CN103353411B - Quasi monodisperse nanometer aerosol generation system - Google Patents
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Abstract
The invention discloses a quasi monodisperse nanometer aerosol generation system which comprises a mistorizer, a mist chamber, an atomizer, a cooler and a diffusion dryer, wherein the mistorizer is inserted into an upper cover of the mist chamber; an outlet air pipe of the mist chamber is connected with the atomizer through a reducing clamping sleeve; a three-way clamping sleeve is arranged at an outlet of the atomizer; one end of the three-way clamping sleeve is inserted into a K type thermocouple, and the other end of the three-way clamping sleeve is connected with an inner pipe of the cooler; a PT100 thermocouple is inserted into a sleeve of the cooler; the outlet of the inner pipe of the cooler is connected with the diffusion dryer through the three-way clamping sleeve. Quasi monodisperse inorganic nanometer aerosol with high concentration can be stably output, and the system has the characteristics of being stable and reliable in performance, convenient and flexible to use and low in cost and is suitable for research o a nanoparticle principle, research on a filtration technology and field efficiency tests.
Description
Technical field
The invention belongs to aerosol technology field, be specifically related to a kind of generation systems that higher Particle density, accurate dispersed nano particulate can occur.
Background technology
Gasoloid refers to can the solid of stable suspersion in gas or liquid particles thing, when describing with fineness spectrum distribution equation, and geometric standard deviation σ
gthe gasoloid of≤1.15 is monodisperse aerosol, 1.15 < σ
gthe monodisperse aerosol that is as the criterion of≤1.5, σ
g>'s 1.5 is polydispersed aerosol.Nanometer aerosol refers in particular to the gasoloid of particle diameter at 1nm to 100nm, and it all plays key player in fields such as amblent air temperature, medical and health health, electronics.There is character (concentration, particle diameter) and stablize controlled nanometer aerosol, for fields such as the research of nano particle basis, commercial Application and purification controls, particularly gasoloid technical development, instrumental calibration correct and filtering and cleaning technique development, significant.Therefore, nanometer aerosol generator is a kind of important instrument equipment of aerosol art.
Can be there is the gasoloid of micron and sub-micron in existing common aerosol generator, be mainly used in the efficiency test etc. of air strainer.Such as, publication number is the Chinese invention patent of CN102069047A, CN1974387A and CN101093218A, relate separately to the generator for generating Large stone droplet, solid-state large-size particles thing and solid sub micronic sodium chloride, but liquid or solid-state nanometer aerosol cannot be produced.Publication number is the Chinese invention patent of CN102706706A, relates to and removes the aerocolloidal generator of molten generation 20nm to 80nm scope for atomization, but cannot produce dispersed nano gasoloid.
Nanometer aerosol generator commercially available at present mainly adopts the occurring principles such as electron spray, electrode discharge and Electrostatic Classification of Fine.
Electron spray nanometer aerosol generator, as Technical Sourcing Internation of the U.S. 3480 type generator, utilizes conducting liquid or suspension to obtain the polydispersion nanometer aerosol of 3nm to 100nm scope.This quasi-instrument has requirement to class of liquids and conductivity, and theory structure is complicated, and operation requirements is high, and prices are rather stiff.Graphite electrode electric discharge nanometer aerosol generator, as the GFG1000 type generator of German PALAS company, utilizes electrode spark discharge to produce carbon black condensate, reunites and touches and the rear carbon black particle producing 20nm to 150nm wide region.Also can use the carbon electrode of simple metal electrode and doping metals, as the APG200 golden nanometer particle generator of Japanese YOTSUBISHI company.Can only be there is polydispersion nanometer aerosol in this quasi-instrument, expensive, and Material selec-tion and the preparation of electrode require higher, as carbon black particle is not suitable for Mass Spectrometer Method requirement.
