CN107064252A - A kind of hydrogen peroxide sensor and preparation method and application - Google Patents
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Abstract
The invention discloses a kind of hydrogen peroxide sensor and preparation method thereof.The preparation method passes through hydro-thermal method, using potassium peroxydisulfate, manganese sulfate, potassium sulfate and sulfuric acid as raw material, sea urchin shape nano material of manganese dioxide is prepared in constant temperature oven, and by its drop coating in glassy carbon electrode surface, with platinized platinum, Ag/AgCl electrode assemblings into hydrogen peroxide sensor.The purity of the sea urchin shape nano material of manganese dioxide is high, distribution is good, size uniform, and the sensor has wider detection range to hydrogen peroxide, and be easy to repeat to prepare, there is great application prospect in fields such as biomedicine, environmental pollution monitoring, Food Inspection.
Description
Technical field
The invention belongs to electrochemical sensor field, more particularly, to a kind of hydrogen peroxide sensor and its preparation side
Method and application.
Background technology
Hydrogen peroxide is the compound that a kind of simplicity is easy to get, in medical diagnosis and treatment, environment mining, weaving food industry, biology
There is important application in the fields such as technology.Except well-known poisonous effect, H2O2As a kind of signaling molecule in organism,
There is weight in a variety of biological regulation processes such as immune cell activation, vascular remodeling, cell death, stomata closure and root growth
The effect wanted.Current detection method has AAS, analysis by titration, electrochemical process etc., and wherein electrochemical process is to be based on
Determinand chemical quantity is transformed into a kind of detection technique that electrical quantities are sensed by the electrochemical properties of test substance.It is specific and
Speech, i.e., by detecting the electric signal such as electric current, resistance or current potential means come target substance content in measure system, because it is simple just
It is prompt, rapidly and efficiently, stable and accurate feature being used in research more.But most electrochemical sensor is the biological biography based on enzyme
Sensor, and the stability of enzyme is poor, require harsh to external conditions such as temperature humidity pH, and the solid means of enzyme are numerous and diverse so that it is being answered
Often it is limited in.Therefore, no enzyme H2O2Sensor turns into the important directions that electrochemical sensor is studied.Noble metal such as gold,
Silver, palladium, H is commonly used for due to its superior electro catalytic activity2O2Without enzyme sensing in.But noble metal is expensive and source is rare, and
It can not be widely used in real life, this facilitate transition metal oxide to H2O2The research of sensing capabilities.
Manganese dioxide is as important transition metal oxide, and due to its special physicochemical properties, not only price is low
Honest and clean, environmental protection, also with high electro catalytic activity.Manganese dioxide composite material is in H2O2Application in electrochemical sensor
Receive much concern.There are some researches show, pattern and structure are the important parameters that nano material determines electro catalytic activity.It is at present to use more
Mn oxide builds hydrogen peroxide sensor with carbon nano tube compound material, and the manganese dioxide/graphene prepared by hydro-thermal method is received
Nano composite material, to H in neutral environment2O2Sensing shows good repeatability, selectivity, stability and catalytic activity.So
And, therefore the same expensive cost for fear of carbon material, is studied the hydrogen peroxide electrochemical sensing of nano material of manganese dioxide
Seem particularly urgent.
The content of the invention
The purpose of the present invention is that there is provided a kind of preparation side of hydrogen peroxide sensor with shortcoming in view of the shortcomings of the prior art
Method.This method has pollution-free nontoxicity, and mild condition is simple to operate, the advantages of sensitivity is high, stability is good.
It is another object of the present invention to provide hydrogen peroxide sensor prepared by a kind of above method.The hydrogen peroxide
Nontoxicity that sensor is pollution-free, mild condition is simple to operate, it is to avoid the noble metal of expensive traditional, carbon composite load, with
And the manganese dioxide nanowire load of weak catalytic activity, the hydrogen peroxide sensor of sea urchin shape manganese dioxide load can stablize,
Efficiently carry out the hydrogen peroxide detection of low concentration, favorable repeatability.
It is still another object of the present invention to provide a kind of application of above-mentioned hydrogen peroxide sensor.
