CN108654377B - Air-cooled Na 131 Dry distillation device for I preparation - Google Patents
Air-cooled Na 131 Dry distillation device for I preparation Download PDFInfo
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- CN108654377B CN108654377B CN201810786989.1A CN201810786989A CN108654377B CN 108654377 B CN108654377 B CN 108654377B CN 201810786989 A CN201810786989 A CN 201810786989A CN 108654377 B CN108654377 B CN 108654377B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/02—Separation by phase transition
- B01D59/04—Separation by phase transition by distillation
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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- C01D3/12—Iodides
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Abstract
The invention discloses an air cooling typeNa 131 The dry distillation device for preparation comprises a workbench, a heating furnace, a distillation absorber, a feeding table, a material loading table and a slide rail. The feeding table and the slide rail are correspondingly and fixedly arranged on two sides of the horizontal center line of the workbench, the heating furnace is fixedly arranged on the workbench of the extension line of the slide rail, the distillation absorber part is arranged in the cavity of the heating furnace, and the material loading table is arranged on the slide rail and is in sliding connection with the slide rail. The dry distillation device can quickly carry the belt and efficiently collect the pile illumination TeO melted at high temperature 2 Distilling high temperature I-131 vapor, and using compressed air flow to carry heat radiation of heating furnace to shorten cooling time of distillation tube and distillation residue therein, and is more favorable for increasing Na 131 I, production efficiency and safety.
Description
Technical Field
The invention belongs to the technical field of radioisotope preparation, and particularly relates to air-cooled Na 131 I dry distillation device for preparation.
Background
Na for producing radiopharmaceuticals 131 I starting material, mainly by passing through high temperature(about 750 ℃) dry distillation reactor irradiated TeO 2 (tellurium dioxide) and absorbing radioactive I-131 (iodine-131) vapor in carrier gas with dilute alkali solution (generally NaOH solution with concentration less than 0.5 mol/L). The institute of Nuclear physical and chemical research, the national institute of atomic energy science and the national institute of Nuclear physical engineering and chemistry, have been published under Na 131 I, in the production process, a vacuum pump is adopted for pumping, high-temperature carrier gas in a distillation furnace is directly introduced into the bottom of an absorption bottle through a pipeline for bubbling, and iodine-131 steam in the carrier gas is converted into Na by dilute alkali liquor in the bottle 131 And (I) solution. However, because the temperature of the carrier gas is very high and the volume of the added absorption liquid is small (generally not more than 20 mL), the heat brought by the high-temperature carrier gas can easily cause the temperature of the absorption liquid to rise rapidly, so that the mist is generated on the upper part of the absorption bottle and is carried by the tail gas to enter the tail gas treatment device, thereby causing the low absorption efficiency of I-131 vapor in the carrier gas and the evaporation loss of the iodine-131-containing absorption liquid, and also causing higher pressure for the online treatment and standard emission of the tail gas. Reducing the flow rate of the carrier gas is beneficial to reducing the evaporation amount of the absorption liquid caused by heat exchange, but is not beneficial to preventing the loss of iodine-131 steam adsorbed by the tube wall due to temperature loss in the gas guide tube, and is also not beneficial to timely carrying out a large amount of iodine-131 in the distillation tube, so that the production (distillation or heat preservation) time is prolonged, and a greater risk of leakage of the iodine-131 steam from the feed inlet exists, particularly when the tellurium dioxide reaches the melting point. Because of domestic dry distillation reactor irradiation TeO 2 Production of Na 131 The device I adopts a vacuum pump to exhaust to keep the carrier gas flowing directionally and keep a certain negative pressure in the distillation furnace cavity so as to prevent iodine-131 steam from leaking, and in order to obtain a product with higher radioactive concentration, a small amount of dilute alkali liquor is added into an absorption bottle. On the other hand, the existing heap photo TeO 2 The retort furnace has no on-line charging and discharging functions, the temperature of the last batch of production furnace is reduced to be at least below 150 ℃ (the sublimation temperature of elemental iodine is about 185 ℃, and is preferably close to the room temperature), the residue is taken out and then can be recharged for next batch of production, otherwise, radioactive pollution is easily caused, the batch production time is often not less than 6 hours, and about 80% of the time is used for natural cooling of the furnace body. Because the simple substance iodine is easy to evaporate and be adsorbed, the high-temperature distillation can be directly carried outThe cooling of the distillation residue at the pipe opening by taking out the residue or removing the plug of the distillation pipe is prohibited, the evaporation loss of the absorption liquid is increased by increasing the flow rate of the carrier gas after the distillation is completed, and the time for the high-temperature furnace body to continuously supply heat to the distillation pipe and the distillation residue therein is not significantly affected by the flow rate of the carrier gas, and the production time is difficult to be significantly shortened unless the distillation pipe is insulated or the furnace body can rapidly dissipate heat. Based on the reasons, the yield of the iodine-131 in the prior art is often lower than 90%, the batch production time is long, the risk of environmental pollution caused by iodine-131 steam leakage is high, and the continuous efficient and safe production of multiple batches is not facilitated. Although a low-temperature zone is added behind the high-temperature distillation zone, and the temperature of the carrier gas at the outlet of the distillation furnace is reduced to reduce the heating effect on the absorption liquid, in order to ensure that the iodine-131 in the carrier gas is not adsorbed by the inner wall of the carrying pipeline before being absorbed by alkali liquor to cause loss, the temperature of the carrier gas is generally controlled to be about 300 ℃, and the heating and evaporation effect on the absorption liquid is still obvious. In addition, the distillation tube and the absorber in the prior art are split, and are connected by adopting a plastic tube or a rubber tube, the strong gamma radiation and high temperature of the radioactive iodine-131 in the carrier gas have great influence on the service life of the connecting tube, and the radioactive iodine-131 steam leakage accident is easily caused by aging cracking in practice, so that the service life is shortened, the risk that production equipment maintenance personnel receive more radiation doses is increased, and the safe production is not facilitated. The distillation tube and absorber integrated dry distillation absorber which has the functions of efficiently cooling alkali absorption liquid and accelerating the cooling of the distillation tube and is suitable for hot rooms or shielding production environment conditions in a working box and has a compact and small structure is adopted, and the integrated dry distillation absorber is a main way for solving the defects of the prior art.
