CN103212349B - Sublimation-desublimation-method nanometer aerosol generation system and application method and application - Google Patents
Sublimation-desublimation-method nanometer aerosol generation system and application method and application Download PDFInfo
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- CN103212349B CN103212349B CN201310153696.7A CN201310153696A CN103212349B CN 103212349 B CN103212349 B CN 103212349B CN 201310153696 A CN201310153696 A CN 201310153696A CN 103212349 B CN103212349 B CN 103212349B
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- gas circuit
- aerosol
- carrier gas
- sublimation
- spinner flowmeter
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- 239000000443 aerosol Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000012159 carrier gas Substances 0.000 claims abstract description 54
- 239000007789 gas Substances 0.000 claims abstract description 53
- 239000000112 cooling gas Substances 0.000 claims abstract description 33
- 239000007787 solid Substances 0.000 claims abstract description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000011780 sodium chloride Substances 0.000 claims abstract description 5
- 229910052709 silver Inorganic materials 0.000 claims abstract description 4
- 239000004332 silver Substances 0.000 claims abstract description 4
- 239000003708 ampul Substances 0.000 claims description 21
- 239000010453 quartz Substances 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 17
- 239000002184 metal Substances 0.000 claims description 17
- 239000010431 corundum Substances 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 230000004907 flux Effects 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 3
- 238000000859 sublimation Methods 0.000 abstract description 3
- 230000008022 sublimation Effects 0.000 abstract description 3
- 238000004164 analytical calibration Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 238000012937 correction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960000074 biopharmaceutical Drugs 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Abstract
The invention belongs to the technical field of environment aerosol, and particularly relates to a sublimation-desublimation-method nanometer aerosol generation system. The system mainly comprises an intake pipeline, a carrier gas circuit (solid sublimation), a cooling gas circuit and a combination gas circuit (steam desublimation), wherein the gas circuits are all completely sealed; the intake gas is divided into carrier gas and cooling gas through an entry tee joint; and the carrier gas circuit mainly comprises a valve, a flowmeter and a tubular resistance furnace. The system can be used for generating solid-state nanometer aerosol including sodium chloride and silver; the solid is sublimed into steam in the resistance furnace and then flows out with the carrier gas, and is mixed with the cooling gas circuit through a mixer downstream; and the average geometrical particle size range of the aerosol generated by steam desublimation is 1-100nm. The system has high working stability, and the average geometrical particle size range of the aerosol generated after 3 hours of continuous operation is within 2%. According to the system, the solvent is not needed, and the purity of the aerosol is high. The system is suitable for instrument calibration, aerosol characteristic research and nanometer material synthesis.
Description
Technical field
The invention belongs to environmental aerosols technical field, particularly a kind of Sublimation-desublimnanometerhod nanometerhod aerosol generation system and using method thereof and application.
Background technology
Aerosol generation systems can be applied to the field such as particle instrumental correction and nanometer aerosol characteristic research.Current most domestic aerosol generation systems, all for bio-pharmaceuticals, medical health field, only has minority to be applied to environmental area.In addition, these systems mainly produce the aerosol that particle diameter is submicron order, are not suitable for nanometer aerosol instrumental correction and related science research.As Chinese invention patent monodisperse aerosol generator (publication number CN101352661A) and bent capillary tube aerosol generator (publication number CN101610805A) make use of the aerosol that principle that capillary tube and cloud condense generates submicron order respectively.
Existing aerosol generation systems structure is comparatively complicated, adds the operation easier of system.Generation systems as Chinese invention patent (publication number CN1974387A) is made up of three parts, and regulating parameter is more, is not easy to use operation.In addition, the above-mentioned patent mentioned and other Chinese patent as sublimating and condensing method generate submicron order aerosol (publication number CN101284220A), aerosol generation systems (publication number CN102069046A) all adopts liquid phase spray-on process to generate aerosol.Impurity in solvent can reduce the aerocolloidal purity of final generation, and simultaneously in system operation, the volatilization of solvent can impact the aerocolloidal stability of generation.
