CN116803900A - Method for preparing carbon nano tube solution - Google Patents

Method for preparing carbon nano tube solution Download PDF

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CN116803900A
CN116803900A CN202210245857.4A CN202210245857A CN116803900A CN 116803900 A CN116803900 A CN 116803900A CN 202210245857 A CN202210245857 A CN 202210245857A CN 116803900 A CN116803900 A CN 116803900A
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solution
liquids
solvents
liquid
carbon
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杨盛贤
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Qujing Huajin Rainforest Technology Co ltd
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Qujing Huajin Rainforest Technology Co ltd
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    • 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
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
    • 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
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment

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  • Engineering & Computer Science (AREA)
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Abstract

The invention discloses a preparation method of a carbon nanotube solution, and belongs to the technical field of nano materials. The invention firstly adds a surfactant and a first dispersing agent into the carbon nano tube solution, carries out preliminary chemical dispersion treatment on the carbon nano tube, then adds a second dispersing agent for dispersion, and finally filters and replaces the carbon nano tube solution by different solvents (solutions), thereby removing various impurities and simultaneously enabling the carbon nano tube to be uniformly dispersed in various solvents (solutions). The invention has the advantages that the carbon nano tube is uniformly dispersed in various solvents (liquids), various impurities in the carbon nano tube are removed efficiently, and the preparation cost of the carbon nano tube is reduced. The carbon nano tube prepared by the method has high purity, good dispersion uniformity, good dispersion stability and high repeatability, and has the possibility of application and popularization.

Description

Method for preparing carbon nano tube solution
Technical Field
The invention belongs to the technical field of new material preparation, and in particular provides a method for preparing a carbon nano tube solution.
Background
The carbon nanotube is one-dimensional material with special structure and is mainly formed into coaxial circular tube with several layers to several tens layers of carbon atoms in hexagonal arrangement and sp 2 Hybridization is dominant. The nano-tube is divided into a single-wall carbon nano-tube, a double-wall carbon nano-tube and a multi-wall carbon nano-tube, the tube diameter is generally from a few hundred nanometers to a meter, and the length can reach a micron level. The carbon nano tube is used as a one-dimensional nano material, has light weight, perfect hexagonal structure connection, excellent mechanical, thermal, electrical and chemical properties and wide application prospect in various fields.
Although carbon nanotubes have many excellent characteristics, two problems exist in practical application, namely, how to uniformly disperse carbon nanotubes in various solvents (liquids); and secondly, how to purify the prepared carbon nano tube.
The carbon nanotubes have strong van der Waals force, large specific surface area and high length-diameter ratio, so that the agglomeration and winding are extremely serious, and the carbon nanotubes are difficult to disperse in various solvents (liquid), so that the application of the carbon nanotubes is limited. The uniformity of the dispersion of the carbon nanotubes in the matrix of the composite material is an important index affecting the performance of the material, the more uniform the dispersion, the more obvious the effect as an additive material, and the better the overall performance of the composite material. In order to embody the excellent performance of the carbon nanotubes in application, one of the key problems is how to uniformly and stably disperse the carbon nanotubes in a solution system. At present, the nano-scale dispersion is realized as much as possible by mainly adopting methods such as mechanical stirring, ball milling, ultrasonic treatment, chemical modification, surfactant addition and the like. However, mechanical stirring only enables the carbon nanotube agglomerates to be macroscopically mixed with the matrix powder, and the carbon nanotube agglomerates cannot be dispersed. The ball milling can cut off the carbon nano tube to form a small aggregate, which is difficult to work on the aggregate and can not solve the problem of aggregation well. The ultrasonic treatment can damage the structure of the carbon nano tube and shake off the carbon nano tube. The chemical modification can introduce hydroxyl, carboxyl and other strong polar groups, so that the conductivity is reduced, and the subsequent filtration and separation process is longer. The addition of the surfactant has no significant effect on the tightly entangled carbon nanotubes, while introducing new impurities.
A large amount of impurities are inevitably generated in various methods for preparing carbon nanotubes, and mainly include metal catalysts containing nickel, iron, cobalt, etc., amorphous carbon, etc. In order to obtain carbon nanotubes with higher purity, these impurities are usually removed with strong acids and strong oxidizing agents. However, the method introduces surface defects such as oxygen-containing groups, five-membered rings, seven-membered rings and the like on the surface of the carbon nano tube while removing impurities, thereby reducing various performances of the carbon nano tube. Meanwhile, chemical reagents used in purification contain elements such as sulfur, nitrogen, chlorine, fluorine, phosphorus and the like, and various impurities are inevitably introduced into the carbon nano tube. The existing technology for dispersing the carbon nanotubes also requires a large amount of surfactant, wherein the surfactant is generally 20% -500% of the mass of the carbon nanotubes, and for downstream application, the surfactant also belongs to impurities. It is very difficult to remove various impurities contained in the carbon nanotubes in industrial production.
Therefore, based on the prior art, a person skilled in the art needs to research an efficient, convenient and low-cost method, and the following two points are achieved in the process of preparing the carbon nanotube solution at the same time: (1) So that the carbon nano-tubes are uniformly dispersed in various solvents (liquids); (2) efficiently removing various impurities in the carbon nanotubes.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing carbon nano tubes, which simultaneously achieves the following two points in the process of preparing carbon nano tube solution: (1) So that the carbon nano-tubes are uniformly dispersed in various solvents (liquids); (2) efficiently removing various impurities in the carbon nanotubes.
The specific principle of action of the invention is as follows.
The invention makes the principle of uniformly dispersing the carbon nano tube in the solution as follows: (1) Adding a surfactant and a first dispersing agent into the carbon nano tube solution, and performing chemical dispersion treatment, wherein small molecules such as the surfactant, the unreacted first dispersing agent, a chemical dispersion treatment product and the like are adsorbed on the surface of the carbon nano tube through interactions such as hydrogen bonds, van der Waals forces, intermolecular forces and the like, so that the carbon nano tube is uniformly dispersed in the solution; (2) After chemical dispersion treatment, adding a second dispersing agent into the carbon nano tube solution, wherein the second dispersing agent has a dispersing effect in the presence of one or more of the following independent or simultaneous conditions: the first case is that the second dispersant reacts with various chemical substances in the carbon nanotube solution after chemical dispersion treatment to generate gas, the second case is that the second dispersant itself decomposes to generate gas, and the third case is that a plurality of second dispersants react with each other to generate gas. The generated gas is one or a mixture of several gases: oxygen, carbon dioxide, nitrogen, ammonia, hydrogen, ozone, fluorine, chlorine, bromine, nitrogen monoxide, nitrogen dioxide, chlorine dioxide. The generated gas is adsorbed on the surface of the carbon nano tube, so that agglomeration is avoided, and the carbon nano tube is kept uniformly dispersed in the solution; (3) After the second dispersant is added, the substances which keep the carbon nano tubes uniformly dispersed become gas and various small molecules.
The principle of the invention for removing impurities in the carbon nano tube is as follows: the gas adsorbed on the surface keeps the dispersion of the carbon nano tube, and the solvent (liquid) can smoothly flow through the inner space of the material, and various impurities in the solution are taken away during filtration, so that the impurities in the carbon nano tube solution are removed. Removed impurities include, but are not limited to: (1) impurities generated during the preparation and purification of carbon nanotubes; (2) The surfactant, the unreacted first dispersant and the chemical dispersion treatment product added in the first step; (3) Unreacted second dispersant and chemical reaction product in the second step; (4) impurities introduced in the preparation of the carbon nanotube solution. The method is simple, quick and efficient, and is beneficial to reducing the production cost of the carbon nano tube.
The invention adds the first dispersing agent into the carbon nano tube solution to carry out chemical dispersion treatment, and has the following three processes: (1) The small molecules of the first dispersing agent are adsorbed on the surface of the carbon nano tube through interactions of hydrogen bonds, van der Waals forces, intermolecular forces and the like, so that the carbon nano tube is uniformly dispersed in the solution; (2) In the prior preparation process of the carbon nano tube, various oxygen-containing functional groups, nitrogen-containing functional groups and sulfur-containing functional groups including carboxyl, hydroxyl, epoxy, carbonyl and the like are inevitably introduced to the surface of the carbon nano tube through the purification process of strong acid and strong oxidant. The first dispersing agent can reduce the carbon nano tube while keeping the carbon nano tube uniformly dispersed, and remove various functional groups such as carboxyl, hydroxyl, epoxy, carbonyl and the like on the surface of the carbon nano tube. Particularly, the functionalized carbon nanotubes such as carboxylated carbon nanotubes and hydroxylated carbon nanotubes generally need reduction treatment when in use, and the first dispersing agent plays a role in reduction. (3) Metals such as nickel, iron, and cobalt contained in the carbon nanotubes react with the first dispersant, and are dissolved in the solution.
The invention can lead the carbon nano tube to be evenly dispersed in different solvents (liquid) according to the following principle: the solution in which the carbon nanotubes are uniformly dispersed in the first solvent (liquid) is replaced with the second solvent (liquid) by utilizing the mutual solubility of the solvents (liquids), and a solution in which the carbon nanotubes are uniformly dispersed in the second solvent (liquid) is obtained.
The principle of the invention for adjusting the concentration of the carbon nano tube solution is as follows: for the uniformly dispersed carbon nanotube solution, a certain amount of solvent (liquid) is newly added, or the excessive solvent (liquid) is removed by filtration, so that the concentration of the solution can be conveniently adjusted. Wherein the concentration of the single-walled carbon nanotube solution is generally 0.1-mg/mL to 10-mg/mL, the concentration of the double-walled carbon nanotube solution is generally 1-mg-20-mg/mL, and the concentration of the multi-walled carbon nanotube solution is generally 5-mg-200-mg/mL. By measuring the concentration of the solution, the uniformity of the dispersion of the carbon nanotubes in the solution is known to be good.
The invention is realized by the following technical scheme, which comprises the following steps:
the method comprises the steps of firstly, adding a surfactant and a first dispersing agent into a carbon nano tube to react in a solution to obtain a carbon nano tube solution subjected to chemical dispersion treatment;
secondly, adding the solution obtained in the first step into a second dispersing agent, mixing and reacting to obtain a solution containing impurities, wherein the solution contains carbon nanotubes uniformly dispersed;
And thirdly, adding the solution obtained in the second step into a solvent (liquid), filtering and replacing to remove impurities in the carbon nanotube solution, and obtaining a solution with uniformly dispersed carbon nanotubes after removing the impurities.
Preferably, the meaning of the solvent (liquid) in the present invention is as follows: according to the general rule, a liquid containing one component is called a solvent, and a liquid containing two or more components is called a solution.
Preferably, the carbon nanotubes in the first step are used as a mixture of one or more of the following: single-walled carbon nanotubes, double-walled carbon nanotubes, multi-walled carbon nanotubes, aminated carbon nanotubes, carboxylated carbon nanotubes, hydroxylated carbon nanotubes, fluorine-doped carbon nanotubes, nitrogen-doped carbon nanotubes, nickel-coated carbon nanotubes, aminated multi-walled carbon nanotubes, carboxylated multi-walled carbon nanotubes, hydroxylated multi-walled carbon nanotubes, fluorine-doped multi-walled carbon nanotubes, nitrogen-doped multi-walled carbon nanotubes, aminated single-walled carbon nanotubes, carboxylated single-walled carbon nanotubes, hydroxylated single-walled carbon nanotubes, fluorine-doped single-walled carbon nanotubes, nitrogen-doped single-walled carbon nanotubes.
Preferably, the solvent (liquid) for preparing the carbon nanotube solution in the first step is a common public solvent (liquid), and one or more of the following are commonly used: water, methanol, ethanol, propanol, acetone, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone.
Preferably, the carbon nanotube solution is prepared in the first step, and the concentration is 0.05-100 mg/mL according to different types of actually used carbon nanotubes, and the common concentration is as follows: 0.05 mg/mL, 0.1 mg/mL, 0.2 mg/mL, 0.3 mg/mL, 0.4 mg/mL, 0.5 mg/mL, 0.6 mg/mL, 0.7 mg/mL, 0.8 mg/mL, 0.9 mg/mL, 1 mg/mL, 1.5 mg/mL, 2 mg/mL, 2.5 mg/mL, 3 mg/mL, 4 mg/mL, 5 mg/mL, 6 mg/mL, 7 mg/mL, 8 mg/mL, 9 mg/mL, 10 mg/mL, 11 mg/mL, 12 mg/mL, 13 mg/mL, 14 mg/mL, 15 mg/mL, 20 mg/mL, 30 mg/mL, 40 mg/mL, 50 mg/mL, 60 mg/mL, 70 mg/mL, 80 mg/mL, 90 mg/mL, and 100/mL.