Disclosure of Invention
To increase Na 131 The production efficiency of the solution I is improved, the safety risk is reduced, and the invention provides the air-cooled Na 131 I dry distillation device for preparation.
The dry distillation device adopts a mode of compressed air flow heat insulation and absorption liquid cooling, and has an integrated structure of the distillation pipe and the absorber, so that high-temperature radioactive iodine-131 steam distilled from a tellurium dioxide raw material activated by a reactor can be quickly carried and efficiently captured, the yield of iodine-131 is up to about 98%, the batch production time is shortened to about 2 hours, the service life of a production device is prolonged, and the safety risk of production is effectively reduced.
The technical scheme for realizing the invention is as follows:
the air-cooled Na of the invention 131 The dry distillation device for preparation is characterized by comprising a workbench, a heating furnace, a distillation absorber, a feeding table, a material loading table and a slide rail; the dry distillation device is connected in a manner that the feeding table and the slide rails are correspondingly and fixedly arranged on two sides of the horizontal center line of the workbench, the heating furnace is fixedly arranged on the workbench of the extension line of the slide rails, the distillation absorber part is arranged in the cavity of the heating furnace, and the material loading table is arranged on the slide rails and is in sliding connection with the slide rails.
The distillation absorber comprises a horizontally arranged distillation sleeve and a vertically arranged absorption tank, and the distillation sleeve is fixedly connected with the absorption tank; the distillation sleeve comprises a sleeve and a distillation pipe, and the absorption tank comprises an alkali liquor tank, a water bath tank and a coil pipe; wherein, one end of the distillation tube is a bell mouth; the device comprises a distillation tube, a sleeve, a plug, an alkali liquor tank, an air inlet pipe, an air outlet pipe, a connecting block and a plug, wherein the sleeve is sleeved outside the distillation tube, one end of the sleeve is fixedly connected with the bell mouth end of the distillation tube in a sealing manner, the plug is arranged in the bell mouth in a matching manner, the other end of the sleeve is vertically and fixedly connected with the upper side wall of the alkali liquor tank, the two ends of the sleeve are respectively provided with the air inlet pipe and the air outlet pipe which are communicated, the pipe wall right below the sleeve is provided with a small hole, and the distillation tube is also fixedly connected with the inner wall of the sleeve through the connecting block; the water bath tank is arranged in the alkali liquor tank, the coil pipe is arranged in the water bath tank, the upper end of the coil pipe obliquely and upwards sequentially penetrates through the water bath tank, the alkali liquor tank and the sleeve pipe, penetrates through the distillation pipe and is respectively fixedly connected with the water bath tank, the alkali liquor tank and the distillation pipe in a sealing manner, the lower end of the coil pipe vertically penetrates through the center of the bottom of the water bath tank and is fixedly connected with the water bath tank in a sealing manner, and an included angle is formed between a pipeline at the upper end of the coil pipe and a horizontal line; the alkali liquor tank is fixedly connected with the water bath tank through a connecting block, and a steel wire mesh which is in contact with the alkali liquor tank and the water bath tank is arranged between the side walls of the alkali liquor tank and the water bath tank; the lateral direction of the top of the alkali liquor tank and the center of the bottom of the alkali liquor tank are respectively and fixedly provided with a communicated three-way valve and a communicated two-way valve, and an annular baffle is fixedly arranged on the inner side wall of the alkali liquor tank between the three-way valve and the top of the water bath tank; the water bath tank is provided with an L-shaped feed pipe, a water inlet pipe and an L-shaped drain pipe, the upper end of the feed pipe horizontally penetrates through the side wall of the alkali liquor tank and is fixedly connected with the alkali liquor tank in a sealing manner, the lower end of the feed pipe vertically penetrates through the water bath tank from top to bottom and is fixedly connected with the water bath tank in a sealing manner, and the lower ends of the water inlet pipe and the drain pipe horizontally penetrate through the middle lower part of the water bath tank and the lower part of the alkali liquor tank side by side and are fixedly connected with the water bath tank and the alkali liquor tank in a sealing manner respectively; the upper port of the water drain pipe is arranged in the water bath tank, and a gap is formed between the upper port of the water drain pipe and the top of the water bath tank; the bottom of the heating furnace is vertically provided with a thermocouple, and the upper end of the thermocouple penetrates through a small hole in the wall of the sleeve to be in contact with the wall of the distillation tube.
