CN110015652A - Fullerene C20-calixarenes Subjective and Objective composite nanocrystalline material and preparation method thereof - Google Patents
Fullerene C20-calixarenes Subjective and Objective composite nanocrystalline material and preparation method thereof Download PDFInfo
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- CN110015652A CN110015652A CN201910338388.9A CN201910338388A CN110015652A CN 110015652 A CN110015652 A CN 110015652A CN 201910338388 A CN201910338388 A CN 201910338388A CN 110015652 A CN110015652 A CN 110015652A
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- butyl
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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 34
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002707 nanocrystalline material Substances 0.000 title claims abstract description 13
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 47
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 32
- 230000001376 precipitating effect Effects 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 11
- 230000008021 deposition Effects 0.000 claims abstract description 11
- 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 41
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 25
- 239000013078 crystal Substances 0.000 claims description 12
- 239000012452 mother liquor Substances 0.000 claims description 11
- 238000002604 ultrasonography Methods 0.000 claims description 11
- 230000015572 biosynthetic process Effects 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
- 239000002178 crystalline material Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000012047 saturated solution Substances 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- VTJUKNSKBAOEHE-UHFFFAOYSA-N calixarene Chemical class 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 description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000005411 Van der Waals force Methods 0.000 claims description 2
- 238000005253 cladding Methods 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 31
- 239000007791 liquid phase Substances 0.000 abstract description 5
- 125000003342 alkenyl group Chemical group 0.000 description 6
- 235000015895 biscuits Nutrition 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229920000858 Cyclodextrin Polymers 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 229920006395 saturated elastomer Polymers 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- -1 azepine calixarenes Chemical class 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design 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
- 150000002678 macrocyclic compounds Chemical class 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- RKCAIXNGYQCCAL-UHFFFAOYSA-N porphin Chemical compound N1C(C=C2N=C(C=C3NC(=C4)C=C3)C=C2)=CC=C1C=C1C=CC4=N1 RKCAIXNGYQCCAL-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007614 solvation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- FHCPAXDKURNIOZ-UHFFFAOYSA-N tetrathiafulvalene Chemical compound S1C=CSC1=C1SC=CS1 FHCPAXDKURNIOZ-UHFFFAOYSA-N 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Classifications
-
- 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
- C01B32/152—Fullerenes
- C01B32/156—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C13/00—Cyclic hydrocarbons containing rings other than, or in addition to, six-membered aromatic rings
- C07C13/28—Polycyclic hydrocarbons or acyclic hydrocarbon derivatives thereof
- C07C13/32—Polycyclic hydrocarbons or acyclic hydrocarbon derivatives thereof with condensed rings
- C07C13/70—Polycyclic hydrocarbons or acyclic hydrocarbon derivatives thereof with condensed rings with a condensed ring system consisting of at least two, mutually uncondensed aromatic ring systems, linked by an annular structure formed by carbon chains on non-adjacent positions of the aromatic ring, e.g. cyclophanes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2603/00—Systems containing at least three condensed rings
- C07C2603/92—Systems containing at least three condensed rings with a condensed ring system consisting of at least two mutually uncondensed aromatic ring systems, linked by an annular structure formed by carbon chains on non-adjacent positions of the aromatic system, e.g. cyclophanes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of composite functional material preparation, in particular to fullerene C60Calixarenes Subjective and Objective composite nanocrystalline material and preparation method thereof.The present invention is with pure fullerene C60Original powder and to tert-butyl-calix [8] aromatic hydrocarbons be raw material；Using aromatic hydrocarbon as solvent；Using isopropanol as precipitating reagent；It is nanocrystalline using liquid phase deposition preparation Subjective and Objective structure composite.Method provided by the invention not only simple process but also can be realized fullerene-calixarenes Subjective and Objective composite nanocrystalline in self assembling process, to the Effective Regulation of shape, improve crystallinity.
Description
Technical field
The invention belongs to the technical field of composite functional material preparation, in particular to the fullerene C of different compositions and shape60
The preparation method of host-guest complex nanocrystalline material.