Preferably, in the first step, a surfactant is added to the carbon nanotube solution, and the surfactant is one or more of the following: polyvinylpyrrolidone, polyethylenimine, dodecyltrimethylammonium bromide, tetradecyltrimethylammonium bromide, hexadecyltrimethylammonium bromide, octadecyltrimethylammonium bromide, sodium dodecylbenzenesulfonate, sodium dodecylsulfate, sodium dodecylsulfonate, alkylphenol ethoxylates, triton x-100, polyethylene glycol, aqueous ammonia, N-diethylpropiolate, octadecylamine, gum arabic, cyclodextrin, sodium polystyrene sulfonate, lithium dodecylsulfate, silane coupling agents, polyoxyethylene lauryl ether, polysorbate, polyethylene glycol octylphenyl ether, polypyrrole, polyaniline, sodium cholate, porphyrin molecules, pyrene compounds, polypeptides, proteins, DNA, amylose, amylopectin, iodine, nonionic trinitrotoluene, perylene diimide, anthracene, phenanthrene, hexabenzol.
Preferably, the surfactant is added to the carbon nanotube solution in the first step, and the mass of the surfactant added varies according to the kind of carbon nanotube, the kind of surfactant and the specific condition of the dispersion solvent. The mass ratio of the carbon nano tube to the surfactant is 1 (0-50), and the mass ratio is as follows: 1:0, 1:0.01, 1:0.02, 1:0.03, 1:0.04, 1:0.05, 1:0.06, 1:0.07, 1:0.08, 1:0.09, 1:0.1, 1:0.15, 1:0.2, 1:0.25, 1:0.3, 1:0.35, 1:0.4, 1:0.45, 1:0.5, 1:0.55, 1:0.6, 1:0.65, 1:0.7, 1:0.75, 1:0.8, 1:0.85, 1:0.9, 1:0.95, 1:1, 1:1.1, 1:1.2, 1:1.3, 1:1.4, 1:1.5, 1:1.6, 1:1.7, 1:1.8, 1:1.9, 1:2, 1:1.5, 1:1.2, 1:1.1.1, 1:1.8, 1:2, 1:1.1.2, 1:1.5, 1:0.8, 1:2.8, 1:0.8, 1. 1:2.2, 1:2.3, 1:2.4, 1:2.5, 1:2.6, 1:2.7, 1:2.8, 1:2.9, 1:3, 1:3.1, 1:3.2, 1:3.3, 1:3.4, 1:3.5, 1:3.6, 1:3.7, 1:3.8, 1:3.9, 1:4, 1:4.1, 1:4.2, 1:4.3, 1:4.4, 1:4.5, 1:4.6, 1:4.7, 1:4.8, 1:4.9, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:20, 1:25, 1:30, 1:35, 1:40.
Preferably, the first dispersant in the first step is one or more of the following: organic acids, borohydrides, citrates, ascorbates, alcohols, saccharides, amino acids, sulfur-containing first dispersants, nitrogen-containing first dispersants, reduced plant extracts, metals, inorganic acids, bases. The organic acids include: ascorbic acid, oxalic acid, gallic acid, citric acid, tannic acid, tartaric acid, formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, oxalic acid, malonic acid, succinic acid, adipic acid, maleic acid, benzoic acid, phenylacetic acid, phthalic acid, terephthalic acid, fatty acids, acrylic acid, trifluoroacetic acid, dehydroascorbic acid, paleo Le Tangsuan, threonic acid; the borohydride includes: lithium borohydride, sodium borohydride, potassium borohydride, rubidium borohydride, aluminum borohydride, beryllium borohydride, calcium borohydride, zinc borohydride, magnesium borohydride, cesium borohydride, strontium borohydride, barium borohydride, cuprous borohydride, titanium borohydride, zirconium borohydride, yttrium borohydride, manganese borohydride, iron borohydride, nickel borohydride, and borane; the citrate salt comprises: lithium citrate, sodium citrate, magnesium citrate, aluminum citrate, potassium citrate, calcium citrate, ammonium citrate, ferric citrate, ferrous citrate, nickel citrate, cobalt citrate, manganese citrate, chromium citrate, copper citrate, zinc citrate, barium citrate; ascorbate salts include: lithium ascorbate, sodium ascorbate, magnesium ascorbate, aluminum ascorbate, potassium ascorbate, calcium ascorbate, ammonium ascorbate, ferrous ascorbate, nickel ascorbate, cobalt ascorbate, manganese ascorbate, chromium ascorbate, copper ascorbate, zinc ascorbate, barium ascorbate, stannous ascorbate; alcohols include: methanol, benzyl alcohol, ethanol, ethylene glycol, propanol, isopropanol, butanol, sorbitol; the saccharides include: monosaccharides (glucose, fructose, galactose), disaccharides (sucrose, lactose, maltose), oligosaccharides (cyclodextrin), polysaccharides (chitosan); amino acids include: l-cysteine, L-glutathione; the sulfur-containing first dispersant includes: thiourea, thiourea dioxide, ethanethiol, thiophene, lawson reagent, lithium persulfate, sodium persulfate, potassium persulfate, ammonium persulfate; the nitrogen-containing first dispersant includes: ammonia, hydrazine (hydrazine), hydrazine hydrate (hydrazine hydrate), ammonia borane, phenylhydrazine, urea, hydroxylamine hydrochloride, pyrrole, pyridine, benzylamine, p-phenylenediamine, ethylenediamine, dimethylketoxime, lithium nitrite, sodium nitrite, magnesium nitrite, aluminum nitrite, potassium nitrite, calcium nitrite, ammonium nitrite, ferric nitrite, ferrous nitrite, nickel nitrite, cobalt nitrite, manganese nitrite, chromium nitrite, copper nitrite, barium nitrite, zinc nitrite, silver nitrite; the reducing plant extract comprises: tea extract, rose extract, sago cycas leaf extract, orange peel extract, ginkgo leaf extract; the metal comprises: lithium, sodium, magnesium, aluminum, potassium, calcium, beryllium, iron, zinc, tin; the inorganic acids include: sulfuric acid, hydrofluoric acid, hydroiodic acid, hydrobromic acid, hydrochloric acid, phosphoric acid, nitric acid, and carbonic acid; the alkali includes: ammonia, lithium hydroxide, sodium hydroxide, potassium hydroxide.
Preferably, the mass ratio of the carbon nanotubes to the first dispersant in the first step is 1 (1-200), and the mass ratio is 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, 1:20, 1:25, 1:30, 1:35, 1:40, 1:45, 1:50.
Preferably, the chemical dispersion treatment reaction in the first step is carried out for a time of 0 to 120 hours. The common usage is: 1, 1.5, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 50, 52, 54, 56, 58, 60, 64, 68, 72, 76, 80, 84, 88, 92, 96, 100, 104, 108, 112, 116, 120.
Preferably, the reaction temperature of the chemical dispersion treatment in the first step is-10 ℃ to 100 ℃, and is usually: -10 ℃, -5 ℃, 0 ℃, 5 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃.
Preferably, the stirring speed of the chemical dispersion treatment reaction in the first step is 0-3000 r/min. The usual rotational speeds are: 0 r/min (i.e. standing), 10 r/min, 20 r/min, 30 r/min, 40 r/min, 50 r/min, 60 r/min, 70 r/min, 80 r/min, 90 r/min, 100 r/min, 110 r/min, 120 r/min, 130 r/min, 140 r/min, 150 r/min, 180 r/min, 200 r/min, 240 r/min, 300 r/min, 500 r/min, 600 r/min, 700 r/min, 800 r/min, 900 r/min, 1000 r/min.
Preferably, the chemical dispersion treatment reaction in the first step can adjust the relevant parameters of the type of the first dispersing agent, the quality of the first dispersing agent, the reaction time, the reaction temperature and the stirring rotation speed in the experimental process.
Preferably, the second dispersant in the second step is one or more of the following: peroxides, superoxides, percarbonates, persulfates, permanganates and permanganates, manganates, ferrates and ferrates, chlorates and chlorates, carbonates, bicarbonates, bisulphates, ammonium salts, dichromates and bichromates, iodic acids and iodates, bromic and bromates, nitrous acids and nitrites, metals, metal hydrides, acids, bases, perborates, halogen intermetallics. The second dispersant is commonly used as a mixture of one or more of the following: hydrogen peroxide, lithium peroxide, sodium peroxide, potassium peroxide, calcium peroxide, magnesium peroxide, zinc peroxide, strontium peroxide, barium peroxide, lead peroxide, urea hydrogen peroxide complex, 2-dihydro propane, 2, 5-dimethyl-2, 5-dihydro hexane, 2-bis- (t-butyl peroxide) propane, 2-bis- (t-butyl peroxide) butane, 2, 5-dimethyl-2, 5-bis- (t-butyl peroxide) hexane, 2-bis- (4, 4-di-t-butyl cyclohexyl peroxide) propane, 2, 5-dimethyl-2, 5-bis- (2-ethylhexanoyl peroxide) hexane 2, 5-dimethyl-2, 5-bis- (3, 5-trimethylhexanoyl) hexane, 2, 5-dimethyl-2, 5-bis- (benzoyl peroxide) hexane, 1-bis- (t-butyl peroxide) cyclohexane, 1-bis- (t-butyl peroxide) -3, 5-trimethylcyclohexane, acetyl sulfonyl peroxide cyclohexane bis- (1-hydroxycyclohexane) peroxide, 3,3,6,6,9,9-hexamethyl-1, 2,4, 5-tetraoxycyclononane, 2, 5-dimethyl-2, 5-bis- (tert-butyl peroxide) -3-hexyne, isopropyl hydroperoxide, 1, 3-tetramethylbutyl hydroperoxide, cumene hydroperoxide, diisopropyl (yl) benzene hydroperoxide, di-tert-butylisopropyl (yl) benzene hydroperoxide pinane, menthane hydroperoxide, tetralin hydroperoxide, di-tert-butyl peroxide, tert-butylbenzene peroxide, tert-butylisopropyl (yl) benzene peroxide, 1, 3-bis- (2-tert-butylisopropyl) benzene peroxide, 1, 4-bis- (2-tert-butylisopropyl) benzene peroxide, diisopropylbenzene peroxide, isobutylmethylketone peroxide, methylethylketone peroxide, acetylacetone peroxide, cyclohexanone peroxide, methylcyclohexanone peroxide, diacetone peroxide, acetyl peroxide, propionyl peroxide, isobutyryl peroxide, n-octanoyl peroxide n-nonanoyl peroxide, isononyl peroxide, decanoyl peroxide, dodecanoyl peroxide, benzoyl peroxide, di- (2-methylbenzoyl) peroxide, di- (2-chlorobenzoyl) peroxide, di- (2, 4-dichlorobenzoyl) peroxide, acetyl benzoyl peroxide, peroxyformic acid, peroxyacetic acid, succinic acid peroxide, azelaic acid diperoxide, dodecanedioic acid diperoxide, benzoyl peroxide, 3-chlorobenzoic acid peroxide, terephthalic acid, t-butylterephthalic acid, t-butyl peroxyacetate, t-butyl peroxydiethyl acetate, ethyl 3, 3-bis- (t-butyl peroxybutyrate, tert-butyl peroxyisobutyrate, n-butyl 4, 4-bis- (tert-butyl peroxypivalate), tert-butyl peroxypivalate, isopropyl peroxypivalate, tert-butyl peroxy2-ethylhexanoate 1, 3-tetramethylbutyl peroxy3, 5-trimethylhexanoate, tert-butyl peroxyneodecanoate, tert-amyl peroxyneodecanoate, isopropyl peroxyneodecanoate, tert-butyl peroxybutenoate, tert-butyl peroxymaleic acid, tert-butyl peroxybenzoate, tert-butyl peroxyphthalate, bis- (tert-butyl peroxyphthalate), tert-butyl peroxyisopropyl carbonate, tert-butyl peroxyoctadecanoyl carbonate 2, 4-trimethylpentyl-2-peroxy phenoxyacetate, 3-tert-butyl-3-o-hydroxymethylbenzoate, diethyl peroxydicarbonate, di-n-propyl peroxydicarbonate, diisopropyl peroxydicarbonate, di-n-butyl peroxydicarbonate, di-sec-butyl peroxydicarbonate, di- (2-ethylhexyl) peroxydicarbonate, di (isotridecyl) peroxydicarbonate, ditetradecyl peroxydicarbonate, dioctadecyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, di- (4-tert-butylcyclohexyl) peroxydicarbonate, diphenyl peroxydicarbonate, bis- (2-phenoxyethyl) peroxydicarbonate, bis- (3, 5-trimethyl-1, 2-dioxolane), pinene peroxide, chenopodium oil, sodium superoxide, potassium superoxide, lithium percarbonate sodium percarbonate, potassium percarbonate, ammonium percarbonate, calcium percarbonate, aluminum percarbonate, magnesium percarbonate, lithium persulfate, sodium persulfate, potassium persulfate, ammonium persulfate, permanganate, lithium permanganate sodium permanganate, potassium permanganate, ammonium permanganate, calcium permanganate, zinc permanganate, magnesium permanganate, silver permanganate, barium permanganate, lithium manganate, sodium manganate, potassium