The charging platform comprises a support, a bottom plate, a sliding plate and a sliding plate groove, the sliding plate is fixedly connected with the support, the sliding plate groove is fixedly connected with the bottom plate, a hopper frame and a bracket are respectively and fixedly arranged on the support and the sliding plate which are positioned on one side of the material loading platform, and a charging hopper which is in sliding connection is arranged on the hopper frame; the material loading platform comprises a sliding seat, a gas loading pipe, a trailer and an I-shaped clamp, wherein the trailer is arranged in the distillation pipe; the gas carrying pipe is fixed in the center of the top of the sliding seat through an I-shaped card, one end of the gas carrying pipe is provided with a gas valve, the other end of the gas carrying pipe sequentially penetrates through the center of the plug and the side wall of the trailer, the gas carrying pipe is connected with the plug through a silicon rubber sleeve, the gas carrying pipe is fixedly connected with the trailer, and a crucible is placed on the trailer.
The included angle between the pipeline at the upper end of the coil pipe and the horizontal line ranges from 5 degrees to 10 degrees.
The clearance between the sleeve and the side wall of the distillation tube is 10 mm-20 mm.
The gas carrying pipe is arranged in parallel with the slide rail; the horizontal axes of the gas carrying pipe, the trailer and the distillation pipe are arranged on the same vertical surface; the horizontal axes of the bucket rack and the bracket are arranged on the same vertical surface in parallel and are arranged in parallel with the sliding rail; the horizontal axes of the sleeve and the distillation tube are overlapped, and the horizontal axis of the sleeve and the longitudinal axis of the alkali liquor tank are crossed; the longitudinal axis lines of the lye tank, the water bath tank and the coil pipe are arranged in a superposition way.
The heating furnace and the thermocouple are externally connected with a controller; one branch pipe of the three-way valve is sequentially externally connected with a tail gas treatment device and a vacuum pump, and the other branch pipe is externally connected with a duplex ball; the water inlet pipe and the water discharge pipe are externally connected with a circulating cooling water device; the charging pipe is externally connected with a peristaltic pump and a storage bottle in sequence; the air inlet pipe is externally connected with a compressed air tank.
The distillation absorber is made of quartz glass; the steel wire mesh is made of stainless steel; the gas carrying pipe and the trailer are made of tungsten alloy.
The invention relates to air-cooled Na 131 I the brief working principle of the dry distillation device for preparation is as follows: under the pumping of a vacuum pump, a reactor TeO arranged in a distillation tube 2 High-temperature iodine-131 steam which is heated to about 750 ℃ and melted to overflow is carried by carrier gas from a distillation tube, is sent to the bottom of an alkali liquor tank through a coil pipe arranged in a water bath tank for bubbling, the carrier gas is gradually cooled in the process of flowing in the coil pipe, and is rapidly carried away by cold water in the water bath tank through heat exchange of the pipe wall when the carrier gas is contacted with the alkali liquor to generate heat exchange and the heat release of I-131 and alkali disproportionation reaction, so that the temperature of absorption liquid is kept at normal temperature or the temperature rise amplitude is smaller in the whole production process; after distillation is finished, a heating power supply is closed, compressed air flow is immediately introduced to rapidly bring away a furnace body to perform rapid temperature reduction on the distillation pipe and the heat supply of distillation residues in the distillation pipe until the temperature reaches a specified value, and then iodine-131 condensed on the inner wall of the coil pipe is soaked and eluted by back pressure absorption liquid, so that the efficient absorption of iodine-131 steam in high-temperature carrier gas and Na absorption of the iodine-131 steam in the high-temperature carrier gas are realized 131 The solution I is produced efficiently and safely.
The dry distillation device adopts the sleeve type distillation tube and the absorption tank with a two-stage cooling sandwich structure, firstly, high-temperature carrier gas is greatly cooled in the absorption tank, then the carrier gas is transferred to the waste heat of absorption liquid and the heat of disproportionation reaction are taken away to the maximum extent, under the condition that cooling water keeps the pressure of common tap water, the high-temperature carrier gas at a higher flow speed (or a larger flow) can be ensured to be unobvious in heating the absorption liquid with a small volume, and the iodine-131 loss caused by the generation of fog is prevented or reduced to the maximum extent; the adoption set up soak intensive wire net in the absorption liquid between lye tank and water bath jar, cut apart the great year bubble and increase with absorption liquid contact area and increase contact time (increased bubble migration distance), effectively guaranteed the absorption efficiency of I-131 vapour in the carrier gas of higher velocity of flow. After distillation is finished, the heating power supply is closed, compressed air is introduced into the sleeve immediately, the air flowing fast takes away heat radiated by the furnace body fast, the distillation tube and distillation residues in the distillation tube play a role in heat insulation and temperature reduction, and the cooling time of the distillation residues is greatly shortened. The dry distillation device has compact and small structure and good safety and reliability.
