CN110965046A - Ultra-thin liquid film rotary separating type vaporizing device - Google Patents
Ultra-thin liquid film rotary separating type vaporizing device Download PDFInfo
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- CN110965046A CN110965046A CN201911421703.0A CN201911421703A CN110965046A CN 110965046 A CN110965046 A CN 110965046A CN 201911421703 A CN201911421703 A CN 201911421703A CN 110965046 A CN110965046 A CN 110965046A
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- 230000008016 vaporization Effects 0.000 title claims abstract description 51
- 239000007788 liquid Substances 0.000 title claims abstract description 33
- 239000012159 carrier gas Substances 0.000 claims abstract description 49
- 238000009834 vaporization Methods 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 34
- 239000007789 gas Substances 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 42
- 238000009413 insulation Methods 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 5
- 230000006641 stabilisation Effects 0.000 claims description 5
- 238000011105 stabilization Methods 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000006200 vaporizer Substances 0.000 claims description 4
- 239000010727 cylinder oil Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims 1
- 239000011521 glass Substances 0.000 abstract description 5
- 239000012071 phase Substances 0.000 description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 3
- 235000017491 Bambusa tulda Nutrition 0.000 description 3
- 241001330002 Bambuseae Species 0.000 description 3
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 3
- 239000011425 bamboo Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 150000003606 tin compounds Chemical class 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 239000002346 layers by function Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000006124 Pilkington process Methods 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/245—Oxides by deposition from the vapour phase
- C03C17/2453—Coating containing SnO2
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/211—SnO2
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/73—Anti-reflective coatings with specific characteristics
- C03C2217/732—Anti-reflective coatings with specific characteristics made of a single layer
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/152—Deposition methods from the vapour phase by cvd
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention relates to an ultrathin liquid film rotary separation type vaporizing device, which solves the technical problems of uneven coating gas phase, difficult thorough vaporization, large vaporizing device and low efficiency of the existing vaporizing device and comprises a cylinder body, a material preheating device, a carrier gas heating device, a mixing device and a heating device, wherein a scraper, a scraper supporting end cover and a sealing cover are arranged inside the cylinder body, an oil heating pipe is arranged inside the supporting end cover, the front end of the cylinder body is respectively connected with the material preheating device and the carrier gas heating device through a top material inlet and a side carrier gas inlet, and the rear end of the cylinder body is respectively connected with the precursor raw material mixed gas mixing device and the heating device through a tail mixed gas outlet and a cylinder body oil inlet and outlet. The invention can be widely applied to the vaporization of the ultrathin liquid film of the precursor raw material for the coated glass.
Description
Technical Field
The invention relates to a rotary-separating type vaporization device for an ultrathin liquid film of a precursor raw material for producing low-radiation coated glass on line on a float production line by using a chemical vapor deposition method, in particular to an organic tin compound as a coating precursor.
Background
The tin dioxide film has a strong reflection effect on the mid-far infrared rays, the low-radiation coated glass is formed by coating the tin dioxide film on the surface of the glass as a functional layer, the thicker the tin dioxide film layer is, the lower the radiation rate is, the stronger the reflection effect of the film on the mid-far infrared rays is, and the better the energy-saving effect is.
The low-radiation coated glass is produced on line by a chemical vapor deposition method, typical functional layer coating precursor raw materials are organic compounds of a plurality of tin, are liquid at normal temperature, have boiling points as high as 221 ℃, and are difficult to vaporize, so that the device capable of providing high-efficiency, stable and uniform coating vapor-phase precursor mixed gas is particularly important.
A bubbler is a more typical evaporation device and is usually operated below the boiling point of the liquid. The gas distribution pipe is immersed in the liquid to a proper depth, the liquid raw material is heated to a set temperature in the container, the carrier gas is continuously introduced to form bubbles, in the rising process, the liquid on the surface of the bubbles evaporates into the bubbles to form saturated vapor at the temperature, and a large amount of saturated vapor is broken and released along with the rising of the bubbles to the liquid surface. The vaporization mode determines that the bubbling temperature must be increased to obtain more gas-phase products under the condition of constant carrier gas flow, but the vapor pressure value curve value of the substance is usually very high in slope in a high-temperature section, and the vapor pressure value is severely changed due to small temperature fluctuation, so that the operation is difficult in production practice. In addition, more gas-phase products can be obtained by increasing the flow rate of the carrier gas in a more gentle temperature section, but the gas-liquid entrainment is easily formed by increasing the flow rate of the carrier gas once under the influence of the surface area size of the bubbler, so that the concentration of the mixed gas is distorted. If an excessively increased bubbler area is used, the cost is also increased, and thus the bubbler cannot provide a highly efficient, stable and uniform coating gas-phase precursor mixture.
