CN103225133A - Active carbon fiber and preparation method thereof - Google Patents
Active carbon fiber and preparation method thereof Download PDFInfo
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- CN103225133A CN103225133A CN2013100646692A CN201310064669A CN103225133A CN 103225133 A CN103225133 A CN 103225133A CN 2013100646692 A CN2013100646692 A CN 2013100646692A CN 201310064669 A CN201310064669 A CN 201310064669A CN 103225133 A CN103225133 A CN 103225133A
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Abstract
The invention discloses an active carbon fiber and a preparation method thereof. The method comprises the following steps: obtaining a benzoxazine solution; obtaining a mixed solution of blending polymers; obtaining a composite nanofiber; and preparing the active carbon fiber. The preparation method is simple, the kinds and the application amounts of reaction reagents required by the method are less, and the cost is low. The active carbon fiber prepared through the method has the advantages of extremely-high specific surface area, good fiber diameter and aperture uniformity, excellent mechanical performances and excellent heat stability.
Description
Technical field
The present invention relates to a kind of activated carbon fiber and preparation method thereof.
Background technology
Activated carbon fiber is with combine a kind of novel absorption material of preparation of carbon fiber and activated carbon technology, has superhigh specific surface area, little mesoporous multilevel hierarchy, the little narrowly distributing in aperture, adsorbance is big and adsorption desorption speed is fast, characteristics such as regeneration easily.Activated carbon fiber precursor raw material is generally pitch, viscose, polyacrylonitrile and phenolic resins at present, and wherein phenolic resin based activated carbon fiber is compared advantages such as having higher carbonization yield, specific area and electric conductivity and received concern widely than other activated carbon fibers.Activated carbon fiber is mainly used in the depollution of environment, how to be applied to air cleaning as good adsorbent, the hydrogen sulfide in the adsorbable coal gas and remove bad smell of perspiration, the environmental pollution that the smelly grade of cigarette makes us feeling bad; Activated carbon fiber is used for water and purifies, and can be used as water purifier, the purification of radioactive pollution and oil refinery waste water.Research as microbe carrier just begins at carbon fiber at present, and the mechanism Journal of Sex Research is demanded urgently deeply.
On the basis of powdery, granular activated charcoal material, activated carbon fiber has the specific area of uniform pore-size distribution and Geng Gao, become desirable sorbing material, therefore, be also referred to as " novel active carbon, fibrous activated carbon ", be widely used in environmental protection, Chu Qing, catalyst carrier and electrochemical field.
In recent years, the development of activated carbon fiber production technology rapidly, also has relevant application being used for aspects such as water pollution control, biochemical reaction, food fermentation as microorganism carrier, but activated carbon fiber preparation method complexity of the prior art, and the surface energy of prepared by this method activated carbon fiber is still not high, also requires further improvement; Simultaneously, the prepared activated carbon fiber intensity of this method is low, and impact resistance is relatively poor, and is not suitable for the processing of large amount of sewage.
Based on the some shortcomings of present activated carbon fiber, also not with its report of in water treatment, using as biofilm carrier.For the performance advantage with activated carbon fiber more effectively is applied in the water treatment procedure, it is imperative further to study the modified activity properties of carbon.
Summary of the invention
The invention discloses a kind of activated carbon fiber and preparation method thereof, this preparation method is simple, and needed reaction reagent kind and consumption are all less, and cost is relatively low.Have high specific area, good fibre diameter and aperture uniformity according to the activated carbon fiber of this method preparation, also have the mechanical performance and the heat endurance of excellence simultaneously.