Electrostatic Classification of Fine device is separated the particle of different electromobility (corresponding different-grain diameter) by scanning voltage of electric field, can export monodisperse particle during fixed voltage.What atomization went molten generator, electron spray generator and spark discharge generator to produce is polydispersed aerosol, need with the coupling of Electrostatic Classification of Fine device to obtain dispersed nano gasoloid.At present, foreign vendor has released the monodisperse nanometer aerosol generation system containing Electrostatic Classification of Fine device, as the 3940 type sub-micron monodisperse aerosol generation systems of Technical Sourcing Internation of the U.S., can produce the monodisperse particle of 10 nanometers to 1 micron.This system comprises the assemblies such as atomizer, neutralizer, Electrostatic Classification of Fine device, diffusion dryer, and the close prices of whole system 1,000,000 yuans, common laboratory is difficult to bear.
Atomization/type of cooling is a kind of effective way that nanometer aerosol occurs, cardinal principle is: utilize atomizer to make material carburation by evaporation formation atom vapor under the high temperature conditions, recycling refrigeratory makes steam rapid condensation in violent temperature-fall period form cluster, and reuniting further produces nano particle.Graphite furnace atomizer commercial instruments can realize room temperature and heat to the program of 3000 DEG C, can meet the atomization demand of most of rare earth and transuranic element.Graphite-pipe should use the inert gases such as argon gas as protection gas, but can not adopt nitrogen, otherwise can generate poisonous CN molecule.In addition, commercially available atomizer is expensive, need regularly replace graphite-pipe.The type of cooling of current report has nature to cool (S C Kim, J Wang, M S Emery, et al.Structuralproperty effect of nanoparticle agglomerates on particle penetration through fibrousfilter.Aerosol Science and Technology, 2009,43:344-355) with gas dilution cooling (IMarshall.Particle number counter calibration/Validation procedure.AEA TechnologyInc., 2007) etc.Too small or the skewness of the apse rate of these two kinds of types of cooling, causes steam cooling procedure rapidly or heterogeneity, can only export polydispersed aerosol.To produce monodisperse aerosol, still need with Electrostatic Classification of Fine device with the use of.In addition, the parameter fluctuation such as gas flow temperature and flow also cause granularity and fluctuation of concentration larger.
Summary of the invention
For overcoming the above-mentioned deficiency of prior art, the present invention proposes a kind of accurate monodisperse nanometer aerosol generation system adopting atomization/cooling principle, it can stablize the higher Particle density of output, accurate monodispersed inorganic nano gasoloid, have stable and reliable for performance, easy to use flexibly, feature that cost is low, be applicable to the research of nano particle principle, filtering technique studied and efficiency on-the-spot test.
Solution of the present invention is:
A kind of accurate monodisperse nanometer aerosol generation system, its special character is:
Comprise atomizer 1, fog chamber 2, atomizer 6, refrigeratory 14 and diffusion dryer 18,
In described fog chamber 2, silica gel 3 is set;
Described atomizer 6 comprises alundum tube 7, heater strip 8, flip-shell heat insulation support case 9, FEEDBACK CONTROL pressure regulator 11; Described heater strip 8 is wrapped in outside alundum tube 7, and described first thermopair 13 is for controlling the output voltage break-make of FEEDBACK CONTROL pressure regulator 11; The inner dense packing effect asbestos 10 of described flip-shell heat insulation support case 9, described alundum tube 7 is through flip-shell heat insulation support case 9;
Described refrigeratory 14 comprises interior pipe and sleeve pipe; Described interior pipe is stainless-steel tube 15; Described casing pipe sleeve is connected on outside interior pipe, and be connected with chilled water in described sleeve pipe, water (flow) direction is contrary with airflow direction, and described second thermopair 16 is for monitoring cooling water temperature;
Described atomizer 1 inserts in fog chamber 2, described fog chamber 2 is connected with the entrance of atomizer 6, described atomizer 6 exports the interior pipe connecing the first thermopair 13 and refrigeratory 14 respectively, insert the second thermopair 16 in the sleeve pipe of described refrigeratory, refrigeratory inner tube outlet is connected with the entrance of diffusion dryer 18.
Above-mentioned diffusion dryer 18 comprises cylindrical case, arrange taper polytetrafluoroethylstephanoporate stephanoporate liner 19 in the enclosure, be arranged on drying agent between cylindrical case and taper polytetrafluoroethylstephanoporate stephanoporate liner 19, the osculum of described taper polytetrafluoroethylstephanoporate stephanoporate liner 19 is connected with cooler outlet, and its large mouth is thief hatch 20.
