CN103771341A - Method for preparing radioactive <124>I ions - Google Patents
Method for preparing radioactive <124>I ions Download PDFInfo
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- CN103771341A CN103771341A CN201310717680.4A CN201310717680A CN103771341A CN 103771341 A CN103771341 A CN 103771341A CN 201310717680 A CN201310717680 A CN 201310717680A CN 103771341 A CN103771341 A CN 103771341A
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Abstract
The invention discloses a method for preparing radioactive <124>I ions. The preparation method comprises the following steps: a, taking aluminium oxide powder and tellurium dioxide powder in a mass ratio of 1:18-22, uniformly mixing the powder, and pressing the obtained mixture into a tellurium target with a thickness of 50-60 mg/cm<2>; b, placing the prepared tellurium target in a circular accelerator, and irradiating the tellurium target 2-3 h by Te (p, n) <124>I, wherein the incident p particle beam intensity is 18-20 mu A, the energy is 18.5-20 MeV, and the angle of incidence is 6-10 DEG; meanwhile, cooling the tellurium target by using water in the process of irradiating, and after the irradiating is completed, placing the tellurium target to cool 4-6 h; c, placing the tellurium target in a quartz distillation tube of a destructive distillation device to distill, meanwhile, controlling the temperature to 750 DEG C so as to heat the tellurium target, so that radioactive <124>I ions are escaped, and collecting the radioactive <124>I ions. The problems that radionuclide <124>I prepared in the prior art is low in yield and low in recovery rate are solved.
Description
Technical field
The invention belongs to the preparation field of radionuclide, relate in particular to one and prepare radioactivity
124the method of I ion.
Background technology
Iodine can form stable compound with various biomolecules such as protein, nucleic acid, amino acid.Radioiodine, because it has good nulcear properties and chemical property, becomes and is being only second to aspect clinical usage quantity
99mthe radionuclide of Tc.
Radioiodine therapy hyperthyroidism has over half a century, thinks that at present it is safe therapeutic modality.Become the most general method for the treatment of hyperthyroidism at U.S.'s radioiodine therapy, approximately there is 70% the first-selected radioiodine therapy of patient, its advantage is good effect, handy and safe, treatment time is short, side effect is little, expense is low and seldom recurrence, be particularly suitable for older, invalid or irritated to medicine, have cardiac disorder or other to be not suitable for the patient of operative treatment.In addition radioiodinated medicine has also become most important cardiovascular and cerebrovascular, tumour and rii receptor medicine.These medicines have the features such as not damaged, highly sensitive, specific selectivity is strong, therefore can accurately carry out early diagnosis.
Radioiodine nucleic has multiple, as
123i,
124i and
131the radionuclides such as I, wherein, radionuclide
124the transformation period of I is 4.2 days, and radionuclide
123the transformation period of I is only 13.2h, so radionuclide
124on the mark that I grows at longer-distance dispensing and video picture cycle request, preponderate.And in view of
124i is low to patient's radiation dose, under same activity, thyroid dosage is only had to radionuclide
1311/100 left and right of I, not only duplicate detection in a short time, and detection efficiency is high, imaging clearly.Therefore, radionuclide
124i is considered to be best suited for one of radionuclide doing in-vivo diagnostic.
At present, radionuclide
124the preparation method of I mainly contains two large classes: the first kind is first to produce with charged particle nuclear reaction
123then Xe is radionuclide by its decay
124i; Equations of The Second Kind is directly to produce radionuclide with charged particle bombardment tellurium target or antimony target
124i.Because the former needs the proton of higher-energy (>50MeV), operational difficulty, has limited application.Therefore, current domestic most employing Equations of The Second Kind method do solid target with antimony and obtain radionuclide
124i.But existing Equations of The Second Kind method still exists and prepares radionuclide
124i yield is low, and the rate of recovery is low, and poor stability produces the problems such as pollution to environment.
Summary of the invention
For this reason, technical problem to be solved by this invention is to solve and in prior art, prepares radionuclide
124i yield is low, the problem that the rate of recovery is low, and then the preparation that a kind of yield is high, the rate of recovery is high radioactivity is provided
124the method of I ion.
For solving the problems of the technologies described above, preparation radioactivity of the present invention
124the method of I ion, comprises the steps:
A. get aluminium sesquioxide and the tellurium dioxide powder that mass ratio is 1:18-22 and mix, and to be pressed into thickness be 50-60mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed in to magnetic resonance acceleator, by Te (p, n)
124i irradiation 2-3h, wherein, the p particle beam intensity of incident is 18-20 μ A, and energy is 18.5-20MeV, and the angle of incident is 6-10 °, and while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 4-6h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.25-0.35MPa, the air in the described quartzy still tube of the dry carrier gas displacement of high purity that flow velocity is 500-1000mL/min; The temperature of now controlling described quartzy still tube rises to 750 ℃ described tellurium target is heated, and prepares described radioactivity
124i ion is overflowed, and collects, and to obtain final product.
