Prepare the spray-fluidized granulation tower of hollow iodine particle and the tincture of iodine
Technical field
The invention belongs to chemical technology field, in particular to a kind of spray-fluidized granulation tower and the using method thereof of preparing hollow iodine particle and the tincture of iodine.
Background technology
Iodine at medicine, agricultural, chemical industry, military project etc. are technical is widely used.Generally, method prepared by iodine is: Air blowing method, makes iodine free and contact with air, blown out by iodine with air with oxidizing containing iodine bittern, after blowout contain iodine air through absorption, crystallization, refine and obtain new product iodine.But the solid iodine irregular shape that blowout method obtains, and specific area is less, application is very limited, because be no matter the smart iodine of 99.5% (Chinese Pharmacopoeia standard C P2005 standard iodine content), or the thick iodine of about 95.0%, the application that granulation formation could meet new and high technology must be carried out, just there are good market prospects, therefore, use better granulating technique to prepare the iodine particle of more Codes and Standards, have the great market demand.
Existing granulating technique has a lot, has fluidized bed prilling, spouted bed granulation, mist projection granulating, stirring rolling granulation, is uniformly mixed granulation, pressure forming granulation, sinter molding granulation, liquid granulation etc.Wherein, be usually used in the technology mainly mist projection granulating of iodine granulation, but because iodine is the relatively close material of a kind of molten boiling point, very easily distil, therefore, in the process of mist projection granulating, the loss of the gaseous iodine after iodine distillation is often larger, therefore, need better atomizing granulating technology and equipment, overcome these problems.
In prior art, prepared by mist projection granulating to the report of the technology of iodine particle, mainly use the technology of high-tower granulation, these technology are not optimized for the structure of granulation tower, and the thermal efficiency is lower, simultaneously, it is incomplete all to there is iodine condensation in the atomization condensing agent used, part iodine is had to distil with condensing agent, so that produce the waste of raw material, and contaminated environment.
Summary of the invention
For the problem in above-mentioned high tower spraying iodine granulation production process, inventors have developed better high tower spraying iodine granulation equipment, make production technology more efficient, solve the various problems in above-mentioned production process simultaneously.
First the present invention relates to a kind of spray-fluidized granulation tower for the production of industrial iodine particle, the tower body top of described granulation tower is provided with liquid iodophor container tank (1), liquid iodophor jet pipe group (2) and liquid iodophor reservoir, probe into top, tower chamber, tower body evenly arranges condensation jet head sets (3), described condensation spray painting head group (3) is connected with compression pump (4) by pipeline, tower body inner bottom part is provided with the screen cloth (5) of the inclination of collecting iodine particle, described screen cloth (5) is positioned at immediately below liquid iodophor jet pipe group (2) to be located, the iodine particle that screen cloth (5) is collected will roll along screen cloth inclined-plane and collect and be stored in container (7), the bottom of tower body tilts to the opposite side of container (7), the liquid iodophor not condensing into solid particle is collected in container (6), described granulation tower body top is provided with the gas pipeline (9) for discharging gas in tower, gas pipeline (9) is provided with equally and bleeds with compression pump (4), being reclaimed by container (6) containing iodine vapor in gas pipeline (9).
The condensing agent that described condensation jet head sets (3) is sprayed is,
1), through the cold air of precooling;
2), through the water mixing cold air of precooling;
3), through the ethanol mixing cold air of precooling;
Or 4), the condensing agent of above-mentioned (1) ~ (3) uses at mutual interval successively.
Described liquid iodophor container tank is provided with constant temperature heating device, ensures that in its tank, temperature is 115-120 DEG C, during work, is extruded by the liquid iodophor in tank by air pressure or hydraulic means by jet pipe in granulation tower.
Described liquid iodophor jet pipe group (2) comprises altogether 6 ~ 10 nozzles evenly arranged, and nozzle inside diameter 1.1mm, by pressure in regulating tank, make the flow of each nozzle be 300 ~ 500g/min, the liquid-drop diameter of outflow is 0.4 ~ 4mm.
