KR20110108888A - The fabrication of nano-porous carbon fiber from the floor carpet scrap of automobile - Google Patents

The fabrication of nano-porous carbon fiber from the floor carpet scrap of automobile Download PDF

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KR20110108888A
KR20110108888A KR1020100028351A KR20100028351A KR20110108888A KR 20110108888 A KR20110108888 A KR 20110108888A KR 1020100028351 A KR1020100028351 A KR 1020100028351A KR 20100028351 A KR20100028351 A KR 20100028351A KR 20110108888 A KR20110108888 A KR 20110108888A
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silica
carbon fiber
fiber
nanoporous carbon
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박순용
이재광
장효섭
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주식회사 디아이티그린
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2055Carbonaceous material
    • B01D39/2065Carbonaceous material the material being fibrous
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/02Types of fibres, filaments or particles, self-supporting or supported materials
    • B01D2239/025Types of fibres, filaments or particles, self-supporting or supported materials comprising nanofibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04Additives and treatments of the filtering material
    • B01D2239/0471Surface coating material

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  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nanotechnology (AREA)
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Abstract

The present invention relates to the production of spherical and chain-shaped nanoporous carbon fibers that effectively removes VOC and formaldehyde using Floor Carpet Scrap and nano silica sol that are incinerated and discarded during automobile manufacturing. Inorganic series sol in which nano silica is uniformly distributed in felt, non-woven or shredded car floor carpet scraps containing any one or more of the following groups: epoxy, polyester resin, phenol resin, and melamine resin. sol) to prepare a fiber-silica composite; Pretreatment step of uniformly coating the fibers of the polymer resin on the surface of the nano-silica to produce a resin-silica that is a carbon fiber precursor; Carbonizing the resin-silica and then removing the silica material to prepare nanoporous carbon fibers capable of effectively removing VOCs; The nanoporous carbon fiber is surface coated with an amphoteric compound catalyst to effectively remove formaldehyde. The spherical-chain nanoporous carbon fiber thus prepared can be utilized as an eco-friendly adsorbent and catalyst support in the form of recycled resources, which can effectively remove VOC and formaldehyde by providing a large specific surface area and rich pores.

Description

The fabrication of Nano-porous Carbon Fiber from the Floor Carpet Scrap of automobile}

Currently, Carpets used in domestic and foreign automobiles are made of PET or Nylon, which is excellent in durability and long-term use, and also excellent in flame resistance, hygroscopicity and sound absorption.It is used for the purpose of improving interior quietness and preventing noise while driving as interior materials for vehicles. have. Such Floor Carpet is molded according to the vehicle mold, and Scrap (residue) is generated in the molding cross section.

As of 2007, domestic floor carpet molding companies are generating and incinerated more than 15,000 tons / year of floor carpet scrap, and the actual amount is estimated to be more than 20,000 tons / year. Floor Carpet Scrap Waste treatment cost is about 1.5 million won / 10 tons, which is incinerated with industrial waste, and this incineration causes secondary environmental pollution that generates harmful gases and greenhouse gases. Can't.

In addition, floor carpet scrap waste disposal costs are estimated to account for more than 3% of the company's top-line revenue. There is no need for substantial recycling and no additional revenue is generated.

According to the recent research results, a polymerized / carbonized process is carried out by injecting a precursor such as a carbohydrate or a polymer monomer into a colloidal crystal template in which spherical silica particles are agglomerated, and then removing the silica template by chemical method to have a regular and constant size. A technique for synthesizing new macro-porous carbon materials has been reported.

However, due to the lack of specific surface area or pores, which are required for the adsorbent, since there are no fine or heavy pores on the walls of the carbon materials, which are easy to adsorb VOC or odor molecules, they are poor in terms of their performance. There is a problem that it is not suitable for various applications required as a porous material.

1) L. FENG, Z. YANG, J. ZHAI, Y. SONG, B. LIU, Y. MA, Z. YANG, L. JIANG and D. ZHU, Angew. Chem. Int. Ed. 42 (2003) 4217.

