CN111509564A - Composite material negative ion release head, preparation method thereof and negative ion generating electrode - Google Patents
Composite material negative ion release head, preparation method thereof and negative ion generating electrode Download PDFInfo
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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
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a composite material negative ion release head. The method comprises the following steps: carrying out surface modification on the carbon nano tube; mixing the carbon nano tube with the surface modified, fullerene and water to obtain a composite material aqueous solution of the carbon nano tube and the fullerene; and putting a conductive metal wire into the composite material aqueous solution of the carbon nano tube and the fullerene, and depositing and growing a composite material layer of the carbon nano tube and the fullerene on the surface of the conductive metal wire to obtain the composite material negative ion release head. The invention also provides a negative ion generating electrode. The composite material negative ion release head prepared by the method can release ecological-grade small-particle-size negative oxygen ions with high concentration, small particle size, high activity and long migration distance under lower negative pressure, the purity of the negative ions is high, and the service life of the composite material negative ion release head is long.
Description
Technical Field
The invention relates to a negative ion generating technology, in particular to a composite material 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 derivatives such as ozone, positive ions and the like.
However, the fullerene negative ion release head on the market generally works under the negative pressure of more than 8000V to ensure the release concentration of negative ions. Such high negative pressure is not only high in cost, but also easily causes the negative ion releasing head and the metal around the negative ion releasing head to generate static electricity, reduces the use safety of the negative ion generator, brings fear to users, and even threatens the personal safety of the users.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a composite material negative ion release head, a preparation method thereof and a negative ion generating electrode. The preparation method provided by the invention can improve the compatibility of the carbon nano tube and the fullerene to obtain the negative ion release head of the composite material of the carbon nano tube and the fullerene, and the negative ion release head of the composite material can release negative ions with higher concentration under lower negative pressure, thereby reducing the cost of generating the negative ions and improving the use safety of the negative ion generator.
In order to achieve the above object, in a first aspect, the present invention provides a method for preparing a composite material negative ion release head, the method comprising:
carrying out surface modification on the carbon nano tube;
mixing the carbon nano tube with the surface modified, fullerene and water to obtain a composite material aqueous solution of the carbon nano tube and the fullerene; and
and putting a conductive metal wire into the composite material aqueous solution of the carbon nano tube and the fullerene, and depositing and growing a composite material layer of the carbon nano tube and the fullerene on the surface of the conductive metal wire to obtain the composite material negative ion release head.
In an embodiment of the present invention, the surface modification of the carbon nanotube may include:
purifying the carbon nano tube;
hydroxylating the purified carbon nano tube; and
and reacting the hydroxylated carbon nano tube with a coupling agent to obtain the surface modified carbon nano tube.
In an embodiment of the present invention, the method used for purifying the carbon nanotubes may include a mixed acid oxidation method;
in an embodiment of the present invention, the conditions of the mixed acid oxidation process may include: the mixed acid is the mixed acid of A acid and B acid, the A acid is concentrated hydrochloric acid and/or concentrated nitric acid, and the B acid is concentrated sulfuric acid.
In the embodiment of the invention, the oxidation time of the mixed acid oxidation method can be 7-11 h;
in the embodiment of the invention, the mass ratio of the A acid to the B acid in terms of pure A acid to pure B acid is 20-70: 1.
In an embodiment of the present invention, the hydroxylating the purified carbon nanotubes may include: and mixing the purified carbon nano tube with a hydroxylation reagent, carrying out hydroxylation reaction, carrying out suction filtration, washing and drying a filter cake to obtain the hydroxylated carbon nano tube.
In an embodiment of the present invention, the hydroxylation treatment conditions may include: the mass ratio of the purified carbon nanotube to the pure hydroxylation reagent is 1: 10-20, and optionally 1: 10-15.
In the embodiment of the invention, the hydroxylation reaction time can be 9-12 h.
In the embodiment of the present invention, the hydroxylating reagent may be a mixed solution of hydrogen peroxide and ferrous sulfate, and optionally, pure H of hydrogen peroxide and ferrous sulfate2O2The mass ratio of the pure ferrous sulfate to the pure ferrous sulfate can be 100-200: 1.
