CN103215691A - Method for preparing hollow structure carbon fibers by using cotton as raw material - Google Patents
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Abstract
The present invention relates to a method for preparing hollow structure carbon fibers by using cotton as a raw material. According to the method, cotton with no treatment is directly placed in a tubular furnace; in the protection of inert gas, temperature programming is performed to achieve a temperature of 400-1800 DEG C; carbonization is performed for 0.5-5 h at the high temperature; and after completing the reaction, cooling is performed to achieve a room temperature in the protection of inert gas to obtain the hollow structure carbon fibers. The hollow structure carbon fibers have the following characteristics that: the hollow structure carbon fibers have a hollow structure, a fiber length is about 1-5 cm, a pore size is about 3-6 mum, and the hollow structure carbon fibers have super-hydrophobic lipophilicity and high adsorption capacity. The method has characteristics of convenient operation and simple equipment, wherein the nature renewable resources are adopted as the raw materials, the preparation cost is low, the method is suitable for large-scale industrial production, and the obtained hollow structure carbon fibers can be used as an efficient adsorbent for crude oil leakage, sewage treatments, air purification and other fields.
Description
Technical field
The present invention relates to carbon fiber, being specifically related to a kind of is the method for feedstock production hollow structure carbon fiber with the cotton.
Background technology
Carbon fiber has the intensity height, density is low, (inert atmosphere is stable to 2000 ℃ for Heat stability is good, 400 ℃ of eremacausises in the air), characteristics such as chemical inertness strong (acid-fast alkali-proof), conductance height, be a kind of new material with unique mechanics, calorifics and electric property.At present, it has obtained extensive use in fields such as the energy, environmental protection and space flight.In recent years, problem of environmental pollution paid more and more attention.Marine oil spill disaster causes the heavy damage of the ecosystem, and any discharging of petrochemical industry and industrial production waste water pollutes freshwater resources, also has indoor volatile organic compounds (VOCs), such as formaldehyde, to the harm of person health.Carbon fiber can be used as adsorbent efficiently and bring into play very important effect in the depollution of environment.
The raw material of carbon fiber can divide chemical synthetic fiber and natural fabric.At present, the carbon fiber product on the market mainly is based on viscose glue base, polyacrylonitrile (PAN) base and asphaltic base three big industrial chemicals systems.Chinese patent CN102051711A and CN 102704042A disclose the preparation method of PAN base and asphalt base carbon fiber respectively.Preparation process mainly comprises the spinning and the carbonization of precursor.The former directly influences the structure and the performance of carbon fiber, and more common method is a high-voltage electrostatic spinning, as Chinese patent CN 102560889A.The latter mainly comprises steps such as pre-oxidation, low-temperature carbonization and high temperature cabonization.As seen, the preparation process of product is tediously long and complicated, and is with high costs, greatly limited the practical application of carbon fiber.The maturation though the PAN base carbon fibre possesses skills, the characteristics that output is big, its production cost is higher, and technical difficulty is big, equipment is required height, and discharge hypertoxic cyanide gas, the serious harm environment.Equally, asphalt base carbon fiber is the technology path complexity not only, and is subjected to the restriction of petroleum resources.As seen, seeking suitable natural reproducible resource, to replace industrial chemicals will be the development trend of producing carbon fiber.
Bast-fibre and bamboo fibrid are mainly adopted in the preparation of natural plants base carbon fibre.Chinese patent CN 101121512A, CN102041585A and CN102677228A disclose sponge gourd, tussah silk and the bamboo method as the feedstock production carbon fiber of using respectively.Recently, Chinese patent CN102131969A discloses and has utilized natural glycerin to be raw material, prepares the PAN fiber by chemical synthesis process, makes carbon fiber by high temperature cabonization.But the natural plants base carbon fibre does not form industrially scalable as yet at present, and its possible cause is that the quality of natural precursor is lower, the process route complexity, and production cost is higher.
