CN216062117U - Automatic separation system for radioactive nuclide - Google Patents
Automatic separation system for radioactive nuclide Download PDFInfo
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- CN216062117U CN216062117U CN202121429055.6U CN202121429055U CN216062117U CN 216062117 U CN216062117 U CN 216062117U CN 202121429055 U CN202121429055 U CN 202121429055U CN 216062117 U CN216062117 U CN 216062117U
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Abstract
The present invention provides an automatic radionuclide separation system, comprising: a first evaporator; a second evaporator; a reagent fill assembly; the chromatographic column comprises a liquid storage part and a separation part which are sequentially arranged from top to bottom, wherein the liquid storage part is communicated with the separation part; the multi-way valve assembly is respectively communicated with the first evaporator, the second evaporator, the reagent filling assembly, the liquid storage part and the separation part through pipelines, the multi-way valve assembly further comprises an air inlet and a feed inlet, the air inlet is communicated with external air, and the feed inlet is suitable for extracting dissolved liquid; and the vacuum pump is respectively communicated with the first evaporator, the second evaporator and the liquid storage part through pipelines. The vacuum pump and the reagent filling assembly can avoid reaction solution from adhering to the pipeline in the process of sequentially filling the reaction solution into the first evaporator, the second evaporator and the chromatographic column, so that the utilization efficiency of the reaction solution is improved, the reaction solution is prevented from being mixed up, and the production rate of the radioactive nuclide is improved.
Description
Technical Field
The utility model relates to the technical field of radionuclide production, in particular to an automatic radionuclide separation system.
Background
Radionuclides are produced by causing charged particles to cause a nuclear reaction by an accelerator, and the produced radionuclides are a major source of nuclides for radiopharmaceuticals. The radionuclides produced by the accelerator are typically neutron-deficient nuclides, mostly with electron capture or emission of beta+The decay of the ionic form is of particular interest in the diagnosis and treatment of medical problems such as cancer. Classical radionuclides include:18F、57Co、64Cu、67Ga、89Zr、103Pd、111In、123I、201tl, and the like. The radionuclide produced by the accelerator and the target element are not isotopes, and the radionuclide with high specific activity and even without carrier can be prepared by a chemical separation method.
In the related art, the specific production process of the radionuclide includes the steps of solid target preparation, accelerator bombardment, target dissolution, separation and purification, and the like. The steps of separating and purifying the radioactive nuclide by using an anion exchange method are the steps with the most complicated operation and the highest artificial participation degree in all the flows, the dissolved feed liquid contains various impurities, a series of quality control problems can be caused, and the higher artificial participation degree can also cause more safety problems. When part of the reaction solution circulates in the pipeline, the reaction solution is adhered to the pipeline, which causes waste of the reaction solution and reduces the productivity of the radionuclide.
SUMMERY OF THE UTILITY MODEL
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the utility model provides the automatic radionuclide separation system, which separates the radionuclides by an anion exchange method, is automatically controlled in the whole process, is beneficial to improving the separation efficiency and quality of the radionuclides, can reduce the manual participation and ensures the safety of operators. In the transfer process of the reaction solution, the gas is continuously introduced into the pipeline, so that the reaction solution is prevented from being adhered to the pipeline, the utilization efficiency of the reaction solution is increased, and the production rate of the radionuclide is improved.
Meanwhile, the utility model also provides an automatic separation method of the radioactive nuclide.
According to a first aspect of the present invention, there is provided an automatic radionuclide separation system, including:
a first evaporator;
a second evaporator;
a reagent fill assembly;
the chromatographic column comprises a liquid storage part and a separation part which are sequentially arranged from top to bottom, wherein the liquid storage part is communicated with the separation part;
the multi-way valve assembly is respectively communicated with the first evaporator, the second evaporator, the reagent filling assembly, the liquid storage part and the separation part through pipelines, the multi-way valve assembly further comprises an air inlet and a feed inlet, the air inlet is communicated with external air, and the feed inlet is suitable for extracting dissolved liquid;
and the vacuum pump is respectively communicated with the first evaporator, the second evaporator and the liquid storage part through pipelines.
According to one embodiment of the utility model, the reagent filling assembly comprises a syringe and a liquid inlet bottle which are communicated with the multi-way valve assembly, and an electric sliding table for driving the syringe.
According to one embodiment of the utility model, the chromatographic column comprises a liquid storage pipe and a separation pipe communicated with the liquid storage pipe, wherein the separation pipe is filled with anion exchange resin;
one end of the liquid storage pipe, which is far away from the separation pipe, is detachably connected with a sealing cover, the sealing cover is provided with a liquid injection hole and an air guide hole, and one end of the separation pipe, which is far away from the liquid storage pipe, is provided with a luer connector;
the liquid injection hole and the Ruhr joint are communicated with the multi-way valve component through a pipeline, and the air guide hole is communicated with the vacuum pump through a pipeline.
According to one embodiment of the utility model, the first evaporator and the second evaporator each comprise an electric heating module and an evaporator bottle;
the electric heating module is provided with a heating groove matched with the bottom of the bottle body of the evaporation bottle, and the evaporation bottle is inserted into the heating groove;
the evaporation bottle is respectively communicated with the multi-way valve component and the vacuum pump through pipelines.