Above-mentioned purpose of the present invention is achieved by the following technical programs：
A kind of preparation method of hydrogen peroxide sensor, comprises the following steps：
S1. deionized water is added after mixing potassium peroxydisulfate, manganese sulfate and potassium sulfate, stirs and the concentrated sulfuric acid is added dropwise, be placed in
140~160 DEG C of reactions；
S2. step S1 products therefroms are stood, sucks supernatant liquor, added deionized water or ethanol is centrifuged, separate
After suck supernatant liquor；
S3. centrifuged 2~3 times described in repeat step S2, product is dried into 12~24h at 60~80 DEG C, sea urchin is obtained
Shape manganese dioxide；
S4. sea urchin shape manganese dioxide is added in ethanol, water and Nafion solution, 30~50min of ultrasound obtains titanium dioxide
Manganese slurries；
S5. manganese dioxide slurries are applied to glassy carbon electrode surface, natural drying obtains working electrode；
S6. by working electrode, reference electrode and electrode is connected with three-electrode system, be put into electrolyte, constitute peroxide
Change hydrogen sensor.
Preferably, the mass ratio of potassium peroxydisulfate, manganese sulfate and potassium sulfate described in step S1 is (1~2):(1~2):(3
~4)；The mass volume ratio of the potassium peroxydisulfate, the gross mass of manganese sulfate and potassium sulfate and deionized water is (50~80):1mg/
The volume ratio of mL, the deionized water and the concentrated sulfuric acid is (30~50):1.
Preferably, the time stirred described in step S1 is 30~50min, and the time of the reaction is 6~8h.
Preferably, the time stood described in step S2 is 20~30min, and the speed of the centrifugation is 4000~6000r/
Min, the time of the centrifugation is 5~10min.
Preferably, the quality cumulative volume ratio of sea urchin shape manganese dioxide described in step S4 and second alcohol and water is (1~1.5):
1mg/mL, the volume ratio of the ethanol, water and Nafion is (1~10):(1~10):(1~2).
Preferably, a diameter of 1.5~2cm of glass-carbon electrode described in step S5.
Preferably, reference electrode described in step S6 is Ag/AgCl electrodes, and described is platinized platinum, the electrolyte to electrode
For PBS solution, the pH=7 of the PBS solution.
It is further preferable that the electrolyte of the Ag/AgCl electrodes is KCl solution, the concentration of the KCl solution for 3~
4mol/L, the specification of the platinized platinum is (0.5~1) × (0.5~1) cm × cm.
Hydrogen peroxide sensor and its application in food medical treatment, environmental pollution monitoring field prepared by the above method.
The hydrogen peroxide sensor of the present invention has pollution-free nontoxicity, and mild condition is simple to operate, and sensitivity is high, steady
Qualitative good the advantages of, raw materials are cheap and easy to get.There are two committed steps in preparation process：The preparation of sea urchin shape manganese dioxide
With manganese dioxide load in glassy carbon electrode surface, and other hydrogen peroxide sensors are prepared according to the method for the invention, such as
The hydrogen peroxide sensor of the transition metal oxides such as cupric oxide, iron oxide, titanium dioxide load, this detects have to hydrogen peroxide
There is very big researching value, the numerous areas such as food medical treatment, environmental pollution monitoring will be widely used in.
Compared with prior art, the invention has the advantages that：
1. the invention provides a kind of preparation method of new hydrogen peroxide sensor, this method can rapidly prepare spirit
The hydrogen peroxide sensor that sensitivity is high, stability is good, preparation method technique is simple, easy to operate, without large-scale instrument and equipment, into
This low performance is good, with good practical extending application value.
2. the pollution-free nontoxicity of hydrogen peroxide sensor prepared by the present invention, mild condition is simple to operate, it is to avoid tradition
The manganese dioxide nanowire load of the noble metal of costliness, carbon composite load, and weak catalytic activity, sea urchin shape manganese dioxide
The hydrogen peroxide sensor of load can stably, efficiently carry out the hydrogen peroxide detection of low concentration, favorable repeatability.This is to mistake
The detection of hydrogen oxide will be widely used in the numerous areas such as food medical treatment, environmental pollution monitoring with very big researching value.
Brief description of the drawings
Fig. 1 is the schematic flow sheet that the present invention builds hydrogen peroxide sensor.
