AU2019101135A4 - Synthesis of Mn/Fe Prussian Blue Analogues and Investigation on Its Catalytic Activity - Google Patents

Synthesis of Mn/Fe Prussian Blue Analogues and Investigation on Its Catalytic Activity Download PDF

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AU2019101135A4
AU2019101135A4 AU2019101135A AU2019101135A AU2019101135A4 AU 2019101135 A4 AU2019101135 A4 AU 2019101135A4 AU 2019101135 A AU2019101135 A AU 2019101135A AU 2019101135 A AU2019101135 A AU 2019101135A AU 2019101135 A4 AU2019101135 A4 AU 2019101135A4
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Zhengnong Huang
Ziliang Jia
Yi Wei
Yenan Xie
Binghan Xu
An ZHANG
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Wei Yi Miss
Xie Yenan Miss
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Xie Yenan Miss
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    • C01C3/08—Simple or complex cyanides of metals
    • C01C3/12—Simple or complex iron cyanides
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    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • B01J27/26—Cyanides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
    • B01J2531/80—Complexes comprising metals of Group VIII as the central metal
    • B01J2531/84—Metals of the iron group
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    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

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Abstract

The innovation revealed the catalytic activity for Mn/Fe PBAs through chromogenic reaction. By the coprecipitation synthesis of MnSO4-H20, polyvinyl pyrrolidone (PVP), and potassium ferricyanide (K3[Fe(CN)6]) solution, Mn/Fe PBAs was produced. Mn/Fe PBAs pH had strong oxidation ability. Temperature during the reaction, the concentration of TMB (substrate), and the concentration of Mn/Fe PBAs significantly affected the oxidase-like activity of Mn/Fe PBAs. The best detection condition for the catalytic activity of Mn/Fe PBAs : pH was 4.0, temperature was 40°C, the concentration of Mn/Fe PBAs was 0.35mg/mL, the concentration of TMB was 16.7mmol/L. Figure1I

