CN108516534A - The method of catalyzed conversion solid carbon materials nano-carbon material - Google Patents
The method of catalyzed conversion solid carbon materials nano-carbon material Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01B32/158—Carbon nanotubes
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- C01B32/162—Preparation characterised by catalysts
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Abstract
A kind of method of catalyzed conversion solid carbon materials nano-carbon material is using the solid carbon materials such as the coal of different rank or different types of biomass as raw material, catalyst is added by way of grinding and is reacted under the high temperature conditions, then through cooling, salt pickling, distillation washing, ultrasonic vibration and centrifugal treating, nano-carbon material is obtained.The present invention prepares nano-carbon material using coal or biomass as raw material, raw material is extensive, simple for process, simple operation, high product value the features such as.
Description
Technical field
The present invention relates to a kind of preparation methods of nano-carbon material, and especially one kind is using carbonaceous organic material as raw material, alkalinity
Substance and iron compound are catalyst, carry out the method that nano-carbon material is made in pyrolytic conversion in the reactor.
Background technology
Nano-carbon material is by carbon atom through SP2The shapes such as the cylindric, spherical of hydridization formation, spheroid shape and synusia, ruler
It is very little in nano level carbon material.The unique structure of nano-carbon material makes it have high mechanical strength, conducts electricity very well, heat transfer property
The features such as fast, makes it obtain extensive use in fields such as composite material, electronic material and energy and materials.Qiu etc. [Qiu J S,
Zhang F, Zhou Y, et al. Carbon nanomaterials from eleven caking coals[J].
Fuel, 2002, 81(11):1509-1514.] it is carried out using the process of 11 kinds of coking coals preparation carbon nanotubes of arc process pair
It investigates, it is found that the thick yield of nano-carbon material obtained by different types of coal is different.Thess etc. [Thess A, Lee R,
Nikolaev P, et al. Crystalline ropes of metallic carbon nanotubes[J].
Science, 1996, 273(5274):483.] by 1200 DEG C laser irradiation contain the graphite rod of Ni, Co catalyst
Uniform diameter and the good nano-carbon material of crystallinity are prepared.[the Jose-Yacaman M, Miki- such as Jose-Yacaman
Yoshida M, Rendon L, et al. Catalytic growth of carbon microtubules with
fullerene structure[J]. Applied physics letters, 1993, 62(6):657-659.] passing through
Learn vapour deposition process using Fe as catalyst the nano-carbon material at the preparation of catalytic pyrolysis acetylene at 700 DEG C.Currently, arc discharge method
Main problem with laser evaporization method is equipment complexity, high energy consumption, cost of material height（7000 ~ 20000 $ of high purity graphite/ton）、
Yield is relatively low, and chemical vapour deposition technique raw material sources are wide, and working condition is mild, and yield and purity are high, is prepared by current magnanimity
The method of high-purity nano carbon material, but there are still cost of material it is high, production cost is high the deficiencies of.Therefore, society be badly in need of magnanimity,
Inexpensive nano-carbon material technology of preparing.
CN104952631A, which is disclosed, " prepares the side of Graphene/carbon nanotube composite material using solid phase cracking technique
Method ", this method with substances such as o-2 potassium acid acid anhydride, urea, nickel chloride, ammonium molybdates, boil, filter, is dense by heated, NaOH solution
Sulfuric acid scrubbing, the distillation processes synthetic phthalocyanine nickel such as water washing, then using Nickel Phthalocyanine as raw material, with the rate of 5 DEG C/min from room temperature
Rise to 300 DEG C and stop 1 hour, after be warming up to 350 DEG C stop 1 hour, after be warming up to 400 DEG C and stop 1 hour, then with 3
DEG C/heating rate of min is warming up to 500 DEG C and stops 4 hours, then the rate of 2 DEG C/min is warming up to 700 ~ 1000 DEG C simultaneously
It stops 4 ~ 8 hours, is finally naturally cooling to room temperature, obtains the composite material of graphene/carbon nano-tube.This method raw material Nickel Phthalocyanine
Preparation process it is complicated and need the risky operation steps such as soda boiling boiling, concentrated sulfuric acid pickling, while by Nickel Phthalocyanine prepare carbon nanotube/
The temperature program of graphene composite material is cumbersome, time-consuming so that this method is complicated for operation, flow is tediously long, it is huge to take, industry
It is relatively low to change application potential.
