WO2019132266A1 - Composition de nanotube de carbone et son procédé de fabrication - Google Patents
Composition de nanotube de carbone et son procédé de fabrication Download PDFInfo
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- WO2019132266A1 WO2019132266A1 PCT/KR2018/014740 KR2018014740W WO2019132266A1 WO 2019132266 A1 WO2019132266 A1 WO 2019132266A1 KR 2018014740 W KR2018014740 W KR 2018014740W WO 2019132266 A1 WO2019132266 A1 WO 2019132266A1
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- carbon nanotube
- nanotube composition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
Definitions
- the present invention relates to a carbon nanotube composition and a method of manufacturing the carbon nanotube composition. More particularly, the present invention relates to a carbon nanotube composition improved in dispersibility and conductivity by controlling the ratio of specific surface area to bulk density.
- Carbon nanotubes which are one kind of fine carbon fibers, are tubular carbon having an average diameter of 1 ⁇ m or less. It is expected to be applied to various fields due to its high conductivity, tensile strength and heat resistance due to its specific structure. However, despite the availability of such carbon nanotubes, the use of carbon nanotubes is limited due to their low solubility and dispersibility.
- the carbon nanotubes were linearly dispersed in a dispersion medium, and a conductive material dispersion was prepared and used. However, carbon nanotubes are not stable in dispersion medium due to strong Van der Waals attraction between them, and coagulation phenomenon occurs.
- An object of the present invention is to provide a carbon nanotube composition excellent in dispersibility and conductivity and a method for producing the same.
- X is a number representing the specific surface area (unit: m2 / g) of the carbon nanotube composition
- Y is a number representing the bulk density (unit: kg / m 3) of the carbon nanotube composition.
- the present invention also relates to a process for preparing a mixture comprising mixing an organic acid and a vanadium precursor in a molar ratio of 1: 0.088 to 1: 0.605 to prepare a mixture; Mixing the mixture with a cobalt precursor to produce a catalyst precursor; Subjecting the aluminum hydroxide to a first heat treatment to produce a support; Supporting a catalyst precursor on the support, and then performing a second heat treatment to produce a supported catalyst; And reacting the supported catalyst with a carbon-based compound.
- the present invention also provides a method for producing a carbon nanotube composition.
- the carbon nanotube composition of the present invention is excellent in dispersibility and conductivity and can be contained at a high concentration in the conductive material dispersion.
- the productivity is excellent.
- a carbon nanotube refers to a pristine carbon nanotube that has not been subjected to any further processing.
- the entangled carbon nanotubes refer to a secondary structure in which a plurality of carbon nanotubes are entangled without a uniform shape such as a bundle or a rope.
- the bundle-type carbon nanotubes are formed by arranging a plurality of carbon nanotube unit pieces in a bundle or a rope ) ≪ / RTI > shape.
- the unit of carbon nanotubes is a graphite sheet having a nano-sized diameter cylinder shape and has an sp 2 bonding structure. At this time, depending on the angle and structure of the graphite surface, the characteristics of the conductor or semiconductor may be exhibited.
- the unit of the carbon nanotube may be a single-walled carbon nanotube (SWCNT), a double-walled carbon nanotube (DWCNT), or a multi-walled carbon nanotube (DWCNT) according to the number of walls MWCNT, and multi-walled carbon nanotubes. The thinner the wall thickness, the lower the resistance.
- the specific surface area of the carbon nanotube composition is measured by the BET method. For example, it can be calculated from the amount of nitrogen gas adsorbed at a liquid nitrogen temperature (77K) using BEL Japan's BELSORP-mino II have.
- the bulk density of the carbon nanotubes can be measured according to ASTM B329, specifically, according to ASTM B329-06.
- the bulk density can be measured using a Scott volumeter (Version USP 616).
- the bulk density of the carbon nanotube composition can be measured in accordance with the laboratory conditions, and substantially the same result as the result based on the above rule can be obtained.
- the average diameter and length of the carbon nanotube unit can be measured using an electric field-type scanning electron microscope.
- the carbon nanotube composition according to an embodiment of the present invention is a carbon nanotube composition including an entangled carbon nanotube and a bundled carbon nanotube.
- the carbon nanotube composition has a specific surface area of 190 to 240 m < 2 > / g, The following formula 1 is satisfied:
- X is a number representing the specific surface area (unit: m2 / g) of the carbon nanotube composition
- Y is a number representing the bulk density (unit: kg / m 3) of the carbon nanotube composition.
- the carbon nanotube composition has a specific surface area of 190 to 240 m < 2 > / g.
