CN109811396B - Porous zinc and preparation and application thereof - Google Patents
Porous zinc and preparation and application thereof Download PDFInfo
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- CN109811396B CN109811396B CN201910068632.4A CN201910068632A CN109811396B CN 109811396 B CN109811396 B CN 109811396B CN 201910068632 A CN201910068632 A CN 201910068632A CN 109811396 B CN109811396 B CN 109811396B
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- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 70
- 239000011701 zinc Substances 0.000 title claims abstract description 70
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 28
- PGTXKIZLOWULDJ-UHFFFAOYSA-N [Mg].[Zn] Chemical compound [Mg].[Zn] PGTXKIZLOWULDJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000011148 porous material Substances 0.000 claims abstract description 18
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 16
- 239000011777 magnesium Substances 0.000 claims abstract description 16
- 235000014653 Carica parviflora Nutrition 0.000 claims abstract description 10
- 241000243321 Cnidaria Species 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000002848 electrochemical method Methods 0.000 claims abstract 2
- 230000007797 corrosion Effects 0.000 claims description 25
- 238000005260 corrosion Methods 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 23
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
- 238000006056 electrooxidation reaction Methods 0.000 claims description 12
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 9
- 229910052697 platinum Inorganic materials 0.000 claims description 9
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 9
- 239000002105 nanoparticle Substances 0.000 claims description 8
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 6
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 6
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003792 electrolyte Substances 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- GTKRFUAGOKINCA-UHFFFAOYSA-M chlorosilver;silver Chemical compound [Ag].[Ag]Cl GTKRFUAGOKINCA-UHFFFAOYSA-M 0.000 claims 1
- 230000003385 bacteriostatic effect Effects 0.000 abstract description 5
- 229910045601 alloy Inorganic materials 0.000 description 21
- 239000000956 alloy Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 14
- BJLGEGPJEIZYQY-UHFFFAOYSA-M C1(OCCO1)=O.Cl(=O)(=O)(=O)[O-].[Li+] Chemical compound C1(OCCO1)=O.Cl(=O)(=O)(=O)[O-].[Li+] BJLGEGPJEIZYQY-UHFFFAOYSA-M 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 239000007783 nanoporous material Substances 0.000 description 4
- 241000588724 Escherichia coli Species 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- -1 nano porous zinc Chemical compound 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002504 physiological saline solution Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The invention relates to porous zinc and preparation and application thereof, and a preparation method of nano porous zinc comprises the following steps: (1) mixing zinc and magnesium, and heating to a molten state to obtain a zinc-magnesium alloy; then cooling to room temperature; (2) an electrochemical method, namely removing magnesium in the zinc-magnesium alloy obtained in the step (1); then cleaning and drying to obtain the nano porous zinc. The nano-porous zinc has a microstructure like coral, and has a pore channel structure and a zinc skeleton structure which are mutually communicated. Meanwhile, the application of the nano-porous zinc in the bacteriostatic field is provided.
Description
Technical Field
The invention belongs to the research field of nano porous materials, and particularly relates to porous nano zinc and preparation and application thereof.
Background
The porous metal is a material with larger specific surface area than a bulk material, wherein the nano-porous material has the unique physical and chemical properties of the nano-material due to the nano-size, and has great application prospects in catalysis, sensing, surface-enhanced Raman scattering and the like at present. At present, the nano porous metal material is mainly an inert metal nano porous material. The preparation of more active metal nanoporous materials has not been reported.
The prior art can only prepare porous structures of relatively inert metals and cannot prepare porous structures of metals as active as zinc. The porous structure of active metal zinc, namely nano porous zinc, is prepared by the method.
Disclosure of Invention
The invention solves the problems: overcomes the defects of the prior art, provides porous zinc and preparation and application thereof, and has good bacteriostatic function.
In order to overcome the problems in the prior art, the invention aims to provide nano-porous zinc and preparation and application thereof.
In order to achieve the above objects and other related objects, the present invention adopts the following technical solutions:
in a first aspect of the invention, a preparation method of nano-porous zinc is provided, which comprises the following steps:
(1) mixing zinc and magnesium, and heating to a molten state to obtain a zinc-magnesium alloy; then cooling to room temperature;
(2) and (2) removing magnesium in the zinc-magnesium alloy obtained in the step (1) by adopting electrochemical corrosion, cutting the zinc-magnesium alloy, placing the zinc-magnesium alloy in a ethylene carbonate solution of lithium perchlorate, corroding by adopting a constant potential electrochemical corrosion method, taking Ag/AgCl as a reference electrode, a platinum electrode as a counter electrode and the zinc-magnesium alloy as a working electrode, applying voltage on the zinc-magnesium alloy electrode, and finishing the corrosion when the corrosion current is lower than 50 mu A. (ii) a Then cleaning and drying the nano-porous zinc.
