CN109941984A - The preparation method and carbon micron tube of carbon micron tube - Google Patents
The preparation method and carbon micron tube of carbon micron tube Download PDFInfo
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- CN109941984A CN109941984A CN201910385662.8A CN201910385662A CN109941984A CN 109941984 A CN109941984 A CN 109941984A CN 201910385662 A CN201910385662 A CN 201910385662A CN 109941984 A CN109941984 A CN 109941984A
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Abstract
The application proposes the preparation method and carbon micron tube of a kind of carbon micron tube, wherein the preparation method of carbon micron tube, comprising: corn stigma is warming up under protective gas calcination temperature, the first duration is kept to obtain carbon micron tube at calcination temperatures by calcining step.The application use with it is from a wealth of sources, be easy to collect, the corn stigma of enormous amount prepares carbon micron tube as raw material; it is low in cost; it is easy to large-scale production; and the carbon micron tube of preparation is advantageous in length; twenties centimetres can be reached; much larger than the existing carbon micron tube using preparations such as catkin, Yang Xu, mosses; furthermore; in this application; calcination temperature is considerably reduced with acid soak corn stigma before being calcined; it is minimum to obtain carbon micron tube in 200 DEG C of temperature lower calcination, to further reduce the cost and the requirement to equipment.
Description
Technical field
This application involves Material Fields, the in particular to preparation method and carbon micron tube of carbon micron tube.
Background technique
Carbon micron tube not only has the excellent performance of carbon nanotube, such as very high mechanical strength, good conductive and thermally conductive
Performance, excellent chemistry and high temperature stability performance, and have the caliber of unique micro-meter scale, the visitor of larger size can be filled
Body molecule, thus led in medication chemistries material such as catalyst carrier, hydrogen storage material, electrode material, absorbing material, medicament slow release etc.
There is broad prospect of application in domain, this is that have the carbon nanotube of minimum caliber incomparable.The preparation side of carbon micron tube at present
Method mainly has chemical vapour deposition technique (CVD), catalyst method, template, self-assembly method, spin processes, biomass carbonization method etc..Its
In, using natural structure of biomass through high temperature cabonization prepare carbon micron tube with low in cost, simple process, morphology controllable, can
The characteristics of prepare with scale, is suitable for amplification production.Application No. is in 201010590224.4 patent of invention, using Yang Xuhe
Catkin is that raw material prepares carbon micron tube；Application No. is in 201711362149.4 patent of invention, use kapok to be raw material through pre-
Processing, crosslinking, carbonization, activation, post-processing obtain hollow carbon micro-pipe；Application No. is in 201710967784.9 patent of invention,
Moss is used to prepare carbon pipe for raw material.
In the prior art, when preparing carbon micron tube as biomass using catkin, Yang Xu, moss, there are the following problems:
One side poplar wadding, catkin and the natural yield of moss are lower, and are not easily recycled, and are highly detrimental to be mass produced, if specially
Door lease place production poplar wadding, catkin and moss can greatly improve production cost again.On the other hand, Yang Xu, catkin and moss
Size it is smaller, it is difficult to prepare the carbon micron tube that axial length is more than 10cm.
In addition, in the prior art, the technique that high-temperature calcination is often used when preparing carbon micron tube, calcination temperature is minimum
No less than 300 DEG C, and calcination temperature is higher, the bigger requirement to device security of energy consumption is higher, and therefore, reducing calcination temperature can
Energy consumption is greatly lowered and to the requirement of equipment, to reduce cost.
Summary of the invention
This application provides a kind of preparation methods of carbon micron tube and carbon micron tube for solving the above problems.
To solve the above-mentioned problems, as the one aspect of the application, a kind of preparation method of carbon micron tube is provided, is wrapped
It includes:
Corn stigma is warming up to calcination temperature, when keeping first at calcination temperatures by calcining step under protective gas
Length obtains carbon micron tube.
Optionally, in calcining step, calcination temperature is 300-1000 DEG C, first when a length of 1-10h.
Optionally, before calcining step, further includes:
Soaking step takes out after corn stigma is impregnated the second duration in acid solution.
Optionally, acid solution is one of hydrochloric acid, nitric acid or sulfuric acid, alternatively,
Acid solution is the mixed liquor of a variety of acid in hydrochloric acid, nitric acid and sulfuric acid.
