CN102677464A - Method for preparing functionalization carbon nanofiber and method for preparing functionalization carbon nanofiber film - Google Patents
Method for preparing functionalization carbon nanofiber and method for preparing functionalization carbon nanofiber film Download PDFInfo
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Abstract
The invention provides a method for preparing a functionalization carbon nanofiber. The method includes the following steps that a) a carbon nanofiber and halogenated alkylene oxide are subjected to a reaction in water to obtain an intermediate product, and b) the intermediate product and beta-cyclodextrin are subjected to a reaction in water to obtain the functionalization carbon nanofiber. A method for preparing a functionalization carbon nanofiber film is further provided. The method for preparing the functionalization carbon nanofiber film includes the following steps that the functionalization carbon nanofiber is dispersed in a solvent, and a film-forming processing is performed to obtain the functionalization carbon nanofiber film. According to the method for preparing the functionalization carbon nanofiber and the method for preparing the functionalization carbon nanofiber film, the prepared functionalization carbon nanofiber contains the beta-cyclodextrin, the beta-cyclodextrin has a good adsorption capacity to organic molecules, organic pollutants in water can be efficiently and rapidly removed, and simultaneously the functionalization carbon nanofiber film is composed of nanofibers and large in porosity, and the pores are uniform, so that the functionalization carbon nanofiber film has a large water flux.
Description
Technical field
The invention belongs to the carbon nano-fiber technical field, relate in particular to a kind of preparation method of functionalization carbon nano-fiber and the preparation method of functionalization carbon nano-fiber film.
Background technology
Carbon nano-fiber is the fibrous nano raw material of wood-charcoal material that is curled and to be formed by the multilayer graphite flake, is a kind of material with carbon element between CNT and common carbon fibers, has higher crystalline orientation degree, conduction and heat conductivility preferably.Carbon nano-fiber is except having characteristics such as low-density, high ratio modulus, high specific strength, high conduction, good heat stability; Also have advantages such as defects count is few, draw ratio is big, specific area is big, compact structure, be widely used in fields such as Aero-Space, traffic, physical culture and leisure goods, medical treatment, weaving.
Prior art discloses the preparation method of multiple carbon nano-fiber, and comparatively commonly used have chemical vapour deposition technique, method of electrostatic spinning, solid-phase synthesis and a hydrothermal carbonization method etc.Wherein, chemical vapour deposition technique is to be raw material with cheap hydrocarbon compound, makes hydrocarbon compound on metallic catalyst, carry out the method that thermal decomposition comes the synthesize nano carbon fiber at a certain temperature; Method of electrostatic spinning is to adopt the solid-phase carbon source carbon nano-fiber that spinning obtains under electrostatic field; Solid-phase synthesis is to be the method for feedstock production carbon nano-fiber with the solid-phase carbon source; The hydrothermal carbonization method is to adopt template as the method for guiding the synthesize nano carbon fiber; Like application number is that 201110077604.2 Chinese patent document at first mixes with glucose tellurium nano-wire in the aqueous solution, carries out obtaining carbon after the carburizing reagent and coats the tellurium nano-cable; Coat adding hydrochloric acid and hydrogen peroxide solution in the tellurium nano-cable to said carbon then, carry out obtaining carbon nano-fiber after the oxidation reaction.The carbon nano-fiber length that adopts this method to prepare can reach hundreds of micron, and diameter can reach 120-140nm, and pliability is good, and there are functional groups such as great amount of hydroxy group on the surface, can be assembled into the carbon nano-fiber film and is used for membrane separation technique.
Cyclodextrin (Cyclodextrin is called for short CD) is the general name of amylose a series of cyclic oligosaccharides of generation under the cyclodextrin glycosyltransferase effect that is produced by bacillus, contains 6 ~ 12 D-glucopyranose units usually.The tapered tubular structure of cyclodextrin molecular, outside a lot of chemically reactive hydroxyls that distributing, possess hydrophilic property; Inside is the hydrophobicity cavity, thereby makes it have good envelope performance, can different molecule or the ions of inclusion, form stable inclusion compound.Therefore; Cyclodextrin and derivative thereof all are widely used in a lot of fields such as medicine, food, cosmetics, amenities, new material; As be used for increasing drug solubility and dissolution rate; Improve medicine stability, prevent the drug volatilization loss, be used for being adsorbed with organic pollutants and obtain clean water etc.The inventor considers, can in carbon nano-fiber, introduce cyclodextrin molecular, thereby obtains being used for the functionalization carbon nano-fiber of sewage disposal, chiral drug separation, medicine control release etc.
Summary of the invention
In view of this; The technical problem that the present invention will solve is to provide a kind of preparation method of functionalization carbon nano-fiber and the preparation method of functionalization carbon nano-fiber film; Functionalization carbon nano-fiber film provided by the invention has bigger water flux density, and organic molecule is had the good adsorption effect.
The invention provides a kind of preparation method of functionalization carbon nano-fiber, may further comprise the steps:
A) carbon nano-fiber and haloalkylene oxide react in water, obtain intermediate product;
B) said intermediate product and beta-schardinger dextrin-react in water, obtain the functionalization carbon nano-fiber.
Preferably, said carbon nano-fiber prepares according to following method:
Tellurium nano-wire is mixed in the aqueous solution with glucose, carry out obtaining carbon coating tellurium nano-cable after the carburizing reagent;
Coat adding hydrochloric acid and hydrogen peroxide solution in the tellurium nano-cable to said carbon, carry out obtaining carbon nano-fiber after the oxidation reaction.