Fig. 2 is the electron scanning micrograph of the sea urchin shape manganese dioxide prepared in embodiment 1.
Fig. 3 is the scanning electron of sea urchin shape manganese dioxide in the manganese dioxide nanowire and embodiment 1 prepared in comparative example 1
Microphotograph.
Fig. 4 is the hydrogen peroxide sensor that builds of manganese dioxide nanowire and sea urchin shape manganese dioxide to 1mmol/L H2O2
Cyclic voltammetry curve.
Fig. 5 is the hydrogen peroxide sensor that builds of manganese dioxide nanowire and sea urchin shape manganese dioxide to H2O2When m- electricity
Stream response comparison diagram.
Embodiment
Present disclosure is further illustrated with reference to specific embodiment, but be should not be construed as limiting the invention.
Unless otherwise specified, the conventional meanses that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, the reagent of the invention used, method and apparatus is the art conventional reagent, methods and apparatus.
In following embodiment 1-5 and comparative example 1：
The raw material are all that analysis is pure, purchased from Guangzhou Chemical Reagent Factory.
Using JEOL JSM-7001F field emission microscopes under 15.0kV accelerating potential to prepared dioxy
Change manganese nano wire and sea urchin shape manganese dioxide is characterized.
Electro-chemical test is carried out to prepared new hydrogen peroxide sensor using Zahner electrochemical workstations.
Fig. 1 prepares the schematic flow sheet of hydrogen peroxide sensor for the present invention.Based on the flow chart, below in conjunction with specific reality
Apply example that technical solution of the present invention is further described.
Embodiment 1
1. 0.17g manganese sulfates, 0.17g potassium peroxydisulfates, 0.51g potassium sulfates are added to polytetrafluoroethylene (PTFE) hydrothermal reaction kettle
In, 15mL deionized waters are added, magnetic rotor is put into, reactor is positioned on magnetic stirring apparatus and stirred 30 minutes, it is rear to add
The 0.5mL concentrated sulfuric acids, are suctioned out rotor using magnet, after inner bag is positioned in reactor, reactor are positioned over 140 DEG C of perseverance
6 hours in warm baking oven.Products therefrom is added in centrifuge tube, stand 20 minutes, after suck supernatant liquor.Add deionized water or
Ethanol, is centrifuged 10 minutes with 5000 revs/min, supernatant liquor is sucked after centrifugation.The above-mentioned centrifugal process of repetition 3 times, will be produced
Thing is placed in 80 DEG C of baking ovens and dried 12 hours, obtains sea urchin shape manganese dioxide；
2. weighing manganese dioxide 1mg to add in centrifuge tube, 500 μ L deionized water, 500 μ L absolute ethyl alcohol and 50 is added
μ L 5% Nafion, ultrasound 30 minutes, obtains slurries.Draw 20 μ L glass carbon of the mixed serum drop coating in a diameter of 1.5cm
Electrode surface, natural drying.
3. by above-mentioned glass-carbon electrode and the reference electrode Ag/AgCl electrodes for including 3mol/LKCl solution, specification be 1cm ×
1cm platinized platinum is connected to electrode with three-electrode system, and electrolyte is 200mL phosphate buffer solutions (pH=7), is constituted a kind of new
Hydrogen peroxide sensor.
Embodiment 2
1. 0.17g manganese sulfates, 0.17g potassium peroxydisulfates, 0.34g potassium sulfates are added to polytetrafluoroethylene (PTFE) hydrothermal reaction kettle
In, 15mL deionized waters are added, magnetic rotor is put into, reactor is positioned on magnetic stirring apparatus and stirred 50 minutes, it is rear to add
The 0.5mL concentrated sulfuric acids, are suctioned out rotor using magnet, after inner bag is positioned in reactor, reactor are positioned over 160 DEG C of perseverance
Reacted 8 hours in warm baking oven.Products therefrom is added in centrifuge tube, stand 20 minutes, after suck supernatant liquor.Add deionization
Water or ethanol, are centrifuged 5 minutes with 6000 revs/min, supernatant liquor are sucked after centrifugation.The above-mentioned centrifugal process of repetition 2 times, will
Product is placed in 60 DEG C of baking ovens and dried 24 hours, obtains sea urchin shape manganese dioxide；
2. weighing manganese dioxide 1mg to add in centrifuge tube, 500 μ L deionized water, 500 μ L absolute ethyl alcohol and 50 is added
μ L Nafion, ultrasound 50 minutes, obtains slurries.Mixed serum drop coating is drawn in a diameter of 2cm glassy carbon electrode surface, it is natural
Drying.