2) R. VACASSY, R. J. FLAT, H. HOFMANN, K. S. CHOI and R. K. SINGH, Journal of Colloid and Interface Science 227 (2000) 302 .; F. SCHUTH, Angew. Chem. Int. Ed. 42 (2003) 3604.

3) Y. YIN, Y. LU, B. GATES and Y. XIA, Chem. Mater. 13 (2001) 1146-1148 .; X. SUN and Y. LI, Angew. Chem. Int. Ed. 43 (2004) 597.

Therefore, there is a need for a carbon material manufacturing technology in which particles are uniform in shape and nano-sized pores are uniformly distributed.

In this regard, recently, methods for producing hollow / spherical carbon capsule structures having mesoporous outer shells are known. The carbon material produced by such a manufacturing method has a specific surface area of about 1400 / g, a pore volume of about 1.2 / g, and the physical properties thereof are comparable to those of commercially available activated carbon.

4) J. W. LEE, K. N. SOHN and T. H. HYEON, J. Am. Chem. Soc. 123 (2001) 5146.

5) S. B. YOON, K. N. SOHN, J. Y. KIM, C. H. SHIN, J. S. YU and T. W. HYEON, Adv. Mater. 14 (2002) 19.

6) Korean Patent Publication No. 2003-68765

However, there is still much room for improvement in the synthesis of this process. In this manufacturing method, most of materials used as raw materials of carbon materials use raw materials such as phenol and styrene, and additives such as formaldehyde and AIBN (Asobis Isobutyronitrile), and the solvents used in the reaction are mostly ethanol, It is composed of organic chemicals such as methanol.

Compared to activated carbon produced from tree nuts such as coconut shells, which are used for food and then discarded, it is necessary to improve the environment in a way that the manufacturing process itself causes environmental pollution. have.

In addition, in order to recover the nanomaterials produced in the final product in such a manufacturing method is used a centrifugation or self-precipitation method, which requires a lot of time in the process and also has a high yield and a large amount of waste water generated. Neither of these is economically or technically desirable.

The present invention to solve the above problem,

(1) To reduce the environmental pollution and reduce global warming emissions by restraining the use of excessive organic chemicals by recycling the waste carpets generated from the automobile production stage as carbon raw materials.

(2) In order to suppress the emission of environmental pollutants, most organic constituents used to prepare nano-silica sol that provides nano-structured form were converted to carbon materials in pretreatment and carbonization processes with waste fibers.

(3) In the process of dissolving the silica material to form nano pores, it was intended to react with the inorganic material and recover and reuse it as a raw material of ceramic materials such as zeolite.

(4) In order to enhance formaldehyde removal performance on nano pores effective for VOC removal, an amphoteric compound which simultaneously expresses an acid / base reaction was coated to increase the value as an adsorbent.

The spherical-chain nanoporous carbon fiber prepared as described above is economical and eco-friendly / recyclable, while maintaining the physical properties of the hollow / spherical carbon nanostructures having mesoporous shells manufactured by the conventional method. It is a product.

In other words, the present invention has a major technical configuration features in improving the post-treatment technology, such as raw materials, carbonization process including pretreatment and product recovery in the production of nanoporous carbon fiber, car waste fibers and nano silica sol Along with the technological progress of suppressing the loss of raw materials and the emission of environmental pollutants in the manufacturing process by carrying out the pretreatment of mixing waste fibers and silica in a certain reactor by mixing and carbonization to convert them into carbon fibers in a single process. It provides eco-friendly technology such as recycling resources such as silica material recovery in the use of fiber and post-treatment process, and improves production yield and effectively removes environmental pollutants such as VOC and formaldehyde by using nanoporous carbon fiber in the form of chain. Efficient and Highly Available Nano Device by Manufacturing Adsorbents Province to obtain carbon fibers.

Accordingly, the present invention provides a spherical-chain nanoporous carbon fiber that is environmentally friendly and economical and has excellent functionality as an adsorbent and a catalyst support than nano carbon materials manufactured by conventional methods by drastically improving the conditions of manufacturing raw materials and processes. The purpose is.