Drawings
FIG. 1 shows an air-cooled Na composition of the present invention 131 I, a general structural schematic diagram of a dry distillation device for preparation;
FIG. 2 shows an air-cooled Na according to the present invention 131 I, a schematic plan view structure of the dry distillation device for preparation;
FIG. 3 is a schematic diagram of the construction of a distillation absorber in the present invention;
FIG. 4 isbase:Sub>A sectional view A-A of FIG. 3;
FIG. 5 is a sectional view taken along line B-B of FIG. 3;
FIG. 6 is a schematic view of the structure of the loading table in the present invention;
in the figure, 1, a workbench 2, a heating furnace 3, a slide rail 4, a sleeve 5, a distillation pipe 6, an alkali liquor tank 7, a water bath tank 8, a coil pipe 9, a plug 10, an air inlet pipe 11, an air outlet pipe 12, a steel wire mesh 13, a three-way valve 14, a two-way valve 15, a baffle 16, a feeding pipe 17, an water inlet pipe 18, a water outlet pipe 19, a support 20, a bottom plate 21, a slide plate 22, a slide plate groove 23, a hopper frame 24, a bracket 25, a feeding hopper 26, a slide seat 27, a carrier air pipe 28, a trailer 29, an I-shaped card 30, an air valve 31, a crucible 32 and a thermocouple are arranged.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
Example 1
FIG. 1 shows an air-cooled Na composition of the present invention 131 I general structural schematic diagram of dry distillation device for preparation, FIG. 2 is a gas-cooled Na of the present invention 131 I schematic structural view in plan view of a dry distillation apparatus for production, FIG. 3 is a schematic structural view of a distillation absorber in the present invention, and FIG. 4 is a schematic structural view of FIG. 3Fig. 5 isbase:Sub>A sectional view taken along line B-B of fig. 3, and fig. 6 isbase:Sub>A schematic structural view of the feed table of the present invention. In FIGS. 1 to 6, an air-cooled Na according to the present invention is shown 131 The dry distillation device for preparation comprises a workbench 1, a heating furnace 2, a distillation absorber, a feeding table, a material loading table and a slide rail 3. The dry distillation device is connected in a manner that the feeding table and the slide rails 3 are correspondingly and fixedly arranged on two sides of the horizontal center line of the workbench 1, the heating furnace 2 is fixedly arranged on the workbench 1 of the extension line of the slide rails 3, the distillation absorber part is arranged in the cavity of the heating furnace 2, and the material carrying table is arranged on the slide rails 3 and is in sliding connection with the slide rails 3. The distillation absorber comprises a horizontally arranged distillation sleeve and a vertically arranged absorption tank, and the distillation sleeve is fixedly connected with the absorption tank. The distillation sleeve comprises a sleeve 4 and a distillation pipe 5, and the absorption tank comprises an alkali liquor tank 6, a water bath tank 7 and a coil pipe 8; wherein, one end of the distillation tube 5 is a bell mouth. The distillation tube 5 is sleeved with the sleeve 4, one end of the sleeve 4 is fixedly connected with the bell-mouth end of the distillation tube 5 in a sealing mode, a plug 9 is arranged in the bell-mouth in a matching mode, the other end of the sleeve 4 is fixedly connected with the upper side wall of the alkaline liquor tank 6 in a vertical mode, an air inlet pipe 10 and an air outlet pipe 11 which are communicated with each other are arranged at two ends of the sleeve 4 respectively, a small hole is formed in the pipe wall under the sleeve 4, and the distillation tube 5 is fixedly connected with the inner wall of the sleeve 4 through a connecting block. Water bath tank 7 set up in lye tank 6, coil pipe 8 sets up in water bath tank 7, upward pass water bath tank 7, lye tank 6, sleeve pipe 4 in proper order in the upper end of coil pipe 8, penetrate distillation tube 5 and with water bath tank 7, lye tank 6, distillation tube 5 leakproofness fixed connection respectively, the lower extreme of coil pipe 8 vertically pass out water bath tank 7 bottom central authorities and with water bath tank 7 leakproofness fixed connection, there is an contained angle between 8 upper end pipelines of coil pipe and the water flat line. The lye tank 6 is fixedly connected with the water bath tank 7 through a connecting block, and a steel wire mesh 12 which is in contact with the lye tank 6 and the water bath tank 7 is arranged between the side walls of the lye tank 6 and the water bath tank 7. The lateral direction of the top of the lye tank 6 and the center of the bottom are respectively and fixedly provided with a three-way valve 13 and a two-way valve 14 which are communicated, and an annular baffle 15 is fixedly arranged on the inner side wall of the lye tank 6 between the three-way valve 13 and the top of the water bath tank 7. The water bath tank 7 is provided with an L-shaped feed pipe 16 and a water inlet pipe17. The drain pipe 18 of L type, 16 upper ends levels of filling tube wear out the lateral wall of lye tank 6 and with lye tank 6 leakproofness fixed connection, the filling tube 16 lower extreme from last to down run through water bath tank 7 and with water bath tank 7 leakproofness fixed connection perpendicularly, inlet tube 17, drain pipe 18 lower extreme side by side level run through water bath tank 7, lye tank 6 middle and lower part and respectively with water bath tank 7, lye tank 6 leakproofness fixed connection. The upper end opening of the drain pipe 18 is arranged in the water bath tank 7 and has a gap with the top of the water bath tank 7. A thermocouple 32 is vertically arranged at the bottom of the heating furnace 2, and the upper end of the thermocouple 32 passes through a small hole on the pipe wall of the sleeve 4 to be contacted with