In an embodiment of the present invention, the reacting the hydroxylated carbon nanotube with the coupling agent may include: and mixing the hydroxylated carbon nano tube with a coupling agent and a dispersing solvent, carrying out coupling reaction, carrying out suction filtration, washing and drying a filter cake to obtain the surface-modified carbon nano tube.
In embodiments of the invention, the conditions of the coupling reaction may include: the temperature is 50-90 ℃, optionally 60-80 ℃, and the time is 5-8 h, optionally 6-7 h.
In an embodiment of the invention, the mass ratio of the hydroxylated carbon nanotube to the coupling agent may be 1: 0.5-4, optionally 1: 1-3.
In embodiments of the invention, the coupling agent may be selected from any one or more of silane coupling agents, optionally, from any one or more of 3-glycidoxypropyltrimethoxysilane, methacryloxypropyltrimethoxysilane, and aminopropyltriethoxysilane.
In the embodiment of the invention, in the composite material aqueous solution of the carbon nano tube and the fullerene, the mass ratio of the carbon nano tube after surface modification to the fullerene can be (0.2-1): 1, and optionally (0.4-0.9): 1.
In the embodiment of the invention, the method used for depositing and growing the composite material layer of the carbon nanotube and the fullerene on the surface of the conductive metal wire can 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, optionally 16 to 30 hours.
In a second aspect, the invention provides the composite material negative ion release head prepared by the method.
In a third aspect, the present invention provides an anion generating electrode, which includes a metal rod, a conductive fixing device, and an anion releasing head, wherein the anion releasing head is fixed on the metal rod through the conductive fixing device, and is electrically connected to the metal rod, and the anion releasing head is the composite anion releasing head as described above or the composite anion releasing head prepared by the method as described above.
The composite material anion releasing head prepared by the method of the embodiment of the invention can release anions with higher concentration under lower negative pressure, can avoid the composite material anion releasing head and metal around the composite material anion releasing head from generating a large amount of static electricity, improves the use safety of an anion generator, and reduces the cost of generating the anions; and the released negative ions are 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 by-products such as ozone, nitrogen oxide and the like are hardly generated. Moreover, the composite material negative ion release head has higher hardness, can bear high negative pressure and can be cleaned frequently, and the service life is long.
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 composite material negative ion release head according to the embodiment of the 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, embodiments of the present invention provide a method for preparing a composite material negative ion release head, the method comprising:
carrying out surface modification on the carbon nano tube;
mixing the carbon nano tube with the surface modified, fullerene and water to obtain a composite material aqueous solution of the carbon nano tube and the fullerene; and
and putting a conductive metal wire into the composite material aqueous solution of the carbon nano tube and the fullerene, and depositing and growing a composite material layer of the carbon nano tube and the fullerene on the surface of the conductive metal wire to obtain the composite material negative ion release head.
The carbon nano tube has the characteristics of unique structure, chemical stability and quasi-one-dimensional transport, has wide application prospect in electronic devices, has strong electron transport property of the carbon nano tube with shorter length, can form coupling with a metal electrode, generates band gap state due to charge transfer caused by the coupling, and plays an important role in the transport property. The carbon nano tube is a homoisomer of fullerene, if the carbon nano tube and the fullerene are compounded together, the formed material has the characteristics of a conductor and a semiconductor, the electron transmission characteristic is possibly superior to that of the single carbon nano tube and the fullerene, and the negative ion release head prepared by adopting the composite material of the carbon nano tube and the fullerene can improve the release concentration of negative ions and realize the release of the negative ions with higher concentration at lower voltage. However, the compatibility of the carbon nanotube with the fullerene is poor, and the carbon nanotube is likely to agglomerate in the fullerene and is difficult to be uniformly dispersed in the fullerene.
According to the preparation method provided by the embodiment of the invention, the carbon nano tube is subjected to surface modification, the compatibility of the carbon nano tube and the fullerene is improved, the composite material of the carbon nano tube and the fullerene is successfully prepared, and the composite material negative ion release head is prepared by adopting the composite material. The composite material has the characteristics of both a conductor and a semiconductor, accords with the quantization transmission principle of a nano electronic device, and has better electron transmission performance than single carbon nano tubes and fullerene, so that anions with higher concentration can be released, and the anions with higher concentration can be formed at lower voltage.