Background technique
Fullerene is the research discovery first in 1985 by scientists such as Kroto (Nature, Vol.318,162,1985)
The pure carbon cage structure material of one kind, improved later by the scientists such as Kratschmer (Nature, Vol.347,354,1990)
And mass production.The C in fullerene family60And C70It is most easily to obtain and highest two members of abundance, with being used as semiconductor material
Material has the excellent characteristics such as optical physics, light guide, superconductivity, superhard characteristic.The material being made of fullerene molecule, especially
The nano material of its different dimensions, in functional material and field of nanometer devices, there is huge potential using values.Therefore rich
The optimization of the synthesis and its structure and performance of strangling alkenyl nanocrystalline material becomes the hot spot and striving direction of scientific research.
It is mostly at present about by pure fullerene (C about the report of the nanocrystalline preparation of fullerene60/C70) constitute nanometer material
The fullerene nanocrystalline material of material or solvation.These materials relative to original fullerene-based material, with novel structure and
Performance, but, the demand that is unable to satisfy in real life and production limited to the ability of regulation and control of fullerene crystal structure and performance.
The preparation of Subjective and Objective material based on macroscopic-void molecular bulk material, have always been considered as be capable of forming new construction,
The effective way of new property functional material.The research discovery of forefathers is when fullerene molecule and big ring organic molecule (such as cyclodextrin, ring
Propylene, calixarenes etc.) it combines, it is capable of forming the design with special Subjective and Objective composite high-molecular structure, for functional material
With directive significance.However, the synthesis and control nanocrystalline for the Subjective and Objective of fowler alkenyl is also rarely reported, being still has
The technical problem of challenge.
Through investigating, the report of the maturation method about fowler alkenyl Subjective and Objective structure nano crystalline substance materials synthesis is not found also.
The synthesis technology of the fowler alkenyl Subjective and Objective material found so far is divided into two classes: small molecule richness pi-electron compound and big ring
Main body self assembly form and fullerene molecule form Supramolecular Assembling.It is reported in the research of forefathers, it will such as: ferrocene, porphin
The small molecules such as quinoline, tetrathiafulvalene π system compound and fullerene-based material are mixedly configured into solution, pass through volatilization mixed solution
The Subjective and Objective supramolecular materials of method acquisition Subjective and Objective structure；The solution evaporation method is also used in macrocycle molecule (cyclodextrin, cup
Aromatic hydrocarbons, azepine calixarenes etc.) in the preparation of the host-guest complex of fullerene molecule.
Existing solution evaporation method can obtain the other fowler alkenyl Subjective and Objective material of powder level, and be unable to control compound receive
The crystallinity of rice material, is also unable to control the pattern of material, affects its physicochemical characteristics, to limit it as micro-nano
The application of device and field of functional materials.Correlative study accumulation has developed many host molecules, has expanded the super of many novelties
Molecular structure.The discovery of these research achievements has inspired people to fowler alkenyl Subjective and Objective material in biology, fine chemistry, military project
The potential application of aspect is explored.In particular, the research and development for the nano crystal material being widely recognized as this century, it is considered to be fowler
Necessary means of the olefinic base material as micro-nano device and functional material.Although also no discovery is not effectively synthesized fullerene in existing method
The method of base Subjective and Objective nanocrystalline material but illustrates form the answering in terms of new and high technology functional material of fullerene aggregation
Importance in.
Summary of the invention
To make up the deficiencies in the prior art, the present invention is obtained using liquid phase processing method with high-crystallinity and nanometer ruler
Very little fullerene C60Calixarenes fullerene is nanocrystalline.
Fullerene C60The preparation method of calixarenes Subjective and Objective composite nanocrystalline material, with pure fullerene C60Original powder and to uncle
Butyl cup [8] aromatic hydrocarbons is raw material；Using aromatic hydrocarbon as solvent；Using isopropanol as precipitating reagent；Subjective and Objective is prepared using liquid phase deposition
Structure composite is nanocrystalline.
