CN104386668B - A kind of method that nickel nano-catalytic prepares spiral carbon nanomaterial - Google Patents

A kind of method that nickel nano-catalytic prepares spiral carbon nanomaterial Download PDF

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CN104386668B
CN104386668B CN201410628627.1A CN201410628627A CN104386668B CN 104386668 B CN104386668 B CN 104386668B CN 201410628627 A CN201410628627 A CN 201410628627A CN 104386668 B CN104386668 B CN 104386668B
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nickel
carbon nanomaterial
spiral carbon
tartaric acid
catalytic
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CN104386668A (en
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简贤
王思源
曾青
唐辉
尹良君
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Chengdu Tianyou Jingchuang Technology Co ltd
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University of Electronic Science and Technology of China
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Abstract

The invention provides a kind of method that nickel nano-catalytic prepares spiral carbon nanomaterial, belong to nano-carbon material preparation field.Comprise the following steps:a)C4H4O6KNa·4H2O and NiCl2·4H2O reacts 5~10min in aqueous, and filtering, filter cake is first washed with water to neutrality, and 1~4h of absolute ethanol washing is then used in apparatus,Soxhlet's;B) step a) gained filter cakes are dried into 2~4h in the vacuum drying chamber at 80~100 DEG C, tartaric acid nickel by powder is obtained;C) the tartaric acid nickel by powder for obtaining step b) is placed in tube furnace, and the catalytic pyrolysis 1h under acetylene atmosphere is heat-treated after 30~60min under 400~800 DEG C, hydrogen or the argon gas atmosphere;Reaction is cooled to room temperature with stove under an argon atmosphere after terminating, and obtains the spiral carbon nanomaterial.The method process is simple, easy to operate, the reaction time is short, improves production efficiency, reduces production cost.

Description

A kind of method that nickel nano-catalytic prepares spiral carbon nanomaterial
Technical field
The invention belongs to nano-carbon material preparation field, and in particular to a kind of nickel nano-catalytic prepares spiral carbon nanomaterial Method.
Background technology
Spiral carbon nanomaterial is a kind of carbon material with novel Microstructure, with high bandwidth microwave absorption, special Electric property and superior mechanical property, have been widely used in hydrogen storage material, electro-magnetic wave absorption, electrode material, field emission device The fields such as part, fuel cell.
Spiral carbon nanomaterial is mainly including spiral carbon nanotubes, spiral carbon nano-fiber etc., currently reported use Transition metal nanoparticles synthesize spiral carbon nano-fiber as catalyst, at a lower temperature catalytic pyrolysis acetylene gas Or spiral carbon nanotubes, but in same system, the spiral of different nanostructureds being obtained according to regulation and control the need for difference The research report of carbon nanomaterial is also less.(the Symmetrictwisted carbon filament s such as V.V.Chesnokov formed from but adiene-1,3 on Ni-Cu/MgO catalyst:growth regularities and Mechanism, Journal of Molecular Catalysis:A,2000,158(1):It is 267-270.) multiple with Ni-Cu/MgO Compound nano particle is catalyst, is 450 DEG C, under conditions of hydrogen and argon gas be impurity gas, prepares in cracking temperature Spiral carbon nanomaterial, but the purity of the spiral carbon nanomaterial for obtaining is relatively low, and spiral prepared by Cu catalyst systems Carbon nano-fiber is amorphous state, needs high-temperature process under an inert gas to obtain carbon fiber, which limits extensively should for the method With.(the Symmetry-related growthof carbon nanocoils from Ni-P based such as D.Y.Ding Alloy particles, Journal of Applied Physics, 2004,95 (9):5006-5009.) it is with Ni-P alloys Catalyst, with argon gas and nitrogen as impurity gas, prepares spiral carbon nanomaterial under 500~700 DEG C of reaction conditions, but should Method can use poisonous catalyst, and low yield, poor reproducibility.(the Catalytic effects of such as S.Motojima metal carb ides,oxides and Ni single crystal onthe vapor growth of micro- Coiled carbon fibers, Carbon, 1996,34 (3):289-296.) respectively with stainless steel plate and Fe-Ni-Cr- Mo-Mn-Sn alloyed powders, with argon gas, nitrogen and sulfurous gas thiophene as impurity gas, react as catalyst at 700~800 DEG C Under the conditions of prepare spiral carbon nanomaterial, but, the method has that poor reproducibility, low yield, catalyst preparation be cumbersome, catalyst The defect such as poisonous, is unfavorable for being widely popularized and applies.
