CN111001423A - Preparation of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme and method for detecting hydrogen peroxide - Google Patents
Preparation of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme and method for detecting hydrogen peroxide Download PDFInfo
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- CN111001423A CN111001423A CN201911359909.5A CN201911359909A CN111001423A CN 111001423 A CN111001423 A CN 111001423A CN 201911359909 A CN201911359909 A CN 201911359909A CN 111001423 A CN111001423 A CN 111001423A
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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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
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
Abstract
The invention relates to a method for preparing semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme and detecting hydrogen peroxide. Uniformly dispersing commercial titanium dioxide (P25) and nickel phosphide into a bismuth ferrite synthesis system, stirring for 24 hours, calcining at high temperature in air, grinding, cleaning and drying to obtain the bismuth ferrite-titanium dioxide-nickel phosphide nano composite. Adding the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme into acetic acid-sodium acetate buffer solutions containing hydrogen peroxide with different concentrations and fixed color developing agent concentrations, standing and reacting for 15 minutes under the conditions of certain pH and temperature, taking out the reaction solution, and analyzing the detection effect of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme on the hydrogen peroxide by adopting a spectrophotometry. The semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme is convenient and rapid to detect peroxide, high in sensitivity, low in cost and environment-friendly.
Description
Technical Field
The invention relates to a method for preparing semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme and detecting hydrogen peroxide, belonging to the technical field of biology and chemical industry.
Background
Hydrogen peroxide is an important representative of the reactive oxygen species and has been considered to be one of the signaling molecules in a wide range of signal transduction processes, such as in normal cellular function or disease progression. Hydrogen peroxide is also involved in chemical, pharmaceutical and environmental processes. Therefore, the determination of the hydrogen peroxide has certain application value in the fields of medical diagnosis, industrial and agricultural production, environmental monitoring and the like. The colorimetric method is widely applied to the fields of biomass detection, immunoassay, environmental prediction and the like all the time due to the advantages of simplicity, convenience, visibility and the like. The traditional colorimetric method based on biological enzyme is used for measuring peroxide, and has the disadvantages of high sensitivity, accuracy and reliability, complex operation and high cost. Recently, colorimetric determination of peroxides based on nanomaterials is receiving more and more attention, because "nanoenzymes" are used instead of biological enzymes, which not only greatly saves cost and simplifies operation steps, but also has higher detection stability. The so-called "nanoenzyme", i.e. the nanomaterial as a catalyst, catalyzes the oxidation of hydrogen peroxide, and in the process, the color-developing agent 3, 3, 5, 5' -tetramethylbenzidine is converted into an oxidation state and changes from colorless to blue.
Various inorganic materials have been found to have peroxide-like activity, such as carbon nanomaterials, metal (hydroxide) oxides, metalloaluminide, noble metal nanomaterials, and the like. Although great progress has been made in designing peroxidase mimetic nanomaterials, there are still some significant drawbacks. In order to make these materials have better catalytic effect, the preparation of composite nano enzyme is one of effective approaches. Bismuth ferrite is an important oxide semiconductor, contains ferroelectric and antiferromagnetic properties, and can be used as a photocatalyst for treating sewage under the irradiation of visible light. It is widely used because of its narrow band gap energy (2.2eV), high physical and chemical stability. Titanium dioxide has excellent performances of hardness, corrosion resistance, wear resistance, antibacterial activity, photocatalytic degradation and the like, and is a nano material with great development prospect. Nickel phosphide nanoparticles are not only promoters that accelerate the transfer of photo-generated electron-hole pairs, but are also good semiconductors with predominant properties. The bismuth ferrite, the titanium dioxide and the nickel phosphide are compounded, so that the specific surface area of the material can be increased, the catalytic performance and the stability of the material are enhanced, and a good catalytic effect is achieved.
Disclosure of Invention
The invention aims to solve the existing problems and provides a method for preparing semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme and detecting hydrogen peroxide.
