CN101503188B - Combustion synthesis apparatus for fullerenes - Google Patents
Combustion synthesis apparatus for fullerenes Download PDFInfo
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- CN101503188B CN101503188B CN2009101111528A CN200910111152A CN101503188B CN 101503188 B CN101503188 B CN 101503188B CN 2009101111528 A CN2009101111528 A CN 2009101111528A CN 200910111152 A CN200910111152 A CN 200910111152A CN 101503188 B CN101503188 B CN 101503188B
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Abstract
The invention relates to a fullerene combustion synthesis device which is safe, easy to control and low in cost, and has a certain yield. The device is provided with a combustion furnace, a burner nozzle, a telescope-feed condenser tube, a filtration tank, a liquid filter, a heat exchanger, a vacuum pump, a vacuum regulating system, an ignition system, a gas supply and control system and a vacuum degree testing and displaying device; wherein, the burner nozzle is fixed on a base plate of the combustion furnace; the telescope-feed condenser tube is connected with downstream of a furnace cover of the combustion furnace; the filtration tank is connected with the telescope-feed condenser tube by a vacuum quick release flange; the liquid filter is connected with a filter tube by a pipeline; the heat exchanger is connected with the liquid filter by the pipeline; the vacuum pump is connected with the heat exchanger by a vacuum ball valve; the vacuum regulating system is provided with an air vent valve and the vacuum ball valve, and the ignition system is connected with a furnace body; the vacuum degree testing and displaying device is communicated with the furnace body of the combustion furnace; and the gas supply and control system is connected with the burner nozzle by an air supply duct.
Description
Technical field
The present invention relates to a kind of combustion synthesis apparatus for fullerenes, especially relate to the common and oxygen incendiary method of a kind of employing acetylene and benzene vapor and prepare C
60, C
70And the device of fullerene derivate and other carbon bunch.
Background technology
Since soccerballene was found in 1985, soccerballene had just caused the extensive concern of scientific circles.Aspects such as the synthetic method of soccerballene and potential using value are studied widely, and theoretical investigation simultaneously is also more and more deep, for experimental study provides necessary theoretical direction, make it become a popular domain in the chemical research rapidly.Since C60 was found, people never stopped for the exploration of soccerballene synthetic method.The synthetic method of soccerballene mainly comprises laser evaporation graphite method, high-frequency resistance stove heating evaporation graphite method, graphite arc discharge method, solar heating graphite method, naphthalene pyrolysis method, microwave process for synthesizing, electric glow discharge method and flame combustion process etc., these methods provide all more options for soccerballene synthetic, have also opened up road for the formation mechanism of research soccerballene.
In 1985～1989 years, people such as Homann set up the experiment of a series of hydrocarbon polymer flame method, and the gas of combustion flame different heights is carried out sampling analysis, detected the ion that has identical molecular weight with the soccerballene that arc process obtains.1991, find and identified C in the Howard research group of MIT benzene/oxygen flame under low pressure
60And C
70Existence, and carried out systematic research, the factors such as kind, gas take-off rate and concentration of their research the is clear and definite pressure of system, C/O atomic ratio, temperature and diluent gas are to C in the benzene/oxygen laminar flame of premix
60And C
70Productive rate has material impact.Studies show that afterwards, acetylene, divinyl, toluene and naphthalene etc. are made raw material and also can be accessed soccerballene, and just to compare productive rate lower with benzene oxygen.
Combustion system in the flame method mainly contains two kinds, i.e. premixed combustion and diffusion combustion.Premixed combustion be fuel gas and oxygen before entering combustion equipment just uniform mixing become the combustion system of inflammable mixture, this is the most basic combustion system.To be fuel gas and oxygen from separately source of release reach by diffusion diffusion combustion is in contact with one another, and burns under the energy excitation that ignition source provided, and combustible gas carried out with mixing in combustion processes of oxygen, i.e. the burning while mixing.