The content of the invention
The defect that the present invention exists for background technology, it is proposed that a kind of nickel nano-catalytic prepares spiral carbon nanomaterial Method.The method can regulate and control the structure of spiral carbon nanomaterial by regulating and controlling cracking temperature, process is simple, low production cost, Yield is high, the spiral carbon nanomaterial function admirable for obtaining.
Technical scheme is as follows:
A kind of preparation method of nickel nano material, comprises the following steps:
Step 1:C4H4O6KNa·4H2O and NiCl2·4H2O reacts 5~10min in aqueous, and filtering, filter cake is first used Then water washing uses 1~4h of absolute ethanol washing, to remove the organic impurities of residual to neutrality in apparatus,Soxhlet's;
Step 2:The filter cake of step 1 gained is dried into 2~4h in the vacuum drying chamber at 80~100 DEG C, obtains tartaric acid Nickel by powder;
Step 3:The tartaric acid nickel by powder that step 2 is obtained is placed in tube furnace, in 400~800 DEG C, hydrogen or argon gas gas 30~60min is heat-treated under atmosphere, then room temperature is cooled to stove and is obtained the nickel nano material.
Wherein, the gas flow of hydrogen described in step 3 or argon gas is 30~35mL/min.
A kind of method that nickel nano-catalytic prepares spiral carbon nanomaterial, comprises the following steps:
Step 1:C4H4O6KNa·4H2O and NiCl2·4H2O reacts 5~10min in aqueous, and filtering, filter cake is first used Then water washing uses 1~4h of absolute ethanol washing, to remove the organic impurities of residual to neutrality in apparatus,Soxhlet's;
Step 2:The filter cake of step 1 gained is dried into 2~4h in the vacuum drying chamber at 80~100 DEG C, obtains tartaric acid Nickel by powder;
Step 3:The tartaric acid nickel by powder that step 2 is obtained is placed in tube furnace, in 400~800 DEG C, hydrogen or argon gas gas 30~60min is heat-treated under atmosphere;After heat treatment terminates, hydrogen or argon gas are closed, acetylene gas are passed through, in 400~800 DEG C, second Catalytic pyrolysis 1h under alkynes gas atmosphere;Reaction is naturally cooling to room temperature with stove under an argon atmosphere after terminating, that is, obtain the spiral shell Rotation carbon nanomaterial.
Wherein, the gas flow of hydrogen described in step 3 or argon gas is 30~35mL/min, and the gas flow of acetylene is 50 ~55mL/min.
Preferably, described in step 3 heat treatment and the temperature of catalytic pyrolysis is 500~600 DEG C.
Used as further preferred scheme, the temperature of heat treatment and catalytic pyrolysis described in step 3 is 550 DEG C.
Beneficial effects of the present invention are:
The maximum output of the catalyst preparation spiral carbon nanomaterial the 1st, reported at present is 21269.6% (Synthesis of Plait-Like Carbon Nanocoils in Ultrahigh Yield,and TheirMicrowaveAbsorption Properties, J.Phys.Chem.C 2008,112,10061-10067), and this Invention yield under the conditions of 550 DEG C has reached 22391.0%, has larger lifting compared to existing maximum output, it is possible to achieve Mass industrialized production.
2nd, the present invention uses C4H4O6KNa·4H2O and NiCl2·4H2O is reactant, prepares tartaric acid nickel, Ran Hou Tartaric acid nickel is decomposed into nickel nanometer under hydrogen atmosphere, spiral carbon is finally cracked into using the nano nickel particles catalyzing acetylene of generation Nano material.Yield that the inventive method prepares spiral carbon nanomaterial is high, function admirable;And the raw material of use is cheap and easy to get, Without using high-temperature high-pressure apparatus, process is simple is easy to operate, asepsis environment-protecting, and safety is easily-controllable, is capable of achieving large-batch industrial life Produce.
