CN115849344B - Simultaneous preparation of two differently sized and self-separating fullerenes C 60 Method for preparing nano rod - Google Patents
Simultaneous preparation of two differently sized and self-separating fullerenes C 60 Method for preparing nano rod Download PDFInfo
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- CN115849344B CN115849344B CN202211479153.XA CN202211479153A CN115849344B CN 115849344 B CN115849344 B CN 115849344B CN 202211479153 A CN202211479153 A CN 202211479153A CN 115849344 B CN115849344 B CN 115849344B
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- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000002073 nanorod Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 229910003472 fullerene Inorganic materials 0.000 claims abstract description 66
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002904 solvent Substances 0.000 claims abstract description 40
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002244 precipitate Substances 0.000 claims abstract description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 8
- 238000001338 self-assembly Methods 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- MARCAKLHFUYDJE-UHFFFAOYSA-N 1,2-xylene;hydrate Chemical compound O.CC1=CC=CC=C1C MARCAKLHFUYDJE-UHFFFAOYSA-N 0.000 description 1
- -1 biomedicine Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for simultaneously preparing two fullerene C with different sizes and self-separation 60 The method for preparing the nanorods comprises the following steps: fullerene C 60 Dissolving in meta-xylene to obtain fullerene C 60 Meta-xylene solution of (2); will H 2 O, N and N-dimethylformamide and isopropanol to obtain fullerene C 60 Is a poor solvent of (a); addition of Fullerene C to poor solvent 60 Adding isopropanol to the interface of the two solutions, immediately turning the solution into turbidity and generating precipitates, standing, layering the precipitates, concentrating at the bottom and the upper part of the solution, and separating the precipitates at the two different positions to obtain fullerene C with two different sizes 60 A nanorod. The invention successfully prepares two kinds of high-quality C by controlling the concentration of the fullerene solution, the step of adding the liquid and other conditions 60 The nano rod has the characteristics of simple preparation method, easy operation and high efficiency.
Description
Technical Field
The invention belongs to the field of preparation and development of fullerene self-assembled structures, and particularly relates to a method for simultaneously preparing two fullerene C with different sizes and self-separation 60 A method for preparing a nano rod.
Background
The related performance of the device of the fullerene material is not only related to the intrinsic characteristic of the fullerene, but also is inseparable from the morphology of the fullerene, and the fullerene structure with fixed morphology such as fullerene nanorods, fullerene nanotubes, fullerene micro-cubes and the like is proved to have development and application potential in the aspects of optics, electricity, electrochemistry, nanomaterials, biomedicine, chemical catalysis and the like. Therefore, the method for preparing the high-quality fullerene micro-nano structure by developing the simple and effective method has very important effect on expanding and developing the application of the fullerene. After decades of research, the current methods for preparing fullerenes are: liquid-liquid interface self-assembly, gas-liquid-solid interface self-assembly, gas-solid interface self-assembly, vacuum solid interface self-assembly, and the like. The two methods of gas-solid interface self-assembly and vacuum solid interface self-assembly are unfavorable for further utilization of fullerene materials due to the fact that complicated instrument and equipment processes and the like are needed. The self-assembly of the liquid-liquid interface and the self-assembly of the gas-liquid-solid interface are independent of equipment, the preparation process is simple and convenient, and the prepared fullerene self-assembled structure has various and adjustable morphology and is widely focused by researchers. Wherein the liquid-liquid interface method is to make fullerene C 60 Fullerene C formed by dissolving in good solvent (such as toluene, benzene, carbon tetrachloride and carbon disulfide) 60 The solution is then formed into an interface with a poor solvent for the fullerene (e.g., methanol, ethanol, isopropanol, t-butanol, etc.), and the fullerene molecules are supersaturated at the interface to nucleate and crystallize. The liquid-liquid interface method can effectively regulate the morphology of the fullerene self-assembled structure by regulating and controlling the types of the fullerene good solvent and the poor solvent, the concentration of the fullerene solution, the ratio of the fullerene solution to the poor solvent and external conditions such as illumination and temperature. For example, when a reagent such as toluene or meta-xylene is used as a good solvent, fullerene C 60 Tends to form one-dimensional nanorods or nanotubesC when carbon tetrachloride is used as a good solvent 60 Tends to form two-dimensional nano-platelet structures.
When a liquid-liquid interface method is adopted, the prepared one-dimensional nanorod structure generally has the condition of nonuniform shape and size, for example, the distribution of the length and the diameter is wider, and the preparation of a high-precision device is not easy; most of the liquid-liquid interface methods can only prepare one sample, limiting the diversity of the method.
Disclosure of Invention
In view of the shortcomings of the prior art, the invention aims to provide a method for simultaneously preparing two fullerene C with different sizes and self-separation 60 Method for preparing nano rod, and two kinds of prepared fullerene C 60 The nanorod size distribution is uniform, which is beneficial to the preparation of high-precision nano devices.