The outer wall of above-mentioned alundum tube 7 is provided with helix groove, and described heater strip 8 is closely wrapped in helix groove, and the two ends iron hoop of described heater strip 8 is fixed on the outer wall of alundum tube 7.
The quality of alumina mark of above-mentioned alundum tube 7 is 90%.
Above-mentioned first thermopair is K type thermopair; Described second thermopair is PT100 thermopair.
Advantage of the present invention is:
1, alundum tube is utilized to make atomizer, also closely heater strip is wound around at its outer wall processing helix groove, the temperature control heating up to 1100 DEG C can be realized by temperature feedback control, compared with graphite furnace atomizer, cost reduces greatly, serviceable life extends, and adapts to the multiple atmosphere such as nitrogen, air, argon gas;
2, the accurate type of cooling of wall is adopted, obtain large and uniform apse rate, realize evenly reuniting rapidly of steam, compare with the gas dilution type of cooling with naturally cooling, process repeatability and parameter controllability strengthen, and export aerocolloidal monodispersity and stability raising;
3, the nanometer aerosol exported is as the criterion monodisperse aerosol, and peak position diameter is about 30nm, Particle density reaches 10 for it
6cm
-3, Particle density fluctuation is less than 5%, flexible and convenient to use, with low cost, stable and reliable for performance, can meet nano particle research and the demand such as filtration efficiency test.
Accompanying drawing explanation
Fig. 1 is the principle schematic of nanometer aerosol generation systems;
When Fig. 2 is atomizer heating-up temperature difference, generation systems exports the aerocolloidal fineness spectrum of NaCl;
Fig. 3 is for advising that under condition of work, generation systems exports the aerocolloidal stability of NaCl continuously;
Reference numeral is: 1-atomizer, 2-fog chamber, 3-silica gel, 4-teflon upper cover, 5-reducing cutting ferrule, 6-atomizer, 7-alundum tube, 8-nickel chromium triangle heater strip, 9-flip-shell heat insulation support case, 10-asbestos, 11-pressure regulator, 12-threeway cutting ferrule, the 13-the first thermopair, 14-refrigeratory, pipe in 15-stainless steel, the 16-the second thermopair, 17-threeway cutting ferrule, 18-diffusion dryer, 19-polytetrafluoroethylstephanoporate stephanoporate liner, 20-thief hatch.
Embodiment
Accurate monodisperse nanometer aerosol generation system, comprise atomizer 1, fog chamber 2, atomizer 6, refrigeratory 14 and diffusion dryer 18 to form, described atomizer 1 inserts the upper cover 4 of fog chamber 2, fog chamber 2 is exported tracheae and is connected with atomizer 6 by reducing cutting ferrule 5, threeway cutting ferrule 12 is installed in atomizer 6 exit, K type thermopair 13 is inserted in one end, the other end is connected with pipe in refrigeratory 14, refrigeratory sleeve pipe interpolation enters PT100 thermopair 16, and refrigeratory inner tube outlet is connected with diffusion dryer 18 by threeway cutting ferrule 17.
The body of fog chamber 2 is cylindrical plastic, internal diameter is between 70mm to 100mm, and height is between 100mm to 150mm, and inside holds silica gel 3, teflon upper cover 4 and bottleneck pass through thread seal, upper cover evenly bores three holes, and wherein, an internal diameter is the through hole of 6mm, by the sealing of O circle after atomizer 1 inserts, a commercially available quick connector being applicable to external diameter 6mm plastics tracheae, a commercially available hangnail joint being applicable to external diameter 16mm to 20mm tracheae, two between joint with upper cover for being threaded.