3rd, the hydrogen or argon gas being passed through during present invention thermal decomposition tartaric acid nickel are a kind of decomposition atmosphere, rather than reaction Reducing agent, course of reaction is simple and easy to control, and the reaction time is short.
4th, the spiral carbon nanomaterial that the inventive method is prepared have lightweight, it is loose the characteristics of, can be widely applied to Hydrogen storage material, ultracapacitor, EMI shield and stealth material field.
Brief description of the drawings
Fig. 1 is the scanning electron microscope diagram (SEM) of the nickel nanometer that the embodiment of the present invention 1 is prepared.Wherein, (a) is SEM figures when multiplication factor is 20000;B () is the SEM figures that multiplication factor is 160000.
Fig. 2 is the scanning electron microscope diagram (SEM) of the nickel nanometer that the embodiment of the present invention 2 is prepared.Wherein, (a) is SEM figures when multiplication factor is 20000;B () is the SEM figures that multiplication factor is 160000.
Fig. 3 is the scanning electron microscope diagram (SEM) of the nickel nanometer that the embodiment of the present invention 3 is prepared.Wherein, (a) is SEM figures when multiplication factor is 20000;B () is the SEM figures that multiplication factor is 160000.
Fig. 4 is the scanning electron microscope diagram (SEM) of the spiral carbon nanomaterial that the embodiment of the present invention 4 is prepared.Its In, (a) is SEM figures when multiplication factor is 80000;B () is the SEM figures that multiplication factor is 160000.
Fig. 5 is the scanning electron microscope diagram (SEM) of the spiral carbon nanomaterial that the embodiment of the present invention 5 is prepared.Its In, (a) is SEM figures when multiplication factor is 80000;B () is the SEM figures that multiplication factor is 160000.
Fig. 6 is the scanning electron microscope diagram (SEM) of the spiral carbon nanomaterial that the embodiment of the present invention 6 is prepared.Its In, (a) is SEM figures when multiplication factor is 80000;B () is the SEM figures that multiplication factor is 160000.
Fig. 7 prepares the curve of the yield with temperature change of spiral carbon nanomaterial for the embodiment of the present invention.
Specific embodiment
The present invention is further introduced with reference to embodiment and accompanying drawing.
Embodiment 1
A kind of preparation method of nickel nano material, comprises the following steps:
Step 1:By the C of 0.1mol4H4O6KNa·4H2O is dissolved in 100mL distilled water, obtains the C of 1mol/L4H4O6KNa Solution, by the NiCl of 0.1mol2·4H2O is dissolved in 100mL distilled water, obtains the NiCl of 1mol/L2Solution;
Step 2:Under agitation, the NiCl for step 1 being prepared2Solution is slowly dropped to the C of step 1 preparation4H4O6KNa is molten In liquid, solution is changed into light green color from colourless, is filtered after reaction 5min, and filter cake first uses distillation water washing 3 times to neutral, then in rope Absolute ethanol washing 3h is used in family name's extractor, to remove the organic impurities of residual;
Step 3:The filter cake of step 2 gained is dried into 3h in the vacuum drying chamber at 90 DEG C, jade-green tartaric acid is obtained Nickel by powder;
Step 4:The tartaric acid nickel by powder that step 3 is obtained is laid in quartz boat, then equipped with tartaric acid nickel by powder Quartz boat be put into tube furnace, be evacuated to below 0.1Pa, being passed through hydrogen to gas atmosphere with the speed of 30mL/min reaches Normal pressure;500 DEG C are to slowly warm up to the heating rate of 5 DEG C/min, 1h is incubated at 500 DEG C, be then cooled to room temperature with stove, i.e., Obtain the nickel nano material.
Fig. 1 is the scanning electron microscope diagram (SEM) of the nickel nanometer that the embodiment of the present invention 1 is prepared.As shown in Figure 1, The nickel nano material that embodiment 1 is obtained is in bulk, and quality is more loose, nano particle of the surface with nickel, but size is uneven.