manganate, ferrate, lithium ferrate, sodium ferrate, potassium ferrate, perchloric acid, lithium perchlorate, sodium perchlorate, potassium perchlorate, magnesium perchlorate, ammonium perchlorate, calcium perchlorate, barium perchlorate, strontium perchlorate, lead perchlorate ferrous perchlorate, silver perchlorate, chloric acid, lithium chlorate, sodium chlorate, potassium chlorate, magnesium chlorate, ammonium chlorate, cesium chlorate, strontium chlorate, barium chlorate, calcium chlorate, copper chlorate, zinc chlorate, silver chlorate, chlorous acid, lithium chlorite, sodium chlorite, potassium chlorite, magnesium chlorite, ammonium chlorite, calcium chlorite, hypochlorous acid, lithium hypochlorite, sodium hypochlorite, potassium hypochlorite, magnesium hypochlorite, calcium hypochlorite, ammonium hypochlorite, barium hypochlorite, chlorine dioxide, lithium carbonate, sodium carbonate, potassium carbonate, ammonium carbonate, calcium carbonate, magnesium carbonate, aluminum carbonate, iron carbonate, copper carbonate, silver carbonate, lithium bicarbonate, sodium bicarbonate, potassium bicarbonate, magnesium bicarbonate, calcium bicarbonate, barium bicarbonate, lithium bisulfate, sodium bisulfate, potassium bisulfate, magnesium bisulfate, calcium bisulfate, ammonium bicarbonate, ammonium nitrate, ammonium hypochlorite, ammonium nitrite, ammonium sulfate, ammonium bisulfate, ammonium fluoride, ammonium chloride, ammonium iodide, ammonium bromide, dichromic acid, lithium dichromate, sodium dichromate, potassium dichromate, ammonium dichromate, magnesium dichromate, silver dichromate, cesium dichromate, barium dichromate, aluminum dichromate, copper dichromate, zinc dichromate, chromium trioxide, periodic acid, ammonium periodate, barium periodate, sodium paraperiodate, sodium metaperiodate, potassium periodate, potassium paraperiodate, potassium metaperiodate, iodic acid, diiodide, ammonium iodate, sodium iodate, potassium iodate-in-iodic acid, potassium iodate-diiodidate, lithium iodate, calcium iodate, strontium iodate, barium iodate, manganese iodate, iron iodate, zinc iodate, silver iodate, cadmium iodate, lead iodate, sodium bromate, potassium bromate, magnesium bromate, strontium bromate, barium bromate, zinc bromate, silver, cadmium bromate lead bromate, hydrobromic acid, sodium bromate, potassium bromate, nitrous acid, lithium nitrite, sodium nitrite, magnesium nitrite, aluminum nitrite, potassium nitrite, calcium nitrite, ammonium nitrite, ferric nitrite, ferrous nitrite, nickel nitrite, cobalt nitrite, manganese nitrite, chromium nitrite, copper nitrite, barium nitrite, zinc nitrite, silver nitrite, lithium, sodium, magnesium, aluminum, potassium, calcium, beryllium, iron, zinc lithium hydride, sodium hydride, aluminum hydride, magnesium hydride, potassium hydride, calcium hydride, barium hydride, nickel hydride, copper hydride, zinc hydride, ascorbic acid, oxalic acid, gallic acid, citric acid, tannic acid, tartaric acid, formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, enanthic acid, caprylic acid, oxalic acid, malonic acid, succinic acid, adipic acid, maleic acid, 2-methylbutyric acid, 2-ethylbutyric acid, 2-ethylhexanoic acid, myristic acid, oleic acid, benzoic acid, phenylacetic acid, phthalic acid, terephthalic acid, fatty acid, acrylic acid, trifluoroacetic acid, dehydroascorbic acid, palo Le Tangsuan, threonic acid, sulfuric acid, hydrofluoric acid, hydroiodic acid, hydrobromic acid, hydrochloric acid, phosphoric acid, nitric acid, carbonic acid, aqueous ammonia, lithium hydroxide, sodium hydroxide, potassium hydroxide, barium perborate, sodium perborate, potassium perborate, rubidium perborate, cesium perborate, calcium perborate, barium perborate, iodine fluoride, bromine monofluoride, chlorine monofluoride, iodine chloride, bromine chloride, iodine bromide, iodine trifluoride, bromine trifluoride, chlorine trifluoride, iodine pentafluoride, bromine pentafluoride, chlorine pentafluoride, iodine heptafluoride.
Preferably, in the second step, the mass ratio of the second dispersant to the initial carbon nanotube is (1-1000): 1, which is usually: 1:1, 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, 11:1, 12:1, 13:1, 14:1, 15:1, 16:1, 17:1, 18:1, 19:1, 20:1, 21:1, 22:1, 23:1, 24:1, 25:1, 26:1, 27:1, 28:1, 29:1, 30:1, 31:1, 32:1, 33:1, 34:1, 35:1, 36:1, 37:1, 38:1, 39:1, 40:1, 41:1, 42:1, 43:1, 44:1, 45:1, 46:1, 47:1, 48:1, 49:1, 50:1, 51:1, 52:1, 53:1, 54:1, 55:1, 56:1, 57:1, 58:1, 60:1, 60:62:1, 64:1). 65:1, 66:1, 67:1, 68:1, 69:1, 70:1, 71:1, 72:1, 73:1, 74:1, 75:1, 76:1, 77:1, 78:1, 79:1, 80:1, 81:1, 82:1, 83:1, 84:1, 85:1, 86:1, 87:1, 88:1, 89:1, 90:1, 91:1, 92:1, 93:1, 94:1, 95:1, 96:1, 97:1, 98:1, 99:1, 100:1, 110:1, 120:1, 130:1, 140:1, 150:1, 160:1, 170:1, 180:1, 190:1, 200:1, 210:1, 220:1, 230:1, 240:1, 250:1, 260:1, 270:1, 280:1, 290:1, 300:1, 350:1, 400:1, 500:1.
Preferably, the reaction time in the second step is 1 minute to 120 hours, and is usually: 1 min, 2 min, 3 min, 4 min, 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, 15 min, 20 min, 25 min, 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min, 65 min, 70 min, 75 min, 80 min, 85 min, 90 min, 95 min, 100 min, 105 min, 110 min, 115 min, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 50, 52, 54, 56, 58, 60, 64, 68, 72, 76, 80, 84, 88, 92, 96, 100, 104, 108, 112, 116, 120.
Preferably, the reaction temperature in the second step is-10 ℃ to 100 ℃, and is usually: -10 ℃, -5 ℃, 0 ℃, 5 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃.
Preferably, the stirring speed of the reaction in the second step is 0-3000 r/min, and is usually: 0 r/min (i.e. standing), 10 r/min, 20 r/min, 30 r/min, 40 r/min, 50 r/min, 60 r/min, 70 r/min, 80 r/min, 90 r/min, 100 r/min, 110 r/min, 120 r/min, 130 r/min, 140 r/min, 150 r/min, 180 r/min, 200 r/min, 240 r/min, 300 r/min, 500 r/min, 600 r/min, 700 r/min, 800 r/min, 900 r/min, 1000 r/min.
Preferably, the dispersing agent in the second step is present singly or in combination of two or more of the following: the first case is that the second dispersant reacts with various chemical substances in the carbon nanotube solution after chemical dispersion treatment to generate gas, the second case is that the second dispersant itself decomposes to generate gas, and the third case is that a plurality of second dispersants react with each other to generate gas. The generated common gas is one or a mixture of the following components: oxygen, carbon dioxide, nitrogen, ammonia, hydrogen, ozone, fluorine, chlorine, bromine, nitrogen monoxide, nitrogen dioxide, chlorine dioxide. The reaction also produces soluble products. Typical examples of the dispersing action of the dispersant are as follows: (1) The first dispersing agent is ascorbic acid, the second dispersing agent is hydrogen peroxide, and the generated gas is: oxygen. (2) The first dispersing agent is ascorbic acid, the second dispersing agent is sodium percarbonate, and the generated gas is as follows: oxygen, carbon dioxide. (3) The first dispersing agent is ascorbic acid, the second dispersing agent is sodium carbonate, and the generated gas is as follows: carbon dioxide. (4) The first dispersing agent is ascorbic acid, the second dispersing agent is hydrogen peroxide and sodium carbonate, and the generated gas is as follows: oxygen, carbon dioxide. (5) The first dispersing agent is ascorbic acid, the second dispersing agent is sodium bicarbonate, and the generated gas is as follows: carbon dioxide. (6) The first dispersing agent is ascorbic acid, the second dispersing agent is hydrogen peroxide and sodium bicarbonate, and the generated gas is as follows: oxygen, carbon dioxide. (7) The first dispersing agent is oxalic acid, the second dispersing agent is hydrogen peroxide, and the generated gas is as follows: oxygen. (8) The first dispersing agent is oxalic acid, the second dispersing agent is sodium percarbonate, and the generated gas is as follows: oxygen, carbon dioxide. (9) The first dispersing agent is oxalic acid, the second dispersing agent is sodium carbonate, and the generated gas is as follows: carbon dioxide. (10) The first dispersing agent is oxalic acid, the second dispersing agent is hydrogen peroxide and sodium carbonate, and the generated gas is as follows: oxygen, carbon dioxide. (11) The first dispersing agent is oxalic acid, the second dispersing agent is sodium bicarbonate, and the generated gas is as follows: carbon dioxide. (12) The first dispersing agent is oxalic acid, the second dispersing agent is hydrogen peroxide and sodium bicarbonate, and the generated gas is as follows: oxygen, carbon dioxide. (13) The first dispersing agent is citric acid, the second dispersing agent is hydrogen peroxide, and the generated gas is as follows: oxygen. (14) The first dispersing agent is citric acid, the second dispersing agent is sodium percarbonate, and the generated gas is as follows: oxygen, carbon dioxide. (15) The first dispersing agent is citric acid, the second dispersing agent is sodium carbonate, and the generated gas is as follows: carbon dioxide. (16) The first dispersing agent is citric acid, the second dispersing agent is hydrogen peroxide and sodium carbonate, and the generated gas is as follows: oxygen, carbon dioxide. (17) The first dispersing agent is citric acid, the second dispersing agent is sodium bicarbonate, and the generated gas is as follows: carbon dioxide. (18) The first dispersing agent is citric acid, the second dispersing agent is hydrogen peroxide and sodium bicarbonate, and the generated gas is as follows: oxygen, carbon dioxide. (19) The first dispersing agent is sodium ascorbate, sodium oxalate and sodium citrate, the second dispersing agent is hydrogen peroxide, and the generated gas is as follows: oxygen. (20) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is hydrogen peroxide, and the generated gas is as follows: oxygen. (21) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is sodium percarbonate, and the generated gas is as follows: oxygen, carbon dioxide. (22) The first dispersing agent is ascorbic acid and citric acid, the second dispersing agent is hydrogen peroxide, and the generated gas is as follows: oxygen. (23) The first dispersing agent is ascorbic acid and citric acid, the second dispersing agent is sodium percarbonate, and the generated gas is as follows: oxygen, carbon dioxide. (24) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is hydrogen peroxide and sodium carbonate, and the generated gas is as follows: oxygen, carbon dioxide. (25) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is hydrogen peroxide and sodium bicarbonate, and the generated gas is as follows: oxygen, carbon dioxide. (26) The first dispersant is ascorbic acid, the second dispersant is potassium dichromate and ammonium sulfate, and the generated gas is: oxygen, nitrogen. (27) The first dispersing agent is ascorbic acid, the second dispersing agent is potassium permanganate, and the generated gas is as follows: oxygen. (28) The