Hollow carbon fiber has shown more excellent performance with its particular structure aspect the depollution of environment.Compare with traditional solid construction carbon fiber, the hollow structure carbon fiber has higher specific area and lower density, is particularly suitable for adsorbing the crude oil that floats on the sea.Compare with CNT (carbon nano-tube), wide-aperture carbon fiber (micron order) can adsorb crude oil quickly, is more prone to reclaim crude oil by fashion of extrusion.At present, the hollow structure carbon fiber mainly uses the chemicals raw material to make, as Chinese patent CN 1746346A, and CN 101768791A and CN 101805943A.The poisonous fume and the harmful waste water that produce in the industrial production cause serious harm to environment.Therefore, the technology of preparing of the hollow structure carbon fiber of economical and practical, the safety and environmental protection of exploitation one cover is for realizing that China's sustainable economic development have its own strategic significance.
Cotton is a kind of fibrous natural organic matter, and its main chemical compositions is cellulose (C
6H
10O
5)
n, a small amount of waxy substance is contained on the surface.The dried cotton fiber of normal mature can be rolled up into hollow banded structure, and its cross section is oblate or oval shape, and there is cavity the centre.Therefore, cotton is particularly suitable for preparing the carbon fiber of hollow structure.The Cotton in China aboundresources, price is relatively cheap.Statistics shows about 7,000,000 tons of China's cotton annual production in 2011, and it is about 30% to account for world's cotton total amount, occupies the first in the world.Cotton had vast market prospect as feedstock production hollow structure carbon fiber, especially fields such as crude oil leakage, sewage disposal and air cleaning.
The invention discloses a kind of is the method for feedstock production hollow structure carbon fiber with the cotton, and prepared material has super-hydrophobic lipophile and than high absorption capacity.
Summary of the invention
The present invention is directed to above-mentioned existing in prior technology weak point, aim to provide a kind of easy to operately, equipment is simple, and preparation cost is cheap, and suitable heavy industrialization prepares the method for hollow structure carbon fiber.
The present invention adopts the natural reproducible resource cotton as raw material, and under inert gas shielding, high temperature cabonization is handled and made carbon fiber.The carbon fiber essential characteristic that this method is made is: hollow structure, fibre length approximately are 1～5cm, and the aperture approximately is 3～6 μ m, have super-hydrophobic lipophile and than high absorption capacity.
Concrete preparation method is as follows:
To directly be positioned over without the cotton raw material of any processing in the tube furnace, under inert gas shielding, gas flow rate is 1～50mL/ minute, adopts 1～10 ℃/minute of heating rate, and carbonization is 0.5～5 hour under 400～1800 ℃ of high temperature.Reaction finishes the back and be cooled to room temperature under inert gas shielding, can make the hollow structure carbon fiber.
Described inert gas is one or several in the following inert gas: nitrogen, helium or argon gas.
The present invention compared with prior art has following advantage:
(1) this preparation method is easy to operate, and equipment is simple, and preparation cost is cheap, is fit to large-scale industrial production.
(2) to adopt the natural reproducible resource cotton be raw material to this preparation method, need not to relate to any poisonous, harmful industrial chemicals, has characteristics such as economy, safety and environmental protection.
(3) carbon fiber that makes of this preparation method is a hollow structure, has super-hydrophobic lipophile and than high absorption capacity.Can be used as good adsorbent and be used for fields such as crude oil leakage, sewage disposal and air cleaning.
Description of drawings
Fig. 1 is the field emission scanning electron microscope figure (multiplication factor * 90, * 2000) of the hollow structure carbon fiber that makes of the embodiment of the invention 1.
Fig. 2 is contact angle test result figure (the left figure: water droplet, right figure: oil droplet) of the hollow structure carbon fiber that makes of the embodiment of the invention 1.
Fig. 3 is the embodiment of the invention 1,2, the XRD spectra of 3, the 4 hollow structure carbon fibers that make.
Fig. 4 is the embodiment of the invention 1,2, and 3, the 4 hollow structure carbon fibers that make are to the absorption property figure of peanut oil, ethylene glycol, toluene, ethanol, the tert-butyl alcohol, glycerine.
Fig. 5 is the field emission scanning electron microscope figure (multiplication factor * 90, * 2000) of the hollow structure carbon fiber that makes of the embodiment of the invention 2.
Fig. 6 is the field emission scanning electron microscope figure (multiplication factor * 9000) of the hollow structure carbon fiber that makes of the embodiment of the invention 2.
Fig. 7 is the field emission scanning electron microscope figure (multiplication factor * 90, * 2000) of the hollow structure carbon fiber that makes of the embodiment of the invention 3.
Fig. 8 is the field emission scanning electron microscope figure (multiplication factor * 5000) of the hollow structure carbon fiber that makes of the embodiment of the invention 3.