Preferably, in the step (1), the atomic ratio of zinc and magnesium is (15-50): (85-50).
Preferably, in the step (1), the atomic ratio of zinc and magnesium is (25-35): (75-65).
Preferably, in the step (1), the heating temperature is in the range of 600 ℃ to 800 ℃; the heating time is 1-10 h.
Preferably, in the step (1), the heating temperature is in the range of 600 ℃ to 800 ℃; the heating time is 3-6 h.
Preferably, in the step (1), the cooling speed is 1-35 ℃/min.
Preferably, in the step (1), the cooling speed is 10 ℃/min to 25 ℃/min.
Preferably, in the step (2), the electrolyte is lithium perchlorate, and the electrochemical corrosion voltage is-1.2V to-1.4V.
Preferably, in the step (2), the concentration of the lithium perchlorate in the ethylene carbonate solution is in the range of 0.05M to 0.5M.
Preferably, in the step (2), the concentration of the lithium perchlorate in the ethylene carbonate solution is in the range of 0.3M to 0.5M.
Preferably, in the step (2), distilled water and ethanol are used for washing.
In a second aspect of the invention, there is provided a nanoporous zinc obtained by the aforementioned preparation method. Preferably, the copper-based composite material comprises a continuous nanometer-sized copper framework and a continuous nanometer-sized pore canal, wherein the nanometer-sized pore canal is communicated with each other, the nanometer-sized copper framework is communicated with each other, and the nanometer-sized copper framework and the nanometer-sized pore canal are mutually interpenetrated.
In a third aspect of the invention, the application of the nano-porous zinc in the bacteriostatic field is provided.
Compared with the prior art, the invention has the following beneficial effects: the invention uses electrochemical corrosion method to prepare active metal zinc porous material, namely nano porous zinc, which is block-shaped by macroscopic observation; the microscopic structure is like coral observed by an electronic scanning microscope and comprises a continuous nanometer copper framework and a continuous nanometer pore canal, the nanometer pore canal is communicated with each other, the nanometer copper framework is communicated with each other, and the nanometer copper framework and the nanometer pore canal are mutually interpenetrated.
Drawings
FIG. 1 is a scanning electron micrograph of the internal structure of the prepared nanoporous zinc of example 1 of the present invention;
FIG. 2 is a comparison diagram of an embodiment of the present invention; as shown in FIG. 2, the tube No. 4 is a control group, and it can be found that the tube Nos. 1, 2 and 3 have obvious bacteriostatic effect on Escherichia coli with porous zinc contents of 50 μ g, 100 μ g and 150 μ g, respectively, while the bacteria in the control group reproduce normally.
Detailed Description
Before the present embodiments are further described, it is to be understood that the scope of the invention is not limited to the particular embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition to the specific methods, devices, and materials used in the examples, any methods, devices, and materials similar or equivalent to those described in the examples may be used in the practice of the invention in addition to the specific methods, devices, and materials used in the examples, in keeping with the knowledge of one skilled in the art and with the description of the invention.
Example 1
(1) According to the proportion that 15 percent of zinc and the balance of magnesium are mixed according to atomic percentage, the temperature is raised to 600 ℃ and kept for 4 hours. After 4 hours, the temperature was lowered to room temperature at 1 ℃ per minute.
(2) Cutting an alloy cube of 2mm x 2mm from the smelted alloy, placing the alloy cube in a lithium perchlorate ethylene carbonate solution with the concentration of 0.05M, adopting a constant potential electrochemical corrosion method to carry out corrosion, taking Ag/AgCl as a reference electrode, a platinum electrode as a counter electrode and a zinc-magnesium alloy as a working electrode, applying a voltage of-1.2V to the zinc-magnesium alloy electrode, and when the corrosion current is lower than 50 muA, judging that the corrosion is finished.
The nano-porous zinc prepared by the embodiment is observed by a scanning electron microscope, and the microstructure of the nano-porous zinc is like coral, and comprises a continuous nano-zinc framework and a continuous nano-pore canal.
Example 2
(1) According to the proportion that 30 percent of the atomic percent is zinc and the rest is magnesium, the temperature is increased to 800 ℃, and the temperature is kept for 5 hours. After 5 hours, the temperature was reduced to room temperature at 15 ℃ per minute.
(2) Cutting an alloy cube of 2mm x 2mm from the smelted alloy, placing the alloy cube in a lithium perchlorate ethylene carbonate solution with the concentration of 0.5M, adopting a constant potential electrochemical corrosion method to carry out corrosion, taking Ag/AgCl as a reference electrode, a platinum electrode as a counter electrode and a zinc-magnesium alloy as a working electrode, applying a voltage of-1.4V to the zinc-magnesium alloy electrode, and when the corrosion current is lower than 50 muA, judging that the corrosion is finished.
