CN106918632A - The preparation method and applications of flower-shaped nickel metal organic framework nano material - Google Patents

The preparation method and applications of flower-shaped nickel metal organic framework nano material Download PDF

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CN106918632A
CN106918632A CN201710251531.1A CN201710251531A CN106918632A CN 106918632 A CN106918632 A CN 106918632A CN 201710251531 A CN201710251531 A CN 201710251531A CN 106918632 A CN106918632 A CN 106918632A
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flower
organic framework
metal organic
nickel metal
nano material
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庞欢
薛俞琪
郑莎莎
唐燚剑
薛怀国
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Yangzhou University
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Yangzhou University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract

The preparation method and applications of flower-shaped nickel metal organic framework nano material, belong to the preparing technical field of anti-ascorbate sensor.Flower-shaped nickel metal organic framework nano material of the invention is prepared from by simple hydro-thermal method, and the raw material of use are nontoxic, environmentally friendly, low cost, process is simple, it is easy to operational control, is suitable to continuous words large-scale production, preparation process environmental protection.This flower-shaped nickel metal organic framework nano material has that outstanding electrochemical response, the range of linearity be wide, sensitivity is high, the advantages of good antijamming capability and preferable electrochemical stability, can be used for electrochemical sensing.

Description

The preparation method and applications of flower-shaped nickel metal organic framework nano material
Technical field
The invention belongs to the preparing technical field of anti-ascorbate sensor.
Background technology
Ascorbic acid is a kind of vitamin needed by human, is also a kind of antioxidant, can improve human body immunity and Respond.It is a kind of naturally occurring organic compound with antioxidant properties, is to safeguard body normal physiological function One of important vitamin, be widely present in fresh fruit, fruit juice and green vegetable.It participates in a series of metabolism in vivo and oxygen Change reduction reaction, additionally aid the cytoplasm such as the first and glutinous polysaccharide of rubber polymer, synthesis, internal oxygen in cortex hormone of aadrenaline It is also indispensable to change in reducing, and human body lacks ascorbic acid can then cause scurvy, therefore the quantitative of Ascorbic Acid to be divided Analysis is respectively provided with significance in medicine, field of food.
At present, the assay method of ascorbic acid mainly include iodimetric titration, ultraviolet spectrophotometry, high performance liquid chromatography and Electrochemical process etc..Experiment condition and operating technology higher is required mostly, some method and steps are loaded down with trivial details, be unfavorable for quick analysis. More in addition the method being analyzed by color is also due to testing sample influences the result for determining per se with color.Cause This, research anti-ascorbate sensor has very big significance determining ascorbic acid.
Metal-organic framework material（MOFs）It is that coordinate bond self assembly shape is passed through by organic ligand and metal ion or cluster Into the hybrid inorganic-organic materials with molecule inner pore.The variable metal center of MOFs materials and organic ligand result in The diversity of its structure and function, it is stored in hydrogen, gas absorption and separate, the neck such as sensor, medicament slow release, catalytic reaction There is important application in domain.With the gradually rise of the increasing and compound MOFs materials of MOFs material categorys, MOFs materials Material will have immeasurable application prospect.Therefore, MOFs and compound MOFs material of the exploitation with functional diversity, and apply In different field, interdisciplinary mutual development will be greatly promoted.
The content of the invention
Existing background technology and a kind of not enough, flower-shaped nickel metal organic framework nano material of present invention proposition for more than Preparation method
The present invention is comprised the following steps：
1）Divalent nickel salt and terephthalic acid (TPA) are dissolved in dimethylformamide, mixed solution is obtained；
2）Mixed solution is mixed with alkaline solution, is placed in 100~150 DEG C of environment after being stirred 1~1.5 hour under normal temperature Water-filling thermal response, obtains greenish precipitate thing；
3）Dried after greenish precipitate thing is washed with DMF and ethanol, obtain final product flower-shaped nickel metal organic framework nano material.
