CN110016712B - Fullerene C70-calixarene host-guest composite nanocrystalline material and preparation method thereof - Google Patents
Fullerene C70-calixarene host-guest composite nanocrystalline material and preparation method thereof Download PDFInfo
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- CN110016712B CN110016712B CN201910338172.2A CN201910338172A CN110016712B CN 110016712 B CN110016712 B CN 110016712B CN 201910338172 A CN201910338172 A CN 201910338172A CN 110016712 B CN110016712 B CN 110016712B
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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 40
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 239000002707 nanocrystalline material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 23
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 239000012716 precipitator Substances 0.000 claims abstract description 8
- 239000007791 liquid phase Substances 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims abstract description 6
- VTJUKNSKBAOEHE-UHFFFAOYSA-N calixarene Chemical compound COC(=O)COC1=C(CC=2C(=C(CC=3C(=C(C4)C=C(C=3)C(C)(C)C)OCC(=O)OC)C=C(C=2)C(C)(C)C)OCC(=O)OC)C=C(C(C)(C)C)C=C1CC1=C(OCC(=O)OC)C4=CC(C(C)(C)C)=C1 VTJUKNSKBAOEHE-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 43
- 239000000243 solution Substances 0.000 claims description 31
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 29
- 239000013078 crystal Substances 0.000 claims description 22
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 8
- 239000012452 mother liquor Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000010413 mother solution Substances 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 239000012047 saturated solution Substances 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 16
- 150000001875 compounds Chemical class 0.000 abstract description 9
- 238000001338 self-assembly Methods 0.000 abstract description 3
- 239000002159 nanocrystal Substances 0.000 description 13
- 239000002245 particle Substances 0.000 description 10
- OLZFZIXORGGLLS-UHFFFAOYSA-N 4-tert-butylcalix[8]arene Chemical compound C1C(C=2O)=CC(C(C)(C)C)=CC=2CC(C=2O)=CC(C(C)(C)C)=CC=2CC(C=2O)=CC(C(C)(C)C)=CC=2CC(C=2O)=CC(C(C)(C)C)=CC=2CC(C=2O)=CC(C(C)(C)C)=CC=2CC(C=2O)=CC(C(C)(C)C)=CC=2CC(C=2O)=CC(C(C)(C)C)=CC=2CC2=CC(C(C)(C)C)=CC1=C2O OLZFZIXORGGLLS-UHFFFAOYSA-N 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 239000008204 material by function Substances 0.000 description 6
- 229920006395 saturated elastomer Polymers 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000002135 nanosheet Substances 0.000 description 3
- 229920000858 Cyclodextrin Polymers 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- OOXWYYGXTJLWHA-UHFFFAOYSA-N cyclopropene Chemical compound C1C=C1 OOXWYYGXTJLWHA-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 150000004032 porphyrins Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- FHCPAXDKURNIOZ-UHFFFAOYSA-N tetrathiafulvalene Chemical compound S1C=CSC1=C1SC=CS1 FHCPAXDKURNIOZ-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/54—Organic compounds
- C30B29/58—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
- C30B7/06—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using non-aqueous solvents
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Abstract
The invention belongs to compound functionsThe technical field of material preparation, in particular to fullerene C70A calixarene host-guest composite nanocrystalline material and a preparation method thereof. The invention uses pure fullerene C70Raw powder and p-tert-butyl cup [8]]Aromatic hydrocarbon is taken as a raw material; aromatic hydrocarbon is taken as a solvent; isopropanol is used as a precipitator; the composite nanocrystalline with the host-guest structure is prepared by a liquid phase deposition method. The method provided by the invention is simple in process, and can realize effective regulation and control of the shape of the fullerene-calixarene host-guest composite nanocrystalline in the self-assembly process and improve the crystallinity.
Description
Technical Field
The invention belongs to the technical field of preparation of composite functional materials, and particularly relates to fullerene C with different compositions and shapes70A method for preparing a host-guest compound nanocrystalline material.
Background of the invention is described.
Fullerenes are a class of pure carbon cage-like structure materials first discovered by scientists such as Kroto (Nature, Vol.318,162,1985) in 1985, and then improved and mass-produced by scientists such as Kratschmer (Nature, Vol.347, 354, 1990). In the fullerene family C60And C70Are the two most readily available and most abundant members, and as semiconductor materials, have excellent properties such as photophysics, photoconductions, superconductivity, super-hard properties, and the like. Materials composed of fullerene molecules, especially nanomaterials with different dimensions, have great potential application values in the fields of functional materials and nano devices. Therefore, the synthesis of the fullerene-based nanocrystalline material, and the optimization of the structure and performance thereof become the hot spots and the efforts of scientific research.
