CN111355134A - Fullerene negative ion release head, preparation method thereof and negative ion generating electrode - Google Patents
Fullerene negative ion release head, preparation method thereof and negative ion generating electrode Download PDFInfo
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- CN111355134A CN111355134A CN201811573785.6A CN201811573785A CN111355134A CN 111355134 A CN111355134 A CN 111355134A CN 201811573785 A CN201811573785 A CN 201811573785A CN 111355134 A CN111355134 A CN 111355134A
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- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 207
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims abstract description 201
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 150000002500 ions Chemical class 0.000 claims abstract description 93
- 150000001450 anions Chemical class 0.000 claims abstract description 45
- 239000007864 aqueous solution Substances 0.000 claims abstract description 41
- 229910052751 metal Inorganic materials 0.000 claims abstract description 37
- 239000002184 metal Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 36
- 238000000151 deposition Methods 0.000 claims abstract description 21
- 230000004048 modification Effects 0.000 claims abstract description 17
- 238000012986 modification Methods 0.000 claims abstract description 17
- -1 oxygen ions Chemical class 0.000 claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- 239000011259 mixed solution Substances 0.000 claims description 28
- 239000003960 organic solvent Substances 0.000 claims description 21
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 19
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 19
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 19
- 239000004094 surface-active agent Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 15
- 239000002244 precipitate Substances 0.000 claims description 14
- 238000002390 rotary evaporation Methods 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 11
- 230000004913 activation Effects 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical class CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- UYMKPFRHYYNDTL-UHFFFAOYSA-N ethenamine Chemical group NC=C UYMKPFRHYYNDTL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
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- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 27
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 24
- 238000012360 testing method Methods 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 15
- 229910021641 deionized water Inorganic materials 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 12
- 238000005119 centrifugation Methods 0.000 description 12
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 9
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- 238000001704 evaporation Methods 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
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- 239000000835 fiber Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052754 neon Inorganic materials 0.000 description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000005456 alcohol based solvent Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 238000012733 comparative method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01T—SPARK GAPS; OVERVOLTAGE ARRESTERS USING SPARK GAPS; SPARKING PLUGS; CORONA DEVICES; GENERATING IONS TO BE INTRODUCED INTO NON-ENCLOSED GASES
- H01T23/00—Apparatus for generating ions to be introduced into non-enclosed gases, e.g. into the atmosphere
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/152—Fullerenes
- C01B32/156—After-treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01T—SPARK GAPS; OVERVOLTAGE ARRESTERS USING SPARK GAPS; SPARKING PLUGS; CORONA DEVICES; GENERATING IONS TO BE INTRODUCED INTO NON-ENCLOSED GASES
- H01T19/00—Devices providing for corona discharge
- H01T19/04—Devices providing for corona discharge having pointed electrodes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a fullerene negative ion release head and a preparation method thereof. The fullerene negative ion releasing head comprises a conductive metal wire and a fullerene layer, wherein the fullerene layer is formed on the surface of the conductive metal wire. The method comprises the following steps: carrying out surface modification on fullerene; preparing fullerene aqueous solution by using fullerene after surface modification; and putting the conductive metal wire into the fullerene aqueous solution, and depositing and growing a fullerene layer on the surface of the conductive metal wire to obtain the fullerene negative ion release head. The invention also discloses an anion generating electrode. The preparation method provided by the invention improves the production efficiency of the negative ion release head, is safe and environment-friendly, and the prepared fullerene negative ion release head can generate ecological-grade small-particle-size negative oxygen ions with small particle size, high activity and long migration distance, and has high negative ion purity and long service life.
Description
Technical Field
The invention relates to a negative ion generating technology, in particular to a fullerene negative ion release head, a preparation method thereof and a negative ion generating electrode.
Background
At present, the most advanced anion generation technology at home and abroad basically adopts a negative high voltage source to make carbon fibers into a discharge electrode, namely an anion release head. The negative ion releasing head is fixed on the metal rod to form a negative ion generating electrode. When the negative ion generating electrode is applied, the negative ion generating electrode is connected with a high-voltage power supply, the negative ion releasing head sprays electrons to the surrounding space at a high speed, the electrons are quickly captured by air ions to form air negative ions, and meanwhile, the positive ions are neutralized and reduced by utilizing the potential induction of a negative electric field to obtain a relatively purified negative ion field. The carbon fiber material adopted by the relatively advanced anion release head on the market at present is mainly fullerene (C60). The fullerene is a superconducting material with the resistance close to zero, is beneficial to the free precipitation of electric ions, can generate ecological-grade small-particle-size negative oxygen ions with small particle size, high activity and long migration distance, has high negative ion purity, and hardly generates byproducts such as ozone, nitrogen oxides, positive ions and the like.