Compare with graphite arc method fullerene synthesis, hydrocarbon fuel prepares soccerballene by flame combustion process and has following advantage: the C that flame method generates
70/ C
60Ratio ranges reaches 0.26～5.7, and graphite method of evaporating variable range has only 0.02～0.18, by adjusting the output that flame condition can significantly improve the more expensive big soccerballene of some specific product, particularly price; Preparation cost is lower.The flame method desired raw material is organic-fuels such as benzene, acetylene, and the high purity graphite rod cost that uses in the graphite arc method significantly reduces; The required energy of soccerballene generation all is to be provided by burning self liberated heat in the flame method, and the graphite arc rule needs highdensity energy input, so running cost is also more cheap; Compare with arc method before, fuel gas and oxygen can access the successive supply in the combustion method, combustion synthesis method makes that the reaction feed process can continue to carry out, and new a large amount of methods that prepare soccerballene not only are provided, and can in very large range control the distribution of product.
The at present external flame synthesizer of beginning to take shape all adopt without exception the mode of premixed combustion organize gas burn synthetic (1, J.B.Howard; J.T.Mckinnon; Y.Makarovsky, A.L.Lafleur, M.E.Johnson.Fullerenes C
60And C
70In flames.[J], Nature 1991,352,139-141; 2, Alford et al., U.S.Pat.No.7,279,137, B2).Premixed combustion can reach higher efficiency of combustion, and flame is shorter, and the excess coefficient of the required oxygen that burns is less.But such combustion system can take off fire and extinguish or be difficult to and light when the mixed gas flow velocity is big, otherwise tempering can take place, flame ignite and flame control aspect harshness requirement is accurately arranged, antibody system fluctuation ability, this is even Howard (Howard et al., U.S.Pat.No.5,273,729) also have to admit flame ignite and control is one " art ".And relative with it, diffusion combustion is safety and steady then, and is the advantage that has premixed combustion to be difficult to be equal to aspect the fluctuation at easily control property, turndown ratio and antibody.Diffusion combustion also is the more a kind of combustion system of report recent years, is considered to more promising combustion system.Report (S.M.Lee, S.S.Yoon, and S.H.Chung, Synergistic effect on soot formationin counterflow diffusion flames of ethylene/propane mixtures with benzene addition.[J] Combustionand Flame 2004,136,493-500) be specifically designed to soccerballene synthetic dispersion device or too complicated, or system mainly to adopt be that glass material (is seen the applicant's Chinese invention patent, notification number is CN101012056A), exist safety on hidden danger and the defective on the synthesis capability.
Summary of the invention
Purpose of the present invention aims to provide a kind of safe, easy control, with low cost, and the combustion synthesis apparatus for fullerenes with certain output.
The present invention is provided with roasting kiln, burner noz(zle), telescope-feed condenser tube, filter tank, liquid filter, heat exchanger, vacuum pump, vacuum regulating system, ignition system, gas supply and Controlling System, vacuum tightness test and display unit.
Burner noz(zle) connects oxygen pipeline and fuel conduit respectively, outer water flowing cooling, and burner noz(zle) is fixed in the roasting kiln chassis; Telescope-feed condenser tube connects the bell downstream of roasting kiln; Filter tank links to each other with telescope-feed condenser tube by vacuum quick-release flange; The liquid filter links to each other with chimney filter by pipeline; Heat exchanger links to each other with the liquid filter by pipeline; Vacuum pump links to each other with heat exchanger by Vacuum ball valve; Vacuum regulating system is provided with breather valve and Vacuum ball valve, and breather valve is located on the roasting kiln body of heater, and Vacuum ball valve is located between vacuum valve and the heat exchanger; Ignition system links to each other with body of heater; The vacuum tightness test communicates with the roasting kiln body of heater with display unit; The gas supply is connected with burner noz(zle) by steam line with Controlling System.
Roasting kiln is provided with chassis, body of heater, bell, and body of heater is provided with flame viewing window and accurate vacuum meter, and flame viewing window lower end and burner noz(zle) top are on the same sea line substantially; The center of bell is a ventpipe, and the ventpipe upper end is-90 ° of turnings, and air communication is crossed the turning flow direction and changed horizontal direction into by original vertical direction.The bell downstream connects telescope-feed condenser tube, and body of heater and bell are provided with interlayer, is used for the water flowing cooling, seals by the O circle between body of heater, chassis and the bell.