3. by above-mentioned glass-carbon electrode and the reference electrode Ag/AgCl electrodes for including 4mol/LKCl solution, specification be 1cm ×
1cm platinized platinum is connected to electrode with three-electrode system, and electrolyte is 150mL phosphate buffer solutions (pH=7), is constituted a kind of new
Hydrogen peroxide sensor.
Embodiment 3
1. 0.17g manganese sulfates, 0.17g potassium peroxydisulfates, 0.68g potassium sulfates are added to polytetrafluoroethylene (PTFE) hydrothermal reaction kettle
In, 25mL deionized waters are added, magnetic rotor is put into, reactor is positioned on magnetic stirring apparatus and stirred 30 minutes, it is rear to add
The 2mL concentrated sulfuric acids, are suctioned out rotor using magnet, after inner bag is positioned in reactor, reactor are positioned over 140 DEG C of constant temperature
6 hours in baking oven.Products therefrom is added in centrifuge tube, stand 20 minutes, after suck supernatant liquor.Add deionized water or second
Alcohol, is centrifuged 10 minutes with 4000 revs/min, supernatant liquor is sucked after centrifugation.The above-mentioned centrifugal process of repetition 3 times, by product
It is placed in 80 DEG C of baking ovens and dries 12 hours, obtains sea urchin shape manganese dioxide；
2. weigh manganese dioxide 1.5mg to add in centrifuge tube, add 500 μ L deionized water, 500 μ L absolute ethyl alcohol and
100 μ L Nafion, ultrasound 30 minutes, obtains slurries.Mixed serum drop coating is drawn in a diameter of 1.5cm glass-carbon electrode table
Face, natural drying.
3. by above-mentioned glass-carbon electrode and the reference electrode Ag/AgCl electrodes for including 3mol/LKCl solution, specification is 0.5cm
× 0.5cm platinized platinum is connected to electrode with three-electrode system, and electrolyte is 200mL phosphate buffer solutions (pH=7), is constituted a kind of
New hydrogen peroxide sensor.
Comparative example 1
The step of preparing manganese dioxide nanowire hydrogen peroxide sensor is as follows:
1. 0.25g potassium permanganate, 0.11 manganese sulfate are added in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, add 15mL go from
Sub- water, is put into magnetic rotor, and reactor is positioned on magnetic stirring apparatus and stirred 30 minutes, rotor is suctioned out using magnet, will
After inner bag is positioned in reactor, reactor is positioned in 160 DEG C of constant temperature oven 24 hours.Products therefrom is added to centrifugation
Guan Zhong, stand 20 minutes, after suck supernatant liquor.Deionized water or ethanol are added, is centrifuged 10 minutes with 5000 revs/min, from
Supernatant liquor is sucked after heart separation.The above-mentioned centrifugal process of repetition 3 times, product is placed in 80 DEG C of baking ovens and dried 12 hours, is obtained
Sea urchin shape manganese dioxide；
2. weighing manganese dioxide 1mg to add in centrifuge tube, 500 μ L deionized water, 500 μ L absolute ethyl alcohol and 50 is added
μ L Nafion, ultrasound 30 minutes, obtains slurries.20 μ L mixed serum drop coating is drawn in a diameter of 1.5cm glass-carbon electrode
Surface, natural drying.
3. by above-mentioned glass-carbon electrode and the reference electrode Ag/AgCl electrodes for including 3mol/LKCl solution, specification be 1cm ×
1cm platinized platinum is connected to electrode with three-electrode system, and electrolyte is 200mL phosphate buffer solutions (pH=7), is constituted a kind of new
Hydrogen peroxide sensor.