- the specific surface area of the carbon nanotube composition may be from 193 to 239 m 2 / g, from 195 to 239 m 2 / g, from 200 m 2 / g to 238 m 2 / g, or from 200 to 235 m 2 / g, g is preferable.
- the conductivity is excellent and can be advantageous for high-concentration dispersion. If it is less than the above-mentioned range, the conductivity is remarkably lowered, and if it exceeds the above-mentioned range, it can not be dispersed at a high concentration in the conductive material dispersion.
- Equation 1 is an index showing the dispersion concentration when the conductive material dispersion is prepared from the carbon nanotube composition, and the value of the formula 1 is 0.1 to 5.29.
- the value of the formula 1 may be from 1 to 5.14, from 1.5 to 5, or from 1.7 to 2.5, preferably from 1.7 to 2.5.
- the carbon nanotubes can be dispersed at a higher concentration in the conductive material dispersion.
- the value of the formula (1) is less than the above-mentioned range, the diameter of the carbon nanotube unit becomes very large and it is difficult to apply it as a conductive material. If it exceeds the above-mentioned range, it is difficult to disperse at a high concentration in the conductive material dispersion.
- the bulk density of the carbon nanotube composition may be 25 to 150 kg / m 3, 35 to 130 kg / m 3, 40 to 125 kg / m 3, 50 to 125 kg / m 3 or 90 to 115 kg / To 115 kg / m < 3 >.
- the dispersion can be dispersed at a high concentration since the dispersion gradually occurs during production of the conductive material dispersion
- the carbon nanotube composition is prepared by mixing the entangled carbon nanotubes and the bundled carbon nanotubes in a ratio of 1: 0.01 to 1: 0.5, preferably 1: 0.02 to 1: 0.3, more preferably 1: 0.05 to 1: 0.2. Weight ratio. When the above-mentioned range is satisfied, there is an advantage of excellent conductivity.
- the average diameter of the carbon nanotubes in the carbon nanotube composition may preferably be 30 nm or less, more preferably 10 to 30 nm. When the above-mentioned range is satisfied, the dispersibility and the conductivity can be improved.
- the average length of the carbon nanotubes may preferably be 0.5 to 200 mu m, more preferably 10 to 60 mu m. When the above-mentioned range is satisfied, it is excellent in electrical conductivity and strength, and stable at room temperature and high temperature.
- the carbon nanotube unit preferably has an aspect ratio defined by the ratio of the length of the carbon nanotube unit (the length of the long axis passing through the center of the unit) to the diameter (the length of the minor axis passing through the center of the unit and perpendicular to the long axis) To 50,000, and more preferably from 10 to 20,000.
- the carbon nanotube layer surface per unit interval is a carbon crystal obtained by X-ray diffraction method (d 002) and to the O.335 O.342 nm, layer surface spacing (d 002) ⁇ O.3448 - 0.0028 (log ⁇ ) ( wherein , and? is the average diameter of the carbon nanotube unit), and the thickness Lc of the crystal in the C axis direction may be 40 nm or less.
- the interplanar spacing (d 002 ) may preferably be less than 0.3444-0.0028 (1og ⁇ ), and more preferably less than 0.3441-0.0028 (log ⁇ ).
- the crystallinity of the carbon nanotube unit is improved, so that the conductivity of the entangled carbon nanotube including the same can be further improved.
- the carbon nanotube composition according to an embodiment of the present invention comprises: 1) mixing an organic acid and a vanadium precursor in a molar ratio of 1: 0.088 to 1: 0.605 to prepare a mixture; 2) preparing a catalyst precursor by mixing the mixture with a cobalt precursor; 3) subjecting the aluminum hydroxide to a first heat treatment to produce a support; 4) supporting a catalyst precursor on the support, and then performing a second heat treatment to produce a supported catalyst; And 5) reacting the supported catalyst with the carbon-based compound.
- an organic acid and a vanadium precursor are mixed in a molar ratio of 1: 0.088 to 1: 0.605 to prepare a mixture.
- the organic acid and the vanadium precursor are preferably mixed in a molar ratio of 1: 0.09 to 1: 0.6.
- a carbon nanotube composition that can be dispersed at a high concentration in the conductive material dispersion can be produced.
- a carbon nanotube composition including an entangled carbon nanotube having a low bulk density and a bundled carbon nanotube having a high bulk density can be produced. If it is less than the above-mentioned range, only the entangled carbon nanotubes are produced without producing the bundled carbon nanotubes. Above the above-mentioned range, bundle-type carbon nanotubes are produced, or the bulk density of the carbon nanotube composition is decreased, so that high-concentration dispersion is difficult.