As described above, the present invention shows a spherical and chain form manufactured using floor carpet scrap and nano silica sol, which are car waste fibers, and at the same time, in order to manufacture nanoporous carbon fibers made of nano pores, It can be used as a carbon raw material to achieve the effect of resource recycling and greenhouse gas reduction, and to increase the carbon yield by converting the organic compound contained in the silica sol into a carbon raw material. In addition, by producing carbon fibers, most of which are formed of nano-pores, it can be widely applied to various applications such as adsorbents, catalyst carriers, batteries, and fuel cell catalyst support materials.

1: Thermogravimetric Analyzer (TGA) results of automotive waste fibers
2: Scanning electron microscope of carbon fiber prepared by Comparative Example 1
SEM: Scanning Electron Microscope
Figure 3: Scanning Electron Microscope (SEM) of the carbon fiber prepared by Example 1
Figure 4: Scanning Electron Microscope (SEM) of the carbon fiber prepared by Example 2
Figure 5: Scanning Electron Microscope (SEM) of the carbon fiber prepared by Example 3
Figure 6: Scanning Electron Microscope (SEM) photograph of the carbon fiber prepared by Example 4
7: Nitrogen adsorption isotherm of carbon fibers prepared by Comparative Example and Example
8: Pore distribution curve of carbon fibers prepared by Comparative Example and Example
Figure 9: Toluene removal curves of the carbon fibers prepared by Comparative Example and Example
Figure 10: Formaldehyde removal curves of the carbon fibers produced by Comparative Examples and Examples

The present invention relates to the production of spherical and chain-shaped nanoporous carbon fibers that effectively remove VOC and formaldehyde using Floor Carpet Scrap and nano silica sol, which are used in automobile waste fibers, including unsaturated polyester resins and epoxy-polyester resins. Fiber-silica composite by mixing inorganic silica sol with uniformly distributed nano-silica to felt, non-woven or shredded car waste fibers containing any one or more of phenol resin and melamine resin And heat-treat the fiber-silica composite to uniformly coat the waste fibers of polymer resin on the surface of silica to prepare resin-silica, and then carbonize the resin-silica composite mold and remove the silica material to recover the silica portion. And nanoporous carbon fiber that can effectively remove VOC The nanoporous carbon fiber is surface-coated with an amphoteric in order to effectively remove formaldehyde.

When explaining the configuration of the invention by more specific manufacturing steps,

1) Nano-silica of 300 ~ 500nm size is uniformly distributed in felt, non-woven or shredded car floor carpet scrap containing at least one of unsaturated polyester, epoxy-polyester, phenol, and melamine-based fibers. Octanesyltrimethoxysilane (C 18 -TMS) to form nanopores with polyoxyethylenealkylether, a nonionic surfactant, to induce nano silica to adhere to the surface of waste fibers by mixing inorganic sol Preparing a fiber-silica composite by recovering ethanol as a solvent while reacting the mixed suspension for 6 to 12 hours at 60 to 80 hours.

2) preparing a resin-silica composite mold by gradually raising the temperature of the fiber-silica composite to 200-300 in an air atmosphere and coating the waste fiber portion, which is a polymer resin, on the surface of silica.

3) preparing a carbon-silica composite mold by carbonizing the resin-silica composite mold in an inert atmosphere at a temperature ranging from 900 to 1000.

4) dissolving and recovering the silica by dissolving and stirring potassium hydroxide or sodium hydroxide aqueous solution to selectively remove the silica portion of the carbon-silica composite mold

5) Nanoporous carbon fiber comprising coating an amphoteric mixture such as sodium phosphate, potassium phosphate, rubidium phosphate, cesium phosphate, etc. to attach a functional group for effectively adsorbing formaldehyde gas to the nanoporous carbon fiber. The manufacturing method is characterized by that.

Hereinafter, the present invention will be described in more detail at each step.

The first process is to prepare a fiber-silica composite using automobile floor carpet scrap and nano silica sol.

Nano silica sol is prepared using tetraethoxysilane (TEOS), ammonia water, ethanol and the like, it is possible to produce a variety of silica particles according to the synthetic conditions.

Silica used in the present invention uses a constant size, and selectively synthesizes a specific size in the range of 300 ~ 500 nm, the synthesis method is known technology-Osseo-Asare, K; Arriagada, F. J. Colloids Surf. 1990, 50, 321; Stober, W .; Fink, A .; Bohn, E. J. Colloid Inter. Sci. The method reported in 1968, 26, 62 was applied.