first dispersant is ascorbic acid, the second dispersant is potassium ferrate, and the generated gas is: oxygen. (29) The first dispersant is ascorbic acid, the second dispersant is sodium persulfate, and the generated gas is: oxygen. (30) The first dispersant is ascorbic acid, the second dispersant is potassium chlorate, and the generated gas is: oxygen. (31) The first dispersant is ascorbic acid, the second dispersant is potassium perchlorate, and the generated gas is: oxygen. (32) The first dispersant is ascorbic acid, the second dispersant is calcium hydride, and the generated gas is: hydrogen gas. (33) The first dispersant is ascorbic acid, the second dispersant is potassium dichromate, and the generated gas is: oxygen. (34) The first dispersing agent is ascorbic acid and hydrazine hydrate, the second dispersing agent is hydrogen peroxide, and the generated gas is as follows: oxygen, nitrogen. (35) The first dispersing agent is ammonia water, sodium borohydride and ascorbic acid, the second dispersing agent is hydrogen peroxide, and the generated gas is: oxygen, nitrogen. (36) The first dispersing agent is ascorbic acid, the second dispersing agent is hydrogen peroxide and potassium permanganate, and the generated gas is as follows: oxygen. (37) The first dispersant is ascorbic acid, the second dispersant is ammonium persulfate, and the generated gas is: oxygen, ammonia. (38) The first dispersing agent is ascorbic acid, the second dispersing agent is potassium manganate and hydrogen peroxide, and the generated gas is as follows: oxygen. (39) The first dispersing agent is ascorbic acid, the second dispersing agent is sodium perborate and sodium bicarbonate, and the generated gas is: oxygen, carbon dioxide. (40) The first dispersing agent is ammonia water, the second dispersing agent is hydrogen peroxide, and the generated gas is as follows: oxygen, nitrogen. (41) The first dispersing agent is ammonia water and glucose, the second dispersing agent is ascorbic acid and hydrogen peroxide, and the generated gas is: oxygen, nitrogen. (42) The first dispersing agent is ammonia water and glucose, the second dispersing agent is hydrogen peroxide, and the generated gas is as follows: oxygen, nitrogen. (43) The first dispersing agent is ammonia water and glucose, the second dispersing agent is ammonium chloride and sodium nitrite, and the generated gas is as follows: nitrogen gas. (44) The first dispersing agent is ammonia water and glucose, the second dispersing agent is ammonium bicarbonate, and the generated gas is as follows: carbon dioxide, ammonia. (45) The first dispersing agent is ammonia water and glucose, the second dispersing agent is ammonium nitrite, and the generated gas is as follows: nitrogen gas. (46) The first dispersing agent is ammonia water and hydrazine hydrate, the second dispersing agent is hydrogen peroxide, and the generated gas is as follows: oxygen, nitrogen. (47) The first dispersing agent is ammonia water and sodium borohydride, the second dispersing agent is hydrogen peroxide, and the generated gas is: oxygen, nitrogen. (48) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is aluminum, and the generated gas is as follows: hydrogen gas. (49) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is hydrogen chloride and aluminum, and the generated gas is as follows: hydrogen gas. (50) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is sodium bicarbonate and aluminum, and the generated gas is as follows: carbon dioxide, hydrogen. (51) The first dispersing agent is ammonia water and glucose, the second dispersing agent is sodium hydroxide and aluminum, and the generated gas is as follows: hydrogen gas. (52) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is sodium percarbonate, hydrogen chloride and aluminum, and the generated gas is as follows: oxygen, carbon dioxide, hydrogen. (53) The first dispersing agent is ascorbic acid and citric acid, the second dispersing agent is zinc, and the generated gas is as follows: hydrogen gas. (54) The first dispersing agent is ascorbic acid and citric acid, the second dispersing agent is hydrogen peroxide and zinc, and the generated gas is as follows: oxygen and hydrogen (55) the first dispersant is ascorbic acid, the second dispersant is hydrogen peroxide, hydrogen chloride and zinc, and the generated gases are: oxygen, hydrogen. (56) The first dispersing agent is ammonia water and glucose, the second dispersing agent is hydrogen peroxide and zinc, and the generated gas is as follows: oxygen, nitrogen, hydrogen. (57) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is sodium carbonate and zinc, and the generated gas is as follows: carbon dioxide, hydrogen. (58) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is sodium carbonate, hydrogen peroxide and zinc, and the generated gas is as follows: oxygen, carbon dioxide, hydrogen. (59) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is sodium carbonate, hydrogen chloride and zinc, and the generated gas is as follows: carbon dioxide, hydrogen. (60) The first dispersing agent is ascorbic acid, oxalic acid and zinc, the second dispersing agent is hydrogen peroxide, and the generated gas is: hydrogen and oxygen. (61) The first dispersing agent is hydroiodic acid, the second dispersing agent is hydrogen peroxide, and the generated gas is as follows: oxygen. (62) The first dispersing agent is ascorbic acid, the second dispersing agent is hydrogen chloride and sodium chlorite, and the generated gas is: chlorine dioxide. (63) The first dispersing agent is ascorbic acid, the second dispersing agent is sodium bicarbonate, sodium bisulfate, hydrogen chloride and sodium chlorite, and the generated gas is as follows: carbon dioxide, chlorine dioxide. (64) The first dispersing agent is ascorbic acid and oxalic acid, the second dispersing agent is sodium bicarbonate, hydrogen chloride and sodium chlorite, and the generated gas is as follows: carbon dioxide, chlorine dioxide. The general examples set forth above are merely illustrative of the principles of the present invention, and the experimental protocols that are actually used are not limited to those set forth above. All experiments performed in accordance with the principles of the present invention and with the various reagents exemplified herein are included within the scope of the present invention.
Preferably, the reaction in the second step can adjust relevant parameters of the second dispersant category, the second dispersant mass, the reaction time, the reaction temperature and the stirring rotation speed in the experimental process.
Preferably, the filtration and displacement in the third step is performed in one or more of the following combinations: normal pressure filtration, reduced pressure filtration, gravity filtration, vacuum filtration, centrifugal filtration, dialysis, and soaking replacement.
Preferably, the filtering and replacing in the third step are performed by using one or more of the following devices according to the length and the number of layers of the carbon nanotubes: a filter screen, a filter membrane, a filter bag and a filter paper with the mesh number of 10-5000 meshes. The usual mesh numbers are: 200 mesh, 250 mesh, 300 mesh, 350 mesh, 400 mesh, 450 mesh, 500 mesh, 550 mesh, 600 mesh, 650 mesh, 700 mesh, 750 mesh, 800 mesh, 1000 mesh.
Preferably, the filtering and replacing in the third step remove impurities in the carbon nanotube solution, wherein the impurity removal standard is that the impurity content in the carbon nanotube solution meets the requirement standard of downstream application on the impurity content in the carbon nanotube. Removed impurities include, but are not limited to: impurities generated during preparation of the carbon nanotubes, impurities introduced during purification of the carbon nanotubes, and impurities introduced during preparation of the carbon nanotube solution.
Preferably, the filtration and displacement in the third step may be performed by using only one solvent (liquid), or may be performed by using a plurality of solvents (liquids) in sequence. The carbon nanotubes uniformly dispersed in one solvent (liquid) are fully replaced by different solvents (liquid) in turn by utilizing the mutual solubility of the solvents (liquid), and uniformly dispersed in other solvents (liquid), so that the solution of the carbon nanotubes uniformly dispersed in the different solvents (liquid) is obtained in turn.
Preferably, the solvent (liquid) used for the filtration and displacement in the third step is one of the following three: an inorganic solvent (liquid), an organic solvent (liquid), and a mixed solution of the inorganic solvent (liquid) and the organic solvent (liquid).
Preferably, the inorganic solvent (liquid) used for the filtration and displacement in the third step is any one of the following: water, a solution formed by adding solute to water.
Preferably, one of the inorganic solutions used for the filtration and displacement in the third step is a solution formed by adding a solute to water, and the solute is one or more of the following: lithium chloride, sodium chloride, magnesium chloride, aluminum chloride, potassium chloride, calcium chloride, ammonium chloride, ferric chloride, ferrous chloride, nickel chloride, cobalt chloride, manganese chloride, chromium chloride, copper chloride, zinc chloride, barium chloride, tin chloride, stannous chloride, lithium fluoride, sodium fluoride, magnesium fluoride, aluminum fluoride, potassium fluoride, calcium fluoride, ammonium fluoride, ferric fluoride, ferrous fluoride, nickel fluoride, cobalt fluoride, manganese fluoride, chromium fluoride, copper fluoride, zinc fluoride, barium fluoride, tin fluoride, stannous fluoride, lithium sulfate, sodium sulfate, magnesium sulfate, aluminum sulfate, potassium sulfate, ammonium sulfate, iron sulfate, ferrous sulfate, nickel sulfate, cobalt sulfate, manganese sulfate, chromium sulfate, copper sulfate, zinc sulfate, tin sulfate, stannous sulfate, lithium nitrate, sodium nitrate, magnesium nitrate, aluminum nitrate, potassium nitrate calcium nitrate, ammonium nitrate, ferric nitrate, ferrous nitrate, nickel nitrate, cobalt nitrate, manganese nitrate, chromium nitrate, copper nitrate, barium nitrate, zinc nitrate, tin nitrate, stannous nitrate, lithium carbonate, sodium carbonate, potassium carbonate, ammonium carbonate, lithium bicarbonate, sodium bicarbonate, magnesium bicarbonate, potassium bicarbonate, calcium bicarbonate, ammonium bicarbonate, lithium acetate, sodium acetate, magnesium acetate, aluminum acetate, potassium acetate, calcium acetate, ammonium acetate, ferric acetate, ferrous acetate, nickel acetate, cobalt acetate, manganese acetate, chromium acetate, copper acetate, zinc acetate, barium acetate, tin acetate, stannous acetate, the surfactant added in the first step described in [0019], the first dispersant used in the first step described in [0021], the second dispersant used in the second step described in [0027 ].