In addition, the preparation method of the embodiment of the invention introduces the conductive metal wire into the negative ion release head, and the conductive metal wire has conductivity, thereby facilitating the transmission and release of current carriers and further improving the release concentration of negative ions. In addition, the conductive metal wire can improve the hardness of the composite material anion release head, so that the composite material anion release head can withstand high negative pressure and can be cleaned frequently, and the service life of the anion release head under the high negative pressure is prolonged.
In an embodiment of the present invention, the surface modification of the carbon nanotube may include:
purifying the carbon nano tube;
hydroxylating the purified carbon nano tube; and
and reacting the hydroxylated carbon nano tube with a coupling agent to obtain the surface modified carbon nano tube.
The C-C bond in the carbon nano tube can be broken and form a C-O bond through purification, then the C-O bond is converted into hydroxyl through subsequent hydroxylation reaction, finally the hydroxyl reacts with silicon hydroxyl in the coupling agent for dehydration, the carbon nano tube and the rest part of the coupling agent are bridged together through-O-, and the compound has good dispersion and solubility in water.
In an embodiment of the present invention, the method used for purifying the carbon nanotubes may include a mixed acid oxidation method. The mixed acid adopted by the mixed acid oxidation method can be the mixed acid of acid A and acid B, wherein the acid A is concentrated hydrochloric acid and/or concentrated nitric acid, and the acid B is concentrated sulfuric acid.
In the invention, the concentrated hydrochloric acid is defined as hydrochloric acid with the mass fraction of 20-36.5%; the concentrated nitric acid is nitric acid with the mass fraction of 50-68%; the concentrated sulfuric acid is 80-98 wt% sulfuric acid.
The mass ratio of the A acid to the B acid in terms of pure A acid and pure B acid can be 20-70: 1. The amount of the mixed acid is only required to be capable of completely immersing the carbon nano tube.
In the embodiment of the invention, the time of the mixed acid oxidation method can be 7-11 h.
In an embodiment of the present invention, the purifying the carbon nanotubes by using a mixed acid oxidation method may include: mixing the mixed acid with the carbon nano tube, and then carrying out ultrasonic dispersion and stirring to promote the reaction. The conditions of the ultrasonic dispersion may include: at room temperature, the power is 200-600W, and the time is 2-4 h. The conditions under which the agitation promotes the reaction may include: the time is 5 to 7 hours, and the stirring speed is 100-300 rpm.
After purification is completed, the filter cake is filtered by suction and washed by deionized water until the pH is close to neutral, for example, the filter cake can be washed until the pH is about 5.5-7, and then dried for 10-15 hours at 100-130 ℃. When testing the pH value, 0.1-0.5 mg of filter cake can be dissolved in 1-5 mg of water, and the pH value can be measured by dipping the solution with pH test paper.
In an embodiment of the present invention, the hydroxylating the purified carbon nanotubes may include: and mixing the purified carbon nano tube with a hydroxylation reagent, carrying out hydroxylation reaction, carrying out suction filtration, washing and drying a filter cake to obtain the hydroxylated carbon nano tube.
In an embodiment of the present invention, the mass ratio of the purified carbon nanotubes to the pure hydroxylation reagent (i.e., excluding the solvent in the hydroxylation reagent) may be 1:10 to 20, and for example, may be 1:10 to 15. This mass ratio ensures that the hydroxylation reaction proceeds relatively completely and that the hydroxylation reagent is not present in excess.
In the embodiment of the invention, the hydroxylating reagent can be a mixed solution of hydrogen peroxide and ferrous sulfate, wherein the mass ratio of the hydrogen peroxide to the ferrous sulfate is (pure H)2O2Ferrous sulfate) may be 100 to 200:1, for example, 100 to 150: 1. In the hydroxylation reagent, hydrogen peroxide participates in hydroxylation reaction, and ferrous sulfate is used as a catalyst. The above mass ratio ensures that the hydroxylation reaction proceeds more fully and the catalyst is not in excess.
In the embodiment of the invention, the hydroxylation reaction time may be 9-12 hours, for example, 11-12 hours.
