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    • 专利摘要:
    Method of obtaining nanomaterials composed of carbonaceous material and metal oxides. The present invention relates to a method for obtaining nanomaterials composed of two or more components, in which at least one of these components is a carbonaceous nanomaterial and at least one of the components is a metal oxide. The method of the present invention allows to prepare these nanomaterials in liquid medium at moderate pressures and temperatures, in industrial quantities and to control the physical/chemical properties of said nanomaterials by controlling the synthesis parameters. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2678419A1
    申请号:ES201830402
    申请日:2018-04-25
    公开日:2018-08-10
    发明作者:María SEARA MARTÍNEZ；Alejandra GARCÍA GÓMEZ；Iñigo LARRAZA ÁLVAREZ；Elisa PEÑA MARTÍN；Víctor BLANCO LÓPEZ；Sara RUIZ MARTÍNEZ-ALCOCER
    申请人:Gnanomat Sl；
    IPC主号:
    专利说明:

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    they have certain advantages and disadvantages and in each case they are used depending on the product you want to obtain.
    The “bottom up” approach is much more popular in the synthesis of nanoparticles, in which said nanoparticles can be synthesized in isolation or as part of another material, however, it involves chemical reactions and are more complex processes methodologically and whose investment costs They are very high.
    In the case of "top down" products are obtained from larger structures and manufacturing techniques are well known, however, products with a higher concentration of imperfections are obtained and the processes offer less control over the product.
    On the other hand, with respect to the method of obtaining depending on morphology, in the last decades, new methods of synthesis have emerged for the production of graphene / nanoparticle hybrids. These new methods range from novel schemes to slight changes in known procedures that provide the production of a desired product (Yu, G .; Xie, X .; Pan, L .; Bao, Z .; Cui, Y. Hybrid Nanostructured Materials for High-Performance Electrochemical Capacitors. Nano Energy 2013, 2 (2), 213-234.)
    More specifically, the synthesis methods for obtaining nanomaterials composed of graphene / metal oxides can be classified as follows:
    (one) Graphene and / or derivatives (r-GO, reduced graphene oxide; and GO, graphene oxide) decorated with nanoparticles.
    (2) Nanoparticles encapsulated with graphene or its derivatives.
    The main difference between these two classes is the relative size relationship between the nanoparticles and the lateral dimensions of the carbonaceous material: when the size of the nanoparticles is in the range of a few nanometers, the nanoparticles are small and can easily decorate the sheet of graphene On the contrary, when the particle size becomes comparable with graphene, this two-dimensional carbonaceous sheet can be used to encapsulate the particles, which leads to the second type of hybrids.
    Although the variety of techniques for the preparation of nanomaterials is very wide, the techniques of Graphene and / or derivatives decorated with nanoparticles are of great interest. These techniques can be divided into “In situ” and “Ex situ”.
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    50 mg of ZnO in 20 mL of a solvent formed by a mixture of malonic acid and water was added in a 1: 6 molar ratio. Similarly and independently, 30 mg of Mn3O4 was added to 20 mL of a solvent identical to the previous one. Both mixtures were sonicated independently in an ultrasonic bath for 1 hour until complete
    5 dissolution of metal oxides.
    Then, both solutions were mixed and 80 mg of graphene nanoplatelets were added. The new mixture was sonicated for an additional 1 hour and then 100 mL of a 5M NaOH solution was added under mechanical stirring with a magnetic bar.
    When the pH of the mixture reached a value of 12, the solid present in the medium was isolated by vacuum filtration, washed with distilled water, ethanol. Finally, it was dried in an oven at 100 ° C for 12 hours, obtaining 157 mg of a dark material.
    For the analysis of the sample, one milligram of said powder was taken and dispersed in 5 mL of
    15 absolute ethanol by 15 minutes of sonication. A few drops of said dispersion were taken and added on a carbon-coated copper grid and observed by electron transmission microscopy (TEM). The image is shown in Figure
    5.
    20 Example 5: Preparation of graphene composite / Mn3O4 / Ag. 30 mg of Mn3O4 was added to 30 mL of a solution composed of a mixture of malonic acid and water in a 1: 6 molar ratio and the mixture was sonicated in an ultrasonic bath for 2 hours. Next, 15.75 mg of AgNO3 was added to the mixture and dissolved
    25 while applying ultrasound for an additional 30 minutes.
    50 mg of graphene nanoplatelets (Graphene-Tech product number GP500 801282-5) were added to the previous mixture and the entire system was sonicated for one more hour.
    30 A magnetic bar was incorporated into the mixture and stirred while 25 mg of NaBH4 was added slowly. After 30 minutes, 300 mL of a 1M NaOH solution was added until alkaline pH. Finally, the solid present in the mixture was filtered under vacuum, washed with distilled water and ethanol and dried in an oven at 100 ° C for 12 hours.