Further, the aromatic hydrocarbon is benzene or toluene.
More specifically, above-mentioned Subjective and Objective structure composite it is nanocrystalline the preparation method is as follows:
S1. by excessive C60Powder is put into benzene or toluene solvant and ultrasonic vibration, then by solution left standstill, to excessive
C60After powder precipitates completely, the saturated solution for removing upper layer is mother liquor A；
S2. simultaneously ultrasonic vibration is put into benzene or toluene solvant to tert-butyl-calix [8] aromatic hydrocarbons powder by excessive, then by solution
Stand, after it is excessive tert-butyl-calix [8] aromatic hydrocarbons is precipitated completely after, the saturated solution for removing upper layer is mother liquor B；
S3. mother liquor A is mixed with mother liquor B with 1:1 volume ratio, and ultrasound 1-2 minutes；
S4. isopropanol is added to above-mentioned mixed solution and 3 times that isopropanol volume is mother liquor A is added as precipitating reagent, and surpass
Sound 1-2 minutes, stand 10-20 hours at room temperature；
It is that control composite nanocrystalline is formed and deposition since isopropanol acts in the present invention, isopropanol volume in an experiment
It is the key that control nanocrystalline formation speed and the control of nanocrystalline shape with liquor capacity ratio.Inventor is studied for a long period of time middle discovery
It is 3 times of mother liquor A when isopropanol volume is added, is that can obtain crystallinity height, morphological rules fullerene C60Calixarenes Subjective and Objective
The most suitable ratio of composite nanocrystalline.
S5. lower sediment is sucked out, is dripped on clean substrate, it is available after solvent and precipitating reagent volatilize naturally
C60To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective structure nano piece crystalline material；
S6. by C obtained in step S560To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective structure nano piece crystal 10-4Pa-
10-3Under Pa pressure, at a temperature of 100 DEG C -120 DEG C, heat 2-3 hours, removal remains in the solvent and deposition agent of crystals
Molecule obtains C60-To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective nanometer sheet monocrystalline.Also known as fullerene C60Calixarenes host and guest's bluk recombination is received
The brilliant material of rice.
Fullerene C60To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective composite nanocrystalline by C60With to tert-butyl-calix [8] aromatic hydrocarbons with
1:1 molar ratio composition.Wherein, fullerene molecule C60Shape is combined by Van der Waals force cladding with to tert-butyl-calix [8] aromatic hydrocarbon molecule
At structural unit as composition primitive.
Wherein, biscuit shaped C60To tert-butyl-calix [8] aromatic hydrocarbons composite nano-grade sheet material, the diameter of nanometer sheet is 2 μm -3 μm,
With a thickness of 200nm-300nm；Quadrangle sheet C60To tert-butyl-calix [8] aromatic hydrocarbons composite nano-grade sheet material, side length is about 2 μm -4 μm,
With a thickness of 200nm-300nm.
The present invention provides the preparation methods of one fullerene-calixarenes Subjective and Objective composite nanocrystalline material.It uses for the first time
The method of liquid deposition regulates and controls crystal structure and crystal shape by the selection to Subjective and Objective component ratio, solvent, at
Function obtains fullerene C abundant60To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective composite nanocrystalline material.Using liquid phase deposition,
The regulation of the rapid synthesis and nanocrystalline shape and crystal structure of fullerene-calixarenes Subjective and Objective structural material may be implemented.
As liquid-phase precipitation agent be the key that using isopropanol it is of the invention, it is fast rapid-result nanocrystalline in the solution that isopropanol plays composite material
Body material, and the effect of fast deposition also act as the effect for controlling nanocrystalline shape.Method provided by the invention not only technique letter
It list and can be realized fullerene-calixarenes Subjective and Objective composite nanocrystalline in self assembling process, to the Effective Regulation of shape, mention
High-crystallinity.