Summary of the invention
Not enough for prior art, the invention provides a kind of Sublimation-desublimnanometerhod nanometerhod aerosol generation system and using method thereof and application.
A kind of Sublimation-desublimnanometerhod nanometerhod aerosol generation system, its entrance point threeway by pipeline respectively with air inlet pipeline, carrier gas gas circuit valve with cool gas circuit valve and be connected, carrier gas gas circuit valve door is connected with carrier gas gas circuit spinner flowmeter entrance by pipeline, the outlet of carrier gas gas circuit spinner flowmeter is connected with the quartz ampoule entrance of tube type resistance furnace by entrance point metal joint, quartz ampoule outlet is connected with port of export threeway by port of export metal joint, corundum boat being set in the quartz ampoule of described tube type resistance furnace, producing aerocolloidal solid for placing;
Cooling gas circuit valve is connected with cooling gas circuit spinner flowmeter entrance by pipeline;
The quartz ampoule outlet of the outlet of cooling gas circuit spinner flowmeter, tube type resistance furnace is connected with port of export threeway respectively with mixer entrance;
In described system, between each several part with pipeline, sealing is connected.
The interface size of described entrance point threeway, carrier gas gas circuit valve and carrier gas gas circuit spinner flowmeter is 3/8 inch.
The range of flow of described carrier gas gas circuit spinner survey is 0.02Lmin
-1~ 6Lmin
-1.
The range of flow of the cooling gas circuit spinner survey in described cooling gas circuit is 2Lmin
-1~ 30Lmin
-1.
The external diameter of described blender is 3/8 inch, and length is 1.75 inches, and wall thickness is 0.065 inch, and hole diameter is 0.2 inch, and is provided with chamfering, to ensure steady air current; The range of flow that described blender is suitable for is 5Lmin
-1~ 30Lmin
-1.
A using method for Sublimation-desublimnanometerhod nanometerhod aerosol generation system, by the temperature that changes in tube type resistance furnace and regulate carrier gas flux and cooling gas flow, regulates generated aerocolloidal domain size distribution.
An application for Sublimation-desublimnanometerhod nanometerhod aerosol generation system, described system is for the preparation of solid nano aerosol.
Described solid nano aerosol is salt or simple substance.
Described salt is sodium chloride, and described simple substance is silver.
Prepared aerosol geometric mean diameter is 1nm ~ 100nm.
Beneficial effect of the present invention is:
What obtained is nanometer aerosol, and its geometric mean diameter is within the scope of 1 ~ 100nm.The method obtain for polydispersed aerosol, minimum grain size can reach 0.6nm, maximum can to 400nm.Utilize sublimating and condensing method to produce aerosol not need to adopt solvent, effectively prevent solvent impurity to the impact generating aerosol purity, it also avoid the impact of solvent volatilization on system works stability.Native system has good job stability, and the aerosol geometric mean diameter fluctuation running generation in continuous 3 hours is no more than 2%, and total number density fluctuation is not higher than 6%.In addition, this system features in convenient, by changing temperature, carrier gas flux and the cooling gas circuit just aerocolloidal domain size distribution of adjustable generation in resistance furnace; System all have employed cutting ferrule and connects in each pipeline connects, and adopts rubber ring to seal, effectively ensure that the air-tightness of system in the junction of quartz ampoule and metal joint.
Accompanying drawing explanation
Fig. 1 is present system apparatus structure schematic diagram;
Fig. 2 is the embodiment of the present invention 1 mixer structure size design schematic diagram;
Number in the figure: 1-air inlet pipeline; The threeway of 2-entrance point; 3-carrier gas gas circuit valve; 4-carrier gas gas circuit spinner flowmeter; 5-entrance point metal joint; 6-quartz ampoule; 7-corundum boat; 8-tube type resistance furnace; 9-port of export metal joint; 10-cools gas circuit valve; 11-cools gas circuit spinner flowmeter; The threeway of the 12-port of export; 13-blender.
Detailed description of the invention
The invention provides a kind of Sublimation-desublimnanometerhod nanometerhod aerosol generation system, below in conjunction with the drawings and specific embodiments, the present invention will be further described.