Preferably, one of the organic solvents (liquids) used in the filtration and displacement in the third step is one or more of the following: hydrocarbon solvents (liquids), halogenated hydrocarbon solvents (liquids), alcohol solvents (liquids), phenol solvents (liquids), ether solvents (liquids), aldehyde solvents (liquids), ketone solvents (liquids), ester solvents (liquids), acid and acid anhydride solvents (liquids), amine solvents (liquids), amide solvents (liquids), and nitrilesA solvent (liquid), a nitrogen-containing compound solvent (liquid), and a sulfur-containing compound solvent (liquid). The common organic solvents (liquids) are one or more of the following mixtures: CBrF 3 、CClF 3 、CCl 2 F 2 、CCl 3 F、CCl 4 、CCl 4 S、CF 4 、CS 2 、CHBrCl 2 、CHBr 2 Cl、CHBr 3 、CHCl 2 F、CHCl 3 、CHF 3 、CHF 3 O 3 S、CH 2 ClBr、CH 2 Br 2 、CH 2 Cl 2 、CH 2 O、CH 2 O 2 、CH 3 Br、CH 3 Cl、CH 3 I、CH 3 NCO、CH 3 ON、CH 3 NO 2 、CH 4 O、CH 5 N、CH 6 ClN 3 O、CH 6 N 2 、C 2 Cl 2 F 4 、C 2 Cl 3 F 3 、C 2 Cl 4 、C 2 Cl 4 F 2 、C 2 Cl 6 、C 2 HCl 2 F 3 、C 2 HCl 2 N、C 2 HCl 3 、C 2 HO 2 Cl 3 、C 2 HCl 5 、C 2 HF 3 O 2 、C 2 H 2 Br 4 、C 2 H 2 ClF 3 、C 2 H 2 ClN、C 2 H 2 Cl 2 、C 2 H 2 Cl 2 O、C 2 H 2 O 2 Cl 2 、C 2 H 2 Cl 4 、C 2 H 2 F 2 、C 2 H 2 O 4 、C 2 H 3 Cl、C 2 H 3 ClF 2 、C 2 H 3 ClO、C 2 H 3 ClO 2 、C 2 H 3 O 2 Cl、C 2 H 3 Cl 3 、C 2 H 3 F 3 O、C 2 H 3 N、C 2 H 4 、C 2 H 4 BrCl、C 2 H 4 Br 2 、C 2 H 4 Cl 2 、C 2 H 4 Cl 2 O、C 2 H 4 F 2 、C 2 H 4 O、C 2 H 4 O 2 、C 2 H 4 O 2 S、C 2 H 4 O 3 、C 2 H 5 Br、C 2 H 5 BrO、C 2 H 5 Cl、C 2 H 5 ClO、C 2 H 5 N、C 2 H 5 ON、C 2 H 5 NO 2 、C 2 H 6 、C 2 H 6 N 2 O、C 2 H 6 O、C 2 H 6 O 2 、C 2 H 6 OS、C 2 H 6 O 2 S、C 2 H 6 O 4 S、C 2 H 6 S、C 2 H 7 N、C 2 H 7 NO、C 2 H 7 O 4 P、C 2 H 8 N 2 、C 3 Cl 2 F 4 O、C 3 F 6 O、C 3 H 3 F 3 O、C 3 H 3 N、C 3 H 4 Cl 2 、C 3 H 4 O、C 3 H 4 O 2 、C 3 H 4 O 3 、C 3 H 4 N 2 、C 3 H 5 BrO、C 3 H 5 BrO 2 、C 3 H 5 Br 2 Cl、C 3 H 5 Br 3 、C 3 H 5 Cl、C 3 H 5 OCl、C 3 H 5 ClO 2 、C 3 H 5 Cl 3 、C 3 H 5 N、C 3 H 5 NO、C 3 H 6 、C 3 H 6 Br 2 、C 3 H 6 Br 2 O、C 3 H 6 ClNO、C 3 H 6 Cl 2 、C 3 H 6 Cl 2 O、C 3 H 6 O、C 3 H 6 O 2 、C 3 H 6 O 3 、C 3 H 6 O 3 S、C 3 H 7 Br、C 3 H 7 Cl、C 3 H 7 ClO、C 3 H 7 ClO 2 、C 3 H 7 I、C 3 H 7 N、C 3 H 7 ON、C 3 H 7 NO 2 、C 3 H 7 NO 3 、C 3 H 8 、C 3 H 8 O、C 3 H 8 O 2 、C 3 H 8 O 3 、C 3 H 8 S、C 3 H 9 BO 3 、C 3 H 9 N、C 3 H 9 NO、C 3 H 9 O 4 P、C 3 H 10 N 2 、C 4 Cl 6 、C 4 F 6 O 3 、C 4 H 4 N 2 、C 4 H 4 O、C 4 H 4 S、C 4 H 5 Cl、C 4 H 5 N、C 4 H 5 NO 2 、C 4 H 6 、C 4 H 6 Cl 2 O 2 、C 4 H 6 O、C 4 H 6 O 2 、C 4 H 6 O 3 、C 4 H 6 O 4 、C 4 H 6 O 4 Pb·3H 2 O、C 4 H 7 N、C 4 H 7 NO、C 4 H 7 ClO 2 、C 4 H 8 、C 4 H 8 Cl 2 、C 4 H 8 O、C 4 H 8 OCl 2 、C 4 H 8 O 2 、C 4 H 8 O 2 S、C 4 H 8 O 3 、C 4 H 8 S、C 4 H 9 Br、C 4 H 9 Cl、C 4 H 9 ClO、C 4 H 9 I、C 4 H 9 N、C 4 H 9 NO、C 4 H 9 NO 2 、C 4 H 10 、C 4 H 10 N 2 O、C 4 H 10 O、C 4 H 10 O 2 、C 4 H 10 O 2 S、C 4 H 10 O 3 、C 4 H 10 O 4 S、C 4 H 10 S、C 4 H 11 N、C 4 H 11 NO、C 4 H 11 NO 2 、C 4 H 11 O 4 P、C 4 H 12 Si、C 4 H 13 N 3 、C 4 H 19 NO 2 、C 5 Cl 6 、C 5 H 4 O 2 、C 5 H 5 N、C 5 H 6 、C 5 H 6 O、C 5 H 6 O 2 、C 5 H 7 NO 2 、C 5 H 8 、C 5 H 8 O、C 5 H 8 O 2 、C 5 H 8 O 3 、C 5 H 9 BrO 2 、C 5 H 9 ClO 2 、C 5 H 9 N、C 5 H 9 ON、C 5 H 9 O、C 5 H 10 、C 5 H 10 Cl 2 、C 5 H 10 N 2 、C 5 H 10 O、C 5 H 10 O 2 、C 5 H 10 O 3 、C 5 H 10 O 4 、C 5 H 11 Br、C 5 H 11 Cl、C 5 H 11 I、C 5 H 11 N、C 5 H 11 NO、C 5 H 11 NO 2 、C 5 H 11 NO 3 、C 5 H 12 、C 5 H 12 N 2 、C 5 H 12 ON 2 、C 5 H 12 O、C 5 H 12 O 2 、C 5 H 12 O 3 、C 5 H 12 O 4 、C 5 H 12 S、C 5 H 13 N、C 5 H 13 NO、C 5 H 13 NO 2 、C 6 F 6 、C 6 H 2 Cl 4 、C 6 H 3 ClN 2 O 4 、C 6 H 3 Cl 3 、C 6 H 3 Cl 3 O、C 6 H 4 BrCl、C 6 H 4 Br 2 、C 6 H 4 ClNO 2 、C 6 H 4 Cl 2 、C 6 H 4 Cl 2 O、C 6 H 4 N 2 O 4 、C 6 H 5 Br、C 6 H 5 BrO、C 6 H 5 Cl、C 6 H 5 ClO、C 6 H 5 F、C 6 H 5 I、C 6 H 5 NO 2 、C 6 H 6 、C 6 H 6 ClN、C 6 H 6 O、C 6 H 6 O 2 、C 6 H 6 OS、C 6 H 6 O 3 、C 6 H 7 N、C 6 H 8 N 2 、C 6 H 8 O、C 6 H 8 O 2 、C 6 H 8 O 4 、C 6 H 10 、C 6 H 10 O、C 6 H 10 O 2 、C 6 H 10 O 3 、C 6 H 10 O 4 、C 6 H 11 N、C 6 H 11 ON、C 6 H 12 、C 6 H 12 ClO、C 6 H 12 Cl 2 O 2 、C 6 H 12 Cl 3 O 4 P、C 6 H 12 O、C 6 H 12 O 2 、C 6 H 12 O 2 S、C 6 H 12 O 3 、C 6 H 12 O 4 、C 6 H 13 Br、C 6 H 13 Cl、C 6 H 13 N、C 6 H 13 NO、C 6 H 14 、C 6 H 14 O、C 6 H 14 O 2 、C 6 H 14 O 3 、C 6 H 14 O 4 、C 6 H 14 O 6 、C 6 H 15 O 3 B、C 6 H 15 N、C 6 H 15 NO、C 6 H 15 NO 2 、C 6 H 15 NO 3 、C 6 H 15 O 4 P、C 6 H 18 NOP、C 6 H 18 N 4 、C 6 H 18 OSi 2 、C 7 H 4 Cl 3 F、C 7 H 5 Cl 3 、C 7 H 5 F 3 、C 7 H 5 N、C 7 H 5 N 3 O 6 、C 7 H 6 Cl 2 、C 7 H 6 O、C 7 H 6 O 2 、C 7 H 7 Br、C 7 H 7 BrO、C 7 H 7 Cl、C 7 H 7 NO、C 7 H 7 NO 2 、C 7 H 7 NO 3 、C 7 H 8 、C 7 H 8 O、C 7 H 8 O 2 、C 7 H 8 O 3 、C 7 H 9 N、C 7 H 10 O 3 、C 7 H 12 、C 7 H 12 O、C 7 H 12 O 2 、C 7 H 12 O 4 、C 7 H 12 O 5 、C 7 H 13 N、C 7 H 14 、C 7 H 14 O、C 7 H 14 O 2 、C 7 H 14 O 3 、C 7 H 14 O 4 、C 7 H 15 Br、C 7 H 16 、C 7 H 16 O、C 7 H 16 O 2 、C 7 H 16 O 3 、C 7 H 16 O 4 、C 7 H 17 N、C 7 H 18 N 2 、C 8 H 4 F 6 、C 8 H 6 、C 8 H 7 N、C 8 H 8 、C 8 H 8 O、C 8 H 8 O 2 、C 8 H 8 O 3 、C 8 H 9 NO、C 8 H 9 NO 3 、C 8 H 9 O、C 8 H 10 、C 8 H 10 O、C 8 H 10 O 2 、C 8 H 11 N、C 8 H 12 、C 8 H 12 O 4 、C 8 H 14 O、C 8 H 14 O 2 、C 8 H 14 O 2 N 2 、C 8 H 14 O 3 、C 8 H 14 O 4 、C 8 H 14 O 5 、C 8 H 14 O 6 、C 8 H 15 N、C 8 H 16 、C 8 H 16 O、C 8 H 16 O 2 、C 8 H 16 O 3 、C 8 H 16 O 4 、C 8 H 17 Cl、C 8 H 18 、C 8 H 18 O、C 8 H 18 O 2 、C 8 H 18 O 3 、C 8 H 18 O 4 、C 8 H 18 O 5 、C 8 H 19 N、C 8 H 19 O 3 P、C 8 H 19 O 4 P、C 8 H 20 O 4 Si、C 8 H 23 N 5 、C 8 H 24 O 4 Si 4 、C 9 H 6 N 2 O 2 、C 9 H 6 O 2 、C 9 H 7 N、C 9 H 7 NO、C 9 H 8 、C 9 H 8 O、C 9 H 9 N、C 9 H 10 、C 9 H 10 O、C 9 H 10 O 2 、C 9 H 10 O 3 、C 9 H 12 、C 9 H 12 O、C 9 H 12 O 2 、C 9 H 13 N、C 9 H 14 O、C 9 H 14 O 6 、C 9 H 16 、C 9 H 16 O、C 9 H 16 O 2 、C 9 H 16 O 4 、C 9 H 17 N、C 9 H 18 、C 9 H 18 O、C 9 H 18 O 2 、C 9 H 18 O 4 、C 9 H 20 、C 9 H 20 O、C 9 H 20 O 2 、C 9 H 20 O 3 、C 9 H 21 N、C 9 H 21 NO 3 、C 10 H 7 Br、C 10 H 7 Cl、C 10 H 8 、C 10 H 10 O、C 10 H 10 O 2 、C 10 H 10 O 4 、C 10 H 11 N、C 10 H 12 、C 10 H 12 O、C 10 H 12 O 2 、C 10 H 12 O 3 、C 10 H 13 NO、C 10 H 14 、C 10 H 14 O、C 10 H 14 NO 5 PS、C 10 H 15 N、C 10 H 16 、C 10 H 16 ClN、C 10 H 16 O、C 10 H 16 O 8 N 2 、C 10 H 18 、C 10 H 18 O、C 10 H 18 O 4 、C 10 H 19 N、C 10 H 20 、C 10 H 20 O、C 10 H 20 O 2 、C 10 H 20 O 4 、C 10 H 21 N、C 10 H 22 、C 10 H 22 O、C 10 H 22 O 2 、C 10 H 22 O 3 、C 10 H 22 O 4 、C 10 H 22 O 5 、C 10 H 22 S、C 10 H 23 N、C 10 H 23 NO、C 11 H 10 、C 11 H 12 O 2 、C 11 H 14 O、C 11 H 14 O 2 、C 11 H 14 O 3 、C 11 H 16 、C 11 H 16 O、C 11 H 17 N、C 11 H 20 、C 11 H 20 O、C 11 H 20 O 2 、C 11 H 20 O 4 、C 11 H 21 N、C 11 H 22 、C 11 H 22 O、C 11 H 22 O 2 、C 11 H 24 、C 11 H 24 O、C 12 H 10 、C 12 H 10 O、C 12 H 12 、C 12 H 14 O 4 、C 12 H 16 、C 12 H 16 O、C 12 H 16 O 2 、C 12 H 16 O 3 、C 12 H 18 、C 12 H 20 O 4 、C 12 H 20 O 7 、C 12 H 22 、C 12 H 22 O、C 12 H 22 O 4 、C 12 H 22 O 6 、C 12 H 23 N、C 12 H 24 、C 12 H 24 O、C 12 H 24 O 2 、C 12 H 25 Br、C 12 H 25 Cl、C 12 H 26 、C 12 H 26 O、C 12 H 26 O 3 、C 12 H 26 S、C 12 H 27 O 3 B、C 12 H 27 N、C 12 H 27 O 4 P、C 13 H 10 O、C 13 H 10 O 3 、C 13 H 12 、C 13 H 18 O、C 13 H 20 、C 13 H 20 O、C 13 H 22 O 2 、C 13 H 24 、C 13 H 24 O、C 13 H 25 N、C 13 H 26 、C 13 H 26 O、C 13 H 26 O 2 、C 13 H 28 、C 14 H 10 、C 14 H 12 O 2 、C 14 H 12 O 3 、C 14 H 14 、C 14 H 14 O、C 14 H 20 O、C 14 H 22 、C 14 H 23 N、C 14 H 26 、C 14 H 26 O、C 14 H 26 O 4 、C 14 H 27 N、C 14 H 28 、C 14 H 28 O、C 14 H 28 O 2 、C 14 H 30 、C 14 H 30 O、C 15 H 22 O、C 15 H 24 、C 15 H 24 O、C 15 H 27 N 3 O、C 15 H 28 、C 15 H 28 O、C 15 H 28 O 2 、C 15 H 29 N、C 15 H 30 、C 15 H 30 O、C 15 H 30 O 2 、C 15 H 32 、C 15 H 32 O、C 15 H 33 O 3 B、C 15 H 33 N、C 16 H 10 、C 16 H 22 O 4 、C 16 H 24 O、C 16 H 26 、C 16 H 27 N、C 16 H 30 、C 16 H 30 O、C 16 H 31 N、C 16 H 32 、C 16 H 32 O、C 16 H 32 O 2 、C 16 H 34 、C 16 H 34 O、C 16 H 35 N、C 16 H 35 O 4 P、C 17 H 28 、C 17 H 32 、C 17 H 33 N、C 17 H 34 、C 17 H 34 O、C 17 H 34 O 2 、C 17 H 36 、C 17 H 36 O、C 18 H 12 、C 18 H 15 O 4 P、C 18 H 18 O 5 、C 18 H 30 、C 18 H 32 O 7 、C 18 H 34 、C 18 H 34 O 2 、C 18 H 34 O 4 、C 18 H 35 N、C 18 H 36 、C 18 H 36 O、C 18 H 36 O 2 、C 18 H 37 N、C 18 H 37 NO、C 18 H 38 、C 18 H 38 O、C 18 H 39 N、C 19 H 16 、C 19 H 20 O 4 、C 19 H 32 、C 19 H 36 、C 19 H 36 O 2 、C 19 H 38 、C 19 H 38 O、C 19 H 38 O 2 、C 19 H 40 、C 20 H 32 O、C 20 H 34 、C 20 H 36 O 4 、C 20 H 38 、C 20 H 38 O 2 、C 20 H 40 、C 20 H 40 O、C 20 H 42 、C 20 H 43 N、C 21 H 21 O 4 P、C 21 H 36 、C 21 H 42 O 4 、C 21 H 44 、C 22 H 34 O 2 、C 21 H 40 、C 21 H 42 、C 22 H 42 O 2 、C 22 H 42 O 4 、C 22 H 42 、C 22 H 44 、C 22 H 44 O 2 、C 22 H 46 、C 23 H 44 、C 23 H 46 、C 23 H 46 O 2 、C 23 H 48 、C 24 H 38 O 4 、C 24 H 46 、C 24 H 48 、C 24 H 50 、C 24 H 51 O 4 P、C 25 H 48 、C 25 H 48 O 4 、C 25 H 50 、C 25 H 52 、C 26 H 42 O 4 、C 26 H 46 、C 26 H 50 、C 26 H 50 O 4 、C 26 H 52 、C 26 H 54 、C 27 H 36 O 2 、C 27 H 52 、C 27 H 54 、C 27 H 56 、C 28 H 54 、C 28 H 56 、C 28 H 58 、C 29 H 56 、C 29 H 58 、C 29 H 60 、C 30 H 54 、C 30 H 58 、C 30 H 60 、C 30 H 62 、C 57 H 104 O 9 Polyethylene glycol (commonly used molecular weight is 100-6000, commonly used is: PEG-100, PEG-200, PEG-300, PEG-400, PEG-500, PEG-600, PEG-800, PEG-1000, PEG-1500, PEG-2000, PEG-4000, PEG-6000), pine oil, turpentine, camphor oil, petroleum ether, gasoline, kerosene, solvent naphtha, liquid paraffin, diesel oil, heavy oil, aviation kerosene, lubricating oil, silicone oil, no. 6 solvent oil, no. 70 solvent oil, no. 120 solvent oil, no. 170 solvent oil, no. 200 solvent oil, no. 260 solvent oil, fusel oil, corn oil, rapeseed oil, olive oil, palm oil, cottonseed oil, peanut oil, soybean oil, coconut oil, tea seed oil, sesame oil, rice bran oil, castor oil, linseed oil, safflower oil, cotton seed oil, walnut oil, grape seed oil, pumpkin seed oil, sunflower seed oil, orange oil, perilla oil, almond oil, lemon oil, sea buckthorn oil, evening primrose oil, glass oil, sesame oil, linseed oil, camellia oil, peony seed oil, lard, tallow, shea butter, chicken oil, fish oil, whale oil, deep sea oil, deep-drum oil. According to the general rules of disclosure, there are two cases of chemical substances expressed by the above formulas: (1) A formula represents a single structure chemical; (2) Isomers of the same formula but different structures, each formula comprising all isomers of the same formula, are shown in the present specification as representing all isomers associated therewith. The mixing of the organic solvents (liquids) includes the following two cases: (1) Mixing organic solvents (liquids) of different molecular formulas with each other; (2) Organic solvent (liquid) formed by mixing isomers with the same molecular formula.