Embodiment 2
A kind of preparation method of nickel nano material, comprises the following steps:
Step 1:By the C of 0.1mol4H4O6KNa·4H2O is dissolved in 100mL distilled water, obtains the C of 1mol/L4H4O6KNa Solution, by the NiCl of 0.1mol2·4H2O is dissolved in 100mL distilled water, obtains the NiCl of 1mol/L2Solution;
Step 2:Under agitation, the NiCl for step 1 being prepared2Solution is slowly dropped to the C of step 1 preparation4H4O6KNa is molten In liquid, solution is changed into light green color from colourless, is filtered after reaction 5min, and filter cake first uses distillation water washing 3 times to neutral, then in rope Absolute ethanol washing 3h is used in family name's extractor, to remove the organic impurities of residual;
Step 3:The filter cake of step 2 gained is dried into 3h in the vacuum drying chamber at 90 DEG C, jade-green tartaric acid is obtained Nickel by powder;
Step 4:The tartaric acid nickel by powder that step 3 is obtained is laid in quartz boat, then equipped with tartaric acid nickel by powder Quartz boat be put into tube furnace, be evacuated to below 0.1Pa, being passed through hydrogen to gas atmosphere with the speed of 30mL/min reaches Normal pressure;600 DEG C are to slowly warm up to the heating rate of 5 DEG C/min, 1h is incubated at 600 DEG C, be then cooled to room temperature with stove, i.e., Obtain the nickel nano material.
Fig. 2 is the scanning electron microscope diagram (SEM) of the nickel nanometer that the embodiment of the present invention 2 is prepared.As shown in Figure 2, Nickel nano material that embodiment 2 is obtained is in bulk, and block structure is closely, and surface nano nickel particles have good uniformity.
Embodiment 3
A kind of preparation method of nickel nano material, comprises the following steps:
Step 1:By the C of 0.1mol4H4O6KNa·4H2O is dissolved in 100mL distilled water, obtains the C of 1mol/L4H4O6KNa Solution, by the NiCl of 0.1mol2·4H2O is dissolved in 100mL distilled water, obtains the NiCl of 1mol/L2Solution;
Step 2:Under agitation, the NiCl for step 1 being prepared2Solution is slowly dropped to the C of step 1 preparation4H4O6KNa is molten In liquid, solution is changed into light green color from colourless, is filtered after reaction 5min, and filter cake first uses distillation water washing 3 times to neutral, then in rope Absolute ethanol washing 3h is used in family name's extractor, to remove the organic impurities of residual;
Step 3:The filter cake of step 2 gained is dried into 3h in the vacuum drying chamber at 90 DEG C, jade-green tartaric acid is obtained Nickel by powder;
Step 4:The tartaric acid nickel by powder that step 3 is obtained is laid in quartz boat, then equipped with tartaric acid nickel by powder Quartz boat be put into tube furnace, be evacuated to below 0.1Pa, being passed through hydrogen to gas atmosphere with the speed of 30mL/min reaches Normal pressure;700 DEG C are to slowly warm up to the heating rate of 5 DEG C/min, 1h is incubated at 700 DEG C, be then cooled to room temperature with stove, i.e., Obtain the nickel nano material.
Fig. 3 is the scanning electron microscope diagram (SEM) of the nickel nanometer that the embodiment of the present invention 3 is prepared.From the figure 3, it may be seen that Nickel nano material that embodiment 3 is obtained is in bulk, and block structure is closely, and surface nano nickel particles have good uniformity.
Embodiment 4
A kind of method that nickel nano-catalytic prepares spiral carbon nanomaterial, comprises the following steps:
Step 1:By the C of 0.1mol4H4O6KNa·4H2O is dissolved in 100mL distilled water, obtains the C of 1mol/L4H4O6KNa Solution, by the NiCl of 0.1mol2·4H2O is dissolved in 100mL distilled water, obtains the NiCl of 1mol/L2Solution;
Step 2:Under agitation, the NiCl for step 1 being prepared2Solution is slowly dropped to the C of step 1 preparation4H4O6KNa is molten In liquid, solution is changed into light green color from colourless, is filtered after reaction 5min, and filter cake first uses distillation water washing 3 times to neutral, then in rope Absolute ethanol washing 3h is used in family name's extractor, to remove the organic impurities of residual;
Step 3:The filter cake of step 2 gained is dried into 3h in the vacuum drying chamber at 90 DEG C, jade-green tartaric acid is obtained Nickel by powder;
Step 4:The tartaric acid nickel by powder that step 3 is obtained is laid in quartz boat, then equipped with tartaric acid nickel by powder Quartz boat be put into tube furnace, be evacuated to below 0.1Pa, being passed through hydrogen to gas atmosphere with the speed of 30mL/min reaches Normal pressure;500 DEG C are to slowly warm up to the heating rate of 5 DEG C/min, 30min is incubated at 500 DEG C;After insulation terminates, hydrogen is closed Gas, acetylene gas 30min is passed through with the speed of 55mL/min;The last catalytic pyrolysis 1h under 500 DEG C, acetylene gas atmosphere;Instead Room temperature is naturally cooling to stove under an argon atmosphere after should terminating, that is, obtains the spiral carbon nanomaterial.