the wall of the distillation pipe 5. The charging platform comprises a support 19, a bottom plate 20, a sliding plate 21 and a sliding plate groove 22, wherein the sliding plate 21 is fixedly connected with the support 19, the sliding plate groove 22 is fixedly connected with the bottom plate 20, a hopper frame 23 and a bracket 24 are respectively fixedly arranged on the support 19 and the sliding plate 21 which are positioned on one side of the loading platform, and a charging hopper 25 which is in sliding connection is arranged on the hopper frame 23. The material loading platform comprises a sliding seat 26, a gas loading pipe 27, a trailer 28 and an I-shaped clamp 29, wherein the trailer 28 is arranged in the distillation pipe 5. The gas carrying pipe 27 is fixed at the center of the top of the sliding seat 26 through an I-shaped clamp 29, one end of the gas carrying pipe 27 is provided with a gas valve 30, the other end of the gas carrying pipe 27 sequentially penetrates through the center of the plug 9 and the side wall of the trailer 28, the gas carrying pipe 27 is connected with the plug 9 through a silicone rubber sleeve, the gas carrying pipe 27 is fixedly connected with the trailer 28, and a crucible 31 is arranged on the trailer. As shown in fig. 1 to 6.
The included angle between the pipeline at the upper end of the coil pipe 8 and the horizontal line ranges from 5 degrees to 10 degrees. The clearance between the sleeve 4 and the side wall of the distillation tube 5 is 10mm to 20mm. The gas carrying pipe 27 is arranged in parallel with the slide rail 3. The horizontal axes of the gas carrying pipe 27, the trailer 28 and the distillation pipe 5 are arranged on the same vertical surface. The horizontal axes of the bucket rack 23 and the bracket 24 are arranged on the same vertical surface in parallel and are arranged in parallel with the slide rail 3. The horizontal axes of the sleeve 4 and the distillation tube 5 are overlapped, and the horizontal axis of the sleeve 4 is crossed with the longitudinal axis of the lye tank 6. The longitudinal axis lines of the alkali liquor tank 6, the water bath tank 7 and the coil pipe 8 are arranged in a superposition way. The heating furnace 2 and the thermocouple 32 are externally connected with a controller. One branch of the three-way valve 13 is sequentially connected with the tail gas treatment device and the vacuum pump in an external mode, and the other branch is connected with the duplex ball in an external mode. The water inlet pipe 17 and the water outlet pipe 18 are externally connected with a circulating cooling water device. The feed pipe 16 is externally connected with a peristaltic pump and a storage bottle in sequence. The air inlet pipe 10 is externally connected with a compressed air tank. The distillation absorber is made of quartz glass. The steel wire mesh 12 is made of stainless steel. The carrier gas pipe 27 and the trailer 28 are made of tungsten alloy. As shown in fig. 1 to 6.
In this embodiment, the heating furnace 2 is composed of an upper half furnace body and a lower half furnace body, both ends of the sleeve 4 are respectively fixed on the lower half furnace body of the heating furnace 2, and the pile irradiation TeO placed in the distillation tube 5 is heated to about 750 DEG C 2 The melted and distilled iodine-131 is contained in the tube and carried into the absorption tank by the carrier gas. The air inlet pipe 10 on the sleeve 4 is externally connected with a compressed air tank, high-speed compressed air is injected from the air inlet pipe 10 and discharged from the exhaust pipe 11 after distillation is finished, and the radiant heat of the high-temperature furnace body to the distillation pipe and the heat of the distillation pipe can be rapidly taken away, so that the temperature of the distillation pipe 5 and the built-in distillation residues thereof is accelerated to be reduced. One branch pipe of the three-way valve 13 on the alkali liquor tank 6 is externally connected with a duplex ball for pressurizing absorption liquid in the alkali liquor tank 6 to enable the absorption liquid to be soaked, eluted and condensed at iodine-131 on the inner wall of the coil pipe 8 from bottom to top, so that the reduction of the absorption loss of the iodine-131 is facilitated, the other branch pipe of the three-way valve 13 is externally connected with a tail gas treatment device and a vacuum pump in sequence, and carrier gas is driven by the vacuum pump to directionally flow through the coil pipe 8, the alkali liquor tank 6 and the tail gas treatment device so as to treat high-temperature carrier gas. The distance between the bottom and the side of the water bath tank 7 and the lye tank 6 is smaller, which is beneficial to reducing the filling amount of the absorption liquid to realize high-concentration Na 131 And I, production. The upper end pipeline of coil pipe 8 set up with certain angle slant, be favorable to preventing that the pressurization from driving the absorption liquid and soaking from supreme liquid down and elute the coil pipe entering distillation sleeve pipe that the absorption liquid overflows when the condensation is at 8 inner walls of coil pipe and causes the loss. The feed tube 8 is externally connected with a peristaltic pump, and the peristaltic pump is used for quantitatively adding the absorption liquid into the lye tank 6. The water inlet pipe 17 and the water outlet pipe 18 are externally connected with a circulating cooling water device to ensure that cooling water in the water bath tank 7 rapidly flows from bottom to top to take away heat transfer of high-temperature carrier gas to the absorption liquid. The baffle 7 is arranged to prevent the absorption liquid from being vigorously bubbled and gushes into the branch pipe of the three-way valve 5 to be lost due to the excessive gas flow. Of thermocouples 