Preferably, the diameter of said carbon nano-fiber is 110nm ~ 150nm.
Preferably, said step a) specifically comprises:
A1) carbon nano-fiber is scattered in the water, obtains first dispersion liquid;
PH value to the 9 ~ 11 back adding haloalkylene oxide of a2) regulating said first dispersion liquid are reacted, and obtain intermediate product.
Preferably, said step a2) in, the temperature of said reaction is 40 ℃ ~ 80 ℃, and the time of said reaction is 3h ~ 12h, and said haloalkylene oxide is chloro expoxy propane or chloro oxirane.
Preferably, said step b) specifically comprises:
B1) said intermediate product is scattered in the water, obtains second dispersion liquid;
B2) in said second dispersion liquid, add beta-schardinger dextrin-, react behind adjusting pH value to 9 ~ 11, obtain the functionalization carbon nano-fiber.
Preferably, said step b2) in, the temperature of said reaction is 40 ℃ ~ 80 ℃, the time of said reaction is 3h ~ 12h.
The invention provides a kind of preparation method of functionalization carbon nano-fiber film, may further comprise the steps:
The described functionalization carbon nano-fiber of technique scheme film is scattered in the solvent, and film forming obtains functionalization carbon nano-fiber film after handling.
Preferably, said solvent is water, ethanol or acetone.
Preferably, said film forming is handled and is specially suction filtration; Perhaps, the dispersion liquid that obtains carries out drying after being applied in backing material.
Compared with prior art, the present invention at first makes carbon nano-fiber and haloalkylene oxide in water, react, and obtains the carbon nano-fiber of haloalkylene oxide functionalization; The carbon nano-fiber of said haloalkylene oxide functionalization and beta-schardinger dextrin-are given birth to reaction at water relaying supervention; Epoxy radicals on beta-schardinger dextrin-and the haloalkylene oxide reacts and finally obtains the carbon nano-fiber of beta-schardinger dextrin-functionalization; This beta-schardinger dextrin-is positioned at the carbon nano-fiber surface, makes carbon nano-fiber have the inclusion ability.The length of the functionalization carbon nano-fiber that the present invention prepares can reach hundreds of microns, and pliability is good, it is carried out film forming handle, and can obtain the self-supporting film of functionalization carbon nano-fiber.Contain beta-schardinger dextrin-in the functionalization carbon nano-fiber that the present invention prepares, it has the good adsorption ability to organic molecule, can remove the organic pollution in the water efficiently, apace; Simultaneously, said functionalization carbon nano-fiber film is made up of nanofiber, porosity more greatly and comparatively even, thereby have bigger water flux density; Functionalization carbon nano-fiber film provided by the invention also has good repeat performance.In addition, preparation method's reaction condition provided by the invention is gentle, and simple to operate easy to control, with low cost pollution-free, products distribution is even, is easy to realize industrialization.Functionalization carbon nano-fiber that the present invention prepares and functionalization carbon nano-fiber film can be used for separation, the medicine of sewage disposal, chiral drug and control fields such as release.
Description of drawings
The stereoscan photograph of the nanofiber that Fig. 1 prepares for the embodiment of the invention 1;
The stereoscan photograph of the intermediate product that Fig. 2 prepares for the embodiment of the invention 2;
The stereoscan photograph of the functionalization carbon nano-fiber that Fig. 3 prepares for the embodiment of the invention 2;
The diameter Distribution figure of the functionalization carbon nano-fiber that Fig. 4 obtains for the embodiment of the invention 2;
The infrared spectrum of the functionalization carbon nano-fiber that Fig. 5 obtains for the embodiment of the invention;
The photoelectron spectroscopy figure of the functionalization carbon nano-fiber that Fig. 6 obtains for the embodiment of the invention;
The phenolphthalein solution that Fig. 7 provides for the embodiment of the invention is handled the ultraviolet-visible light spectrogram behind the 4h;
Fig. 8 handles the ultraviolet-visible light spectrogram of the phenolphthalein solution behind the different time for the carbon nano-fiber of the beta-schardinger dextrin-functionalization that adopts the embodiment of the invention 2 preparations;
The phenolphthalein solution that Fig. 9 provides for the embodiment of the invention sees through the curve that flows through of nano fibrous membrane;
The phenolphthalein solution that Figure 10 provides for the embodiment of the invention sees through the curve that flows through of the functionalization carbon nano-fiber film that recycles;
Ultraviolet-visible light spectrogram behind the acid fuchsin solution-treated 4h that Figure 11 provides for the embodiment of the invention;
Figure 12 handles the ultraviolet-visible light spectrogram of the acid fuchsin solution behind the different time for the carbon nano-fiber of the beta-schardinger dextrin-functionalization that adopts the embodiment of the invention 2 preparations;
The functionalization carbon nano-fiber that Figure 13 provides for the embodiment of the invention is to the adsorption isothermal curve of acid fuchsin solution;
The acid fuchsin solution that Figure 14 provides for the embodiment of the invention sees through the curve that flows through of functionalization carbon nano-fiber film.
The specific embodiment
The invention provides a kind of preparation method of functionalization carbon nano-fiber, may further comprise the steps:
A) carbon nano-fiber and haloalkylene oxide react in water, obtain intermediate product;
B) said intermediate product and beta-schardinger dextrin-react in water, obtain the functionalization carbon nano-fiber.