CN104555986A discloses " a kind of preparation method of carbon nano-tube being pyrolyzed based on solid phase ", it is characterized in that using
Sonogarshira and other compounds of the reaction synthesis with oxygen-containing group and triple carbon-carbon bonds, are then added under nitrogen protection
Co2(CO)8, corresponding organometal compound is prepared, finally product is placed in inert containers and carries out temperature-programmed pyrolysis, is obtained
Carbon nanotube.Nanosphere is changed into nanotube, existing main problem is required raw material by this method by introducing oxygen-containing group
A, B preparation process is complicated, time-consuming, and wherein A preparation process includes：45 DEG C are reacted 12 hours, and 50 DEG C are reacted 12 hours, and room temperature is stirred
It mixes 2 times overnight；B needs to be stirred overnight at room temperature 1 time, in addition, the agglomeration of product carbon nanotube is serious, quality is not high, needs
Follow-up decentralized processing is carried out, this method industrial applications potentiality are low.
CN106006604A discloses the method for solid carbon materials carbon nanotube " catalysis pyrolysis ", its main feature is that with coal or
Biomass is raw material, and catalyst is loaded to raw material surface by the way of dipping, then in height by the way of two sections of heatings
Reaction is carried out under the conditions of temperature prepares carbon nanotube.Find that this method catalyst load factor efficiency is low in experiment, dip time is for 24 hours
When, lignite catalyst load factor is about 25%, and anthracite catalyst load factor is about 18%, and low-load rate makes catalyst imitate
Fruit is poor, meanwhile, the dip time of catalyst and two sections of temperature-rise periods cause this method time-consuming, low production efficiency.In addition, the party
Catalyst is added to ferrocene in method, and since ferrocene is not soluble in water, when impregnating stirring, ferrocene is in carbon material surface
Distributed pole is uneven, meanwhile, ferrocene just completes distillation in Temperature Programmed Processes and escapes carbon material, far from catalysis reaction
Center, therefore the catalytic action of ferrocene is limited.Meanwhile this method product is only carbon nanotube, and cannot prepare graphene or
The nano-carbon materials such as Nano capsule.
Existing literature discloses report and shows there are many nano-carbon material technologies of preparing, but often in the presence of time-consuming, prepares
The problems such as process is complicated, yet there are no using alkaline matter and iron compound is that catalyst warp is simple, efficiently reaction process prepares carbon
The short-cut method of the nano-carbon materials such as nanotube, graphene or Nano capsule.
Invention content
The object of the present invention is to provide a kind of methods of catalyzed conversion solid carbon materials nano-carbon material, to solve to receive
The problem that rice carbon material preparation process is complicated, time-consuming, of high cost.
The present invention the taken measure that solves the above problems is to be achieved through the following technical solutions.
A kind of method of catalyzed conversion solid carbon materials nano-carbon material, the raw material composition and its content of the method are pressed
Weight ratio is incorporated the catalyst of 10-40% using the carbon material of 60-90% as raw material, carries out pyrolytic conversion in the reactor, is made
Nano-carbon material, specific method follow these steps to carry out：
（1）At 100-110 DEG C, 74 μm of carbon material is respectively less than to granularity and catalyst is dried, the two moisture is made to drop
To 0-1%（wt%）；
（2）By lapping mode by after drying carbon material and catalyst by proportion uniformly mix, be subsequently placed in reactor, then
Reactor is risen to 250-500 DEG C with the rate of 10-50 DEG C/min, then rises to 450-850 DEG C with the rate of 5-30 DEG C/min,
Then it is warming up to 750-1100 DEG C with the rate of 3-15 DEG C/min, constant temperature time 0-90 min are reacted；
（3）After reaction, it when reactor is cooled to room temperature, takes out surplus material and is put into hydrochloric acid solution, stir 10-
Then 60min is filtered and is washed with distilled water 5-8 times, obtain crude product；
（4）Crude product is placed in dispersion liquid, then ultrasonic vibration 10-40 min centrifuge 0- under conditions of 0-1500r/min
15min finally takes upper layer suspension and drying, that is, obtains nano-carbon material；
The catalyst is the mixture of alkaline matter and iron compound, and the ratio of iron compound is 0-20% in the mixture
（wt%）；
The alkaline matter is one kind in potassium carbonate, sodium carbonate, potassium hydroxide and sodium hydroxide, or arbitrary several mixing；
The iron compound is one kind in ferrous sulfate, ferrous sulfide, ferrous oxide, ferrous carbonate and ferrous disulfide, or
Arbitrary several mixing.