However, fullerenes are poorly soluble in water, limiting the use of aqueous fullerene solutions for the preparation of negative ion-releasing heads. Fullerene can only be dissolved in an organic solvent, but fullerene dispersions prepared using organic solvents cannot be directly used for preparing negative ion release heads.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a fullerene negative ion release head, a preparation method thereof and a negative ion generating electrode. The method for preparing the fullerene negative ion release head can avoid the problem of directly dissolving fullerene in water, improve the production efficiency of the negative ion release head and reduce the cost.
In order to achieve the above object, in a first aspect, an embodiment of the present invention provides a fullerene negative ion releasing head including a conductive wire and a fullerene layer formed on a surface of the conductive wire.
In an embodiment of the invention, the thickness of the fullerene layer may be 2 to 10 nm.
In an embodiment of the present invention, the conductive metal wire may be a titanium wire, a molybdenum wire, a tungsten wire, or an iron wire.
In a second aspect, embodiments of the present invention provide a method for preparing a fullerene negative ion release head, the method comprising:
carrying out surface modification on fullerene;
preparing fullerene aqueous solution by using fullerene after surface modification; and
and putting the conductive metal wire into the fullerene aqueous solution, and depositing and growing a fullerene layer on the surface of the conductive metal wire to obtain the fullerene negative ion release head.
In an embodiment of the present invention, the surface modification of fullerene may include:
dissolving fullerene in an organic solvent to obtain a first mixed solution;
dissolving a surfactant in a dispersing agent to obtain a second mixed solution;
mixing the first mixed solution with the second mixed solution so as to modify the surface of fullerene; and
and (5) removing impurities from the system.
In an embodiment of the invention, the surfactant may be an N-vinyl amide surfactant, optionally polyvinylpyrrolidone.
In an embodiment of the present invention, the dispersant may be selected from any one or more of aromatic hydrocarbons, halogenated aromatic hydrocarbons, alcohol solvents, and halogenated alkanes, and optionally, chloroform.
In an embodiment of the invention, the mass ratio of the fullerene to the surfactant may be 1:80 to 200, optionally 1:100 to 150.
In an embodiment of the present invention, the dissolving of the fullerene in the organic solvent may include: mixing fullerene with an organic solvent in a container, and ultrasonically dispersing until no fullerene is attached to the inner wall of the container and the solution in the container is not layered.
In an embodiment of the present invention, the performing impurity removal processing on the system may include:
performing rotary evaporation on the system until the solution in the system is completely evaporated to dryness;
mixing the solid obtained by rotary evaporation with water, and performing ultrasonic dispersion; and
and adding water into the solution subjected to ultrasonic dispersion, and centrifuging until the pH value of the lower-layer precipitate is 6.5-7.5 to obtain the fullerene with the modified surface.
In embodiments of the invention, the temperature of the rotary evaporation may be 50 to 100 ℃, optionally 60 to 80 ℃.
In an embodiment of the present invention, the preparing the fullerene aqueous solution using the surface-modified fullerene may include:
dissolving the fullerene with the modified surface in water to obtain a primary aqueous solution of the fullerene;
concentrating the primary aqueous solution to obtain a concentrated solution; and
and activating the concentrated solution to obtain the fullerene aqueous solution.
In an embodiment of the present invention, the concentration process may include: and drying the primary aqueous solution at the temperature of 20-30 ℃ for 3-5 hours.
In an embodiment of the present invention, the activation treatment may include: and sintering the concentrated solution in an inert atmosphere at 90-120 ℃ for 0.5-1.5 hours, and controlling the concentrated solution in the fullerene aqueous solution, wherein the volume fraction of fullerene is 5-30%.
In the embodiment of the present invention, the method used when the fullerene layer is deposited and grown on the surface of the conductive metal wire may be a vertical deposition method.
In an embodiment of the present invention, the conditions of the vertical deposition method may include: the temperature is 50-120 ℃, and optionally, the temperature is 60-100 ℃; the time is 15 to 31 hours.
In a third aspect, the embodiment of the invention provides the fullerene negative ion release head prepared by the method.
In a fourth aspect, an embodiment of the present invention provides an anion generating electrode, where the anion generating electrode includes a metal rod, a conductive fixing device, and an anion releasing head, the anion releasing head is fixed on the metal rod by the conductive fixing device, and the anion releasing head is electrically connected to the metal rod, and the anion releasing head is a fullerene anion releasing head as described above or a fullerene anion releasing head prepared by the method as described above.
The method for preparing the fullerene negative ion release head provided by the embodiment of the invention improves the solubility of fullerene in water through surface modification, obviously shortens the process time for preparing the fullerene negative ion release head by adopting fullerene aqueous solution, improves the production efficiency of the negative ion release head and reduces the cost. Moreover, the fullerene is finally dissolved into water, so that the preparation method is safe, environment-friendly and pollution-free.