- the organic acid may be at least one member selected from the group consisting of citric acid, tartaric acid, fumaric acid, malic acid, acetic acid, butyric acid, palmitic acid and oxalic acid, of which citric acid is preferable.
- the vanadium precursor may be a salt of a vanadium compound, preferably at least one selected from the group consisting of NH 4 VO 3 , NaVO 3 , V 2 O 5 and V (C 5 H 7 O 2 ) 3 , NH 4 VO 3 is more preferable.
- the mixture and the cobalt precursor are then mixed to produce a catalyst precursor.
- the mixture and the cobalt precursor may be mixed so that the molar ratio of vanadium and cobalt is 1: 1 to 1: 100, preferably 1: 5 to 1:20.
- the mixture and the cobalt precursor that is, the organic acid, the vanadium precursor, and the cobalt precursor can be used in the form of a solution dissolved in a solvent, and the solvent can be at least one kind selected from the group consisting of water, methanol and ethanol, desirable.
- the concentration of the citric acid, vanadium precursor and cobalt precursor in the solution may be preferably 0.1 to 3 g / ml, more preferably 0.5 to 2 g / ml, even more preferably 0.7 to 1.5 g / ml .
- Al (OH) 3 aluminum hydroxide (Al (OH) 3 ) is subjected to a first heat treatment to produce a support.
- the aluminum hydroxide may be pretreated before performing the first heat treatment.
- the pretreatment may be carried out at 50 to 150 ° C for 1 to 24 hours. By performing the pretreatment, the residual solvent or impurities that may be present on the surface of the aluminum hydroxide can be removed.
- the aluminum hydroxide may have an average particle diameter of 20 to 200 ⁇ ⁇ , a porosity of 0.1 to 1.0 cm3 / g, and a specific surface area of less than 1 m2 / g.
- the first heat treatment may be performed at 250 to 500 ° C, preferably 400 to 500 ° C. Also, the first heat treatment may be performed in an air atmosphere.
- Aluminum (OH) 3 is contained in an amount of 30 wt% or more, Al (OH) 3 is 70 wt% or less, specifically, AlO (OH) 3 is contained in an amount of 60% by weight or less, but does not contain Al 2 O 3 .
- the support may further include a metal oxide such as ZrO 2 , MgO, and SiO 2 .
- the shape of the support is not particularly limited, but may be spherical or potato-shaped.
- the support may have a porous structure, a molecular sieve structure, a honeycomb structure, or the like so as to have a relatively high surface area per unit mass or unit volume.
- a catalyst precursor is supported on the support and then subjected to a second heat treatment to produce a supported catalyst.
- the support may be such that the support and the catalyst precursor are uniformly mixed and aged for a predetermined time.
- the mixing can be carried out specifically by rotating or stirring at a temperature of 45 to 80 ⁇ ⁇ .
- the aging can be carried out for 3 to 60 minutes.
- the catalyst precursor may be supported on the support and then dried.
- the drying may be carried out at 60 to 200 ° C for 4 to 16 hours.
- the second heat treatment may be carried out under an additional pressure of from 0.1 to 2 bar or from 0.5 to 1.5 bar, preferably from 0.5 to 1.5 bar.
- the second heat treatment is performed under the above-described pressure, the bulk density of the carbon nanotube composition can be more appropriately maintained, so that high-concentration dispersion can be facilitated.
- the additional pressure of 0.1 to 2 bar during the second heat treatment may be the internal pressure of the container for performing the second heat treatment (hereinafter referred to as the second heat treatment container), that is, the pressure further applied at the atmospheric pressure.
- the second heat treatment container the internal pressure of the container for performing the second heat treatment
- the lid of the second heat treatment vessel is partially opened by the internal pressure, so that the gas in the vessel can be discharged to the outside.
- the lid may be closed again. The second heat treatment may be performed while repeating this process.
- the second heat treatment may be performed in an air atmosphere for 1 to 6 hours.
- the second heat treatment may be performed at 500 to 800 ° C, preferably 700 to 800 ° C.
- a supported catalyst in which the catalyst precursor is present in a state coated on the surface and the pores of the support is produced.
- the carbon nanotube composition as a final product manufactured using the supported catalyst satisfies the above-described bulk density and formula (1).
- the supported catalyst is reacted with the carbon-based compound.
- the reaction of the supported catalyst with the carbon-based compound can be carried out by a chemical vapor synthesis method.
- the supported catalyst is fed into a horizontal fixed bed reactor or a fluidized bed reactor, and the temperature of the catalyst is maintained at a temperature not lower than the pyrolysis temperature of the carbon-based compound in the gaseous state (hereinafter referred to as').