After preparing such silica sol, the silica particles are coated with nanoporous silica particles of uniform size on the surface of the waste fiber.

In other words, a suspension containing oxydecyltrimethoxysilane (C 18 -TMS) mixed in order to form nano pores with polyoxyethylene alkyl ether, which is a nonionic surfactant, was reacted at 60 to 80 for 6 to 12 hours. While recovering ethanol as a solvent, only fiber-silica as a solid is preserved.

Instead of the nano-silica used in this process, solid form materials such as activated carbon, silica, zeolite series, and the like may be used.

The second process is to prepare a resin-silica composite mold by coating the waste fiber which is a polymer resin on the solid silica surface.

Applying heat to the fiber-silica composite prepared above to convert the car waste fibers, which are polymer resins, into a highly viscous gel state and coating them on the surface of silica.The raw materials of the polymer resins are unsaturated polyester, epoxy-polyester, and phenol. And those containing melamine series fibers can be used.

That is, the resin-silica composite mold is prepared by coating a fiber-silica composite on the surface of silica by gradually raising the temperature to 200-300 in an air atmosphere.

In this process, by controlling the amount of resin and applying an appropriate amount to the spherical silica, a precursor for producing carbon fibers in spherical and chain form at the same time as nano-sized pores is obtained. Since the shape of the final carbon fiber is determined, the weight ratio of silica sol and waste fiber is an important manufacturing process variable.

The third step is to prepare a carbon-silica composite mold by maintaining the resin-silica composite mold in an inert atmosphere and carbonized at a temperature range of 900 ~ 1000.

The resin-silica composite mold prepared above is injected into a carbonization furnace in which an inert atmosphere such as nitrogen and helium is injected to form an inert atmosphere, and then the temperature is increased from 900 to 1000 at a rate of 10 / min or less for 5 to 10 hours. After holding, cooling is performed to prepare a carbon-silica composite mold.

In the fourth process, the silica of the carbon-silica composite template is selectively removed to prepare carbon fibers having nanoporosity.

The carbon-silica composite template is added to an aqueous alkali solution to selectively dissolve and remove only silica. As alkali, sodium hydroxide, potassium hydroxide, or the like may be used.

That is, the carbon-silica composite template is added to NaOH or KOH aqueous solution to selectively elute silica and then filtered to recover the silica portion and the remaining carbon portion is dried at 100 to 12 hours or more.

The nanoporous carbon fiber thus obtained has a spherical and chain-like carbon fiber shape formed by nano-pores having a center at the core (macro-pore) and the outer shell having a uniform 2-4 nm size. The nanopore volume of the nanoporous carbon fiber can be controlled by controlling the amount of waste fiber and the amount of nonionic surfactant and C 18 -TMS constituting the outer surface of the silica surface, and have a uniform nano-size without additional post-treatment. The specific surface area and volume are increased.

In other words, the specific surface area is 1200 / g and the average pore volume is about 0.4 / g in the case of the high quality of the existing commercial activated carbon, the specific surface area is 1400 ~ 1800 / in the case of nanoporous carbon fiber produced by the method of the present invention g, the average pore volume was about 1.2 ~ 2.4 / g, it can be seen that the specific surface area and the volume of the nano-pores significantly increased.

The fifth process is to prepare a catalytic nanoporous carbon fiber by coating the amphoteric mixture on the nanoporous carbon fiber.

That is, the prepared nano-porous carbon fiber is effective to adsorb VOCs such as toluene, but there are almost no surface functional groups capable of adsorbing aldehyde gases such as formaldehyde. In order to attach a functional group for effective adsorption, alternatively, an amphoteric mixture such as sodium phosphate, potassium phosphate, rubidium phosphate, cesium phosphate, etc. may be dissolved in an aqueous solution and then injected into the nanoporous carbon fiber and dried at 100. The process takes place.

This process produces a catalytic nanoporous carbon fiber coated with a functional group capable of effectively removing formaldehyde gas on the surface of the nanoporous carbon fiber.