The invention aims to realize the purpose, and the preparation method of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme is characterized by comprising the following steps:
(1) respectively weighing 1.5-2g of nickel acetate and 1.5-2g of sodium hypophosphite, placing the nickel acetate and the sodium hypophosphite in a quartz crucible, placing the quartz crucible in a vacuum tube furnace, calcining the quartz crucible for 1-2 hours at the high temperature of 400 ℃ in the nitrogen atmosphere, and grinding the quartz crucible into powder nickel phosphide;
(2) weighing 1.975-3.95g of bismuth nitrate and 1.209-2.418g of ferric nitrate, and respectively dispersing in 50ml of 2.5M nitric acid and deionized water to obtain solutions;
(3) mixing the solution in the step (2) in a 250ml beaker, and adjusting the pH of the solution to 10 by using 6M NaOH;
(4) adding 1.06-6.36g of nickel phosphide in the step (1) and 1.06-6.36g of titanium dioxide (P25) into the step (3), magnetically stirring for 24-26 hours, then placing the mixture into an oven to be dried for 24 hours at the temperature of 60-80 ℃, and grinding the mixture into powder to obtain a bismuth ferrite-titanium dioxide-nickel phosphide precursor;
(5) and (3) placing the precursor obtained in the step (4) in a quartz crucible, placing the quartz crucible in a vacuum tube furnace, calcining the quartz crucible for 2 to 3 hours at the high temperature of 600-700 ℃ under the air, grinding the quartz crucible into powder, respectively washing the powder by using ethanol and ultrapure water, and drying the powder at the temperature of 60 to 80 ℃ to obtain the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme.
In the step (4), the mass ratio of the bismuth ferrite to the titanium dioxide to the nickel phosphide is (1-3): 1: 1, magnetically stirring for 24-26 hours;
the method for detecting hydrogen peroxide by using the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme is characterized by comprising the following specific steps of:
a) dispersing 1-5 mg of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme into 1 ml of water to prepare a semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension with the concentration of 1-5 mg/ml;
b) adding 10 microliters of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension, a color-developing agent with fixed concentration and hydrogen peroxide with different concentrations into an acetic acid-sodium acetate (acetate) buffer solution for culture;
c) and (4) measuring the concentration of the hydrogen peroxide in the mixed solution obtained in the step (6) by using a spectrophotometer.
The concentration of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension is 1-5 mg/ml, a reaction system consists of 10 microliters of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension, 10 microliters of hydrogen peroxide with different concentrations, 250 microliters of 1-2 millimoles/liter of color developing agent and 730 microliters of 0.1 millimoles/liter of acetate buffer solution, the pH value of the buffer solution is 3-5, the culture temperature is 30-50 ℃, and the culture time is 10-20 minutes.
The invention is scientific and reasonable, and the method for preparing the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme and detecting hydrogen peroxide comprises the following steps: (1) respectively weighing 1.5-2g of nickel acetate and sodium hypophosphite, placing the nickel acetate and the sodium hypophosphite in a quartz crucible, placing the quartz crucible in a vacuum tube furnace, calcining the quartz crucible in a nitrogen atmosphere at the high temperature of 400 ℃ for 1-2 hours, and grinding the quartz crucible into powder to obtain the nickel phosphide. (2) Weighing 1.975-3.95g of bismuth nitrate and 1.209-2.418g of ferric nitrate, and respectively dispersing in 50ml of 2.5M nitric acid and deionized water; (3) mixing the solution in the step (2) in a 250ml beaker, and adjusting the pH of the solution to 10 by using 6M NaOH; (4) adding 1.06-6.36g of nickel phosphide in the step (1) and 1.06-6.36g of titanium dioxide (P25) into the step (3), magnetically stirring the nickel phosphide for 24-26 hours, then placing the nickel phosphide into an oven for drying for 24 hours at the temperature of 60-80 ℃, and grinding the nickel phosphide powder into powder to obtain a bismuth ferrite-titanium dioxide-nickel phosphide precursor; (5) placing the precursor obtained in the step (4) in a quartz crucible, placing the quartz crucible in a vacuum tube furnace, calcining for 2-3 hours at the high temperature of 600-700 ℃ under the air, grinding into powder, respectively washing with ethanol and ultrapure water, and drying at the temperature of 60-80 ℃ to obtain the bismuth ferrite-titanium dioxide-nickel phosphide nano compound; (6) the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme obtained in the step (5) is used for detecting hydrogen peroxide, and the specific process is as follows: a) dispersing 1-5 mg of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme into water to prepare a semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension with the concentration of 1-5 mg/ml; b) adding 10 microliters of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension, a color-developing agent with fixed concentration and hydrogen peroxide with different concentrations into an acetic acid-sodium acetate (acetate) buffer solution for culture; c) and (4) measuring the concentration of the hydrogen peroxide in the mixed solution obtained in the step (6) by using a spectrophotometer. The calcination temperature in the step (1) is 300-400 ℃, and the calcination time is 2-3 hours; in the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide composite material in the step (4), the mass ratio of bismuth ferrite to titanium dioxide to nickel phosphide is (1-3): 1: 1, magnetically stirring for 24-26 hours; the calcination temperature in the step (5) is 600-700 ℃, and the calcination time is 2-3 hours; the concentration of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension in the step (6) is 1-5 mg/ml, a reaction system consists of 10 microliter of 1-5 mg/ml semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension, 10 microliter of hydrogen peroxide with different concentrations, 250 microliter of 1-2 mmol/l color developing agent and 730 microliter of 0.1 mol/l acetate buffer solution, the pH value of the buffer solution is 3-5, the culture temperature is 30-50 ℃, and the culture time is 10-20 minutes.