In granulation tower, the condensing agent of precooling is sprayed by the shower nozzle (3) be connected with described pump (4), the condensing agent temperature of described precooling is less than 15 DEG C, pump described in connection and the pipeline of shower nozzle are arranged in the heat-insulation layer (8) of tower outer wall, form the loop type cooling tube system of circulation rotating.
Described shower nozzle is arranged at and gos deep into 10 ~ 20mm place, distance tower surface in tower chamber, and each radial direction has 3-8, and the spacing between the nozzle of vertical direction is 0.5m ~ 1m, is often separated by 60 ~ 90 degree arranges one group of shower nozzle in the side of cylindrical tower body.
By regulating the pressure of pump and the bore of shower nozzle, make the condensing agent of precooling be pressurized to 80-100PSIG (pound/square inch), the speed that the condensing agent of precooling sprays in tower is: 80cm
3/ min, when condensing agent is gas-liquid mixture, the particle of the atomized drop sprayed into is 10-150 μm.
Inclined-plane is set to bottom granulation tower, so that collection has been dissolved the ethanolic solution of iodine or has been dissolved the aqueous solution of iodine, container is preinstalled with alcohol solvent in (6), dissolved the ethanolic solution of iodine by container (6) recovery or dissolved the aqueous solution of iodine, obtaining concentration is the iodine solution of 1 ~ 2%.
The screen cloth that described screen cloth (5) is formed for flexible material, the screen-aperture of wire side is 0.1 ~ 0.3mm, for collecting the complete iodine particle of granulation and the solid-state iodine fragment of filtering or dissolved the cooling fluid of iodine, the iodine particle collected is rolled in container (7) by the screen cloth tilted.
The method of hollow iodine particle and iodine solution prepared by the granulation tower that the invention still further relates to described in use, and described method comprises:
(1) open pump (4) injects by precooling cryogen in cool cycles pipeline, is sprayed the condensing agent of precooling by condensation fog spray head in tower chamber;
(2) iodine in container tank is heated to 115-120 DEG C, obtains liquid iodophor, by pressurization, liquid iodophor is sprayed with drops from jet pipe;
(3) liquid iodophor drop becomes hollow iodine particle by condensing agent cooling in the process fallen, by being arranged at inclination screen cloth at the bottom of tower and collecting iodine particle and the solid-state iodine fragment of filtering or dissolved the cooling fluid of iodine, be collected in the iodine particle collector at the bottom of tower, and the ethanolic solution having dissolved iodine or the aqueous solution that dissolved iodine are collected in the returnable of opposite side at the bottom of tower, obtain iodine solution.
As required, method of the present invention also comprises,
(4) use successively the cold air through precooling, water mixing cold air through precooling, through precooling ethanol mixing cold air as condensing agent, prepare described hollow iodine particle.
The present invention uses the condensing agent of multiple precooling to spray in granulation tower and forms cooling mist, and meanwhile, condensing agent forms cooling layer in the pipeline around tower wall, compared to traditional single type air-atomizing tower, has better cooling effect.Meanwhile, when condensing agent is gas-liquid mixed cooling mist, better heat exchange effect, better thermal capacitance or better cycle efficieny is had.Especially when three kinds of condensing agents use alternately, air cooling-down speed is very fast, water+air mixture can provide larger thermal capacitance, and the iodine vapor of ethanol to the iodine fragment and distillation of failing to condense into particle has good solvability, the loss of the iodine of pelletization can be avoided, iodine solution can be obtained while granulation.To sum up, the present invention has better environment friendly and more up to iodine recovery utilization rate.
