KR20170024311A - Aerogel based on cellulose including nanoparticles and fabrication method thereof - Google Patents
Aerogel based on cellulose including nanoparticles and fabrication method thereof Download PDFInfo
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Abstract
The present invention relates to a composite airgel having a three-dimensional network including nanoparticles and a method of manufacturing the same. More particularly, the present invention relates to a manufacturing method for enhancing strength and thermal stability by adding metal, ceramic or carbon nanoparticles to a cellulose base, which is a polymer, and its application.
Description
The present invention relates to a composite airgel having a three-dimensional network including nanoparticles and a method of manufacturing the same. More particularly, the present invention relates to a manufacturing method and an application thereof for improving thermal stability, electrical conductivity, and strength characteristics by adding a metal, ceramic, or carbon nanoparticle to a cellulose base, which is a polymer.
Worldwide, researches on renewable materials are being actively pursued due to depletion of fossil fuels. Cellulose, one of the environmentally friendly materials, is the most common organic compound on the planet. The main component of the plant cell wall is 10 14 kg of cellulosic per year, which is the largest organic compound on earth, and cellulose in plants accounts for 33% of the total mass.
Cellulose is a substance found in other plants such as wood, cotton, and was first isolated from trees in 1885 by Charles F. Cross and Edward Bevan at the Jodrell Laboratory in the Royal Botanic Garden of London.
Cellulose has been actively studied for various applications in many areas over a long period of time. In particular, cellulose has characteristics that it does not transmit heat, electricity, sound, shock, etc., and it is not only heavy in weight but also heavy in weight as well as in mechanical strength. Therefore, The research on synthesis of aerogels has been going on. Aerogels synthesized in a three-dimensional network structure are used as insulation materials, soundproofing materials, and filter materials because they have lightweight, heat-insulating properties.
In the conventional cellulose aerogels manufacturing method, many researches on reconstruction solvent and substitution solvent for improving specific surface area using calcium thiocyanate and NMMO have been carried out. However, Various attempts have been demanded.
US Patent Publication No. 2013/0018112 discloses a process for preparing cellulose nanoparticle aerogels, but in this case it comprises a pretreatment step for increasing the purity of the cellulose, wherein the cellulose-based airgel containing nanoparticles It is possible to manufacture one, improve physical properties through substitution solvent, and can be applied to improvement of heat insulation, fire resistance, soundproofing, deodorization and the like.
It is intended to provide a functional cellulose aerogel capable of controlling thermal stability, electrical conductivity, and strength properties, not limited to specific surface properties, by adding nanoparticles to a cellulose-based airgel base, and a method for producing the functional cellulose aerogels.
However, the problems to be solved by the present invention are not limited to the problems described above, and other problems not described can be clearly understood by those skilled in the art from the following description.
One aspect of the present invention provides a cellulosic-based aerogels comprising nanoparticles. Nano powders can be added to a cellulosic-based airgel base, which is a porous structure, to control the functions such as thermal stability, electrical conductivity, and strength characteristics.
Another aspect of the present invention provides a method of treating cellulosic fibers comprising: pretreating cellulose; Dissolving the pretreated cellulose; Gelling the dissolved cellulose through a reconstitution solvent; Washing the gelled cellulose with distilled water; Replacing the washed cellulosic with a solution comprising nanoparticles; And drying the substituted cellulose in a supercritical CO 2 drying apparatus. The present invention also provides a method for producing a cellulosic-based aerogel and a cellulose-based aerogel.
Yet another aspect of the present invention provides a method of treating cellulosic fibers comprising: pretreating cellulose; Hydrolyzing the pretreated cellulose with a sulfuric acid solution; Dialyzing and neutralizing the hydrolyzed cellulose with a membrane; Subjecting the neutralized cellulose to ultrasonic treatment to form a gel; Replacing the gelled cellulose with a solution comprising nanoparticles; And drying the substituted cellulose in a supercritical CO 2 drying apparatus. The present invention also provides a method for producing a cellulosic-based aerogel and a cellulose-based aerogel.
The solvent of the solution containing the nanoparticles may be an organic solvent, and may be an alcohol (methanol, ethanol, t-butanol, etc.), acetone, benzene or toluene. But is not limited to.