Optionally, the concentration of acid solution is 0.1-2mol/L, and/or, second when a length of 6-12h.
Optionally, the concentration of acid solution is 0.1-2mol/L, second when a length of 6-12h；
In calcining step, calcination temperature is 250-1000 DEG C, first when a length of 1-10h.
Optionally, acid solution is the sulfuric acid of mass fraction 30-70%, second when a length of 10-12h, acid solution and corn stigma
Mass ratio be 1-10:1, calcination temperature be 200-240 DEG C.
Optionally, after soaking step, before calcining step, further includes:
Cleaning step washs corn stigma to neutral and dry；
Optionally, protective gas is nitrogen or argon gas.
The application also proposes a kind of carbon micron tube, is prepared using any the method that the application proposes, carbon micron tube
Carbon content is 92at%-94at%, oxygen content 5at%-7at%, nitrogen content 1at%-2at%, and internal diameter is 11.5 μm -47
μm, wall thickness is 5.2 μm -21.1 μm, apparent density 0.16-0.18g/cm3。
Present applicant proposes a kind of preparation method of carbon micron tube and carbon micron tube, the application use have it is from a wealth of sources,
Be easy to collect, the corn stigma of enormous amount prepares carbon micron tube as raw material, low in cost, be easy to large-scale production, and system
Standby carbon micron tube is advantageous in length, can reach twenties centimetres, uses catkin, Yang Xu, moss etc. much larger than existing
The carbon micron tube of preparation, in addition, in this application, considerably reducing calcining temperature with acid soak corn stigma before being calcined
Degree, it is minimum to obtain carbon micron tube in 200 DEG C of temperature lower calcination, thus further reduce the cost and the requirement to equipment, this
Outside, in the preparation method that the application proposes, without using activator, preparation process is simple, mild condition, and yield is high.
Detailed description of the invention
Fig. 1 is a kind of preparation method of carbon micron tube in the embodiment of the present application；
Fig. 2 is the length schematic diagram of corn stigma and the carbon micron tube of preparation in the embodiment of the present application；
Fig. 3 is the scanning electron microscope diagram of corn stigma in the embodiment of the present application；
Fig. 4 is the scanning electron microscope diagram of the carbon micron tube prepared in the embodiment of the present application 3；
Fig. 5 is the scanning electron microscope diagram of the carbon micron tube prepared in the embodiment of the present application 4；
Fig. 6 is the length schematic diagram of corn stigma and the carbon micron tube of preparation in the embodiment of the present application 9.
Specific embodiment
To keep the purposes, technical schemes and advantages of the application clearer, below in conjunction with the application specific embodiment and
Technical scheme is clearly and completely described in corresponding attached drawing.Obviously, described embodiment is only the application one
Section Example, instead of all the embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not doing
Every other embodiment obtained under the premise of creative work out, shall fall in the protection scope of this application.
It should be noted that the description and claims of this application and term " first " in above-mentioned attached drawing, "
Two " etc. be to be used to distinguish similar objects, without being used to describe a particular order or precedence order.It should be understood that using in this way
Data be interchangeable under appropriate circumstances, so as to embodiments herein described herein can in addition to illustrating herein or
Sequence other than those of description is implemented.In addition, term " includes " and " having " and their any deformation, it is intended that cover
Covering non-exclusive includes to be not necessarily limited to for example, containing the process, method of a series of steps or units, device, product or air-conditioning
Step or unit those of is clearly listed, but may include be not clearly listed or for these process, methods, product
Or other step or units that air-conditioning is intrinsic.
Embodiment 1
In the prior art, when preparing carbon micron tube as biomass using catkin, Yang Xu, moss, due to poplar wadding, catkin
It is lower with the natural yield of moss, it can only be produced in particular season, and be not easily recycled, be highly detrimental to be mass produced, such as
Fruit specially leases place production poplar wadding, catkin and moss can greatly improve production cost again.
Corn is the main cereal crops in China, 3544.5 ten thousand hectares of China's corn seeding area in 2017, and total output is
2.16 hundred million tons, the corn stigma yield as by-product is at 1,000 ten thousand tons or so.However most of corn stigma cannot be utilized adequately
And it is dropped.