A kind of Sublimation-desublimnanometerhod nanometerhod aerosol generation system, its entrance point threeway 2 by pipeline respectively with air inlet pipeline 1, carrier gas gas circuit valve 3 with cool gas circuit valve 10 and be connected, carrier gas gas circuit valve 3 is connected with carrier gas gas circuit spinner flowmeter 4 entrance by pipeline, carrier gas gas circuit spinner flowmeter 4 is exported and is connected with quartz ampoule 6 entrance of tube type resistance furnace 8 by entrance point metal joint 5, quartz ampoule 6 is exported and is connected with port of export threeway 12 by port of export metal joint 9, in the quartz ampoule 6 of described tube type resistance furnace 8, corundum boat 7 is set, for collecting aerosol solid;
Cooling gas circuit valve 10 is connected with cooling gas circuit spinner flowmeter 11 entrance by pipeline;
Cooling gas circuit spinner flowmeter 11 exports, the quartz ampoule 6 of tube type resistance furnace 8 exports and is connected with port of export threeway 12 respectively with blender 13 entrance;
In described system, between each several part with pipeline, sealing is connected.
Described entrance point threeway 2, carrier gas gas circuit valve 3 are 3/8 inch with the interface size of carrier gas gas circuit spinner flowmeter 4.
The range of flow that described carrier gas gas circuit spinner flowmeter 4 is measured is 0.02Lmin
-1~ 6Lmin
-1.
The range of flow that cooling gas circuit spinner flowmeter 11 in described cooling gas circuit is measured is 2Lmin
-1~ 30Lmin
-1.
The external diameter of described blender 13 is 3/8 inch, and length is 1.75 inches, and wall thickness is 0.065 inch, and hole diameter is 0.2 inch, and is provided with chamfering, to ensure steady air current; The range of flow that described blender 13 is suitable for is 5Lmin
-1~ 30Lmin
-1.
A using method for Sublimation-desublimnanometerhod nanometerhod aerosol generation system, by the temperature that changes in tube type resistance furnace 8 and regulate carrier gas flux and cooling gas flow, regulates generated aerocolloidal domain size distribution.
An application for Sublimation-desublimnanometerhod nanometerhod aerosol generation system, described system is for the preparation of solid nano aerosol.
Described solid nano aerosol is salt or simple substance.
Described salt is sodium chloride, and described simple substance is silver.
Prepared aerosol geometric mean diameter is 1nm ~ 100nm.
This system is formed with cooling gas circuit primarily of tube type resistance furnace, carrier gas gas circuit.The compressed air of clean dried enters carrier gas gas circuit and cooling gas circuit by air inlet pipeline 1 through entrance point threeway 2 shunting, the uninterrupted of carrier gas gas circuit is carried out respectively regulating by carrier gas gas circuit valve 3 and carrier gas gas circuit spinner flowmeter 4 and measures, and the uninterrupted of cooling gas circuit carries out respectively regulating by cooling gas circuit valve 10 with cooling gas circuit spinner flowmeter 11 and measures.Carrier gas enters entrance point metal joint 5 after carrier gas gas circuit spinner flowmeter 4, entrance point metal joint 5 is connected with the entrance point of quartz ampoule 6 in tube type resistance furnace 8, and adopt rubber ring to seal junction, ensure that air-tightness and the job stability of system.Be placed in the corundum boat 7 in interior quartz ampoule 6 for generation of aerocolloidal solid (as salt, simple substance etc.).In tube type resistance furnace 8, the solid sublimation of heating becomes gaseous molecular, and enters into downstream with carrier gas.Port of export metal joint 9 is connected with quartz ampoule 6 port of export, and the same rubber ring that uses seals.High temperature carrier gas is through port of export metal joint 9 and metallic conduit laggard inlet/outlet end threeway 12, and converge with refrigerating gas, blender 13 can realize the abundant mixing of high temperature carrier gas and refrigerating gas.The nanoparticles that gaseous molecular simultaneously in gas circuit is sublimated needed for formation under refrigerating gas effect.