- the gas-phase carbon compound or a gas mixture of the gas-phase carbon compound and a reducing gas (for example, hydrogen) and a carrier gas (for example, nitrogen) is injected to decompose the gas- And then growing the carbon nanotubes.
- the carbon nanotubes produced by the chemical vapor synthesis method as described above have a crystal growth direction nearly parallel to the tube axis and a high crystallinity of the graphite structure in the tube length direction. As a result, the diameter of the unit is small, and the electrical conductivity and strength are high.
- the carbon nanotube composition may be prepared at 500 to 800 ° C, preferably at 550 to 750 ° C. In the reaction temperature range, the weight of the carbon nanotubes is maintained while maintaining the bulk size of the carbon nanotubes while minimizing the generation of amorphous carbon, so that the dispersibility according to the reduction of the bulk density can be further improved.
- the heat source for the heat treatment induction heating, radiation heat, laser, IR, microwave, plasma, surface plasmon heating and the like can be used.
- the carbon-based compound can supply carbon, and can be used without limitation, as long as it can exist in a vapor state at a temperature of 300 ° C or higher.
- the carbon-based compound may be a carbon-based compound having a carbon number of 6 or less, and may be a carbon-based compound such as carbon monoxide, methane, ethane, ethylene, ethanol, acetylene, propane, propylene, butane, butadiene, pentane, pentene, cyclopentadiene, And toluene are preferable.
- the production method of the present invention can selectively carry out a removal step for removing metal impurities from the metal catalyst remaining in the carbon nanotube composition.
- the metal impurity removing step may be performed according to a conventional method such as washing and acid treatment.
- Aluminum hydroxide (Al (OH) 3 ) as an aluminum-based support precursor was first heat-treated at 450 DEG C for 4 hours in an air atmosphere to prepare an aluminum-based support containing AlO (OH) in an amount of 40 wt% or more.
- NH 4 VO 3 aqueous solution was prepared by adding citric acid and NH 4 VO 3 in water at a molar ratio of 1: 0.09 and dissolving them.
- Co V molar ratio of 10: Co so that the 1 (NO 3) 2 ⁇ 6H 2 O and NH 4 VO 3 Aqueous solution to prepare a clear aqueous solution of catalyst precursor aqueous solution.
- the support and the catalyst precursor aqueous solution were mixed such that the Co and Al contents of the catalyst precursor aqueous solution were 23 moles and 2.3 moles, respectively, based on 100 moles of Al in the support.
- the catalyst precursor aqueous solution was supported on the support in a thermostatic chamber at 60 DEG C for 5 minutes and then dried in an air atmosphere at 120 DEG C for 12 hours. Subsequently, the supported catalyst was subjected to a second heat treatment at 720 ⁇ ⁇ for 4 hours in an air atmosphere to prepare a supported catalyst.
- a carbon nanotube composition was prepared in the same manner as in Example 1, except that NH 4 VO 3 aqueous solution was prepared by adding citric acid and NH 4 VO 3 at a molar ratio of 1: 0.096 to water and dissolving them to prepare an NH 4 VO 3 aqueous solution.
- Citrate and NH 4 VO 3 1 a molar ratio of 0.115 was added to the water and dissolved NH 4 VO 3 Carbon nanotube composition was prepared in the same manner as in Example 1, except that an aqueous solution was prepared.
- a carbon nanotube composition was prepared in the same manner as in Example 1, except that NH 4 VO 3 aqueous solution was prepared by adding citric acid and NH 4 VO 3 in water at a molar ratio of 1: 0.144 and dissolving them to prepare an NH 4 VO 3 aqueous solution.
- Aluminum hydroxide (Al (OH) 3 ) as an aluminum-based support precursor was first heat-treated at 450 DEG C for 4 hours in an air atmosphere to prepare an aluminum-based support containing AlO (OH) in an amount of 40 wt% or more.
- NH 4 VO 3 aqueous solution was prepared by adding citric acid and NH 4 VO 3 in water at a molar ratio of 1: 0.58 and dissolving them.
- Co V molar ratio of 10: Co so that the 1 (NO 3) 2 ⁇ 6H 2 O and NH 4 VO 3 Aqueous solution to prepare a clear aqueous solution of catalyst precursor aqueous solution.
- the support and the catalyst precursor aqueous solution were mixed such that the Co and Al contents of the catalyst precursor aqueous solution were 16 moles and 1.6 moles, respectively, based on 100 moles of Al in the support.
- the catalyst precursor aqueous solution was supported on the support in a thermostatic chamber at 60 DEG C for 5 minutes and then dried in an air atmosphere at 120 DEG C for 12 hours. Subsequently, the catalyst was subjected to a second heat treatment under air at 720 ° C for 4 hours under 1.0 bar to prepare a supported catalyst.