The present invention is a raw material with carbon nano-fiber and beta-schardinger dextrin-, prepares the functionalization carbon nano-fiber that beta-schardinger dextrin-is positioned at the carbon nano-fiber surface.Contain beta-schardinger dextrin-in the said functionalization carbon nano-fiber, it has the good adsorption ability to organic molecule, can remove the organic pollution in the water efficiently, apace; Simultaneously, said functionalization carbon nano-fiber film is made up of nanofiber, porosity more greatly and comparatively even, thereby have bigger water flux density; Functionalization carbon nano-fiber film provided by the invention also has good repeat performance.In addition, preparation method's reaction condition provided by the invention is gentle, and simple to operate easy to control, with low cost pollution-free, products distribution is even, is easy to realize industrialization.
The present invention is raw material with the carbon nano-fiber, and functional groups such as great amount of hydroxy group are contained on said carbon nano-fiber surface, obtains the functionalization carbon nano-fiber thereby can react with functional group.In the present invention, said carbon nano-fiber is preferably and adopts the hydrothermal carbonization method to prepare, and more preferably adopts following method to prepare:
Tellurium nano-wire is mixed in the aqueous solution with glucose, carry out obtaining carbon coating tellurium nano-cable after the carburizing reagent;
Coat adding hydrochloric acid and hydrogen peroxide solution in the tellurium nano-cable to said carbon, carry out obtaining carbon nano-fiber after the oxidation reaction.
Said method has detailed description in application number is 201110077604.2 Chinese patent document, the present invention repeats no more at this, and those skilled in the art can be with reference to the record of above-mentioned patent documentation.
In the present invention, the diameter of said carbon nano-fiber is preferably 110nm ~ 150nm, more preferably 120nm ~ 140nm; The length of said carbon nano-fiber is preferably 10 microns ~ 1000 microns, more preferably 100 microns ~ 800 microns.
The present invention at first introduces epoxy radicals on carbon nano-fiber, even carbon nano-fiber and haloalkylene oxide react, detailed process is following:
A1) carbon nano-fiber is scattered in the water, obtains first dispersion liquid;
PH value to the 9 ~ 11 back adding haloalkylene oxide of a2) regulating said first dispersion liquid are reacted, and obtain intermediate product.
At first carbon nano-fiber is scattered in the water, forms first dispersion liquid.The present invention does not have particular restriction to said process for dispersing, and process for dispersing well known to those skilled in the art gets final product.The mass volume ratio of said carbon nano-fiber and said water does not have particular restriction yet, and carbon nano-fiber can fully, evenly disperse to get final product.
After obtaining first dispersion liquid, its pH value is adjusted to 9 ~ 11, preferably is adjusted to 9.5 ~ 10.5.The present invention preferably adopts NaOH solution to carry out the adjusting of pH value, and the mass concentration of said NaOH solution is preferably 10% ~ 50%, and more preferably 30%.
The pH value adds haloalkylene oxide after regulating and finishing in the mixed solution that obtains, haloalkylene oxide and carbon nano-fiber are reacted, and obtains intermediate product.Halogen in the haloalkylene oxide can react with the hydroxyl on carbon nano-fiber surface, thereby epoxy radicals is introduced in the carbon nano-fiber.In the present invention, said haloalkylene oxide and said carbon nano-fiber preferably react under stirring condition, more preferably under the condition of magnetic agitation, react; The temperature of said reaction is preferably 40 ℃ ~ 80 ℃, more preferably 45 ℃ ~ 75 ℃; The time of said reaction is preferably 3h ~ 12h, more preferably 5h ~ 10h.The present invention does not have particular restriction to the mass ratio of said haloalkylene oxide and said carbon nano-fiber, and for the more beta-schardinger dextrin-of introducing, haloalkylene oxide is preferably excessive.In the present invention, said haloalkylene oxide is preferably the chloro alkylene oxide, and more preferably chloro oxirane, chloro expoxy propane or chloro epoxy butane most preferably are the chloro expoxy propane.
After obtaining intermediate product,, beta-schardinger dextrin-is introduced in the carbon nano-fiber, is obtained the carbon nano-fiber of beta-schardinger dextrin-functionalization, specifically may further comprise the steps said intermediate product and beta-schardinger dextrin-hybrid reaction:
B1) said intermediate product is scattered in the water, obtains second dispersion liquid;
B2) in said second dispersion liquid, add beta-schardinger dextrin-, react behind adjusting pH value to 9 ~ 11, obtain the functionalization carbon nano-fiber.
After haloalkylene oxide and carbon nano-fiber reaction finish,, obtain second dispersion liquid with being scattered in once more in the water after the intermediate product washing that obtains.The present invention does not have particular restriction to said process for dispersing, and process for dispersing well known to those skilled in the art gets final product.The mass volume ratio of said intermediate product and said water does not have particular restriction yet, and intermediate product can fully, evenly disperse to get final product.