The utility model discloses a chinese utility model patent of application number is CN02215556.2, the name is vaporizer of chemical vapor deposition proplastid, an upper portion cylinder is described, the lower part is the obconic, there is the barrel of a plurality of baffles in the centre, barrel upper portion is equipped with proplastid atomizer, the proplastid after preheating at first passes through the atomizer, be atomized into 5-30 micron fog drops, the carrier gas of heating drives the fog drop and moves to the bottom gas outlet between the S type passageway that the baffle formed, in-process fog drop and section of thick bamboo wall contact, absorbed energy and vaporization after being heated by section of thick bamboo wall, the S type is led to and is increased the fog drop vaporization and becomes, nevertheless can't ensure in all fog drop strokes totally by section of thick bamboo wall heating back vaporization, need a huge barrel to ensure effectual vaporization efficiency for this reason. In addition, the difference in the droplet diameter also leads to differences in the homogeneity of the mixture concentration during the vaporization process. Therefore, the vaporizer is not suitable for providing high-efficiency, stable and uniform coating gas-phase precursor mixed gas.
Disclosure of Invention
The invention provides an ultrathin liquid film rotary-separation type vaporizing device which solves the technical problems of uneven coating gas phase, difficult thorough vaporization, large vaporizing device and low efficiency of the existing vaporizing device and has the advantages of even coating gas phase, thorough vaporization, compact structure and high efficiency.
The invention provides an ultrathin liquid film rotary vaporization device, which is provided with a horizontal uniform-section jacket cylinder, a material preheating device, a carrier gas heating device, a precursor raw material mixed gas mixing device and a heating device, wherein a scraper is arranged in the jacket cylinder, scraper supporting end covers and sealing covers are arranged at the front end and the rear end of the jacket cylinder, a heating pipe is arranged in each supporting end cover, the front end of the jacket cylinder is respectively connected with the material preheating device and the carrier gas heating device through a top material inlet and a side carrier gas inlet, the rear end of the jacket cylinder is respectively connected with the precursor raw material mixed gas mixing device and the heating device through a tail mixed gas outlet and a cylinder oil inlet and outlet, the scraper is driven by a motor to rotate to vaporize the preheated and premixed material into an ultrathin liquid film, the ultrathin liquid film is heated and vaporized through the inner wall of the liquid film jacket cylinder, the mixed steam enters the precursor raw material mixed steam mixing device through the tail mixed steam outlet, and enters the coating reactor after being uniformly mixed by force.
Preferably, the scraper is a six-piece symmetrical fixed scraper, the scraper divides the interior of the cylinder into a premixing area, a forced vaporization area and a homogenization stabilization area, the scraper is positioned in the forced vaporization area, the material preheating device and the carrier gas heating device are directly communicated with the premixing area, and the precursor raw material mixed gas mixing device is directly communicated with the homogenization stabilization area.
Preferably, the top feed inlet is disposed within the premixing zone at a 90 ° angle to the side carrier gas inlet and is in the same cross-section.
Preferably, the raw material preheating device comprises a preheater, a material flow meter and a heat conducting oil furnace valve, wherein a thermocouple is arranged on the preheater, and the preheating temperature of the preheater is 160 +/-1 ℃.
Preferably, the precursor raw material mixed steam mixing device comprises a mixer, an electric tracing heat insulation pipeline, an electric tracing band and a patch thermal resistor, the mixed steam is conveyed through the electric tracing heat insulation pipeline, and the temperature of the electric tracing heat insulation pipeline is controlled to be 180 +/-1 ℃.