The present invention relates to an aerogel using a cellulose including nanoparticles and a method for producing the same, and is capable of being used as a material for a high value-added business out of the conventional paper and textile industries utilizing cellulose, Based airgel capable of controlling the strength and thermal stability through the formation of a network in which the water-soluble polymer is combined with the cellulose-based airgel.
1 is an image comparing the porosity size of an aerosol according to the reconstituting solvent of Example 1. Fig.
Figure 2a is a cellulose image produced by Example 2 and Figure 2b is an image of a dried cellulose gel.
FIG. 3A is an SEM image of the crystalline cellulose prepared in Example 3, and FIG. 3B is a crystalline cellulose image obtained by sonication.
Hereinafter, embodiments and examples of the present invention will be described in detail with reference to the accompanying drawings, which will be readily apparent to those skilled in the art to which the present invention pertains. It should be understood, however, that the present invention may be embodied in many different forms and is not limited to the embodiments and examples described herein. In order to clearly explain the present invention in the drawings, parts not related to the description are omitted.
Throughout this specification, when an element "includes" an element, it means that the element may include other elements as well, without departing from the other elements unless specifically stated otherwise.
Also, throughout the present specification, the phrase " step "or" step "does not mean" step for.
Hereinafter, embodiments of the present invention are described in detail, but the present invention is not limited thereto.
One aspect of the present invention provides a cellulosic-based aerogels comprising nanoparticles. Airgel is an ultra lightweight material that is manufactured by replacing the gel liquid with a gas and aerosol based on silica or carbon is a sponge-like structure composed of pores interconnected with randomly arranged nanoparticles do. Airgel, known for its very low density, is an excellent heat transfer material, but its use is limited by its brittleness. Accordingly, the present invention aims to overcome the brittleness of aerogels using light cellulose and to improve thermal stability and electrical conductivity by incorporating metal nanoparticles into aerogels.
In one embodiment of the present invention, the nanoparticles include at least one selected from the group consisting of metals, ceramics, and carbon particles. For example, the nanoparticles Ag, Zn, Fe, Co, Cu, W, Pd, Pt, Ta, Ni, Al, Au, Cu-Ni, NiO, CoO, Al 2 O 3, SiO 2, Fe 2 O 3, CeO 2, Cr 2 O 3, TiO 2, SiC, CdS, PbS, CdSe, ZnO, Tb 2 O 3, ZrO 2, SnO 2, mullite (mullite), In 2 O 3 , Al 2 O 3 / SnO 2, YBaCuO, Si 3 N 4, YSZ, WC, TiC, TiCN, T 2 O 3, MnO 2, Y 2 O 3, BaTiO 3, ZrO 2 (Y 2 O 3), La 0.15 Sr 0.15 CrO 3- y, BaCeO 3 (Nd 2 O 3), YGa 2 Cu 3 O 7-y, the exhaust catalyst (exhaust catalyst), mica (mica), fullerenes (fullerene), 1 is selected from carbon black, and combinations thereof Including, but not limited to, species.
In one embodiment of the invention, the nanoparticles are characterized by having an oxidizing functional group or a hydroxyl group (e.g., -COOH, -OH) that has been subjected to ozone treatment or plasma treatment. The oxidative functional group or the hydroxyl group not only improves the dispersibility of the metal, ceramic, or carbon ionic particles but also enables hydrogen bonding with the cellulose base, thereby facilitating formation of a three-dimensional network structure.
In one embodiment of the invention, the nanoparticles may be in the form of nanosheets, nanowires, nanorods, or nanotubes of a two-dimensional plate-like structure, and in particular graphene, carbon nanotubes, boron nitride nanosheets, But are not limited to, boron nitride nanotubes, MoS 2 nanosheets, silicon nanowires, silver nanowires, and the like.
In one embodiment of the invention, the size of the nanoparticles may be from 1 nm to 1000 nm, but is not limited thereto. For example, the size of the nanoparticles may be in the range of 1 nm to 1000 nm, 100 nm to 1000 nm, 200 nm to 1000 nm, 300 nm to 1000 nm, 400 nm to 1000 nm, 500 nm to 1000 nm, 1 nm to 900 nm, 1 nm to 800 nm, 1 nm to 700 nm, , Or 1 nm to 500 nm, but is not limited thereto.
In one embodiment of the present invention, the cellulose is crystalline cellulose, and the size of the crystalline cellulose particles is 150 nm to 300 nm. However, the present invention is not limited thereto. For example, the size of the crystalline nanocellulose particles may be 150 nm to 300 nm, 200 nm to 300 nm, 250 nm to 300 nm, 150 nm to 250 nm, or 150 nm to 200 nm, but is not limited thereto.