According to one embodiment of the utility model, the device further comprises an alkali treatment bottle, wherein the alkali treatment bottle comprises a waste inlet and a suction opening;
the waste inlet is communicated with the first evaporator, the second evaporator, the liquid storage part and the multi-way valve assembly, and the air pumping port is communicated with the vacuum pump.
According to one embodiment of the present invention, further comprising a rack assembly platform connected to the first vaporizer, the second vaporizer, the reagent fill assembly, the chromatography column, and the multi-way valve assembly;
and/or, the vacuum pump and the control system are arranged in the accommodating space.
According to one embodiment of the utility model, the device further comprises a temperature sensor, a position sensor and a radioactivity activity probe;
the temperature sensors are arranged on the first evaporator and the second evaporator;
the position sensor is arranged at the positions of the electric sliding table and the multi-way valve assembly;
the radioactivity probe is disposed at the positions of the first evaporator, the second evaporator and the separating part of the chromatographic column.
According to one embodiment of the utility model, the separation part of the chromatography column is externally sleeved with a tungsten steel sleeve.
In a second aspect, the embodiment of the present invention provides an automatic radionuclide separation method, including the following steps:
extracting the dissolving liquid, evaporating the dissolving liquid to dryness to obtain a first product, and continuously exhausting air in the pipeline for the first time after the dissolving liquid is extracted;
filling a first reagent, dissolving the first product to obtain a second product, and continuously ventilating the pipeline for a second time after filling the first reagent;
injecting the second product into the chromatographic column, and continuously ventilating the pipeline for a third time after the injection is finished;
and leaching the second product to obtain a target leacheate, and evaporating the target leacheate to obtain a third product.
According to an embodiment of the present invention, the leaching the second product to obtain a target leacheate, and evaporating the target leacheate to obtain a third product specifically includes:
filling a second reagent into the chromatographic column, then injecting air, and repeating the processes to obtain a first eluent;
filling a third reagent into the chromatographic column, then injecting air, and repeating the processes to obtain a second eluent;
filling a fourth reagent into the chromatographic column, then injecting air, and repeating the processes to obtain target leacheate;
and evaporating the target leacheate to obtain a third product.
One or more technical solutions in the present invention have at least one of the following technical effects:
the automatic radionuclide separation system comprises a first evaporator, a second evaporator, a reagent filling assembly, a chromatographic column, a multi-way valve assembly and a vacuum pump, wherein the chromatographic column comprises a liquid storage part and a separation part which are sequentially arranged from top to bottom. Through anion exchange method separation radionuclide, full automation control is favorable to promoting radionuclide's separation efficiency and quality, can also reduce artifical participation, ensures operating personnel's safety. The vacuum pump and the reagent filling assembly can avoid reaction solution from adhering to the pipeline in the process of sequentially filling the reaction solution into the first evaporator, the second evaporator and the chromatographic column, so that the utilization efficiency of the reaction solution is improved, the reaction solution is prevented from being mixed up, and the production rate of the radioactive nuclide is improved.
Drawings
Fig. 1 is a perspective view of an automatic radionuclide separation system according to an embodiment of the present invention;
fig. 2 is a rear view of an automatic radionuclide separation system according to an embodiment of the present invention;
fig. 3 is a sectional view of a first evaporator and a second evaporator provided in an embodiment of the present invention;
FIG. 4 is a cross-sectional view of a chromatography column provided in an embodiment of the utility model;
fig. 5 is a schematic structural view of an automatic radionuclide separation system according to an embodiment of the present invention;
FIG. 6 is a first flowchart of an automatic radionuclide separation method according to an embodiment of the present invention;
FIG. 7 is a second flowchart of the method for automatically separating radionuclides provided by the present invention;
fig. 8 is a third flowchart of the method for automatically separating radionuclides according to the embodiment of the present invention.
Reference numerals:
100. dissolving the feed liquid; 1. a first evaporator; 11. an electric heating module; 111. a heating tank; 12. an evaporation bottle; 2. a second evaporator; 3. a reagent fill assembly; 31. an injector; 32. an electric sliding table; 33. a liquid inlet bottle; 4. a chromatographic column; 41. a liquid storage pipe; 42. a separation tube; 43. a sealing cover; 431. a liquid injection hole; 432. an air vent; 44. a luer fitting; 5. a multi-way valve assembly; 6. a vacuum pump; 7. an alkali treatment bottle; 8. a chassis; 91. a temperature sensor; 92. a position sensor; 420. a tungsten steel sleeve; 10. and (4) a support assembling platform.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be clearly described below with reference to the accompanying drawings of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. Based on the embodiments in the utility model, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the utility model.
In the description of the embodiments of the present invention, it should be noted that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the embodiments of the present invention and simplifying the description, but do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the embodiments of the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the embodiments of the present invention, it should be noted that, unless explicitly stated or limited otherwise, the terms "connected" and "connected" are to be interpreted broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. Specific meanings of the above terms in the embodiments of the present invention can be understood in specific cases by those of ordinary skill in the art.
In embodiments of the utility model, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through intervening media. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of an embodiment of the utility model. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
In the related art, the specific production process of the radionuclide includes the steps of solid target preparation, accelerator bombardment, target dissolution, separation and purification, and the like. The steps of separating and purifying the radioactive nuclide by using an anion exchange method are the steps with the most complicated operation and the highest artificial participation degree in all the flows, the dissolved feed liquid contains various impurities, a series of quality control problems can be caused, and the higher artificial participation degree can also cause more safety problems. When part of the reaction solution circulates in the pipeline, the reaction solution is adhered to the pipeline, which causes waste of the reaction solution and reduces the productivity of the radionuclide.