After obtaining second dispersion liquid,, react after then the pH value of the solution that obtains being adjusted to 9 ~ 11, can obtain the functionalization carbon nano-fiber to wherein adding beta-schardinger dextrin-.Beta-schardinger dextrin-can react with the epoxy radicals in the surperficial haloalkylene oxide of carbon nano-fiber, thereby obtains the carbon nano-fiber of beta-schardinger dextrin-functionalization.The present invention preferably adopts NaOH solution to carry out the adjusting of pH value, more preferably is adjusted to 9.5 ~ 10.5, and the mass concentration of said NaOH solution is preferably 10% ~ 50%, and more preferably 30%.In the present invention, the haloalkylene oxide on said beta-schardinger dextrin-and carbon nano-fiber surface preferably reacts under stirring condition, more preferably under the condition of magnetic agitation, reacts; The temperature of said reaction is preferably 40 ℃ ~ 80 ℃, more preferably 45 ℃ ~ 75 ℃; The time of said reaction is preferably 3h ~ 12h, more preferably 5h ~ 10h.In the present invention, the mass ratio of said beta-schardinger dextrin-and said carbon nano-fiber is preferably 0.1 ~ 100, and more preferably 0.5 ~ 70, most preferably be 1 ~ 50.
After reaction finishes, adopt water and ethanol that the product that obtains is carried out the routine washing, can obtain functionalized nano-fiber.
After obtaining functionalized nano-fiber; Respectively it is carried out scanning electron microscope analysis, infrared spectrum analysis and photoelectron spectroscopy analysis; The result shows; Adopt method provided by the invention can prepare the carbon nano-fiber of beta-schardinger dextrin-functionalization, and the even pliability of functionalization carbon nano-fiber diameter Distribution that the present invention prepares is better, can be made into the self-supporting film.
After obtaining functionalized nano-fiber, it is scattered in the solvent, carries out to obtain functionalization carbon nano-fiber film after film forming is handled.
After obtaining functionalized nano-fiber, it is scattered in the solvent according to method well known to those skilled in the art, obtains dispersion liquid.Said solvent is preferably water, ethanol or acetone, more preferably water.
After obtaining dispersion liquid, said dispersion liquid is carried out the film forming processing can obtain the functionalization carbon nano-fiber.The present invention handles said film forming does not have particular restriction, can be suction filtration well known to those skilled in the art, can carry out according to following method yet:
Said being scattered in is applied on the backing material, obtains functionalization carbon nano-fiber film after the dried.
The present invention preferably adopts simple and easy to do suction filtration method film forming, when adopting suction filtration method film forming, and the parameters such as shape, size and thickness of the functionalization carbon nano-fiber that the diameter that can be through control suction filtration device and the quality adjustment of functionalization carbon nano-fiber obtain.To this, the present invention does not have particular restriction.
After obtaining functionalization carbon nano-fiber film, it is carried out electronic microscope photos, the result shows that its porosity is bigger, and water flux is bigger;
After obtaining functionalization carbon nano-fiber film; Measure the strainability of organic substances such as itself and phenolphthalein, acid fuchsin; The result shows; Functionalization carbon nano-fiber film provided by the invention has suction-operated efficiently to phenolphthalein, can absorb the acid fuchsin molecule fast and efficiently, and has good repeat performance.Can be used for fields such as sewage disposal, chiral drug separation and medicine control release.
The present invention at first makes carbon nano-fiber and haloalkylene oxide in water, react, and obtains the carbon nano-fiber of haloalkylene oxide functionalization; The carbon nano-fiber of said haloalkylene oxide functionalization and beta-schardinger dextrin-are given birth to reaction at water relaying supervention; Epoxy radicals on beta-schardinger dextrin-and the haloalkylene oxide reacts and finally obtains the carbon nano-fiber of beta-schardinger dextrin-functionalization; This beta-schardinger dextrin-is positioned at the carbon nano-fiber surface, makes carbon nano-fiber have the inclusion ability.The length of the functionalization carbon nano-fiber that the present invention prepares can reach hundreds of microns, and pliability is good, it is carried out film forming handle, and can obtain the self-supporting film of functionalization carbon nano-fiber.Contain beta-schardinger dextrin-in the functionalization carbon nano-fiber that the present invention prepares, it has the good adsorption ability to organic molecule, can remove the organic pollution in the water efficiently, apace; Simultaneously, said functionalization carbon nano-fiber film is made up of nanofiber, porosity more greatly and comparatively even, thereby have bigger water flux density; Functionalization carbon nano-fiber film provided by the invention also has good repeat performance.In addition, preparation method's reaction condition provided by the invention is gentle, and simple to operate easy to control, with low cost pollution-free, products distribution is even, is easy to realize industrialization.
In order to further specify the present invention, the preparation method of functionalization carbon nano-fiber provided by the invention and the preparation method of functionalization carbon nano-fiber film are described in detail below in conjunction with embodiment.
Embodiment 1
In 10mL tellurium nano-wire solution, add 30mL acetone, the 6000rmp centrifugal purification obtains first mixed liquor; Under intense stirring condition, said first mixed liquor being distributed to 80mL contains in the aqueous solution of 5g glucose; 160 ℃ of following hydrothermal treatment consists; After disposing, cooling naturally is with the filter membrane filtration of 0.22 μ m; Water and washing with alcohol obtain the carbon bag tellurium nano-wire of purifying for several times until the filtrating clarification respectively;
Said carbon bag tellurium nano-wire is dispersed in the acid hydrogen peroxide solution, stirred 5 hours under the room temperature, filter, be washed till neutrality, obtain carbon nano-fiber with distilled water; Time through the control hydrothermal treatment consists, can obtain the carbon nano-fiber that diameter is 110nm, 120nm and 130nm respectively; Said carbon nano-fiber is carried out electronic microscope photos, and the result is referring to Fig. 1, the stereoscan photograph of the nanofiber that Fig. 1 prepares for the embodiment of the invention 1.