Meanwhile, the fullerene negative ion release head prepared by the embodiment of the invention can generate ecological-grade small-particle-size negative oxygen ions with small particle size, high activity and long migration distance, and the negative ions have high purity and almost do not generate by-products such as ozone, nitrogen oxides and the like. Moreover, the hardness of the fullerene negative ion release head is improved by introducing the conductive metal wire, so that the fullerene negative ion release head can bear high negative pressure and can be cleaned frequently, and the service life is prolonged. In addition, the fullerene layer in the fullerene negative ion releasing head is not easy to fall off from the metal wire or is affected by external environment such as acid-base corrosion, and the like, and can release negative ions with higher concentration for a longer time, namely, the service life is longer.
Drawings
Fig. 1 is a schematic structural view of a negative ion generating electrode according to an embodiment of the present invention.
Fig. 2 is a process flow chart of the preparation of the fullerene negative ion release head according to the embodiment of the present invention.
Reference numerals in the drawings denote:
1-metal rod 2-conductive fixing device 3-negative ion release head
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In a first aspect, an embodiment of the present invention provides a fullerene negative ion releasing head, including a conductive wire and a fullerene layer formed on a surface of the conductive wire.
Compared with the existing negative ion release head made of fullerene fibers, the fullerene negative ion release head disclosed by the embodiment of the invention has higher hardness, can withstand high negative pressure and frequent cleaning and has longer service life.
In an embodiment of the invention, the thickness of the fullerene layer may be 2 to 10 nm. The fullerene layer with the thickness has good adhesiveness on the conductive metal wire, is not easy to fall off from the conductive metal wire, and can ensure that the fullerene anion release head releases anions with higher concentration.
In an embodiment of the present invention, the conductive metal wire may be a titanium wire, a molybdenum wire, a tungsten wire, or an iron wire. In other embodiments of the present invention, stainless steel wire may also be used in place of the conductive wire of the present invention.
In the embodiment of the invention, 20-40 conductive metal wires can be arranged on 1 fullerene negative ion release head.
In a second aspect, embodiments of the present invention provide a method for preparing a fullerene negative ion release head, the method comprising:
carrying out surface modification on fullerene;
preparing fullerene aqueous solution by using fullerene after surface modification; and
and putting the conductive metal wire into the fullerene aqueous solution, and depositing and growing a fullerene layer on the surface of the conductive metal wire to obtain the fullerene negative ion release head.
The method for preparing the fullerene negative ion release head improves the solubility of fullerene in water through surface modification, obviously shortens the process time of preparing the fullerene negative ion release head by adopting fullerene aqueous solution, improves the production efficiency of the negative ion release head and reduces the cost. Moreover, the fullerene is finally dissolved into water, so that the preparation method is safe, environment-friendly and pollution-free.
Meanwhile, the surface modification does not bring adverse effects on the performance of the fullerene negative ion release head, the prepared fullerene negative ion release head can still generate ecological-grade small-particle-size negative oxygen ions with small particle size, high activity and long migration distance, the purity of the negative ions is high, and almost no byproducts such as ozone, nitrogen oxides and the like are generated. In addition, the fullerene layer in the fullerene negative ion releasing head is not easy to fall off from the metal wire or is affected by external environment such as acid-base corrosion, and the like, and can release negative ions with higher concentration for a longer time, namely, the service life is longer.
In an embodiment of the present invention, the surface modification of fullerene may include:
dissolving fullerene in an organic solvent to obtain a first mixed solution;
dissolving a surfactant in a dispersing agent to obtain a second mixed solution;
mixing the first mixed solution with the second mixed solution so as to modify the surface of fullerene; and
and (5) removing impurities from the system.
In an embodiment of the present invention, the dissolving of the fullerene in the organic solvent may include: mixing fullerene with an organic solvent in a container, and ultrasonically dispersing until no fullerene is attached to the inner wall of the container and the solution in the container is not layered.
The organic solvent may be selected from commonly used nonpolar organic solvents for dissolving fullerene, for example, toluene, cyclohexane, chloroform, etc. The amount of the organic solvent is only required to ensure that the fullerene is completely immersed, and for example, the mass ratio of the fullerene to the organic solvent can be 0.5-1: 1. The frequency of the ultrasonic dispersion can be 100-150 times/min.
In an embodiment of the invention, the surfactant may be an N-vinyl amide surfactant, for example, polyvinylpyrrolidone (PVP). The dispersant is used for dispersing PVP and can be selected from any one or more of aromatic hydrocarbon, halogenated aromatic hydrocarbon, alcohol solvent and halogenated alkane, for example, the dispersant can be selected from any one or more of chlorotoluene, chloroform, toluene, methanol and ethanol, and optionally the dispersant is chloroform. In the second mixed solution, the mass fraction of PVP may be 5% to 15%.
