CN108107101B - Three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material and application thereof - Google Patents
Three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material and application thereof Download PDFInfo
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Abstract
The invention discloses a three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material and application thereof, wherein the preparation method comprises the following steps: placing the carbon cloth in nitric acid with the concentration of 3mol/L, and reacting for 2 hours at the reaction temperature of 120 ℃ to obtain the functionalized three-dimensional carbon cloth; and soaking the functionalized three-dimensional carbon cloth in a mixture of ferric nitrate, nickel nitrate, urea and ammonium fluoride, reacting for 6-10 hours at the reaction temperature of 100-120 ℃, cooling to room temperature, washing and drying to obtain the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material. The three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material can be used as a working electrode for detecting nitrite ions in a water body. The preparation method is simple, has high charge transfer efficiency, can be used for quickly, efficiently and selectively detecting nitrite ions in water, and has a wider linear detection range and a lower detection limit.
Description
Technical Field
The invention relates to the technical field of detection of nitrite in water, in particular to a three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material and application thereof.
Background
Nitrite, an important intermediate in the nitrogen cycle, is widely present in the natural environment. In the food industry, nitrite is used as a food additive and has a certain antibacterial and antiseptic effect. However, excess nitrite entering the body oxidizes methemoglobin in the blood to methemoglobin, losing the ability to transport oxygen, and causing hypoxic damage to the tissue. In addition, nitrite can react with secondary amine which is a protein decomposition product to generate nitrosamine which is a strong carcinogen, so that the method has important significance for accurately detecting nitrite in environmental water and food.
At present, methods for detecting nitrite in water mainly include ion chromatography, chemiluminescence, spectrophotometry, raman spectroscopy, electrochemical analysis, and the like. However, most of these detection methods require the use of sophisticated instruments, complicated testing procedures and specialized sample preparation techniques, which largely hamper their practical application. Compared with other detection methods, the electrochemical analysis method has the advantages of convenient operation, simple instrument, rapidness, sensitivity, high selectivity and the like, and is deeply valued by people. However, in the existing electrochemical analysis method, the preparation process of the electrode material is complicated, and the use of the binder greatly hinders the charge transfer efficiency of the electrode surface, so that an electrode material which is simple in preparation method, high in charge transfer efficiency, and capable of rapidly, efficiently and selectively detecting nitrite ions in a water body is urgently needed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material and the application thereof, the preparation method is simple, the charge transfer efficiency is high, the nitrite ions in the water body can be rapidly, efficiently and selectively detected, and the linear detection range and the lower detection limit of the nitrite ion concentration in the water body are wide.
The purpose of the invention is realized by the following technical scheme:
a three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material comprises the following steps:
step A, placing the carbon cloth in nitric acid with the concentration of 3mol/L, and reacting for 2 hours at the reaction temperature of 100-120 ℃ to obtain the functionalized three-dimensional carbon cloth;
step B, soaking the functionalized three-dimensional carbon cloth in a mixture of ferric nitrate, nickel nitrate, urea and ammonium fluoride, reacting for 6-10 hours at the reaction temperature of 100-120 ℃, cooling to room temperature, washing and drying to obtain the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material; wherein the molar ratio of the ferric nitrate to the nickel nitrate to the urea to the ammonium fluoride is 0.5:1.5:10: 5.
Preferably, every 6cm2The dosage of the ferric nitrate required by the carbon cloth is 0.5mmol, and the dosage of the nickel nitrate is 1.5mThe mol, the dosage of urea is 10mmol, and the dosage of ammonium fluoride is 5 mmol.
Preferably, in step B, the reaction temperature is 120 ℃ and the reaction time is 8 hours.
The three-dimensional carbon cloth/nickel-iron layered hydroxide nanosheet composite material is directly used as a working electrode for detecting nitrite ions in a water body.
According to the technical scheme provided by the invention, the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material provided by the invention is prepared by taking functionalized carbon cloth as a substrate, mixing ferric nitrate, nickel nitrate, urea and ammonium fluoride according to a molar ratio of 0.5:1.5:10:5 to serve as a reactant, and reacting for 6-10 hours at 100-120 ℃ by a hydrothermal method; the three-dimensional carbon cloth/nickel-iron layered hydroxide nanosheet composite material can be directly used as a working electrode for electrochemical detection of nitrite ions in a water body without using a binder, and has a wider linear range, a lower detection limit and good selectivity, so that the preparation method is simple, the charge transfer efficiency is high, and quick, efficient and selective detection of the nitrite ions in the water body can be realized.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a scanning electron microscope photograph of the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in example 1 of the present invention.