In an embodiment of the present invention, the hydroxylation reaction may include a hydroxylation reaction under ultrasonic dispersion conditions and a hydroxylation reaction under standing conditions. The hydroxylation reaction under the ultrasonic dispersion condition can comprise ultrasonic dispersion for 2-4 hours at the power of 200-600W at room temperature. The hydroxylation reaction time under the standing condition can be 8-10 h.
After the hydroxylation reaction is finished, the filter cake is filtered, washed by deionized water until the pH value is close to neutral, for example, the filter cake can be washed until the pH value is about 6.7-8, and then dried for not less than 12 hours at the temperature of 100-130 ℃. When testing the pH value, 0.1-0.5 mg of filter cake can be dissolved in 1-5 mg of water, and the pH value can be measured by dipping the solution with pH test paper.
In an embodiment of the present invention, the reacting the hydroxylated carbon nanotube with the coupling agent may include: and mixing the hydroxylated carbon nano tube with a coupling agent and a dispersing solvent, carrying out coupling reaction, carrying out suction filtration, washing and drying a filter cake to obtain the surface-modified carbon nano tube.
In the embodiment of the invention, the temperature of the coupling reaction may be 50 to 90 ℃, for example, 60 to 80 ℃; the time can be 5 to 8 hours, for example, 6 to 7 hours.
In the embodiment of the invention, the mass ratio of the hydroxylated carbon nanotube to the coupling agent can be 1: 0.5-4, and can be 1: 1-3.
In the embodiment of the present invention, the coupling agent may be selected from any one or more of silane coupling agents, for example, any one or more selected from 3-glycidoxypropyltrimethoxysilane (KH560), methacryloxypropyltrimethoxysilane (KH570), and aminopropyltriethoxysilane (KH550), preferably KH 560.
After the hydroxylated carbon nano tube is mixed with the coupling agent and the dispersing solvent, the mixture can be ultrasonically dispersed for 1-2 hours at the power of 200-600W, and then the coupling reaction is carried out at the temperature of 60-80 ℃.
In an embodiment of the present invention, the dispersion solvent may be ethanol, methanol, or toluene. The dispersion solvent is used for dispersing the hydroxylated carbon nanotubes and the coupling agent, and the amount of the dispersion solvent is not critical as long as the carbon nanotubes and the coupling agent can be sufficiently dispersed, and for example, the ratio of the mass of the dispersion solution to the total mass of the hydroxylated carbon nanotubes and the coupling agent can be 3-5: 1.
After the coupling reaction is completed, a solvent is needed to wash off the coupling agent which is not completely reacted in the filter cake, and the solvent can be acetone. And then, drying the filter cake in a vacuum drying oven at the temperature of 80-100 ℃ for more than or equal to 12 hours.
In the embodiment of the invention, when preparing the aqueous solution of the composite material of the carbon nano tube and the fullerene, the carbon nano tube, the fullerene and the water after surface modification can be mixed in a container, and then ultrasonic dispersion is carried out at the power of 200-600W until the carbon nano tube and the fullerene are not attached to the inner wall of the container and the solution in the container is not layered, wherein the ultrasonic dispersion time is generally more than or equal to 2 h.
In the embodiment of the invention, in the composite material aqueous solution of the carbon nano tube and the fullerene, the mass ratio of the carbon nano tube after the surface modification to the fullerene can be (0.2-1): 1, for example, (0.4-0.9): 1. The mass ratio can ensure that the carbon nano tube and the fullerene can be uniformly dispersed in water, and the carbon nano tube can better improve the concentration of negative ions.
In the embodiment of the invention, the method used for depositing and growing the composite material layer of the carbon nanotube and the fullerene on the surface of the conductive metal wire can be a vertical deposition method. The method for depositing the composite material layer by adopting the vertical deposition method is simple, the growth temperature is low, the viscosity of the growth solution is low, the integrity of the grown composite material layer is good, and the surface is more uniform.
In an embodiment of the present invention, the conditions of the vertical deposition method may include: the temperature is 50 to 120 ℃, for example, the temperature is 60 to 100 ℃; the time is 15 to 31 hours, for example, 16 to 30 hours. The deposition temperature of 50-120 ℃ is favorable for forming a composite material layer with good compactness, and the speed of forming the composite material layer is high. The deposition time of 15-31 hours is beneficial to forming a composite material layer with a desired thickness, and the deposition time of 15-31 hours is beneficial to forming the composite material layer with the desired thickness.