Referring to fig. 1 to 5, an automatic radionuclide separation system according to a first aspect of the present invention includes a first vaporizer 1, a second vaporizer 2, a reagent filling assembly 3, a chromatographic column 4, a multi-way valve assembly 5, and a vacuum pump 6.
The first evaporator 1 is used to evaporate the dissolution feed solution 100, and the second evaporator 2 is used to evaporate the target leacheate. The first evaporator 1 and the second evaporator 2 have certain corrosion resistance, and can bear strong acid, strong oxidation and radioactive corrosive environments under high-temperature conditions.
According to one embodiment of the present invention, each of the first vaporizer 1 and the second vaporizer 2 includes an electric heating module 11 and a vaporizing flask 12.
The electric heating module 11 is provided with a heating groove 111 matched with the bottom of the bottle body of the evaporation bottle 12, and the evaporation bottle 12 is inserted in the heating groove 111.
The bottom of the evaporation bottle 12 is attached to the heating groove 111, so that the evaporation bottle 12 is heated uniformly, and the evaporation bottle 12 is prevented from being broken due to over-high local temperature. The electric heating module 11 is connected to a control system, and can remotely control the temperature during evaporation.
The evaporation bottle 12 is respectively communicated with the multi-way valve assembly 5 and the vacuum pump 6 through pipelines, and the vacuum pump 6 pumps air at the top of the evaporation bottle 12, so that the air pressure in the evaporation bottle 12 is reduced, and the reaction solution can be sucked through the multi-way valve assembly 5.
In one embodiment, the electrical heating module 11 is made of copper plate with a maximum temperature of 240 degrees celsius.
The reagent filling assembly 3 is used for quantitatively extracting air or reaction reagents and then injecting the air or the reaction reagents into the corresponding reaction links.
In one embodiment, reagent fill assembly 3 includes syringe 31, power slide 32, and fluid inlet bottle 33.
The syringe 31 is a piston type syringe, and a precise amount of reagent or air can be drawn during pumping.
The power slide 32 is connected to the syringe 31 for driving the syringe 31 to draw the reagent or air, and the accuracy of the power slide 32 determines the accuracy of the reagent or air dosage.
In one embodiment, the positioning accuracy of the power slide 32 is not more than 0.1mm, ensuring that the syringe 31 draws liquid and air with no more than 3% error.
The syringe 31 and the liquid inlet bottle 33 communicate with the multi-way valve assembly 5.
When the multi-way valve assembly is used, the multi-way valve assembly 5 is adjusted, the node at the position of the liquid inlet bottle 33 is opened, and the syringe 31 extracts the reagent in the liquid inlet bottle 33. And adjusting the multi-way valve assembly 5 again, closing the node at the liquid inlet bottle 33, injecting a reagent into the multi-way valve assembly 5, wherein the reagent can be directly injected into the first evaporator 1, the second evaporator 2 or the chromatographic column 4, or generating negative pressure through the vacuum pump 6, and pumping the reagent into the first evaporator 1, the second evaporator 2 or the chromatographic column 4.
It should be noted that the multi-way valve assembly 5 may be connected to a plurality of liquid feeding bottles 33, a first reaction liquid is added to a first liquid feeding bottle 33, a second reaction liquid is added to a second liquid feeding bottle 33, and so on.
When the multi-way valve assembly is used, the multi-way valve assembly 5 is adjusted, the injector 31 extracts a certain amount of first reaction liquid, the multi-way valve assembly 5 is adjusted again, the injector 31 extracts a certain amount of second reaction liquid, and the first reaction liquid and the second reaction liquid can be mixed according to a ratio to form reagents with different concentrations.
Similarly, by adjusting the multi-way valve assembly 5, a mixture of multiple reagents can be obtained.
In the separation process of the radioactive nuclide, different reaction reagents are needed to be used in different reaction links, the reaction reagents can be configured on site through the injector 31, the electric sliding table 32, the multi-way valve assembly 5 and the plurality of liquid inlet bottles 33, a plurality of reagent bottles and a plurality of reagent bottles do not need to be installed, and the occupied space is reduced.
In one embodiment, the first reaction solution is a 6.00mol/L hydrochloric acid solution, and the second reaction solution is ultrapure water. The first reaction solution and the second reaction solution are mixed to prepare hydrochloric acid solutions with different concentrations.
The chromatographic column 4 comprises a liquid storage part and a separation part which are sequentially arranged from top to bottom, the liquid storage part is communicated with the separation part, and the chromatographic column 4 is used for separating metal ions.
According to one embodiment of the present invention, the chromatography column 4 comprises a liquid storage tube 41 and a separation tube 42, wherein the separation tube 42 is filled with anion exchange resin.
In one embodiment, the separation tube 42 is a quartz glass tube having a length of not less than 150mm, and the reservoir tube 41 is a quartz tube having a length of 20-40 mm. The diameter of the quartz tube is at least 5mm larger than that of the quartz glass tube, and the quartz glass tube is used for storing liquid and balancing column pressure.
In order to ensure the tightness of the separation process, a sealing cover 43 is detachably connected to the end of the liquid storage tube 41 far away from the separation tube 42, a luer connector 44 is arranged at the end of the separation tube 42 far away from the liquid storage tube 41, and the sealing cover 43 and the luer connector 44 can prevent the volatilization and leakage of the radioactive liquid.
