CN108557803A - A kind of Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur, preparation method and applications - Google Patents
A kind of Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur, preparation method and applications Download PDFInfo
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- CN108557803A CN108557803A CN201810429712.3A CN201810429712A CN108557803A CN 108557803 A CN108557803 A CN 108557803A CN 201810429712 A CN201810429712 A CN 201810429712A CN 108557803 A CN108557803 A CN 108557803A
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- 241000143432 Daldinia concentrica Species 0.000 title claims abstract description 61
- 229910021392 nanocarbon Inorganic materials 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 31
- PFRUBEOIWWEFOL-UHFFFAOYSA-N [N].[S] Chemical compound [N].[S] PFRUBEOIWWEFOL-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000007790 solid phase Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000015572 biosynthetic process Effects 0.000 title claims description 16
- 238000003786 synthesis reaction Methods 0.000 title claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 70
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000000843 powder Substances 0.000 claims abstract description 56
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 40
- 239000011734 sodium Substances 0.000 claims abstract description 33
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 33
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 29
- -1 sodium olefin sulfonates Chemical class 0.000 claims abstract description 29
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 28
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000005864 Sulphur Substances 0.000 claims abstract description 27
- 229920006242 ethylene acrylic acid copolymer Polymers 0.000 claims abstract description 24
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 5
- 239000001257 hydrogen Substances 0.000 claims abstract description 5
- 230000001699 photocatalysis Effects 0.000 claims abstract description 5
- 238000007146 photocatalysis Methods 0.000 claims abstract description 5
- 238000003860 storage Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 24
- 239000004570 mortar (masonry) Substances 0.000 claims description 24
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 7
- 229920006243 acrylic copolymer Polymers 0.000 claims description 7
- 239000007822 coupling agent Substances 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 7
- 229910000077 silane Inorganic materials 0.000 claims description 7
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 6
- XYXNTHIYBIDHGM-UHFFFAOYSA-N ammonium thiosulfate Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=S XYXNTHIYBIDHGM-UHFFFAOYSA-N 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 230000008878 coupling Effects 0.000 claims description 6
- 238000010168 coupling process Methods 0.000 claims description 6
- 238000005859 coupling reaction Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 6
- 150000001336 alkenes Chemical class 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 4
- 239000003990 capacitor Substances 0.000 claims description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
- FDPGUECLKNPLOB-UHFFFAOYSA-N (n-phenylanilino)urea Chemical compound C=1C=CC=CC=1N(NC(=O)N)C1=CC=CC=C1 FDPGUECLKNPLOB-UHFFFAOYSA-N 0.000 claims description 3
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 3
- 229930091371 Fructose Natural products 0.000 claims description 3
- 239000005715 Fructose Substances 0.000 claims description 3
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 3
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 150000001413 amino acids Chemical class 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000008101 lactose Substances 0.000 claims description 3
- 102000004169 proteins and genes Human genes 0.000 claims description 3
- 108090000623 proteins and genes Proteins 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims 4
- 238000002156 mixing Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 238000000227 grinding Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000010923 batch production Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001420 photoelectron spectroscopy Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004711 α-olefin Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention discloses Nano carbon balls, preparation method and applications that a kind of solid phase microwave method synthesizes doping nitrogen sulphur, the Nano carbon balls, including following raw material：Carbon source, nitrogen source, sulphur source, graphene energy powder, silane coupling agent KH 57, α sodium olefin sulfonates, ethylene-acrylic acid copolymer, the Nano carbon balls be by mixing, grinding, microwave reaction and etc. made of.The present invention has the characteristics that raw material batch production simple and easy to get, simple for process, easy to operate, environmentally protective, efficiently easy；For carbon ball diameter prepared by the present invention at 30 60 nanometers, which is expected to have huge application prospect in fields such as hydrogen storage, ultracapacitor, photocatalysis.
Description
【Technical field】
The present invention relates to a kind of novel preparation methods of nitrogen sulphur codope Nano carbon balls, and in particular to solid-phase grinding, microwave carbon
Change technology prepares nitrogen sulphur codope Nano carbon balls.
【Background technology】
It is excellent that Nano carbon balls have that density is low, chemical property is stable, good conductivity, large specific surface area, biocompatibility are strong etc.
Point has potential application in fields such as electrode material, catalyst, catalyst carrier, composite material reinforcement body and drug packages
Foreground.Carbon material leverages the promotion of its comprehensive performance due to the defect of this body structure, limits its further application.
