CN107271517A - A kind of sweat lactic acid device for fast detecting - Google Patents
A kind of sweat lactic acid device for fast detecting Download PDFInfo
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- CN107271517A CN107271517A CN201710534484.1A CN201710534484A CN107271517A CN 107271517 A CN107271517 A CN 107271517A CN 201710534484 A CN201710534484 A CN 201710534484A CN 107271517 A CN107271517 A CN 107271517A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3271—Amperometric enzyme electrodes for analytes in body fluids, e.g. glucose in blood
- G01N27/3272—Test elements therefor, i.e. disposable laminated substrates with electrodes, reagent and channels
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3277—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction being a redox reaction, e.g. detection by cyclic voltammetry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3278—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction involving nanosized elements, e.g. nanogaps or nanoparticles
Abstract
The present invention relates to technical field of medical detection, more particularly to a kind of sweat lactic acid device for fast detecting, including flexible substrate layer, electrode layer, separation layer and electronic monitoring layer, flexible substrate layer is made up of porous flexible material, electrode layer is included to electrode, working electrode, reference electrode and reaction chamber, working electrode includes the second carbon paste wire, carbon paste electrode III and reaction electrode, and reaction electrode includes oxidation enzyme layer and three-dimensional graphene composite material layer, and three-dimensional graphene composite material is by nano-TiO2It is dispersed on graphene and is made, three-dimensional graphene composite material layer has tiny balloon network structure, and pore-size distribution is in 20nm~40nm, specific surface area 1500m2/ g~1650m2/ g, separation layer is pasted on the insulating layer, and electronic monitoring layer includes voltage control unit, current measuring unit and data preparation unit.The detection means of the present invention is without taking a blood sample, sustainable monitor and detection human body lactic acid production, and higher with detection sensitivity, stability is stronger, the features such as easy to carry.
Description
Technical field
The present invention relates to technical field of medical detection, more particularly to a kind of sweat lactic acid device for fast detecting.
Background technology
Fatigue is a kind of extremely complex physiology and psychological phenomena, and it is not by single, clear and definite factors composition, at present
Also there is very big difference to the definition of fatigue.In general, fatigue is the result of work, is labourer in one section of continuous work
Between after, because the nervous mental or physical exertion of long-term causes the function of whole body to reduce.From biomedicine in theory
Say, work is the process of energy expenditure, this process continues to a certain extent, and central nervous system will produce inhibitory action, after
It is exactly the fatigue of allocinesis nervous system after central nervous system fatigue, reflects the sensitivity reduction of action, operating efficiency
Decline.In long-time intensity movements, muscle is in constant motion, then constantly consumed energy and fat, accelerates human body fluid
Circulation and metabolic process, now, blood can not supply oxygen to muscle fast enough, it is impossible to meet the high-energy need of contraction of muscle
Ask, once available oxygen depletion, the muscle in motion will ferment generation lactic acid, while can also discharge a large amount of sweat by sweat gland
Liquid, is that body radiates and maintenance body thermal balance by sweat evaporation.
Once the lactic acid produced in analysis detection, motion process described in many documents, small part have been carried out to sweat composition
It can be discharged with sweat, and with the extension of run duration, concentration ratio of the lactic acid in sweat is bigger.In addition, extensive and profound in meaning Buddhist nun
Theory based on biomethanics has made further analysis, due to that can produce liquid after lactic acidosis, is trapped in musculature
Do not taken away by blood, make muscle swelling, and then oppress blood vessel between muscle so that muscle blood supply is not enough all the more.If living in anxiety
After dynamic, it can rest in time, liquid will be pulled away；If rest is insufficient, continuation activity can promote liquid to increase again.If
Fluid accumulation between a certain piece of muscle, muscle is persistently used excessively to make muscle swelling serious in a period of time, result is intramuscular
The formation of fibrous matter, this will influence the normal contraction of muscle, or even cause permanent damage.7 phases in 2014《Teach in Qinghai
Educate》One entitled " lactic acid accumulation causes mechanism and the elimination of fatigue " has been published, wherein, describe and " carrying out strenuous exercise
When, because lactic acid accumulation causes pH value of human body to decline in myocyte, the activity of enzyme receives suppression, so as to cause glycolysis and fat
Metabolism slows down or interrupted, and energy supplying system is destroyed, and produces fatigue ".It therefore, it can analyze the tired journey of judgement by detecting lactic acid
In order to judge the internal lactic acid metabolism state of personalization in degree, sporting world's (sports medical science), science selects physical culture and sports personnel, can be in fortune
Many sampling site intermittent Plasma lactates are carried out in dynamic, important evidence is provided for scientific and reasonable strength training.