Compared with the prior art, the invention has the following beneficial effects:
① the calcining temperature, time and heating rate in the step (1) must be controlled in a proper range to ensure that the nickel acetate and the sodium hypophosphite are fully combined under the protection of nitrogen and the synthesis of nickel phosphide is promoted.
②, controlling the mass ratio of bismuth ferrite to titanium dioxide to nickel phosphide in the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide composite material to be (1-3): 1: 1. titanium dioxide has excellent catalytic performance, nickel phosphide nano particles are not only a cocatalyst for accelerating the transfer of photo-generated electron-hole pairs, but also a good semiconductor with main performance.
③ step (5) the calcining temperature, time and heating rate must be controlled within a proper range to be fully combined in the substance to promote the synthesis of the composite material.
④ step (6) is used to detect hydrogen peroxide with a wide linear range of 8-500 micromoles/liter.
In summary, the invention relates to a method for preparing semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme and detecting hydrogen peroxide. The method comprises the following steps: mixing a certain amount of nickel acetate and sodium hypophosphite, calcining at high temperature under the protection of nitrogen, and grinding into powder to obtain the nickel phosphide. Uniformly dispersing a certain amount of commercial titanium dioxide (P25) and nickel phosphide into a bismuth ferrite synthesis system, stirring for 24 hours, drying, calcining at high temperature in air, grinding, cleaning and drying to obtain the bismuth ferrite-titanium dioxide-nickel phosphide nano composite. Adding a certain amount of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme into acetic acid-sodium acetate buffer solution containing hydrogen peroxide with different concentrations and fixed color developing agent concentration, standing and reacting for 15 minutes under the conditions of certain pH and temperature, taking out the reaction solution, and analyzing the detection effect of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme on the hydrogen peroxide by adopting a spectrophotometry. The semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme is used for detecting hydrogen peroxide, and has the advantages of high sensitivity, low pollution, low cost and the like. The semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme is convenient and rapid to detect peroxide, high in sensitivity, low in cost and environment-friendly. If the method can be marketized, better economic benefit can be obtained.
Drawings
FIG. 1 is a scanning electron microscope image of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide composite of example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide complex of example 1 of the present invention.
FIG. 3 is a diagram showing the ultraviolet absorption spectrum of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme for detecting hydrogen peroxide in example 2 of the present invention;
FIG. 4 is a graph showing the relationship between hydrogen peroxide concentration and absorbance at 652nm according to the present invention.
Detailed Description
The invention will be further illustrated with reference to specific embodiments.
The invention relates to a preparation method of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme, which sequentially comprises the following steps:
example 1
(1) 1.5g of nickel acetate and 1.5g of sodium hypophosphite are respectively weighed, placed in a quartz crucible, placed in a vacuum tube furnace, calcined at the high temperature of 300 ℃ for 2 hours in the nitrogen atmosphere, and ground into powder to obtain the nickel phosphide.
(2) Weighing 1.975g of bismuth nitrate and 1.209g of ferric nitrate, and respectively dispersing in 50ml of 2.5M nitric acid and deionized water;
(3) mixing the solution in the step (2) in a 250ml beaker, and adjusting the pH of the solution to 10 by using 6M NaOH;
(4) adding 2.2g of nickel phosphide and 2.2g of titanium dioxide (P25) in the step (1) into the step (3), magnetically stirring the nickel phosphide for 24 hours, then placing the nickel phosphide into an oven to be dried for 24 hours at the temperature of 80 ℃, and grinding the nickel phosphide into powder to obtain a bismuth ferrite-titanium dioxide-nickel phosphide precursor;
(5) placing the precursor obtained in the step (4) in a quartz crucible, placing the quartz crucible in a vacuum tube furnace, calcining for 3 hours at the high temperature of 600 ℃ in the air, grinding into powder, respectively washing with ethanol and ultrapure water, and drying at the temperature of 80 ℃ to obtain the bismuth ferrite-titanium dioxide-nickel phosphide nano composite;
fig. 1 and 2 are scanning electron micrographs of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme complex prepared in this example. It can be seen that the resulting composite has a three-dimensional structure resembling popcorn
The method for detecting hydrogen peroxide by using the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme is further illustrated by combining specific examples.