The performance of carbon material and its crystallinity, microstructure and surface characteristic etc. are closely related, and carbon material can be effectively reduced by doping
The defect of itself further increases its stability and electric conductivity.As introducing hetero-atoms can reduce the resistance of electric charge transfer and change
Kind wetability, to enhance capacitive property, the hetero atom of the doping reported at present have nitrogen phosphate and sulfur and boron can singly adulterate or
The form of person's codope is adulterated with modified carbonaceous components.Compared with singly adulterating, codope carrying in overall performance due to synergistic effect
Rising has apparent advantage.Up to the present, single nitrogen-doped carbon nanosphere document report is more, and codope such as nitrogen sulphur codope
Nano carbon balls document report is less, and mostly uses arc discharge, laser sintered method, chemical vapour deposition technique or vacuum
Heat treating process, these preparation methods need higher energy expenditure, expensive instrument and equipment, reaction time length and complicated experiment
The shortcomings of operating procedure, limits popularization of its material in actual development application.Therefore, explore it is a kind of it is simple, energy saving, efficient,
The nitrogen sulphur codope Nano carbon balls preparation method of low cost has important scientific research meaning and actual application value.
【Invention content】
The present invention provides a kind of Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur, preparation method and applications, with solution
Certainly the technical issues of the prior art.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur, including following raw material：Carbon source, nitrogen source, sulphur source, graphite
Alkene energy powder, silane coupling agent KH-57, α-sodium olefin sulfonate, ethylene-acrylic acid copolymer；
The graphene energy powder, silane coupling agent KH-57, α-sodium olefin sulfonate, ethylene-acrylic acid copolymer
Molar ratio is (0.06-0.15):(0.02-0.04):(0.03-0.05):(0.1-0.2.
Further, as unit of molar part, including following raw material：1 part of carbon source, 2-3.5 parts of nitrogen source, 1.2-3 parts of sulphur source,
0.06-0.15 parts of graphene energy powder .02-0.04 parts of Silane coupling reagent KH-570, α -0.03-0.05 parts of sodium olefin sulfonate,
0.1-0.2 parts of ethylene-acrylic acid copolymer.
Further, as unit of molar part, including following raw material：1 part of carbon source, 2.5 parts of nitrogen source, 2.3 parts of sulphur source, graphite
0.09 part of alkene energy powder .03 parts of Silane coupling reagent KH-570,0.04 part of α-sodium olefin sulfonate, ethylene-acrylic acid copolymer
0.2 part.
Further, the carbon source is one kind in glucose, sucrose, fructose, lactose and citric acid.
Further, the nitrogen source is one kind in amino acid, protein, melamine, urea.
Further, the sulphur source is one kind in thiocarbamide, diphenylsemicarbazide, ATS (Ammonium thiosulphate).
The present invention also provides the preparation methods that a kind of solid phase microwave method synthesizes the Nano carbon balls of doping nitrogen sulphur, including following step
Suddenly：
(1) by carbon source, nitrogen source, sulphur source, α-sodium olefin sulfonate, example mixes in molar ratio, and 10- is ground on agate mortar
Mixture is made in 20min；
(2) graphene is ground to 10-20min crushing on agate mortar, powder is made, gained powder is in magnetic field intensity
6300-6800GS, ultrasonic power 500-600W, temperature are 50-55 DEG C, and rotating speed is to stir 30- under 200-300r/min
Graphene energy powder is made in 40min；
(3) by graphene energy powder, alkane coupling agent KH-57, second made from mixture made from step (1), step (2)
Example mixes alkene-acrylic copolymer in molar ratio, and 15-25min is ground on agate mortar, mixed-powder is made, and what is obtained is mixed
It closes powder to be put into microwave special glass beaker, then beaker is put into micro-wave oven, temperature setting is middle high fiery or high fire,
Room temperature is naturally cooled to after reaction 5-15min, mixture after reaction is made；
(4) mixture after step (3) reaction obtained on agate mortar is ground into 10-20min, mixed carbon nanometer is made
Ball.
Further, a diameter of 30-60nm of the Nano carbon balls.
The present invention also provides a kind of solid phase microwave methods to synthesize the Nano carbon balls of doping nitrogen sulphur in hydrogen storage, capacitor, photocatalysis
Application in equal fields.