The preparation method of activated carbon fiber of the present invention comprises the steps:
(1) at ambient temperature, benzoxazine monomer and curing catalysts with weight portion in stirred tank are dissolved in the solvent, and speed of agitator is 100-300rpm, and mixing time is 10-30min, obtains benzoxazine solution;
(2) at ambient temperature, the blending polymer is joined in the benzoxazine solution that the first step obtains, speed of agitator is 500-1200rpm, and mixing time is 3-10h, evenly mixes, and obtains the mixed solution of blending polymer;
(3) be under the condition of 30-70% in room temperature and relative humidity, the flow velocity of second mixed solution that obtain of step with 0.3-4mL/h is input on the spinning head of electrospinning device, simultaneously spinning head is connected the 10-40kV power supply and carry out electrostatic spinning and prepare the benzoxazine composite nano-fiber membrane, the distance between receiving system and the spinning head is 10-35cm;
(4) the benzoxazine composite nano-fiber membrane of gained is put into baking oven and be cured processing in air atmosphere, place potassium hydroxide solution to soak 60-180min the benzoxazine composite nano-fiber membrane after solidifying, take out the back and in vacuum drying oven, carry out drying, baking temperature is 60-120 ℃, be 30-240min drying time, obtains composite nano fiber;
(5) absolute ethyl alcohol is added round-bottomed flask; under 40 ℃ of water bath condition; add non-ionic surface active agent F127 stirring and dissolving; after treating the solution clarification; composite nano fiber is added wherein; after stirring 10min; mixed solution is poured in the culture dish that is equipped with the active carbon fiber felt of quality such as phenolic resins; naturally volatilization ethanol 8h changes culture dish over to 100 ℃ of baking ovens, thermal polymerization 24h then; the product that obtains is scraped; under the nitrogen protection condition, be fired to target temperature 700-900 ℃, keep 3h, obtain activated carbon fiber through certain heating schedule.
Described benzoxazine monomer is bisphenol-A-aniline type, bisphenol-A-2,6-difluoroaniline type, phenol-m-benzotrifluoride amine type, bisphenol AF-4-fluoroaniline type, naphthols-aniline type, phenol-aniline type, bisphenol AF-aniline type, bisphenol AF-m-benzotrifluoride amine type, naphthols-4-fluoroaniline type, phenol-2, at least a in 6-difluoroaniline type and naphthols-m-benzotrifluoride amine type.
Described curing catalysts is at least a in benzoic acid, adipic acid, oxalic acid, benzylamine and the imidazoles.
Described blending polymer is a polyacrylonitrile, nylon 6, polymethyl methacrylate, polyvinyl alcohol, polystyrene, polyvinyl chloride, Kynoar, polyvinyl butyral resin, Merlon, polyvinyl acetate, PEI, polyacrylamide, polyimides, poly(ethylene oxide), polyethylene glycol, polysulfones, polyacrylic acid, polyacrylamide, polyethylene glycol oxide, cellulose acetate, ethyl cellulose, shitosan, gelatin, zein, polyglycolic acid, PLA, polypyrrole, polyvinylpyrrolidone, polyethylene terephthalate, the mixture of one or more in polytrimethylene terephthalate and the polybutylene terephthalate (PBT).
Described cured is taked gradient increased temperature, and its temperature-rise period is: be warming up to 100～170 ℃, insulation 10～30min is warming up to 180～210 ℃, and insulation 10～30min is warming up to 240～300 ℃, insulation 30～60min.
The preparation method of activated carbon fiber of the present invention is simple, and needed reaction reagent kind and consumption are all less, and cost is relatively low.Degraded uses back activated carbon fiber elution process very simple, has still shown good catalytic degradation activity behind deionized water washing by soaking natural air drying, reuses 6 times, and degradation rate illustrates that all more than 78% its regenerability is good, can reuse.
The invention also discloses a kind of activated carbon fiber according to method for preparing.This activated carbon fiber has high specific area, good fibre diameter and aperture uniformity, has also demonstrated excellent mechanical performance and heat endurance simultaneously.In solvent recovery, air cleaning, catalyst carrier, fields such as ozone filter, water treatment, electrode material, super capacitor material, gasoline capture all are with a wide range of applications.
The specific embodiment
Below in conjunction with the embodiment of the invention technical scheme of the present invention is described in detail, but following embodiment only is in order to understanding the present invention, and can not limits the present invention, the multitude of different ways that the present invention can be defined by the claims and cover is implemented.