At present, what the assay method of lactic acid was conventional has chemical method and enzyme process, and chemical method accuracy is poor, trivial operations, inspection
Survey less efficient；Enzyme process has dehydrogenation enzyme process and enzymatic measurement, and dehydrogenation enzyme process includes the colorimetric of ultraviolet method and coupling tetrazolium again
Method, there is also problems, such as while lactic acid being oxidized into pyruvic acid with lactic dehydrogenase NAD be reduced into NADH, it is necessary to
Coupling ALT and glutamic acid remove substrate pyruvate to accelerate reaction, or coupling PMS and NBT colorimetric estimations, but react endless
Point, it is more difficult to judge；Enzymatic measurement sensitivity is higher, and accuracy is also higher, but this method is to need large-scale blood the problem of exist
The special device such as liquid Biochemical Analyzer or ultraviolet specrophotometer, it is necessary to gather finger tip hematometry lactic acid content, equipment cost compared with
Height, detection time is longer, and pain can be also brought to tester, and detection is extremely inconvenient, it is impossible to which meeting people, detection is internal immediately
The demand of lactic acid content change.
The content of the invention
In view of this, it is an object of the invention to provide a kind of sweat lactic acid device for fast detecting, it is sustainable without blood sampling
Monitor and detection human body lactic acid production, higher with detection sensitivity, stability is stronger, the features such as easy to carry.
The present invention solves above-mentioned technical problem by following technological means：
A kind of sweat lactic acid device for fast detecting, including set gradually from top to bottom flexible substrate layer, electrode layer, isolation
Layer and electronic monitoring layer, the flexible substrate layer are made up of porous flexible material；The electrode layer is included to electrode, work electricity
Pole, reference electrode and reaction chamber, the first carbon paste wire, carbon paste electrode I and the carbon paste electrode for including being sequentially connected to electrode
II, the working electrode includes the second carbon paste wire, carbon paste electrode III and the reaction electrode being sequentially connected, the reaction electrode bag
The three-dimensional graphene composite material layer for including oxidation enzyme layer and being attached in oxidation enzyme layer, the reference electrode includes the silver being sequentially connected
Wire, silver/silver chloride electrode I and silver/silver chloride electrode II, the carbon paste electrode II, reaction electrode and silver/silver chloride electrode II
In reaction chamber, the reaction chamber is externally provided with insulating barrier, the insulating barrier covering carbon paste electrode I, carbon paste electrode III and silver/chlorine
Change silver electrode I；The separation layer is pasted on the insulating layer, and the electronic monitoring layer, which is arranged on separation layer, to be used to monitor electrode layer
Reactions change.
Further, the electronic monitoring layer is including the voltage control unit for control electrode layer voltage, for measuring electricity
Pole layer electric current current measuring unit and for data acquisition, conversion, store data preparation unit.Further, the oxidation
Contain LO, citric acid, chitosan and carboxymethyl cellulose in enzyme layer.
Further, LO, citric acid, chitosan and the carboxymethyl cellulose weight ratio in the oxidation enzyme layer are
8:0.3:0.5:1.2。
Further, the three-dimensional graphene composite material is by nano-TiO2It is dispersed on graphene and is made, it is described
Three-dimensional graphene composite material layer has tiny balloon network structure, and pore-size distribution is in 20nm~40nm, specific surface area 1500m2/
G~1650m2/g。
Further, the preparation method of the three-dimensional graphene composite material is as follows：
The preparation of graphene, using sargassum as raw material, segment is cleaned, and is dried, after air-flow crushing to micron grain size, by powder
Broken sargassum adds (C2H302)2In Ni solution, 9h is stirred, filter residue is dried after filtering, added after the uniform mixing of activator,
Add under deionized water ultrasound 5min~8min of 1.2 times of volumes, normal temperature and impregnate after 13h~15h, be filtered under diminished pressure drying and obtain
Residue, by residue be placed in baking oven dry after, crushing be transferred in horizontal pipe furnace, be passed through argon gas, be to slowly warm up to 860 DEG C~
950 DEG C of 1.0~1.5h of calcining, are cooled to after normal temperature, add in acid solution and clean, add in ethanol or deionized water and clean,
Drying obtains the graphene with porous three-dimensional structure.