The sealing lid 43 is provided with a filling hole 431 and a gas vent 432, the filling hole 431 and the luer 44 are both communicated with the multi-way valve assembly 5, and the gas vent 432 is communicated with the vacuum pump 6.
The liquid storage tube 41 receives the reaction solution in the process through the liquid injection hole 431, the air guide hole 432 is used for balancing air pressure, and the flow of the reagent or air is realized by the negative pressure generated by the vacuum pump 6.
In one embodiment, the sealing cap 43 is connected to the liquid storage tube 41 by a screw thread, and a sealing ring is disposed at a contact position between the sealing cap 43 and the liquid storage tube 41, so as to increase the sealing performance of the chromatographic column 4 and prevent leakage of radioactive reactants.
The multi-way valve assembly 5 is respectively communicated with the first evaporator 1, the second evaporator 2, the reagent filling assembly 3, the liquid storage part and the separation part through pipelines.
The multi-way valve component 5 is also provided with an air inlet and a feed inlet, the air inlet is communicated with the outside air, and the feed inlet is communicated with the dissolving liquid 100 and is suitable for extracting the dissolving liquid 100.
The vacuum pump 6 is respectively communicated with the first evaporator 1, the second evaporator 2, the multi-way valve component and the liquid storage part through pipelines.
When the device is used, the vacuum pump 6 generates negative pressure in the first evaporator 1, the first evaporator 1 is communicated with the multi-way valve assembly 5, and the dissolved feed liquid 100 can be pumped into the first evaporator 1. After the dissolving liquid 100 is pumped out, the vacuum pump 6 continuously pumps air in the first evaporator 1, and the dissolving liquid adhered to the pipeline can be blown into the first evaporator 1, so that the utilization efficiency of the dissolving liquid is increased, the reaction solution is prevented from being mixed up, and the production rate of the radioactive nuclide is improved.
The vacuum pump 6 generates negative pressure again in the first vaporizer 1, and can draw the reaction reagent in the reagent filling module 3. After the extraction of reaction reagent is accomplished, vacuum pump 6 is continuously bled at first evaporimeter 1, can blow in the reaction reagent of adhesion in the pipeline in first evaporimeter 1, has increased reaction reagent's utilization efficiency, has avoided reaction reagent to appear obscuring.
After the vacuum pump 6 extracts the reaction solution, the gas is continuously introduced into the pipeline for a period of time, so that the reaction solution cannot be adhered to the pipeline in each link, and the utilization efficiency of the reaction solution is improved.
In one embodiment, the vacuum pump 6 is a diaphragm type vacuum pump, and a certain negative pressure is formed at the pumping port by reciprocating an internal diaphragm, wherein the negative pressure ranges from 0kPa to 100kPa, and the flow rate ranges from 10 mL/min to 30 mL/min.
It should be noted that in the automatic radionuclide separation system provided in the embodiment of the present invention, the multi-way valve assembly 5 is respectively communicated with the first evaporator 1, the second evaporator 2, the reagent filling assembly 3, the liquid storage portion, the separation portion, the air inlet, the feed inlet, the vacuum pump 6, and the electric slide table 32 through pipelines as motive power for the reaction solution to flow in each link. During separation, all the treatment links are closely connected, so that the contents of manual transportation, dumping, cleaning and the like are reduced, and the separation efficiency of the radioactive nuclide is improved.
Compared with the manual operation adopted in the traditional technology, the embodiment of the utility model can save 45-90min when the single radionuclide separation process is executedHas important significance for some radionuclides with short half-life. To be provided with64For the example of Cu, the alloy is,64the half-life period of Cu is about 12.7h, the necessary time of production, separation, purification, transportation and other processes is deducted, and the utilization efficiency of the radionuclide is obviously improved within 45-90 min.
The efficient automatic radionuclide separation system can enable the radionuclide with short half-life period to enter the commercial or civil field, so that the possibility that the original radionuclide which cannot be fully utilized is applied is realized, and the utilization range of the radionuclide with short half-life period is expanded. Meanwhile, the utilization time of the radionuclide with longer half-life is prolonged on the basis of the related technology.
The automatic radionuclide separation system provided by the embodiment of the utility model can generate waste gas or waste liquid in the evaporation or separation process, can cause certain pollution to the air, and can cause damage to operators, so that waste materials generated in the separation process need to be collected and treated uniformly.
According to one embodiment of the utility model, the separation system further comprises an alkaline treatment flask 7, the alkaline treatment flask 7 comprising a waste inlet and a suction opening.
The waste inlet is communicated with the first evaporator 1, the second evaporator 2, the liquid storage part and the multi-way valve assembly 5, and the air exhaust port is communicated with the vacuum pump 6.
All gas and liquid that vacuum pump 6 extracted in the piece-rate system all need handle through alkali treatment bottle 7, avoid revealing the back contaminated air or harm operating personnel.
In one embodiment, the alkali treatment bottle 7 is filled with 2.00-4.00mol/L sodium hydroxide solution, and the acid gas recovery process is completed through acid-base neutralization reaction.
According to one embodiment of the present invention, the automated radionuclide separation system further comprises a rack assembly platform 10, the rack assembly platform 10 being connected to the first vaporizer 1, the second vaporizer 2, the reagent filling assembly 3, the chromatography column 4, and the multi-way valve assembly 5. The stand assembly platform 10 serves to support and secure the various components in a stable positional relationship.