(1) at ambient temperature, in stirred tank, the benzoxazine monomer of 1-40 weight portion and the curing catalysts of 0.1-5 weight portion are dissolved in the solvent of 10-300 weight portion, speed of agitator is 100-300rpm, mixing time is 10-30min, and obtaining mass concentration is the benzoxazine solution of 4-35%;
(2) at ambient temperature, the blending polymer of 2-50 weight portion is joined in the benzoxazine solution that the first step obtains, and speed of agitator is 500-1200rpm, and mixing time is 3-10h, evenly mix, obtaining blending polymer quality concentration is the mixed solution of 5-35%;
(3) be under the condition of 30-70% in room temperature and relative humidity, the flow velocity of second mixed solution that obtain of step with 0.3-4mL/h is input on the spinning head of electrospinning device, simultaneously spinning head is connected the 10-40kV power supply and carry out electrostatic spinning and prepare the benzoxazine composite nano-fiber membrane, the distance between receiving system and the spinning head is 10-35cm;
(4) the benzoxazine composite nano-fiber membrane of gained is put into baking oven and be cured processing in air atmosphere, it is that the potassium hydroxide solution of 15-35% soaks 60-180min that benzoxazine composite nano-fiber membrane after solidifying is placed mass concentration, take out the back and in vacuum drying oven, carry out drying, baking temperature is 60-120 ℃, be 30-240min drying time, obtains composite nano fiber;
(5) 20 weight portion absolute ethyl alcohols are added round-bottomed flask; under 40 ℃ of water bath condition; add non-ionic surface active agent F127 stirring and dissolving; after treating the solution clarification; composite nano fiber is added wherein; after stirring 10min; mixed solution is poured in the culture dish that is equipped with the active carbon fiber felt of quality such as phenolic resins; naturally volatilization ethanol 8h changes culture dish over to 100 ℃ of baking ovens, thermal polymerization 24h then; the product that obtains is scraped; under the nitrogen protection condition, be fired to target temperature 700-900 ℃, keep 3h, obtain activated carbon fiber through certain heating schedule.
Described heating schedule is: set 20 ℃ of initial temperatures, rise to 350 ℃ and keep 5h with the speed of 1 ℃/min, the speed with 2 ℃/min rises to target temperature x ℃ again.
Embodiment 1
(1) at room temperature, in stirred tank, 1.3g bisphenol AF-aniline type benzoxazine monomer (reagent model P8423) and 0.1g benzylamine are dissolved in 25.3g N, in the dinethylformamide, speed of agitator is 100rpm, mixing time is 10min, obtains mass concentration and be 4.1% benzoxazine solution;
(2) at ambient temperature, 2.1g nylon 6 (molecular weight 70,000) is joined in the benzoxazine solution, speed of agitator is 500rpm, and mixing time is 3h, mixes, and obtains blending amount concentration and be 5.9% solution;
(3) be under 30% the condition at room temperature with relative humidity, the mixed solution that the obtains flow velocity with 0.3mL/h is input on the spinning head of electrospinning device, simultaneously spinning head being connected the 10kV power supply carries out electrostatic spinning and prepares the benzoxazine composite nano-fiber membrane, receiving system is a copper mesh, and the distance between receiving system and the spinning head is 10cm;
(4) gained benzoxazine composite nano-fiber membrane is put into baking oven and carry out the gradient increased temperature cured in air atmosphere, heating schedule is for being warming up to 100 ℃, and insulation 10min is warmed up to 180 ℃ then, keeps 10min, is warmed up to 240 ℃ at last, keeps 30min; Place the KOH solution of mass concentration 15% to soak 60min the tunica fibrosa after solidifying, take out the back and carry out drying in vacuum drying oven, vacuum is 0.1MPa, and baking temperature is 60 ℃, and be 30min drying time, obtains composite nano fiber;
(5) the 20g absolute ethyl alcohol is added round-bottomed flask, under 40 ℃ of water bath condition, add 1.0g non-ionic surface active agent F127 (sigma, EO
106PO
70EO
106) stirring and dissolving; after treating the solution clarification; add the composite nano fiber that obtains in the step 4; after stirring 10min; mixed solution is poured in the culture dish that 1.0g active carbon fiber felt (ACF has been cut into about 3cm * 6cm size) is housed; naturally ethanol 8h volatilizees; then culture dish is changed over to 100 ℃ of baking ovens; thermal polymerization 24h; the product that obtains is scraped, under the nitrogen protection condition, be fired to target temperature x ℃ (700-900 ℃), keep 3h through certain heating schedule; take out the cooling back, obtains activated carbon fiber.