The preparation of three-dimensional graphene composite material, weighs nano-TiO2It is dissolved in deionized water, being configured to mass concentration is
0.2g/mL~0.3g/mL solution, weighs graphene and adds in solution, stir and evenly mix, ultrasonic disperse obtains dispersion liquid, be transferred to
Into reactor, reactor is placed in hydro-thermal reaction 32h under 180 DEG C of water-baths, reaction solution is obtained, it is laggard that reaction solution is cooled to normal temperature
Row decompression suction filtration, filter residue is washed with absolute ethyl alcohol, after the filter residue drying after washing, is transferred into Muffle furnace in 550 DEG C~800
DEG C calcining 3h~5h, obtain inter-adhesive around the three-dimensional grapheme with tiny balloon network structure formed by nano particle
Composite.
Further, in the graphene preparation process by dried sargassum air-flow crushing to 80 μm~150 μm.
Further, the activator in the graphene preparation process is one kind in sodium carbonate, sodium hydroxide, potassium carbonate.
Further, the acid solution in the graphene preparation process is one kind in hydrochloric acid, nitric acid, phosphoric acid.Further, institute
State the nano-TiO weighed in three-dimensional graphene composite material preparation process2Weight ratio with graphene is 1:7~1:9.
The sweat lactic acid device for fast detecting of the present invention employs flexible substrate, and tensility is strong, and suitable wearing can be right
The lactic acid that human motion is produced in real time, accurately detect.When human body has sweat to flow through lactic acid device for fast detecting, sweat
In lactic acid be oxidized LO oxidation in enzyme layer, occur redox reaction so as to changing size of current, three-dimensional stone
Black alkene composite layer serves as the conducting element of the redox center of electrode surface and LO, realizes electronics biography
Pass so that electrode layer is able to detect that the change of electric current, and calculates corresponding lactic acid content by electronic measuring device arrangement, real
Now to real-time, the accurate detection of human body lactic acid.The lactic acid device for fast detecting is detected and need not taken a blood sample during lactic acid, it is to avoid blood sampling is caused
Wound, stability is stronger, can be achieved to continue the purpose of monitor and detection human body lactic acid production.
The present invention sweat lactic acid device for fast detecting in oxidation enzyme layer in citric acid as LO increasing
Agent living, is conducive to improving the sensitivity of the detection means lactate detection；Chitosan can as LO live keeping agent, with
Extend the service life of the detection means, while chitosan has suction-operated to lactic acid, the sensitivity of detection is improved again；
Carboxymethyl cellulose is hydrophilic high mol, the hydration permeability of oxidation enzyme layer can be effectively improved with reference to chitosan, further
Improve detection rates and sensitivity.
The sweat lactic acid device for fast detecting of the present invention employs three-dimensional graphene composite material modified electrode, graphene tool
There are the design feature and good electron mobility of uniqueness, it is mixed with nano titanium oxide passes through ultrasonic disperse, hydro-thermal reaction,
After calcining, titanium dioxide nanoparticle is dispersed on graphene, with abundant three-dimensional conductive network structure and huge
Specific surface area, can delicately detect rapidly the electronic variable of redox reaction generation, effectively improve sweat breast
The sensitivity and real-time of sour device for fast detecting.