Fig. 9 is the field emission scanning electron microscope figure (multiplication factor * 90, * 2000) of the hollow structure carbon fiber that makes of the embodiment of the invention 4.
Figure 10 is the field emission scanning electron microscope figure (multiplication factor * 5000) of the hollow structure carbon fiber that makes of the embodiment of the invention 4.
The specific embodiment
Following examples will be further described content of the present invention in conjunction with the accompanying drawings, but be not to be any type of restriction.
Embodiment 1
To directly be positioned over without the cotton raw material of any processing in the tube furnace, under nitrogen protection, gas flow rate is 1mL/ minute, adopts 2 ℃/minute of heating rates, and carbonization is 1 hour under 400 ℃ of high temperature.Reaction finishes the back and be cooled to room temperature under nitrogen protection, can make the hollow structure carbon fiber.As seen from Figure 1, the carbon fiber structural that cotton makes after through 400 ℃ of carbonization treatment is complete, and fibre length approximately is 1～5cm.As seen from Figure 2, water droplet is in contact angle＞150 that carbon fiber surface forms °, and oil droplet is absorbed fully on its surface.Therefore, the carbon fiber that makes has super-hydrophobic lipophile.As seen from Figure 3,400 ℃ of following prepared fibrous materials (CCFs-400) mainly are made up of non-type carbon and graphite grains.As seen from Figure 4, the carbon fiber that makes is respectively the adsorption capacity of peanut oil, ethylene glycol, toluene, ethanol, the tert-butyl alcohol, glycerine: 57.1 ± 1.6g/g, 67.4 ± 4.2g/g, 37.1 ± 1.0g/g, 41.7 ± 2.0g/g, 32.7 ± 0.4g/g, 101.0 ± 2.3g/g is far superior to the raw material cotton.
Embodiment 2
To directly be positioned over without the cotton raw material of any processing in the tube furnace, under nitrogen protection, gas flow rate is 1mL/ minute, adopts 2 ℃/minute of heating rates, and carbonization is 1 hour under 600 ℃ of high temperature.Reaction finishes the back and be cooled to room temperature under nitrogen protection, can make the hollow structure carbon fiber.As seen from Figure 5, the carbon fiber that makes after through 600 ℃ of carbonization treatment of cotton structural integrity still.As seen from Figure 6, carbon fiber has hollow structure, and the aperture approximately is 4.6 μ m.This novel structure can improve the absorption property of carbon fiber greatly, and conveniently adsorbed material is reclaimed from micropore.As seen from Figure 3,600 ℃ of following prepared fibrous materials (CCFs-600) mainly are made up of non-type carbon and graphite grains.As seen from Figure 4, the carbon fiber that makes is respectively the adsorption capacity of peanut oil, ethylene glycol, toluene, ethanol, the tert-butyl alcohol, glycerine: 44.7 ± 2.4g/g, 53.5 ± 0.8g/g, 31.7 ± 1.5g/g, 35.4 ± 1.4g/g, 29.8 ± 0.7g/g, 97.1 ± 1.5g/g, be far superior to the raw material cotton, but be inferior to 400 ℃ of prepared carbon fibre materials down slightly.
Embodiment 3
To directly be positioned over without the cotton raw material of any processing in the tube furnace, under nitrogen protection, gas flow rate is 2mL/ minute, adopts 2 ℃/minute of heating rates, and carbonization is 1 hour under 800 ℃ of high temperature.Reaction finishes the back and be cooled to room temperature under nitrogen protection, can make the hollow structure carbon fiber.As seen from Figure 7, the carbon fiber that makes after through 800 ℃ of carbonization treatment of cotton structural integrity still.As seen from Figure 8, carbon fiber has hollow structure, and the aperture approximately is 3.8 μ m.As seen from Figure 3,800 ℃ of following prepared fibrous materials (CCFs-800) mainly are made up of non-type carbon and graphite grains, and ° peak of locating is high-visible in 2 θ=44.36, illustrate that the content of graphite is increasing.As seen from Figure 4, the carbon fiber that makes is respectively the adsorption capacity of peanut oil, ethylene glycol, toluene, ethanol, the tert-butyl alcohol, glycerine: 42.9 ± 1.8g/g, 46.1 ± 0.9g/g, 28.1 ± 1.0g/g, 27.3 ± 0.6g/g, 30.5 ± 0.6g/g, 94.7 ± 2.4g/g, be far superior to the raw material cotton, but be inferior to prepared carbon fibre material under 400 ℃ and 600 ℃ slightly.