In one embodiment of the invention, the cellulose-based aerogels comprising the nanoparticles are characterized in that they further comprise a chelating agent. For example, the chelating agent may be one selected from Fe 2 SO 4 , FeCl 2 , FeCl 3 , or Fe 2 (SO 4 ) 3 , but is not limited thereto.
Another aspect of the present invention provides a method for preparing cellulose, comprising: pretreating cellulose at pH between 12 and 70 캜; Dissolving the pretreated cellulose at -10 ° C to 20 ° C; Gelling the dissolved cellulose through a reconstitution solvent; Washing the gelled cellulose with distilled water; Replacing the washed cellulosic with a solution comprising nanoparticles; And drying the substituted cellulose in a supercritical CO 2 drying apparatus. The present invention also provides a method for producing a cellulosic based aerogel.
The solvent of the nanoparticle-containing solution may be an organic solvent, and may be methanol, ethanol, tert-butanol, acetone, or the like, but is not limited thereto.
In the pretreatment step, a solvent comprising at least 5% by weight of hydrogen peroxide, at least 3.5% by weight of sodium silicate, at least 0.5% by weight of diethylene triamine pentaacetic acid (DTPA) ONA and at least 0.5% by weight of magnesium sulfate, based on the amount of wood pulp containing cellulose, The wood pulp is added and the pH is adjusted to 12 with sodium hydroxide. The main components of the wood are cellulose, hemicellulose, and lignin, with the exception of cellulose, which acts as an inhibitor of the physical properties and reactivity of the cellulose-based aerogels to be obtained herein. Therefore, a pretreatment step for removing hemicellulose and lignin contained in the wood pulp is required, and it is possible to increase the purity of the cellulose. At this time, it is preferable that the pulp has a cellulose content of 10% by weight or less in the pretreatment step. After the pre-treatment step, the pretreated cellulose particles were dried in an oven at 90 to 105 ° C, and a solvent containing not less than 7% by weight of sodium hydroxide and not less than 12% by weight of urea was prepared based on 100% by weight of the aqueous solution, % Or more at -10 캜 to 20 캜. 10 mg to 1000 mg of the dissolved cellulose nanoparticles were added to 1 ml of distilled water, ethanol, acetone, or methanol solvent as a reconstitution solvent to perform a gelation process. It is also possible to freeze-dry the cellulose nanoparticles for 12 hours to 24 hours to improve dispersibility of the cellulose nanoparticles before the step of gelling with the reconstitution solvent. Crystalline nanocellulose has a tendency to aggregate due to its nano-sized size, so drying with heat, such as an oven, is undesirable.
Yet another aspect of the present invention provides a method for preparing cellulose, comprising: pre-treating the cellulose at 70 DEG C to 80 DEG C to pH 12; Hydrolyzing the pretreated cellulose with a sulfuric acid solution; Dialyzing the hydrolyzed cellulose to a pH of 7 using a membrane to neutralize the hydrolyzed cellulose; Subjecting the neutralized cellulose to ultrasonic treatment to form a gel; Replacing the gelled cellulose with a solution comprising nanoparticles; And drying the substituted cellulose in a supercritical CO 2 drying apparatus. The present invention also provides a method for producing a crystalline cellulose-based aerogel.
The solvent of the nanoparticle-containing solution may be an organic solvent, and may be methanol, ethanol, tert-butanol, acetone, or the like, but is not limited thereto.
Specifically, in order to obtain the crystalline cellulose nanoparticles, cellulose pulp is dissolved in 8 ml to 10 ml of a sulfuric acid solution prepared from 45% by weight to 65% by weight on the basis of 1 g of cellulose pulp, and the cellulose pulp is dried at 45 ° C to 55 ° C for 30 minutes to 1 hour Lt; / RTI > At this time, the amorphous region of the cellulose was hydrolyzed to obtain crystalline cellulose nanoparticles. The diameter of the crystalline cellulose nanoparticles was determined to be 150 nm to 300 nm. Thereafter, the acidified crystalline cellulose nanoparticles were neutralized by dialysis to a pH of 7 using a molecular weight of 10,000 to 12,000 membranes. The neutralized crystalline cellulose nanoparticles were subjected to sonication and tip sonication to obtain a crystalline cellulose gel.