Filter tank is provided with tank body and filter core, and by the sealing of O circle, the filter tank downstream links to each other with the liquid filter by pipeline between filter core and the tank body.Wherein filter core is divided into three layers, is respectively from inside to outside: Porous Stainless Steel supporter, non-woven fabrics and filter paper.
The liquid filter is provided with cylinder body cavity and following cylinder body cavity, and last cylinder body cavity links to each other by airway with following cylinder body cavity, and the bottom of cylinder body cavity is down pressed close in the airway lower end, and last cylinder body cavity is used to control the suck-back of filtrate.
Heat exchanger preferably adopts recuperative heat exchanger, links to each other with the vacuum pump in downstream by Vacuum ball valve.
Vacuum pump is the end of this synthesizer.Adopt the sealing of RUBBER O circle between each operating unit of vacuum regulating system, connect between operating unit and pipeline and pipeline and the pipeline and adopt vacuum quick-release flange, the Vacuum ball valve of being located between heat exchanger and the vacuum pump is used to regulate the pumping speed of vacuum pump to whole system, and the breather valve of being located at the roasting kiln body of heater is used for to the system bubbling air to increase system pressure.Under the prerequisite of not considering nozzle air current speed, the adjusting of system vacuum tightness can be realized by Vacuum ball valve and common adjusting of being located on the body of heater of breather valve.
Ignition system is provided with boost-up circuit, tetrafluoroethylene ring flange and copper electrode, and copper electrode passes the tetrafluoroethylene ring flange.
The vacuum tightness test can be adopted accurate vacuum meter with display unit, communicates with the roasting kiln body of heater.
In gas supply and Controlling System, oxygen and acetylene are all by the steel cylinder air feed, by mass flowmeter pilot-gas flow velocity; Benzene vapor is then provided by the Sheng benzene container body in the thermostat container, and the device of control benzene vapor flow velocity is a spinner-type flowmeter, and also as in the thermostat container, under meter to the supply air line of burner noz(zle) then adopts hot blast air blast insulation.
Compare with existing combustion synthesis apparatus for fullerenes, outstanding advantage of the present invention is:
(1) possesses synthesis capability preferably.
(2) compare with the graphite arc method, the synthetic cost is comparatively cheap.
(3) flame stability is good, and fluctuation of antibody system and external interference ability are strong.Flame can not cause extinguishing of flame because of the fluctuation on the air feed air-flow after the trouble-free burning, can resist the sudden change of system pressure to a certain extent, even can keep the stable sustained combustion of flame in the high vacuum below 5torr yet.
(4) security is good, is grasping the elasticity height.This is the advantage that the diffusion combustion nozzle is adopted in this device design, uses this device needn't worry to explode and the problem of detonation, also needn't worry to cause extinguishing suddenly of flame because of the problem on the operation skill.
(5) vacuum regulating system is not only simple, and the efficient height.Pumping speed by Vacuum ball valve and breather valve control vacuum pump and can obtain and maintain a certain comparatively stable vacuum tightness value to the outgassing rate of roasting kiln.
(6) filtering system is not only simple, and the efficient height.This device adopts filter paper and non-woven fabrics as the main filtering material of cigarette ash, can not only stop most cigarette ashes, and simple, inexpensive, is easy to change; The liquid filter then can filter the cigarette ash that trace is not stopped, with the protection vacuum pump.
Description of drawings
Fig. 1 is the structural representation of the embodiment of the invention.
Fig. 2 is the liquid chromatograph mass spectrography base peak figure of the methylbenzene extraction liquid of cigarette ash that the embodiment of the invention is produced.In Fig. 2, X-coordinate is time T ime (min), and ordinate zou is mass spectrum ionic strength Intens * 10
5A peak, b peak are that mass-to-charge ratio is 720 product, and the c peak is that mass-to-charge ratio is 840 product; The peak of 93min and 114min corresponds to C
60And C
70
Embodiment
Following examples will the invention will be further described in conjunction with the accompanying drawings.
Referring to Fig. 1, the present invention is provided with roasting kiln, burner noz(zle), telescope-feed condenser tube, filter tank, liquid filter, heat exchanger, vacuum pump, vacuum regulating system, ignition system, gas supply and Controlling System, vacuum tightness test and display unit.