Embodiment 2
With the diameter of 10g embodiment 1 preparation is that the carbon nano-fiber of 110nm is scattered in the 100mL distilled water, forms first dispersion liquid; Using mass concentration is after 30% NaOH solution is regulated the said first dispersion liquid pH value to 10, to add excessive epoxychloropropane, under 60 ℃, magnetic agitation condition, reacts 5h, obtains intermediate product; Said intermediate product is carried out electronic microscope photos, and the result is referring to Fig. 2, the stereoscan photograph of the intermediate product that Fig. 2 prepares for the embodiment of the invention 2;
Said intermediate product is scattered in the distilled water after with distilled water wash again, forms second dispersion liquid; In said second dispersion liquid, add the 5g beta-schardinger dextrin-; Using mass concentration is after 30% NaOH solution is regulated pH value to 9; Under 60 ℃, magnetic agitation condition, react 3h,, obtain the carbon nano-fiber of beta-schardinger dextrin-functionalization with the product that distilled water and washing with alcohol obtain.
After obtaining the carbon nano-fiber of beta-schardinger dextrin-functionalization, it is carried out scanning electron microscope analysis, the result is referring to Fig. 3, the stereoscan photograph of the functionalization carbon nano-fiber that Fig. 3 prepares for the embodiment of the invention 2.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the diameter Distribution analysis; The result is referring to Fig. 4; The diameter Distribution figure of the functionalization carbon nano-fiber that Fig. 4 obtains for the embodiment of the invention 2 can be known by Fig. 4, and the functionalization carbon nano-fiber diameter Distribution that the present invention prepares is comparatively even.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out infrared analysis; The result is referring to Fig. 5; The infrared spectrum of the functionalization carbon nano-fiber that Fig. 5 obtains for the embodiment of the invention, wherein, the infrared spectrum of the intermediate product that curve a obtains for embodiment 2; The infrared spectrum of the carbon nano-fiber that curve b prepares for embodiment 1, the infrared spectrum of the carbon nano-fiber of the beta-schardinger dextrin-functionalization that curve c obtains for embodiment 2.Can know by Fig. 5, have beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the photoelectron spectroscopy analysis; The result is referring to Fig. 6; The photoelectron spectroscopy figure of the functionalization carbon nano-fiber that Fig. 6 obtains for the embodiment of the invention, wherein, the photoelectron spectroscopy figure of the functionalization carbon nano-fiber that curve a obtains for embodiment 2; The photoelectron spectroscopy figure of the carbon nano-fiber that curve b obtains for embodiment 1, curve c are the photoelectron spectroscopy figure of beta-schardinger dextrin-.Can know by Fig. 6, have beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Respectively the carbon nano-fiber of 10g embodiment 1 preparation and the carbon nano-fiber of said beta-schardinger dextrin-functionalization are scattered in the 100mL distilled water, obtain carbon nano-fiber film and functionalization carbon nano-fiber film behind the suction filtration respectively.
Be the phenolphthalein solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber and the functionalization carbon nano-fiber absorption property to phenolphthalein, the result is referring to Fig. 7 and Fig. 8, and the phenolphthalein solution that Fig. 7 provides for the embodiment of the invention is handled the ultraviolet-visible light spectrogram behind the 4h; Wherein, Curve a is the ultraviolet-visible light spectrogram of phenolphthalein solution, and curve b is for handling the ultraviolet-visible light spectrogram that obtains behind the phenolphthalein solution with the carbon nano-fiber of embodiment 1 preparation, and curve c handles the ultraviolet-visible light spectrogram that obtains behind the phenolphthalein solution with the carbon nano-fiber of the beta-schardinger dextrin-functionalization of embodiment 2 preparations; Fig. 8 handles the ultraviolet-visible light spectrogram of the phenolphthalein solution behind the different time for the carbon nano-fiber of the beta-schardinger dextrin-functionalization that adopts the embodiment of the invention 2 preparations; Wherein, curve a-g is respectively the ultraviolet-visible light spectrogram of handling phenolphthalein solution behind 0min, 2min, 5min, 15min, 90min, 4h and the 10h.Can know that by Fig. 7 and Fig. 8 the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to phenolphthalein solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber film and functionalization carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the phenolphthalein solution of 12.0mg/L, measures carbon nano-fiber film and the functionalization carbon nano-fiber film strainability to phenolphthalein, and the result is referring to Fig. 9 and Figure 10; Wherein, the phenolphthalein solution that Fig. 9 provides for the embodiment of the invention sees through the curve that flows through of nano fibrous membrane, wherein; Curve a is the curve that flows through that phenolphthalein solution sees through nano fibrous membrane, and curve b is the curve that flows through of the phenolphthalein solution carbon nano-fiber film that sees through the beta-schardinger dextrin-functionalization; The phenolphthalein solution that Figure 10 provides for the embodiment of the invention sees through the curve that flows through of the functionalization carbon nano-fiber film that recycles; Wherein curve a recycles 2 times the curve that flows through for this functionalization carbon nano-fiber film, and curve b recycles 3 times the curve that flows through for this functionalization carbon nano-fiber film.Can know that by Fig. 9 and Figure 10 functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of phenolphthalein molecule, and has the good property of can be recycled.