Fig. 2 is sea urchin shape manganese dioxide electron scanning micrograph.Wherein, Fig. 2 (a) is sea urchin shape manganese dioxide, Fig. 2
(b) for sea urchin shape manganese dioxide partial enlarged drawing electron scanning micrograph.As can be seen that sea urchin shape two from Fig. 2 a
Manganese oxide pattern is complete and is evenly distributed, and can be seen that manganese dioxide from Fig. 2 b is the three-dimensional knot by nanotubes self-assemble
Structure, illustrates that by this method the sea urchin shape manganese dioxide that growth is uniform, pattern is complete can be prepared.
Manganese dioxide nanowire and the electron scanning micrograph of sea urchin shape manganese dioxide that Fig. 3 is.Wherein.Fig. 3 (a)
The manganese dioxide nanowire prepared for comparative example 1, Fig. 3 (b) is sea urchin shape manganese dioxide prepared by embodiment 1.As can be seen that institute
The manganese dioxide nanowire prepared not only grows inequality, is interspersed, and sea urchin shape manganese dioxide size uniformity, distribution are
It is even.
Embodiment 4
The present invention is with sea urchin shape manganese dioxide prepared by embodiment 1-3 and comparative example 1 and manganese dioxide nanowire peroxidating
Hydrogen sensor carries out H2O2Detection.Fig. 4 is the hydrogen peroxide sensor pair that manganese dioxide nanowire and sea urchin shape manganese dioxide are built
1mmol/LH2O2Cyclic voltammetry curve.(a) is the hydrogen peroxide sensor of manganese dioxide nanowire structure to 1mmol/ in Fig. 4
LH2O2Cyclic voltammetric response curve, (b) be sea urchin shape manganese dioxide build hydrogen peroxide sensor to 1mmol/L H2O2
Cyclic voltammetric response curve.From fig. 4, it can be seen that two kinds of hydrogen peroxide sensors are all to H2O2Produce current-responsive, titanium dioxide
Manganese hydrogen peroxide sensor is to 1mmol/LH2O2Response effect, comprise the following steps that：
1. each electrode is accordingly connected with electrochemical workstation by hydrogen peroxide sensor, volt-ampere test is started the cycle over, is swept
Retouch speed and be set as 250mV/s, the scanning number of turns 20 is enclosed；
2. after magnetic rotor is added into system, be positioned on magnetic stirring apparatus, stirred with 300 revs/min of speed, together
When the μ L of 30% hydrogenperoxide steam generator 20 are added dropwise, after 2 minutes stop stirring；
3. sweep speed is set as into 50mV/s, the scanning number of turns 1 is enclosed, and is started the cycle over volt-ampere test, is obtained CV curves.
Embodiment 5
The present invention is with the sea urchin shape manganese dioxide prepared by embodiment 1-3 and comparative example 1 and manganese dioxide nanowire peroxide
Change hydrogen sensor and carry out H2O2Detection, the time current curve that various concentrations hydrogen peroxide is added dropwise.Hydrogen peroxide sensor pair
H2O2When m- current-responsive, comprise the following steps that：
1. each electrode is accordingly connected with electrochemical workstation by hydrogen peroxide sensor, volt-ampere test is started the cycle over, is swept
Retouch speed and be set as 250mV/s, the scanning number of turns 20 is enclosed；
2. after magnetic rotor is added into system, be positioned on magnetic stirring apparatus, stirred with 300 revs/min of speed, will
When m- testing current constant potential be set to -0.8V, the time is set as starting within 2000 seconds test；
3. adding the hydrogenperoxide steam generator of various concentrations into system, ladder response curve is obtained.