In an embodiment of the present invention, a mass ratio of the fullerene to the surfactant may be 1:80 to 200, for example, 1:100 to 150. The mass ratio of the fullerene to the surfactant can obtain a good dispersing effect, and the problem of overlong subsequent impurity removal treatment time caused by the excessive amount of the surfactant can be avoided. In an embodiment of the present invention, the performing impurity removal processing on the system may include:
performing rotary evaporation on the system until the solution in the system is completely evaporated to dryness;
mixing the solid obtained by rotary evaporation with water, and performing ultrasonic dispersion; and
and adding water into the solution subjected to ultrasonic dispersion, and centrifuging until the pH value of the lower-layer precipitate is 6.5-7.5 to obtain the fullerene with the modified surface.
Most of impurities such as organic solvents, surfactants, dispersants and the like in the system can be removed through rotary evaporation. In the embodiment of the invention, the temperature of the rotary evaporation can be 50-100 ℃, for example, 60-80 ℃, and the temperature can not only ensure the efficiency of the rotary evaporation, but also can not change the performance of the fullerene. The rotation speed can be 100-200 r/min.
The solid obtained by rotary evaporation is mixed with water and subjected to ultrasonic dispersion, so that a small amount of residual organic solvent, surfactant and dispersant in the system can be dispersed in the water, and the subsequent centrifugation is facilitated to completely separate the residual organic solvent, surfactant and dispersant from the system. The mass ratio of the solid obtained by rotary evaporation to water can be 0.5-1: 10, and the ultrasonic frequency can be 100-150 times/min until a uniformly mixed dispersion solution is formed.
The centrifugation can utilize the action of gravity to precipitate the fullerene with larger molecular weight at the lower layer, and the organic solvent with smaller molecular weight, the surfactant and the dispersant are dispersed in the solution at the upper layer. After each centrifugation, the upper layer solution is poured off, the lower layer precipitate is taken out and dissolved in water, and the pH of the lower layer precipitate is measured, for example, 0.1 to 0.5mg of the lower layer precipitate is taken out and dissolved in 1 to 5mg of water, and the pH of the solution is measured by dipping the solution with a pH test paper, and the pH is taken as the pH of the lower layer precipitate. And when the pH value of the lower-layer precipitate is 6.5-7.5, the organic solvent, the surfactant and the dispersant in the system are basically removed completely. The centrifugation times can be 2-4 times, the centrifugation speed can be 6000-7500 rpm, the time of each centrifugation can be 5-10 min, the volume ratio of the water added in each centrifugation to the dispersion solution before the centrifugation can be 1/3-1/2: 1, the solution on the upper layer is poured out after each centrifugation is finished, and the next centrifugation is carried out after the water is added again.
In an embodiment of the present invention, the preparing the fullerene aqueous solution using the surface-modified fullerene may include:
dissolving the fullerene with the modified surface in water to obtain a primary aqueous solution of the fullerene;
concentrating the primary aqueous solution to obtain a concentrated solution; and
and activating the concentrated solution to obtain the fullerene aqueous solution.
In the embodiment of the present invention, the concentration process may be performed in a dry manner. The conditions for drying may include: the temperature is 20-30 ℃ and the time is 3-5 hours. For example, the temperature is 22-25 ℃; the time is 4-5 hours.
The purpose of the concentration treatment includes: evaporating part of water in the solution to avoid the subsequent activation treatment in an environment with more water vapor, which is easy to generate impurities; and secondly, the concentration of the solution is improved to a certain extent, so that a fullerene layer with proper thickness and uniform particles can be grown in a subsequent deposition mode. Because the water content in the system is low, the first purpose and the second purpose of concentration treatment can be realized after drying for 3-5 hours at the temperature of 20-30 ℃.
In the embodiment of the present invention, the activation treatment may be performed by sintering under an inert atmosphere. The conditions for sintering may include: the temperature is 90-120 ℃, the time is 0.5-1.5 hours, and the volume fraction of fullerene in the fullerene aqueous solution is controlled to be 5-30%, for example, the temperature is 100-110 ℃, and the time is 1-1.2 hours.
On one hand, the fullerene can be excited through activation treatment, so that the performance of the fullerene can be better exerted; on the other hand, the residual organic solvent can be further evaporated and removed.
If the concentration treatment step is omitted and the activation is directly carried out, at the activation temperature, water in the system is converted into water vapor and is sealed in a closed activation device, so that the activation environment is changed, and impurities are easily generated.
In an embodiment of the present invention, the inert atmosphere may be selected from any one or more of helium (He), neon (Ne), and argon (Ar). Activation in an inert atmosphere can prevent the fullerene from being oxidized.
In the embodiment of the present invention, the method used when the fullerene layer is deposited and grown on the surface of the conductive metal wire may be a vertical deposition method. The vertical deposition method has the advantages of simple process, low growth temperature, low viscosity of the growth solution, good integrity of the grown fullerene layer and more uniform surface.