Roasting kiln is the main part of the embodiment of the invention, is made up of by the sealing of O circle chassis 1, body of heater 3 and bell 7 respectively from bottom to up.Chassis 1 is a stainless steel disk, and a circular hole is opened in the center, and by welding the internal diameter pipe 2 identical with circular hole to increase the length of round passage, establishes groove in this passage, fixes and seal the burner noz(zle) that therefrom passes by rubber cradle.Body of heater 3 highly designs should be higher than flame height, and this device is designed to 500mm; The diameter design should reach 200mm at least, and to give the annealing space of flame with 100mm, body of heater 3 internal diameters of this device are designed to 300mm.Viewing window 4 is for being horizontally disposed with the vertical furnace wall of medullary ray.Be connected with accurate vacuum meter 5 on the body of heater 3, be used to show the vacuum tightness of system.Be connected with breather valve 6 on the body of heater 3, breather valve 6 the other ends are identical with atmosphere.Inclined weld has a pipe flange 23 on the body of heater 3, the end flange dish with in wear copper electrode 22 tetrafluoroethylene ring flange 24 join.Bell 7 is designed to taper, conical top is connected with ventpipe and-90 ° of turnings 8, the design of bell 7 breather line diameters can not be too little, otherwise the deposition of cigarette ash in the building-up process that can occur burning and make the free area of breather line reduce and occur the pumping speed of roasting kiln is significantly reduced, and then influence the vacuum tightness of roasting kiln.Bell 7 breather lines link to each other by the telescope-feed condenser tube 13 in quick-release flange and downstream.Wherein body of heater 3, bell 7 design respectively the water flowing interlayer.
Burner noz(zle) mainly is made up of three layers of different stainless steel tube of size, is respectively inner tube, middle tube and outer tube from inside to outside.Inner tube is an oxygen channel, and the lower end links to each other with oxygen steam line 9, and the inner tube internal diameter is 8mm, wall thickness 1mm, the circular channel between middle tube and the inner tube then is the passage of benzene vapor and acetylene, links to each other with the steam line 10 of benzene vapor and acetylene, the internal diameter of middle tube is 16mm, wall thickness 2mm.Inner tube is than the low 15mm of middle tube, this difference of altitude is to consider diffusive mixing between oxygen and the fuel gas and burner noz(zle) coking degree set, height difference is more little, burner noz(zle) is not easy coking more, but the oxygen in the inner tube and the diffusive mixing effect of the fuel gas in the middle tube are also weak more, are unfavorable for the raising of flame temperature and the generation of soccerballene; Otherwise height difference is big more, though the mixing effect of fuel gas and oxygen strengthens, but this moment, the flame burning mode trended towards premix, and it is unstable that flame can become, and for example takes off fiery phenomenon, and the possibility that serious coking takes place is also big more, influences the lasting building-up process of device.The gaseous species that is led in each layer pipe also is determined by experiment, if inner tube is made as the fuel gas passage, and the circular channel is made as oxygen channel between middle tube and the inner tube, then can increase the probability that detonation takes place burner noz(zle) greatly when spark initiation, the failure that causes flame to ignite.Circular channel between outer tube and the middle tube is the passage of water coolant, and the bottom is repeatedly kicked into water pipe 11 and rising pipe 12 respectively, and wherein end distance circular channel tip designs is 6mm on the rising pipe, has so just guaranteed the cooling of water of condensation to nozzle top.
Because the combustion reactions gas circuit is in dynamic steady state all the time, vacuum pump 20 needs continuous air extraction just can be maintained the vacuum tightness of system, the cigarette ash that burning generates must filter through filtration unit, otherwise too much cigarette ash enters vacuum pump, influence the works better and the life-span of pump, and the output of cigarette ash also can be impaired.Filter tank in the filtering system is a main device of holding back synthetic cigarette ash.Filter tank links to each other with the telescope-feed condenser tube 13 of upstream and the liquid filter in downstream respectively by the quick-release flange.Filter tank mainly is made up of stainless steel tank body 14 and filter core 15, and both link to each other by flange.Filter core 15 innermost layers are the porous stainless steel cylinder, and stainless steel cylinder only plays a supportive role, and skin is surrounded by non-woven fabrics and multilayer filter paper.The design of filter core 15 is enough to satisfy the filteration to synthetic cigarette ash, and most cigarette ashes all are retained down, and has only a little cigarette ash to be taken away through filter core 15 and enters the liquid filter.The liquid filter is provided with two continuous stainless steel cylinder body cavitys, link to each other by airway, the bottom of cylinder body cavity 17 is down pressed close in the airway lower end, last cylinder body cavity 16 is used to control the suck-back of filtrate, in the following cylinder body cavity 17 light lubricating oil is housed, loadings is taken away to suitable not make oil, and the liquid filter can be used for filtering out the cigarette ash that is not stopped by filter tank on a small quantity, and can absorb a spot of organic composition in the waste gas.Liquid filter downstream connects heat exchanger 18.