In atomizer 6, the salic massfraction of alundum tube 7 is 90%, the high temperature of resistance to 1200 DEG C, special mechanical can be utilized to process, be easy to obtain and cost greatly reduce than graphite-pipe, internal diameter is 8mm to 10mm, external diameter is 16mm to 20mm, and length is 300mm to 600mm; Be connected with upstream and downstream parts with cutting ferrule 4,12 after the outside surface polishing of two ends; Pipe outer wall processing helix groove, groove depth and groove width 1.5mm to 2.5mm, slot pitch 2mm to 3mm, the axial overall length 200mm to 500mm of groove, nickel chromium triangle heater strip 8 is closely wrapped in groove, and heater strip two ends iron hoop is fixed; Alundum tube outlet threeway place installs K type thermopair 13, the output voltage break-make of FEEDBACK CONTROL pressure regulator 11, realizes temperature control heating; Flip-shell heat insulation support case 9, inner dense packing effect asbestos 10, alundum tube keeps flat wherein and through reserved circular hole, will renovate and buckle, and realize heat-insulation and heat-preservation and electrical isolation during use.Commercially available alundum tube mainly divides 90% content and 99% content, and the latter's performance is better, but the former better processes.
Refrigeratory 14 is sleeve structure, and interior pipe is the stainless-steel tube 15 of inner wall smooth, and internal diameter is 12mm to 14mm, and external diameter is 16mm to 20mm, and length is 200mm to 300mm; Chilled water realizes high-precision temperature control refrigeration (0.01 DEG C) by circulating refrigerator, and under external submersible pump drives, flow through sleeve pipe, direction is contrary with airflow direction, and the water temperature in sleeve pipe is monitored by PT100 thermopair 16.
Barrel and the both sides end cap of diffusion dryer 18 are organic glass material and are threaded connection, barrel external diameter is 90mm to 130mm, wall thickness 3mm to 5mm, length is 300mm to 500mm, polytetrafluoroethylstephanoporate stephanoporate liner 19 is the conical surface, thickness is 1mm to 2mm, desiccant-filled between liner and barrel, outlet end cap has thief hatch 20.
The course of work of the present invention:
There is polydisperse aerosol droplet with atomizer 1 atomized soln, mix with the dispersed gas introduced through upper cover plastics tracheae in fog chamber 2, and go molten through silica gel 3, exported by teflon upper cover 4 under gas carrier band, enter atomizer 6 through reducing cutting ferrule 5.In atomizer, nickel chromium triangle heater strip 8 is closely wrapped in the helix groove of alundum tube 7 outer wall, can heat alundum tube equably; Exit flow temperature monitored by K type thermopair 13, and FEEDBACK CONTROL pressure regulator 11 controls heating voltage break-make, and realize the temperature control heating up to 1100 DEG C, the solute making fusing point lower is (as NaCl and AgNO
3) and impurity generation atomization; The multiple gases such as nitrogen, air and argon gas can be used as carrier gas.Steam enters rapidly refrigeratory 14 by threeway cutting ferrule 12 joint.Utilize the water quench wall accurately freezing, circulate, during steady air current, in stainless steel, pipe 15 forms comparatively large and uniform apse rate, and steam can be made to reunite rapidly and equably, forms the close cluster of size and even nano particle; Coolant water temperature by PT100 thermocouple monitoring, and feeds back external circulating refrigerator.Elementide and carrier gas enter diffusion dryer 18 through threeway cutting ferrule 17 joint, and higher, the accurate mono-dispersed nano particle of final formation Particle density, by the removed use of thief hatch 20.The clean gas flow introduced, comprise atomization gas, dispersed gas and carrier gas, all controlled by electromagnetic type mass flow controller, heating-up temperature and chilling temperature are by thermopair on-line monitoring, and design of feedback circuit.
Measure generation systems with calibrated scanning mobility particle spectrometer and export aerocolloidal size-grade distribution, the performance of assessment generation systems.Atomization NaCl solution, atomizer different heating temperature (T
h) under export aerosol granularity spectrum see Fig. 2, test use particle spectrometer cannot measure the particle being less than 20nm, the shadow region in corresponding diagram.Work as T
hwhen=700 DEG C, particle peak position diameter is less than 20nm.T
hwhen=800 DEG C, exporting aerocolloidal peak position diameter is 22.9nm, and fineness spectrum is carried out lognormal distribution matching, and frequency function is:
Obtain coefficient R
2=0.9995, geometric standard deviation σ
g=1.32.T
hwhen=900 DEG C, peak position diameter is 30.5nm, and total number density reaches 9.7 × 10
5cm
-3, obtain R by lognormal distribution matching
2=0.9972, σ
g=1.35.Steady job condition, the NaCl gasoloid stability that generator exports continuously is fine, and see Fig. 3, peak position diameter is 28.1nm, obtains R by lognormal distribution matching
2=0.9985, σ
g=1.31, the short-term fluctuation of total number density is 2.3%.Under these conditions, continuous coverage 6 times, exports aerocolloidal geometric standard deviation and is all less than 1.5, all visual monodisperse aerosol that is as the criterion.