In the embodiment of the invention, the temperature for depositing and growing the fullerene layer by using the vertical deposition method may be 50 to 120 ℃, for example, 60 to 100 ℃. The deposition temperature of 50-120 ℃ is favorable for forming the fullerene layer with good compactness, and the speed of forming the fullerene layer is high. The deposition time may be 15 to 31 hours, for example, 16 to 30 hours. The deposition time of 15 to 31 hours is favorable for forming a fullerene layer with a desired thickness. The thickness of the fullerene layer may be 2 to 10 nm.
In an embodiment of the invention, the method further comprises: and after the growth of the fullerene layer is finished, taking the fullerene negative ion releasing head out of the fullerene aqueous solution and drying. The drying can be realized by a constant-temperature drying mode, the drying temperature can be 60-80 ℃, and the drying time can be 30-60 minutes.
In a third aspect, the embodiment of the invention provides the fullerene negative ion release head prepared by the method.
In a fourth aspect, an embodiment of the present invention provides an anion generating electrode, as shown in fig. 1, the anion generating electrode includes a metal rod 1, a conductive fixing device 2, and an anion releasing head 3, the anion releasing head 3 is fixed on the metal rod 1 through the conductive fixing device 2, the anion releasing head 3 is electrically connected to the metal rod 1, and the anion releasing head 3 is a fullerene ion releasing head as described above or a fullerene anion releasing head prepared by the method as described above.
Examples
The present invention will be described in detail below by way of examples, but the present invention is not limited thereto. In the following examples, unless otherwise specified, all methods used are conventional in the art, and all reagents used are commercially available.
The conductive fixing devices used in the following examples are all copper wires.
Example 1
As shown in fig. 2, the method for preparing a fullerene negative ion releasing head according to the present embodiment includes:
s1: adding toluene into a container containing fullerene, controlling the mass ratio of the fullerene to the toluene to be 1:1, and ultrasonically dispersing at the frequency of 100 times/min until no fullerene is attached to the inner wall of the container and the solution in the container is not layered to obtain a first mixed solution;
s2: mixing polyvinylpyrrolidone with chloroform to obtain a second mixed solution, controlling the mass fraction of polyvinylpyrrolidone in the second mixed solution to be 15%, adding the first mixed solution obtained in the step S1 into the second mixed solution, controlling the mass ratio of fullerene to polyvinylpyrrolidone to be 1:100, and stirring by magnetic force to fully mix the fullerene and the polyvinylpyrrolidone;
s3: rotationally evaporating the solution obtained in the step S2 at 60 ℃, wherein the rotational speed is 100r/min until the solution in the system is completely evaporated to dryness;
s4: adding deionized water into the solid obtained in the step S3, controlling the mass ratio of the solid obtained in the step S3 to the deionized water to be 0.5:10, and then carrying out ultrasonic dispersion for 20min at the frequency of 100 times/min to form a uniformly mixed dispersion solution;
s5: adding deionized water into the dispersed solution obtained in the step S4, centrifuging at 6000rpm for 10min, repeatedly centrifuging for 2 times, wherein the volume ratio of the deionized water added in each centrifugation to the dispersed solution obtained in the step S4 is 1/2:1, centrifuging for 2 times, pouring out the upper layer solution, dissolving 0.1mg of lower layer precipitate in 1mg of water, measuring the pH value to be 6.7, and dissolving the obtained lower layer precipitate in deionized water to obtain a primary aqueous solution of fullerene;
s6: drying the primary aqueous solution at 20 ℃ for 5 hours to obtain a concentrated solution;
s7: sintering the concentrated solution for 1.5 hours at 90 ℃ in a helium atmosphere to obtain a fullerene aqueous solution; wherein, in the fullerene aqueous solution, the volume fraction of fullerene is 15%;
s8: bundling 25 titanium wires on a titanium rod through a conductive fixing device, putting the titanium wires into the fullerene aqueous solution obtained in the step S7, then putting the titanium wires into a thermostat, setting the temperature of the thermostat to be 60 ℃ and the time to be 30 hours, and growing a fullerene layer with the thickness of 2nm on the titanium wires by adopting a vertical deposition method, thereby obtaining the fullerene negative ion release head;
s9: and taking the fullerene negative ion release head out of the fullerene water solution, and drying at the constant temperature of 60 ℃ for 60 minutes.