Vacuum regulating system comprises the sealing of various terminal, Vacuum ball valve 19 and breather valve 6.The sealing of RUBBER O circle is adopted in connection in each operating unit, connect by vacuum quick-release flange between operating unit and pipeline and pipeline and the pipeline, be located at the pumping speed that Vacuum ball valve 19 between heat exchanger 18 and the vacuum pump 20 is used to regulate 20 pairs of whole systems of vacuum pump, the breather valve 6 of being located at roasting kiln body of heater 3 is used for to the system bubbling air to increase system pressure.Under the prerequisite of not considering nozzle air current speed, the adjusting of system vacuum tightness and keep and can realize easily by the breather valve 6 common adjustings of Vacuum ball valve 19 and body of heater 3.
The core of ignition system is a boost-up circuit 21, by boost-up circuit 21 voltage that saves conventional accumulators is risen to about 3000V, making can be with the certain frequency continuous discharge between copper electrode 22 and the burner noz(zle), what guiding copper electrode 22 entered roasting kiln is tetrafluoroethylene ring flange 24, flange center's line and body of heater 3 center thread 45s, selecting tetrafluoroethylene is factors of considering furnace temperature as the making material of ring flange 24.Copper electrode 22 links to each other by the positive pole of cable with boost-up circuit 21, and another relative with copper electrode 22 be burner noz(zle) very, and the burner noz(zle) bottom links to each other by the negative pole of cable with boost-up circuit 21.
Gas supply and Controlling System relate generally to the insulation of benzene vapor and the flow control problem of all gases.This device is controlled by mass flowmeter 25 for the flow of acetylene and oxygen, the phenomenon that flow strengthened when air communication was crossed mass flowmeter 25 and system vacuum tightness can not take place risen, and this phenomenon can't be avoided when using spinner-type flowmeter 26 control high pressure gas flow velocitys.And the flow of benzene vapor is to be that the flow velocity of benzene vapor is limited in this device by spinner-type flowmeter 26 control reasons, and above-mentioned phenomenon can not take place, so use spinner-type flowmeter 26 can satisfy flow rate control and demonstration to benzene vapor.The insulation of benzene vapor is adopted and is realized containing benzene container and steam line heat tracing, containing benzene container and spinner-type flowmeter 26 is incubated by thermostat container, this thermostat container has the air blast function, for the benzene pipeline then by adding the ventilator trunk that links to each other with thermostat container for the benzene pipeline, heat branch in the thermostat container is drained by ventilator trunk, and this process has promptly realized the insulation for the benzene pipeline.
Below provide using method of the present invention:
1. preparation work: connect each pipeline and operating unit, and check the resistance to air loss of whole apparatus system.Adjust the distance at burning shower nozzle and copper electrode tip, can continue spark discharge with certain frequency between the two after making ignition switch open.Open the breather valve on the roasting kiln body of heater, close Vacuum ball valve, and open water coolant.
2. open the ignition system ignition switch, make between copper electrode and the burner noz(zle) and discharge.
3. open acetylene supply air line mass flowmeter switch, acetylene is ignited by electrical spark during by the burner noz(zle) mouth, and open oxygen quality under meter switch this moment, makes the burner noz(zle) aerating oxygen.
4. the flow velocity with acetylene and oxygen is adjusted to preset value rapidly, opens vacuum pump and bleeds, and this moment, vacuum pump can not vacuumize system because Vacuum ball valve is closed.