The application proposes a kind of preparation method of carbon micron tube, comprising:
Corn stigma is warming up to calcination temperature, when keeping first at calcination temperatures by calcining step under protective gas
Length obtains carbon micron tube.
Specifically, calcination temperature is 300-1000 DEG C, described first when a length of 1-10h, in calcining step on corn stigma
The evaporation of water is adsorbed, the thermal decomposition of the components such as removing and lignin, cellulose, hemicellulose in conjunction with water finally makes
Corn stigma is dehydrated into carbon micron tube.One of them main inventive point of the application is that corn stigma is used to prepare carbon micron as raw material
Pipe, in the prior art with poplar wadding, catkin and moss technical solution compared with, the yield of corn stigma is far longer than poplar wadding, catkin
And moss, and in harvesting corn, corn stigma largely flocks together as byproduct, is highly susceptible to being recycled, cost
Well below poplar wadding, catkin and moss, prepare with scale carbon micron tube can be realized without leasing place production corn stigma, and adopt
When using poplar wadding, catkin and moss as raw material, naturally-produced poplar wadding, catkin and moss low output, and it is distributed dispersion, hardly possible
With recycling, it is highly detrimental to large-scale production.The application prepares carbon micron tube as raw material using corn stigma and is greatly lowered
The cost of large-scale production.
On the other hand, it is sent out after being observed using carbon micron tube of the microscope to the method preparation proposed using the application
It is existing, when the length of corn stigma of the application using length not less than 30cm, the carbon micron tube prepared at this time is not less than 20cm, with poplar
Wadding, catkin prepare carbon micron tube as raw material with moss and compare, since poplar wadding, catkin and the size of moss are smaller, rarely
Poplar wadding, catkin and moss of the size greater than 10cm, the axial length of the carbon micron tube of preparation often only have several centimetres, the application system
Standby carbon micron tube is because the axial length of corn stigma is longer, as long as it is enough axial long to guarantee that the corn stigma selected has
Degree can easily prepare the carbon micron tube that length reaches 10 centimetres or more even up to more than 20 centimetres.
Optionally, as shown in Figure 1, the application proposes the preparation method of another carbon micron tube, including
Soaking step takes out after corn stigma is impregnated the second duration in acid solution；
Corn stigma is warming up to calcination temperature, when keeping first at calcination temperatures by calcining step under protective gas
Length obtains carbon micron tube.
Optionally, after soaking step, before calcining step, further includes: cleaning step washs corn stigma into
Property and drying；The process of cleaning is to prevent from polluting to remove the acid solution on corn stigma surface.
Optionally, the acid solution is one of hydrochloric acid, nitric acid or sulfuric acid, alternatively, the acid solution is hydrochloric acid, nitric acid
With the mixed liquor of acid a variety of in sulfuric acid.The concentration of the acid solution is 0.1-2mol/L.Optionally, second impregnated in acid solution
Shi Changwei 6-12h.
In the present embodiment, the effect that the immersion treatment of acid solution is carried out to corn stigma includes reducing sintering temperature and going to decontaminate
Stain, acid solution itself can remove the attachment on corn surface, and some alkaline matters contained by corn stigma are removed, organic moiety
Hydrolysis, soluble metal ion are dissolved, and are conducive to the quality for improving carbon micron tube, and on the other hand, acid solution has certain
Dehydrating effect, can partially remove the moisture in corn stigma surface fiber element, realize it is partially carbonized, due to corn stigma surface
Water is removed, so the cellulose in the middle part of corn stigma is easy to be heated dehydration, in calcination process later so as to substantially
Degree, which reduces, calcines required temperature.In the prior art often using lye (such as NaOH, KOH or strong acid weak base salt) to life
Substance is handled, this is because plant cell wall contains hemicellulose, dissolution is easy under alkaline environment, the application uses
Acid solution especially carries out decontamination and dehydration carbonization treatment with sulfuric acid, the hydrone that will directly remove in cellulose, without molten
Cell wall is solved, and reduces calcination temperature.Preferably, be 0.1-2mol/L in the concentration of acid solution, second when a length of 6-12h
When, in calcining step, calcination temperature can be 250-1000 DEG C, described first when a length of 1-10h.