In the embodiment of the invention, the thickness of the composite material layer can be 2-10 nm. The composite material layer with the thickness can release negative ions with higher concentration, has better adhesiveness on the conductive metal wire and is not easy to fall off.
In an embodiment of the present invention, the method may further include: and after the growth of the composite material layer is finished, taking the composite material negative ion release head out of the composite material aqueous solution of the carbon nano tube and the fullerene, 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 second aspect, the embodiment of the invention provides a composite material negative ion release head prepared by the method.
In a third 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 composite anion releasing head prepared by the above method.
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 negative ion release head.
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 concentrated nitric acid used in the following examples is commercially available concentrated nitric acid with a mass fraction of 68%, and the concentrated sulfuric acid is commercially available concentrated sulfuric acid with a mass fraction of 98%.
Example 1
As shown in fig. 2, the method for preparing the negative ion discharging head and the negative ion generating electrode of the present embodiment includes:
s1: adding carbon nano tubes into mixed acid of concentrated nitric acid and concentrated sulfuric acid to enable the carbon nano tubes to be completely immersed, ultrasonically dispersing for 4 hours at the power of 200W, stopping ultrasonic dispersion, stirring for 7 hours at the speed of 100rpm at room temperature, performing suction filtration, washing filter cakes with deionized water, dissolving 0.1mg of the filter cakes in 1mg of the deionized water after washing is finished, dipping the solution with pH test paper to measure the pH value to be 6.8, and drying the filter cakes for 15 hours at the temperature of 100 ℃ to obtain purified carbon nano tubes; wherein, the mass ratio of the concentrated nitric acid to the concentrated sulfuric acid is 30:1 by taking the pure nitric acid and the pure sulfuric acid as the reference;
s2: adding a mixed solution of hydrogen peroxide and ferrous sulfate into the purified carbon nano tube, ultrasonically dispersing for 4h at the power of 200W, standing for reacting for 8h, carrying out suction filtration, washing a filter cake with deionized water, dissolving 0.1mg of the filter cake in 1mg of deionized water after washing, dipping the solution with pH test paper to measure the pH value to be 7.1, and drying the filter cake for 18h at the temperature of 100 ℃ to obtain the hydroxylated carbon nano tube; wherein, pure H is used2O2And ferrous sulfate, wherein the mass ratio of the purified carbon nano tube, the hydrogen peroxide and the ferrous sulfate is 10:100: 1;
s3: mixing the hydroxylated carbon nanotube with KH550, adding ethanol with the mass of 3 times that of the mixture, ultrasonically dispersing for 2h at the power of 200W, then reacting for 7h at the constant temperature of 60 ℃, carrying out suction filtration, washing a filter cake with acetone, then putting the filter cake into a vacuum drying oven, and drying for 20h at the temperature of 80 ℃ to obtain the surface-modified carbon nanotube; wherein the mass ratio of the hydroxylated carbon nanotube to the KH550 is 1: 1;
s4: mixing the surface-modified carbon nano tube, fullerene and deionized water in a container according to the mass ratio of 0.4:1:1, and ultrasonically dispersing at the power of 200W until no carbon nano tube and fullerene are attached to the inner wall of the container and the solution in the container is not layered to obtain the composite material aqueous solution of the carbon nano tube and the fullerene;
s5: bundling 25 titanium wires on a titanium rod through copper wires, putting the titanium wires into the composite material aqueous solution of the carbon nano tube and the fullerene, 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 composite material layer of the carbon nano tube and the fullerene with the thickness of 4nm on the titanium wires by adopting a vertical deposition method, thereby obtaining a composite material negative ion release head;
s6: and taking the composite material negative ion release head out of the composite material water solution of the carbon nano tube and the fullerene, and drying for 60 minutes at a constant temperature of 60 ℃.