The current reports on the preparation of fullerene nanocrystals relate to the preparation of fullerenes from pure fullerene (C)60/C70) Constituent nanomaterials, or solvated fullerene nanocrystalline materials. Compared with the original fullerene material, the materials have novel structures and properties, but have limited regulation and control capability on the fullerene crystal structure and properties, and cannot meet the requirements in actual life and production.
The preparation of host-guest materials based on the large-cavity molecular host materials is always considered to be an effective way for forming new-structure functional materials with new properties. The previous researches find that when fullerene molecules are combined with macrocyclic organic molecules (such as cyclodextrin, cyclopropene, calixarene and the like), a special host-guest compound polymer structure can be formed, and the method has guiding significance for the design of functional materials. However, the synthesis and control of host-guest nanocrystals of fullerene groups have been reported and remain challenging technical challenges.
Through investigation, no report about a mature method for synthesizing the fullerene-based host-guest structure nanocrystalline material is found. The synthesis processes for fullerene-based host-guest materials found so far fall into two categories: the small molecule pi electron-rich compound and the large ring main body form a self-assembly form to form supermolecular assembly with fullerene molecules. Previous studies reported that compounds such as: mixing small-molecule pi system compounds such as ferrocene, porphyrin and tetrathiafulvalene with a fullerene material to prepare a solution, and obtaining a host-guest supramolecular material with a host-guest structure by a method of volatilizing the mixed solution; the solution volatilization method is also used in the preparation of host-guest complexes of macrocyclic molecules (cyclodextrin, calixarene, azacalixarene, etc.) with fullerene molecules.
The existing solution volatilization method can obtain a fullerene-based host-guest material at a powder level, cannot control the crystallinity of a composite nano material and cannot control the morphology of the material, and the physicochemical characteristics of the composite nano material are influenced, so that the application of the composite nano material in the fields of micro-nano devices and functional materials is limited. Related researches accumulate and develop a plurality of main molecules and develop a plurality of novel supermolecular structures. The discovery of the research results inspires the potential application exploration of the fullerene-based host-guest materials in the aspects of biology, fine chemistry and military industry. In particular, the development of a widely recognized nano-crystalline material in this century is considered to be an essential means for a fullerene-based material as a micro-nano device and a functional material. Although no method for effectively synthesizing the fullerene-based host-guest nanocrystalline material is found in the existing method, the importance of the form of the fullerene aggregate in the application of high-tech functional materials is explained.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention obtains the fullerene C with high crystallinity and nanometer size by using a liquid phase treatment method70Calixarene fullerene nanocrystals.
Fullerene C70Preparation method of-calixarene host-guest composite nanocrystalline material using pure fullerene C70Raw powder and p-tert-butyl cup [8]]Aromatic hydrocarbon is taken as a raw material; aromatic hydrocarbon is taken as a solvent; isopropanol is used as a precipitator; preparing host and guest by liquid phase depositionStructurally compounded with nanocrystals.
Further, the aromatic hydrocarbon is benzene or toluene.
More specifically, the preparation method of the host-guest structure composite nanocrystal comprises the following steps:
s1, adding excessive C70Putting the powder into benzene or toluene solvent and carrying out ultrasonic oscillation, then standing the solution until excessive C is obtained70After the powder is completely precipitated, removing the upper saturated solution to obtain mother liquor A;
s2, putting excessive para-tert-butylcalix [8] arene powder into a benzene or toluene solvent, performing ultrasonic oscillation, standing the solution, and removing an upper saturated solution to obtain a mother solution B after the excessive para-tert-butylcalix [8] arene is completely precipitated;
s3, mixing the mother liquor A and the mother liquor B in a ratio of 1:1 volume ratio, and carrying out ultrasonic treatment for 1-2 minutes;
s4, adding isopropanol serving as a precipitator into the mixed solution, adding isopropanol with the volume being 10 times that of the mother solution A, performing ultrasonic treatment for 1-2 minutes, and standing at room temperature for 10-20 hours;
since isopropanol plays a role in the present invention to control complex nanocrystal formation and deposition, the isopropanol volume to solution volume ratio is critical in controlling the rate of nanocrystal formation and control of nanocrystal shape in experiments. The inventor finds that fullerene C with high crystallinity and regular appearance can be obtained when the volume of the added isopropanol is 10 times of that of mother liquor A70-the most suitable ratio of calixarene host-guest composite nanocrystals.