32The upper end of the distillation tube is contacted with the wall of the distillation tube 5 after passing through a small hole on the tube wall of the sleeve 4, which is beneficial to accurately measuring the temperature of the distillation tube wall below the trailer 28 so as to judge the temperature of the distillation residues in the crucible. The mounting position of the charging platform on the workbench 1 should ensure that the horizontal axis of the bracket 24 is positioned on the same vertical plane with the horizontal axes of the carrier gas pipe 27 and the trailer 28 at the maximum stroke of the sliding plate 21 moving towards the direction of the charging platform. The carrier 27 should have sufficient strength to ensure that the trailer 28 does not deform or deforms very little during the loading, unloading and horizontal movement of the crucible 31, and the carrier 27 should be mounted at a height that ensures that the trailer 28 can slide easily on the lower wall of the retort and can be safely moved into and out of the retort. The setting height of the bracket 24 is matched with that of the trailer 28, so that the crucible 31 is taken and placed and the gas carrier pipe 27 is not seriously deformed due to external force when charging, and the safe use is not influenced. The slide 26 slides on the slide rail 3 with a mechanical hand of a hot chamber or work box arrangement.
In this embodiment, an angle between the upper end of the coil pipe 8 and the horizontal line is 5 ° in an oblique direction; the gap between the sleeve 4 and the side wall of the distillation tube 5 is 10mm; the slide rail be two parallel arrangement, slide rail 3 is one of them.
The working process of the invention is as follows, a manipulator configured by a hot chamber or a work box pushes a sliding seat 26 back to the heating furnace 2, a trailer 28 is dragged to the pipe orifice of the distillation tube 5, then a bracket 24 is clamped and pulled out to the direction of a material loading platform to a certain position, then the sliding seat 26 is continuously pushed to enable the trailer 28 to be placed on the bracket 24, and then a crucible 31 is placed in the trailer 28; the sliding hopper 25 is adjusted to cut the pile irradiation TeO in the target cylinder 2 After pouring into the crucible 31 through the charging hopper 25, pushing the sliding seat 26 towards the heating furnace 2 to feed the trailer 28 into the pipe orifice of the distillation pipe 5, then pushing the bracket 24 to reset, then continuing to push the sliding seat 26 to feed the trailer 28 into the distillation pipe 5 and tightly plugging the plug 9; starting a peristaltic pump to inject a certain amount of absorption liquid into the lye tank 6 through a feeding pipe 16, then starting a circulating cooling water device to inject cooling water from the bottom of the water bath tank 7 through a water inlet pipe 17 and discharge the cooling water from the top of the water bath tank 7 through a water discharge pipe 18, and respectively cooling the absorption liquid and the coil pipe 8; the air valve 30, the three-way valve 13, the vacuum pump and the external controller of the heating furnace 2 on the carrier gas pipe 27 are opened in sequence, and the air valve 30 and the three-way valve 13 are connectedAdjusting the flow rate of the carrier gas to control the irradiation TeO placed in the distillation tube 5 2 Heating to about 750 ℃ and keeping the temperature for about 40 minutes, wherein distilled iodine-131 steam is sent to the bottom of the lye tank 6 to bubble by the carrier gas through the coil pipe 8 arranged in the water bath tank 7, the carrier gas is gradually cooled in the process of flowing from top to bottom in the coil pipe 8, the bubbles contact the absorption liquid in the lye tank 6 and penetrate through the steel wire mesh 12 soaked in the absorption liquid from the bottom of the lye tank 6 upwards, and then the heat exchanged to the absorption liquid in the process of discharging from the three-way valve 13 and the reaction heat of I-131 and alkali are rapidly taken away by cold water in the water bath tank 7 through heat exchange, so that the temperature of the absorption liquid is kept at normal temperature or the temperature rise amplitude is small in the whole production process. After the distillation is finished and the heating power supply is turned off, normal-temperature compressed air is introduced from the air inlet pipe 14, and the heat radiation of the high-temperature furnace body to the distillation pipe 5 and the heat of the distillation pipe 5 are quickly taken away, so that the distillation pipe 5 and the distillation residues in the distillation pipe are quickly cooled; detecting that the temperature of the distillation tube 5 is lower than 150 ℃ through a thermocouple 32 (preferably close to room temperature), closing a three-way valve 13 to be communicated with a tail gas treatment device and communicated with a branch tube connected with a bigeminy ball, soaking and washing iodine-131 condensed on the inner wall of the coil tube 8 by using bigeminy ball back pressure absorption liquid from bottom to top, then removing the pressure of the bigeminy ball, enabling soaking eluent to flow back to the lye tank 6 to be mixed with the residual absorption liquid at the bottom, and then opening a two-way valve 14 to place the absorption liquid in the lye tank 6 into a special glass bottle and transfer the absorption liquid to a specified place; the carriage 26 is pushed in the manner described above to pull the trailer 28 onto the carriage 24, the distillation residue crucible 31 is removed and disposed of properly, and the trailer 28 is returned to the distillation tube 5. So far, the stacking illumination TeO is realized 2 Production of Na by dry distillation 131 The solution I is produced efficiently and safely.