Be the acid fuchsin solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber, functionalization carbon nano-fiber and the functionalization carbon nano-fiber film absorption property to acid fuchsin, the result is referring to Figure 11 and Figure 12, the ultraviolet-visible light spectrogram behind the acid fuchsin solution-treated 4h that Figure 11 provides for the embodiment of the invention; Wherein, Curve a is the ultraviolet-visible light spectrogram of acid fuchsin solution, and curve b is for handling the ultraviolet-visible light spectrogram that obtains behind the acid fuchsin solution with the carbon nano-fiber of embodiment 1 preparation, and curve c handles the ultraviolet-visible light spectrogram that obtains behind the acid fuchsin solution with the carbon nano-fiber of the beta-schardinger dextrin-functionalization of embodiment 2 preparations; Figure 12 handles the ultraviolet-visible light spectrogram of the acid fuchsin solution behind the different time for the carbon nano-fiber of the beta-schardinger dextrin-functionalization that adopts the embodiment of the invention 2 preparations; Wherein, curve a-f is respectively the ultraviolet-visible light spectrogram of handling acid fuchsin solution behind 0min, 2min, 5min, 15min, 90min and the 4h.Can know that by Figure 11 and Figure 12 the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to acid fuchsin solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber film and functionalization carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the acid fuchsin solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of acid fuchsin, and the result is referring to Figure 13 and Figure 14; The functionalization carbon nano-fiber that Figure 13 provides for the embodiment of the invention is to the adsorption isothermal curve of acid fuchsin solution; Wherein, curve a is the adsorption isothermal curve of functionalization carbon nano-fiber to acid fuchsin solution, and curve b is the adsorption isothermal curve of active carbon to acid fuchsin solution; The acid fuchsin solution that Figure 14 provides for the embodiment of the invention sees through the curve that flows through of functionalization carbon nano-fiber film, and wherein curve a is for seeing through the curve that flows through of functionalization carbon nano-fiber film, and curve b is for seeing through the curve that flows through of carbon nano-fiber film.Can know that by Figure 13 and Figure 14 functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of acid fuchsin molecule, and has the good property of can be recycled.
Embodiment 3
With the diameter of 10g embodiment 1 preparation is that the carbon nano-fiber of 120nm is scattered in the 150mL distilled water, forms first dispersion liquid; Using mass concentration is after 30% NaOH solution is regulated the said first dispersion liquid pH value to 11, to add excessive epoxychloropropane, under 60 ℃, magnetic agitation condition, reacts 3h, obtains intermediate product;
Said intermediate product is scattered in the distilled water after with distilled water wash again, forms second dispersion liquid; In said second dispersion liquid, add the 50g beta-schardinger dextrin-; Using mass concentration is after 30% NaOH solution is regulated pH value to 10; Under 60 ℃, magnetic agitation condition, react 5h,, obtain the carbon nano-fiber of beta-schardinger dextrin-functionalization with the product that distilled water and washing with alcohol obtain.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the diameter Distribution analysis, and the result shows that the functionalization carbon nano-fiber diameter Distribution that the present invention prepares is comparatively even.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out infrared analysis, and the result shows, has beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the photoelectron spectroscopy analysis, and the result shows, has beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Respectively the carbon nano-fiber of 10g embodiment 1 preparation and the carbon nano-fiber of said beta-schardinger dextrin-functionalization are scattered in the 100mL distilled water, obtain carbon nano-fiber film and functionalization carbon nano-fiber film behind the suction filtration respectively.
Be the phenolphthalein solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber, functionalization carbon nano-fiber and the functionalization carbon nano-fiber film absorption property to phenolphthalein, the result shows that the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to phenolphthalein solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber film and functionalization carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the phenolphthalein solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of phenolphthalein, and the result shows; Functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of phenolphthalein molecule, and has the good property of can be recycled.
Be the acid fuchsin solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter with solution and carbon nano-fiber and functionalization carbon nano-fiber with separate; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber and the functionalization carbon nano-fiber absorption property to acid fuchsin, the result shows that the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to acid fuchsin solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber film and functionalization carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the acid fuchsin solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of acid fuchsin, and the result shows; Functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of acid fuchsin molecule, and has the good property of can be recycled.
Embodiment 4
With the diameter of 10g embodiment 1 preparation is that the carbon nano-fiber of 120nm is scattered in the 80mL distilled water, forms first dispersion liquid; Using mass concentration is after 30% NaOH solution is regulated the said first dispersion liquid pH value to 9.5, to add excessive epoxychloropropane, under 60 ℃, magnetic agitation condition, reacts 8h, obtains intermediate product;
Said intermediate product is scattered in the distilled water after with distilled water wash again, forms second dispersion liquid; In said second dispersion liquid, add the 20g beta-schardinger dextrin-; Using mass concentration is after 30% NaOH solution is regulated pH value to 10; Under 60 ℃, magnetic agitation condition, react 12h,, obtain the carbon nano-fiber of beta-schardinger dextrin-functionalization with the product that distilled water and washing with alcohol obtain.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the diameter Distribution analysis, and the result shows that the functionalization carbon nano-fiber diameter Distribution that the present invention prepares is comparatively even.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out infrared analysis, and the result shows, has beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the photoelectron spectroscopy analysis, and the result shows, has beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
The carbon nano-fiber of 10g embodiment 1 preparation and the carbon nano-fiber of said beta-schardinger dextrin-functionalization are scattered in the 100mL distilled water, obtain carbon nano-fiber film and functionalization carbon nano-fiber film behind the suction filtration respectively.