Detailed description of the invention
The biscuit shaped C that Fig. 1 is obtained using benzene as organic solvent60-To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective nanometer sheet monocrystalline
SEM picture；
The biscuit shaped C that Fig. 2 is obtained using benzene as organic solvent60-To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective nanometer sheet monocrystalline
XRD diffraction picture；
Fig. 3 infrared absorpting light spectra, wherein the biscuit shaped C that (a) is obtained using benzene as organic solvent60-To tert-butyl-calix
[8] the infrared absorpting light spectra piece of aromatic hydrocarbons Subjective and Objective nanometer sheet monocrystalline；(b) and (c) is respectively as the original C compareed60-To uncle
The infrared absorpting light spectra piece of butyl cup [8] aromatic hydrocarbons；
The rectangular C that Fig. 4 is obtained using toluene as organic solvent60-To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective nanometer sheet monocrystalline
SEM picture.
Specific embodiment
The present invention is described in further detail in the following with reference to the drawings and specific embodiments, but is not used in and limits protection model of the invention
It encloses.
Embodiment 1
S1. by excessive C60Powder is put into benzene simultaneously ultrasound 1-2 minutes, and solution is then stood to 2-5 hours at room temperature, to
Excessive C60Completely after precipitating, upper solution is removed, this solution is to be saturated C60Benzole soln；
S2. tert-butyl-calix [8] aromatic hydrocarbons powder is put into benzene simultaneously ultrasound 1-2 minutes by excessive, then by solution in room temperature
Lower standing 2-5 hours, after it is excessive tert-butyl-calix [8] aromatic hydrocarbons is precipitated completely after, upper solution is removed, this solution is full
With to tert-butyl-calix [8] aromatic hydrocarbons benzole soln；
S3. with pipette by above-mentioned configured saturation C60Benzole soln and saturation to tert-butyl-calix [8] aromatic hydrocarbons benzole soln with
The mixing of 1:1 volume ratio, and ultrasound 1-2 minutes；
S4. isopropanol is added as precipitating reagent to above-mentioned mixed solution, it is saturation C that isopropanol volume, which is added,60The 3 of benzole soln
Times, and ultrasound 1-2 minutes, stand 10-20 hours at room temperature；
S5. the precipitating of lower layer in reaction utensil is sucked out with rubber head dropper, is dripped on clean substrate, to solvent and precipitating reagent
Naturally available biscuit shaped C after volatilizing60To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective structure nano piece crystalline material；
S6. by C obtained in step S560To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective structure nano piece crystal in pressure
5x10-4It under Pa, at 100 DEG C of temperature, heats 2-3 hours, removal remains in the solvent and deposition agent molecule of crystals, is had
There is the C of tetragonal structure60-To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective nanometer sheet monocrystalline, wherein component C60With to tert-butyl-calix
[8] aromatic hydrocarbons molar ratio is 1:1.
Embodiment 2
S1. by excessive C60Powder is put into toluene simultaneously ultrasound 1-2 minutes, and solution is then stood to 2-5 hours at room temperature,
To excessive C60Completely after precipitating, upper solution is removed, this solution is to be saturated C60Toluene solution；
S2. tert-butyl-calix [8] aromatic hydrocarbons powder is put into toluene simultaneously ultrasound 1-2 minutes by excessive, then by solution in room
Temperature is lower to stand 2-5 hours, after it is excessive tert-butyl-calix [8] aromatic hydrocarbons is precipitated completely after, upper solution is removed, this solution is
Saturation is to tert-butyl-calix [8] aromatic hydrocarbons toluene solution；
S3. with pipette by above-mentioned configured saturation C60Toluene solution and saturation are molten to tert-butyl-calix [8] aromatic hydrocarbons toluene
Liquid is mixed with 1:1 volume ratio, and ultrasound 1-2 minutes；
S4. isopropanol is added as precipitating reagent to above-mentioned mixed solution, it is saturation C that isopropanol volume, which is added,60Toluene solution
3 times, and ultrasound 1-2 minutes, stand 10-20 hours at room temperature；
S5. the precipitating of lower layer in reaction utensil is sucked out with rubber head dropper, is dripped on clean substrate, to solvent and precipitating reagent
Naturally available four horn shapes C after volatilizing60To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective structure nano piece crystalline material；
S6. by C obtained in step S560To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective structure nano piece crystal in pressure
5x10-4It under Pa, at 100 DEG C of temperature, heats 2-3 hours, removal remains in the solvent and deposition agent molecule of crystals, is had
There is the C of tetragonal structure60-To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective nanometer sheet monocrystalline, wherein component C60With to tert-butyl-calix
[8] aromatic hydrocarbons molar ratio is 1:1.