The invention has the advantages that：
(1) by the data of embodiment 1-3 and comparative example 1-5 as it can be seen that lacking graphene energy powder, silane coupling agent KH-
57, α-sodium olefin sulfonate, ethylene-acrylic acid copolymer can influence specific capacitance and specific capacitance conservation rate, increase stone in the feed
Black alkene energy powder, silane coupling agent KH-57, α-sodium olefin sulfonate, ethylene-acrylic acid copolymer, can be improved specific capacitance and ratio
Capacity retention；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment.
(2) by embodiment 1 and the data of comparative example 1-5 as it can be seen that graphene energy powder, silane coupling agent KH-57, α-alkene
Base sodium sulfonate, ethylene-acrylic acid copolymer play synergistic effect in preparing Nano carbon balls, collaboration improve specific capacitance and
Specific capacitance conservation rate, this may be：Graphene energy powder, silane coupling agent KH-57, α-sodium olefin sulfonate, ethylene-propylene
Acid copolymer is as raising specific capacitance and specific capacitance conservation rate system, using graphene energy powder as major ingredient, after graphene fills energy
With stronger electric conductivity, be conducive to the chemical property for improving material；Using silane coupling agent KH-57 as graft modification agent, α-
Sodium olefin sulfonate have excellent surface-active, ethylene-acrylic acid copolymer have excellent dispersion performance, carbon source, nitrogen source,
The rate of microwave reaction can be improved under silane coupling agent KH-57, α-sodium olefin sulfonate effect in sulphur source, and graphene energy powder
The addition at end improves the specific capacitance and specific capacitance conservation rate of Nano carbon balls, and the presence of ethylene-acrylic acid copolymer can make to be made
Nano carbon balls effectively avoid reuniting, to make Nano carbon balls electrode material obtained show higher specific capacity and preferable
Cyclical stability.
(3) Nano carbon balls prepared by the present invention, a diameter of 30-60nm and uniform in size, good dispersion, specific surface area
400m2·g-1More than.When it is as super capacitor material, analysis and tests show that, in current density 1Ag-1When, specific capacitance
Up to 244.7Fg-1More than；After cycle charge-discharge 2000 times, specific capacitance conservation rate is 92.1% or more, shows higher specific volume
Amount and preferable stable circulation.
(4) present invention have raw material it is simple and easy to get, it is simple for process, easy to operate, environmentally protective, efficiently easily produce in batches
Feature；Nitrogen sulphur codope Nano carbon balls prepared by the present invention are Functional carbon material, nitrogen and sulfur heteroatom doped with conducive to subtracting
The fault of construction of few Nano carbon balls, improves its composite material stability and electric conductivity；Nitrogen sulphur codope prepared by the method for the present invention
Nano carbon balls can be applied to the fields such as hydrogen storage, ultracapacitor, photocatalysis.
【Description of the drawings】
Fig. 1 is the XRD diffraction patterns of Nano carbon balls prepared by embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of Nano carbon balls prepared by embodiment 2；
Fig. 3 is the photoelectron spectroscopy XPS figures of Nano carbon balls prepared by embodiment 3.
【Specific implementation mode】
For ease of more fully understanding the present invention, it is illustrated by the following examples, these examples belong to the protection of the present invention
Range, but do not limit the scope of the invention.
In embodiment, the Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur, as unit of molar part, including
Following raw material：1 part of carbon source, 2-3.5 parts of nitrogen source, 1.2-3 parts of sulphur source, 0.06-0.15 parts of graphene energy powder, silane coupling agent
KH-570.02-0.04 parts, α -0.03-0.05 parts of sodium olefin sulfonate, 0.1-0.2 parts of ethylene-acrylic acid copolymer.
The carbon source is one kind in glucose, sucrose, fructose, lactose and citric acid.
The nitrogen source is one kind in amino acid, protein, melamine, urea.
The sulphur source is one kind in thiocarbamide, diphenylsemicarbazide, ATS (Ammonium thiosulphate).