Flower-shaped nickel metal organic framework nano material of the invention is prepared from by simple hydro-thermal method, the raw material of use Nontoxic, environmentally friendly, low cost, process is simple, it is easy to operational control, are suitable to continuous words large-scale production, preparation process environmental protection. It is experimentally verified that, this flower-shaped nickel metal organic framework nano material has outstanding electrochemical response, the range of linearity wide, sensitive The advantages of spending antijamming capability and preferable electrochemical stability high, good, can be used for electrochemical sensing.
Further, due to metal-organic framework materials by nickel slaine as source metal and terephthalic acid (TPA) as organic Part is constituted, and in order to obtain, product morphology is optimal and best performance, and terephthalic acid (TPA) of the present invention and divalent nickel salt feed intake Mol ratio is 3: 1, and other raw materials are solvent and do not feed intake specifically requirement.
The divalent nickel salt is Ni (NO3)2•6H2O、NiSO4•H2O or Ni (CH3COO)2•4H2O.It is bright through real probatio inspectionem pecuoarem, due to The acid group of this several slaine institutes band is easily sloughed, and is more easy to obtain required product, therefore preferentially use this several slaine.
The alkaline solution is the NaOH aqueous solution or the KOH aqueous solution.In common water soluble alkali, NaOH and KOH stabilizations It is easy to get and cheap, therefore pays the utmost attention to use in the present invention.
In addition, the present invention also proposes flower-shaped nickel metal organic framework nano material prepared by above method in the sensor Using, it is characterised in that：Under ultrasound condition, flower-shaped nickel metal organic framework nano material is dissolved in perfluorosulfonic acid type polymer In solution, then modify on glass-carbon electrode, dry, that is, sensor is obtained.
Sensor electrode Ascorbic Acid prepared by the present invention can be responded rapidly, and the range of linearity is wide, and sensitivity is high, Good stability, the lower limit for detecting are low.
Advantage of the invention is that：
1st, linearity test interval range：0.5 μM of -8 mM ascorbic acid；
2nd, detection sensitivity：Sensitivity is 2401.1 mA mM-1cm-2；
3rd, anti-interference：Have to glucose, uric acid, dopamine, sodium chloride in the detection process of ascorbic acid and resist well Jamming performance；
4th, compared with prior art, ascorbic acid electrochemical sensor Ascorbic Acid detection range of the invention is wide, is 0.5 μM ~8 μM.Detection sensitivity is high, has good interference free performance to glucose, uric acid, dopamine, sodium chloride.
Brief description of the drawings
Fig. 1 is the small multiplying power scanning electron microscope (SEM) photograph of flower-shaped nickel metal organic framework nano-electrode material prepared by the present invention.
Fig. 2 is the big multiplying power scanning electron microscope (SEM) photograph of flower-shaped nickel metal organic framework nano-electrode material prepared by the present invention.
Fig. 3 is that flower-shaped nickel metal organic framework nano-electrode material prepared by the present invention is applied to detect following for ascorbic acid Ring volt-ampere curve figure.
Fig. 4 be the present invention prepare flower-shaped nickel metal organic framework nano-electrode material detection ascorbic acid concentrations electric current- Time graph.
Fig. 5 is the linearly interval that flower-shaped nickel metal organic framework nano-electrode material prepared by the present invention detects ascorbic acid Fitted figure.
Fig. 6 is the when m- electricity of the flower-shaped nickel metal organic framework nano-electrode material to disturbance thing of present invention preparation Stream response diagram.
Fig. 7 is the weight that flower-shaped nickel metal organic framework nano-electrode material prepared by the present invention is applied to detect ascorbic acid Existing property time current curve.
Fig. 8 is that flower-shaped nickel metal organic framework nano-electrode material prepared by the present invention is applied to detect the steady of ascorbic acid Characteristic time-current curve.
Specific embodiment：
With example, the invention will be further described with reference to the accompanying drawings and detailed description, but not limited to this.
First, the technique for preparing flower-shaped nickel metal organic framework nano material：
Weigh 0.096g Ni (NO3)2•6H2O and 0.166g terephthalic acid (TPA)s（C8H6O4）It is dissolved in dimethylformamide（DMF）, obtain To mixed solution I.
The accurate configuration 2 mL 0.4 M NaOH aqueous solution delays, then slow to instill mixed solution I, obtains mixed solution I I, often Temperature descends stirring 1 hour, then hydro-thermal reaction 8 hours under the conditions of 100 DEG C.The greenish precipitate for obtaining, then divided with DMF and ethanol Xi Di not be dried after 3 times, obtain flower-shaped nickel metal organic framework nano material.