Description

Synthesis of Mn/Fe Prussian Blue Analogues and Investigation on Its Catalytic Activity
FIELD OF THE INVENTION
The present invention that related to Mn/Fe PBAs predominated a significant potential in pharmacology, physics, biomedical engineering and many different fields.
BACKGROUND OF THE INVENTION
Nanozyme is nanomaterials which have the catalytic activity of nanozymes. Compare with a natural enzyme, nanozyme has the advantages of lower cost, easy preparation, higher stability, recycling utilization, which provides the bases for the application of industrial catalytic enzyme. Unlike natural enzyme, artificial nanozyme can remain 85% catalytic activity in harsh condition ( pH and temperature). nanozyme is widely applied in the medical, chemical industry and agriculture field. Wang Wen-teyenal etc. produced a metallic-oxide nanozyme which has better catalytic performance. Yang Ruitao etc. used a bimetallic metal-organic framework material as nanozyme for colourimetric detection of hydrogen perox1
2019101135 30 Sep 2019 ide[ 1], This research discovered that this bimetallic MOF material can act as peroxidase mimic enzymes and oxide mimic enzyme for the first time. Through the review of the previous studies home and aboard, scholars prepared nanozyme successfully through the hydrothermal method, sacrificial template, U-shaped tube for double scattering, common reduction methods.
Manganese-iron alloy, which is manganese and iron composition of the ferroalloy, used as a deoxidizer and alloy additives in steelmaking. It is the most frequently used ferrous alloy in this industry. Prussian blue (Fe7(CN)i8· 14H2O) is not only stable, incompatible with strong acids, strong oxidizing agents, ammonia but also light-sensitive. Zheng Wei etc. researched PBNPs (Prussian Blue Nano Particles) in-depth[2]. First of all, they found that PBNPs have the activities of several different mimic enzymes such as peroxidase (POD), catalase (CAT), superoxide dismutase (SOD) and ascorbate oxidase (AAO). Secondly, from the study of PBNPs’ catalytic mechanism, it is found that its POD-like activity is much higher than the that of iron oxide nanoparticles (IONPs). From the previous literature research, it is found that PBNPs follow the electron transfer mechanism while IONPs follow the Fenton reaction mechanism. A systematic safety assessment of PBNPs inside the human body was carried out, and the data from the safety assessment of PBNPs indicate that PBNPs is completely safe to human.
In this research, we dissolved the MnSO4- H2O and PVP in a mixture solution of ethanol and deionized water, which was marked as solution A. Then the aqueous solution of K3 [Fe (CN) 6] was slowly added into solution A under the magnetic
2019101135 30 Sep 2019 stirring. After centrifugation and washing followed by a drying process, Mn/Fe PBAs were obtained. This method was simple, speedy, easy to operate and was able to produce manganese iron in a large-scale. The catalytic activity of Mn/Fe PBAs was strong. These advantages made manganese-iron nanozyme a promising candidate for analytical application. The mechanism of detection of catalytic activity of nanozymes is that TMB is oxidized by OH radicals to oxTMB which is a blue substance. In this research, the best reaction condition was obtained by changing the pH value, temperature, TMB concentration and concentration of nanozyme respectively.
SUMMARY OF THE INVENTION
The purpose of the experiment was to find whether the Mn/Fe PBAs owned the chemical characteristic of catalytic activity, which always appeared in nanozyme. To explore the chemical characteristic of high catalytic activity on Mn/Fe PBAs, Mn/Fe PBAs was produced by the coprecipitation method. To exactly know the best condition of the production of Mn/Fe PBAs, the influence factors of the catalytic reaction, pH, the concentration of TMB, the concentration of Mn/Fe PBAs, and temperature during the reaction, were needed. Finally, it was ensured that Mn/Fe PBAs had the chemical characteristic of the oxidase-like catalytic activity and this high catalytic activity was for oxidation.
2019101135 30 Sep 2019
Experiment instrument magnetic stirrer centrifuge thermo shaker
Five pH Meter
The absorption spectra were collected on a 96-well plate in Molecular Devices Spectra max M5 microplate reader.
Transmission electron microscopy (TEM) images of Mn/Fe PBAs were collected on a transmission electron microscope (FEI Tecnai G2 20 S-TWIN) operating at an accelerating voltage of 200 kV
SEM images of Mn/Fe PBAs were collected on a scanning electron microscopy (SEM, Hitachi S-4800)
Experiment reagent
Potassium Phosphate Monobasic (Sinopharm Chemical Reagent Beijing Co., Ltd)
Dipotassium hydrogen phosphate (Sinopharm Chemical Reagent Beijing Co., Ltd)
Manganese (II) Sulfate MonohydrateMnSO4 · H2O (Sigma-Aldrich)
PVP (polyvinyl pyrrolidone) (Sigma-Aldrich) potassium ferricyanide (Acros Organics) 3,3’,5,5’-Tetramethylbenzidine (TMB) (Acros Organics)
Ethanol (Beijing Chemical Works)
2019101135 30 Sep 2019
The water used throughout all experiments was purified by a Milli-Q system (18 ΜΩ-cm).
Preparation of Mn/Fe PBAs:
0.05 g MnSCfi-EfO and 0.25 g PVP were dissolved in the mixed solution which contained 10 mL pure ethanol and 10 mL deionized water. This solution was recorded as solution A. Then, 0.07 g K3[Fe (CN)6] was dissolved in 10 mL deionized water. This solution was recorded as solution B. Under the stirring condition of solution A, solution B was slowly added to solution A. After that, the reaction solution was being continuously stirring for 3 h. After the solution was centrifuged in 5000 rpm for 7 min, the sediment was washed by the mixed solution which contained deionized water and pure ethanol in 5000 rpm for 7 min, twice. The sediment was washed by pure ethanol solution in 5000 rpm for 7 min, twice. Finally, the sediment was dried overnight and weighed.
The highest absorbance was in pH 4.0, 16.7 mmol/L TMB, 0.43 mg/mL Mn/Fe PBAs, and 40 °C, which implied that Mn/Fe PBAs had the best catalytic activity in these conditions
DESCRIPTION OF DRAWING
Figure 1 shows the SEM image of the Mn/Fe PBAs.
2019101135 30 Sep 2019
Figure 2 shows the TEM image of the Mn/Fe PBAs.
Figure 3 shows the catalytic activity of Mn/Fe PBAs change with pH.
Figure 4 shows the catalytic activity of Mn/Fe PBAs change with concentration of TMB.
Figure 5 shows the catalytic activity of Mn/Fe PBAs change with concentration of Mn/Fe PBAs.
DESCRIPTION OF PREFERRED EMBODIMENTS
The embodiment of the present invention will be detailly introduced in order that the present invention can be easily realized.
The present invention successfully prepared Mn/Fe PBAs. Besides, the fact that the Mn/Fe PBAs has catalytic activity was proved, and the best reaction condition was found, indicating below :
The Preparation of Mn/Fe PBAs:
0.05g MnSO4-H2O and 0.25g PVP were dissolved into the mixed solution of 10 mL deionized water and 10 mL pure ethanol, which was recorded as solution A.
0.07 g K3[Ee (CN)6] was dissolved into 10 mL deionized water, which was recorded as solution B.
2019101135 30 Sep 2019
Solution A was continuously stirred by a magnetic mixer, then solution B was added into solution A slowly. After the solution B was completely added, this stirring lasted for 3 hours.
The sediment was centrifuged at 5000 rpm for 8 min by the mixed solution which contained 4 mL deionized water and 4 mL pure ethanol, twice.
The sediment was centrifuged at 5000 rpm for 8 min by 4 mL pure ethanol, twice.
The sediment was Dried overnight and weighed.
the mass of Mn/Fe PBAs= the mass of the after drying sediment in the 1.5 mL centrifuge tube - the mass of the empty 1.5 mL centrifuge tube (0.0545 g = 3.3133 g- 3.2588 g) the concentration of the Mn/Fe PBAs solution is 0.5 mg/mL
Impacts of pH Value:
0.6 mL pH 3-9 solutions were added in seven 1.5 mL centrifuge tubes, respectively· pL Mn/Fe PBAs was added into seven 1.5 mL centrifuge tubes, respectively.
pL TMB was added into seven 1.5 mL centrifuge tubes, respectively.
After 8 min, the colour changes of these solutions were detected at 650 nm absorbance, to observe the influence factor, pH, on catalytic reaction and determine the optimal pH for the reaction.
Repeated above steps three times.
2019101135 30 Sep 2019
The highest absorbance was in pH 4.0, which implied that Mn/Fe PBAs had the best catalytic activity at pH 4.0
Impacts of the Concentration of Substrate:
4.0 pH TMB solution in 0.4 mL was added into six 1.5 mL centrifugal tubes, respectively.
pL Mn/Fe PBAs was added into six 1.5 mL centrifugal tubes, respectively.
3.33(6.67/10/13.3/16.7/20) mmol/L TMB in 30 pL was added into six 1.5 mL centrifugal tubes, respectively.
After 8 min, the colour changes of these solutions were detected at 650 nm absorbance, to observe the influence factor, the concentration of TMB, on catalytic reaction and determine the optimal concentration of TMB for the reaction.
Repeated above steps three times.
The highest absorbance was 16.7 mmol/L, which implied that Mn/Fe PBAs had the best catalytic activity at 16.7 mmol/L TMB.
Impacts of the concentration of Mn/Fe PBAs:
4.0 pH TMB solution in 0.4 mL was added into six 1.5 mL centrifugal tubes, respectively.
16.7 mmol/L TMB in 30 pL was added into six 1.5 mL centrifugal tubes, respectively.
2019101135 30 Sep 2019
0.14(0.21/0.29/0.36/60.43/0.5) mg/mL Mn/Fe PBAs in 70 pL was added into the six 1.5 mL centrifugal tubes, respectively.
After 10 min, the colour changes of these solutions were detected at 650 nm absorbance, to observe the influence factor, the concentration of Mn/Fe PBAs, on catalytic reaction and determine the optimal concentration of Mn/Fe PBAs for the reaction.
Repeated above steps three times.
The highest absorbance was 0.43 mg/mL, which implied that Mn/Fe PBAs had the best catalytic activity at 0.43 mg/mL Mn/Fe PBAs.
Impacts of Temperature during the Reaction:
4.0 pH TMB solution in 0.4 mL was added into five 1.5 mL centrifugal tubes, respectively.
16.7 mmol/L TMB in 30 pL was added into the five 1.5 mL centrifugal tubes, respectively.
0.43 mg/mL Mn/Fe PBAs in 70 pL was added into the five 1.5 mL centrifugal tubes, respectively.
Under 20(30/40/50/60) °C, the reaction was conducted for 13 min.
The colour changes of these solutions were detected at 650 nm absorbance, to observe the influence factor, the temperature during the reaction, on the catalytic reaction and determine the optimal temperature for the catalytic reaction.
Repeated above steps three times.
2019101135 30 Sep 2019
The highest absorbance was 40 °C, which implied that Mn/Fe PBAs had the best catalytic activity at 40 °C
Causing the high catalytic activity of Mn/Fe PBAs, this new material could be used in capacitor, battery, the adsorption material for polluted water, and the detection for the pesticide reminds.