Brief description of the drawings
Fig. 1 is a kind of structural representation of sweat lactic acid device for fast detecting of the invention；
Fig. 2 is the structural representation of electrode layer in a kind of sweat lactic acid device for fast detecting of the invention；
Wherein, flexible substrate layer 1, electrode layer 2, to electrode 21, the first carbon paste wire 211, carbon paste electrode I 212, carbon paste electricity
Pole II 213, working electrode 22, the second carbon paste wire 221, carbon paste electrode III 222, reaction electrode 223, reference electrode 23, silver are led
Line 231, silver/silver chloride electrode I 232, silver/silver chloride electrode II 233, reaction chamber 24, separation layer 3, electronic monitoring layer 4, voltage
Control unit 41, current measuring unit 42, data preparation unit 43, insulating barrier 5.
Embodiment
Below with reference to the drawings and specific embodiments, the present invention is described in detail：
As depicted in figs. 1 and 2, a kind of sweat lactic acid device for fast detecting of the invention, including set gradually from top to bottom
Flexible substrate layer 1, electrode layer 2, separation layer 3 and electronic monitoring layer 4, flexible substrate layer 1 is made up of porous flexible material；Electrode
Layer 2 is included to electrode 21, working electrode 22, reference electrode 23 and reaction chamber 24, the first carbon for including being sequentially connected to electrode 21
Wire 211, carbon paste electrode I 212 and carbon paste electrode II 213 are pasted, working electrode 22 includes the second carbon paste wire being sequentially connected
221st, carbon paste electrode III 222 and reaction electrode 223, the three-dimensional that reaction electrode 223 includes oxidation enzyme layer and is attached in oxidation enzyme layer
Graphene composite material layer, reference electrode 23 includes silver wire 231, silver/silver chloride electrode I 232 and the silver/chlorination being sequentially connected
Silver electrode II 233, carbon paste electrode II 213, reaction electrode 223 and silver/silver chloride electrode II 233 are located in reaction chamber 24, reaction
Chamber 24 is externally provided with insulating barrier 5, the covering of insulating barrier 5 carbon paste electrode I 212, carbon paste electrode III 222 and silver/silver chloride electrode I 232；Every
Absciss layer 3 is pasted onto on insulating barrier 5, and electronic monitoring layer 4, which is arranged on, is used for the reactions change for monitoring electrode layer 2 on separation layer 3.
Wherein, electronic monitoring layer 4 is including the voltage control unit 41 for the voltage of control electrode layer 2, for measuring electrode
Layer 2 electric current current measuring unit 42 and for data acquisition, conversion, store data preparation unit 43.Pass through electronic monitoring
Layer 4 can monitor lactic acid content in real time.
Aoxidize and contain LO, citric acid, chitosan and carboxymethyl cellulose in enzyme layer, the lactic acid in oxidation enzyme layer
Oxidizing ferment, citric acid, chitosan and carboxymethyl cellulose weight ratio are 8:0.3:0.5:1.2.Citric acid is used as LO
Activity increase agent, be conducive to improve the detection means lactate detection sensitivity；Chitosan can as LO keep-alive
Agent, to extend the service life of the detection means, can further improve the sensitivity of detection again；Carboxymethyl cellulose is hydrophilic
Macromolecule, the hydration permeability of oxidation enzyme layer can be effectively improved with reference to chitosan, further improve detection rates and sensitive
Degree.
Three-dimensional graphene composite material is by nano-TiO2It is dispersed on graphene and is made, graphene is with sargassum
For solid-phase carbon source, it is made by chemical activation and high-temperature calcination, for the graphene with porous three-dimensional structure, on the graphene
Ultrasonic disperse nano-TiO2, carry out after hydro-thermal reaction, calcining obtains inter-adhesive around being formed with hollow by nano particle
The three-dimensional graphene composite material of microballoon network structure, its pore-size distribution is in 20nm~40nm, specific surface area 1500m2/ g~
1650m2/g.When human body has sweat to flow through lactic acid device for fast detecting, the lactic acid in sweat is oxidized the lactic acid oxygen in enzyme layer
Change oxydasis, occur redox reaction to change size of current, three-dimensional graphene composite material serves as electrode surface and breast
The conducting element of the redox center of acid oxidase, realizes electron transmission so that electrode layer is able to detect that the change of electric current
Change, and corresponding lactic acid content is calculated by electronic measuring device arrangement, realize real-time, the accurate detection to human body lactic acid.Should
Lactic acid device for fast detecting is detected and need not taken a blood sample during lactic acid, it is to avoid the wound that blood sampling is caused, stability is stronger, and lasting supervise can be achieved
The purpose of control detection human body lactic acid production.