Embodiment 1
Fig. 1 is present system apparatus structure schematic diagram.The compressed air of clean dried enters by air inlet pipeline 1 the entrance point threeway 2 that interface is 3/8 inch, splits into carrier gas gas circuit and cooling gas circuit.Cutting ferrule is all used to be connected between pipeline with threeway, to ensure gas circuit sealing.Carrier gas gas circuit caliber is 3/8 inch, and the uninterrupted of gas circuit is carried out respectively regulating by carrier gas gas circuit valve 3 and carrier gas gas circuit spinner flowmeter 4 and measures, and the measurement category of carrier gas gas circuit spinner flowmeter 4 is 0.02Lmin
-1~ 6Lmin
-1; The uninterrupted of cooling gas circuit carries out respectively regulating by cooling gas circuit valve 10 with cooling gas circuit spinner flowmeter 11 and measures, and the measurement category of cooling gas circuit spinner flowmeter 11 is 2Lmin
-1~ 30Lmin
-1.Carrier gas enters entrance point metal joint 5 after carrier gas gas circuit spinner flowmeter 4, entrance point metal joint 5 is connected with the entrance point of quartz ampoule 6 in tube type resistance furnace 8, and adopt rubber ring to seal junction, ensure that air-tightness and the job stability of system.
Quartz ampoule 6 pipe range in tube type resistance furnace 8 is 1.00m, and internal-and external diameter is respectively 36mm and 41mm.Be placed on for generation of aerocolloidal solid (as salt, simple substance etc.) in the corundum boat 7 in quartz ampoule 6.Corundum boat length 10cm, wall thickness is 3mm.The adjustable position of corundum boat 7 in tube type resistance furnace 8 of steel ruler can be utilized, thus change the aerocolloidal domain size distribution of generation.Solid carries out heating sublimation at resistance furnace and becomes gaseous molecular, and enters into downstream with carrier gas.Regulate the temperature in tube type resistance furnace 8 can change equally and generate aerocolloidal domain size distribution, the temperature control error of resistance in-furnace temperature is ± 1 DEG C, when in-furnace temperature is increased to 780 DEG C from 650 DEG C, the sodium chloride aerosol geometric mean diameter of generation increases to 83.9nm from 22.8nm.
Port of export metal joint 9 is connected with quartz ampoule 6 port of export, and the same rubber ring that uses seals.High temperature carrier gas enters into the port of export threeway 12 in downstream through metal joint and metallic conduit, converges with refrigerating gas.Port of export threeway 12 caliber is standard size 3/8 inch.In order to make high temperature carrier gas fully mix with refrigerating gas better, be provided with blender 13 in port of export threeway 12 downstream.The operation principle of blender 13 is: the aperture increasing a specific dimensions in the duct, causes interference to air-flow, forms turbulent flow, thus realizes the abundant mixing of gas fast.Blender external diameter in present system is 3/8 inch, and wall thickness is 0.065 inch, and hole diameter is 0.2 inch, and the range of flow be suitable for is 5Lmin
-1~ 30Lmin
-1.Blender 13 aperture place is provided with chamfering, to ensure steady air current.In the process that high temperature carrier gas mixes with refrigerating gas, heat the nano-scale particle thing that the gaseous molecular generated is sublimated needed for formation under cooling effect.
Increase carrier gas flux keeps constant can the increase of refrigerating gas to generate aerocolloidal concentration, when carrier gas flux is from 1Lmin simultaneously
-1be increased to 2.33Lmin
-1time, generate aerosol Particle density from ~ 10
7individual cm
-3increase to ~ 10
8individual cm
-3, and geometric mean diameter does not have significant change.