Embodiment 4
To directly be positioned over without the cotton raw material of any processing in the tube furnace, under nitrogen protection, gas flow rate is 5mL/ minute, adopts 2 ℃/minute of heating rates, and carbonization is 1 hour under 1000 ℃ of high temperature.Reaction finishes the back and be cooled to room temperature under nitrogen protection, can make the hollow structure carbon fiber.As seen from Figure 9, the carbon fiber that makes after through 1000 ℃ of carbonization treatment of cotton structural integrity still.As seen from Figure 10, carbon fiber has hollow structure, and the aperture approximately is 5.7 μ m.As seen from Figure 3, prepared fibrous material (CCFs-1000) mainly is made up of non-type carbon and graphite grains under 1000 ℃, ° peak of locating is high-visible in 2 θ=44.36, and peak increase to some extent by force, and the content that graphite is described is to raise with temperature to increase.As seen from Figure 4, the carbon fiber that makes is respectively the adsorption capacity of peanut oil, ethylene glycol, toluene, ethanol, the tert-butyl alcohol, glycerine: 44.3 ± 0.8g/g, 42.0 ± 0.8g/g, 28.9 ± 0.4g/g, 26.4 ± 0.4g/g, 30.4 ± 0.6g/g, 88.6 ± 1.2g/g, be far superior to the raw material cotton, but be inferior to prepared carbon fibre material under 400 ℃, 600 ℃ and 800 ℃ slightly.
Embodiment 5
To directly be positioned over without the cotton raw material of any processing in the tube furnace, under argon shield, gas flow rate is 5mL/ minute, adopts 3 ℃/minute of heating rates, and carbonization is 2 hours under 1200 ℃ of high temperature.Reaction finishes the back and be cooled to room temperature under argon shield, can make the hollow structure carbon fiber.
Embodiment 6
To directly be positioned over without the cotton raw material of any processing in the tube furnace, under the helium protection, gas flow rate is 2mL/ minute, adopts 5 ℃/minute of heating rates, and carbonization is 0.5 hour under 1600 ℃ of high temperature.Reaction finishes the back and be cooled to room temperature under the helium protection, can make the hollow structure carbon fiber.
Claims (7)
1. one kind is the method for feedstock production hollow structure carbon fiber with the cotton; it is characterized in that: be raw material with the cotton; directly be positioned over raw material in the tube furnace; under inert gas shielding; gas flow rate is 1～50mL/ minute; adopt 1～10 ℃/minute of heating rate, carbonization is 0.5～5 hour under 400～1800 ℃ of high temperature.Reaction finishes the back and be cooled to room temperature under inert gas shielding, can make the hollow structure carbon fiber.
2. according to claim 1 a kind of be the method for feedstock production hollow structure carbon fiber with the cotton, it is characterized in that described raw material is a cotton.
3. according to claim 1 a kind of be the method for feedstock production hollow structure carbon fiber with the cotton, it is characterized in that described inert gas is one or several in the following inert gas: nitrogen, helium or argon gas.
4. according to claim 1 a kind of be the method for feedstock production hollow structure carbon fiber with the cotton, it is characterized in that described gas flow rate is 1～50mL/ minute.
5. according to claim 1 a kind of be the method for feedstock production hollow structure carbon fiber with the cotton, it is characterized in that described heating rate is 1～10 ℃/minute.
6. according to claim 1 a kind of be the method for feedstock production hollow structure carbon fiber with the cotton, it is characterized in that described carburizing temperature is 400～1800 ℃.
7. according to claim 1 a kind of be the method for feedstock production hollow structure carbon fiber with the cotton, it is characterized in that described carbonization time is 1～5 hour.