S5, sucking out the lower layer precipitate, dripping the lower layer precipitate onto a clean substrate, and naturally volatilizing the solvent and the precipitating agent to obtain a spherical C70-p-tert-butyl cup [8]]An aromatic hydrocarbon host-guest structure nano-particle crystal material;
s6, C obtained in the step S570-p-tert-butyl cup [8]]The nano-sheet crystal with the aromatic hydrocarbon host-guest structure is 10-4Pa-10-3Heating at 100-120 deg.C under Pa pressure for 2-3 hr to remove solvent and deposition agent molecules remained in the crystal to obtain fullerene C70-Para-tert-butyl cup [8]]Single crystals of aromatic host-guest nanoparticles, also known as Fullerene C70Calixarene mainA guest composite nanocrystalline material.
Fullerene C70-Para-tert-butyl cup [8]]Aromatic hydrocarbon host-guest compound nanocrystalline C70And p-tert-butyl cup [8]]The aromatics were composed in a 2:1 molar ratio. Wherein the fullerene molecule C70And p-tert-butyl cup [8]]The aromatic hydrocarbon molecules are coated and combined by van der Waals force to form a structural unit as a composition element. C70-p-tert-butyl cup [8]]The arene composite nanometer particle is in a nanometer spherical shape, and the diameter of the arene composite nanometer particle is 30nm-60 nm.
The invention provides a preparation method of a fullerene-calixarene host-guest compound nanocrystalline material. The rich fullerene C is obtained by regulating and controlling the crystal structure and the crystal shape by the selection of the host-guest component proportion and the solvent through a liquid phase deposition method for the first time70-p-tert-butyl cup [8]]An aromatic hydrocarbon host-guest compound nanocrystalline material. By adopting a liquid phase deposition method, the fast synthesis of the host-guest structure material of fullerene-calixarene and the regulation and control of the shape and the crystal structure of the nanocrystalline can be realized. The isopropanol is used as a liquid phase precipitator, so that the composite material can be quickly formed into a nano crystal material in a solution and can be quickly deposited, and the shape of the nano crystal can be controlled. The method provided by the invention is simple in process, and can realize effective regulation and control of the shape of the fullerene-calixarene host-guest composite nanocrystalline in the self-assembly process and improve the crystallinity.
Drawings
FIG. 1C obtained using benzene as organic solvent70-Para-tert-butyl cup [8]]TEM pictures of the aromatic hydrocarbon host-guest nano single crystal particles;
FIG. 2C obtained using benzene as organic solvent70-p-tert-butyl cup [8]]XRD diffraction picture of nano single crystal particles of aromatic host object.
Detailed Description
The invention will be further described in the following with reference to the drawings and specific examples, which are not intended to limit the scope of the invention.
Example 1
S1, adding excessive C70Putting the powder into benzene, performing ultrasonic treatment for 1-2 minutes, standing the solution at room temperature for 2-5 hours,c to be excessive70After complete precipitation, the upper solution is removed, and the solution is saturated C70Benzene solution;
s2, putting excessive p-tert-butylcalix [8] arene powder into benzene, performing ultrasonic treatment for 1-2 minutes, standing the solution at room temperature for 2-5 hours, and removing the upper-layer solution after excessive p-tert-butylcalix [8] arene is completely precipitated, wherein the solution is a saturated p-tert-butylcalix [8] arene benzene solution;
s3, using a pipette to mix the prepared saturated C70Benzene solution and p-tert-butylcalix [8]]Mixing aromatic benzene solution in a volume ratio of 1:1, and performing ultrasonic treatment for 1-2 minutes;
s4, adding isopropanol serving as a precipitator into the mixed solution by using a pipette, wherein the volume of the added isopropanol is saturated C 7010 times of benzene solution, performing ultrasonic treatment for 1-2 minutes, and standing for 10-20 hours at room temperature;
s5, sucking out the precipitate of the middle and lower layers of the reaction vessel by using a rubber head dropper, dropping the precipitate onto a clean substrate, and obtaining a spherical C after the solvent and the precipitating agent are naturally volatilized70-Para-tert-butyl cup [8]]An aromatic hydrocarbon host-guest structure nano crystal particle material;
s6, C obtained in the step S570-Para-tert-butyl cup [8]]Pressure of nano-sheet crystal particle with aromatic hydrocarbon host-guest structure is 5x10-4Heating at 100 deg.C under Pa for 2-3 hr to remove solvent and precipitant molecules remained in the crystal to obtain C with simple cubic crystal structure70-Para-tert-butyl cup [8]]Aromatic host-guest nano single crystal particles, wherein the component C70And p-tert-butyl cup [8]]The aromatic hydrocarbon molar ratio is 2: 1.