5. slowly open Vacuum ball valve, make vacuum pump begin to bleed system, and about the gas flow rate of regulating breather valve makes system vacuum tightness near 20Torr.Open the switch of benzene vapor pipeline spinner-type flowmeter this moment, and burner noz(zle) begins to introduce benzene vapor, opens the thermostat container power switch, begins containing benzene container, spinner-type flowmeter and supply air line air blast heating.In general, calorstat temperature is set to 40 ℃ and can makes the flow of benzene vapor reach the need for equipment amount.Fine setting Vacuum ball valve and breather valve make the vacuum tightness of system maintain about 15Torr, treat that it promptly is picking up counting the time of this device burning building-up process that temperature-stable for the benzene system gets off.The bottom of stable back flame is sapphirine, and top is pale brown look, and has cigarette to generate.
6. end to be synthesized then needs knock down the flame and cuts off in the running and install.At first turn off switch, cut off the supply of benzene vapor and turn off the power supply of thermostat container for the benzene pipeline; Then be the mass flowmeter switch of turning off acetylene and oxygen, and close the valve on acetylene and the oxygen bottle that this moment, flame extinguished; Open breather valve, put into air, system vacuum tightness is descended; Close vacuum pump, this moment, system vacuum tightness continued to descend and finally equate with external atmosphere pressure; Close Vacuum ball valve and water coolant.It should be noted that the working order that finishes reaction can not change, otherwise fuel gas might occur sucking in the oxygen pipeline or make, cause igniting next time that detonation, flame ignite difficulty and other danger take place for oxygen intake or air in the benzene pipeline.
7. cut off after the reaction, begin to filter irritate and roasting kiln in cigarette ash clean and collect, extract and separation detection, and in time remove coking material in the combustion head.
Below result of the present invention is described further.
1. combustion conditions is to the influence of soccerballene generation.
In the diffusion combustion of this device was synthetic, the fuel that uses was acetylene and benzene vapor.Adopt the premixed combustion in oxygen of high pressure benzene vapor or acetylene mostly about the flame fullerene synthesis in the document, wherein the low-pressure combustion of acetylene and benzene all has the fullerene product to generate, just the content of soccerballene will be higher than acetylene in the benzene vapor burning gained cigarette ash, in other words, the ability of acetylene combustion generation soccerballene is worse than benzene slightly.But from another angle, acetylene is that rate of combustion is the fastest in all gas-phase carbon hydrogen fuels, its rate of combustion in oxygen is higher than 10m/s, and rate of combustion Gao Ze shows as flame stabilization in diffusion combustion, immunity from interference is strong, be not easy to take off fire, and the temperature of alkynes oxygen fireworks flame also is higher than benzene oxygen flame, and the raising of flame temperature also is favourable for the generation of soccerballene.So we adopt with the benzene vapor in the research of attempting the diffusion combustion fullerene synthesis is main fuel, when burning, add the method for a little acetylene again, can make the stable easily control of flame building-up process again to reach the output that can guarantee soccerballene as stationary flame and raising flame temperature.
The influence that vacuum tightness generates soccerballene.This device is when burning is synthetic, and the output of the carbon ash that obtains under the higher pressure is very big, but C in the carbon ash
60And C
70Amount considerably less, and the content that can extract composition in the carbon ash is seldom, has lower solvent extraction rate.Be lower than in vacuum tightness under the condition of 40Torr, can obtain a large amount of carbon ashes by burning soon, the product extracting solution is through LC-MS even can not detect C
60And C
70Mass spectra peak, soluble part mainly is a polycyclic aromatic hydrocarbons in the carbon ash.Be higher than under the 40Torr condition the corresponding lifting of the ratio of soccerballene in cigarette ash.When vacuum tightness bring up to 20Torr and 20Torr thereof with interior situation under, can from base peak figure, can obviously see C
60And C
70Component be that group in the cigarette ash extract is wanted composition, have suitable content, the result of this and document conforms to.Reach when vacuum tightness under the condition of 15Torr or even 10Torr, the content of soccerballene in extract improves a lot again, compare with lower vacuum tightness, the amount that generates the carbon ash under high vacuum condition has reduced a lot, but the extraction yield of carbon ash is than higher, and wherein the content of soccerballene is significantly improved.This reason wherein may be the raising owing to vacuum tightness, and the diffusion of benzene and oxygen increases, and it is more abundant to burn, and the temperature of reaction increases, and more helps the generation of soccerballene.Comprehensive above vacuum degree condition is considered the content of soccerballene in the growing amount of cigarette ash and the cigarette ash, and vacuum tightness was made as 15～20Torr when this device synthesized.