Nanoporous carbon fiber of the present invention prepared as described above can be widely applied to various applications such as adsorbent, battery, fuel cell catalyst support. EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated further more concretely based on a comparative example and an Example.

Figure 1 shows the results obtained by calorimetric gravimetric analysis (TGA) of the waste fibers in a nitrogen atmosphere in order to set the carbonization conditions of the automobile waste fibers used in the present invention.

As shown in FIG. 1, the waste fibers began to melt at about 120, and as the temperature increased, the weight thereof decreased and then became constant from above 800. In the present invention, the carbonization temperature was performed based on 800 degrees.

Comparative Example 1:

Felt, nonwoven or shredded car waste fibers containing any one or more of unsaturated polyester, epoxy-polyester, phenol, and melamine-based fibers are sieved using a fiber grinder to prepare a 4-6 mesh uniform size. . The prepared waste fibers are carbonized under conditions of an elevated temperature of 1 / min, a final temperature of 900, and a holding time of 5 hours in an air atmosphere to prepare simple carbon fibers.

2 shows a SEM photograph of the carbon fiber prepared by Comparative Example 1.

As shown in FIG. 2, the carbon fiber simply prepared by Comparative Example 1 exhibited a carbonized surface of a general fiber, and showed a form difficult to develop pores.

Felt, nonwoven or shredded car waste fibers containing any one or more of unsaturated polyester, epoxy-polyester, phenol, and melamine-based fibers are sieved using a fiber grinder to prepare a 4-6 mesh uniform size. . Silica sol was prepared by the sol-gel method of adding 8% ethyl alcohol, 4% ammonia water (25%) and 6% tetraethoxysilane and stirring at room temperature for 6 hours. Inject to a weight ratio of 50%. In order to induce nanosilica to adhere to the surface of the waste fiber, 10% of the silica sol weight ratio added to the non-ionic surfactant, polyoxyethylene alkyl ether, was added for 3 hours, followed by octadecyltrimethoxysilane (C 18 -TMS). 2% of the weight ratio of the added silica sol was reacted at 80 hours for 6 hours while evaporating and recovering ethanol as a solvent, leaving only solid content. The solid portion is gradually raised in an air atmosphere at a temperature rising rate of 1 / min to 300, and then maintained for 1 hour, and then cooled to room temperature to prepare a resin-silica composite mold. The resin-silica composite mold was carbonized under conditions of increasing the temperature increase rate 1 / min to 900 temperature in an inert atmosphere and maintained for 5 hours to prepare a carbon-silica composite mold. In order to selectively remove the silica portion of the carbon-silica composite mold, an aqueous sodium hydroxide solution was dissolved in 50% of the carbon-silica weight ratio in distilled water, mixed with carbon-silica, stirred at 80 hours for 6 hours, and filtered to obtain a solid and a solution. After separation, the solid is dried at 100 to 12 hours to prepare nanoporous carbon fibers.

3 shows a SEM photograph of the nanoporous carbon fiber prepared in Example 1.

As shown in Figure 3, the carbon fiber prepared under the conditions of Example 1 does not show the shape of the nano-spheres, which is determined that the amount of silica sol injected is insufficient compared to the waste fiber.

In Example 1, the silica sol is prepared by injecting the waste fiber in a weight ratio of 100%.

Figure 4 shows a SEM photograph of the nano-porous carbon fiber prepared in Example 2.

As shown in FIG. 4, the carbon fibers prepared under the conditions of Example 2 were found to form slightly spherical nanospheres, which shows that more silica sol is required than waste fibers.

In Example 1, the silica sol is prepared by injecting the waste fiber in a weight ratio of 150%.

5 shows a SEM photograph of the nanoporous carbon fiber prepared in Example 3.

As shown in FIG. 5, the carbon fiber prepared by Example 3 showed the shape of the nanospheres more clearly in FIG. 4.

In Example 1, a silica sol is prepared by injecting a waste fiber weight ratio of 200%.

6 shows a SEM photograph of the nanoporous carbon fiber prepared in Example 4.

As shown in FIG. 6, the carbon fiber prepared under the conditions of Example 4 had a nanosphere having a distinct shape, and also showed a chain form derived from the shape of the waste fiber. It suggests the best appearance.