Above Ni (NO3)2•6H2O can also use NiSO4•H2O or Ni (CH3COO)2•4H2O is substituted.
The above NaOH aqueous solution can also be substituted with the KOH aqueous solution.
2nd, the performance test of flower-shaped nickel metal organic framework nano material：
1st, flower-shaped nickel metal organic framework nano material SEM is tested, Fig. 1 is that nickel metal organic framework nano material amplifies 5000 Electron scanning micrograph under times, test result shows, the nickel metal organic framework nano material size shape base of synthesis This uniformity.
2nd, flower-shaped nickel metal organic framework nano material SEM is tested, Fig. 2 is single flower-shaped nickel metal organic framework nanometer Material amplifies the electron scanning micrograph under 1000 times, and test result shows that colored average diameter is about 15 μm.
3rd, anti-ascorbate sensor electrode is prepared：
By a diameter of 3 millimeters of glass-carbon electrode respectively with the sand paper for having adsorbed 1 micrometer alumina suspension and to have adsorbed 0 .05 micro- The sand papering polishing of rice aluminum oxide suspension, obtains clean glass-carbon electrode.
The flower-shaped nickel metal organic framework nano material for taking 10 mg preparations is dissolved in 1 mL concentration（Quality）It is 1% perfluor sulphur In acid-based polymer solution, it is well mixed under ultrasound condition, is made mixed solution.Then by 5 μ L mixed solutions using coating Method modification a diameter of 3 mm clean glassy carbon electrode surface, dry naturally, obtain final product sensor electrode.
4th, apply：
1st, electrolyte is configured：Using cushioning liquid as electrolyte, wherein, the pH value of cushioning liquid is 7.2.
2nd, detecting electrode chemical property：
Flower-shaped nickel metal organic framework sensor electrode is placed in cushioning liquid and is measured：Between -0.1~0.8 V Current potential under, sweep speed is controlled to 0.1 V/s, is circulated voltammetric scan, molten with blank assay and 500 μM of ascorbic acid Liquid is compareed, and observes current-responsive result；Under 0.25 V potentiostatic scannings, sample nickel metal organic framework nano material electricity The ascorbic acid of various concentrations is extremely continuously added dropwise in the liquid of cushioning liquid bottom and is stirred continuously carries out detection current versus time curve； Sample nickel metal organic framework nano material electrode is distinguished in the cushioning liquid bottom liquid that current potential 0.25 V, PH are 7.2 with concentration It is 100 μM of ascorbic acid, 5 μM of glucose, 5 μM of uric acid, 5 μM of dopamines, 5 μM of sodium chloride and 100 μM of ascorbic acid Standard liquid carry out dropwise addition test；The reappearance of electrode material is tested, in the cushioning liquid bottom liquid that PH is 7.2, addition is repeated anti- Bad hematic acid (100 μM) 10 times, observes curent change；The stability of detecting electrode material, liquid (100 μM) at ascorbic acid bottom After middle electro-catalysis 4000 seconds, curent change is observed.
Fig. 3 solid lines are 500 μM of ascorbic acid solutions, and dotted line is tested for blank, shown by Fig. 3：Nickel metal has Machine skeleton nano material sensor electrode material is swept under speed 0.1 V/s's, and 500 μM of ascorbic acid solution oxidation peaks substantially compare Blank group experiment is strong.
Fig. 4 shows that nickel metal organic framework nano material sensor electrode is carried out to the ascorbic acid bottom liquid of various concentrations Detection current versus time curve, it can be seen that quickly, sensitively urging occurs in sample nickel metal organic framework nano material Ascorbic Acid Change responding ability.
Fig. 5 shows that the concentration range of linearity of acquisition is 0.5 μM of -8 mM, and linear equation is [R=0.9953, Current I (μA) = 0.03119 + 1.6964*10^-4C (μM)], sensitivity is 2401.1 mA mM-1cm-2。
Fig. 6 shows that the electrode of sample Ni MOF is respectively 100 μ in the liquid of cushioning liquid bottom in the V of current potential 0.25 with concentration M ascorbic acid, 5 μM of glucose, 5 μM of uric acid, 5 μM of dopamines, 5 μM of sodium chloride and 100 μM of standard liquids of ascorbic acid are carried out Test is added dropwise, as a result shows, electrode material has fabulous antijamming capability.
Fig. 7 shows, in the cushioning liquid bottom liquid that PH is 7.2, repeats to add ascorbic acid (100 μM) 10 times, has Almost identical current-responsive, electrode material has fabulous reappearance.
Fig. 8 shows, in the ascorbic acid bottom liquid (100 μM) after electro-catalysis 4000 seconds, response current is kept approximately constant, Electrode material has fabulous stability.