The nano-porous zinc prepared by the embodiment of the invention is observed by a scanning electron microscope, and the microstructure of the nano-porous zinc is like coral, and comprises a continuous nano-zinc framework and a continuous nano-pore canal.
Example 3
(1) The temperature was raised to 700 c at 50 atomic percent zinc, the remainder being magnesium, and held at that temperature for 3 hours. After 3 hours, the temperature was reduced to room temperature at 12 ℃ per minute.
(2) Cutting an alloy cube of 2mm x 2mm from the smelted alloy, placing the alloy cube in a lithium perchlorate ethylene carbonate solution with the concentration of 0.35M, adopting a constant potential electrochemical corrosion method to carry out corrosion, taking Ag/AgCl as a reference electrode, a platinum electrode as a counter electrode and a zinc-magnesium alloy as a working electrode, applying a voltage of-1.3V to the zinc-magnesium alloy electrode, and when the corrosion current is lower than 50 muA, judging that the corrosion is finished.
As shown in fig. 1, the nano-porous zinc prepared by the present embodiment of the invention is observed by a scanning electron microscope, and the microstructure of the nano-porous zinc is like coral, and comprises a continuous nano-sized zinc skeleton and a continuous nano-sized pore channel.
Example 4
(1) The temperature was raised to 780 ℃ at 25 atomic percent zinc and the balance magnesium and held at this temperature for 2 hours. After 2 hours, the temperature was reduced to room temperature at 2 ℃ per minute.
(2) Cutting an alloy cube of 2mm x 2mm from the smelted alloy, placing the alloy cube in a lithium perchlorate ethylene carbonate solution with the concentration of 0.25M, adopting a constant potential electrochemical corrosion method to carry out corrosion, taking Ag/AgCl as a reference electrode, a platinum electrode as a counter electrode and a zinc-magnesium alloy as a working electrode, applying a voltage of-1.3V to the zinc-magnesium alloy electrode, and when the corrosion current is lower than 50 muA, judging that the corrosion is finished.
The nano-porous zinc prepared by the embodiment is observed by a scanning electron microscope, and the microstructure of the nano-porous zinc is like coral, and comprises a continuous nano-zinc framework and a continuous nano-pore canal.
Example 5
(1) The temperature was raised to 950 ℃ at 40 atomic percent zinc, the balance magnesium, and held at this temperature for 5 hours. After 5 hours, the temperature was reduced to room temperature at 20 ℃ per minute.
(2) Cutting an alloy cube of 2mm x 2mm from the smelted alloy, placing the alloy cube in a lithium perchlorate ethylene carbonate solution with the concentration of 0.2M, adopting a constant potential electrochemical corrosion method to carry out corrosion, taking Ag/AgCl as a reference electrode, a platinum electrode as a counter electrode and a zinc-magnesium alloy as a working electrode, applying a voltage of-1.25V to the zinc-magnesium alloy electrode, and when the corrosion current is lower than 50 muA, judging that the corrosion is finished.
The nano-porous zinc prepared by the embodiment of the invention is observed by a scanning electron microscope, and the microstructure of the nano-porous zinc is like coral, and comprises a continuous nano-zinc framework and a continuous nano-pore canal.
Example 6
(1) The temperature was raised to 650 ℃ at 35 atomic percent zinc, the remainder being magnesium, and held at this temperature for 6 hours. After 6 hours, the temperature was reduced to 7 ℃ per minute and the temperature was reduced to room temperature.
(2) Cutting an alloy cube of 2mm x 2mm from the smelted alloy, placing the alloy cube in a lithium perchlorate ethylene carbonate solution with the concentration of 0.15M, adopting a constant potential electrochemical corrosion method to carry out corrosion, taking Ag/AgCl as a reference electrode, a platinum electrode as a counter electrode and a zinc-magnesium alloy as a working electrode, applying a voltage of-1.35V to the zinc-magnesium alloy electrode, and when the corrosion current is lower than 50 muA, judging that the corrosion is finished.
The nano-porous zinc prepared by the embodiment of the invention is observed by a scanning electron microscope, and the microstructure of the nano-porous zinc is like coral, and comprises a continuous nano-zinc framework and a continuous nano-pore canal.
Example 7
(1) The temperature was raised to 730 ℃ at 45 atomic% zinc and the remainder magnesium, and held at this temperature for 1 hour. After 1 hour, the temperature was reduced to 25 ℃ per minute and the temperature was reduced to room temperature.
