasound 1h, so
Afterwards directly toward addition 100mg PI in mixed solution, continuous ultrasound 3h, finally unnecessary to remove by product centrifugation at room temperature
NaCl and PI.Eccentric cleaning rotating speed is 6500rpm, and centrifugation time is 15min, that is, the PI/GO/ of electrochemical performance is made
SWCNTs nano composite materials.
Embodiment 3
A kind of PEI/GO/SWCNTs composites that the present embodiment is provided, it is mainly by graphene oxide, single
Pipe and PEI are made and obtained.Wherein, graphene oxide and single-walled carbon nanotube mass ratio are 1.2:1.
The present embodiment also provides a kind of method for preparing PEI/GO/SWCNTs composites：
Weigh GO and SWCNTs (mass ratioes 1.2:1) (0.8M) is placed in 50mL NaCl solutions, at room temperature ultrasound 2h, so
Afterwards directly toward addition 90mg PEI in mixed solution, continuous ultrasound 2h, finally unnecessary to remove by product centrifugation at room temperature
NaCl and PEI.Eccentric cleaning rotating speed is 7500rpm, and centrifugation time is 25min, that is, the PEI/ of electrochemical performance is made
GO/SWCNTs nano composite materials.
Embodiment 4
A kind of PDDA/GO/SWCNTs composites that the present embodiment is provided, it is mainly received by graphene oxide, single wall carbon
Mitron and PDDA, which are made, to be obtained.Wherein, graphene oxide and single-walled carbon nanotube mass ratio are 0.9:1.
The present embodiment also provides a kind of method for preparing PDDA/GO/SWCNTs composites：
Weigh GO and SWCNTs (mass ratioes 0.9:1) (1.1M) is placed in 50mL NaCl solutions, at room temperature ultrasound 1.3h,
Then directly toward addition 100mg PDDA in mixed solution, continuous ultrasound 2.7h, finally centrifuges product many to remove at room temperature
Remaining NaCl and PI.Eccentric cleaning rotating speed is 7200rpm, and centrifugation time is 22min, that is, electrochemical performance is made
PDDA/GO/SWCNTs nano composite materials.
Experimental example
In order to carry out test verification to the performance of composite in the embodiment of the present invention, this test example chooses embodiment 1
Composite as this test example sample, applied in SDS detection carry out experimental analysis test.
Specifically operating procedure is：6.0 μ L PDDA/GO/SWCNTs (18.0mg/mL) drop coatings are measured to the glass polished
On carbon electrode (GCE), Fe (CN) is dipped into after drying in atmosphere6 3-/4-(5mM) 20min in solution, then by modification
GCE electrodes, which are placed in secondary water, to be rinsed several times, unnecessary Fe (CN) to remove6 3-/4-Molecule, is finally placed in air and dries in the air
It is dry.Then be immersed in certain density SDS solution react 15min after, modified electrode is placed in secondary water rinse it is several
Secondary, unnecessary to remove SDS molecules, are placed in air and dry.
Experimental example 1
Detect in water body whether contain SDS using cyclic voltammetric and differential pulse voltammetry technology (DPV) respectively.
The testing result of cyclic voltammetry is Fig. 2, and curve a is the composite modified electrode of embodiment 1 in pH=in Fig. 2
Detection curve in 7.0 PBS, after curve b is the composite modified electrode absorption potassium ferricyanide containing embodiment 1
Detection curve in pH=7.0 PBS, curve c is the composite modified electrode absorption iron cyanogen containing embodiment 1
Change the detection curve in containing SDS buffer solutions after potassium.It can be seen from Fig. 2, composite and Fe (CN)6 3-/4-After effect
0.15V or so occur Strong oxdiative reduction peak (curve b), and after being acted on SDS 0.15V or so Strong oxdiative reduction peak weakened
(curve c) illustrates that the composite can detect whether contain in solution according to 0.15V or so Strong oxdiative reduction peak Strength Changes
There is SDS.
The testing result of DPV technologies is shown in that curve a is the composite modified electrode of embodiment 1 in pH=7.0 in Fig. 3, Fig. 3
PBS in detection curve, curve b for containing embodiment 1 composite modified electrode absorption the potassium ferricyanide after
Detection curve in pH=7.0 PBS, curve c is the composite modified electrode absorption iron cyaniding containing embodiment 1
Detection curve after potassium in containing SDS buffer solutions.It can be seen from Fig. 3, composite and Fe (CN)6 3-/4-In 0.15V after effect
Left and right occur Strong oxdiative reduction peak (curve b), and after being acted on SDS 0.15V or so Strong oxdiative reduction peak weakened (curve
C), illustrate that the composite can detect whether contain in solution according to 0.15V or so Strong oxdiative reduction peak Strength Changes
SDS。
Meanwhile, whether comparison diagram 2 and Fig. 3 have found, not high using the detection precision of cyclic voltammetry, for containing in solution
There is SDS sensitivity poor, and detected that sensitivity is improved significantly using DPV technologies, it is therefore, follow-up to use
DPV technologies are detected.
Experimental example 2
SDS selectivity is detected using differential pulse voltammetry technology (DPV).Concrete outcome is shown in Fig. 4.According to Fig. 4
Testing result understand that the electrode pair SDS of the composite of drop coating embodiment 1 analysis detection has good selectivity.
In summary, positively charged composite that 1-3 of the embodiment of the present invention is provided and its preparation method and application.Should
The positive charge that composite material surface is carried can optionally electroactive cloudy anion in adsorbent solution, then can be specifically
Replaced with high polyanion by anionexchangetechnique, and then enable the composite prepared quick, high
Imitate and Electrochemical Detection specifically is carried out to high polyanionic compound.And prepare the method operating procedure letter of the composite
Short, operating condition is gentle, it is easy to accomplish, can large-scale application in industrial production.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of preparation method of positively charged composite, it is characterised in that comprise the following steps：
Using electrostatic adsorption by positively charged SURFACTANT ADSORPTION to graphene oxide and CNT.
2. the preparation method of positively charged composite according to claim 1, it is characterised in that described positively charged
Surfactant be PDDA, PEI and polyimides in any one.
3. the preparation method of positively charged composite according to claim 2, it is characterised in that the CNT
For single-walled carbon nanotube.
4. the preparation method of positively charged composite according to claim 3, it is characterised in that the graphite oxide
The mass ratio of alkene and the CNT is 0.8-1.2:1.
5. the preparation method of the positively charged composite according to claim 2-4 any one, it is characterised in that will
The positively charged SURFACTANT ADSORPTION is to being by the graphite oxide outside the graphene oxide and the CNT
Alkene mixed with the CNT after with the positively charged surfactant ultrasonic mixing.
6. the preparation method of positively charged composite according to claim 5, it is characterised in that the graphite oxide
It is that the graphene oxide with the CNT is dispersed in sodium chloride solution and carried out that alkene is mixed with the CNT
Ultrasound.
7. the preparation method of positively charged composite according to claim 6, it is characterised in that the sodium chloride is molten
The molar concentration 0.8-1.2M of liquid.
8. the preparation method of positively charged composite according to claim 5, it is characterised in that by the oxidation stone
Black alkene, the CNT are centrifuged after being mixed with the positively charged surfactant, and the rotating speed of centrifugation is 6500-
7500rpm, centrifugation time is 15-25 minutes.
9. a kind of positively charged composite, it is characterised in that it is as the positively charged as described in claim 1-8 any one
The preparation method of the composite of lotus is prepared.
10. application of the positively charged composite in detection SDS described in claim 9.
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