Based on the method for above-mentioned catalyzed conversion solid carbon materials nano-carbon material, further supplementary technology scheme is such as
Under.
The carbon material is one kind of peat, lignite, bituminous coal, sawdust and stalk, or arbitrary several mixing.
The reactor is stainless steel cauldron or crystal reaction tube.
The dispersion liquid is the one or both mixing in ethyl alcohol, N-Methyl pyrrolidone.
The nano-carbon material is carbon nanotube, one kind of Nano capsule, graphene, or arbitrary several mixing.
In the technical solution of aforementioned present invention, reaction process is concentrated mainly on the temperature rise period, and carbon material is from room temperature quilt
It is heated to that pyrolysis can occur during specified reaction temperature, it is anti-that pyrolysis main chemical reactions can be divided into first cracking
Answer, the reaction of the second pyrolysis of first pyrolysis product and three processes such as polycondensation reaction, corresponding temperature be respectively from low to high low temperature,
In mild high temperature.Wherein, it is happened at the first cracking reaction process of cold stage, representativeness chemical reaction has in carbon material
Bridged bond fracture generates the reactions such as free radical, aliphatic side chains cracking, oxygen-containing functional group cracking and low molecular compound cracking.In medium temperature
The representative chemical reaction in stage, the second pyrolysis reaction of first pyrolysis product has the reactions such as cracking reaction, bridged bond decomposition.High temperature
As long as the polycondensation reaction of the macromolecular containing phenyl ring occurs for the stage.It is above-mentioned it is several represent chemical reaction process can generate gaseous hydrocarbon and
Some carbon containing volatile materials, these hydrocarbon gas and carbon containing volatile materials are under the group of alkaline matter and iron use by splitting
Carbon conversion in gaseous hydrocarbon and volatile materials is finally carbon nanotube, graphene or nanometer by the processes such as solution, deposition, precipitation
The nano-carbon materials such as capsule.When containing abundant iron in carbon material, suitable alkaline matter is only added at this time and carries out catalysis turn
Change, you can obtain carbon nanotube；When containing in carbon material on a small quantity or being free of ferro element, suitable alkaline matter is only added at this time
Catalyzed conversion is carried out, graphene can be obtained；When containing in carbon material on a small quantity or being free of ferro element, it is incorporated a certain amount of basic species
Matter and iron compound carry out catalyzed conversion, and the mixture of the substances such as graphene, carbon nanotube or Nano capsule can be obtained.
Compared with prior art, the method for catalyzed conversion solid carbon materials nano-carbon material provided by the present invention is had
The advantages of having, is with good effect：Raw material needed for this method is the lower peat of degree of metamorphism, lignite, bituminous coal and straw
Deng deriving from a wealth of sources and price be relatively low, in addition, required instrument is common device, required precision is low, and nano-carbon material is prepared into
Originally it is greatly reduced.Catalyst can be added in carbon material only by way of grinding for this method, and only need by a speed change
Reaction can be completed in temperature-rise period, and operating process is easy, reaction process is succinct, when greatly reducing preparation needed for nano-carbon material
Between, method is simple and practicable.In addition, this method can the forms such as synthesizing carbon nanotubes, graphene and Nano capsule nano-carbon material,
Product is various.
Description of the drawings
Fig. 1 is the process flow chart of the method for the present invention.
Fig. 2 is carbon nanotube scanning electron microscopic picture prepared by embodiment 1.
Fig. 3 is carbon nanotube and graphene transmission electron microscope picture prepared by embodiment 2.
Fig. 4 is Nano capsule and graphene transmission electron microscope picture prepared by embodiment 3.
Fig. 5 is graphene transmission electron microscope picture prepared by embodiment 4.
Fig. 6 is graphene transmission electron microscope picture prepared by embodiment 5.
Specific implementation mode
In order to better understand the content of the present invention, the specific implementation mode of the present invention is made further below
It is bright, but the protection content of the present invention is not limited to following embodiment.
Embodiment 1
Such as attached drawing 1, the present embodiment 1 is tested by raw material of peat, iron content 0.7%（wt%）.