Example 2
As shown in fig. 2, the method for preparing a fullerene negative ion releasing head according to the present embodiment includes:
s1: adding toluene into a container containing fullerene, controlling the mass ratio of the fullerene to the toluene to be 0.5:1, and ultrasonically dispersing at the frequency of 130 times/min until no fullerene is attached to the inner wall of the container and the solution in the container is not layered to obtain a first mixed solution;
s2: mixing polyvinylpyrrolidone with chloroform to obtain a second mixed solution, controlling the mass fraction of polyvinylpyrrolidone in the second mixed solution to be 10%, adding the first mixed solution obtained in the step S1 into the second mixed solution, controlling the mass ratio of fullerene to polyvinylpyrrolidone to be 1:125, and stirring by magnetic force to fully mix the fullerene and the polyvinylpyrrolidone;
s3: rotationally evaporating the solution obtained in the step S2 at 70 ℃, wherein the rotational speed is 150r/min until the solution in the system is completely evaporated to dryness;
s4: adding deionized water into the solid obtained in the step S3, controlling the mass ratio of the solid obtained in the step S3 to the deionized water to be 0.7:10, and then carrying out ultrasonic dispersion for 15min at the frequency of 130 times/min to form a uniformly mixed dispersion solution;
s5: adding deionized water into the dispersed solution obtained in the step S4, centrifuging at 7000rpm for 8min, repeatedly centrifuging for 3 times, wherein the volume ratio of the deionized water added in each centrifugation to the dispersed solution obtained in the step S4 is 1/3:1, centrifuging for 3 times, pouring out the upper solution, dissolving 0.3mg of lower precipitate in 3mg of water, measuring the pH value to be 6.9, and dissolving the obtained lower precipitate in deionized water to obtain a primary aqueous solution of fullerene;
s6: drying the primary aqueous solution at 25 ℃ for 4 hours to obtain a concentrated solution;
s7: sintering the concentrated solution for 1 hour at 105 ℃ in a neon atmosphere; wherein, in the fullerene aqueous solution, the volume fraction of fullerene is 10%;
s8: binding 30 molybdenum wires on a molybdenum rod through a conductive fixing device, putting the molybdenum wires into the fullerene aqueous solution obtained in the step S7, then putting the molybdenum wires into a thermostat, setting the temperature of the thermostat to be 80 ℃, and growing a fullerene layer with the thickness of 7nm on the molybdenum wires by adopting a vertical deposition method for 25 hours, thereby obtaining a fullerene negative ion release head;
s9: and taking the fullerene negative ion release head out of the fullerene water solution, and drying at the constant temperature of 70 ℃ for 50 minutes.
Example 3
As shown in fig. 2, the method for preparing a fullerene negative ion releasing head according to the present embodiment includes:
s1: adding toluene into a container containing fullerene, controlling the mass ratio of the fullerene to the toluene to be 0.5:1, and ultrasonically dispersing at the frequency of 150 times/min until no fullerene is attached to the inner wall of the container and the solution in the container is not layered to obtain a first mixed solution;
s2: mixing polyvinylpyrrolidone with chlorotoluene to obtain a second mixed solution, controlling the mass fraction of the polyvinylpyrrolidone in the second mixed solution to be 5%, adding the first mixed solution obtained in the step S1 into the second mixed solution, controlling the mass ratio of fullerene to polyvinylpyrrolidone to be 1:150, and stirring by magnetic force to fully mix the fullerene and the polyvinylpyrrolidone;
s3: rotationally evaporating the solution obtained in the step S2 at 80 ℃, wherein the rotational speed is 200r/min until the solution in the system is completely evaporated to dryness;
s4: adding deionized water into the solid obtained in the step S3, controlling the mass ratio of the solid obtained in the step S3 to the deionized water to be 1:10, and then carrying out ultrasonic dispersion for 10min at the frequency of 150 times/min to form a uniformly mixed dispersion solution;
s5: adding deionized water into the dispersed solution obtained in the step S4, centrifuging at 7500rpm for 5min, repeating the centrifuging for 4 times, wherein the volume ratio of the deionized water added in each centrifuging to the dispersed solution obtained in the step S4 is 1/3:1, centrifuging for 4 times, pouring out the upper solution, dissolving 0.5mg of lower precipitate in 5mg of water, measuring the pH value to be 7.2, and dissolving the obtained lower precipitate in deionized water to obtain a primary aqueous solution of fullerene;
s6: drying the primary aqueous solution at 30 ℃ for 3 hours to obtain a concentrated solution;
s7: sintering the concentrated solution for 0.5 hour at 120 ℃ in an argon atmosphere to obtain a fullerene aqueous solution; wherein, in the fullerene aqueous solution, the volume fraction of fullerene is 30%;
s8: binding 35 tungsten filaments on a tungsten rod through a conductive fixing device, putting the tungsten filaments into the fullerene aqueous solution obtained in the step S7, then putting the tungsten filaments into a thermostat, setting the temperature of the thermostat to be 100 ℃, and growing a fullerene layer with the thickness of 10nm on the tungsten filaments by adopting a vertical deposition method for 15 hours, thereby obtaining a fullerene negative ion release head;
s9: and taking the fullerene negative ion release head out of the fullerene water solution, and drying at the constant temperature of 80 ℃ for 30 minutes.
Example 4
This example differs from example 2 only in that: in step S2, the mass ratio of fullerene to polyvinylpyrrolidone is 1: 80.
Example 5
This example differs from example 2 only in that: the temperature of the rotary evaporation in step S3 was 100 ℃.
Example 6
This example differs from example 2 only in that: the temperature of the oven in step S6 was 120 ℃ for 15 hours.