Example 2
As shown in fig. 2, the method for preparing the negative ion discharging head and the negative ion generating electrode of the present embodiment includes:
s1: adding carbon nano tubes into mixed acid of concentrated nitric acid and concentrated sulfuric acid to enable the carbon nano tubes to be completely immersed, ultrasonically dispersing for 3 hours at the power of 400W, stopping ultrasonic dispersion, stirring for 6 hours at the speed of 200rpm at room temperature, performing suction filtration, washing filter cakes with deionized water, dissolving 0.3mg of the filter cakes in 3mg of the deionized water after washing is finished, dipping the solution with pH test paper to measure the pH value to be 6.9, and drying the filter cakes for 13 hours at the temperature of 120 ℃ to obtain purified carbon nano tubes; wherein, the mass ratio of the concentrated nitric acid to the concentrated sulfuric acid is 45:1 by taking the pure nitric acid and the pure sulfuric acid as the reference;
s2: adding a mixed solution of hydrogen peroxide and ferrous sulfate into the purified carbon nano tube, ultrasonically dispersing for 3h at the power of 400W, standing for reaction for 9h, carrying out suction filtration, washing a filter cake with deionized water, dissolving 0.1mg of the filter cake in 1mg of deionized water after washing, dipping the solution with pH test paper to measure the pH value to be 7.0, and drying the filter cake for 16h at the temperature of 90 ℃ to obtain the hydroxylated carbon nano tube; wherein, pure H is used2O2And ferrous sulfate, wherein the mass ratio of the purified carbon nano tube, the hydrogen peroxide and the ferrous sulfate is 12:150: 1;
s3: mixing the hydroxylated carbon nanotube with KH560, adding methanol with 4 times of the mass of the mixture, ultrasonically dispersing for 2h at the power of 400W, then reacting for 6.5h at the constant temperature of 70 ℃, filtering, washing a filter cake with acetone, then putting the filter cake into a vacuum drying oven, and drying for 17h at the temperature of 90 ℃ to obtain the surface-modified carbon nanotube; wherein the mass ratio of the hydroxylated carbon nanotube to the KH560 is 1: 2;
s4: mixing the surface-modified carbon nano tube, fullerene and deionized water in a container according to the mass ratio of 0.6:1:1, and ultrasonically dispersing at the power of 400W until no carbon nano tube and fullerene are attached to the inner wall of the container and the solution in the container is not layered to obtain the composite material aqueous solution of the carbon nano tube and the fullerene;
s5: bundling 30 molybdenum wires on a molybdenum rod through copper wires, putting the molybdenum wires into the composite material aqueous solution of the carbon nano tube and the fullerene, then putting the molybdenum wires into a thermostat, setting the temperature of the thermostat to be 80 ℃ and the time to be 20 hours, and growing a composite material layer of the carbon nano tube and the fullerene with the thickness of 6nm on the molybdenum wires by adopting a vertical deposition method, thereby obtaining a composite material negative ion release head;
s6: and taking the composite material negative ion release head out of the composite material water solution of the carbon nano tube and the fullerene, and drying for 50 minutes at a constant temperature of 70 ℃.
Example 3
As shown in fig. 2, the method for preparing the negative ion discharging head and the negative ion generating electrode of the present embodiment includes:
s1: adding carbon nano tubes into mixed acid of concentrated nitric acid and concentrated sulfuric acid to enable the carbon nano tubes to be completely immersed, ultrasonically dispersing for 2 hours at the power of 600W, stopping ultrasonic dispersion, stirring for 5 hours at the speed of 300rpm at room temperature, performing suction filtration, washing filter cakes with deionized water, dissolving 0.5mg of the filter cakes in 5mg of the deionized water after washing is finished, dipping the solution with pH test paper to measure the pH value to be 6.5, and drying the filter cakes for 10 hours at the temperature of 130 ℃ to obtain purified carbon nano tubes; wherein, the mass ratio of the concentrated nitric acid to the concentrated sulfuric acid is 60:1 by taking the pure nitric acid and the pure sulfuric acid as the reference;
s2: adding a mixed solution of hydrogen peroxide and ferrous sulfate into the purified carbon nano tube, ultrasonically dispersing for 2h at 600W, standing for 10h for reaction, carrying out suction filtration, washing a filter cake with deionized water, dissolving 0.3mg of the filter cake into 3mg of deionized water, dipping the solution with pH test paper to measure the pH of the solution to be 6.9, and drying the filter cake at 130 ℃ for 13h to obtain a hydroxylated carbon nano tube; wherein the pure H is used2O2And ferrous sulfate, wherein the mass ratio of the purified carbon nano tube to the hydrogen peroxide to the ferrous sulfate is 13:200: 1;