Claims (3)

1. A synthesis of Mn/Ee prussian blue analogues (Mn/Ee PBAs), which includes a new nanozyme which had the catalytic activity for oxidation, wherein:
the Μη/Le PBAs ((Μη/Le Prussian blue analogues)) is prepared using the following procedures:
a) MnSO4-H2O and polyvinyl pyrrolidone(PVP) are dissolved into the mixed solution of deionized water and pure ethanol, which is recorded as solution A;
b) K3[Pe (CN)6] is dissolved into deionized water, which is recorded as solution B;
c) Solution A is continuously stirred by a magnetic mixer while solution B is being added into solution A slowly, the obtained mixture was centrifuged, washed and dried;
d) The sediment is washed by a mixed solution of deionized water and pure ethanol twice;
e) The sediment is washed by 4mL pure ethanol twice;
f) The sediment is dried overnight and weighed;
2019101135 30 Sep 2019 in procedure a), the optimal volume ratio of water to ethanol is 1:1;
in procedure d), the optimal reaction time is 3 hours;
The morphology of Mn/Fe PBAs is a cube whose diameter is 1 pm.
2. The synthesis of Mn/Fe prussian blue analogues (Mn/Fe PBAs) of claim 1, wherein the Mn/Fe PBAs prepared by coprecipitation is proved to have high oxidase catalytic activity, which is first proved in this essay, via colourimetry by catalysing TMB to become oxTMB.
3. The synthesis of Mn/Fe prussian blue analogues (Mn/Fe PBAs) of claim 2, the best catalysis condition for the FeMn nanozyme are achieved by the control variate method; best conditions are as follow:
Temperature: 40 Celsius degree
TMB concentration: 16.7 mM
Nanozyme concentration: 0.429 mg/mL pH: 4 this method for the preparation of the Mn/Fe PBAs is simple and rapid; the Mn/Fe PBAs owns the high catalytic activity, which is applied in a large scale.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112058287A (en) * 2020-08-25 2020-12-11 浙江工业大学 In-situ preparation method of two-dimensional metal selenide @ MXene composite electrocatalyst
CN112142069A (en) * 2020-09-27 2020-12-29 广州大学 Prussian blue analogue and morphology control method and application thereof
CN112630179A (en) * 2020-12-09 2021-04-09 安徽师范大学 Prussian blue quantum dot with oxide mimic enzyme property, preparation method thereof and method for detecting L-cysteine
CN112919593A (en) * 2021-01-12 2021-06-08 同济大学 Preparation method of graphene-coated cobalt Prussian blue nanocrystalline composite material, method for preparing working electrode by using graphene-coated cobalt Prussian blue nanocrystalline composite material and application of graphene-coated cobalt Prussian blue nanocrystalline composite material
CN113402726A (en) * 2021-06-25 2021-09-17 福州大学 Prussian blue analogue nano-framework material and preparation method and application thereof
CN114414514A (en) * 2022-01-20 2022-04-29 中山大学 Preparation method of manganese Prussian blue nano-enzyme and application of manganese Prussian blue nano-enzyme in alcohol concentration detection
CN114506860A (en) * 2022-01-07 2022-05-17 清华大学 Iron-manganese-based Prussian blue solid solution and preparation method thereof
CN114985006A (en) * 2022-05-23 2022-09-02 北京师范大学珠海校区 Two-dimensional layered catalytic membrane material, preparation method and application

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112058287B (en) * 2020-08-25 2023-04-18 浙江工业大学 In-situ preparation method of two-dimensional metal selenide @ MXene composite electrocatalyst
CN112058287A (en) * 2020-08-25 2020-12-11 浙江工业大学 In-situ preparation method of two-dimensional metal selenide @ MXene composite electrocatalyst
CN112142069A (en) * 2020-09-27 2020-12-29 广州大学 Prussian blue analogue and morphology control method and application thereof
CN112630179A (en) * 2020-12-09 2021-04-09 安徽师范大学 Prussian blue quantum dot with oxide mimic enzyme property, preparation method thereof and method for detecting L-cysteine
CN112630179B (en) * 2020-12-09 2023-07-21 安徽师范大学 Prussian blue quantum dot with oxide mimic enzyme property, preparation method thereof and method for detecting L-cysteine
CN112919593A (en) * 2021-01-12 2021-06-08 同济大学 Preparation method of graphene-coated cobalt Prussian blue nanocrystalline composite material, method for preparing working electrode by using graphene-coated cobalt Prussian blue nanocrystalline composite material and application of graphene-coated cobalt Prussian blue nanocrystalline composite material
CN113402726A (en) * 2021-06-25 2021-09-17 福州大学 Prussian blue analogue nano-framework material and preparation method and application thereof
CN114506860A (en) * 2022-01-07 2022-05-17 清华大学 Iron-manganese-based Prussian blue solid solution and preparation method thereof
CN114506860B (en) * 2022-01-07 2023-08-22 清华大学 Iron-manganese-based Prussian blue solid solution and preparation method thereof
CN114414514A (en) * 2022-01-20 2022-04-29 中山大学 Preparation method of manganese Prussian blue nano-enzyme and application of manganese Prussian blue nano-enzyme in alcohol concentration detection
CN114414514B (en) * 2022-01-20 2023-12-22 中山大学 Preparation method of manganese Prussian blue nano enzyme and application of manganese Prussian blue nano enzyme in alcohol concentration detection
CN114985006A (en) * 2022-05-23 2022-09-02 北京师范大学珠海校区 Two-dimensional layered catalytic membrane material, preparation method and application
CN114985006B (en) * 2022-05-23 2023-11-14 北京师范大学珠海校区 Two-dimensional layered catalytic membrane material, preparation method and application

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