In the above manufacturing methods, when the distilled water is not replaced with a t-butanol solution or the like, the bond between the cellulose clust and the metal, carbon, or ceramic clust can be broken. In this case, it is required to replace the distilled water with a t-butanol solution. When t-butanol is used, it is possible to uniformly disperse the nano powder in an amount of 10 wt% or less based on the weight of t-butanol.
As the substitution solution, various organic solvents such as acetone, methanol, ethanol, benzene, and toluene can be used in addition to tert-butyl alcohol.
In one embodiment of the invention, the step of irradiating the radicals for radical formation prior to the step of drying the substituted cellulose in a supercritical CO 2 drying apparatus may further comprise the step of irradiating the substituted cellulose.
When cellulose is reacted with thionyl chloride or dimethylformamide to form an amino group and then reacted with a compound having an amine group at both ends of the alkyl chain, .
Hereinafter, preferred embodiments of a cellulose-based aerogel including nanoparticles of the present invention and a method of manufacturing the same will be described in detail with reference to the accompanying drawings.
However, the following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1 <Comparison of Porosity Size of Airgel According to Substitution Solvent>
A commercially available V60 product was used as the cellulose raw material used. To gelify the cellulose, a solvent containing 7% by weight of sodium hydroxide and 12% by weight of urea was prepared on the basis of the weight of the aqueous solution of 100% to dissolve at least 1% by weight of the cellulose pulp. Distilled water, ethanol, acetone, and methanol were used as reconstitution solvents. The comparison of the porosity according to distilled water, ethanol, acetone, and methanol used as reconstitution solvent is shown in FIG.
Example 2 < Preparation of cellulose-based airgel containing nanoparticles >
A commercially available V60 product was used as the cellulose raw material used. Cellulose was prepared by dissolving cellulose water pulp in a solvent containing 7% by weight of sodium hydroxide and 12% by weight of urea based on 100% by weight aqueous solution, and the dissolution temperature was 0 ° C. The dissolved cellulose was dispersed in methanol as a reconstitution solvent. Cellulose gelled by the reconstitution solvent was washed with distilled water, and the washed cellulose was substituted with tert-butyl alcohol solution containing 10% by weight of Ag or Cu nanoparticles. Thereafter, it was dried in a CO 2 supercritical drying apparatus at 40 bar and 45 ° C for 4 hours to obtain a cellulose-based aerogel containing Ag or Cu nanoparticles.
Example 3 < Preparation of crystalline cellulose-based airgel containing nanoparticles >
A commercially available V60 product was used as the cellulose raw material used. The reaction was carried out at 45 캜 for 30 minutes in 8 ml of sulfuric acid prepared at 65% by weight based on 1 g of cellulose pulp. At this time, the amorphous region of the cellulose was hydrolyzed to obtain crystalline nanocellulose having a diameter of 300 nm. The acidicized crystalline nanocellulose was neutralized by dialysis to a pH of 7 using a 10,000 molecular weight membrane. The neutralized crystalline nanocellulose was subjected to sonication and tip sonication to obtain a gelatinized crystalline cellulose. Subsequently, the cellulose was replaced with tert-butyl alcohol solution containing 10% by weight of Ag or Cu nanoparticles. Subsequently, drying was carried out in a CO 2 supercritical drying apparatus at 40 bar and 45 ° C for 4 hours to obtain a crystalline cellulose-based aerogel containing Ag or Cu nanoparticles.
Cellulose refers to chemical pulp extracted from wood-based chemical pulp as well as non-wood materials such as kenaf and rice hull. In the case of such pulp, since impurities such as hemicellulose and lignin are contained in a trace amount depending on the process, cellulose A pretreatment process is required. As suggested in the above solution, removal of more effective impurities is possible through hydrogen peroxide, metal salts, and sodium hydroxide solvents. However, in the case of pulp having a cellulose purity of 90% or more, a pretreatment step is not required. Due to the nature of the biomaterial, moisture is contained in a certain amount, and cellulose having a large amount of water is difficult to be pulverized. Therefore, it is preferable to dry the cellulose after the pretreatment at 105 deg. The water content of the cellulose is less than 5% by weight, which is suitable for pulverization and the present manufacturing method. A grinder means a general mill for pulverizing cellulose, but a pulverized cellulase uses a grinder to make the particles finer.