The preferable specific embodiment of the above, only the invention, but the protection scope of the invention is not
It is confined to this, anyone skilled in the art is in the technical scope that the invention discloses, according to the present invention
The technical solution of creation and its inventive concept are subject to equivalent substitution or change, should all cover the invention protection scope it
It is interior.
Claims (4)
1. fullerene C60The preparation method of calixarenes Subjective and Objective composite nanocrystalline material, which is characterized in that with pure fullerene C60It is former
Powder and to tert-butyl-calix [8] aromatic hydrocarbons be raw material；Using aromatic hydrocarbon as solvent；Using isopropanol as precipitating reagent；Using liquid deposition legal system
Standby Subjective and Objective structure composite is nanocrystalline.
2. the method according to claim 1, wherein the aromatic hydrocarbon is benzene or toluene.
3. according to right want 1 described in method, which is characterized in that fullerene C60Calixarenes Subjective and Objective composite nanocrystalline material
It is specific the preparation method is as follows:
S1. by excessive C60Powder is put into benzene or toluene solvant and ultrasonic vibration, then by solution left standstill, to excessive C60Powder is complete
After full precipitating, the saturated solution for removing upper layer is mother liquor A；
S2. simultaneously ultrasonic vibration is put into benzene or toluene solvant to tert-butyl-calix [8] aromatic hydrocarbons powder by excessive, it is then that solution is quiet
Set, after it is excessive tert-butyl-calix [8] aromatic hydrocarbons is precipitated completely after, the saturated solution for removing upper layer is mother liquor B；
S3. mother liquor A is mixed with mother liquor B with 1:1 volume ratio, and ultrasound 1-2 minutes；
S4. isopropanol is added as precipitating reagent to above-mentioned mixed solution, 3 times that isopropanol volume is mother liquor A, and ultrasound 1- is added
2 minutes, stand 10-20 hours at room temperature；
S5. lower sediment is sucked out, is dripped on clean substrate, the available C after solvent and precipitating reagent volatilize naturally60It is right
Tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective structure nano piece crystalline material；
S6. by C obtained in step S560To tert-butyl-calix [8] aromatic hydrocarbons Subjective and Objective structure nano piece crystal 10-4Pa-10-3Pa
Under pressure, at a temperature of 100 DEG C -120 DEG C, to heat 2-3 hours, removal remains in the solvent and deposition agent molecule of crystals,
Obtain fullerene C60Calixarenes Subjective and Objective nanometer sheet monocrystalline.
4. fullerene C60Calixarenes Subjective and Objective composite nanocrystalline material, which is characterized in that by C60With to tert-butyl-calix [8] aromatic hydrocarbons
It is formed with 1:1 molar ratio, wherein fullerene molecule C60It is combined with to tert-butyl-calix [8] aromatic hydrocarbon molecule by Van der Waals force cladding
The structural unit of formation is as composition primitive.
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| CN101550591A (en) * | 2009-04-01 | 2009-10-07 | 吉林大学 | Monodisperse C* nano unit crystal material and method for preparing same |
| CN101649482A (en) * | 2009-09-21 | 2010-02-17 | 吉林大学 | C60 nano monocrystal assembly materials in different shapes and preparation method thereof |
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