(2) Cutting an alloy cube of 2mm x 2mm from the smelted alloy, placing the alloy cube in a lithium perchlorate ethylene carbonate solution with the concentration of 0.1M, adopting a constant potential electrochemical corrosion method to carry out corrosion, taking Ag/AgCl as a reference electrode, a platinum electrode as a counter electrode and a zinc-magnesium alloy as a working electrode, applying a voltage of-1.27V to the zinc-magnesium alloy electrode, and when the corrosion current is lower than 50 muA, judging that the corrosion is finished.
The nano-porous zinc prepared by the embodiment of the invention is observed by a scanning electron microscope, and the microstructure of the nano-porous zinc is like coral, and comprises a continuous nano-zinc framework and a continuous nano-pore canal.
Example 8
(1) 100 μ L of sterilized normal saline solution is added into EP tube 1.5m L, labeled as 1, 2, 3, 4, 50 μ g, 100 μ g, 150 μ g porous zinc is added into tubes 1, 2, 3, respectively, and ultrasonic dispersion is performed.
(2) Taking 10 μ L of 107CFU/m L Escherichia coli is added into the above four EP tubes respectively, and placed into a shaker at 37 deg.C for 25min, 10 μ L of the mixed solution is added into 990 μ L of physiological saline, and shaken well.
(3) From the above (2), 100. mu.L of the solution was uniformly applied to a plate. Photographs were taken after 2 days of growth.
As shown in FIG. 2, tube No. 4 is a control group, and it can be found that tubes No. 1, 2 and 3 have obvious bacteriostatic effect on Escherichia coli, while the bacteria in the control group reproduce normally.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and equivalent arrangements, which are equivalent to the embodiments of the present invention, without departing from the spirit and scope of the present invention, and which may be made by utilizing the techniques disclosed above; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the nano-porous zinc is characterized by comprising the following steps:
(1) mixing zinc and magnesium, and heating to a molten state to obtain a zinc-magnesium alloy; then cooling to room temperature;
(2) and (2) removing magnesium in the zinc-magnesium alloy obtained in the step (1) by adopting an electrochemical method, cutting the zinc-magnesium alloy, placing the cut zinc-magnesium alloy in a ethylene carbonate solution of lithium perchlorate, corroding by adopting a constant potential electrochemical corrosion method, taking Ag/AgCl as a reference electrode, a platinum electrode as a counter electrode and the zinc-magnesium alloy as a working electrode, applying voltage on the zinc-magnesium alloy electrode, and when the corrosion current is lower than 50 mu A, determining that the corrosion is finished, then cleaning and drying to obtain the nano porous zinc.
2. The method for preparing nanoporous zinc according to claim 1, wherein: in the step (1), the atomic ratio range of zinc and magnesium is (15-50): (85-50).
3. The method for preparing nanoporous zinc according to claim 1, wherein: in the step (1), the heating temperature range is 600-800 ℃; the heating time is 1-6 h.
4. The method for preparing nanoporous zinc according to claim 1, wherein: in the step (1), the cooling speed is 1-25 ℃/min.
5. The method for preparing nanoporous zinc according to claim 1, wherein: in the step (2), the electrolyte is lithium perchlorate, the voltage is-1.2V-1.4V, and the reference electrode is a silver-silver chloride electrode.
6. The method for preparing nanoporous zinc according to claim 1, wherein: in the step (2), the concentration range of the ethylene carbonate solution of the electrolyte is 0.05M-0.5M.
7. The method for preparing nanoporous zinc according to claim 1, wherein: in the step (2), the action time is 24-96 h.
8. The method for preparing nanoporous zinc according to claim 1, wherein: and (3) cleaning by using distilled water and ethanol in the step (2).
9. A nanoporous zinc obtainable by the process according to any one of claims 1 to 8, wherein: the microstructure of the nano-porous zinc is like coral, and comprises continuous nano-sized zinc frameworks and continuous nano-sized pore canals, wherein the nano-sized pore canals are communicated with each other, the nano-sized zinc frameworks are communicated with each other, and the nano-sized zinc frameworks and the nano-sized pore canals are mutually interpenetrated.
10. Use of nanoporous zinc according to claim 9 in the field of bacteriostasis.
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Denomination of invention: A Kind of Porous Zinc and Its Preparation and Application Effective date of registration: 20230719 Granted publication date: 20200428 Pledgee: Bank of China Limited Shijiazhuang Gaocheng sub branch Pledgor: Changzhou Zhiyi Zinc Industry Co.,Ltd. Registration number: Y2023980048816 |
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Denomination of invention: A porous zinc and its preparation and application Granted publication date: 20200428 Pledgee: Bank of China Limited Shijiazhuang Gaocheng sub branch Pledgor: Changzhou Zhiyi Zinc Industry Co.,Ltd. Registration number: Y2024980035981 |
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