Preferably, the carrier gas heating device comprises a carrier gas heater, a heater thermocouple, a pressure reducer, a valve and a storage tank, a carrier gas flowmeter is further arranged between the carrier gas heater and the storage tank to control the flow rate of the carrier gas, and the flow rate of the section of the cylinder body controlled by the carrier gas flowmeter ranges from 0.3 m/s to 1 m/s.
Preferably, the heat supply device comprises an oil pump, a heat conduction oil furnace, a heat conduction thermocouple and a heat conduction oil furnace valve, a heat medium is input into the cylinder jacket through the cylinder oil inlet and outlet, the heat supply device also provides the heat medium for the raw material preheating device, the carrier gas heating device and the heating pipe in the cylinder end cover, the heat medium is heat conduction oil, the heat medium is heated by the heat conduction oil furnace in the heat supply device and forms heat conduction oil closed circulation, and the temperature of the heat conduction oil is 180 +/-1 ℃.
Preferably, the clearance between the six symmetrical fixed scrapers in the forced vaporization region and the inner wall of the cylinder is less than 1mm, and the linear speed of the scrapers is 10-12 m/s.
Preferably, the vaporization area of the ultrathin liquid film rotary vaporization device is 1.6 to 1.9 square meters, the vaporization amount of the material reaches 1.8 to 2.1kg/min, and the material is organic tin compound.
Preferably, a mixed steam flow meter is arranged on the mixer, the mixed steam flow meter can monitor the vaporization efficiency on line, and the material vaporization efficiency is changed by adjusting the heating temperature of the cylinder body, the rotating speed of the scraper blade and the flow of the carrier gas.
The invention has the beneficial effects that:
the invention has high vaporization efficiency, uniform gas mixture after vaporization of the precursor, and can force vaporization of the mutually soluble multicomponent precursor raw materials.
Repeated experiments show that the vaporization rate of the organic tin compound reaches 100 percent, and the utilization rate of raw materials is improved by nearly 45 percent; the vaporization speed is improved by about 2 times compared with the prior art, and the uniformity and the stability of the mixed steam of the raw material precursor are also obviously improved.
Drawings
FIG. 1 is a schematic view of the main apparatus of the present invention in connection with a preheater and a mixer;
FIG. 2 is a schematic view showing the connection of the main body apparatus of the present invention with a carrier gas heater and a heat-conducting oil furnace.
Description of the symbols of the drawings:
1. a material flow meter; 2. a preheater; 3. the end cover is provided with an oil inlet and outlet flange; 4. a sealing device; 5. a variable frequency motor; 6. heating a tube; 7. supporting the end cap; 8. a carrier gas inlet; 9. a pre-mixing zone; 10. a forced vaporization area 11, a fixed scraper; 12. a homogenization stabilization zone; 13. an outlet thermocouple; 14. a material inlet; 15. the cylinder body is provided with an oil inlet and an oil outlet; 16. a horizontally arranged constant-section jacket type cylinder body; 17. a tail mixed gas outlet; 18. a mixer; 19. a mixed gas flowmeter; 20. coating a film reactor; 21. a storage tank; 22. a pressure reducer; 23. a valve; 24. a carrier gas flow meter; 25. a gap is formed between the scraper and the inner wall of the cylinder body; 26. an oil pump; 27. a heat conducting oil furnace valve; 28. a heat-conducting oil furnace; 29. a carrier gas heater; 30. a heater thermocouple; 31. a heat tracing pipeline; 32. a heat conducting oil thermocouple; 33. a thermocouple; 34. an electric tracing band; 35. a patch thermal resistor.
Detailed Description
The present invention is further described below with reference to the drawings and examples so that those skilled in the art can easily practice the present invention.
Example 1: as shown in the figure 1-2, the invention is provided with a transverse uniform-section jacketed cylinder 16, six symmetrical fixed scrapers 11, a scraper support end cover 7, a sealing device 4, a top material inlet 14, a side carrier gas inlet 8 and a tail mixed gas outlet 17, and the auxiliary equipment comprises a heat conduction oil furnace 28, a material flow meter 1, a material preheater 2, a carrier gas flow meter 24, a carrier gas heater 29, a mixer 18, a heat tracing pipeline 31, a mixed gas flow meter 19 and temperature, rotating speed and flow control devices.