After the nanoporous carbon fiber prepared in Example 4 was loaded to 50% in the weight ratio of distilled water, and dissolved sodium phosphate in distilled water to be 5% of the weight ratio of carbon fiber, mixed and dried at 100 for 24 hours Catalytic nanoporous carbon fibers are prepared.

Figure 7 shows the nitrogen adsorption isotherm of the carbon fibers prepared in Comparative Examples and Examples.

As shown in FIG. 7, the carbon fiber prepared in the comparative example showed almost no nitrogen adsorption capacity, and in the case of the example, the carbon fiber prepared in Example 3 showed the most nitrogen adsorption amount. Most of the isotherms of the embodiment show the shape of the isotherm represented by a material having nano-sized pores.

Figure 8 shows the pore distribution curve of the carbon fibers prepared in the Comparative Example and Example.

As shown in FIG. 8, most of the carbon fibers manufactured in Examples were formed of 3-4 nm nano-sized mesopores, and the carbon fibers manufactured in Example 4 formed the most mesopores.

Table 1 shows the specific surface area, pore volume and average pore size calculated from the nitrogen adsorption isotherm and pore distribution curve.

Item Specific surface area Pore volume Pore size [m2 / g] [cc / g] [nm] Comparative Example 1 4 0.012 11 Example 1 500 0.31 2.5 Example 2 1200 1.1 3.6 Example 3 1700 2 4.8 Example 4 1400 1.7 4.7

As shown in Table 1, the specific surface area and pore volume were the best in the carbon fiber prepared in Example 3. However, in FIG. 8, the volume of the nanopores is shown to be the largest in Example 4, and in Example 3, it can be estimated that the micropores of 1 nm or less are more developed than other carbon fibers.

Adsorption performance test was conducted in the following manner to confirm the adsorption performance of VOC and formaldehyde of the carbon fibers produced in Comparative Examples and Examples as described above. In this test, 1) 30g of carbon fiber was placed in a 30L acrylic chamber, and 3) a predetermined amount of toluene and formaldehyde standard gas was injected into the chamber. Toluene was 40ppm and formaldehyde was 10ppm. Then, 4) the concentration of gas in the chamber was measured while passing the carbon fiber equipped with the gas formed in the chamber by using a fan having a maximum air flow rate of 1 m 3 / min. At this time, the temperature in the chamber was maintained at 25 and the average relative humidity was 50-60%. The concentration analysis was performed using a flame ion detector tube (FID) mounted on a gas chromatograph (GC).

9 shows the toluene removal curves of the carbon fibers prepared in Comparative Examples and Examples.

As shown in FIG. 9, the carbon fibers produced by Comparative Example 1 showed insufficient adsorption of toluene, whereas the carbon fibers prepared in Examples showed significantly increased adsorption performance. In addition, the removal performance of toluene was shown to be the best in Examples 4 and 5. As shown in FIG. 8, the more nano-sized mesopores are developed, the better the adsorption capacity of VOCs such as toluene, and Example 5 is prepared by Example 4 by coating a catalyst on carbon fiber of Example 4. It shows that the pores of the carbon fiber are well preserved.

Figure 10 shows the formaldehyde removal curves of the carbon fibers prepared in the Comparative Example and Example.

As shown in FIG. 10, the carbon fiber prepared in Comparative Example 1 was inferior in formaldehyde adsorption capacity as in toluene, but the carbon fibers produced in Examples showed that the adsorption performance was significantly increased. In addition, formaldehyde adsorption was shown to increase in proportion to the size of the specific surface area shown in Table 1 and the carbon fiber of Example 3 showed the best adsorption performance. However, as shown in Example 5, the catalytic carbon fiber coated with the catalyst of the carbon fiber of Example 4 was found to significantly improve the adsorption performance of Example 4, which was formed by the role of the catalyst coated on the surface. It was confirmed that the adsorption performance was increased.

Table 2 shows the manufacturing conditions applied to Comparative Example 1 and Examples 1 to 5, and the specific surface area of the obtained carbon fibers and their respective removal efficiencies measured at 1 minute and 3 minutes of toluene and formaldehyde. The removal efficiency at this time was calculated by Equation 1.