Preferably, one of the organic solvents (liquids) used for the filtration and displacement in the third step is a solution of a solute as described in [0041] added to the organic solvent (liquid), and the solute is a solute as described in [0040 ].
Preferably, the mixed solution of the inorganic solvent (liquid) and the organic solvent (liquid) used in the filtration and replacement in the third step is a mixed solution of the inorganic solvent (liquid) described in [0039] and the organic solvent (liquid) described in [0041 ]. The mass ratio of the inorganic solvent (liquid) to the organic solvent (liquid) in the mixed solution is 1 (0-100), and the common mass ratio is: 1:0, 1:0.01, 1:0.02, 1:0.03, 1:0.04, 1:0.05, 1:0.06, 1:0.07, 1:0.08, 1:0.09, 1:0.1, 1:0.15, 1:0.2, 1:0.25, 1:0.3, 1:0.35, 1:0.4, 1:0.45, 1:0.5, 1:0.55, 1:0.6, 1:0.65, 1:0.7, 1:0.75, 1:0.8, 1:0.85, 1:0.9, 1:0.95, 1:1, 1:1.1, 1:1.2, 1:1.3, 1:1.4, 1:1.5, 1:1.6, 1:1.7, 1:1.8, 1:1.9, 1:2, 1:2.2, 1:2.5, 1:1:0.8, 1:0.3, 1:2.2.2, 1:2.5, 1:2.1.2.3, 1:2.2.1.2, 1:2.1.2.5, 1:2.2.1.2.1.0.9; 1:2.8, 1:2.9, 1:3, 1:3.1, 1:3.2, 1:3.3, 1:3.4, 1:3.5, 1:3.6, 1:3.7, 1:3.8, 1:3.9, 1:4, 1:4.1, 1:4.2, 1:4.3, 1:4.4, 1:4.5, 1:4.6, 1:4.7, 1:4.8, 1:4.9, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:20, 1:25, 1:30, 1:35, 1:40, 1:45, 1:50, 1:55, 1:60, 1:65, 1:70, 1:75, 1:80, 1:85, 1:90, 1:100.
Preferably, the mixed solution of the inorganic solvent (liquid) and the organic solvent (liquid) used in the filtration and displacement in the third step further comprises a solution formed by adding a solute to the mixed solution described in [0043], wherein the solute is the solute described in [0040 ].
Preferably, the filtering and replacing in the third step further comprises uniformly dispersing the carbon nanotubes in the first solvent (liquid), and replacing with the second solvent (liquid) to obtain a solution in which the carbon nanotubes are uniformly dispersed in the second solvent (liquid). The second solvent (liquid) used for replacement is one of the following three: the mixed solution of the inorganic solvent (liquid), the organic solvent (liquid) and the organic solvent (liquid) is the solution described in [0039], [0040], [0041], [0042], [0043], [0044 ].
Preferably, in order to meet the requirement of the concentration of the carbon nanotube solution in the application, the method for preparing the carbon nanotube solution can add more solvent (liquid) into the solution or filter and remove the redundant solvent (liquid) in the solution.
Preferably, in order to meet the requirement of drying materials in application, the method for preparing the carbon nanotube solution is used for drying in a common manner to obtain the dried carbon nanotubes. Common drying modes include: air drying, natural air drying, freeze drying, vacuum drying, spray drying, microwave drying, and supercritical drying.
Preferably, the carbon nanotube solution prepared by the present invention can be used in the following fields: lithium ion batteries, sodium ion batteries, potassium ion batteries, magnesium ion batteries, solid state batteries, conductive agents, carbon nanotube paper, supercapacitors, solar cells, light transmitting coatings, flexible display devices, transparent conductive films, photodetectors, heat dissipating coatings, heat sinks, heat generating sheets, conductive coatings, conductive inks, conductive viscose, antistatic coatings, antistatic plastics, conductive rubber, conductive films, anti-corrosion coatings, metal composites, cable materials, hydrogels, aerogels, 3D printing materials, electromagnetic shielding materials, chemical sensors, biological sensors, blood sensors, gas sensors, drug carriers, medical imaging, building materials, abrasion resistant coatings, reinforced plastics, carbon nanotube tires, foaming materials, water impermeable plastics, reinforcing materials, carbon nanotube fibers, carbon nanotube brake pads, carbon composites, oil absorbing sponges, sea water desalination, sewage purification, sea water uranium extraction, sea water lithium extraction, separation membranes, ion screens, masks, catalyst carriers, hydrogen evolution catalysts, oxygen evolution catalysts.
The beneficial effects of the invention are as follows: the invention provides a method for preparing a carbon nano tube solution, which enables carbon nano tubes to be uniformly dispersed in various solvents (liquids) and can efficiently and conveniently remove various impurities in the carbon nano tubes. The solvent (liquid) for dispersing the carbon nanotubes includes various inorganic solvents (liquids), organic solvents (liquids), and mixed solutions of inorganic solvents (liquids) and organic solvents (liquids). The invention is beneficial to improving the quality of the carbon nano tube, reducing the production cost of the carbon nano tube and conveniently adjusting the concentration of the carbon nano tube solution.
Drawings
Fig. 1 is a graph comparing the dispersion of raw untreated carbon nanotubes in a solution (left) with a carbon nanotube solution prepared according to the present invention (right).
Fig. 2 is an X-ray diffraction pattern of raw untreated carbon nanotubes.
FIG. 3 is an X-ray diffraction pattern of a carbon nanotube prepared and treated according to the present invention.
FIG. 4 shows the measured values, average values and standard deviations of the concentrations of the carbon nanotube solutions prepared according to the present invention.
Fig. 5 shows the conductivity test results of the carbon nanotube solution.
FIG. 6 is a schematic diagram of the steps of the present invention.
Detailed Description
Example 1.
Taking 1 g single-walled carbon nanotubes, adding 0.1 g polyvinylpyrrolidone into 2L pure water, and stirring ultrasonically for 2 hours to form a carbon nanotube solution.
Adding 5 g ascorbic acid into the solution, uniformly mixing, standing at 15 ℃ for reaction for 24 hours, and obtaining the carbon nano tube solution subjected to chemical dispersion treatment.
100 mL of 30% perhydrogen solution was added to the above solution, and after stirring and reacting at a rotational speed of 100 r/min for 5 minutes at 15℃the solution was allowed to stand for 24 hours, to obtain a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 350 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Example 2.
Taking 2 g single-wall carbon nanotubes, adding 0.2 g polyvinylpyrrolidone into 2L pure water, and ultrasonically stirring for 2 hours to form a carbon nanotube solution.
Adding 8 g ascorbic acid into the solution, uniformly mixing, standing at 0 ℃ for reaction for 60 hours, and obtaining the carbon nano tube solution subjected to chemical dispersion treatment.
Adding 60 g sodium percarbonate into the solution, stirring at a rotating speed of 100 r/min for reaction for 5 minutes at 0 ℃, and stirring at a rotating speed of 10 r/min for reaction for 24 hours to obtain a uniformly dispersed carbon nano tube solution.
The above solution was filtered using a 300 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding ethanol into the solution for multiple times, repeatedly filtering, and replacing water with ethanol to obtain solution with carbon nanotubes uniformly dispersed in ethanol.
Example 3.
Taking 5 g multiwall carbon nanotubes, adding 0.5 g polyvinylpyrrolidone into the mixture to dissolve in 5L pure water, and stirring the mixture with ultrasound for 2 hours to form a carbon nanotube solution.
Adding 20 g ascorbic acid into the solution, uniformly mixing, and standing at 5 ℃ for reaction for 24 hours to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
200 ml of 30% perhydrogen solution and 30 g sodium carbonate are added into the solution, and after stirring and reacting for 5 minutes at a rotation speed of 100 r/min at 5 ℃, the mixture is left to stand for 20 hours, thus obtaining a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 400 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding ethanol into the solution for multiple times, repeatedly filtering, and replacing water with ethanol to obtain solution with carbon nanotubes uniformly dispersed in ethanol.
Example 4.
Adding 2 g polyvinylpyrrolidone into 20 g multiwall carbon nanotubes, dissolving in 2L pure water, and stirring with ultrasound for 2 hr to obtain carbon nanotube solution.