example 2
S1, adding excessive C70Putting the powder into toluene and performing ultrasonic treatment for 1-2 min, standing the solution at room temperature for 2-5 hr until excessive C is obtained70After complete precipitation, the upper solution is removed, and the solution is saturated C70A toluene solution;
s2, putting excessive p-tert-butylcalix [8] arene powder into toluene, carrying out ultrasonic treatment for 1-2 minutes, standing the solution at room temperature for 2-5 hours, and removing the upper-layer solution after excessive p-tert-butylcalix [8] arene is completely precipitated, wherein the solution is a saturated p-tert-butylcalix [8] arene toluene solution;
s3, using a pipette to mix the prepared saturated C70Toluene solution and p-tert-butylcalix [8]]Mixing aromatic toluene solution in a volume ratio of 1:1, and performing ultrasonic treatment for 1-2 minutes;
s4, adding isopropanol serving as a precipitator into the mixed solution by using a pipette, wherein the volume of the added isopropanol is saturated C 7010 times of toluene solution, performing ultrasonic treatment for 1-2 minutes, and standing for 10-20 hours at room temperature;
s5, sucking out the precipitate of the middle and lower layers of the reaction vessel by using a rubber head dropper, dropping the precipitate onto a clean substrate, and obtaining a spherical C after the solvent and the precipitating agent are naturally volatilized70-Para-tert-butyl cup [8]]An aromatic hydrocarbon host-guest structure nano crystal particle material;
s6, C obtained in the step S570-Para-tert-butyl cup [8]]Pressure of nano-sheet crystal particle with aromatic hydrocarbon host-guest structure is 5x10-4Heating at 100 deg.C under Pa for 2-3 hr to remove residual solvent and precipitant molecules in the crystal to obtain C with cubic crystal structure70-Para-tert-butyl cup [8]]Aromatic host-guest nano single crystal particles, wherein the component C70And p-tert-butyl cup [8]]The aromatic hydrocarbon molar ratio is 2: 1.
the above description is only for the purpose of creating a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (1)
1. Fullerene C70The preparation method of the-calixarene host-guest composite nanocrystalline material is characterized in that pure fullerene C is used70Raw powder and p-tert-butyl cup [8]]Aromatic hydrocarbon is taken as a raw material; benzene or toluene is used as a solvent; isopropanol is used as a precipitator; the composite nanocrystalline with the host-guest structure is prepared by a liquid phase deposition method, and the preparation method comprises the following steps:
s1, adding excessive C70Adding the powder into benzene or tolueneDissolving in solvent, ultrasonic vibrating, standing to remove excessive C70After the powder is completely precipitated, removing the upper saturated solution to obtain mother liquor A;
s2, putting excessive para-tert-butylcalix [8] arene powder into a benzene or toluene solvent, performing ultrasonic oscillation, standing the solution, and removing an upper saturated solution to obtain a mother solution B after the excessive para-tert-butylcalix [8] arene is completely precipitated;
s3, mixing the mother liquor A and the mother liquor B in a ratio of 1:1 volume ratio, and carrying out ultrasonic treatment for 1-2 minutes;
s4, adding isopropanol serving as a precipitator into the mixed solution, adding isopropanol with the volume being 10 times that of the mother solution A, performing ultrasonic treatment for 1-2 minutes, and standing at room temperature for 10-20 hours;
s5, sucking out the lower layer precipitate, dripping the lower layer precipitate onto a clean substrate, and naturally volatilizing the solvent and the precipitating agent to obtain a spherical C70-p-tert-butyl cup [8]]An aromatic hydrocarbon host-guest structure nano-particle crystal material;
s6, C obtained in the step S570-p-tert-butyl cup [8]]The aromatic hydrocarbon host-guest structure nano-particle crystal material is 10-4Pa-10-3Heating at 100-120 deg.C under Pa pressure for 2-3 hr to remove solvent and precipitant molecules in the crystal to obtain fullerene C70-single crystals of calixarene host-guest nanoparticles.
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