In another embodiment, the automated radionuclide separation system further comprises a cabinet 8 that constitutes a sealed containment space. The vacuum pump 6, the electric sliding table 32 and the control system are arranged in the accommodating space of the case 8, and the components, such as the first evaporator 1, the second evaporator 2, the injector 31, the liquid inlet bottle 33, the chromatographic column 4, the multi-way valve assembly 5 and the like, in which the reaction solution flows are isolated at the outer side of the case 8.
In one embodiment, the volume of the enclosure 8 is no more than 0.0027m3The space of the radioactive hot chamber can be occupied less.
According to one embodiment of the present invention, a sensor assembly is further provided on the automated radionuclide separation system. The sensor assembly includes a temperature sensor 91, a position sensor 92, and a radioactivity probe.
The temperature sensors 91 are provided on the first evaporator 1 and the second evaporator 2 for monitoring the temperature at the time of evaporation in real time.
In the case where the first and second evaporators 1 and 2 include the electric heating module 11 and the evaporation flask 12, the temperature sensor 91 is provided at a position where the electric heating module 11 is close to the evaporation flask 12.
The position sensor 92 can accurately reflect and record the position and the stroke of the moving structure, and the position precision of the moving structure can be improved.
The position sensor 92 is arranged at the position of the electric sliding table 32 and the multi-way valve assembly 5, and is used for monitoring the movement amount of the electric sliding table 32 and the opening and closing state of the multi-way valve assembly 5 in real time.
In one embodiment, the position sensor 92 is a travel switch, a micro switch, a proximity switch, etc. that does not require direct mechanical contact with the moving structure, and has the advantages of reliable operation, stable performance, fast response frequency, long service life, strong anti-interference capability, water and shock resistance, and corrosion resistance.
In the production process of radioactive nuclide, the detection of nuclide activity is realized by a radioactive activity probe. The radioactivity probe converts gamma rays generated by nuclides into electric pulse signals according to the interaction principle of the rays and substances so as to display corresponding radioactivity.
The radioactivity probe is disposed at positions where the first evaporator 1, the second evaporator 2, and the separation unit of the column 4 are located, and detects the activity of the radionuclide at a plurality of stages of the separation process.
According to one embodiment of the utility model, the outside of the separation section of the chromatography column 4 is fitted with a tungsten steel sleeve 420. The tungsten steel sleeve 420 can wrap the separation part to shield gamma rays, so that damage to operators is avoided.
It should be noted that the automatic radionuclide separation system provided in the embodiment of the present invention further includes an upper computer software system and a control system, the upper computer software system is responsible for outputting instructions, and a controller in the control system transmits the instructions to the actuators of the respective components.
The controller adopts a programmable controller and is used for controlling the starting and stopping of the actuator, reading the state data of the equipment, converting the state data into a digital signal and feeding the digital signal back to an upper computer software system.
In one embodiment, the controller is a German Siemens PLC controller, the type is ET200SP distributed I/O, and the controller is appropriate in size and simple and convenient to operate.
The actuator consists of a sensor assembly, an electric sliding table and a valve steering driving module, and the valve steering driving module is arranged in the multi-way valve assembly and used for controlling the flow state of the multi-way valve assembly.
Meanwhile, the embodiment of the second aspect of the utility model provides an automatic radionuclide separation method which is suitable for being used in18F、57Co、64Cu、67Ga、68Ge、89Zr、103Pd、109Cd、111In, referring to fig. 6 to 8, the separation of multiple radionuclides, including the following steps:
and S1, extracting the dissolving liquid, evaporating the dissolving liquid to dryness to obtain a first product, and continuously exhausting air in the pipeline for the first time after the dissolving liquid is extracted.
It is understood that the solute solution is a reaction product of the target solution and the target piece, and contains radionuclides, metal impurities, and the like. And pumping the dissolving liquid from the production device or the storage device into an evaporator by using a vacuum pump or other pumping components, and evaporating the dissolving liquid to obtain a first product.
When in use, different drying strategies are adopted according to the volume or weight of the dissolved feed liquid.
In one embodiment, the evaporation temperature is controlled at 120-220 ℃, and the evaporation time is controlled at 30-60 min. The evaporator adopts an electric heating evaporator, and the working temperature and the working duration of the electric heating evaporator are accurately controlled through a control system and a temperature sensing unit.
It should be noted that the evaporation temperature is related to the weight, volume or kind of the dissolution liquid, and an appropriate temperature-time combination needs to be determined by experiments in advance before sending an evaporation instruction to the electric heating evaporator.
After the dissolving liquid is pumped into the evaporator, the pipeline is continuously pumped for a period of time, and the dissolving liquid remained in the pipeline can be completely pumped into the first evaporator.
In one embodiment, after the dissolution liquid is extracted, the pipeline is continuously pumped for 20-60s, so that the dissolution liquid remained in the pipeline can be completely blown into the evaporator, and the waste of the dissolution liquid is avoided.
The continuous air suction can keep the cleanness in the pipeline, so that the pollution condition in the flowing process of the reagent in the subsequent link is avoided, the purity of the reaction reagent is increased, and the impurities in the reaction product are reduced.
Waste gas that the evaporation to dryness in-process produced lets in waste gas collection device, avoids waste gas pollution environment or causes the damage to operating personnel.