And (3) working preheating stage:
hot oil is heated in a heat conduction oil furnace 28, a thermocouple 32 of the heat conduction oil furnace controls the temperature, the oil circulates among the heat conduction oil furnace 28, a jacket cylinder 16, a support end cover 7 and a preheater 2, the oil quantity is adjusted by a valve 27 of the heat conduction oil furnace, the temperature is controlled by a patch thermal resistance thermocouple 33, the temperature of the preheating oil of the materials is controlled to be 160 +/-1 ℃ in order to reduce the evaporation of the materials in advance. The quantity of the heat-conducting oil entering the jacket through the inlet and the outlet 15 of the cylinder is regulated by a heat-conducting oil furnace valve 27, and the temperature of the heat-conducting oil is controlled to 180 +/-1 ℃ by a heat-conducting oil furnace thermocouple 32. Nitrogen is used as carrier gas, is controlled by a valve 23 from a storage tank 21 through a pressure reducer 22, is controlled at 80-120m3/h through a flow meter 24, and is controlled at the temperature of 180 +/-1 ℃ through a heater 29 and a heater thermocouple 30. The mixer tube 31 is heated by the electric tracing band 34 and the patch heating resistor 35 is controlled to 180 + -1 deg.C.
The working stage is as follows:
when the system reaches the working temperature, the material enters from a material inlet 14 at the top of the vaporizer, the nitrogen enters from a carrier gas inlet 8 at the side surface, the material inlet and the carrier gas inlet are arranged in a premixing area 9 to form an included angle of 90 degrees and are positioned on the same section, the continuous liquid material flow is directly blown away by the carrier gas to form liquid drops and fog drops, the carrier gas pushes the liquid drops and the fog drops to pass through a forced vaporization area 10, the clearance 25 between six symmetrical fixed scrapers 11 in the forced vaporization area 10 and the inner wall of the cylinder body is less than 1mm, the rotating speed of the scrapers is adjusted by a variable frequency motor 5, the linear speed of the scrapers is controlled to be 10-12m/s, the liquid drops and the fog drops are forced to rotate away from the inner wall of the cylinder body to form ultrathin heat conduction oil under the centrifugal force action of the continuous rotating scrapers, the heat conduction, the gas-carrier flow meter 24 controls the flow rate of the gas carrier to ensure that the section flow rate of the cylinder 16 with the equal section is in the range of 0.3-1m/s, and in order to prevent the mixed gas from condensing on the supporting end cover 7 and reduce the vaporization efficiency, the oil heating pipes 6 are distributed in the supporting end cover 7 and connected with the heat-conducting oil furnace 28 through the end cover oil inlet and outlet flange 3 to prevent the cold wall effect. The precursor mixed gas passes through the homogenizing and stabilizing zone 12, enters the mixer 18 through the gas outlet 17 to be forcibly mixed, and flows through the heat tracing pipeline through the mixed gas flowmeter 19 (high-temperature vortex shedding flowmeter) to be conveyed to the coating reactor. The value of the outlet thermocouple 13 and the converted value of the material flowmeter 1 are compared with the difference value between the mixed gas flowmeter 19 and the carrier gas flowmeter 24, and the heating temperature of the cylinder, the rotating speed of the scraper and the flow of the carrier gas are adjusted to greatly improve the vaporization efficiency of the organotin compound.
The above description is only for the purpose of illustrating preferred embodiments of the present invention and is not to be construed as limiting the present invention, and it is apparent to those skilled in the art that various modifications and variations can be made in the present invention. All changes, equivalents, modifications and the like which come within the scope of the invention as defined by the appended claims are intended to be embraced therein.
Claims (10)
1. A super-thin liquid film rotary-separation type vaporizing device is characterized by comprising a transverse uniform-section jacket barrel, a material preheating device, a carrier gas heating device, a precursor raw material mixed gas mixing device and a heating device, wherein a scraper is arranged in the jacket barrel, scraper supporting end covers and sealing covers are arranged at the front end and the rear end of the jacket barrel, a heating pipe is arranged in each supporting end cover, the front end of the jacket barrel is respectively connected with the material preheating device and the carrier gas heating device through a top material inlet and a side carrier gas inlet, the rear end of the jacket barrel is respectively connected with the precursor raw material mixed gas mixing device and the heating device through a tail mixed gas outlet and a barrel oil inlet and outlet, the scraper is driven to rotate by a motor to vaporize a preheated premixed material to form a super-thin liquid film jacket, the super-thin liquid film is heated and vaporized through the inner wall of the barrel and is mixed with hot carrier gas, the mixed steam enters the precursor raw material mixed steam mixing device through the tail mixed steam outlet, is uniformly mixed by force and then enters the coating reactor.