Adding 5 g ascorbic acid and 15 g oxalic acid into the solution, uniformly mixing, and standing at 5 ℃ for reaction for 36 hours to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
Adding 40 g sodium bicarbonate into the solution, stirring at a rotation speed of 100 r/min for reaction for 5 minutes at a temperature of 5 ℃, and standing for reaction for 16 hours to obtain a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 300 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding ethanol into the solution for multiple times, repeatedly filtering, and replacing water with ethanol to obtain solution with carbon nanotubes uniformly dispersed in ethanol.
And adding N-methyl pyrrolidone into the solution for multiple times, repeatedly filtering, and replacing ethanol with the N-methyl pyrrolidone to obtain a solution with carbon nanotubes uniformly dispersed in the N-methyl pyrrolidone.
Example 5.
Dissolving 4 g carboxylated carbon nanotubes in 2L pure water, and ultrasonically stirring for 2 hours to form a carbon nanotube solution.
Adding 20 g ascorbic acid into the solution, uniformly mixing, and standing at 5 ℃ for reaction for 32 hours to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
60 g potassium dichromate and 20 g ammonium sulfate are added into the solution, and after stirring and reacting for 5 minutes at a rotating speed of 100 r/min at 20 ℃, the solution is kept stand for 24 hours, thus obtaining a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 350 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding ethanol into the solution for multiple times, repeatedly filtering, and replacing water with ethanol to obtain solution with carbon nanotubes uniformly dispersed in ethanol.
And adding ethyl acetate into the solution for multiple times, repeatedly filtering, and replacing ethanol with ethyl acetate to obtain a solution with carbon nanotubes uniformly dispersed in the ethyl acetate.
Example 6.
Adding 0.5 g polyvinylpyrrolidone into 5 g hydroxylated carbon nanotubes, dissolving in 2L pure water, and stirring with ultrasound for 2 hr to obtain carbon nanotube solution.
Adding 30 g ascorbic acid into the solution, uniformly mixing, standing at 10 ℃ for reaction for 24 hours, and obtaining the carbon nano tube solution subjected to chemical dispersion treatment.
50 g potassium permanganate is added into the solution, stirred and reacted for 5 minutes at the rotating speed of 100 r/min at the temperature of 20 ℃, and then the mixture is stood for reaction for 24 hours, so that the uniformly dispersed carbon nano tube solution is obtained.
The above solution was filtered using a 400 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding ethanol into the solution for multiple times, repeatedly filtering, and replacing water with ethanol to obtain solution with carbon nanotubes uniformly dispersed in ethanol.
Adding gasoline into the solution for multiple times, repeatedly filtering, and replacing ethanol with gasoline to obtain solution with carbon nanotubes uniformly dispersed in the gasoline.
Example 7.
Taking 5 g carboxylated multiwall carbon nanotubes and 5 g hydroxylated multiwall carbon nanotubes, adding 1 g polyvinylpyrrolidone, dissolving in 2L pure water, and stirring with ultrasound for 2 hours to form a carbon nanotube solution.
Adding 15 g ascorbic acid and 5 g hydrazine hydrate into the solution, uniformly mixing, and standing at 10 ℃ for reaction for 24 hours to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
300 ml of 30% perhydrogen solution was added to the above solution, and after stirring and reacting at 20℃and a rotational speed of 100 r/min for 5 minutes, the solution was allowed to stand for 24 hours, thereby obtaining a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 400 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding ethanol into the solution for multiple times, repeatedly filtering, and replacing water with ethanol to obtain solution with carbon nanotubes uniformly dispersed in ethanol.
Adding methanol into the solution for multiple times, repeatedly filtering, and replacing ethanol with methanol to obtain solution with carbon nanotubes uniformly dispersed in methanol.
And adding acetone into the solution for multiple times, repeatedly filtering, and replacing methanol with acetone to obtain a solution with carbon nanotubes uniformly dispersed in the acetone.
Example 8.
Adding 0.2 g polyvinylpyrrolidone into 5 g hydroxylated multiwall carbon nanotubes, dissolving in 2L pure water, and stirring with ultrasound for 2 hr to obtain carbon nanotube solution.
And adding 25-g sodium ascorbate into the solution, uniformly mixing, and standing at 10 ℃ for reaction for 24 hours to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
200 mL of 30% perhydrogen solution was added to the above solution, and the mixture was stirred at a rotation speed of 100 r/min at 15℃for 5 minutes, followed by standing for 24 hours, to obtain a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 400 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
And adding N, N-dimethylformamide into the solution for multiple times, repeatedly filtering, and replacing water by using the N, N-dimethylformamide to obtain the solution with carbon nano tubes uniformly dispersed in the N, N-dimethylformamide.
Example 9.
Taking 1 g single-wall carbon nano tube, adding 0.05 g sodium dodecyl sulfate and 0.05 g polyvinylpyrrolidone into 2L pure water, and stirring for 2 hours by ultrasonic to form a carbon nano tube solution.
Adding 4 g ascorbic acid and 4 g oxalic acid into the solution, uniformly mixing, and standing at 0 ℃ for reaction for 28 hours to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
100 mL of 30% hydrogen peroxide solution was added to the above solution, and the mixture was stirred at a rotation speed of 100 r/min at 5℃for 5 minutes, followed by standing for 24 hours, to obtain a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 300 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
And adding N-methyl pyrrolidone into the solution for multiple times, repeatedly filtering, and replacing water by using the N-methyl pyrrolidone to obtain the solution with the carbon nano tubes uniformly dispersed in the N-methyl pyrrolidone.
Example 10.
Adding 0.5 g sodium dodecyl sulfonate into 2L pure water to obtain 2 g hydroxylated carbon nanotube and 2 g carboxylated carbon nanotube, and ultrasonic stirring for 2 hr to obtain carbon nanotube solution.
20 mL of 25% ammonia water solution and 5 g glucose were added to the above solution, and the mixture was stirred at a stirring speed of 100 r/min at 90℃for 2 hours to obtain a carbon nanotube solution subjected to chemical dispersion treatment.
400 mL of 30% perhydrogen solution was added to the above solution, and after stirring and reacting at a rotation speed of 100 r/min at 5℃for 5 minutes, the mixture was allowed to stand for 24 hours to obtain a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 300 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding ethanol into the solution for multiple times, repeatedly filtering, and replacing water with ethanol to obtain solution with carbon nanotubes uniformly dispersed in ethanol.
And (3) placing the sample into a two-carbon supercritical drying device, and replacing ethanol in the sample by utilizing two carbons to obtain the carbon nano tube composite material after the two-carbon supercritical drying.
Example 11.
Dissolving 2 g hydroxylated carbon nanotubes and 2 g carboxylated carbon nanotubes in 2L pure water, and ultrasonically stirring for 2 hours to form a carbon nanotube solution.
Adding a proper amount of ammonia water into the solution, adjusting the pH to be 11, adding 15 g glucose, and stirring at the rotation speed of 600 r/min for reaction for 2 hours at the temperature of 90 ℃ to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
13.5 g ammonium chloride and 17.25 g sodium nitrite are added into the solution, and the mixture is stirred and reacted for 4 hours at the temperature of 85 ℃ and the rotating speed of 100 r/min, so as to obtain the uniformly dispersed carbon nano tube solution.
The above solution was filtered using a 300 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding hydrogen peroxide solution into the solution for multiple times, repeatedly filtering, and replacing water by using the hydrogen peroxide solution to obtain the solution with carbon nano tubes uniformly dispersed in the hydrogen peroxide solution.
Example 12.
Taking 3 g multiwall carbon nanotubes, adding 0.05 g sodium dodecyl sulfate into 2L pure water, and stirring for 2 hours by ultrasonic to form a carbon nanotube solution.
Adding a proper amount of ammonia water into the solution, adjusting the pH to be 11, adding 5 g glucose, and stirring at the rotating speed of 120 r/min for reaction for 2 hours at the temperature of 90 ℃ to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
Adding 20 g ammonium bicarbonate and 20 g ammonium nitrite into the solution, and stirring at 90 ℃ and a rotating speed of 30 r/min for reaction for 3 hours to obtain a uniformly dispersed carbon nano tube solution.
The above solution was filtered using a 300 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding sodium chloride solution into the solution for multiple times, repeatedly filtering, and replacing water by using the sodium chloride solution to obtain the solution with carbon nanotubes uniformly dispersed in the sodium chloride solution.
Example 13.
Adding 0.5 g sodium dodecyl benzene sulfonate into 4 g carboxylated carbon nanotubes, dissolving in 2L pure water, and ultrasonically stirring for 2 hours to form a carbon nanotube solution.
Adding a proper amount of ammonia water into the solution, adjusting the pH to be 11, adding 20 g hydrazine hydrate, and stirring and reacting for 2 hours at the rotation speed of 120 r/min at the temperature of 90 ℃ to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
500 mL of 30% perhydrogen solution was added to the above solution, and the mixture was stirred at a rotation speed of 100 r/min at 20℃for 5 minutes, followed by standing for 24 hours, to obtain a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 400 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding ethanol into the solution for multiple times, repeatedly filtering, and replacing water with ethanol to obtain solution with carbon nanotubes uniformly dispersed in ethanol.
And (3) carrying out spray drying on the solution to obtain the carbon nano tube with the impurities removed.
Example 14.
Taking 3g carboxylated carbon nanotubes and 3g hydroxylated carbon nanotubes, adding 0.5 g alkylphenol ethoxylates to dissolve in 2L pure water, and stirring ultrasonically for 2 hours to form a carbon nanotube solution.
Adding 2 g ascorbic acid, 13g oxalic acid and 5 g citric acid into the solution, uniformly mixing, and standing at 10 ℃ for reaction for 32 hours to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
20 g sodium carbonate, 20 mL of 37% hydrogen chloride solution and 5 g aluminum powder are added into the solution, and after stirring and reacting for 15 minutes at the rotating speed of 100 r/min at the temperature of 20 ℃, standing and reacting for 24 hours, the uniformly dispersed carbon nano tube solution is obtained.
The above solution was filtered using a 400 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding ethanol into the solution for multiple times, repeatedly filtering, and replacing water with ethanol to obtain solution with carbon nanotubes uniformly dispersed in ethanol.
Adding chloroform into the solution for multiple times, repeatedly filtering, and replacing ethanol with chloroform to obtain solution with carbon nanotubes uniformly dispersed in chloroform.
Example 15.
And adding 5 g polyvinylpyrrolidone into 2L pure water to obtain 2 g-coated nickel carbon nanotubes, and ultrasonically stirring for 2 hours to obtain a carbon nanotube solution.
Adding 10 g hydrazine hydrate and 20 g oxalic acid into the solution, uniformly mixing, and standing at 15 ℃ for reaction for 24 hours to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
50 g sodium bicarbonate and 10 g aluminum powder are added into the solution, and the mixture is stirred and reacted for 24 hours at 15 ℃ and the rotating speed of 100 r/min, so as to obtain the uniformly dispersed carbon nano tube solution.
The above solution was filtered using a 400 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding ethanol into the solution for multiple times, repeatedly filtering, and replacing water with ethanol to obtain solution with carbon nanotubes uniformly dispersed in ethanol.
And adding dimethylbenzene into the solution for multiple times, repeatedly filtering, and replacing ethanol with dimethylbenzene to obtain a solution with carbon nanotubes uniformly dispersed in the dimethylbenzene.
Example 16.
10 g carboxylated multiwall carbon nanotubes and 3 g nickel-coated carbon nanotubes are taken, 1 g sodium dodecyl sulfate is added to be dissolved in 2L pure water, and the mixture is ultrasonically stirred for 2 hours to form a carbon nanotube solution.
Adding 10 g sodium ascorbate, 10 g citric acid and 10 g oxalic acid into the solution, uniformly mixing, and standing at 15 ℃ for reaction for 24 hours to obtain the carbon nanotube solution subjected to chemical dispersion treatment.
10 mL of 37% hydrogen chloride solution and 10 g zinc powder were added to the above solution, and after stirring and reacting at a rotational speed of 100 r/min for 5 minutes at 20 ℃, the mixture was allowed to stand for 24 hours to obtain a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 400 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Acetonitrile was added to the above solution a plurality of times, and filtration was repeated, and water was replaced with acetonitrile to obtain a solution in which carbon nanotubes were uniformly dispersed in acetonitrile.
Example 17.
Adding 0.2 g sodium dodecyl sulfate and 0.3 g polyvinylpyrrolidone into 5 g carboxylated multiwall carbon nanotubes, dissolving in 2L pure water, and stirring with ultrasound for 2 hours to form carbon nanotube solution.