Three-dimensional graphene composite material prepares embodiment one
Sargassum is cut into segment, after soaking and washing is clean repeatedly, is dried under reduced pressure to water content below 5%, by gas
Stream is crushed to after 80 μm~150 μm of micron grain size；The concentration for weighing the sargassum addition 1L of 50g crushing is 0.5mol/L's
(C2H302)2In Ni solution, 9h is stirred at room temperature, filter residue is dried in filtering, add after the uniform mixing of activator sodium carbonate, then add
Enter the deionized water ultrasound 5min of 1.2 times of volumes, in being impregnated under normal temperature after 15h, be filtered under diminished pressure drying and obtain residue；Residue is put
Enter in horizontal pipe furnace, be passed through argon gas, 860 DEG C of calcining 1.5h are to slowly warm up to the speed of 10 DEG C of heating per minute, cooling takes
Go out；Add in hydrochloric acid solution and clean, add in ethanol and clean, drying obtains graphene.
Weigh 5g nano-TiOs2It is dissolved in deionized water, is configured to the solution that mass concentration is 0.2g/mL, weighs 35g stones
Black alkene is added in solution, is stirred and evenly mixed, under conditions of frequency 20kHz, power 100w, ultrasonic disperse 0.5h obtains dispersion liquid,
It is transferred in reactor, reactor is placed in hydro-thermal reaction 32h under 180 DEG C of water-baths, reaction solution is obtained, reaction solution is cooled to normal temperature
Decompression suction filtration is carried out afterwards, filter residue is washed with absolute ethyl alcohol, after the filter residue drying after washing, is transferred into Muffle furnace in 550 DEG C
3h is calcined, three-dimensional graphene composite material is obtained.
The graphene of the present embodiment is carried out to full scan Electron microscopy and transmission electron microscope detection, hair respectively
Now the graphene has sheet porous three-dimensional network structure, and each lamella includes number layer graphene, is cross-linked with each other to form three-dimensional
Network structure.The three-dimensional graphene composite material that the present embodiment is prepared carries out full scan Electron microscopy and transmission
Electron microscopy, it is inter-adhesive around the porous baseball formed by nano particle to find the three-dimensional graphene composite material
Shape structure, using conventional aperture and the measuring method of specific surface area, measures the three-dimensional meso-hole graphene that the present embodiment is prepared
Pore-size distribution in 20nm~60nm, specific surface area is 1500m2/g。
Three-dimensional graphene composite material prepares embodiment two
Sargassum is cut into segment, after soaking and washing is clean repeatedly, is dried under reduced pressure to water content below 5%, by gas
Stream is crushed to after 80 μm~150 μm of micron grain size；The concentration for weighing the sargassum addition 0.8L of 40g crushing is 0.5mol/L's
(C2H302)2In Ni solution, 9h is stirred at room temperature, filter residue is dried in filtering, add after the uniform mixing of activator sodium hydroxide, then
The deionized water ultrasound 6min of 1.2 times of volumes is added, in being impregnated under normal temperature after 14h, drying is filtered under diminished pressure and obtains residue；By residue
It is put into horizontal pipe furnace, is passed through argon gas, 950 DEG C of calcining 1.0h, cooling is to slowly warm up to the speed of 10 DEG C of heating per minute
Take out；Add in salpeter solution and clean, add in deionized water and clean, drying obtains graphene.
Weigh 4g nano-TiOs2It is dissolved in deionized water, is configured to the solution that mass concentration is 0.25g/mL, weighs 32g stones
Black alkene is added in solution, is stirred and evenly mixed, under conditions of frequency 25kHz, power 100w, ultrasonic disperse 0.6h obtains dispersion liquid,
It is transferred in reactor, reactor is placed in hydro-thermal reaction 32h under 180 DEG C of water-baths, reaction solution is obtained, reaction solution is cooled to normal temperature
Decompression suction filtration is carried out afterwards, filter residue is washed with absolute ethyl alcohol, after the filter residue drying after washing, is transferred into Muffle furnace in 700 DEG C
5h is calcined, three-dimensional graphene composite material is obtained.