In order to achieve the above purpose, the invention adopts the following technical scheme:
simultaneously preparing two fullerene C with different sizes and self-separation 60 A method of nanorods, comprising the steps of:
(1) Preparation of Fullerene C 60 The concentration of the meta-xylene solution is 0.75-1.75mg/ml: proper amount of fullerene C 60 The powder was added to 50ml of meta-xylene solvent and sonicated for 30 minutes.
(2) Preparing mixed poor solvent: will first H 2 O, N mixing N-dimethylformamide and isopropanol at a volume ratio of 1:1:1 to obtain fullerene C 60 Is a poor solvent of (a). The poor solvent is insoluble in water and meta-xylene, so that the poor solvent and fullerene C can be reacted 60 Forming a layered state upon initial contact of the meta-xylene solution of (2); the density of the poor solvent can be regulated and controlled to a certain extent by the N, N-dimethylformamide; the main function of isopropanol is to promote the growth of fullerene nanorods.
(3) The preparation process comprises the following steps: 2ml of Fullerene C 60 Is added into a 10ml clean glass bottle, and then 1ml fullerene C is added 60 In which fullerene C is visible 60 Is insoluble in the meta-xylene solution and poor solvent, and is formed at the contact pointForming an interface; then adding 1ml of isopropanol at the interface of the two solutions, wherein the isopropanol can form supersaturation with the fullerene solution to promote nucleation and growth of the fullerene nanorods, the solution becomes turbid immediately, precipitates appear, the precipitates are layered and respectively concentrated at the bottom and the upper part of the solution after standing, and the precipitates at the two positions are separated to obtain fullerene C with two different sizes 60 A nanorod.
Compared with the prior art, the invention has the beneficial effects that:
the invention prepares fullerene C respectively 60 Meta-xylene solution, mixed poor solvent, and then fullerene C 60 Adding meta-xylene solution into poor solvent, adding isopropanol at interface, standing for separation to obtain fullerene C with two different sizes 60 A nanorod. The invention successfully prepares two kinds of high-quality C by controlling the conditions of the concentration of the fullerene solution (the excessive concentration or the insufficient concentration of the fullerene solution can cause layering failure or only one structure, the isopropanol solvent around the fullerene with excessive concentration is too little, the fullerene molecules are too aggregated, the growth is blocked to easily generate only one structure, the subsequent continuous growth of the fullerene molecules is reduced due to the small concentration of the fullerene, the subsequent growth of the fullerene is not facilitated), the step of adding liquid and the like 60 The nanorods have the characteristics of simple preparation method, easy operation and high efficiency; and two kinds of prepared fullerene C 60 The nanorod size distribution is uniform, which is beneficial to the preparation of high-precision nano devices.
Drawings
FIG. 1 shows the simultaneous preparation of two fullerenes C of different sizes in example 1 of the present invention 60 A process map of the nanorods;
FIG. 2 shows two fullerene C of different sizes 60 SEM images of nanorods at different magnifications;
FIG. 3 is a schematic diagram showing the preparation of fullerene C in comparative example 1 60 A process map of the nanorods;
FIG. 4 is a schematic diagram showing the preparation of fullerene C in comparative example 2 60 Process diagram of nanorods.
Detailed Description
The present invention will be further described with reference to examples, which are not intended to be limiting, so that those skilled in the art will better understand the present invention and practice it.
In addition, the preparation processes in the following examples are conventional means in the art unless specifically described, and therefore, will not be described in detail; the raw materials used in the following experiments are all commercially available products and are commercially available.
Examples
Simultaneously preparing two fullerene C with different sizes and self-separation 60 A method of nanorods, comprising the steps of:
(1) Preparation of Fullerene C 60 M-xylene solution of (c): 62.5mg of Fullerene C 60 Adding the powder into 50ml of meta-xylene solvent, and performing ultrasonic treatment for 30 minutes to obtain fullerene C 60 Meta-xylene solution of (2).
(2) Preparing mixed poor solvent: will H 2 O, N and mixing N-dimethylformamide and isopropanol at a volume ratio of 1:1:1 to obtain fullerene C 60 Is a poor solvent of (a).
(3) The preparation process comprises the following steps: 4ml of Fullerene C 60 Is added into a 10ml clean glass bottle, and then 1ml fullerene C is added 60 In which fullerene C is visible 60 The meta-xylene solution and the poor solvent are not dissolved each other, and an interface is formed at a position where they are contacted as shown in fig. 1 (a). Subsequently 1ml of isopropanol solvent was added at their interface, at which point the solution turned immediately turbid with the appearance of a precipitate, as shown in fig. 1 (b); standing for 24 hr, layering and concentrating at the bottom and upper part of the solution respectively, as shown in figure 1 (C), separating the precipitate at the two different positions to obtain fullerene C with two different sizes 60 A nanorod.