Example 2
The structure of this embodiment is the same as that of embodiment 1, except that the angle between the upper end of the coil 8 and the horizontal line is 10 ° and the gap between the sleeve 4 and the side wall of the distillation tube 5 is 20mm.
Claims (6)
1. Air-cooled Na 131 I dry distillation device for preparation, which is characterized in that: the dry distillation device comprises a workbench (1), a heating furnace (2), a distillation absorber and a feeding materialA platform, a material loading platform and a slide rail (3); the dry distillation device is connected in a manner that the feeding table and the slide rail (3) are correspondingly and fixedly arranged at two sides of the horizontal center line of the workbench (1), the heating furnace (2) is fixedly arranged on the workbench (1) of the extension line of the slide rail (3), the distillation absorber part is arranged in the cavity of the heating furnace (2), and the material loading table is arranged on the slide rail (3) and is in sliding connection with the slide rail (3);
the distillation absorber comprises a horizontally arranged distillation sleeve and a vertically arranged absorption tank, and the distillation sleeve is fixedly connected with the absorption tank; the distillation sleeve comprises a sleeve (4) and a distillation pipe (5), and the absorption tank comprises an alkali liquor tank (6), a water bath tank (7) and a coil pipe (8); wherein, one end of the distillation tube (5) is a bell mouth; the distillation tube is characterized in that the sleeve (4) is sleeved outside the distillation tube (5), one end of the sleeve (4) is fixedly connected with the bell mouth end of the distillation tube (5) in a sealing mode, a plug (9) is arranged in the bell mouth in a matching mode, the other end of the sleeve (4) is vertically and fixedly connected with the upper side wall of the alkali liquor tank (6), an air inlet pipe (10) and an air outlet pipe (11) which are communicated with each other are arranged at two ends of the sleeve (4) respectively, a small hole is formed in the wall of the tube right below the sleeve (4), and the distillation tube (5) is further fixedly connected with the inner wall of the sleeve (4) through a connecting block; the water bath tank (7) is arranged in the alkali liquor tank (6), the coil pipe (8) is arranged in the water bath tank (7), the upper end of the coil pipe (8) obliquely and upwards penetrates through the water bath tank (7), the alkali liquor tank (6) and the sleeve pipe (4) in sequence, penetrates through the distillation pipe (5) and is fixedly connected with the water bath tank (7), the alkali liquor tank (6) and the distillation pipe (5) in a sealing manner respectively, the lower end of the coil pipe (8) vertically penetrates out of the center of the bottom of the water bath tank (7) and is fixedly connected with the water bath tank (7) in a sealing manner, and an included angle is formed between a pipeline at the upper end of the coil pipe (8) and a horizontal line; the alkali liquor tank (6) is fixedly connected with the water bath tank (7) through a connecting block, and a steel wire mesh (12) which is in contact with the alkali liquor tank (6) and the water bath tank (7) is arranged between the side walls of the alkali liquor tank (6) and the water bath tank (7); a three-way valve (13) and a two-way valve (14) which are communicated are respectively and fixedly arranged on the lateral side of the top and the center of the bottom of the lye tank (6), and an annular baffle plate (15) is fixedly arranged on the inner side wall of the lye tank (6) between the three-way valve (13) and the top of the water bath tank (7); the water bath tank (7) is provided with an L-shaped feed pipe (16), a water inlet pipe (17) and an L-shaped drain pipe (18), the upper end of the feed pipe (16) horizontally penetrates through the side wall of the alkali liquor tank (6) and is fixedly connected with the alkali liquor tank (6) in a sealing manner, the lower end of the feed pipe (16) vertically penetrates through the water bath tank (7) from top to bottom and is fixedly connected with the water bath tank (7) in a sealing manner, and the lower ends of the water inlet pipe (17) and the drain pipe (18) horizontally penetrate through the middle lower part of the water bath tank (7) and the lower part of the alkali liquor tank (6) side by side and are fixedly connected with the water bath tank (7) and the alkali liquor tank (6) in a sealing manner respectively; the upper port of the drain pipe (18) is arranged in the water bath tank (7) and a gap is formed between the upper port and the top of the water bath tank (7); a thermocouple (32) is vertically arranged at the bottom of the heating furnace (2), and the upper end of the thermocouple (32) penetrates through a small hole in the pipe wall of the sleeve (4) to be in contact with the wall of the distillation pipe (5);
the feeding table comprises a support (19), a bottom plate (20), a sliding plate (21) and a sliding plate groove (22), the sliding plate (21) is fixedly connected with the support (19), the sliding plate groove (22) is fixedly connected with the bottom plate (20), a hopper frame (23) and a bracket (24) are fixedly arranged on the support (19) and the sliding plate (21) which are positioned on one side of the loading table respectively, and a feeding hopper (25) which is connected in a sliding manner is arranged on the hopper frame (23); the material loading platform comprises a sliding seat (26), a gas loading pipe (27), a trailer (28) and an I-shaped clamp (29), wherein the trailer (28) is arranged in the distillation pipe (5); the air carrying pipe (27) is fixed at the center of the top of the sliding seat (26) through an I-shaped clamp (29), an air valve (30) is arranged at one end of the air carrying pipe (27), the other end of the air carrying pipe (27) sequentially penetrates through the center of the plug (9) and the side wall of the trailer (28), the air carrying pipe (27) is connected with the plug (9) through a silicon rubber sleeve, the air carrying pipe (27) is fixedly connected with the trailer (28), and a crucible (31) is placed on the trailer.