The preparation method of the Nano carbon balls of the solid phase microwave method synthesis doping nitrogen sulphur, includes the following steps：
(1) by carbon source, nitrogen source, sulphur source, α-sodium olefin sulfonate, example mixes in molar ratio, and 10- is ground on agate mortar
Mixture is made in 20min；
(2) graphene is ground to 10-20min crushing on agate mortar, powder is made, gained powder is in magnetic field intensity
6300-6800GS, ultrasonic power 500-600W, temperature are 50-55 DEG C, and rotating speed is to stir 30- under 200-300r/min
Graphene energy powder is made in 40min；
(3) by graphene energy powder, alkane coupling agent KH-57, second made from mixture made from step (1), step (2)
Example mixes alkene-acrylic copolymer in molar ratio, and 15-25min is ground on agate mortar, mixed-powder is made, and what is obtained is mixed
It closes powder to be put into microwave special glass beaker, then beaker is put into micro-wave oven, temperature setting is middle high fiery or high fire,
Room temperature is naturally cooled to after reaction 5-15min, mixture after reaction is made；
(4) mixture after step (3) reaction obtained on agate mortar is ground into 10-20min, a diameter of 30- is made
The Nano carbon balls of 60nm.
The Nano carbon balls can be in the application in the fields such as hydrogen storage, capacitor, photocatalysis.
Below by more specifically examples illustrate the present invention.
Embodiment 1
A kind of Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur, as unit of molar part, including following raw material：Carbon source
1 part, 2.5 parts of nitrogen source, 2.3 parts of sulphur source, 0.09 part of graphene energy powder .03 parts of Silane coupling reagent KH-570, α-olefin sulfonic acid
0.04 part of sodium, 0.2 part of ethylene-acrylic acid copolymer.
The carbon source is glucose.
The nitrogen source is urea.
The sulphur source is thiocarbamide.
The preparation method of the Nano carbon balls of the solid phase microwave method synthesis doping nitrogen sulphur, includes the following steps：
(1) by carbon source, nitrogen source, sulphur source, α-sodium olefin sulfonate, example mixes in molar ratio, and 10min is ground on agate mortar,
Mixture is made；
(2) graphene is ground to 10min crushing on agate mortar, powder is made, gained powder is in magnetic field intensity
6500GS, ultrasonic power 560W, temperature are 53 DEG C, and rotating speed is to stir 36min under 250r/min, and graphene energy is made
Powder；
(3) by graphene energy powder, alkane coupling agent KH-57, second made from mixture made from step (1), step (2)
Example mixes alkene-acrylic copolymer in molar ratio, and 22min is ground on agate mortar, mixed-powder, obtained mixing is made
Powder is put into microwave special glass beaker, and then beaker is put into micro-wave oven, and temperature setting is middle high fire, reacts 10min
After naturally cool to room temperature, be made reaction after mixture；
(4) mixture after step (3) reaction obtained on agate mortar is ground into 10min, a diameter of 32-55nm is made
Nano carbon balls, it is as shown in Figure 1 to measure XRD diffraction patterns.
Embodiment 2
A kind of Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur, as unit of molar part, including following raw material：Carbon source
1 part, 3 parts of nitrogen source, 1.2 parts of sulphur source, 0.06 part of graphene energy powder .02 parts of Silane coupling reagent KH-570, α-sodium olefin sulfonate
0.05 part, 0.1 part of ethylene-acrylic acid copolymer.
The carbon source is glucose.
The nitrogen source is urea.
The sulphur source is thiocarbamide.
The preparation method of the Nano carbon balls of the solid phase microwave method synthesis doping nitrogen sulphur, includes the following steps：
(1) by carbon source, nitrogen source, sulphur source, α-sodium olefin sulfonate, example mixes in molar ratio, and 20min is ground on agate mortar,
Mixture is made；
(2) 12min crushing will be ground on agate mortar, powder is made, and gained powder is 6300GS in magnetic field intensity, is surpassed
Acoustic power is 500W, and temperature is 55 DEG C, and rotating speed is to stir 40min under 200r/min, and graphene energy powder is made；
(3) by graphene energy powder, alkane coupling agent KH-57, second made from mixture made from step (1), step (2)
Example mixes alkene-acrylic copolymer in molar ratio, and 25min is ground on agate mortar, mixed-powder, obtained mixing is made
Powder is put into microwave special glass beaker, and then beaker is put into micro-wave oven, and temperature setting is that height is fiery, after reaction 5min certainly
It so is cooled to room temperature, mixture after reaction is made；
(4) mixture after step (3) reaction obtained on agate mortar is ground into 10min, a diameter of 30-53nm is made
Nano carbon balls, it is as shown in Figure 2 to measure scanning electron microscope (SEM) photograph.