Comparative example 1
The negative ion emitting head of this comparative example was composed of fullerene fibers and the same metal rod as in example 2 of the present invention, and the preparation method was carried out by putting the metal rod into an aqueous fullerene solution and depositing and growing a 7nm fullerene layer on the surface of the metal rod, in accordance with steps S7 to S9 of the examples.
In the preparation of the negative ion emitting head of comparative example 1, the step of dissolving fullerene in water takes 25 to 30 hours. The steps S1-S7 of examples 1-6 took about 7-12 hours in total, and significantly reduced the process time compared to the comparative method for preparing fullerene releasing heads.
Performance testing
1. Anion release test
1) Testing instrument
Hand-held atmospheric negative ion tester-manufacturer: hua Si Tong; the instrument model is as follows: WST-3200 Pro.
2) Test conditions
Temperature: 18 deg.C
Relative humidity: 18 percent of
PM2.5：30μg/m2
Output voltage connected to one end of the metal rod: 40 kV.
3) Test procedure
A tester holds the atmosphere negative ion tester, respectively stands in the positive front, the left side of the negative ion release head to be tested in the direction of 22.5 degrees, and the right side of the negative ion release head to be tested in the direction of 22.5 degrees, and respectively stands at the positions 2 and 4m away from the negative ion release head to be tested, and the quantity of negative ions released by the negative ion release head to be tested is tested.
4) Test result 1
After the anion releasing heads of each example and comparative example were prepared, the use was continued for 10 hours, and then the test was performed. The results of the test of the anion releasing concentration of the anion releasing heads of each example and comparative example are shown in Table 1 (note: the left, middle and right in Table 1 respectively indicate the 22.5 degree left direction, the right direction and the front direction of the anion releasing head, and the 22.5 degree right direction).
TABLE 1
As can be seen from table 1, the negative ion release amount of the fullerene negative ion releasing head of the example of the present invention is not reduced or even more compared to that of the comparative example. The invention is proved that the fullerene is subjected to surface modification, negative ions are not adversely affected in release amount, and ecological-grade small-particle-size negative oxygen ions with small particle size, high activity and long migration distance can be generated.
5) Test result two
The negative ion emitting heads of each example and comparative example were used under the same environment and output voltage for 600 days, and then cleaned, and then tested for the negative ion emitting concentration, respectively. The test results showed that the anion emission concentrations of the anion releasing heads of examples 1 to 6 were decreased by 3%, 2%, 4%, 6.5%, 6% and 6.6%, respectively, compared with the data of table 1, and that the anion emission concentration of the anion releasing head of comparative example 1 was decreased by 10%, compared with the data of table 1.
Generally, when ash falls on the anion discharging head, the anion discharging concentration is reduced, but after the anion discharging head is cleaned, the anion discharging concentration can be restored to be close to the data in the table 1. However, it can be seen from the second test result that, even though the anion discharging head of comparative example 1 is cleaned after 600 days of use, the anion discharging concentration is reduced by 10% compared with the data in table 1, and the anion discharging concentration of the anion discharging head of the embodiment of the present invention is reduced significantly less. It is illustrated that the fullerene layer on the negative ion release head of comparative example 1 is peeled off or is affected by external environments such as acid-base corrosion, etc., and the fullerene layer of the negative ion release head of the embodiment of the present invention is less peeled off or less affected by external environments such as acid-base corrosion, etc.
2. Ozone and nitrogen oxides (NO and NO)2) Release amount test
1) Testing instrument
Nitrogen oxide tester-manufacturer: polyclone; the instrument model is as follows: WSQ-NOX;
ozone tester-manufacturer: polyclone; the instrument model is as follows: WSQ-O3.
2) Test conditions
Temperature: 18 deg.C
Relative humidity: 18 percent of
PM2.5：30μg/m2
Output voltage connected to one end of the metal rod: 40 kV.
3) Test procedure
A tester holds a nitrogen oxide tester or an ozone tester by hands, respectively stands in the positions which are respectively in the positive front, the left side and the right side of the negative ion release head to be tested and are respectively 2 m and 4m away from the negative ion release head in the direction of 22.5 degrees, and tests the concentration of ozone and nitrogen oxide released by the negative ion release head to be tested.
4) Test results
After the anion releasing heads of each example and comparative example were prepared, the use was continued for 10 hours, and then the test was performed. Ozone and nitrogen oxide release amounts (NO and NO) of anion releasing heads of examples and comparative examples2Total amount released) the test results are shown in table 2.
TABLE 2
As can be seen from table 2, the fullerene anion releasing heads of the examples of the present invention did not release nitrogen oxide and the amount of ozone released was reduced relative to the anion releasing heads of the comparative examples, compared to the fullerene anion releasing heads of the comparative examples, indicating that the surface modification of the present invention did not affect the purity of anions released from the anion releasing heads.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A fullerene negative ion releasing head, comprising a conductive wire and a fullerene layer formed on a surface of the conductive wire.