- the pressure applied during the second heat treatment means the internal pressure in the second heat treatment vessel.
- the lid of the second heat treatment vessel is partially opened by the internal pressure,
- the lid is closed again. This process was repeated for 4 hours, and the second heat treatment was performed.
- a carbon nanotube composition was prepared in the same manner as in Example 1, except that NH 4 VO 3 aqueous solution was prepared by adding citric acid and NH 4 VO 3 to water at a molar ratio of 1: 0.6 and dissolving the solution.
- a carbon nanotube composition was prepared in the same manner as in Example 1, except that NH 4 VO 3 aqueous solution was prepared by adding citric acid and NH 4 VO 3 at a molar ratio of 1: 0.085 to water and dissolving them to prepare an NH 4 VO 3 aqueous solution.
- a carbon nanotube composition was prepared in the same manner as in Example 1, except that NH 4 VO 3 aqueous solution was prepared by adding citric acid and NH 4 VO 3 at a molar ratio of 1: 0.61 to water and dissolving them to prepare an NH 4 VO 3 aqueous solution.
- Citric acid and NH 4 VO 3 were added to water at a molar ratio of 1: 2.3 and dissolved to form NH 4 VO 3 was prepared in the same manner as in Example 1 except that the support and the catalyst precursor aqueous solution were mixed so that the amount of Co and the amount of V in the catalyst precursor aqueous solution were 14 moles and 1.4 moles, respectively, per 100 moles of Al in the support.
- a carbon nanotube composition was prepared in the same manner as in Comparative Example 1, except that aluminum hydroxide (Al (OH) 3 ) as an aluminum-based support precursor was subjected to a first heat treatment at 800 ⁇ ⁇ for 4 hours in an air atmosphere.
- Al (OH) 3 aluminum hydroxide
- BET specific surface area The amount of nitrogen gas adsorbed at a temperature of liquid nitrogen (77K) was measured using BEL Japan's BELSORP-mino II.
- Powder resistance value (ohm-cm @ 1 g / cc):
- the carbon nanotube was filled into an insulating mold so as to have a density of 1 g / cc and pressurized.
- Loresta-GX (trade name: MITSUBISHI CHEMICAL ANALYTECH) The surface current and voltage were measured with four probes and the powder resistance was calculated.
- Comparative Example 1 prepared by adding citric acid and NH 4 VO 3 at a molar ratio of 1: 0.085, the specific surface area to bulk density was 1.85, and the specific surface area was 185 m 2 / g. It was confirmed that it is not suitable for use as a conductive material dispersion.
- Comparative Example 2 prepared by adding citric acid and NH 4 VO 3 at a molar ratio of 1: 0.61, the specific surface area to the bulk density was 5.58, so the powder resistance was low and the conductivity was excellent. However, It was confirmed that it was not suitable for use as a conductive material dispersion.
- Comparative Examples 3 and 4 prepared by adding citric acid and NH 4 VO 3 at a molar ratio of 1: 2.3 are bundle-type carbon nanotubes, and the specific surface area to bulk density is 9.47 and 10.5, respectively.
- the conductivity was excellent, but the dispersion concentration was too low to confirm that it was not suitable for the conductive material dispersion.
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Abstract
La présente invention concerne une composition de nanotubes de carbone contenant des nanotubes de carbone du type enchevêtré et des nanotubes de carbone du type groupé, la composition de nanotubes de carbone ayant une surface spécifique de 190-240 m2/g et un rapport de la surface spécifique à la masse volumique apparente de 0,1 à 5,29.
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
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US16/624,743 US11565938B2 (en) | 2017-12-26 | 2018-11-27 | Carbon nanotube composition and method of preparing the same |
CN201880041613.6A CN110785378B (zh) | 2017-12-26 | 2018-11-27 | 碳纳米管组合物及其制备方法 |
EP18896593.3A EP3628641A4 (fr) | 2017-12-26 | 2018-11-27 | Composition de nanotube de carbone et son procédé de fabrication |
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KR20170179769 | 2017-12-26 | ||
KR10-2017-0179769 | 2017-12-26 | ||
KR1020180146926A KR102379595B1 (ko) | 2017-12-26 | 2018-11-26 | 탄소나노튜브 조성물 및 이의 제조방법 |
KR10-2018-0146926 | 2018-11-26 |
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KR20150037661A (ko) * | 2013-09-30 | 2015-04-08 | 주식회사 엘지화학 | 탄소나노튜브 제조용 촉매 및 이를 이용하여 제조된 탄소나노튜브 |
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