Fig. 2 is an X-ray diffraction pattern of the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in example 1 of the present invention.
Fig. 3 is a cyclic voltammetry curve diagram of the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in example 1 of the present invention for nitrite ions of different concentrations and a linear relationship diagram of nitrite ion concentration and oxidation peak current.
Fig. 4 is a current-time curve diagram of the three-dimensional carbon cloth/nickel-iron layered hydroxide nanosheet composite material prepared in embodiment 1 according to the present invention for nitrite ions of different concentrations and a linear relationship diagram of nitrite ion concentration and current intensity.
Fig. 5 is a current-time curve diagram of the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in example 1 of the present invention for different ions.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material and the application thereof provided by the invention are described in detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art.
A three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material comprises the following steps:
and step A, placing the carbon cloth in nitric acid with the concentration of 3mol/L, and reacting for 2 hours at the reaction temperature of 100-120 ℃ to obtain the functionalized three-dimensional carbon cloth.
Step B, soaking the functionalized three-dimensional carbon cloth in ferric nitrate (namely Fe (NO)3)3) Nickel nitrate (i.e., Ni (NO))3)2) Urea (i.e., CO (NH))2)2) And ammonium fluoride (i.e., NH)4F) In the mixture, the molar ratio of the ferric nitrate to the nickel nitrate to the urea to the ammonium fluoride is 0.5:1.5:10:5, and the reaction temperature is 100-120 DEG CReacting for 6-10 hours, cooling to room temperature, washing and drying to obtain the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material.
In particular, every 6cm2The using amount of the ferric nitrate required by the carbon cloth is 0.5mmol, the using amount of the nickel nitrate is 1.5mmol, the using amount of the urea is 10mmol, and the using amount of the ammonium fluoride is 5mmol, so that the prepared three-dimensional carbon cloth/nickel-iron layered hydroxide nanosheet composite material has good charge transfer efficiency, and nitrite ions in a water body can be rapidly, efficiently and selectively detected; for example: if the carbon cloth with the size of 2cm multiplied by 3cm is made into the functionalized three-dimensional carbon cloth in the step A, 0.5mmol of ferric nitrate, 1.5mmol of nickel nitrate, 10mmol of urea and 5mmol of ammonium fluoride are preferably dissolved in 35ml of deionized water in the step B, the two materials are mixed together, the functionalized three-dimensional carbon cloth is soaked in the mixture and is continuously stirred for 10 minutes, then the mixture is transferred into a 50ml high-pressure reaction kettle and reacts for 8 hours at the temperature of 120 ℃, the temperature is cooled to room temperature after the reaction is finished, the obtained product is taken out and fully washed to remove the physical attachments on the surface of the product, and then the product is dried at the temperature of 60 ℃, so that the three-dimensional carbon cloth/nickel iron layered nanosheet hydroxide composite material can be prepared.
Further, the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material provided by the invention can be directly used as a working electrode for electrochemical detection of nitrite ions in a water body without using a binder, and the specific embodiment thereof is as follows: on CHI760E electrochemical workstation, the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material provided by the invention is directly used as a working electrode, a silver/silver chloride electrode is used as a reference electrode, a platinum wire electrode is used as a counter electrode for electrochemical detection, and Na is used at room temperature2HPO4And NaH2PO4Preparing phosphate buffer solution with pH value of 7 and concentration of 0.1mol/L as electrolyte solution, introducing nitrogen gas continuously, adding sodium nitrite solution with different amount under the condition of continuous stirring, and adopting Cyclic Voltammetry (CV) and time powerThe flow curve (I-T) electrochemical technology is used for signal monitoring, and the detection limit is calculated according to the linear relation between the electrochemical signal and the concentration of the added nitrite ions, so that the following conditions can be obtained: the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material provided by the invention can be used for quickly, efficiently and selectively detecting nitrite ions in a water body, and has a wider linear detection range and a lower detection limit on the concentration of the nitrite ions in the water body.
In conclusion, the embodiment of the invention has the advantages of simple preparation method, high charge transfer efficiency, capability of quickly, efficiently and selectively detecting nitrite ions in the water body, and wider linear detection range and lower detection limit on the concentration of nitrite ions in the water body.