2. A fullerene negative ion releasing head according to claim 1 wherein the fullerene layer has a thickness of 2 to 10 nm; and/or
The conductive metal wire is a titanium wire, a molybdenum wire, a tungsten wire or an iron wire.
3. A method of making a fullerene negative ion release head, the method comprising:
carrying out surface modification on fullerene;
preparing fullerene aqueous solution by using fullerene after surface modification; and
and putting the conductive metal wire into the fullerene aqueous solution, and depositing and growing a fullerene layer on the surface of the conductive metal wire to obtain the fullerene negative ion release head.
4. The method of claim 3, wherein said surface modifying fullerenes comprises:
dissolving fullerene in an organic solvent to obtain a first mixed solution;
dissolving a surfactant in a dispersing agent to obtain a second mixed solution;
mixing the first mixed solution with the second mixed solution so as to modify the surface of fullerene; and
and (5) removing impurities from the system.
5. The method of claim 4, wherein the surfactant is an N-vinyl amide surfactant, optionally, polyvinylpyrrolidone; and/or
The dispersing agent is selected from any one or more of aromatic hydrocarbon, halogenated aromatic hydrocarbon, alcohol solvent and halogenated alkane; and/or
The mass ratio of the fullerene to the surfactant is 1: 80-200, and optionally 1: 100-150; and/or
The dissolving of the fullerene in the organic solvent comprises: mixing fullerene with an organic solvent in a container, and ultrasonically dispersing until no fullerene is attached to the inner wall of the container and the solution in the container is not layered.
6. The method of claim 4, wherein the dedoping of the system comprises:
performing rotary evaporation on the system until the solution in the system is completely evaporated to dryness;
mixing the solid obtained by rotary evaporation with water, and performing ultrasonic dispersion; and
adding water into the solution after ultrasonic dispersion, and centrifuging until the pH value of the lower-layer precipitate is 6.5-7.5 to obtain the fullerene with the modified surface;
optionally, the temperature of the rotary evaporation is 50-100 ℃, and further optionally 60-80 ℃.
7. The method of claim 3, wherein said preparing the aqueous fullerene solution from the surface-modified fullerene comprises:
dissolving the fullerene with the modified surface in water to obtain a primary aqueous solution of the fullerene;
concentrating the primary aqueous solution to obtain a concentrated solution; and
and activating the concentrated solution to obtain the fullerene aqueous solution.
8. The method of claim 7, wherein the concentration process comprises: drying the primary aqueous solution at 20-30 ℃ for 3-5 hours; and/or
The activation treatment comprises: and sintering the concentrated solution in an inert atmosphere at 90-120 ℃ for 0.5-1.5 hours, and controlling the concentrated solution in the fullerene aqueous solution, wherein the volume fraction of fullerene is 5-30%.
9. The method according to any one of claims 3 to 8, wherein the method used in the deposition growth of the fullerene layer on the surface of the conductive wire is a vertical deposition method, and the conditions of the vertical deposition method include: the temperature is 50-120 ℃, and optionally, the temperature is 60-100 ℃; the time is 15 to 31 hours.
10. An anion generating electrode, characterized in that, the anion generating electrode comprises a metal rod, a conductive fixing device and an anion releasing head, the anion releasing head is fixed on the metal rod by the conductive fixing device, and the anion releasing head is electrically connected with the metal rod, the anion releasing head is the fullerene anion releasing head of claim 1 or 2 or the fullerene anion releasing head prepared by the method of any one of claims 3 to 9.
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| CN2524406Y (en) * | 2001-12-30 | 2002-12-04 | 西安交通大学 | Negative ion generator for growing nano carbon tube array on discharge terminal |
| CN205265040U (en) * | 2015-12-03 | 2016-05-25 | 刘延兵 | Positive and negative ions emitter |
| CN206947732U (en) * | 2017-01-23 | 2018-01-30 | 上海氧咖健康科技有限公司 | One kind receives sub- fullerene negative ion release |
| CN108423662A (en) * | 2018-04-09 | 2018-08-21 | 合肥国轩高科动力能源有限公司 | A method of high concentration graphene is prepared based on abstraction technique |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2524406Y (en) * | 2001-12-30 | 2002-12-04 | 西安交通大学 | Negative ion generator for growing nano carbon tube array on discharge terminal |
| CN205265040U (en) * | 2015-12-03 | 2016-05-25 | 刘延兵 | Positive and negative ions emitter |
| CN206947732U (en) * | 2017-01-23 | 2018-01-30 | 上海氧咖健康科技有限公司 | One kind receives sub- fullerene negative ion release |
| CN108423662A (en) * | 2018-04-09 | 2018-08-21 | 合肥国轩高科动力能源有限公司 | A method of high concentration graphene is prepared based on abstraction technique |
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