In one embodiment, the waste gas collecting device is an alkali treatment bottle, and 2-4mol/L sodium hydroxide solution is filled in the alkali treatment bottle.
And S2, filling a first reagent, dissolving the first product to obtain a second product, and continuously ventilating the pipeline for a second time after the first reagent is filled.
It will be appreciated that a first reagent is added to the evaporator, the type and concentration of the first reagent being related to the first product.
To accelerate the dissolution of the first product, the temperature of the reaction may be increased after the addition of the first reagent.
After the first reagent is filled into the evaporator, the first reagent is continuously ventilated in the pipeline through which the first reagent circulates, so that the first reagent is prevented from being adhered to the pipeline.
At the same time, the continuous aeration may create an agitation effect on the first reagent within the evaporator, increasing the reaction rate of the first reagent and the first product.
And S3, injecting the second product into the chromatographic column, and continuously ventilating the pipeline for a third time after the injection is finished.
It is understood that the first product is re-dissolved to obtain a liquid second product, which contains various impurities and needs to be purified and separated by a chromatographic column.
Injecting the liquid second product into the liquid storage part of the chromatographic column to gradually separate different metal ions.
And S4, leaching the second product to obtain a target leacheate, and evaporating the target leacheate to obtain a third product.
It can be understood that different reagents are added into the chromatographic column, so that impurities in the second product can be separated, and finally the target nuclide with higher purity is obtained.
The chromatographic column is based on that different complex anions are formed by metal ions and anions in an acid medium, and the distribution coefficients of the different complex anions between resin and the acid medium are different, so that the separation of target nuclide and other metal ion impurities is realized.
The chromatographic column is filled with anion exchange resin, and corresponding types of anion exchange resin can be selected for different radionuclides.
The radionuclide automatic separation method provided by the embodiment of the utility model can gradually separate different impurities when the second product is leached.
According to an embodiment of the present invention, the leaching the second product to obtain a target leacheate, and evaporating the target leacheate to obtain a third product specifically includes:
and S41, filling a second reagent into the chromatographic column, then injecting air, and repeating the above processes to obtain a first leacheate.
It will be appreciated that the second reagent is added to the column multiple times along with air, which acts as a flow pressure to drive the mobile phase of the column and may clean the tubing of the remaining second reagent.
The first leacheate contains impurity metal ions, and the first leacheate is collected, so that the metal ions in the first leacheate can be recovered, the metal waste is reduced, and the environment pollution can be avoided.
It should be noted that when the second reagent and the air are filled, the dosage of the second reagent and the air needs to be precisely controlled, and the filling process is performed by using precise equipment.
And S42, filling a third reagent into the chromatographic column, then injecting air, and repeating the above processes to obtain a second eluent.
It will be appreciated that the column is filled with the third reagent and air multiple times, the air acting as a flow pressure to drive the mobile phase of the column and allowing the third reagent remaining in the tubing to be purged.
The third reagent is used for leaching impurities in the second product, and the second leaching solution is introduced into the alkali treatment bottle, so that the discharge of waste liquid is reduced.
It should be noted that when the third reagent and the air are filled, the dosage of the third reagent and the air needs to be precisely controlled, and the filling process is performed by using precise equipment.
And S43, filling a fourth reagent into the chromatographic column, then injecting air, and repeating the above processes to obtain the target leacheate.
It will be appreciated that the column is filled with the fourth reagent and air multiple times, the air acting as a flow pressure to drive the mobile phase of the column and allowing the tubing to be purged of the remaining fourth reagent.
The fourth reagent is used for eluting the radionuclide in the second product, and the radionuclide with higher purity can be obtained by collecting the target eluent.
It should be noted that, when the fourth reagent and the air are filled, the dosage of the fourth reagent and the air needs to be precisely controlled, and the filling process is performed by using precise equipment.
S44, evaporating the target leacheate to obtain a third product.
It will be appreciated that the target eluate, after evaporation to dryness, provides a solid third product comprising the higher purity radionuclide.
The high purity radionuclides may be collected for storage, or further processing may be performed to bring the radionuclides to or near the application stage.
According to an embodiment of the present invention, the evaporating the target leacheate to obtain a third product further comprises:
and S5, adding a fifth reagent, and dissolving the third product to obtain a final product.
It will be appreciated that the final product, which is the target radionuclide product, can be prepared as desired.
On the premise of meeting the application, preparing a final product and entering a subsequent application link.
On the premise that the application is not met, the third product is temporarily stored and the final product is prepared when needed.
It is understood that the radionuclide with higher purity can be obtained through the above steps, and the conditions in the reaction process are adjusted according to the kinds of the radionuclide, the solid target and the reagent.
According to one embodiment of the present invention, the first, second, third, fourth and fifth reagents are each formulated with ultra pure water by 6.00mol/L hydrochloric acid solution. The 6.00mol/L hydrochloric acid solution is placed in the first liquid feeding bottle, the ultrapure water is placed in the second liquid feeding bottle, the reagent filling assembly can extract the 6.00mol/L hydrochloric acid solution and the ultrapure water according to a certain proportion, the preparation process can be set through the control system, the use is flexible and convenient, and various storage devices do not need to be connected. When other reagents are required, the preparation is carried out in the same manner.