It is different that diffusion combustion and premixed combustion prepare soccerballene, though the output of cigarette ash and composition are very responsive to the change in flow of fuel and oxygen, the actual air input of fuel and oxygen may not directly reflect the C/O ratio.Fuel gas enters combustion head with oxygen from different pipelines, carry out the phase mutual diffusion at combustion head, and burn, so consider a very important factor when degree of mixing of gas also is the burner noz(zle) design, the degree of mixing of different spaces gas has the variation of gradient, and the temperature of this zone flame also can be different thereupon.In fact, the incendiary situation is very complicated, and incendiary Several Factors such as mixed effect, flow velocity, flame temperature, system pressure are interactional in fact.From the situation of this device, benzene vapour flow velocity 1.2～1.4L/min, acetylene flow velocity 0.5～0.6L/min, O
2Flow velocity 1.1～1.2L/min is more satisfactory, can guarantee to generate a certain amount of carbon ash, can guarantee C in the carbon ash again
60, C
70And the existence of other more species.Under this condition, cigarette ash output can reach more than the 4g/h.Why selecting this synthesis condition is directly related with our research purpose also, and the starting point that we design this combustion synthesis apparatus for fullerenes is not purely in order to obtain C
60And C
70, but for the derivative of non-classical soccerballene of Separation Research and soccerballene, the mechanism and the approach that generate with the burning of research soccerballene.
2. cigarette ash analysis
Because burning synthetic soccerballene and other product are present in the middle of the cigarette ash, so generally need carry out solvent extraction to cigarette ash, extracting solution is by separating and analyzing and could identify the component that wherein exists.At present, it is comparatively desirable that the use high performance liquid chromatography separates the component effect of cigarette ash extracting solution, uses mass spectroscopy also can satisfy the evaluation of component substantially.
The cigarette ash that takes a morsel is put into beaker, adds an amount of toluene excusing from death and extracts 60min, makes that soluble part dissolves as far as possible in the cigarette ash, and placement is spent the night, and filters, and gets clear liquid and carries out compartment analysis.Sample uses efficient liquid phase chromatographic analysis: stationary phase is anti-phase C18 post, Discovery C18 Column (SUPELCO), 5 μ m particle size, 8nm pore size, 4.6 * 250mm; Moving phase is methyl alcohol, ethanol, hexanaphthene (moving phase all attach most importance to steaming).The eluent gradient condition sees Table 1.
Table 1
Experiment shows that as shown in Figure 2, the carbon ash extract component more complicated of combustion method preparation is except main C
60, C
70The outer less polycyclic aromatic hydrocarbons of various molecular weights in addition.If a little low-molecular-weight polycyclic aromatic hydrocarbonss of component group before the retention time 40min, wherein the peak of 93min and 114min corresponds to C
60And C
70And a peak wherein, b peak obtain by mass spectroscopy is that mass-to-charge ratio is 720 product, may be number of C
60Unsettled derivative, promptly broken by mass spectrum ionization process molecule; What the c peak obtained by mass spectroscopy is that mass-to-charge ratio is 840 product, may be C
70Unsettled derivative, also broken by the mass spectrum ionization process, the existence of these fullerene derivates is very useful for research soccerballene burning formation mechanism.At present, growth mechanism for soccerballene in the flame system exists many disputes, various possible growth pathway all can not be explained all problems, and stay in the stage of hypothesis and conjecture basically, in this sense, the growth mechanism of soccerballene is a job highly significant in the flame combustion process for illustrating with other non-classical soccerballene to separate the derivative that obtains these soccerballenes.