Embodiment 3
A kind of Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur, as unit of molar part, including following raw material：Carbon source
1 part, 2.5 parts of nitrogen source, 1.2 parts of sulphur source, 0.15 part of graphene energy powder .04 parts of Silane coupling reagent KH-570, α-olefin sulfonic acid
0.03 part of sodium, 0.2 part of ethylene-acrylic acid copolymer.
The carbon source is glucose.
The nitrogen source is melamine.
The sulphur source is thiocarbamide.
The preparation method of the Nano carbon balls of the solid phase microwave method synthesis doping nitrogen sulphur, includes the following steps：
(1) by carbon source, nitrogen source, sulphur source, α-sodium olefin sulfonate, example mixes in molar ratio, and 18min is ground on agate mortar,
Mixture is made；
(2) 15min crushing will be ground on agate mortar, powder is made, and gained powder is 6600GS in magnetic field intensity, is surpassed
Acoustic power is 580W, and temperature is 53 DEG C, and rotating speed is to stir 30min under 300r/min, and graphene energy powder is made；
(3) by graphene energy powder, alkane coupling agent KH-57, second made from mixture made from step (1), step (2)
Example mixes alkene-acrylic copolymer in molar ratio, and 15min is ground on agate mortar, mixed-powder, obtained mixing is made
Powder is put into microwave special glass beaker, and then beaker is put into micro-wave oven, and temperature setting is middle high fire, reacts 12min
After naturally cool to room temperature, be made reaction after mixture；
(4) mixture after step (3) reaction obtained on agate mortar is ground into 14min, a diameter of 42-60nm is made
Nano carbon balls, it is as shown in Figure 3 to measure photoelectron spectroscopy XPS figure.
Comparative example 1
It is essentially identical with the preparation process of embodiment 1, have only unlike prepare in the raw materials of Nano carbon balls and lack graphite
Alkene energy powder, silane coupling agent KH-57, α-sodium olefin sulfonate, ethylene-acrylic acid copolymer.
Comparative example 2
It is essentially identical with the preparation process of embodiment 1, have only unlike prepare in the raw materials of Nano carbon balls and lack graphite
Alkene energy powder.
Comparative example 3
It is essentially identical with the preparation process of embodiment 1, have only unlike prepare in the raw materials of Nano carbon balls and lack silane
Coupling agent KH-57.
Comparative example 4
It is essentially identical with the preparation process of embodiment 1, have only unlike prepare in the raw materials of Nano carbon balls and lack α-alkene
Base sodium sulfonate.
Comparative example 5
It is essentially identical with the preparation process of embodiment 1, have only unlike prepare in the raw materials of Nano carbon balls and lack second
Alkene-acrylic copolymer.
Performance test：
Using Nano carbon balls as working electrode, Hg/HgO electrodes are reference electrode, and nickel foam is to electrode.Use electrochemical operation
(CHI 660D) is stood in 6molL-1KOH electrolyte in, test Nano carbon balls electrode material in potential window -1.0-0V in 25 DEG C
The specific capacity value and cycle charge discharge electrical property of material.Detect specific capacitance when current density 1Ag-1；Detect cycle charge-discharge 2000
Specific capacitance conservation rate after secondary, the results are shown in table below.
As seen from the above table：(1) by the data of embodiment 1-3 and comparative example 1-5 as it can be seen that lacking graphene energy powder, silicon
Alkane coupling agent KH-57, α-sodium olefin sulfonate, ethylene-acrylic acid copolymer can influence specific capacitance and specific capacitance conservation rate,
Increase graphene energy powder, silane coupling agent KH-57, α-sodium olefin sulfonate, ethylene-acrylic acid copolymer in raw material, can carry
High specific capacitance and specific capacitance conservation rate；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment.
(2) by embodiment 1 and the data of comparative example 1-5 as it can be seen that graphene energy powder, silane coupling agent KH-57, α-alkene
Base sodium sulfonate, ethylene-acrylic acid copolymer play synergistic effect in preparing Nano carbon balls, collaboration improve specific capacitance and
Specific capacitance conservation rate, this may be：Graphene energy powder, silane coupling agent KH-57, α-sodium olefin sulfonate, ethylene-propylene
Acid copolymer is as raising specific capacitance and specific capacitance conservation rate system, using graphene energy powder as major ingredient, after graphene fills energy
With stronger electric conductivity, be conducive to the chemical property for improving material；Using silane coupling agent KH-57 as graft modification agent, α-
Sodium olefin sulfonate have excellent surface-active, ethylene-acrylic acid copolymer have excellent dispersion performance, carbon source, nitrogen source,
The rate of microwave reaction can be improved under silane coupling agent KH-57, α-sodium olefin sulfonate effect in sulphur source, and graphene energy powder
The addition at end improves the specific capacitance and specific capacitance conservation rate of Nano carbon balls, and the presence of ethylene-acrylic acid copolymer can make to be made
Nano carbon balls effectively avoid reuniting, to make Nano carbon balls electrode material obtained show higher specific capacity and preferable
Cyclical stability.