Described heating schedule is: set 20 ℃ of initial temperatures, rise to 350 ℃ and keep 5h with the speed of 1 ℃/min, the speed with 2 ℃/min rises to target temperature x ℃ again.
Embodiment 2
(1) at room temperature, in stirred tank, 8.1g naphthols-aniline type benzoxazine monomer (reagent model P8417) and 1.4g imidazoles are dissolved in the 67.2g oxolane, speed of agitator is 150rpm, and mixing time is 15min, obtains mass concentration and be 12.4% benzoxazine solution;
(2) at ambient temperature, 17.3g polyacrylonitrile (molecular weight 90,000) is joined in the benzoxazine solution, speed of agitator is 600rpm, and mixing time is 5h, mixes, and obtains blending amount concentration and be 18.4% solution;
(3) be under 45% the condition at room temperature with relative humidity, the blending solution that the obtains flow velocity with 1mL/h is input on the spinning head of electrospinning device, simultaneously spinning head being connected the 18kV power supply carries out electrostatic spinning and prepares the benzoxazine composite nano-fiber membrane, receiving system is an aluminium foil, and the distance between receiving system and the spinning head is 15cm;
(4) gained benzoxazine composite nano-fiber membrane is put into baking oven and carry out the gradient increased temperature cured in air atmosphere, heating schedule is for being warming up to 130 ℃, and insulation 15min is warmed up to 180 ℃ then, keeps 15min, is warmed up to 260 ℃ at last, keeps 30min; Place the KOH solution of mass concentration 20% to soak 90min the tunica fibrosa after solidifying, take out the back and carry out drying in vacuum drying oven, vacuum is 0.1MPa, and baking temperature is 65 ℃, and be 60min drying time, obtains composite nano fiber;
(5) the 20g absolute ethyl alcohol is added round-bottomed flask, under 40 ℃ of water bath condition, add 1.0g non-ionic surface active agent F127 (sigma, EO
106PO
70EO
106) stirring and dissolving, treat solution clarification after, add composite nano fiber; after stirring 10min; mixed solution is poured in the culture dish that the 1.0g active carbon fiber felt is housed, and volatilization ethanol 8h changes culture dish over to 100 ℃ of baking ovens then naturally; thermal polymerization 24h; the product that obtains is scraped, under the nitrogen protection condition, be fired to target temperature 700-900 ℃, keep 3h through certain heating schedule; take out the cooling back, obtains activated carbon fiber.
Benzoxazine monomer can Co., Ltd buy in Sigma in the foregoing description; Blending polymer and solvent can buy in Shanghai crystalline substance pure reagent Co., Ltd; High voltage source is the DW-P303-1ACD8 type that east, Tianjin civilian high voltage source factory produces; The T100/17 type that vacuum tube furnace is produced for Henan Luoyang Sigma Instrument Manufacture Co., Ltd.; The ASAP2020 type that the pore Structure Analysis instrument is produced for U.S. Merck ﹠ Co., Inc.
The activated carbon fiber specific area that is provided by activated carbon fiber preparation method of the present invention is greater than 1000m
2/ g, because specific area is big, pore-size distribution is reasonable, adsorptivity is higher, by adopting surface modifying method provided by the present invention, make it have excellent biocompatibility, can not only be by the suction-operated purifying water body of self, and can attract microorganism species fast, form on its surface, these microorganisms are energy source with the organic pollution, by the organic pollution in the metabolism degraded water body of self.After this active-carbon fibre material biofilm CODcr and ammonia nitrogen removal frank are significantly improved.
Ecological carbon fibre composite provided by the present invention has interception function by the organic fiber looped pile of planting at skin to microorganism in the sewage and organic pollution, help activated carbon fiber absorption microorganism species and organic pollution, the ring-type looped pile self that is made of polypropylene fiber and polyster fibre simultaneously also has the biofilm effect, form microbial film on its surface, by the organic pollution in the metabolism degraded water body.