Claims (6)

1. a kind of preparation method of flower-shaped nickel metal organic framework nano material, it is characterised in that comprise the following steps：
1）Divalent nickel salt and terephthalic acid (TPA) are dissolved in dimethylformamide, mixed solution is obtained；
2）Mixed solution is mixed with alkaline solution, is placed in 100~150 DEG C of environment after being stirred 1~1.5 hour under normal temperature Water-filling thermal response, obtains greenish precipitate thing；
3）Dried after greenish precipitate thing is washed with DMF and ethanol, obtain final product flower-shaped nickel metal organic framework nano material.
2. preparation method according to claim 1, it is characterised in that the terephthalic acid (TPA) and feeding intake for divalent nickel salt are rubbed You are than being 3: 1.
3. preparation method according to claim 1, it is characterised in that the divalent nickel salt is Ni (NO3)2•6H2O、NiSO4• H2O or Ni (CH3COO)2•4H2O。
4. preparation method according to claim 1, it is characterised in that the alkaline solution is that the NaOH aqueous solution or KOH are water-soluble Liquid.
5. preparation method according to claim 1, it is characterised in that the step 2）Stirred 1 hour under middle normal temperature, 100 Hydro-thermal reaction is carried out under the conditions of DEG C.
6. the flower-shaped nickel metal organic framework nano material that prepared by method as claimed in claim 1 application in the sensor, its It is characterised by：Under ultrasound condition, flower-shaped nickel metal organic framework nano material is dissolved in perfluorosulfonic acid type polymer solution, Then modify on glass-carbon electrode, dry, that is, sensor is obtained.
CN201710251531.1A 2017-04-18 2017-04-18 The preparation method and applications of flower-shaped nickel metal organic framework nano material Pending CN106918632A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN108982626A (en) * 2018-05-30 2018-12-11 海南师范大学 It is a kind of for detecting the nano electrochemical enzyme sensor and its preparation method and application of trichloroacetic acid or sodium nitrite
CN109085206A (en) * 2018-07-11 2018-12-25 齐鲁工业大学 A kind of Fe2O3-TiO2The preparation method of gas sensor
CN109301217A (en) * 2018-09-30 2019-02-01 西北有色金属研究院 A kind of preparation method and applications of layered laminate NiO micro Nano material
CN109553779A (en) * 2018-11-20 2019-04-02 三峡大学 A kind of preparation method and application of three-dimensional manometer flower metal-organic framework material
CN110828193A (en) * 2019-12-02 2020-02-21 桂林电子科技大学 Nano flower-shaped Ni-MOF material and preparation method and application thereof
CN113963954A (en) * 2021-11-05 2022-01-21 扬州大学 NHNO nano array, preparation method thereof and application of NHNO nano array in supercapacitor electrode

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108982626A (en) * 2018-05-30 2018-12-11 海南师范大学 It is a kind of for detecting the nano electrochemical enzyme sensor and its preparation method and application of trichloroacetic acid or sodium nitrite
CN109085206A (en) * 2018-07-11 2018-12-25 齐鲁工业大学 A kind of Fe2O3-TiO2The preparation method of gas sensor
CN109301217A (en) * 2018-09-30 2019-02-01 西北有色金属研究院 A kind of preparation method and applications of layered laminate NiO micro Nano material
CN109553779A (en) * 2018-11-20 2019-04-02 三峡大学 A kind of preparation method and application of three-dimensional manometer flower metal-organic framework material
CN109553779B (en) * 2018-11-20 2021-05-18 三峡大学 Preparation method and application of three-dimensional nanoflower metal organic framework material
CN110828193A (en) * 2019-12-02 2020-02-21 桂林电子科技大学 Nano flower-shaped Ni-MOF material and preparation method and application thereof
CN113963954A (en) * 2021-11-05 2022-01-21 扬州大学 NHNO nano array, preparation method thereof and application of NHNO nano array in supercapacitor electrode

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Application publication date: 20170704