As a result show, with the sea urchin shape manganese dioxide hydrogen peroxide sensor prepared by embodiment 1-3 to hydrogen peroxide
Detection results are clearly more powerful.Meanwhile, the present invention is with the sea urchin shape of the manganese dioxide nanowire prepared by comparative example 1 and embodiment 1
Manganese dioxide is carried out to H2O2Detect the comparison of response.Fig. 4 is the peroxide that manganese dioxide nanowire and sea urchin shape manganese dioxide are built
Change hydrogen sensor to 1mmol/LH2O2Cyclic voltammetry curve.As can be seen from Figure 4, sea urchin shape manganese dioxide hydrogen peroxide sensor pair
The peak point current of hydrogen peroxide response is 1.3 times of manganese dioxide nanowire, so that the sea urchin shape manganese dioxide hydrogen peroxide obtained
Sensor has more excellent electrochemical response.Fig. 5 is the hydrogen peroxide that manganese dioxide nanowire and sea urchin shape manganese dioxide are built
Sensor is to H2O2When m- current-responsive comparison diagram.Wherein, Fig. 5 (A) is that the hydrogen peroxide that manganese dioxide nanowire is built is passed
Sensor is to H2O2When m- electric current ladder response curve, Fig. 5 (B) be sea urchin shape manganese dioxide build hydrogen peroxide sensor pair
H2O2When m- electric current ladder response curve.From figure 5 it can be seen that under constant voltage -0.8V, being continuously added a certain amount of
H2O2Solution, response current is consequently increased, and can reach that electric current is stable in 5s.Pass through interpolation concentration-current correction figure
Understand, sea urchin shape manganese dioxide hydrogen peroxide sensor has higher sensitivity and smaller minimum detection limit, is conducive to
Carry out the detection of hydrogen peroxide.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, is combined and simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of hydrogen peroxide sensor, it is characterised in that comprise the following steps：
S1. will potassium peroxydisulfate, manganese sulfate and potassium sulfate mix after add deionized water, stir and the concentrated sulfuric acid be added dropwise, be placed in 140~
160 DEG C of reactions；
S2. step S1 products therefroms are stood, sucks supernatant liquor, added deionized water or ethanol is centrifuged, inhaled after separation
Remove supernatant liquor；
S3. centrifuged 2~3 times described in repeat step S2, product is dried into 12~24h at 60~80 DEG C, sea urchin shape two is obtained
Manganese oxide；
S4. sea urchin shape manganese dioxide is added in ethanol, water and Nafion solution, 30~50min of ultrasound, obtains manganese dioxide slurry
Liquid；
S5. manganese dioxide slurries are applied to glassy carbon electrode surface, natural drying obtains working electrode；
S6. by working electrode, reference electrode and electrode is connected with three-electrode system, be put into electrolyte, constitute hydrogen peroxide
Sensor.
2. the preparation method of hydrogen peroxide sensor according to claim 1, it is characterised in that persulfuric acid described in step S1
The mass ratio of potassium, manganese sulfate and potassium sulfate is (1~2):(1~2):(3~4)；The potassium peroxydisulfate, manganese sulfate and potassium sulfate
The mass volume ratio of gross mass and deionized water is (50~80):The volume ratio of 1mg/mL, the deionized water and the concentrated sulfuric acid is
(30~50):1.
3. the preparation method of hydrogen peroxide sensor according to claim 1, it is characterised in that stirred described in step S1
Time is 30~50min, and the time of the reaction is 6~8h.
4. the preparation method of hydrogen peroxide sensor according to claim 1, it is characterised in that stood described in step S2
Time is 20~30min, and the speed of the centrifugation is 4000~6000r/min, and the time of the centrifugation is 5~10min.
5. the preparation method of hydrogen peroxide sensor according to claim 1, it is characterised in that sea urchin shape described in step S4
The quality cumulative volume ratio of manganese dioxide and second alcohol and water is (1~1.5):1mg/mL, the volume ratio of the ethanol, water and Nafion
For (1~10):(1~10):(1~2).
6. the preparation method of hydrogen peroxide sensor according to claim 1, it is characterised in that the electricity of glass carbon described in step S5
A diameter of 1.5~2cm of pole.
7. the preparation method of hydrogen peroxide sensor according to claim 1, it is characterised in that the electricity of reference described in step S6
Extremely Ag/AgCl electrodes, described is platinized platinum to electrode, and the electrolyte is PBS solution, the pH=7 of the PBS solution.
8. the preparation method of hydrogen peroxide sensor according to claim 7, it is characterised in that the Ag/AgCl electrodes
Electrolyte is KCl solution, and the concentration of the KCl solution is 3~4mol/L, the specification of the platinized platinum for (0.5~1) × (0.5~
1)cm×cm。
9. the hydrogen peroxide sensor prepared according to any one of claim 1-8 methods described.
10. application of the hydrogen peroxide sensor described in claim 9 in food medical treatment, environmental pollution monitoring field.
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