The graphene of the present embodiment is carried out to full scan Electron microscopy and transmission electron microscope detection, hair respectively
Now the graphene has sheet porous three-dimensional network structure, and each lamella includes number layer graphene, is cross-linked with each other to form three-dimensional
Network structure.The three-dimensional graphene composite material that the present embodiment is prepared carries out full scan Electron microscopy and transmission
Electron microscopy, it is inter-adhesive around the hollow baseball formed by nano particle to find the three-dimensional graphene composite material
The mixture of shape structure and tiny balloon shape structure, using conventional aperture and the measuring method of specific surface area, measures the present embodiment
The pore-size distribution of the three-dimensional meso-hole graphene prepared is in 20nm~50nm, and specific surface area is 1580m2/g。
Three-dimensional graphene composite material prepares embodiment three
Sargassum is cut into segment, after soaking and washing is clean repeatedly, is dried under reduced pressure to water content below 5%, by gas
Stream is crushed to after 80 μm~150 μm of micron grain size；The concentration for weighing the sargassum addition 1.2L of 60g crushing is 0.5mol/L's
(C2H302)2In Ni solution, 9h is stirred at room temperature, filter residue is dried in filtering, add after the uniform mixing of activator potassium carbonate, then add
Enter the deionized water ultrasound 8min of 1.2 times of volumes, in being impregnated under normal temperature after 13h, be filtered under diminished pressure drying and obtain residue；Residue is put
Enter in horizontal pipe furnace, be passed through argon gas, 900 DEG C of calcining 1.3h are to slowly warm up to the speed of 8 DEG C of heating per minute, cooling takes
Go out；Add in phosphoric acid solution and clean, add in deionized water and clean, drying obtains graphene.
Weigh 4g nano-TiOs2It is dissolved in deionized water, is configured to the solution that mass concentration is 0.3g/mL, weighs 36g stones
Black alkene is added in solution, is stirred and evenly mixed, under conditions of frequency 30kHz, power 100w, ultrasonic disperse 0.6h obtains dispersion liquid,
It is transferred in reactor, reactor is placed in hydro-thermal reaction 32h under 180 DEG C of water-baths, reaction solution is obtained, reaction solution is cooled to normal temperature
Decompression suction filtration is carried out afterwards, filter residue is washed with absolute ethyl alcohol, after the filter residue drying after washing, is transferred into Muffle furnace in 800 DEG C
4h is calcined, three-dimensional graphene composite material is obtained.
The graphene of the present embodiment is carried out to full scan Electron microscopy and transmission electron microscope detection, hair respectively
Now the graphene has sheet porous three-dimensional network structure, and each lamella includes number layer graphene, is cross-linked with each other to form three-dimensional
Network structure.The three-dimensional graphene composite material that the present embodiment is prepared carries out full scan Electron microscopy and transmission
Electron microscopy, it is inter-adhesive around the tiny balloon formed by nano particle to find the three-dimensional graphene composite material
Shape structure, using conventional aperture and the measuring method of specific surface area, measures the three-dimensional meso-hole graphene that the present embodiment is prepared
Pore-size distribution in 20nm~40nm, specific surface area is 1650m2/g。
The above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to preferred embodiment to this hair
It is bright to be described in detail, it will be understood by those within the art that, technical scheme can be modified
Or equivalent substitution, without departing from the objective and scope of technical solution of the present invention, it all should cover the claim in the present invention
Among scope.The technology of the invention not being described in detail, shape, construction part are known technology.
Claims (10)
1. a kind of sweat lactic acid device for fast detecting, it is characterised in that including set gradually from top to bottom flexible substrate layer, electricity
Pole layer, separation layer and electronic monitoring layer, the flexible substrate layer are made up of porous flexible material；
The electrode layer is included to electrode, working electrode, reference electrode and reaction chamber, it is described electrode is included being sequentially connected the
One carbon paste wire, carbon paste electrode I and carbon paste electrode II, the working electrode include the second carbon paste wire, the carbon paste being sequentially connected
Electrode III and reaction electrode, the three-dimensional graphene composite material that the reaction electrode includes oxidation enzyme layer and is attached in oxidation enzyme layer
Layer, the reference electrode includes silver wire, silver/silver chloride electrode I and the silver/silver chloride electrode II being sequentially connected, the carbon paste
Electrode II, reaction electrode and silver/silver chloride electrode II are located in reaction chamber, and the reaction chamber is externally provided with insulating barrier, the insulation
Layer covering carbon paste electrode I, carbon paste electrode III and silver/silver chloride electrode I；
The separation layer is pasted on the insulating layer, and the electronic monitoring layer, which is arranged on, is used for the reaction for monitoring electrode layer on separation layer
Change.