In Example 1, it was easy to disperse cellulose powder having a particle size of 0.5 mm or less. A solvent containing 7% by weight or more of sodium hydroxide and 12% by weight or more of urea based on 100% by weight of the aqueous solution was prepared to dissolve at least 1% by weight of the cellulose pulp. The dissolution temperature of the cellulose was adjustable in the range of -10 ° C to 20 ° C and the dissolution was possible even at the temperature above the melting point, but the dissolution was not effective due to the low molecular weight of the cellulose.
The reconstituted cellulose may be distilled water, ethanol, acetone or methanol, and more than 10% by weight of the reconstitution solvent is used based on 100% by weight of the dissolved cellulose. The cellulose was reconstructed to form a chain between the cellulose and the chain and the chain were combined to form a cluster. The cluster and the cluster were combined to form a network. Since the gelled composition contains a basic solvent and a reconstitution solvent, it was washed with distilled water.
In the case of the substituted and dispersed nano-sized metal particles, strong hydrogen bonding between cellulose and nano-metal particles can be induced by imparting an oxidizing functional group, a hydroxyl group (for example, -COOH, -OH) through ozone treatment or plasma treatment . The state of the cellulose gel in which the nanoparticles were dispersed was dried in a CO 2 supercritical drying apparatus at 40 bar and 40 ° C to 55 ° C for 4 hours. However, the range of the conditions may vary depending on the design standards of each apparatus and the size of the specimen have.
Claims (11)
Wherein the nanoparticles have an oxidizing functional group or a hydroxyl group that has been subjected to ozone treatment or plasma treatment.
The nanoparticles Ag, Zn, Fe, Co, Cu, W, Pd, Pt, Ta, Ni, Al, Au, Cu-Ni, NiO, CoO, Al 2 O 3, SiO 2, Fe 2 O 3, CeO 2 , Cr 2 O 3 , TiO 2 , SiC, CdS, PbS, CdSe, ZnO, Tb 2 O 3 , ZrO 2 , SnO 2 , mullite, In 2 O 3 , Al 2 O 3 / SnO 2 , YBaCuO Y 2 O 3 , BaTiO 3 , ZrO 2 (Y 2 O 3 ), La 0.15 Sr 0.15 CrO 3-y , BaCeO 3 , Y 2 O 3 , Si 3 N 4 , YSZ, WC, TiC, TiCN, T 2 O 3 , MnO 2 , (Nd 2 O 3 ), YGa 2 Cu 3 O 7-y , exhaust catalyst, mica, fullerene, carbon black, and combinations thereof. Lt; RTI ID = 0.0 > 1, < / RTI >
Wherein the nanoparticles comprise at least one selected from the group consisting of nanosheets, nanowires, nanorods, nanotubes, and combinations thereof.
Wherein the nanoparticles are selected from the group consisting of graphene, carbon nanotubes, boron nitride nanosheets, boron nitride nanotubes, MoS 2 nanosheets, silicon nanowires, silver nanowires, and combinations thereof Based on the total weight of the cellulose-based aerogels.
Wherein the cellulose is crystalline cellulose, and the size of the crystalline cellulose particles is from 150 nm to 300 nm.
A cellulosic based aerogels characterized by adding a chelating agent to the aerogels.
Wherein the chelating agent is at least one selected from Fe 2 SO 4 , FeCl 2 , FeCl 3 , or Fe 2 (SO 4 ) 3 .
Dissolving the pretreated cellulose;
Gelling the dissolved cellulose through a reconstitution solvent;
Washing the gelled cellulose with distilled water;
Replacing the washed cellulosic with a solution comprising nanoparticles;
Drying the substituted cellulose in a supercritical CO 2 drying apparatus
≪ RTI ID = 0.0 > 1, < / RTI >
Hydrolyzing the pretreated cellulose with a sulfuric acid solution;
Dialyzing and neutralizing the hydrolyzed cellulose with a membrane;
Subjecting the neutralized cellulose to ultrasonic treatment to form a gel;
Replacing the gelled cellulose with a solution comprising nanoparticles;
Drying the substituted cellulose in a supercritical CO 2 drying apparatus
≪ RTI ID = 0.0 > 1, < / RTI >
Further comprising UV irradiation for radical formation prior to drying the substituted cellulose in a supercritical CO 2 drying apparatus.
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