s3: mixing the hydroxylated carbon nanotube with KH570, adding ethanol with the mass of 4 times that of the mixture, ultrasonically dispersing for 1h at the power of 600W, then reacting for 6h at the constant temperature of 80 ℃, carrying out suction filtration, washing a filter cake with acetone, then putting the filter cake into a vacuum drying oven, and drying for 13h at the temperature of 100 ℃ to obtain the surface-modified carbon nanotube; wherein the mass ratio of the hydroxylated carbon nanotube to the KH570 is 1: 3;
s4: mixing the surface-modified carbon nano tube, fullerene and deionized water in a container according to the mass ratio of 0.9:1:1, and ultrasonically dispersing at the power of 600W until no carbon nano tube and fullerene are attached to the inner wall of the container and the solution in the container is not layered to obtain the composite material aqueous solution of the carbon nano tube and the fullerene;
s5: bundling 30 tungsten wires on a tungsten rod through copper wires, putting the tungsten wires into the composite material aqueous solution of the carbon nano tube and the fullerene, then putting the tungsten wires into a thermostat, setting the temperature of the thermostat to be 100 ℃ and the time to be 16 hours, and growing a composite material layer of the carbon nano tube and the fullerene with the thickness of 10nm on the tungsten wires by adopting a vertical deposition method, thereby obtaining a composite material negative ion release head;
s6: and taking the composite material negative ion release head out of the composite material water solution of the carbon nano tube and the fullerene, and drying for 30 minutes at a constant temperature of 80 ℃.
Example 4
This example differs from example 2 only in that: the mass ratio of the carbon nano tube, the hydrogen peroxide and the ferrous sulfate purified in the step S2 is 7.5:150: 1.
Example 5
This example differs from example 2 only in that: the isothermal reaction in step S3 was carried out at 50 ℃ for 8 h.
Example 6
This example differs from example 2 only in that: the mass ratio of the surface-modified carbon nanotubes, the fullerene and the deionized water in the step S4 is 0.2:1: 1.
Example 7
This example differs from example 2 only in that: the temperature of the oven in step S5 was 120 ℃.
Comparative example 1
The negative ion emitting head of this comparative example comprises fullerene and the same molybdenum rod as in example 2 of the present invention, and fibers of the fullerene are bundled on the molybdenum rod.
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
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. 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
The test results of the negative ion emitting heads of examples and comparative examples are shown in Table 1 (note: the left, middle and right in Table 1 indicate the 22.5 degree left direction, the right direction and the front direction of the negative ion emitting head, respectively).
TABLE 1
As can be seen from table 1, compared with the fullerene anion release head of the comparative example, the anion release amount of the composite anion release head of the embodiment of the present invention is significantly increased, which indicates that the introduction of the carbon nanotubes increases the release amount of anions, so that the composite anion release head of the embodiment of the present invention can generate ecological-grade small-particle-size negative oxygen ions with a large number of small particle sizes, high activity and a long migration distance.
Moreover, the introduction of the conductive metal wire improves the hardness of the anion release head, thereby prolonging the service life of the anion release head.
5) Test result two
The negative ion emitting heads of each example and comparative example 1 were allowed to emit negative ions at approximately the same concentration, and the output voltage required for the negative ion emitting heads of each example was tested, that is, at a vertical distance of 2m, the left-concentration of negative ions emitted from the negative ion emitting heads of each example was allowed to be 29 × 104～34×104pcs/cm3Medium-concentration of 38 × 104～45×104pcs/cm3Right-concentration of 29 × 104～36×104pcs/cm3The maximum output voltages required for the negative ion emitting heads of examples 1 to 7 were 35kV, 32kV, 34kV, 37kV, 38kV, 38.5kV and 39kV, respectively, which were lower than the output voltage of 40kV required for the negative ion emitting head of the comparative example, indicating that the negative pressure required for the negative ion emitting head of the composite material of the example of the present invention was lower, so that the safety of use of the negative ion generator could be improved and the cost of generating negative ions could be reduced.