Characterization of these two precipitates to analyze the differences and formation mechanism of the two precipitates, FIG. 2 (a, b) is an SEM image of the upper layer of precipitates, which is seen to be a one-dimensional nanorod structure, which was flattened by statisticsAnd has a mean diameter of about 230nm and a length of several tens to several hundreds of micrometers. Fig. 2 (c, d) is an SEM image of the underlying precipitate, which is also seen to be a one-dimensional nanorod structure, but of different dimensions, with an average diameter of about 986nm and an average length of about 14.93 μm by statistics. From this set of data, it can be analyzed that the nanorods on the upper layer are elongated while the precipitates on the lower layer are coarse and short. In conclusion, the method provided by the invention successfully obtains the fullerene C with two different sizes at the same time 60 Nanorods, and fullerene C of two different sizes 60 The nanorods are respectively gathered at different positions in the reaction solution due to the difference of structures, and are in a self-separation state, so that the nanorods are convenient to separate and treat respectively, the preparation process is simple, and the operation is easy.
Comparative example 1:
(1) Preparation of Fullerene C 60 M-xylene solution of (c): 62.5mg of Fullerene C 60 Adding the powder into 50ml of meta-xylene solvent, and performing ultrasonic treatment for 30 minutes to obtain fullerene C 60 Meta-xylene solution of (2).
(2) Preparing mixed poor solvent: will H 2 Mixing O and isopropanol in the volume ratio of 1:1 to obtain fullerene C 60 Is a poor solvent of (a).
(3) The preparation process comprises the following steps: 4ml of Fullerene C 60 Is added into a 10ml clean glass bottle, and then 1ml fullerene C is added 60 As in fig. 3 (a). Subsequently 1ml of isopropanol solvent was added at their interface and after standing for 24 hours the precipitate did not delaminate only at the bottom of the solution, with a small amount of unassembled fullerene solution on top.
The comparative example differs from the example in that: n, N-dimethylformamide was not added to the poor solvent.
Comparative example 2
(1) Preparation of Fullerene C 60 M-xylene solution of (c): 200mg of Fullerene C 60 Adding the powder into 50ml of meta-xylene solvent, and performing ultrasonic treatment for 30 minutes to obtain fullerene C 60 Meta-xylene solution of (2).
(2) Preparation of Mixed poor solvent: will H 2 O, N and mixing N-dimethylformamide and isopropanol at a volume ratio of 1:1:1 to obtain fullerene C 60 Is a poor solvent of (a).
(3) The preparation process comprises the following steps: 4ml of Fullerene C 60 Is added into a 10ml clean glass bottle, and then 1ml fullerene C is added 60 In which fullerene C is visible 60 The meta-xylene solution and the poor solvent are not dissolved each other, and an interface is formed at a position where they are contacted as shown in fig. 4 (a). Subsequently, 1ml of isopropanol solvent was added at their interface, and after 24 hours of standing, the precipitate was mostly concentrated at the bottom of the bottle, and no significant delamination occurred.
The comparative example differs from the example in that: fullerene C 60 The concentration of meta-xylene is different.
It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (4)
1. Simultaneously preparing two fullerene C with different sizes and self-separation 60 A method of nanoroding, characterized by: the method comprises the following steps:
(1) Fullerene C 60 Dissolving in meta-xylene to obtain fullerene C 60 Meta-xylene solution of (2); the fullerene C 60 Fullerene C in meta-xylene solution 60 The concentration of (2) is 0.75-1.75mg/ml;
(2) Will H 2 O, N and N-dimethylformamide and isopropanol to obtain fullerene C 60 Is a poor solvent of (a); the fullerene C 60 H in poor solvent of (C) 2 O, N the volume ratio of N-dimethylformamide to isopropanol is 1:1:1;
(3) Adding fullerene C to the poor solvent 60 Due to fullerene C 60 Is incompatible with poor solvents, forms an interface at the location where they contactThe method comprises the steps of carrying out a first treatment on the surface of the Adding isopropanol to the interface, immediately turning the solution into turbid and generating precipitate, standing, layering the precipitate, concentrating at the bottom and upper part of the solution, and separating the precipitate at the two different positions to obtain fullerene C with two different sizes 60 A nanorod;
in step (3), fullerene C is added to the poor solvent 60 Poor solvent and fullerene C in meta-xylene solution 60 The volume ratio of the meta-xylene solution is 2:1.
2. Simultaneous preparation of two differently sized and self-separating fullerenes C according to claim 1 60 A method of nanoroding, characterized by: in step (1), fullerene C 60 Fullerene C is treated by ultrasound while dissolved in meta-xylene 60 Uniformly dispersed in meta-xylene.
3. Simultaneous preparation of two differently sized and self-separating fullerenes C according to claim 2 60 A method of nanoroding, characterized by: the time of the ultrasonic treatment is 20-40 minutes.
4. Simultaneous preparation of two differently sized and self-separating fullerenes C according to claim 1 60 A method of nanoroding, characterized by: in the step (3), the standing time is 12-48h.
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