Adding a proper amount of ammonia water into the solution, adjusting the pH to be 11, adding 10 g glucose, and stirring at the rotating speed of 120 r/min for reaction for 2 hours at the temperature of 90 ℃ to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
400 mL of 30% perhydrogen solution and 20 g zinc powder were added to the above solution, and after stirring and reacting at a rotational speed of 100 r/min for 5 minutes at 20 ℃, the mixture was allowed to stand for 24 hours to obtain a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 400 mesh screen to give a black viscous sample.
Adding pure water into the sample for multiple times, repeatedly filtering to remove impurities until the conductivity of the filtrate is equal to that of the pure water, and obtaining a solution in which the carbon nanotubes are uniformly dispersed in the pure water.
Adding the mixed solution of methanol and ethanol into the solution for multiple times, repeatedly filtering, and replacing water by the mixed solution of methanol and ethanol to obtain the solution with carbon nanotubes uniformly dispersed in the mixed solution of methanol and ethanol.
Example 18.
Dissolving 0.5. 0.5 g carboxylated carbon nano tube in 250 mL of N, N-dimethylformamide, and ultrasonically stirring for 2 hours to form a carbon nano tube solution.
Adding 1 g ascorbic acid and 4 g sodium borohydride into the solution, and stirring at a rotation speed of 200 r/min at 15 ℃ for reaction for 6 hours to obtain the carbon nano tube solution subjected to chemical dispersion treatment.
50 mL of 30% perhydrogen solution was added to the above solution, and the mixture was stirred at 20℃and a rotation speed of 200 r/min for 5 minutes, followed by standing for 18 hours, to obtain a uniformly dispersed carbon nanotube solution.
The above solution was filtered using a 300 mesh screen to give a black viscous sample.
Adding N, N-dimethylformamide into the solution for multiple times, repeatedly filtering, and removing impurities to obtain a solution in which the carbon nanotubes are uniformly dispersed in the N, N-dimethylformamide.
Summary of the effects of the invention.
The dispersion effect of the carbon nanotube solution prepared by the present invention is shown in fig. 1. On the left of fig. 1, the original untreated carbon nanotubes are directly dispersed in water, and it is observed that the carbon nanotubes cannot be uniformly dispersed. The right side of fig. 1 is a photograph of an aqueous solution of carbon nanotubes prepared according to the present invention, and it can be observed that the carbon nanotubes are well dispersed in water.
The effect of the invention in removing impurities from carbon nanotube composites can be characterized by X-ray diffraction patterns. Fig. 2 is an X-ray diffraction spectrum of an original untreated carbon nanotube, wherein the spectrum has 4 characteristic peaks, 2θ=25.98 degrees corresponds to a (002) crystal plane of the carbon nanotube, 2θ=44.2 degrees corresponds to a (111) crystal plane of nickel, 2θ=51.62 degrees corresponds to a (200) crystal plane of nickel, and 2θ=76.02 degrees corresponds to a (220) crystal plane of nickel. The 3 characteristic peaks of nickel are all obvious in intensity, which indicates that the carbon nano tube contains a large amount of nickel, and the nickel is derived from the catalyst used in the preparation of the carbon nano tube. Fig. 3 is an X-ray diffraction pattern of the processed carbon nanotubes according to the present invention, only characteristic peaks of the carbon nanotubes, and 3 characteristic peaks of nickel are all disappeared, illustrating that nickel in the carbon nanotubes is removed after a series of preparation processes. Similarly, the X-ray diffraction pattern has no characteristic peak of other impurities, which indicates that other impurities are removed, and the purified carbon nanotube is obtained.
The uniformity of the dispersion of the carbon nanotubes in the solution can be judged by measuring the mean value and standard deviation of the concentration. A total of 12 samples were measured, 7 samples were taken from each group, and the mean and standard deviation of the concentrations were calculated from the measured values. FIG. 4 shows the measurement result of the concentration of the carbon nanotube solution, wherein the average concentration distribution of the sample is 7.09-7.17 mg/mL, and the standard deviation is 0.066-0.111 mg/mL. In consideration of experimental errors, the standard deviation of each sample is small, the concentration is uniform, and the uniformity of dispersion in the carbon nanotube solution is good. After the second dispersing agent is added, the surface of the carbon nano tube adsorbs gas, more spaces are reserved among the tubes, and other materials are more facilitated to enter the carbon nano tube to form a composite material, so that the carbon nano tube has more application scenes in the downstream industry.
The effect of removing impurities in the carbon nanotubes can be illustrated by the conductivity of the solution, and the lower the conductivity of the solution is, the lower the impurity content is. FIG. 5 shows the conductivity of the carbon nanotube solution, the conductivity before filtration is high, and the conductivity after multiple filtration is equal to the conductivity of the solution, indicating that the impurities in the solution are removed. Removed impurities include, but are not limited to: impurities generated during preparation of the carbon nanotubes, impurities introduced during purification of the carbon nanotubes, and impurities introduced during preparation of the carbon nanotube solution.
In summary, the present invention provides a method for preparing a carbon nanotube solution, which enables carbon nanotubes to be uniformly dispersed in various solvents (solutions), and can efficiently and conveniently remove various impurities in the carbon nanotubes. Solutions for dispersing carbon nanotubes include various inorganic solvents (liquids), organic solvents (liquids), and mixed solutions composed of an inorganic solvent (liquid) and an organic solvent (liquid). The invention is beneficial to improving the quality of the carbon nano tube, reducing the production cost of the carbon nano tube and conveniently adjusting the concentration of the carbon nano tube solution.
The invention is not a matter of the known technology.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.

Claims (10)

1. A method for preparing a carbon nanotube solution, comprising the steps of:
the method comprises the steps of firstly, adding a surfactant and a first dispersing agent into a carbon nano tube to react in a solution to obtain a carbon nano tube solution subjected to chemical dispersion treatment;
Secondly, adding the solution obtained in the first step into a second dispersing agent, mixing and reacting to obtain a solution containing impurities, wherein the solution contains carbon nanotubes uniformly dispersed;
and thirdly, adding the solution obtained in the second step into a solvent (liquid), filtering and replacing to remove impurities in the carbon nanotube solution, and obtaining a solution with uniformly dispersed carbon nanotubes after removing the impurities.
2. The method of preparing a carbon nanotube solution of claim 1, wherein the surfactant in the first step is one or more of the following: polyvinylpyrrolidone, polyethylenimine, dodecyltrimethylammonium bromide, tetradecyltrimethylammonium bromide, hexadecyltrimethylammonium bromide, octadecyltrimethylammonium bromide, sodium dodecylbenzenesulfonate, sodium dodecylsulfate, sodium dodecylsulfonate, alkylphenol ethoxylates, triton x-100, polyethylene glycol, aqueous ammonia, N-diethylpropiolate, octadecylamine, gum arabic, cyclodextrin, sodium polystyrene sulfonate, lithium dodecylsulfate, silane coupling agent, polyoxyethylene lauryl ether, polysorbate, polyethylene glycol octylphenyl ether, polypyrrole, polyaniline, sodium cholate, porphyrin-like molecules, pyrene-like compounds, polypeptides, proteins, DNA, amylose, amylopectin, iodine, nonionic trinitrotoluene, perylene diimide, anthracene, phenanthrene, hexabenzol; the mass ratio of the carbon nano tube to the surfactant is 1 (0-50).
3. The method of preparing a carbon nanotube solution of claim 1, wherein the first dispersant in the first step is one or more of the following: organic acids, borohydrides, citrates, ascorbates, alcohols, saccharides, amino acids, sulfur-containing first dispersants, nitrogen-containing first dispersants, reduced plant extracts, metals, inorganic acids, bases; the mass ratio of the carbon nano tube to the first dispersing agent is 1 (1-200).
4. The method for preparing a carbon nanotube solution according to claim 1, wherein the reaction time of the chemical dispersion treatment in the first step is 0 to 120 hours, the reaction temperature is-10 to 100 ℃, and the stirring speed of the reaction is 0 to 3000 r/min.
5. The method of preparing a carbon nanotube solution of claim 1, wherein the second dispersant in the second step is one or more of the following: peroxides, superoxides, percarbonates, persulfates, permanganates and permanganates, manganates, ferrates and ferrates, chlorates and chlorates, carbonates, bicarbonates, bisulphates, ammonium salts, dichromates and bichromates, iodic acids and iodates, bromic and bromates, nitrous acids and nitrites, metals, metal hydrides, acids, bases, perborates, halogen intermetallics.
6. The method of preparing a carbon nanotube solution according to claim 1, wherein the mass ratio of the second dispersant to the initial carbon nanotubes in the second step is (1-1000): 1.
7. The method for preparing a carbon nanotube solution according to claim 1, wherein the reaction time after adding the solution obtained in the first step into the second dispersant and mixing is 1 minute to 120 hours, the reaction temperature is-10 ℃ to 100 ℃, and the reaction stirring speed is 0 to 3000 r/min.
8. The method for preparing a carbon nanotube solution according to claim 1, wherein the solvent (liquid) is added in the third step for filtration and replacement, and the solvent (liquid) used is one of the following three types: an inorganic solvent (liquid), an organic solvent (liquid), and a mixed solution of the inorganic solvent (liquid) and the organic solvent (liquid); wherein the inorganic solvent (liquid) is any one of the following: water, a solution formed by adding solute into water; wherein the organic solvent (liquid) is one or more of the following mixture: hydrocarbon solvents (liquids), halogenated hydrocarbon solvents (liquids), alcohol solvents (liquids), phenol solvents (liquids), ether solvents (liquids), aldehyde solvents (liquids), ketone solvents (liquids), ester solvents (liquids), acid and acid anhydride solvents (liquids), amine solvents (liquids), amide solvents (liquids), nitrile solvents (liquids), nitrogen-containing compound solvents (liquids), sulfur-containing compound solvents (liquids), and solutions formed by adding solutes to the above-mentioned various organic solvents (liquids); the mode of use is one or more of the following combinations: normal pressure filtration, reduced pressure filtration, gravity filtration, vacuum filtration, centrifugal filtration, dialysis and soaking replacement; the equipment used is one or more of the following combinations: a filter screen, a filter membrane, a filter bag and a filter paper with the mesh number of 10-5000 meshes.
9. The method for preparing a carbon nanotube solution according to claim 1, wherein the removing of the impurities in the carbon nanotube solution in the third step means adding a solvent (liquid) into the solution containing the impurities which is uniformly dispersed in the carbon nanotube solution for filtration and replacement until the content of the impurities in the carbon nanotube solution reaches the required standard for the content of the impurities in the carbon nanotube solution by downstream application, thereby obtaining the solution with uniformly dispersed carbon nanotubes from which the impurities are removed.
10. The method for preparing a carbon nanotube solution according to claim 1, wherein the filtering and replacing in the third step further comprises uniformly dispersing carbon nanotubes in the first solvent (liquid), filtering and replacing with the second solvent (liquid) to obtain a solution in which carbon nanotubes are uniformly dispersed in the second solvent (liquid), and filtering and replacing with one of the following solvents (liquid): an inorganic solvent (liquid), an organic solvent (liquid), and a mixed solution composed of the inorganic solvent (liquid) and the organic solution; wherein the inorganic solvent (liquid) is any one of the following: water, a solution formed by adding solute into water; wherein the organic solvent (liquid) is one or more of the following mixture: hydrocarbon solvents (liquids), halogenated hydrocarbon solvents (liquids), alcohol solvents (liquids), phenol solvents (liquids), ether solvents (liquids), aldehyde solvents (liquids), ketone solvents (liquids), ester solvents (liquids), acid and acid anhydride solvents (liquids), amine solvents (liquids), amide solvents (liquids), nitrile solvents (liquids), nitrogen-containing compound solvents (liquids), sulfur-containing compound solvents (liquids), and solutions formed by adding solutes to the above-mentioned various organic solvents (liquids).
CN202210245857.4A 2022-03-17 2022-03-17 Method for preparing carbon nano tube solution Pending CN116803900A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117410493A (en) * 2023-12-12 2024-01-16 成都方大炭炭复合材料股份有限公司 Sodium vanadium phosphate positive electrode material based on carbon nanotube dispersion stabilization process and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117410493A (en) * 2023-12-12 2024-01-16 成都方大炭炭复合材料股份有限公司 Sodium vanadium phosphate positive electrode material based on carbon nanotube dispersion stabilization process and preparation method and application thereof
CN117410493B (en) * 2023-12-12 2024-04-02 成都方大炭炭复合材料股份有限公司 Sodium vanadium phosphate positive electrode material based on carbon nanotube dispersion stabilization process and preparation method and application thereof

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