Calcining step can carry out in tube furnace, in this application, because having carried out acid soak to corn stigma,
It can be calcined using lower temperature, so that energy consumption and the requirement to equipment are considerably reduced, in the prior art,
Calcination temperature when preparing carbon micron tube is higher than 300 DEG C mostly, needs a large amount of energy and the high requirements on the equipment.It is optional
, calcine a length of 1-10h, preferably 2h and 4h when used first.
Preferably, in this application, a length of 10-12h when the sulfuric acid that acid solution is mass fraction 30-70%, second, and
When the mass ratio of corn stigma and the acid solution is 1-10:1, calcination temperature can be used 200-240 DEG C.Calcination temperature in the application
Minimum temperature is 200 DEG C, shortest time 1h, can be realized in the case where being far below temperature and time in the prior art fast
The low temperature preparation carbon micron tube of speed.It is impregnated using sulfuric acid solution there are two effect, first is that promotion lignin, cellulose, hemicellulose
The hydrolysis of the components such as element；It is carbonized second is that can be dehydrated to corn stigma, the two effects finally reduce carburizing temperature.It needs
It is noted that the concentration of sulfuric acid needs to control in mass fraction 30-70%, and the mass ratio of sulfuric acid and corn stigma is 1-10:
1.When sulfuric acid concentration is too low, corn stigma surface will be hydrolyzed, carbonizing degree is incomplete, cannot reach the work for being substantially reduced calcination temperature
With；When sulfuric acid concentration is too high, corn stigma can be made thoroughly to be carbonized, corn stigma is made to collapse, destroy the cellular structure of carbon pipe.
Optionally, before soaking step, including prerinse step, prerinse is carried out to corn.Cleaning process can adopt
With the prior art, it can be and cleaned with clear water, be also possible to clean to neutrality with clear water with after caustic dip.
Embodiment 2
The corn stigma that length is 32cm is chosen, cleans, drying, is put into tube furnace and is warming up to 600 DEG C under nitrogen atmosphere, protect
3h is held, is taken out after cooling, the carbon micron tube of a length of 21cm is made.
The length of the carbon micron tube of the corn stigma and preparation that are used in the present embodiment as shown in Fig. 2, carbon micron tube internal diameter
It is 11.5 microns, wall thickness is 5.2 microns, and structure is the identical hollow pipeline in both ends, and crystal form is unformed carbon structure, and conductivity reaches
To 3.1 × 105S/m, from the figure, it can be seen that axial length is reduced carbon micron tube after calcining, present inventor's warp
Overtesting discovery, when the length of the corn stigma of selection is not less than 30cm, it is ensured that the length of the carbon micron tube of preparation reaches
20cm or more, therefore the application preferably uses the corn stigma of 30cm or more.
Embodiment 3
10 grams of corn stigmas are weighed, corn stigma length is 22cm, and the scanning electron microscopic picture of corn stigma is as shown in figure 3, corn stigma
Wall thickness is dipped in 0.1mol/L nitric acid solution in 16 microns after cleaning up corn stigma, and deionization is washed after 12 hours
It is dry to neutrality.Sample after drying is put into tube furnace and is warming up to 600 DEG C under nitrogen atmosphere, 3h is kept, is taken after cooling
Out, carbon micron tube is made, the length of carbon micron tube is 16cm, and attached drawing 4 is the scanning electron microscope (SEM) photograph of prepared carbon micron tube, preparation
The internal diameter of obtained carbon micron tube is 40.1 microns, and wall thickness is 12.3 microns, and structure is the identical hollow pipeline in both ends, and crystal form is
Unformed carbon structure, conductivity reach 3.2 × 105S/m carries out atom content measurement, test result to the carbon micron tube of preparation
Show that the carbon content in carbon micron tube is 93.3at%, oxygen content 5.23at%, nitrogen content 1.47at%, the application selects
The raw material for preparing be natural biomass corn stigma, there is corn stigma itself natural hollow pipeline configuration to be very suitable to prepare carbon micron
Pipe, carbon content is high, while having nitrogen, and the carbon micron tube that preparation may be implemented has natural N doping performance, and N doping is made
At the variation of local charge density, the formation of electric double layer is contributed, the electro-chemical activity of material can be improved and improves electrolysis
Liquid wetability in the material simultaneously increases specific capacitance, and avoids artificial nitrating and cause anomalad and structure to carbon micron tube
On destruction.