Example 2
The semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme obtained in the example 1 is used for detecting hydrogen peroxide, and the specific process is as follows:
(1) dispersing 1 mg of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme into 1 ml of water to prepare 1 mg/ml of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension;
(2) 10 microliter of a 1 mg/ml semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension, 10 microliter of hydrogen peroxide solutions with different concentrations, 250 microliter of a 1 mmol/l color-developing agent and 730 microliter of a 0.1 mol/l acetate buffer solution were mixed, the pH of the buffer solution was 4, and the mixture was incubated at 45 ℃ for 15 minutes.
(3) The absorbance of the mixed solution obtained in step (2) was measured at a wavelength of 652nm using a spectrophotometer.
FIG. 3 is a diagram of the ultraviolet absorption spectrum of the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme for detecting hydrogen peroxide with different concentrations.
Example 3
The absorbance at 652nm of example 2 was plotted against the hydrogen peroxide concentration (FIG. 4) to obtain a linear plot.
As can be seen in fig. 4: the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme keeps good linear relation with hydrogen peroxide in the range of 8 to 500 micromoles/liter. The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention. In addition to the above-mentioned examples, the present invention may be implemented in other ways, for example, by appropriately amplifying the concentration of the color-developing agent, the incubation temperature and the incubation time. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention. Technical features of the present invention which are not described may be implemented by or using the prior art, and will not be described herein.
Claims (4)
1. A preparation method of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme is characterized by comprising the following steps:
(1) respectively weighing 1.5-2g of nickel acetate and 1.5-2g of sodium hypophosphite, placing the nickel acetate and the sodium hypophosphite in a quartz crucible, placing the quartz crucible in a vacuum tube furnace, calcining the quartz crucible for 1-2 hours at the high temperature of 400 ℃ in the nitrogen atmosphere, and grinding the quartz crucible into powder nickel phosphide;
(2) weighing 1.975-3.95g of bismuth nitrate and 1.209-2.418g of ferric nitrate, and respectively dispersing in 50ml of 2.5M nitric acid and deionized water to obtain solutions;
(3) mixing the solution in the step (2) in a 250ml beaker, and adjusting the pH of the solution to 10 by using 6M NaOH;
(4) adding 1.06-6.36g of nickel phosphide in the step (1) and 1.06-6.36g of titanium dioxide (P25) into the step (3), magnetically stirring for 24-26 hours, then placing the mixture into an oven to be dried for 24 hours at the temperature of 60-80 ℃, and grinding the mixture into powder to obtain a bismuth ferrite-titanium dioxide-nickel phosphide precursor;
(5) and (3) placing the precursor obtained in the step (4) in a quartz crucible, placing the quartz crucible in a vacuum tube furnace, calcining the quartz crucible for 2 to 3 hours at the high temperature of 600-700 ℃ under the air, grinding the quartz crucible into powder, respectively washing the powder by using ethanol and ultrapure water, and drying the powder at the temperature of 60 to 80 ℃ to obtain the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme.
2. The method for preparing the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme as claimed in claim 1, wherein in the step (4), the mass ratio of bismuth ferrite to titanium dioxide to nickel phosphide is (1-3): 1: 1, the magnetic stirring time is 24 to 26 hours.
3. The method for detecting hydrogen peroxide by using the semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme prepared by the method according to any one of claims 1 to 2 is characterized by comprising the following specific steps of:
a) dispersing 1-5 mg of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme into 1 ml of water to prepare a semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension with the concentration of 1-5 mg/ml;
b) adding 10 microliters of semiconductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension, a color developing agent with fixed concentration and hydrogen peroxide with different concentrations into acetate buffer solution for culture;
c) and (4) measuring the concentration of the hydrogen peroxide in the mixed solution obtained in the step (6) by using a spectrophotometer.
4. The method of claim 1, wherein the concentration of the semi-conductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension is 1-5 mg/ml, the reaction system comprises 10 microliters of 1-5 mg/ml semi-conductor bismuth ferrite-titanium dioxide-nickel phosphide nanoenzyme suspension, 10 microliters of hydrogen peroxide with different concentrations, 250 microliters of 1-2 millimoles/liter of color-developing agent and 730 microliters of 0.1 millimole/liter of acetate buffer solution, the pH of the buffer solution is 3-5, the culture temperature is 30-50 ℃, and the culture time is 10-20 minutes.
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