The above content is it cannot be assumed that present invention specific implementation is confined to these explanations, for the technical field of the invention
Those of ordinary skill for, under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all answers
When being considered as belonging to present invention scope of patent protection determined by the appended claims.
Claims (9)
1. a kind of Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur, which is characterized in that including following raw material：Carbon source, nitrogen source,
Sulphur source, graphene energy powder, silane coupling agent KH-57, α-sodium olefin sulfonate, ethylene-acrylic acid copolymer；
Mole of the graphene energy powder, silane coupling agent KH-57, α-sodium olefin sulfonate, ethylene-acrylic acid copolymer
Than for (0.06-0.15):(0.02-0.04):(0.03-0.05):(0.1-0.2).
2. the Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur according to claim 1, which is characterized in that with molar part
For unit, including following raw material：1 part of carbon source, 2-3.5 parts of nitrogen source, 1.2-3 parts of sulphur source, graphene energy powder 0.06-0.15
Part .02-0.04 parts of Silane coupling reagent KH-570, α -0.03-0.05 parts of sodium olefin sulfonate, ethylene-acrylic acid copolymer 0.1-
0.2 part.
3. the Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur according to claim 2, which is characterized in that with molar part
For unit, including following raw material：It is 1 part of carbon source, 2.5 parts of nitrogen source, 2.3 parts of sulphur source, 0.09 part of graphene energy powder, silane coupled
KH-570.03 parts of agent, 0.04 part of α-sodium olefin sulfonate, 0.2 part of ethylene-acrylic acid copolymer.
4. synthesizing the Nano carbon balls of doping nitrogen sulphur according to claim 1-3 any one of them solid phase microwave methods, which is characterized in that
The carbon source is one kind in glucose, sucrose, fructose, lactose and citric acid.
5. synthesizing the Nano carbon balls of doping nitrogen sulphur according to claim 1-3 any one of them solid phase microwave methods, which is characterized in that
The nitrogen source is one kind in amino acid, protein, melamine, urea.
6. synthesizing the Nano carbon balls of doping nitrogen sulphur according to claim 1-3 any one of them solid phase microwave methods, which is characterized in that
The sulphur source is one kind in thiocarbamide, diphenylsemicarbazide, ATS (Ammonium thiosulphate).
7. a kind of preparation side for the Nano carbon balls synthesizing doping nitrogen sulphur according to claim 1-6 any one of them solid phase microwave methods
Method, which is characterized in that include the following steps：
(1) by carbon source, nitrogen source, sulphur source, α-sodium olefin sulfonate, example mixes in molar ratio, and 10-20min is ground on agate mortar,
Mixture is made；
(2) graphene is ground to 10-20min crushing on agate mortar, powder is made, gained powder is in magnetic field intensity
6300-6800GS, ultrasonic power 500-600W, temperature are 50-55 DEG C, and rotating speed is to stir 30- under 200-300r/min
Graphene energy powder is made in 40min；
(3) by graphene energy powder, alkane coupling agent KH-57, ethylene-made from mixture made from step (1), step (2)
Example mixes acrylic copolymer in molar ratio, and 15-25min is ground on agate mortar, mixed-powder, obtained mixed powder is made
End is put into microwave special glass beaker, and then beaker is put into micro-wave oven, and temperature setting is middle high fire or high fire, reaction
Room temperature is naturally cooled to after 5-15min, and mixture after reaction is made；
(4) mixture after step (3) reaction obtained on agate mortar is ground into 10-20min, Nano carbon balls is made.
8. the preparation method of the Nano carbon balls of solid phase microwave method synthesis doping nitrogen sulphur according to claim 7, feature exist
In a diameter of 30-60nm of the Nano carbon balls.
9. it is a kind of according to claim 1-6 any one of them solid phase microwave methods synthesize doping nitrogen sulphur Nano carbon balls hydrogen storage,
Application in the fields such as capacitor, photocatalysis.
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