10g granularities are less than 74 μm, moisture 0.5% using mortar（wt%）The sodium hydroxide dried of peat and 1.5g it is equal
Even mixing is then placed in crystal reaction tube and seals reaction tube.Then reaction tube is warming up to 350 with the rate of 30 DEG C/min
DEG C, 600 DEG C then are warming up to the rate of 15 DEG C/min, is then warming up to 900 DEG C with the rate of 8 DEG C/min, after constant temperature 50min
Stop heating, wait for that reaction tube is cooled to room temperature, reaction mass is removed and placed in beaker, 40ml concentration then is added toward beaker
For the hydrochloric acid solution of 1mol/L, filters and be washed with distilled water 6 times after magnetic agitation 10min, then by remaining solid and 100ml
Ethyl alcohol mixing and ultrasonic vibration 10min, take supernatant and are dried, you can obtain carbon nanotube, carbon nanotube scanning electron microscope
See attached drawing 2.
Embodiment 2
Such as attached drawing 1, the present embodiment 2 is tested by raw material of lignite, iron content 0.1%（wt%）.
10g granularities are less than 74 μm, moisture 0.3% using mortar（wt%）Lignite and 5g drying potassium hydroxide and
The ferrous disulfide of 0.5g dryings, the ferrous sulfate of 0.5g dryings uniformly mix, and are then placed in crystal reaction tube and seal reaction
Pipe.Then reaction tube is warming up to 400 DEG C with the rate of 40 DEG C/min, is then warming up to 700 DEG C with the rate of 20 DEG C/min, so
1000 DEG C are warming up to the rate of 10 DEG C/min afterwards, stops heating after constant temperature 70min, waits for that reaction tube is cooled to room temperature, will react
Material is removed and placed in beaker, and the hydrochloric acid solution of a concentration of 1mol/L of 100ml, magnetic agitation 20min are then added toward beaker
After filter and be washed with distilled water 6 times, then remaining solid is mixed and ultrasonic vibration 20min with 100ml ethyl alcohol, is then existed
15min is centrifuged under conditions of 200 r/min, then take supernatant and is dried, you can obtains carbon nanotube and graphene
Mixture, mixture scanning electron microscope are shown in attached drawing 3.
Embodiment 3
Such as attached drawing 1, the present embodiment 3 is tested by raw material of bituminous coal, iron content 0.04%（wt%）.
10g granularities are less than 74 μm, moisture 0.9% using mortar（wt%）Bituminous coal and 3g drying potassium hydroxide and
The ferrous sulfide of 0.3g dryings uniformly mixes, and is then placed in stainless steel cauldron and seals.Then by reaction kettle with 50 DEG C/min
Rate be warming up to 500 DEG C, be then warming up to 800 DEG C with the rate of 30 DEG C/min, be then warming up to the rate of 15 DEG C/min
1100 DEG C, stops heating after constant temperature 90min, wait for that reaction kettle is cooled to room temperature, reaction mass is removed and placed in beaker, then
The hydrochloric acid solution of 70ml a concentration of 1mol/L is added toward beaker, filtered after magnetic agitation 30min and is washed with distilled water 8 times, so
Remaining solid is mixed to simultaneously ultrasonic vibration 30min with 100ml N-Methyl pyrrolidones afterwards, then under conditions of 500 r/min
10min is centrifuged, supernatant is then taken and is dried, you can obtains the mixture of Nano capsule and graphene, mixture transmission
Electronic Speculum is shown in attached drawing 4.
Embodiment 4
Such as attached drawing 1, the present embodiment 4 is tested by raw material of sawdust, iron content 0.01%（wt%）.
10g granularities are less than 74 μm, moisture 0.2% using mortar（wt%）Sawdust and 1g drying potassium hydroxide and 1g
The ferrous oxide that ferrous carbonate, the 0.35g of dry sodium carbonate, 0.15g dryings are dried uniformly mixes, and it is anti-to be then placed in stainless steel
It answers kettle and seals.Then reaction kettle is warming up to 300 DEG C with the rate of 20 DEG C/min, is then warming up to the rate of 10 DEG C/min
550 DEG C, 800 DEG C then are warming up to the rate of 5 DEG C/min, stops heating after constant temperature 30min, waits for that reaction kettle is cooled to room temperature,
Reaction mass is removed and placed in beaker, the hydrochloric acid solution of a concentration of 1mol/L of 45ml, magnetic agitation are then added toward beaker
It filters and is washed with distilled water 7 times after 60min, then mix remaining solid and 50ml N-Methyl pyrrolidones and 50ml ethyl alcohol
Merge ultrasonic vibration 40min, 5min is then centrifuged under conditions of 1000 r/min, supernatant is then taken and is dried, i.e.,
Graphene can be obtained, graphene transmission electron microscope is shown in attached drawing 5.
Embodiment 5
Such as attached drawing 1, the present embodiment 5 is tested by raw material of stalk, iron content 0.015%（wt%）.