Fig. 4 is the scanning electron microscope diagram of the spiral carbon nanomaterial of the nickel that the embodiment of the present invention 4 is prepared (SEM).As shown in Figure 4, the spiral carbon nanomaterial that embodiment 4 is obtained includes spiral carbon nanotubes and spiral carbon nano-fiber, Consistent appearance, helicity is good, and carbon nanotube density is smaller.
Embodiment 5
A kind of method that nickel nano-catalytic prepares spiral carbon nanomaterial, comprises the following steps:
Step 1:By the C of 0.1mol4H4O6KNa·4H2O is dissolved in 100mL distilled water, obtains the C of 1mol/L4H4O6KNa Solution, by the NiCl of 0.1mol2·4H2O is dissolved in 100mL distilled water, obtains the NiCl of 1mol/L2Solution;
Step 2:Under agitation, the NiCl for step 1 being prepared2Solution is slowly dropped to the C of step 1 preparation4H4O6KNa is molten In liquid, solution is changed into light green color from colourless, is filtered after reaction 5min, and filter cake first uses distillation water washing 3 times to neutral, then in rope Absolute ethanol washing 3h is used in family name's extractor, to remove the organic impurities of residual;
Step 3:The filter cake of step 2 gained is dried into 3h in the vacuum drying chamber at 90 DEG C, jade-green tartaric acid is obtained Nickel by powder;
Step 4:The tartaric acid nickel by powder that step 3 is obtained is laid in quartz boat, then equipped with tartaric acid nickel by powder Quartz boat be put into tube furnace, be evacuated to below 0.1Pa, being passed through hydrogen to gas atmosphere with the speed of 30mL/min reaches Normal pressure;550 DEG C are to slowly warm up to the heating rate of 5 DEG C/min, 30min is incubated at 550 DEG C;After insulation terminates, hydrogen is closed Gas, acetylene gas 30min is passed through with the speed of 55mL/min;The last catalytic pyrolysis 1h under 550 DEG C, acetylene gas atmosphere;Instead Room temperature is naturally cooling to stove under an argon atmosphere after should terminating, that is, obtains the spiral carbon nanomaterial.
Fig. 5 is the scanning electron microscope diagram of the spiral carbon nanomaterial of the nickel that the embodiment of the present invention 5 is prepared (SEM).As shown in Figure 5, the spiral carbon nanomaterial that embodiment 5 is obtained includes spiral carbon nanotubes and spiral carbon nano-fiber, Consistent appearance, helicity is good, and carbon nanotube density is high.