2. The ultrathin liquid film rotary evaporation device as claimed in claim 1, wherein the scraper is a six-piece symmetrical fixed scraper, the scraper divides the inside of the cylinder into a premixing zone, a forced evaporation zone and a homogenization stabilization zone, the scraper is located in the forced evaporation zone, the material preheating device and the carrier gas heating device are directly communicated with the premixing zone, and the precursor raw material mixed gas mixing device is directly communicated with the homogenization stabilization zone.
3. The apparatus of claim 1, wherein the top material inlet and the side carrier gas inlet are arranged in the premixing area at an angle of 90 ° and located at the same cross section.
4. The ultra-thin liquid film cyclone vaporization device according to claim 1, wherein the raw material preheating device comprises a preheater, a material flow meter and a heat conducting oil furnace valve, a thermocouple is provided on the preheater, and the preheating temperature of the preheater is 160 ± 1 ℃.
5. The ultra-thin liquid film spin-off vaporizer of claim 1, wherein the precursor-material mixture-vapor mixer comprises a mixer, an electric tracing heat-insulation pipe, an electric tracing band, and a patch-type thermal resistor, and the mixture vapor is transported through the electric tracing heat-insulation pipe, and the temperature of the electric tracing heat-insulation pipe is controlled to be 180 ± 1 ℃.
6. The ultra-thin liquid film spin-off vaporizing device according to claim 1, wherein the carrier gas heating device comprises a carrier gas heater, a heater thermocouple, a pressure reducer, a valve and a storage tank, a carrier gas flow meter is further arranged between the carrier gas heater and the storage tank to control the flow rate of the carrier gas, and the flow rate of the carrier gas flow meter controls the cross section of the cylinder to be in the range of 0.3-1 m/s.
7. The ultra-thin liquid film cyclone vaporization device according to claim 1, wherein the heat supply device comprises an oil pump, a heat conduction oil furnace, a heat conduction thermocouple and a heat conduction oil furnace valve, a heat medium is fed into the inside of the cylinder jacket through the cylinder oil inlet and outlet, and the heat supply device also provides a heat medium for the raw material preheating device, the carrier gas heating device and the heating pipe in the cylinder end cap, the heat medium is heat conduction oil, the heat medium is heated by the heat conduction oil furnace in the heat supply device, and a closed circulation of the heat conduction oil is formed, and the temperature of the heat conduction oil is 180 ± 1 ℃.
8. The ultra-thin liquid film cyclone vaporization device according to claim 1, wherein the vaporization area of the ultra-thin liquid film cyclone vaporization device is 1.6 to 1.9 square meters, the vaporization amount of the material is 1.8 to 2.1kg/min, and the material is an organotin compound.
9. The ultra-thin liquid film spin-off vaporizing device according to claim 2, wherein the clearance between the six symmetrical fixed scrapers in the forced vaporizing zone and the inner wall of the cylinder is less than 1mm, and the linear velocity of the scrapers is 10-12 m/s.
10. The ultra-thin liquid film rotary vaporization device according to claim 5, wherein the mixer is provided with a mixed gas flow meter, the mixed gas flow meter can monitor the vaporization efficiency on line, and the vaporization efficiency of the material can be changed by adjusting the heating temperature of the cylinder, the rotation speed of the scraper and the flow rate of the carrier gas.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911421703.0A CN110965046B (en) | 2019-12-31 | 2019-12-31 | Ultra-thin liquid film rotary-off type vaporizing device |
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| CN201911421703.0A CN110965046B (en) | 2019-12-31 | 2019-12-31 | Ultra-thin liquid film rotary-off type vaporizing device |
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| CN110965046A true CN110965046A (en) | 2020-04-07 |
| CN110965046B CN110965046B (en) | 2024-05-28 |
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Citations (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE661242A (en) * | 1964-03-17 | 1965-09-17 | ||
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