    The resulting mixture was filtered under vacuum and the solid obtained was washed with distilled water and ethanol and finally dried at 100 ° C for 12 h. For the analysis of the sample, a
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    milligram of said powder and was dispersed in 5 mL of absolute ethanol by 15 minutes of sonication. A few drops of said dispersion were taken and added on a carbon-coated copper grid and observed by electron transmission microscopy (TEM). The image is shown in Figure 6.
    5
    Example 6: Preparation of composite active carbon / Mn3O4 / Fe3O4. 30 mg of Mn3O4 and 20 mg of Fe3O4 were added to an aqueous solution of oxalic acid
    0.1 M and the mixture was subjected to sonication in an ultrasonic bath, for one hour
    10 approximately, until all the solid material was completely dissolved. Then, 50 mg of activated carbon (Haycarb HCE 202) was added to the previous mixture and the whole was sonicated for an additional 30 minutes. Then, 10mL of an aqueous solution of 5M NaOH was slowly added to the mixture while everything was vigorously stirred with a magnetic bar.
    Finally, the mixture was filtered under vacuum, obtaining a dark material that was washed with distilled water, ethanol and dried in an oven at 100 ° C.
    The sample was analyzed by scanning electron microscopy (SEM), using 5 mg 20 of material without modification. The image is shown in Figure 7.
    Example 7: Preparation of graphene composite / carbon nanotubes / Mn3O4 / Fe3O4. 30 mg of Mn3O4 and 20 mg of Fe3O4 were added to an aqueous solution of oxalic acid
    0.1 M and the mixture was subjected to sonication in an ultrasonic bath, for one hour
    25 approximately, until all the solid material was completely dissolved. Then, 30 mg of graphene nanoplatelets (Graphene-Tech product number GP500 801282-5) and 20 mg of carbon nanotubes (Carbon Solutions, Inc. AP-SWNT) were added to the previous mixture and the whole was sonicated for 30 more minutes Then, 10 mL of a 5 M aqueous NaOH solution was added slowly to the mixture while everything was stirred.
    30 vigorously with a magnetic bar. Finally, the mixture was filtered under vacuum, obtaining a dark material that was washed with distilled water, ethanol and dried in an oven at 100 ° C. The sample was analyzed by scanning electron microscopy (SEM), using 5 mg of material without modification. The image is shown in Figure 8.
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    权利要求:
    Claims (1)
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    类似技术:
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    同族专利:
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    JP2021521091A|2021-08-26|
    WO2019206989A1|2019-10-31|
    EP3784622A1|2021-03-03|
    US20210130172A1|2021-05-06|
    ES2678419B2|2018-11-29|
    KR20210003733A|2021-01-12|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    WO2015044478A1|2013-09-24|2015-04-02|Consejo Superior De Investigaciones Científicas |Exfoliation of graphite with deep eutectic solvents|
    KR101286106B1|2011-05-30|2013-07-16|한국과학기술연구원|The method for producing graphene by chemical exfoliation|
    CN105289515B|2015-11-27|2018-04-13|安徽师范大学|A kind of preparation method and application of magnetic oxygenated graphene sorbent material|
    法律状态:
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    优先权:
    申请号 | 申请日 | 专利标题
    ES201830402A|ES2678419B2|2018-04-25|2018-04-25|METHOD OF OBTAINING NANOMATERIALS COMPOSITES OF CARBON MATERIAL AND METAL OXIDES|ES201830402A| ES2678419B2|2018-04-25|2018-04-25|METHOD OF OBTAINING NANOMATERIALS COMPOSITES OF CARBON MATERIAL AND METAL OXIDES|
    KR1020207027704A| KR20210003733A|2018-04-25|2019-04-24|Method for obtaining nanomaterials composed of carbonaceous materials and metal oxides|
    US17/049,837| US20210130172A1|2018-04-25|2019-04-24|Method of obtainment of nanomaterials composed of carbonaceous material and metal oxides|
    CN201980028181.XA| CN112041266A|2018-04-25|2019-04-24|Method for obtaining nano material composed of carbon-containing material and metal oxide|
    EP19720819.2A| EP3784622A1|2018-04-25|2019-04-24|Method of obtainment of nanomaterials composed of carbonaceous material and metal oxides|
    JP2020556857A| JP2021521091A|2018-04-25|2019-04-24|How to obtain nanomaterials composed of carbonaceous substances and metal oxides|
    PCT/EP2019/060500| WO2019206989A1|2018-04-25|2019-04-24|Method of obtainment of nanomaterials composed of carbonaceous material and metal oxides|
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