2. An air-cooled Na according to claim 1 131 I dry distillation device is used in preparation, its characterized in that: the included angle between the pipeline at the upper end of the coil pipe (8) and the horizontal line ranges from 5 degrees to 10 degrees.
3. An air-cooled Na according to claim 1 131 I dry distillation device for preparation, which is characterized in that: the gap between the sleeve (4) and the side wall of the distillation tube (5) is between 10mm and 20mm.
4. An air-cooled Na according to claim 1 131 I dry distillation device for preparation, which is characterized in that: the gas carrying pipe (27) is arranged in parallel with the sliding rail (3); the horizontal axes of the gas carrying pipe (27), the trailer (28) and the distillation pipe (5) are arranged on the same vertical surface; the horizontal axes of the bucket rack (23) and the bracket (24) are arranged on the same vertical surface in parallel and are arranged in parallel with the sliding rail (3); the horizontal axes of the sleeve (4) and the distillation tube (5) are superposed, and the horizontal axis of the sleeve (4) is crossed with the longitudinal axis of the lye tank (6); the vertical axis of the lye tank (6), the water bath tank (7) and the coil pipe (8) is overlapped.
5. An air-cooled Na according to claim 1 131 I dry distillation device for preparation, which is characterized in that: the heating furnace (2) and the thermocouple (32) are externally connected with a controller; one branch pipe of the three-way valve (13) is sequentially and externally connected with a tail gas treatment device and a vacuum pump, and the other branch pipe is externally connected with a duplex ball; the water inlet pipe (17) and the water outlet pipe (18) are externally connected with a circulating cooling water device; the feed pipe (16) is sequentially externally connected with a peristaltic pump and a storage bottle; the air inlet pipe (10) is externally connected with a compressed air tank.
6. The air-cooled Na of claim 1 131 I dry distillation device for preparation, which is characterized in that: the distillation absorber is made of quartz glass; the steel wire mesh (12) is made of stainless steel; the gas carrying pipe (27) and the trailer (28) are made of tungsten alloy.
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CN115957527A (en) * | 2022-12-31 | 2023-04-14 | 中国工程物理研究院核物理与化学研究所 | High-efficiency production of Na 131 I device of solution |
CN116036837A (en) * | 2022-12-31 | 2023-05-02 | 中国工程物理研究院核物理与化学研究所 | High-temperature gas auxiliary heating type iodine-131 steam treatment device |
CN115945035A (en) * | 2022-12-31 | 2023-04-11 | 中国工程物理研究院核物理与化学研究所 | I-131 dry distillation absorber driven by compressed air |
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MX9504452A (en) * | 1995-10-20 | 1997-04-30 | Inst Nac De Investigaciones Nu | Equipment for 131i dry distillation from teo2. |
CN2304653Y (en) * | 1998-02-25 | 1999-01-20 | 中国原子能科学研究院 | Dry distiller for producing radioactive iodine |
CN103771341A (en) * | 2013-12-23 | 2014-05-07 | 米度(南京)生物技术有限公司 | Method for preparing radioactive <124>I ions |
CN104524957A (en) * | 2015-01-26 | 2015-04-22 | 中国工程物理研究院核物理与化学研究所 | Radioiodine-131 vapor trapping device |
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MX9504452A (en) * | 1995-10-20 | 1997-04-30 | Inst Nac De Investigaciones Nu | Equipment for 131i dry distillation from teo2. |
CN2304653Y (en) * | 1998-02-25 | 1999-01-20 | 中国原子能科学研究院 | Dry distiller for producing radioactive iodine |
CN103771341A (en) * | 2013-12-23 | 2014-05-07 | 米度(南京)生物技术有限公司 | Method for preparing radioactive <124>I ions |
CN104524957A (en) * | 2015-01-26 | 2015-04-22 | 中国工程物理研究院核物理与化学研究所 | Radioiodine-131 vapor trapping device |
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