Claims (7)
1. a combustion synthesis apparatus for fullerenes is characterized in that being provided with roasting kiln, burner noz(zle), telescope-feed condenser tube, filter tank, liquid filter, heat exchanger, vacuum pump, vacuum regulating system, ignition system, gas supply and Controlling System, vacuum tightness test and display unit;
Burner noz(zle) is respectively inner tube, middle tube and outer tube from inside to outside, inner tube is an oxygen channel, the inner tube lower end links to each other with the oxygen steam line, circular channel between middle tube and the inner tube is the passage of benzene vapor and acetylene, circular channel between described middle tube and the inner tube links to each other with the steam line of benzene vapor and acetylene, inner tube is lower than middle tube, the circular channel water flowing cooling between outer tube and the middle tube, and burner noz(zle) is fixed in the roasting kiln chassis; Telescope-feed condenser tube connects the bell downstream of roasting kiln; Filter tank links to each other with telescope-feed condenser tube by vacuum quick-release flange; The liquid filter links to each other with filter tank by pipeline; Heat exchanger links to each other with the liquid filter by pipeline; Vacuum pump links to each other with heat exchanger by Vacuum ball valve; Vacuum regulating system is provided with breather valve and Vacuum ball valve, and breather valve is located on the roasting kiln body of heater, and Vacuum ball valve is located between vacuum pump and the heat exchanger; Ignition system links to each other with body of heater; The vacuum tightness test communicates with the roasting kiln body of heater with display unit; The gas supply is connected with burner noz(zle) by steam line with Controlling System.
2. a kind of combustion synthesis apparatus for fullerenes as claimed in claim 1 is characterized in that roasting kiln is provided with chassis, body of heater, bell, and body of heater is provided with flame viewing window and accurate vacuum meter, and body of heater and bell are provided with and are used for water flowing refrigerative interlayer.
3. a kind of combustion synthesis apparatus for fullerenes as claimed in claim 1 is characterized in that filter tank is provided with tank body and filter core, and by the sealing of O circle, filter core is divided into three layers, is respectively from inside to outside: Porous Stainless Steel supporter, non-woven fabrics and filter paper between filter core and the tank body.
4. a kind of combustion synthesis apparatus for fullerenes as claimed in claim 1 is characterized in that the liquid filter is provided with cylinder body cavity and following cylinder body cavity, and last cylinder body cavity links to each other by airway with following cylinder body cavity.
5. a kind of combustion synthesis apparatus for fullerenes as claimed in claim 1 is characterized in that heat exchanger is a recuperative heat exchanger.
6. a kind of combustion synthesis apparatus for fullerenes as claimed in claim 1 is characterized in that ignition system is provided with boost-up circuit, tetrafluoroethylene ring flange and copper electrode, and copper electrode passes the tetrafluoroethylene ring flange.
7. a kind of combustion synthesis apparatus for fullerenes as claimed in claim 1 is characterized in that the vacuum tightness test is a vacuum meter with display unit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101111528A CN101503188B (en) | 2009-03-02 | 2009-03-02 | Combustion synthesis apparatus for fullerenes |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101111528A CN101503188B (en) | 2009-03-02 | 2009-03-02 | Combustion synthesis apparatus for fullerenes |
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| CN101503188A CN101503188A (en) | 2009-08-12 |
| CN101503188B true CN101503188B (en) | 2010-12-08 |
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| CN2009101111528A Expired - Fee Related CN101503188B (en) | 2009-03-02 | 2009-03-02 | Combustion synthesis apparatus for fullerenes |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139871B (en) * | 2010-01-29 | 2013-03-06 | 沈阳科友真空技术有限公司 | Vacuum equipment for continuously preparing fullerene |
| CN102001647B (en) * | 2010-12-16 | 2012-08-29 | 中国科学院高能物理研究所 | Preparation method of fullerene |
| CN102173404A (en) * | 2011-02-24 | 2011-09-07 | 厦门大学 | Non-isolated pentagon ring fullerene C50H10 and synthesis method and application thereof |
| CN106744815A (en) * | 2017-03-07 | 2017-05-31 | 内蒙古碳谷科技有限公司 | A kind of burner for preparing fullerene |
| CN109467075B (en) | 2018-12-24 | 2020-04-24 | 厦门大学 | Continuous combustion production equipment for synthesizing ton-level fullerene and synthesis method thereof |
| CN115285974A (en) * | 2022-08-18 | 2022-11-04 | 安徽建马防护用品科技有限公司 | Method and device for manufacturing alkene carbon material |
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| CN101503188A (en) | 2009-08-12 |
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