In order to more clearly show the technical scheme and the technical effects provided by the present invention, the following detailed description of the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material and the application thereof are provided in specific embodiments.
Example 1
A three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material comprises the following steps:
step a, placing the carbon cloth with the size of 2cm multiplied by 3cm in a high-pressure reaction kettle filled with 3mol/L nitric acid, and reacting for 2 hours at the reaction temperature of 120 ℃, thereby preparing the functionalized three-dimensional carbon cloth.
And b, dissolving 0.5mmol of ferric nitrate, 1.5mmol of nickel nitrate, 10mmol of urea and 5mmol of ammonium fluoride in the same 35ml of deionized water, mixing the ferric nitrate, the nickel nitrate, the urea and the ammonium fluoride together, soaking the functionalized three-dimensional carbon cloth in the mixture, continuously stirring for 10 minutes, transferring the mixture into a 50ml high-pressure reaction kettle, reacting for 8 hours at 120 ℃, cooling to room temperature after the reaction is finished, taking out the obtained product, fully washing to remove physical attachments on the surface of the product, and drying the product at 60 ℃ to obtain the three-dimensional carbon cloth/nickel-iron layered hydroxide nanosheet composite material.
Specifically, microstructure observation, composition analysis and nitrite ion electrochemical detection effect test are performed on the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in embodiment 1 of the invention, so that the following test results are obtained:
(1) observing and shooting the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in the embodiment 1 of the invention by using a scanning electron microscope, so as to obtain a scanning electron microscope picture shown in fig. 1; wherein, fig. 1a is a scanning electron microscope picture of the functionalized three-dimensional carbon cloth prepared in the embodiment 1 of the present invention; fig. 1b, fig. 1c and fig. 1d are scanning electron microscope pictures of the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material in example 1 of the present invention at different resolutions. As can be seen from fig. 1 a: the functionalized three-dimensional carbon cloth prepared in the step a in the embodiment 1 of the invention is of a three-dimensional beam-shaped interweaving structure, and the surface of the functionalized three-dimensional carbon cloth is smooth; as can be seen from fig. 1b, 1c and 1 d: the three-dimensional carbon cloth/nickel-iron layered hydroxide nanosheet composite material prepared in the embodiment 1 of the invention is prepared through simple hydrothermal reaction, and the surface of the three-dimensional carbon cloth is rough and uniformly distributed with a nickel-iron layered hydroxide nanosheet array.
(2) Analyzing the components of the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in the embodiment 1 of the invention by using an X-ray diffractometer, so as to obtain an X-ray diffraction pattern shown in figure 2; in fig. 2, the ordinate represents intensity and the abscissa represents 2 θ (i.e., diffraction angle). As can be seen from fig. 2: diffraction peaks of the final product prepared in the embodiment 1 of the invention at 11.4 degrees, 23.2 degrees, 33.6 degrees, 34.3 degrees, 38.8 degrees, 46.4 degrees, 59.8 degrees and 61.2 degrees can be matched with Ni0.75Fe0.25(CO3)0.125(OH)2·0.38H2O (JCPDS.40-0215) has one-to-one correspondence between the (003), (006), (101), (012), (015), (018), (110) and (113) crystal planes, which indicates that the product prepared in example 1 of the present invention is indeed a nickel-iron layered hydroxide.