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| CN103253649A (en) * | 2013-04-19 | 2013-08-21 | 东南大学 | Preparation method and application of carbon sponge |
| CN104071770A (en) * | 2014-07-06 | 2014-10-01 | 太原理工大学 | Method for preparing porous functional carbon fiber cluster from waste cotton textiles |
| CN104099688A (en) * | 2014-07-15 | 2014-10-15 | 李文军 | Cotton activated carbon fiber and production method thereof |
| CN104525117A (en) * | 2014-12-31 | 2015-04-22 | 中国地质大学（武汉） | Preparation method and usage of carbon-based epsilon-MnO2 high-efficiency arsenic adsorption material |
| CN106252616A (en) * | 2016-07-30 | 2016-12-21 | 复旦大学 | A kind of nickelous selenide/hollow carbon fiber composite and preparation method thereof |
| CN107190367A (en) * | 2017-06-30 | 2017-09-22 | 天津工业大学 | The preparation method of nitrogen sulphur codope porous carbon fiber |
| CN107190366A (en) * | 2017-06-30 | 2017-09-22 | 天津工业大学 | The preparation method of ultracapacitor N doping porous carbon fiber |
| CN108648922A (en) * | 2018-04-23 | 2018-10-12 | 中国石油大学(华东) | The preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material |
| CN109473291A (en) * | 2018-11-09 | 2019-03-15 | 天津工业大学 | A kind of N of the superelevation specific capacitance based on cotton, the novel preparation method of P codope Porous hollow Carbon fibe |
| CN110146554A (en) * | 2019-05-28 | 2019-08-20 | 新疆大学 | A kind of method of cotton carbonizatin method preparation high-performance gas sensor |
| CN112210397A (en) * | 2020-09-27 | 2021-01-12 | 长江大学 | Carbon fiber/nano silicon dioxide compound and preparation method and application thereof |
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- 2012-12-15 CN CN 201210571359 patent/CN103215691A/en active Pending
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| CN103253649A (en) * | 2013-04-19 | 2013-08-21 | 东南大学 | Preparation method and application of carbon sponge |
| CN104071770A (en) * | 2014-07-06 | 2014-10-01 | 太原理工大学 | Method for preparing porous functional carbon fiber cluster from waste cotton textiles |
| CN104071770B (en) * | 2014-07-06 | 2015-12-02 | 太原理工大学 | A kind of method utilizing waste and old cotton textiles to prepare porous Functional Carbon Fiber bunch |
| CN104099688A (en) * | 2014-07-15 | 2014-10-15 | 李文军 | Cotton activated carbon fiber and production method thereof |
| CN104099688B (en) * | 2014-07-15 | 2016-06-01 | 李文军 | Cotton activated carbon fiber and production method thereof |
| CN104525117A (en) * | 2014-12-31 | 2015-04-22 | 中国地质大学（武汉） | Preparation method and usage of carbon-based epsilon-MnO2 high-efficiency arsenic adsorption material |
| CN106252616A (en) * | 2016-07-30 | 2016-12-21 | 复旦大学 | A kind of nickelous selenide/hollow carbon fiber composite and preparation method thereof |
| CN107190366A (en) * | 2017-06-30 | 2017-09-22 | 天津工业大学 | The preparation method of ultracapacitor N doping porous carbon fiber |
| CN107190367A (en) * | 2017-06-30 | 2017-09-22 | 天津工业大学 | The preparation method of nitrogen sulphur codope porous carbon fiber |
| CN108648922A (en) * | 2018-04-23 | 2018-10-12 | 中国石油大学(华东) | The preparation method of cotton carbon fiber/nickel aluminium hydroxide combination electrode material |
| CN109473291A (en) * | 2018-11-09 | 2019-03-15 | 天津工业大学 | A kind of N of the superelevation specific capacitance based on cotton, the novel preparation method of P codope Porous hollow Carbon fibe |
| CN110146554A (en) * | 2019-05-28 | 2019-08-20 | 新疆大学 | A kind of method of cotton carbonizatin method preparation high-performance gas sensor |
| CN112210397A (en) * | 2020-09-27 | 2021-01-12 | 长江大学 | Carbon fiber/nano silicon dioxide compound and preparation method and application thereof |
| CN113371779A (en) * | 2021-06-08 | 2021-09-10 | 中石化南京化工研究院有限公司 | Alkali liquor purification treatment method |
| CN114737279A (en) * | 2022-03-25 | 2022-07-12 | 北京科技大学 | Biomass hollow carbon fiber, preparation method thereof, electrode material and battery |
| CN114737279B (en) * | 2022-03-25 | 2023-02-24 | 北京科技大学 | Biomass hollow carbon fiber, preparation method thereof, electrode material and battery |
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