In addition, ecological carbon fibre composite provided by the present invention passes through above-mentioned activated carbon fiber as sandwich layer, and at sandwich layer arranged outside polypropylene fiber eyelet fabric to play humidification, make it when having above-mentioned advantage, have higher intensity, so sturdy and durable, be convenient to clean and maintenance, mud is received in difficult Tibetan, has reduced the replacing number of times, has prolonged service life.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.Within the spirit and principles in the present invention all, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. the preparation method of an activated carbon fiber is characterized in that, comprises the steps:
(1) at ambient temperature, benzoxazine monomer and curing catalysts with weight portion in stirred tank are dissolved in the solvent, and speed of agitator is 100-300rpm, and mixing time is 10-30min, obtains benzoxazine solution;
(2) at ambient temperature, the blending polymer is joined in the benzoxazine solution that the first step obtains, speed of agitator is 500-1200rpm, and mixing time is 3-10h, evenly mixes, and obtains the mixed solution of blending polymer;
(3) be under the condition of 30-70% in room temperature and relative humidity, the flow velocity of second mixed solution that obtain of step with 0.3-4mL/h is input on the spinning head of electrospinning device, simultaneously spinning head is connected the 10-40kV power supply and carry out electrostatic spinning and prepare the benzoxazine composite nano-fiber membrane, the distance between receiving system and the spinning head is 10-35cm;
(4) the benzoxazine composite nano-fiber membrane of gained is put into baking oven and be cured processing in air atmosphere, place potassium hydroxide solution to soak 60-180min the benzoxazine composite nano-fiber membrane after solidifying, take out the back and in vacuum drying oven, carry out drying, baking temperature is 60-120 ℃, be 30-240min drying time, obtains composite nano fiber;
(5) absolute ethyl alcohol is added round-bottomed flask; under 40 ℃ of water bath condition; add non-ionic surface active agent F127 stirring and dissolving; after treating the solution clarification; composite nano fiber is added wherein; after stirring 10min; mixed solution is poured in the culture dish that is equipped with the active carbon fiber felt of quality such as phenolic resins; naturally volatilization ethanol 8h changes culture dish over to 100 ℃ of baking ovens, thermal polymerization 24h then; the product that obtains is scraped; under the nitrogen protection condition, be fired to target temperature 700-900 ℃, keep 3h, obtain activated carbon fiber through certain heating schedule.
2. preparation method as claimed in claim 1, it is characterized in that, described benzoxazine monomer is bisphenol-A-aniline type, bisphenol-A-2,6-difluoroaniline type, phenol-m-benzotrifluoride amine type, bisphenol AF-4-fluoroaniline type, naphthols-aniline type, phenol-aniline type, bisphenol AF-aniline type, bisphenol AF-m-benzotrifluoride amine type, naphthols-4-fluoroaniline type, phenol-2, at least a in 6-difluoroaniline type and naphthols-m-benzotrifluoride amine type.
3. preparation method as claimed in claim 1 is characterized in that, described curing catalysts is at least a in benzoic acid, adipic acid, oxalic acid, benzylamine and the imidazoles.
4. preparation method as claimed in claim 1, it is characterized in that described blending polymer is a polyacrylonitrile, nylon 6, polymethyl methacrylate, polyvinyl alcohol, polystyrene, polyvinyl chloride, Kynoar, polyvinyl butyral resin, Merlon, polyvinyl acetate, PEI, polyacrylamide, polyimides, poly(ethylene oxide), polyethylene glycol, polysulfones, polyacrylic acid, polyacrylamide, polyethylene glycol oxide, cellulose acetate, ethyl cellulose, shitosan, gelatin, zein, polyglycolic acid, PLA, polypyrrole, polyvinylpyrrolidone, polyethylene terephthalate, the mixture of one or more in polytrimethylene terephthalate and the polybutylene terephthalate (PBT).
5. preparation method as claimed in claim 1 is characterized in that described cured is taked gradient increased temperature, its temperature-rise period is: be warming up to 100～170 ℃, insulation 10～30min is warming up to 180～210 ℃, insulation 10～30min is warming up to 240～300 ℃, insulation 30～60min.
6. an activated carbon fiber is characterized in that, described activated carbon fiber is according to each described preparation method's preparation in the claim 1～5.
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| CN109868528A (en) * | 2019-01-30 | 2019-06-11 | 西南大学 | A kind of one-dimensional porous carbon nanofiber material and its preparation method and application |
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Application publication date: 20130731 |