The automated radionuclide separation method is described below with reference to specific examples:
example one
The target sheet is a copper substrate, gold is plated on the copper substrate, then nickel is plated, and the nickel plating layer is generated after bombardment of particles generated by a cyclotron64Ni(p,n)64And (4) carrying out Cu nuclear reaction. Preparing target solution by adopting 4.00-6.00mol/L hydrochloric acid solution and hydrogen peroxide solution, and dissolving the solid target to obtain solution material.
The dissolving material liquid in the target dissolving groove is pumped into the first evaporator through the vacuum pump, the first time is continuously pumped in the pipeline after the dissolving material liquid is completely pumped, the first time is 30s, and the dissolving material liquid remained in the pipeline can be pumped into the first evaporator. And then automatically starting the program to heat and evaporate to dryness, wherein the heating temperature is 200 ℃, the time for completely evaporating the dissolved material liquid is 40min, a first product is obtained, and waste gas generated in the evaporation process is introduced into an alkali treatment bottle.
6.00mol/L hydrochloric acid and ultrapure water are extracted to prepare 0.01mol/L hydrochloric acid solution as a first reagent, and the 0.01mol/L hydrochloric acid solution is extracted into a first evaporator through a vacuum pump. The vacuum pump continues to pump air for a second time of 60 seconds, and the hydrochloric acid solution remaining in the pipeline can be completely blown into the first evaporator. The continuous air exhaust can also stir 0.01mol/L hydrochloric acid solution, so that the dissolution of the first product is accelerated. And when the first product is dissolved, controlling the temperature at 90 ℃, and obtaining a second product after the first product is dissolved.
The AG1-X8 ion exchange column was used as the column, and the dissolved second product was pumped into the liquid storage part of the column by a vacuum pump, and then the vacuum pump continued to pump for a third time of 60 seconds to ensure that no solution remained in the line.
The reagent filling assembly 3 extracts 5mL of 6.00mol/L hydrochloric acid solution as a second reagent, injects the second reagent into the liquid storage part of the chromatographic column, extracts 5mL of air as the flowing pressure for driving the mobile phase of the chromatographic column, and continuously extracts air to clean the residual hydrochloric acid solution on the pipeline, and the operation steps are repeated for four times. The total amount of the 6.00mol/L hydrochloric acid solution is 20mL, and the flow rate of the mobile phase is controlled to be 1.0-2.0 mL/min.
And obtaining a first leacheate after leaching is finished, and injecting the first leacheate into the first evaporator for recovering nickel.
And (4) extracting 6.00mol/L hydrochloric acid solution and ultrapure water by the reagent filling assembly 3 to prepare 4.00mol/L hydrochloric acid solution as a third reagent, leaching the third reagent in the same step (4), wherein the second leaching solution comprises various impurities, and injecting the second leaching solution into the alkali treatment bottle.
Extracting 6.00mol/L hydrochloric acid solution and ultrapure water by the reagent filling assembly 3 to prepare 0.10mol/L hydrochloric acid solution as a fourth reagent, leaching the fourth reagent in the same step 4, and obtaining a mobile phase by an anion exchange chromatographic column64Cu product to be made of64A target rinse of Cu is injected into the second evaporator.
Starting the second evaporator to obtain64And evaporating the leacheate of the Cu product to dryness at 200 ℃ to obtain a third product, and feeding acid gas generated in the evaporation process into an alkali treatment bottle.
Extracting 6.00mol/L hydrochloric acid solution and ultrapure water as required, preparing 0.01mol/L hydrochloric acid solution as a fifth reagent, and dissolving the evaporated hydrochloric acid solution64And (3) continuously ventilating and stirring the Cu product in the dissolving process.
Example two
Using yttrium foil as target, bombarding by particles generated by cyclotron89Y(p,n)89Zr nuclear reaction. Adopting 0.50-6.00mol/L hydrochloric acid solution to prepare target dissolving solution, and dissolving the solid target to obtain solution.
The dissolving material liquid in the target dissolving groove is pumped into the first evaporator through the vacuum pump, the first time is continuously pumped in the pipeline after the dissolving material liquid is completely pumped, the first time is 30s, and the dissolving material liquid remained in the pipeline can be pumped into the first evaporator. And then automatically starting the program to heat and evaporate to dryness, wherein the heating temperature is 200 ℃, the time for completely evaporating the dissolved material liquid is 40min, a first product is obtained, and waste gas generated in the evaporation process is introduced into an alkali treatment bottle.
A hydrochloric acid solution of 1.00mol/L of the first reagent was pumped into the first evaporator by a vacuum pump. The vacuum pump continues to pump air for a second time of 60 seconds, and the hydrochloric acid solution remaining in the pipeline can be completely blown into the first evaporator. The continuous air exhaust can also stir the 1.00mol/L hydrochloric acid solution, so that the dissolution of the first product is accelerated. And when the first product is dissolved, controlling the temperature at 90 ℃, and obtaining a second product after the first product is dissolved.
And pumping the dissolved feed liquid into a liquid storage part of the chromatographic column by using a vacuum pump, filling the chromatographic column by using ZR resin, and ensuring that no solution is left in the pipeline when the vacuum pump pumps for the third time, wherein the third time is 60 s.
The reagent filling assembly 3 extracts 2mL of 1.00mol/L hydrochloric acid solution as a second reagent, injects the second reagent into the liquid storage part of the chromatographic column, extracts 2mL of air as the flowing pressure for driving the mobile phase of the chromatographic column, continues to extract the air to clean the residual hydrochloric acid solution on the pipeline, and repeats the operation steps five times. The total amount of 1.00mol/L hydrochloric acid solution used is 10mL, and the flow rate of the mobile phase is controlled between 1.0 and 2.0 mL/min.