10g granularities are less than 74 μm, moisture 0.6% using mortar（wt%）Stalk and 2g drying sodium hydroxide,
The potassium carbonate of 2.1g dryings and the ferrous carbonate of 0.2g dryings uniformly mix, and are then placed in stainless steel cauldron and seal.It connects
It and reaction kettle is warming up to 280 DEG C with the rate of 10 DEG C/min, then 470 DEG C are warming up to the rate of 8 DEG C/min, then with 3
DEG C/rate of min is warming up to 770 DEG C, stop heating after constant temperature 10min, waits for that reaction kettle is cooled to room temperature, reaction mass is taken out
And be put into beaker, the hydrochloric acid solution of a concentration of 1mol/L of 70ml is then added toward beaker, filters and is used in combination after magnetic agitation 45min
It distills water washing 5 times, then remaining solid is mixed to simultaneously ultrasonic vibration with 70ml N-Methyl pyrrolidones and 30ml ethyl alcohol
40min, then centrifuges 1min under conditions of 1400 r/min, then takes supernatant and is dried, you can graphene is obtained,
Graphene transmission electron microscope analysis is shown in attached drawing 6.
Claims (5)
1. a kind of method of catalyzed conversion solid carbon materials nano-carbon material, the raw material composition and its content of the method are by weight
Amount ratio is incorporated the catalyst of 10-40% using the carbon material of 60-90% as raw material, carries out pyrolytic conversion in the reactor, is made and receives
Rice carbon material, specific method follow these steps to carry out：
（1）At 100-110 DEG C, 74 μm of carbon material is respectively less than to granularity and catalyst is dried, the two moisture is made to drop
To 0-1%（wt%）；
（2）By lapping mode by after drying carbon material and catalyst by proportion uniformly mix, be subsequently placed in reactor, then
Reactor is risen to 250-500 DEG C with the rate of 10-50 DEG C/min, then rises to 450-850 DEG C with the rate of 5-30 DEG C/min,
Then it is warming up to 750-1100 DEG C with the rate of 3-15 DEG C/min, constant temperature time 0-90 min are reacted；
（3）After reaction, it when reactor is cooled to room temperature, takes out surplus material and is put into hydrochloric acid solution, stir 10-
Then 60min is filtered and is washed with distilled water 5-8 times, obtain crude product；
（4）Crude product is placed in dispersion liquid, then ultrasonic vibration 10-40 min centrifuge 0- under conditions of 0-1500r/min
15min finally takes upper layer suspension and drying, that is, obtains nano-carbon material；
The catalyst is the mixture of alkaline matter and iron compound, and the ratio of iron compound is 0-20% in the mixture
（wt%）；
The alkaline matter is one kind in potassium carbonate, sodium carbonate, potassium hydroxide and sodium hydroxide, or arbitrary several mixing；
The iron compound is one kind in ferrous sulfate, ferrous sulfide, ferrous oxide, ferrous carbonate and ferrous disulfide, or
Arbitrary several mixing.
2. the method as described in claim 1, the carbon material is one kind of peat, lignite, bituminous coal, sawdust and stalk, or is appointed
It anticipates several mixing.
3. the method as described in claim 1, the reactor is stainless steel cauldron or crystal reaction tube.
4. the method as described in claim 1, the dispersion liquid is that the one or both in ethyl alcohol, N-Methyl pyrrolidone is mixed
It closes.
5. the method as described in claim 1, the nano-carbon material is carbon nanotube, one kind of Nano capsule, graphene, or
Arbitrary several mixing.
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| CN110713179A (en) * | 2019-10-10 | 2020-01-21 | 太原理工大学 | Coal-based carbon nanotube for deoxidizing low-concentration coal bed gas and preparation and purification methods thereof |
| CN111547709A (en) * | 2020-05-09 | 2020-08-18 | 九江学院 | Biomass three-dimensional porous graphene and preparation method thereof |
| CN111620321A (en) * | 2020-05-25 | 2020-09-04 | 太原理工大学 | Method for preparing carbon nano tube by using high-sulfur high-sodium coal |
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| CN110713179B (en) * | 2019-10-10 | 2023-02-28 | 太原理工大学 | Coal-based carbon nano tube for deoxidizing low-concentration coal bed gas and preparation and purification methods thereof |
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| CN111620321B (en) * | 2020-05-25 | 2023-04-14 | 太原理工大学 | Method for preparing carbon nano tube by using high-sulfur high-sodium coal |
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Application publication date: 20180911 |