Claims (4)
1. an accurate monodisperse nanometer aerosol generation system, is characterized in that:
Comprise atomizer (1), fog chamber (2), atomizer (6), the first thermopair (13), the second thermopair (16), refrigeratory (14) and diffusion dryer (18),
Silica gel (3) is set in described fog chamber (2);
Described atomizer (6) comprises alundum tube (7), heater strip (8), flip-shell heat insulation support case (9), FEEDBACK CONTROL pressure regulator (11); Described heater strip (8) is wrapped in alundum tube (7) outside,
Described first thermopair (13) is for controlling the output voltage break-make of FEEDBACK CONTROL pressure regulator (11); The inner dense packing effect asbestos (10) of described flip-shell heat insulation support case (9), described alundum tube (7) is through flip-shell heat insulation support case (9);
Described refrigeratory (14) comprises interior pipe and sleeve pipe; Described interior pipe is stainless-steel tube (15); Described casing pipe sleeve is connected on outside interior pipe, and be connected with chilled water in described sleeve pipe, water (flow) direction is contrary with airflow direction, and described second thermopair (16) is for monitoring cooling water temperature;
Described atomizer (1) inserts in fog chamber (2), described fog chamber (2) is connected with the entrance of atomizer (6), described atomizer (6) outlet connects the interior pipe of the first thermopair (13) and refrigeratory (14) respectively, insert the second thermopair (16) in the sleeve pipe of described refrigeratory, refrigeratory inner tube outlet is connected with the entrance of diffusion dryer (18);
Diffusion dryer (18) comprises cylindrical case, arrange taper polytetrafluoroethylstephanoporate stephanoporate liner (19) in the enclosure, be arranged on drying agent between cylindrical case and taper polytetrafluoroethylstephanoporate stephanoporate liner (19), the osculum of described taper polytetrafluoroethylstephanoporate stephanoporate liner (19) is connected with cooler outlet, and its large mouth is thief hatch (20).
2. accurate monodisperse nanometer aerosol generation system according to claim 1, it is characterized in that: the outer wall of described alundum tube (7) is provided with helix groove, described heater strip (8) is closely wrapped in helix groove, and the two ends iron hoop of described heater strip (8) is fixed on the outer wall of alundum tube (7).
3. accurate monodisperse nanometer aerosol generation system according to claim 2, is characterized in that: the quality of alumina mark of described alundum tube (7) is 90%.
4. accurate monodisperse nanometer aerosol generation system according to claim 3, is characterized in that: described first thermopair is K type thermopair; Described second thermopair is PT100 thermopair.
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| CN104707448A (en) * | 2013-12-15 | 2015-06-17 | 中国科学院大连化学物理研究所 | Gas dewatering device and using method thereof |
| CN104826561B (en) * | 2015-04-03 | 2017-01-18 | 清华大学 | Two-stage evaporation and condensation type quasi-monodisperse aerosol generating apparatus |
| CN106053422A (en) * | 2016-08-23 | 2016-10-26 | 江苏德林环保技术有限公司 | Autonomous heating type atomizer |
| ES2679721B1 (en) | 2017-01-18 | 2019-06-21 | Univ Zaragoza | GENERATOR OF NANOPARTICULATED AEROSOLS AND PROCEDURE FOR GENERATION OF CONTINUOUS AEROSOLS ASSOCIATED WITH SUCH GENERATOR |
| CN107271236B (en) * | 2017-06-27 | 2020-01-21 | 中国科学院化学研究所 | Core-shell type aerosol generating system and application thereof in preparation of core-shell type aerosol |
| CN111500423A (en) * | 2020-04-13 | 2020-08-07 | 武汉轻工大学 | Sampling system and sampling method for sampling RNA viruses in liquid and aerosol |
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