And obtaining a first leacheate after leaching is finished, wherein the first leacheate contains various impurities and is injected into the alkali treatment bottle.
And (3) extracting 2mL of ultrapure water as a third reagent, performing leaching operation in the same step (2), wherein the second leaching solution also comprises various impurities, and injecting the second leaching solution into the alkali treatment bottle.
Draw 1.00m2mL of oxalic acid solution of ol/L is used as a fourth reagent, the leaching operation is the same as the step 2, and the mobile phase is obtained by a ZR chromatographic column89Zr nuclide, will contain89The target leacheate of Zr was injected into the second evaporator.
Starting the second evaporator to obtain89The Zr nuclide leacheate is evaporated to dryness at 170 ℃, and acid gas generated in the evaporation process enters an alkali treatment bottle.
Extracting 0.01mol/L hydrochloric acid solution as fifth reagent as required, dissolving the evaporated89Continuously aerating and stirring the Zr nuclide in the dissolving process.
In summary, the automatic radionuclide separation system and method provided in the embodiments of the present invention include a first evaporator, a second evaporator, a reagent filling assembly, a chromatography column, a multi-way valve assembly, and a vacuum pump, wherein the chromatography column includes a liquid storage portion and a separation portion sequentially arranged from top to bottom. Through anion exchange method separation radionuclide, full automation control is favorable to promoting radionuclide's separation efficiency and quality, can also reduce artifical participation, ensures operating personnel's safety. The vacuum pump and the reagent filling assembly can avoid reaction solution from adhering to the pipeline in the process of sequentially filling the reaction solution into the first evaporator, the second evaporator and the chromatographic column, so that the utilization efficiency of the reaction solution is improved, the reaction solution is prevented from being mixed up, and the production rate of the radioactive nuclide is improved.
Under the condition that the chromatographic column comprises a sealing cover, a sealing ring and a luer connector, the sealing performance of the chromatographic column can be ensured, the leakage of radioactive substances is reduced, and the environmental pollution and the damage to operators are avoided.
Under the condition that the separation part of the chromatographic column is sleeved with the tungsten steel sleeve, the tungsten steel sleeve can wrap the separation part to play a role in shielding gamma rays.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the utility model, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. An automatic radionuclide separation system comprising:
a first evaporator;
a second evaporator;
a reagent fill assembly;
the chromatographic column comprises a liquid storage part and a separation part which are sequentially arranged from top to bottom, wherein the liquid storage part is communicated with the separation part;
the multi-way valve assembly is respectively communicated with the first evaporator, the second evaporator, the reagent filling assembly, the liquid storage part and the separation part through pipelines, the multi-way valve assembly further comprises an air inlet and a feed inlet, the air inlet is communicated with external air, and the feed inlet is suitable for extracting dissolved liquid;
and the vacuum pump is respectively communicated with the first evaporator, the second evaporator and the liquid storage part through pipelines.
2. The automated radionuclide separation system of claim 1, wherein the reagent filling assembly comprises a syringe and a feed bottle in communication with the multi-port valve assembly, and a motorized slide to drive the syringe.
3. The automated radionuclide separation system according to claim 1, wherein the chromatographic column comprises a liquid storage tube and a separation tube connected to the liquid storage tube, the separation tube being filled with an anion exchange resin;
one end of the liquid storage pipe, which is far away from the separation pipe, is detachably connected with a sealing cover, the sealing cover is provided with a liquid injection hole and an air guide hole, and one end of the separation pipe, which is far away from the liquid storage pipe, is provided with a luer connector;
the liquid injection hole and the Ruhr joint are communicated with the multi-way valve component through a pipeline, and the air guide hole is communicated with the vacuum pump through a pipeline.
4. The automated radionuclide separation system according to claim 1, wherein the first and second vaporizers each comprise an electrical heating module and a vaporizer bottle;
the electric heating module is provided with a heating groove matched with the bottom of the bottle body of the evaporation bottle, and the evaporation bottle is inserted into the heating groove;
the evaporation bottle is respectively communicated with the multi-way valve component and the vacuum pump through pipelines.
5. The automated radionuclide separation system according to claim 1, further comprising an alkaline treatment vial comprising a waste inlet and a suction port;
the waste inlet is communicated with the first evaporator, the second evaporator, the liquid storage part and the multi-way valve assembly, and the air pumping port is communicated with the vacuum pump.
6. The automated radionuclide separation system of claim 1, further comprising a rack assembly platform connected to the first vaporizer, the second vaporizer, the reagent fill assembly, the chromatography column, and the multi-port valve assembly;
and/or, the vacuum pump and the control system are arranged in the accommodating space.
7. The automated radionuclide separation system according to claim 2, further comprising a temperature sensor, a position sensor, and a radioactivity probe;
the temperature sensors are arranged on the first evaporator and the second evaporator;
the position sensor is arranged at the positions of the electric sliding table and the multi-way valve assembly;
the radioactivity probe is disposed at the positions of the first evaporator, the second evaporator and the separating part of the chromatographic column.
8. The automated radionuclide separation system according to claim 1, wherein a tungsten steel sleeve is sleeved outside the separation part of the chromatographic column.
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