Accompanying drawing explanation
The spray-fluidized granulation tower of Fig. 1, the hollow iodine particle of preparation of the present invention and the tincture of iodine
Detailed description of the invention
Below by way of specific embodiment, technical scheme of the present invention is described
The production (condensing agent is air) of the solid-state hollow iodine particle of embodiment 1. and the tincture of iodine
As shown in Figure 1, granulation tower tower height 3 meters, the volume being positioned at the liquid iodophor container tank (1) of tower top is 15L, be heated to temperature 120 degree in tank, melting solid-state iodine is liquid iodophor, and the nozzle sets (2) below tank arranges altogether 6, each nozzle diameter 1.1mm, the liquid iodophor flow of single-nozzle is 400g/min, and the liquid-drop diameter oozed is 0.4-5mm.
Precooled air is as cooling agent, circulating cooling pipe is pumped into by pump (4), and in tower, carry out atomized spray by shower nozzle (3), temperature in tower body and tower chamber is cooled to less than 15 DEG C by described cooling agent, in this circulatory system, cold air is pressurized to 80-100PSIG (pound/square inch), and the speed of spraying in tower is: 80cm
3/ min.Tower wall has the radial jet head sets of 6 covers, the shower nozzle distribution in each direction, equidistant setting, and the air in tower chamber is extracted out by pump by the pipeline (9) being arranged at tower top, and by returnable (6) recovery iodine wherein.
Liquid iodophor drop through misting cooling is frozen into solid-state iodine in dropping process, due to condensation process expand with heat and contract with cold and capillary uneven, form the hollow spherical particle of 0.5 ~ 4mm diameter, by being arranged at the liquid iodophor and particle disintegrating slag that at the bottom of tower, screen cloth 5 elimination is not condensed, solid-state iodine powder collection is in container 7, the iodine vapor of distillation collected by ethanol in container 6, obtains iodine solution.
Described screen cloth is flexible material, can effectively prevent falling of iodine particle cracked.
The production (condensing agent is the water mixing cold air through precooling) of the solid-state hollow iodine particle of embodiment 2. and the tincture of iodine
As shown in Figure 1, granulation tower tower height 3 meters, the volume being positioned at the liquid iodophor container tank (1) of tower top is 15L, be heated to temperature 120 degree in tank, melting solid-state iodine is liquid iodophor, and the nozzle sets (2) below tank arranges altogether 6, each nozzle diameter 1.1mm, the liquid iodophor flow of single-nozzle is 400g/min, and the liquid-drop diameter oozed is 0.4-5mm.
Through the water mixing cold air of precooling as condensing agent, the circulating cooling pipe being arranged in insulating (8) is pumped into by pump (4), and in tower, carry out atomized spray by shower nozzle (3), temperature in tower body and tower chamber is cooled to less than 15 DEG C by described cooling fluid, in this circulatory system, condensing agent is pressurized to 80-100PSIG (pound/square inch), and the speed of spraying in tower is: 80cm
3/ min, the droplet particles of the atomization condensing agent sprayed into is 10-150 μm.Tower wall has the radial jet head sets of 6 covers, the shower nozzle distribution in each direction, equidistant setting, and the air in tower chamber is extracted out by pump by the pipeline (9) being arranged at tower top, and by returnable (6) recovery iodine wherein.
Liquid iodophor drop through misting cooling is frozen into solid-state iodine in dropping process, due to condensation process expand with heat and contract with cold and capillary uneven, form the hollow spherical particle of 0.5 ~ 4mm diameter, by being arranged at screen cloth 5 elimination condensate liquid at the bottom of tower, solid-state iodine powder collection is in container 7, and the condensing agent having dissolved iodine is collected in container 6.Described screen cloth is flexible material, can effectively prevent falling of iodine particle cracked.The aqueous solution having dissolved a small amount of iodine flows into returnable (6), and the gas containing iodine vapor is recovered in container (6) by pipeline (9), obtains iodine solution.