Embodiment 4: weighing 10 grams of corn stigmas, be dipped in 2mol/L nitric acid solution after cleaning up, deionization after 12 hours
It is washed to neutrality, it is dry.Sample after drying is put into tube furnace and is warming up to 800 DEG C under nitrogen atmosphere, 1h is kept, after cooling
It takes out, carbon micron tube is made.Attached drawing 5 is prepared carbon micron tube.It can see from Fig. 3 and Fig. 5, the carbon in the present embodiment
The tube wall of micron tube is in 5 microns, far below 16 microns of wall thickness of corn stigma.Atom content is carried out to the carbon micron tube of preparation
Measurement, test result show that the carbon content in carbon micron tube is 93.86at%, oxygen content 4.83at%, and nitrogen content is
1.31at%, conductivity are 3.2 × 105S/m。
Embodiment 5: weighing 10 grams of corn stigmas, be dipped in 2mol/L sulfuric acid solution after cleaning up, deionization after 12 hours
It is washed to neutrality, it is dry.Sample after drying is put into tube furnace and is warming up to 260 DEG C under nitrogen atmosphere, 3h is kept, after cooling
It takes out, carbon micron tube is made.
Embodiment 6: weighing corn stigma, is dipped in 1.5mol/L sulfuric acid solution after cleaning up, and spends after impregnating 12 hours
Corn stigma is washed till neutrality by ionized water, dry.Corn stigma sample after drying is put into tube furnace under nitrogen atmosphere and is warming up to
290 DEG C, 3h is kept, is taken out after cooling, carbon micron tube is made.
Embodiment 7: weighing 10 grams of corn stigmas, is dipped in mass fraction 30%L sulfuric acid solution after cleaning up, sulfuric acid and jade
The mass ratio of rice palpus is 5:1, and corn stigma is washed till neutrality with deionized water after impregnating 12 hours, dry.By the corn after drying
Palpus sample, which is put into tube furnace, is warming up to 240 DEG C under nitrogen atmosphere, keep 3h, take out after cooling, carbon micron tube is made.
Embodiment 8: weighing 10 grams of corn stigmas, is dipped in 50% sulfuric acid solution of mass fraction after cleaning up, sulfuric acid and jade
The mass ratio of rice palpus is 5:1, and corn stigma is washed till neutrality with deionized water after impregnating 12 hours, dry.By the corn after drying
Palpus sample, which is put into tube furnace, is warming up to 220 DEG C under nitrogen atmosphere, keep 3h, take out after cooling, carbon micron tube is made.
Embodiment 9: weighing 10 grams of corn stigmas, and length 20cm is dipped in 50% sulphur of mass fraction after cleaning up corn stigma
In acid solution, the mass ratio of sulfuric acid and corn stigma is 10:1, and corn stigma is washed till neutrality with deionized water after impregnating 12 hours, is done
It is dry.Corn stigma sample after drying is put into tube furnace and is warming up to 200 DEG C under nitrogen atmosphere, 3h is kept, is taken out after cooling, made
16cm carbon micron tube, 40 microns of caliber, 7.47 microns of wall thickness.
Embodiment 10: weighing 10 grams of corn stigmas, is dipped in 70% sulfuric acid solution of mass fraction after cleaning up, sulfuric acid and jade
The mass ratio of rice palpus is 5:1, and corn stigma is washed till neutrality with deionized water after impregnating 12 hours, dry.By the sample after drying
It is put into tube furnace and is warming up to 200 DEG C under nitrogen atmosphere, keep 3h, taken out after cooling, carbon micron tube is made.
Embodiment 11: weighing 10 grams of corn stigmas, is dipped in 70% sulfuric acid solution of mass fraction after cleaning up, sulfuric acid and jade
The mass ratio of rice palpus is 10:1, and deionized water is washed till neutrality after 12 hours, dry.Sample after drying is put into nitrogen in tube furnace
It is warming up to 200 DEG C under gas atmosphere, keeps 1h, is taken out after cooling, carbon micron tube is made.