(3) The three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in the embodiment 1 of the invention is used as a working electrode, a saturated calomel electrode is used as a reference electrode, and a platinum wire electrode is used as a platinum wire electrodeCounter electrode, then under the condition of room temperature, taking phosphate buffer solution with pH value of 7 and concentration of 0.1mol/L as electrolyte solution, continuously introducing nitrogen, under the condition of continuously stirring, adding sodium nitrite solutions with different amounts, and utilizing cyclic voltammetry (sweep rate of 50mV/s) to carry out electrochemical detection on nitrite ions in water body, thereby obtaining a cyclic voltammetry curve chart and a linear relation chart of nitrite ion concentration and oxidation peak current shown in figure 3; fig. 3a is a cyclic voltammetry curve diagram of the three-dimensional carbon cloth/nickel-iron layered hydroxide nanosheet composite material prepared in example 1 of the present invention for nitrite ions of different concentrations, and fig. 3b is a linear relationship diagram of nitrite ion concentration and oxidation peak current of the three-dimensional carbon cloth/nickel-iron layered hydroxide nanosheet composite material prepared in example 1 of the present invention. As can be seen from fig. 3a and 3 b: with the addition of nitrite ions, a peak potential, namely an oxidation peak of nitrite ions, appears at a potential of about 0.9V; in addition, the oxidation peak current increases with the concentration of nitrite ions, and the peak current and the concentration of nitrite ions are in a linear relation, and the linear equation is Ipa(mA)＝0.47+0.54C(mM)，R2＝0.994。
(4) On CHI760E electrochemical workstation, the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in the embodiment 1 of the invention is directly used as a working electrode, a silver/silver chloride electrode is used as a reference electrode, a platinum wire electrode is used as a counter electrode for electrochemical detection, under the condition of room temperature, phosphate buffer solution with the pH value of 7 and the concentration of 0.1mol/L is taken as electrolyte solution, nitrogen is continuously introduced, under the condition of continuous stirring, adding sodium nitrite solution with different amounts, utilizing current-time curve method (oxidation potential is 0.9V) to measure linear range of nitrite ions in water body, and calculates the detection limit of the nitrite ions by the linear relationship between the electrochemical signal and the concentration of the added nitrite ions, thereby obtaining a current-time curve chart and a linear relation chart of the nitrite ion concentration and the current intensity as shown in figure 4; wherein, fig. 4a shows that the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in example 1 of the present invention has different pairsFig. 4b is a linear relationship diagram of the nitrite ion concentration and the current intensity of the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in example 1 of the present invention. As can be seen from fig. 4a and 4 b: in the three-dimensional carbon cloth/nickel-iron layered hydroxide nanosheet composite material prepared in the embodiment 1 of the invention, the nitrite ion concentration and the current intensity have a good linear relation (R) in the range of 5-1000 mu M of nitrite ion concentration20.999), linear equation is Ipa(μ a) ═ 0.8036C (μ M) +73.69, with a detection limit of 0.02 μ M.
(5) The three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in the embodiment 1 of the invention is directly used as a working electrode for detecting nitrite ions, and the selectivity of the working electrode is tested by using a current-time curve method (the oxidation potential is 0.9V) in a phosphate buffer solution with the pH value of 7 and the concentration of 0.1mol/L, so that a current-time curve graph of the working electrode on different ions shown in FIG. 5 is obtained. As can be seen from fig. 5: after adding other interfering ions (e.g. NO)3 -、CH3COO-、CO3 2-、SO4 2-、Zn2+、Cl-、K+、Mg2+、Ca2+、NaBrO3、NaIO3And H2O2) When NO is added, the current does not change but once NO is added2 -The current can be increased within a short time, which shows that the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material prepared in the embodiment 1 of the invention has good selectivity when being directly used as a working electrode for detecting nitrite ions.
In conclusion, the embodiment of the invention has the advantages of simple preparation method, high charge transfer efficiency, capability of quickly, efficiently and selectively detecting nitrite ions in the water body, and wider linear detection range and lower detection limit on the concentration of nitrite ions in the water body.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (4)
1. A three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material is characterized in that the preparation method comprises the following steps:
step A, placing the carbon cloth in nitric acid with the concentration of 3mol/L, and reacting for 2 hours at the reaction temperature of 100-120 ℃ to obtain the functionalized three-dimensional carbon cloth;
step B, soaking the functionalized three-dimensional carbon cloth in a mixture of ferric nitrate, nickel nitrate, urea and ammonium fluoride, reacting for 6-10 hours at the reaction temperature of 100-120 ℃, cooling to room temperature, washing and drying to obtain the three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material;
wherein the molar ratio of the ferric nitrate to the nickel nitrate to the urea to the ammonium fluoride is 0.5:1.5:10: 5.
2. The three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite of claim 1, wherein each 6cm of the composite is2The dosage of the ferric nitrate, the nickel nitrate, the urea and the ammonium fluoride required by the carbon cloth is 0.5mmol, 1.5mmol, 10mmol and 5mmol respectively.
3. The three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite of claim 1 or 2, wherein in step B, the reaction temperature is 120 ℃ and the reaction time is 8 hours.
4. The three-dimensional carbon cloth/nickel iron layered hydroxide nanosheet composite material of any one of claims 1 to 3 is directly used as a working electrode for detecting nitrite ions in a water body.
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