Figure pat00001

The removal efficiency calculated by Equation 1 shows the performance when the gas present in the 30L chamber is treated once, which is related to the adsorption capacity as well as the adsorption rate.

Item fiber Silica catalyst Specific surface area toluene Formaldehyde [wt-%] [wt-%] [%] [m2 / g] [% -1 min] [% -3min] Comparative Example 1 100 0 0 4 5 11 Example 1 95 5 0 500 25 24 Example 2 90 10 0 1200 32 35 Example 3 70 30 0 1700 33 40 Example 4 60 40 0 1400 35 39 Example 5 60 40 5 1400 36 43

As shown in Table 2, toluene showed that nano-sized mesopores were effective for removal efficiency, and formaldehyde showed that the specific surface area was a major factor. However, the catalytic nanoporous carbon fiber prepared in Example 5 was shown to significantly increase the efficiency of formaldehyde while maintaining the efficiency of Example 4.

Claims (4)

1) Manufacturing the fiber-silica composite to induce nano silica to adhere to the surface of waste fiber by mixing inorganic silica sol with nano silica uniformly distributed on car floor carpet scrap, recovering solvent ethanol and leaving only solid content ;
2) preparing a resin-silica composite mold by coating the fiber-silica composite on a silica surface by gradually raising the temperature in an air atmosphere to polymer waste fiber portions;
3) carbonizing the resin-silica composite mold in an inert atmosphere to produce a carbon-silica composite mold;
4) to selectively remove the silica portion of the carbon-silica composite template by adding potassium hydroxide or aqueous sodium hydroxide solution, stirring and filtering to recover the silica, and drying the solid to prepare nanoporous carbon fibers;
5) preparing a catalytic nanoporous carbon fiber by coating an amphoteric mixture to attach a functional group for effectively adsorbing formaldehyde gas to the nanoporous carbon fiber;
Nanoporous carbon fiber and catalytic nanoporous carbon fiber manufacturing method comprising a.
The nanoporous carbon according to claim 1, wherein the car floor carpet scrap in the form of felt, nonwoven fabric or shredded form containing at least one of unsaturated polyester, epoxy-polyester, phenol, melamine-based fibers and nano silica sol Fiber manufacturing method. The non-ionic surfactant polyoxyethylene alkyl ether is mixed with octadecyltrimethoxysilane (C 18 -TMS) to form nanopores. Nanoporous carbon fiber manufacturing method to recover the ethanol as a solvent while adding a suspension (suspension) for 6 to 12 hours at 60-80. The catalytic nanoporous carbon according to claim 1, wherein the nanoporous carbon fiber is coated with an amphoteric mixture such as sodium phosphate, potassium phosphate, rubidium phosphate, cesium phosphate, or the like to attach a functional group for effectively adsorbing formaldehyde gas. Manufacturing method for producing the fiber.
KR1020100028351A 2010-03-30 2010-03-30 The fabrication of nano-porous carbon fiber from the floor carpet scrap of automobile KR20110108888A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105155815A (en) * 2015-09-10 2015-12-16 浙江康辉木业有限公司 Novel nano-carbon-fiber heating floor and preparation method thereof
KR101941126B1 (en) * 2017-08-01 2019-01-23 한국세라믹기술원 Manufacturing method for porous zeolite nanofiber composite having high specific surfcae area
CN111962183A (en) * 2020-08-26 2020-11-20 中山大学 Hollow carbon sphere fiber and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105155815A (en) * 2015-09-10 2015-12-16 浙江康辉木业有限公司 Novel nano-carbon-fiber heating floor and preparation method thereof
CN105155815B (en) * 2015-09-10 2018-01-05 浙江康辉木业有限公司 A kind of preparation method on nano carbon fiber heating floor
KR101941126B1 (en) * 2017-08-01 2019-01-23 한국세라믹기술원 Manufacturing method for porous zeolite nanofiber composite having high specific surfcae area
CN111962183A (en) * 2020-08-26 2020-11-20 中山大学 Hollow carbon sphere fiber and preparation method thereof

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