The application also proposes a kind of carbon micron tube, proposes prepared by any the method using the application, the carbon of carbon micron tube
Content is 92at%-94at%, oxygen content 5at%-7at%, nitrogen content 1at%-2at%, and internal diameter is 11.5 μm of -47 μ
M, wall thickness are 5.2 μm -21.1 μm.The carbon micron tube length of preparation is up to twenties centimetres, and whole straight, there are fold, table in surface
Sight density is 0.16-0.18g/cm3, compared to the carbon micron tube prepared using catkin or moss, the carbon micron of the application preparation
More lengthening, straight and tube wall are thicker, and easily operated single carbon micron tube is easy, does not need that carbon micron can be completed by optical microscopy
Pipe is selected, and machinability is good, convenient for the operation of micro fabrication.Since prepared carbon micron tube has big major diameter
Than providing excellent storage capacity.Prepared carbon micron tube exports electronics from whole continuous carbon pipe, because
This is with excellent conductivity.Since prepared carbon micron tube internal diameter is 11.5-47 microns, as load channel, can meet
Demand of the fields such as biological medicine conveying, biochip, microelectronics, microfluidic device to large scale pipeline.The foregoing is merely
Preferred embodiment of the present application is not intended to limit this application, and for those skilled in the art, the application can be with
There are various modifications and variations.Within the spirit and principles of this application, any modification, equivalent replacement, improvement and so on,
It should be comprising within the scope of protection of this application.
Claims (10)
1. a kind of preparation method of carbon micron tube characterized by comprising
Corn stigma is warming up to calcination temperature by calcining step under protective gas, keeps growing when first at calcination temperatures
To carbon micron tube.
2. the preparation method of carbon micron tube according to claim 1, which is characterized in that
In calcining step, calcination temperature is 300-1000 DEG C, described first when a length of 1-10h.
3. the preparation method of carbon micron tube according to claim 1, which is characterized in that before calcining step, further includes:
Soaking step takes out after corn stigma is impregnated the second duration in acid solution.
4. the preparation method of carbon micron tube according to claim 3, which is characterized in that
The acid solution is one of hydrochloric acid, nitric acid or sulfuric acid, alternatively,
The acid solution is the mixed liquor of a variety of acid in hydrochloric acid, nitric acid and sulfuric acid.
5. the preparation method of carbon micron tube according to claim 3 or 4, which is characterized in that
The concentration of the acid solution is 0.1-2mol/L, and/or, described second when a length of 6-12h.
6. the preparation method of carbon micron tube according to claim 5, which is characterized in that
The concentration of the acid solution is 0.1-2mol/L, described second when a length of 6-12h；
In calcining step, calcination temperature is 250-1000 DEG C, described first when a length of 1-10h.
7. the preparation method of carbon micron tube according to claim 4, which is characterized in that
The acid solution is the sulfuric acid of mass fraction 30-70%, described second when a length of 10-12h, the acid solution and the jade
The mass ratio of rice palpus is 1-10:1, and the calcination temperature is 200-240 DEG C.
8. according to claim 3,4,6 or the preparation method of 7 described in any item carbon micron tubes, which is characterized in that walked impregnating
After rapid, before calcining step, further includes:
Cleaning step washs corn stigma to neutral and dry.
9. the preparation method of any one of -4,6 or 7 carbon micron tubes stated according to claim 1, which is characterized in that
The protective gas is nitrogen or argon gas.
10. a kind of carbon micron tube, which is characterized in that using such as any the method preparation of claim 1-9；
The carbon content of the carbon micron tube is 92at%-94at%, oxygen content 5at%-7at%, nitrogen content 1at%-
2at%, internal diameter are 11.5 μm -47 μm, and wall thickness is 5.2 μm -21.1 μm, apparent density 0.16-0.18g/cm3。
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| CN112047322A (en) * | 2020-08-19 | 2020-12-08 | 广东工业大学 | Modified carbon microtube carbonized by silver willow and preparation method and application thereof |
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| CN112047322A (en) * | 2020-08-19 | 2020-12-08 | 广东工业大学 | Modified carbon microtube carbonized by silver willow and preparation method and application thereof |
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