2. a kind of sweat lactic acid device for fast detecting according to claim 1, wherein, the electronic monitoring layer includes being used for
The voltage control unit of control electrode layer voltage, for measuring electrode layer electric current current measuring unit and for data acquisition,
Conversion, the data preparation unit of storage.
3. a kind of sweat lactic acid device for fast detecting according to claim 2, wherein, contain lactic acid in the oxidation enzyme layer
Oxidizing ferment, citric acid, chitosan and carboxymethyl cellulose.
4. a kind of sweat lactic acid device for fast detecting according to claim 3, wherein, the lactic acid oxygen in the oxidation enzyme layer
It is 8 to change enzyme, citric acid, chitosan and carboxymethyl cellulose weight ratio:0.3:0.5:1.2.
5. a kind of sweat lactic acid device for fast detecting according to any of the above-described claim, wherein, the three-dimensional grapheme
Composite is by nano-TiO2It is dispersed on graphene and is made, the three-dimensional graphene composite material layer has hollow micro-
Ball network structure, pore-size distribution is in 20nm~40nm, specific surface area 1500m2/ g~1650m2/g。
6. a kind of sweat lactic acid device for fast detecting according to claim 5, wherein, the three-dimensional graphene composite material
Preparation method it is as follows：
The preparation of graphene, using sargassum as raw material, segment is cleaned, and is dried, after air-flow crushing to micron grain size, is added
(C2H302)2In Ni solution, 9h is stirred, filter residue is dried after filtering, added after the uniform mixing of activator, add deionized water
Impregnated under ultrasonic 5min~8min, normal temperature after 13h~15h, be filtered under diminished pressure drying and obtain residue, residue is placed in baking oven and dried
Afterwards, crush and be transferred in horizontal pipe furnace, be passed through argon gas, be to slowly warm up to 860 DEG C~950 DEG C calcining 1.0h~1.5h, be cooled to
After normal temperature, add in acid solution and clean, add in ethanol or deionized water and clean, drying is obtained with porous three-dimensional structure
Graphene；
The preparation of three-dimensional graphene composite material, weighs nano-TiO2It is dissolved in deionized water, is configured to mass concentration for 0.2g/
ML~0.3g/mL solution, weighs graphene and adds in solution, stir and evenly mix, ultrasonic disperse obtains dispersion liquid, be transferred to reaction
In kettle, reactor is placed in hydro-thermal reaction 32h under 180 DEG C of water-baths, obtains after reaction solution, reaction solution decompression suction filtration, uses anhydrous second
Alcohol wash filter residue, by after washing filter residue drying after, be transferred into Muffle furnace in 550 DEG C~800 DEG C calcine 3h~5h, obtain by
Nano particle is inter-adhesive around the three-dimensional graphene composite material with tiny balloon network structure formed.
7. a kind of sweat lactic acid device for fast detecting according to claim 6, wherein, will in the graphene preparation process
Dried sargassum air-flow crushing is to 80 μm~150 μm.
8. a kind of sweat lactic acid device for fast detecting according to claim 7, wherein, in the graphene preparation process
Activator is one kind in sodium carbonate, sodium hydroxide, potassium carbonate.
9. a kind of sweat lactic acid device for fast detecting according to claim 8, wherein, in the graphene preparation process
Acid solution is one kind in hydrochloric acid, nitric acid, phosphoric acid.
10. a kind of sweat lactic acid device for fast detecting according to claim 9, wherein, the three-dimensional grapheme composite wood
The nano-TiO weighed in material preparation process2Weight ratio with graphene is 1:7~1:9.
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