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
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. 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 2m 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
Ozone and nitrogen oxides (NO and NO) of anion discharge heads of examples and comparative examples2Total release) test results are shown in table 2.
TABLE 2
As can be seen from table 2, the composite material 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, as compared to the fullerene anion releasing heads of the comparative examples, indicating that the introduction of carbon nanotubes and conductive wires did not adversely affect the purity of anions.
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 method of making a composite negative ion release head, the method comprising:
carrying out surface modification on the carbon nano tube;
mixing the carbon nano tube with the surface modified, fullerene and water to obtain a composite material aqueous solution of the carbon nano tube and the fullerene; and
and putting a conductive metal wire into the composite material aqueous solution of the carbon nano tube and the fullerene, and depositing and growing a composite material layer of the carbon nano tube and the fullerene on the surface of the conductive metal wire to obtain the composite material negative ion release head.
2. The method of claim 1, wherein the surface modifying the carbon nanotubes comprises:
purifying the carbon nano tube;
hydroxylating the purified carbon nano tube; and
and reacting the hydroxylated carbon nano tube with a coupling agent to obtain the surface modified carbon nano tube.
3. The method of claim 2, wherein the method for purifying the carbon nanotubes comprises a mixed acid oxidation method;
optionally, the conditions of the mixed acid oxidation process include: the mixed acid is the mixed acid of acid A and acid B, the acid A is concentrated hydrochloric acid and/or concentrated nitric acid, and the acid B is concentrated sulfuric acid; and/or
The oxidation time is 7-11 h;
optionally, the mass ratio of the A acid to the B acid calculated by pure A acid to pure B acid is 20-70: 1.
4. The method of claim 2, wherein the hydroxylating the purified carbon nanotubes comprises: mixing the purified carbon nano tube with a hydroxylation reagent, carrying out hydroxylation reaction, carrying out suction filtration, washing and drying a filter cake to obtain a hydroxylated carbon nano tube;
optionally, the hydroxylation treatment conditions include: the mass ratio of the purified carbon nano tube to the pure hydroxylation reagent is 1: 10-20, and optionally 1: 10-15; and/or
The hydroxylation reaction time is 9-12 h;
also optionally, the hydroxylating agentIs a mixed solution of hydrogen peroxide and ferrous sulfate, further optionally pure H of hydrogen peroxide and ferrous sulfate2O2The mass ratio of the pure ferrous sulfate to the pure ferrous sulfate is 100-200: 1.
5. The method of claim 2, wherein reacting the hydroxylated carbon nanotubes with a coupling agent comprises: mixing the hydroxylated carbon nano tube with a coupling agent and a dispersing solvent, carrying out coupling reaction, carrying out suction filtration, washing and drying a filter cake to obtain a surface-modified carbon nano tube;
optionally, the conditions of the coupling reaction include: the temperature is 50-90 ℃, optionally 60-80 ℃, the time is 5-8 hours, and optionally 6-7 hours; and/or
The mass ratio of the hydroxylated carbon nanotube to the coupling agent is 1: 0.5-4, and optionally 1: 1-3.
6. The method of claim 5, wherein the coupling agent is selected from any one or more of silane coupling agents, optionally from any one or more of 3-glycidoxypropyltrimethoxysilane, methacryloxypropyltrimethoxysilane, and aminopropyltriethoxysilane.
7. The method according to claim 1, wherein the mass ratio of the surface-modified carbon nanotubes to the fullerenes in the aqueous composite solution of carbon nanotubes and fullerenes is (0.2-1): 1, optionally (0.4-0.9): 1.
8. The method of claim 1, wherein the method for depositing and growing the composite material layer of carbon nanotubes and fullerenes on the surface of the conductive metal wire is a vertical deposition method;
optionally, the conditions of the vertical deposition process include: the temperature is 50-120 ℃, and further optionally, the temperature is 60-100 ℃; the time is 15 to 31 hours, and further optionally 16 to 30 hours.
9. A composite negative ion-releasing head prepared by the method of any one of claims 1-8.
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 through the conductive fixing device, and the anion releasing head is electrically connected with the metal rod, the anion releasing head is the composite anion releasing head of claim 9.
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