The production (condensing agent is the ethanol mixing cold air through precooling) of the solid-state hollow iodine particle of embodiment 3. and the tincture of iodine
As shown in Figure 1, granulation tower tower height 3 meters, the volume being positioned at the liquid iodophor container tank (1) of tower top is 15L, be heated to temperature 120 degree in tank, melting solid-state iodine is liquid iodophor, and the nozzle sets (2) below tank arranges altogether 6, each nozzle diameter 1.1mm, the liquid iodophor flow of single-nozzle is 400g/min, and the liquid-drop diameter oozed is 0.4-5mm.
Through the ethanol mixing cold air of precooling as condensing agent, the circulating cooling pipe being arranged in insulating (8) is pumped into by pump (4), and in tower, carry out atomized spray by shower nozzle (3), temperature in tower body and tower chamber is cooled to less than 15 DEG C by described cooling fluid, in this circulatory system, condensing agent is pressurized to 80-100PSIG (pound/square inch), and the speed of spraying in tower is: 80cm
3/ min, the droplet particles of the atomization condensing agent sprayed into is 10-150 μm.Tower wall has the radial jet head sets of 6 covers, the shower nozzle distribution in each direction, equidistant setting, and the air in tower chamber is extracted out by pump by the pipeline (9) being arranged at tower top, and by returnable (6) recovery iodine wherein.
Liquid iodophor drop through misting cooling is frozen into solid-state iodine in dropping process, due to condensation process expand with heat and contract with cold and capillary uneven, form the hollow spherical particle of 0.5 ~ 4mm diameter, by being arranged at screen cloth 5 elimination condensing agent at the bottom of tower, solid-state iodine powder collection is in container 7, and the condensing agent having dissolved iodine is collected in container 6.Described screen cloth is flexible material, can effectively prevent falling of iodine particle cracked.The condensing agent having dissolved a small amount of iodine flows into returnable (6), and the gas containing iodine vapor is recovered in container (6) by pipeline (9), obtains iodine solution.
The production (condensing agent is used alternatingly successively) of the solid-state hollow iodine particle of embodiment 4. and the tincture of iodine
As shown in Figure 1, granulation tower tower height 3 meters, the volume being positioned at the liquid iodophor container tank (1) of tower top is 15L, be heated to temperature 120 degree in tank, melting solid-state iodine is liquid iodophor, and the nozzle sets (2) below tank arranges altogether 6, each nozzle diameter 1.1mm, the liquid iodophor flow of single-nozzle is 400g/min, and the liquid-drop diameter oozed is 0.4-5mm.
Be used alternatingly successively the cold air through precooling, water mixing cold air through precooling, through precooling ethanol mixing cold air as condensing agent, the circulating cooling pipe being arranged in insulating (8) is pumped into by pump (4), and in tower, carry out atomized spray by shower nozzle (3), temperature in tower body and tower chamber is cooled to less than 15 DEG C by described cooling fluid, in this circulatory system, condensing agent is pressurized to 80-100PSIG (pound/square inch), and the speed of spraying in tower is: 80cm
3/ min, when condensing agent is gas-liquid mixture, the droplet particles of the atomization condensing agent sprayed into is 10-150 μm.Tower wall has the radial jet head sets of 6 covers, the shower nozzle distribution in each direction, equidistant setting, and the air in tower chamber is extracted out by pump by the pipeline (9) being arranged at tower top, and by returnable (6) recovery iodine wherein.
Liquid iodophor drop through misting cooling is frozen into solid-state iodine in dropping process, due to condensation process expand with heat and contract with cold and capillary uneven, form the hollow spherical particle of 0.5 ~ 4mm diameter, by being arranged at screen cloth 5 elimination condensing agent at the bottom of tower, solid-state iodine powder collection is in container 7, and the condensing agent having dissolved iodine is collected in container 6.Described screen cloth is flexible material, can effectively prevent falling of iodine particle cracked.The condensing agent having dissolved a small amount of iodine flows into returnable (6), and the gas containing iodine vapor is recovered in container (6) by pipeline (9), obtains iodine solution.
Finally it should be noted that, above embodiment only understands the essence of technical solution of the present invention for those skilled in the art, and is not used in explanation protection scope of the present invention.