Be the phenolphthalein solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber, functionalization carbon nano-fiber and the functionalization carbon nano-fiber film absorption property to phenolphthalein, the result shows that the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to phenolphthalein solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber and functionalization carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the phenolphthalein solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of phenolphthalein, and the result shows; Functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of phenolphthalein molecule, and has the good property of can be recycled.
Be the acid fuchsin solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber, functionalization carbon nano-fiber and the functionalization carbon nano-fiber film absorption property to acid fuchsin, the result shows that the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to acid fuchsin solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber film and functionalization carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the acid fuchsin solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of acid fuchsin, and the result shows; Functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of acid fuchsin molecule, and has the good property of can be recycled.
With the diameter of 10g embodiment 1 preparation is that the carbon nano-fiber of 130nm is scattered in the 100mL distilled water, forms first dispersion liquid; Using mass concentration is after 30% NaOH solution is regulated the said first dispersion liquid pH value to 9.5, to add excessive epoxychloropropane, under 60 ℃, magnetic agitation condition, reacts 6h, obtains intermediate product;
Said intermediate product is scattered in the distilled water after with distilled water wash again, forms second dispersion liquid; In said second dispersion liquid, add the 8g beta-schardinger dextrin-; Using mass concentration is after 30% NaOH solution is regulated pH value to 11; Under 60 ℃, magnetic agitation condition, react 4h,, obtain the carbon nano-fiber of beta-schardinger dextrin-functionalization with the product that distilled water and washing with alcohol obtain.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the diameter Distribution analysis, and the result shows that the functionalization carbon nano-fiber diameter Distribution that the present invention prepares is comparatively even.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out infrared analysis, and the result shows, has beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the photoelectron spectroscopy analysis, and the result shows, has beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Carbon nano-fiber with said carbon nano-fiber of 10g and said beta-schardinger dextrin-functionalization is scattered in the 100mL distilled water respectively, obtains carbon nano-fiber film and functionalization carbon nano-fiber film behind the suction filtration respectively.
Be the phenolphthalein solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber and the functionalization carbon nano-fiber absorption property to phenolphthalein, the result shows that the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to phenolphthalein solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber and functionalization carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the phenolphthalein solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of phenolphthalein, and the result shows; Functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of phenolphthalein molecule, and has the good property of can be recycled.
Be the acid fuchsin solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber and the functionalization carbon nano-fiber absorption property to acid fuchsin, the result shows that the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to acid fuchsin solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber film and above-mentioned functions carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the acid fuchsin solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of acid fuchsin, and the result shows; Functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of acid fuchsin molecule, and has the good property of can be recycled.
Embodiment 6
With the diameter of 10g embodiment 1 preparation is that the carbon nano-fiber of 130nm is scattered in the 120mL distilled water, forms first dispersion liquid; Using mass concentration is after 30% NaOH solution is regulated the said first dispersion liquid pH value to 11, to add excessive epoxychloropropane, under 60 ℃, magnetic agitation condition, reacts 12h, obtains intermediate product;
Said intermediate product is scattered in the distilled water after with distilled water wash again, forms second dispersion liquid; In said second dispersion liquid, add the 40g beta-schardinger dextrin-; Using mass concentration is after 30% NaOH solution is regulated pH value to 9.5; Under 60 ℃, magnetic agitation condition, react 12h,, obtain the carbon nano-fiber of beta-schardinger dextrin-functionalization with the product that distilled water and washing with alcohol obtain.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the diameter Distribution analysis, and the result shows that the functionalization carbon nano-fiber diameter Distribution that the present invention prepares is comparatively even.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out infrared analysis, and the result shows, has beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the photoelectron spectroscopy analysis, and the result shows, has beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Respectively the carbon nano-fiber of 10g embodiment 1 preparation and the carbon nano-fiber of said beta-schardinger dextrin-functionalization are scattered in the 100mL distilled water, obtain carbon nano-fiber film and functionalization carbon nano-fiber film behind the suction filtration respectively.
Be the phenolphthalein solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber and the functionalization carbon nano-fiber absorption property to phenolphthalein, the result shows that the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to phenolphthalein solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber film and functionalization carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the phenolphthalein solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of phenolphthalein, and the result shows; Functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of phenolphthalein molecule, and has the good property of can be recycled.
Be the acid fuchsin solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber, functionalization carbon nano-fiber and the functionalization carbon nano-fiber film absorption property to acid fuchsin, the result shows that the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to acid fuchsin solution.
It is that 10mL, effective film area are 4.1cm that carbon nano-fiber film and above-mentioned functions carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the acid fuchsin solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of acid fuchsin, and the result shows; Functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of acid fuchsin molecule, and has the good property of can be recycled.