Claims (10)
1. a Sublimation-desublimnanometerhod nanometerhod aerosol generation system, it is characterized in that: entrance point threeway (2) by pipeline respectively with air inlet pipeline (1), carrier gas gas circuit valve (3) is connected with cooling gas circuit valve (10), carrier gas gas circuit valve (3) is connected with carrier gas gas circuit spinner flowmeter (4) entrance by pipeline, carrier gas gas circuit spinner flowmeter (4) outlet is connected with quartz ampoule (6) entrance of tube type resistance furnace (8) by entrance point metal joint (5), quartz ampoule (6) outlet is connected with port of export threeway (12) by port of export metal joint (9), in the quartz ampoule (6) of described tube type resistance furnace (8), corundum boat (7) is set, aerocolloidal solid is produced for placing,
Cooling gas circuit valve (10) is connected with cooling gas circuit spinner flowmeter (11) entrance by pipeline;
Quartz ampoule (6) outlet of cooling gas circuit spinner flowmeter (11) outlet, tube type resistance furnace (8) is connected with port of export threeway (12) respectively with blender (13) entrance;
In described system, between each several part with pipeline, sealing is connected.
2. system according to claim 1, is characterized in that: described entrance point threeway (2), carrier gas gas circuit valve (3) are 3/8 inch with the interface size of carrier gas gas circuit spinner flowmeter (4).
3. system according to claim 1, is characterized in that: the range of flow that described carrier gas gas circuit spinner flowmeter (4) is measured is 0.02Lmin
-1~ 6Lmin
-1.
4. system according to claim 1, is characterized in that: the range of flow that the cooling gas circuit spinner flowmeter (11) in described cooling gas circuit is measured is 2Lmin
-1~ 30Lmin
-1.
5. system according to claim 1, is characterized in that: the external diameter of described blender (13) is 3/8 inch, and length is 1.75 inches, and wall thickness is 0.065 inch, and hole diameter is 0.2 inch, and is provided with chamfering, to ensure steady air current; The range of flow that described blender (13) is suitable for is 5Lmin
-1~ 30Lmin
-1.
6. the using method of a Sublimation-desublimnanometerhod nanometerhod aerosol generation system as claimed in claim 1, it is characterized in that: by the temperature that changes in tube type resistance furnace (8) and regulate carrier gas flux and cooling gas flow, regulate generated aerocolloidal domain size distribution.
7. an application for Sublimation-desublimnanometerhod nanometerhod aerosol generation system as claimed in claim 1, is characterized in that: described system is for the preparation of solid nano aerosol.
8. application according to claim 7, is characterized in that: described solid nano aerosol is salt or simple substance.
9. application according to claim 8, is characterized in that: described salt is sodium chloride, and described simple substance is silver.
10. application according to claim 7, is characterized in that: prepared aerosol geometric mean diameter is 1nm ~ 100nm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310153696.7A CN103212349B (en) | 2013-04-27 | 2013-04-27 | Sublimation-desublimation-method nanometer aerosol generation system and application method and application |
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|---|---|---|---|
| CN201310153696.7A CN103212349B (en) | 2013-04-27 | 2013-04-27 | Sublimation-desublimation-method nanometer aerosol generation system and application method and application |
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| Publication Number | Publication Date |
|---|---|
| CN103212349A CN103212349A (en) | 2013-07-24 |
| CN103212349B true CN103212349B (en) | 2015-02-18 |
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| CN116510513A (en) | 2018-04-13 | 2023-08-01 | 江苏新世纪江南环保股份有限公司 | Oxidation method and device for ammonia desulfurization solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284220A (en) * | 2008-06-03 | 2008-10-15 | 清华大学 | Quasi-monodispersed submicron aerosol generating device using vaporization condensation process |
| CN101352661A (en) * | 2008-09-18 | 2009-01-28 | 中国建筑科学研究院 | Monodisperse aerosol generator |
| CN102036724A (en) * | 2008-05-19 | 2011-04-27 | 赢创德固赛有限公司 | Process for the phase transformation of substances |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2006200755B2 (en) * | 2005-07-11 | 2011-02-10 | Cyclomedica Australia Pty Limited | Improved process for the production of a radioactive aerosol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102036724A (en) * | 2008-05-19 | 2011-04-27 | 赢创德固赛有限公司 | Process for the phase transformation of substances |
| CN101284220A (en) * | 2008-06-03 | 2008-10-15 | 清华大学 | Quasi-monodispersed submicron aerosol generating device using vaporization condensation process |
| CN101352661A (en) * | 2008-09-18 | 2009-01-28 | 中国建筑科学研究院 | Monodisperse aerosol generator |
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