Embodiment 6
A kind of method that nickel nano-catalytic prepares spiral carbon nanomaterial, comprises the following steps:
Step 1:By the C of 0.1mol4H4O6KNa·4H2O is dissolved in 100mL distilled water, obtains the C of 1mol/L4H4O6KNa Solution, by the NiCl of 0.1mol2·4H2O is dissolved in 100mL distilled water, obtains the NiCl of 1mol/L2Solution;
Step 2:Under agitation, the NiCl for step 1 being prepared2Solution is slowly dropped to the C of step 1 preparation4H4O6KNa is molten In liquid, solution is changed into light green color from colourless, is filtered after reaction 5min, and filter cake first uses distillation water washing 3 times to neutral, then in rope Absolute ethanol washing 3h is used in family name's extractor, to remove the organic impurities of residual;
Step 3:The filter cake of step 2 gained is dried into 3h in the vacuum drying chamber at 90 DEG C, jade-green tartaric acid is obtained Nickel by powder;
Step 4:The tartaric acid nickel by powder that step 3 is obtained is laid in quartz boat, then equipped with tartaric acid nickel by powder Quartz boat be put into tube furnace, be evacuated to below 0.1Pa, being passed through hydrogen to gas atmosphere with the speed of 30mL/min reaches Normal pressure;600 DEG C are to slowly warm up to the heating rate of 5 DEG C/min, 30min is incubated at 600 DEG C;After insulation terminates, hydrogen is closed Gas, acetylene gas 30min is passed through with the speed of 55mL/min;The last catalytic pyrolysis 1h under 600 DEG C, acetylene gas atmosphere;Instead Room temperature is naturally cooling to stove under an argon atmosphere after should terminating, that is, obtains the spiral carbon nanomaterial.
Fig. 6 is the scanning electron microscope diagram of the spiral carbon nanomaterial of the nickel that the embodiment of the present invention 6 is prepared (SEM).It will be appreciated from fig. 6 that the spiral carbon nanomaterial topographical difference that embodiment 6 is obtained is larger, product quality declines, wherein containing More micron order impurity.
Fig. 7 prepares the curve of the yield with temperature change of spiral carbon nanomaterial for the embodiment of the present invention, as shown in Figure 7, The yield that spiral carbon nanomaterial is prepared at 550 DEG C using the inventive method is up to 22391.0%, compared to current maximum product Rate is greatly improved.

Claims (6)

1. a kind of preparation method of nickel nano material, comprises the following steps:
Step 1:C4H4O6KNa·4H2O and NiCl2·4H2O reacts 5~10min in aqueous, and filtering, filter cake is first washed with water Wash to neutrality, 1~4h of absolute ethanol washing is then used in apparatus,Soxhlet's;
Step 2:The filter cake of step 1 gained is dried into 2~4h in the vacuum drying chamber at 80~100 DEG C, obtains tartaric acid nickel powder End;
Step 3:The tartaric acid nickel by powder that step 2 is obtained is placed in tube furnace, under 400~800 DEG C, hydrogen or argon gas atmosphere 30~60min of heat treatment, is then cooled to room temperature and obtains the nickel nano material with stove.
2. the preparation method of nickel nano material according to claim 1, it is characterised in that hydrogen described in step 3 or argon The gas flow of gas is 30~35mL/min.
3. a kind of method that nickel nano-catalytic prepares spiral carbon nanomaterial, comprises the following steps:
Step 1:C4H4O6KNa·4H2O and NiCl2·4H2O reacts 5~10min in aqueous, and filtering, filter cake is first washed with water Wash to neutrality, 1~4h of absolute ethanol washing is then used in apparatus,Soxhlet's;
Step 2:The filter cake of step 1 gained is dried into 2~4h in the vacuum drying chamber at 80~100 DEG C, obtains tartaric acid nickel powder End;
Step 3:The tartaric acid nickel by powder that step 2 is obtained is placed in tube furnace, under 400~800 DEG C, hydrogen or argon gas atmosphere 30~60min of heat treatment;After heat treatment terminates, hydrogen or argon gas are closed, acetylene gas are passed through, in 400~800 DEG C, acetylene gas Catalytic pyrolysis 1h under body atmosphere;Reaction is naturally cooling to room temperature with stove under an argon atmosphere after terminating, that is, obtain the spiral carbon Nano material.
4. the method that nickel nano-catalytic according to claim 3 prepares spiral carbon nanomaterial, it is characterised in that step 3 Described in the gas flow of hydrogen or argon gas be 30~35mL/min, the gas flow of the acetylene is 50~55mL/min.
5. the method that nickel nano-catalytic according to claim 3 prepares spiral carbon nanomaterial, it is characterised in that step 3 Described in heat treatment and catalytic pyrolysis temperature be 500~600 DEG C.
6. the method that nickel nano-catalytic according to claim 5 prepares spiral carbon nanomaterial, it is characterised in that step 3 Described in heat treatment and catalytic pyrolysis temperature be 550 DEG C.
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