Embodiment 7
With the diameter of 10g embodiment 1 preparation is that the carbon nano-fiber of 110nm is scattered in the 100mL distilled water, forms first dispersion liquid; Using mass concentration is after 30% NaOH solution is regulated the said first dispersion liquid pH value to 9, to add excessive epoxychloropropane, under 60 ℃, magnetic agitation condition, reacts 3h, obtains intermediate product;
Said intermediate product is scattered in the distilled water after with distilled water wash again, forms second dispersion liquid; In said second dispersion liquid, add the 15g beta-schardinger dextrin-; Using mass concentration is after 30% NaOH solution is regulated pH value to 9; Under 60 ℃, magnetic agitation condition, react 5h,, obtain the carbon nano-fiber of beta-schardinger dextrin-functionalization with the product that distilled water and washing with alcohol obtain.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the diameter Distribution analysis, and the result shows that the functionalization carbon nano-fiber diameter Distribution that the present invention prepares is comparatively even.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out infrared analysis, and the result shows, has beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Carbon nano-fiber to said beta-schardinger dextrin-functionalization carries out the photoelectron spectroscopy analysis, and the result shows, has beta-schardinger dextrin-functional group on the carbon nano-fiber of said beta-schardinger dextrin-functionalization.
Respectively the carbon nano-fiber of 10g embodiment 1 preparation and the carbon nano-fiber of said beta-schardinger dextrin-functionalization are scattered in the 100mL distilled water, obtain carbon nano-fiber film and functionalization carbon nano-fiber film behind the suction filtration respectively.
Be the phenolphthalein solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber and the functionalization carbon nano-fiber absorption property to phenolphthalein, the result shows that the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to phenolphthalein solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber and functionalization carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the phenolphthalein solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of phenolphthalein, and the result shows; Functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of phenolphthalein molecule, and has the good property of can be recycled.
Be the acid fuchsin solution rapid mixing of 12.0mg/L with the carbon nano-fiber of 10mg embodiment 1 preparation and above-mentioned functions carbon nano-fiber and concentration respectively; After placing 15min; With millipore filter solution is separated with the functionalization carbon nano-fiber with carbon nano-fiber; Measure the uv-visible absorption spectra that separates back solution; Analyze carbon nano-fiber and the functionalization carbon nano-fiber absorption property to acid fuchsin, the result shows that the carbon nano-fiber of beta-schardinger dextrin-functionalization provided by the invention has the good adsorption function to acid fuchsin solution.
It is that 10mL, effective film area are 4.1cm that above-mentioned carbon nano-fiber film and functionalization carbon nano-fiber film are placed volume capacity
2The ultrafiltration cup (Model 8010, Millpore Co., USA) in; Adopt silicon rubber O type circle to compress film, prevent side leakage, with peristaltic pump (Model DHL-B; Shanghai Hu Xi Instr Ltd.) control concentration is the flow velocity of the acid fuchsin solution of 12.0mg/L, and measurement function carbon nano-fiber film is to the strainability of acid fuchsin, and the result shows; Functionalization carbon nano-fiber film provided by the invention is better to the adsorption capacity of acid fuchsin molecule, and has the good property of can be recycled.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (10)
1. the preparation method of a functionalization carbon nano-fiber may further comprise the steps:
A) carbon nano-fiber and haloalkylene oxide react in water, obtain intermediate product;
B) said intermediate product and beta-schardinger dextrin-react in water, obtain the functionalization carbon nano-fiber.
2. preparation method according to claim 1 is characterized in that, said carbon nano-fiber prepares according to following method:
Tellurium nano-wire is mixed in the aqueous solution with glucose, carry out obtaining carbon coating tellurium nano-cable after the carburizing reagent;
Coat adding hydrochloric acid and hydrogen peroxide solution in the tellurium nano-cable to said carbon, carry out obtaining carbon nano-fiber after the oxidation reaction.
3. preparation method according to claim 1 is characterized in that, the diameter of said carbon nano-fiber is 110nm ~ 150nm.
4. preparation method according to claim 1 is characterized in that, said step a) specifically comprises:
A1) carbon nano-fiber is scattered in the water, obtains first dispersion liquid;
PH value to the 9 ~ 11 back adding haloalkylene oxide of a2) regulating said first dispersion liquid are reacted, and obtain intermediate product.
5. preparation method according to claim 4 is characterized in that, said step a2) in, the temperature of said reaction is 40 ℃ ~ 80 ℃, and the time of said reaction is 3h ~ 12h, and said haloalkylene oxide is chloro expoxy propane or chloro oxirane.
6. preparation method according to claim 1 is characterized in that, said step b) specifically comprises:
B1) said intermediate product is scattered in the water, obtains second dispersion liquid;
B2) in said second dispersion liquid, add beta-schardinger dextrin-, react behind adjusting pH value to 9 ~ 11, obtain the functionalization carbon nano-fiber.
7. preparation method according to claim 6 is characterized in that, said step b2) in, the temperature of said reaction is 40 ℃ ~ 80 ℃, the time of said reaction is 3h ~ 12h.
8. the preparation method of a functionalization carbon nano-fiber film may further comprise the steps:
Any described functionalization carbon nano-fiber film of claim 1 ~ 7 is scattered in the solvent, and film forming obtains functionalization carbon nano-fiber film after handling.
9. preparation method according to claim 8 is characterized in that, said solvent is water, ethanol or acetone.
10. preparation method according to claim 8 is characterized in that, said film forming is handled and is specially suction filtration; Perhaps, the dispersion liquid that obtains carries out drying after being applied in backing material.
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| CN115160983B (en) * | 2022-08-12 | 2023-07-28 | 吉林化工学院 | Composite electromagnetic wave absorbing material and preparation method thereof |
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Application publication date: 20120919 |