Preferably, comprise the steps:
A. get aluminium sesquioxide and the tellurium dioxide powder that mass ratio is 1:20 and mix, and to be pressed into thickness be 55mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed in to magnetic resonance acceleator, by Te (p, n)
124i irradiation 2.5h, wherein, the p particle beam intensity of incident is 19 μ A, and energy is 19MeV, and the angle of incident is 8 °, and while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 5h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.3MPa, the air in the described quartzy still tube of the dry carrier gas displacement of high purity that flow velocity is 800mL/min; The temperature of controlling subsequently described quartzy still tube rises to 750 ℃ described tellurium target is heated, and prepares described radioactivity
124i ion is overflowed, and collects, and to obtain final product.
In described step c, the step of the quartzy still tube intensification of described control specifically comprises: control temperature rises to 110-130 ℃ of maintenance 9-11min, control temperature rises to 440-460 ℃ and keeps 9-11min, control temperature to rise to 590-610 ℃ of maintenance 2-4min, and in the time that the actual temperature of described quartzy still tube reaches 700-720 ℃, stops intensification.
Preferably, in described step c, the step of the quartzy still tube intensification of described control specifically comprises: control temperature rises to 120 ℃ of maintenance 10min, control temperature rises to 450 ℃ and keeps 10min, control temperature to rise to 600 ℃ of maintenance 3min, and in the time that the actual temperature of described quartzy still tube reaches 710 ℃, stops intensification.
Preferably, in described step c, described collection radioactivity
124the step of I ion, comprises and controls described radioactivity
124the step that I ion absorbs by the NaOH solution of 0.02M.
Preferably, in described step c, described collection radioactivity
124after the step of I ion is also included in NaOH solution and absorbs, by remaining radioactivity
124the step that I ion adsorbs by the mixture of soda-lime and charcoal.
Preferably, in described step c, described carrier gas is helium, argon gas or the neon of purity more than 99.99%.
Before described step a, also comprise the step of preparing described tellurium dioxide, specifically comprise:
A, get the tellurium powder of 8-10 weight part, add the 6M salpeter solution of 40-60 parts by volume to dissolve, described tellurium abundance >=99.0%;
B, to be neutralized to pH to the ammonium hydroxide that adds liquefaction in the lysate obtaining in above-mentioned steps A be 6.5-7.5, with solution described in post-heating to dry;
C, the concentrated hydrochloric acid 15-20 parts by volume of getting 12M are redissolved dried residue in above-mentioned steps;
D, again with liquefying hydrogen ammonium oxide, the solution after described redissolution is neutralized to pH6.5-7.5, with solution described in post-heating until approach boiling, and drip the Hexamine solution that mass concentration is 15-25% in solution, make tellurium dioxide precipitation, placement is filtered after spending the night, get solid dry at 150 ℃, obtain described tellurium dioxide.
Preferably, the step of the described tellurium dioxide of described preparation, specifically comprises:
A, get the tellurium powder of 10 weight parts, add the 6M salpeter solution of 50 parts by volume to dissolve, described tellurium abundance >=99.0%;
B, to be neutralized to pH to the ammonium hydroxide that adds liquefaction in the lysate obtaining in above-mentioned steps A be 7, with solution described in post-heating to dry;
C, concentrated hydrochloric acid 18 parts by volume of getting 12M are redissolved dried residue in above-mentioned steps;
D, again take liquefying hydrogen ammonium oxide, the solution after described redissolution is neutralized to pH as 7, with solution described in post-heating until approach boiling, and be 20% Hexamine solution to dripping mass concentration in solution, make tellurium dioxide precipitation, placement is filtered after spending the night, get solid dry at 150 ℃, obtain described tellurium dioxide.
The pass of described weight part and parts by volume is the relation of g/mL.
The invention provides a kind of radioactivity being prepared by aforesaid method
124i ion.
Technique scheme of the present invention has the following advantages compared to existing technology:
(1) preparation radioactivity of the present invention
124the method of I ion, with TeO
2for tellurium target carries out
124the preparation of I, and specifically define the design parameter in destructive distillation preparation process after practicing shooting and practicing shooting, overcome in prior art with
123xe or directly prepare radionuclide with tellurium target or antimony target
124the yield that I causes is low, and the rate of recovery is low, and poor stability produces the problems such as pollution, the radioactivity that the method for the invention makes to environment
124i ion not only yield is high, and the rate of recovery is high, and the high and "dead" gas leakage in safe preparation process;
(2) preparation radioactivity of the present invention
124in the method for I ion, further by controlling the heating schedule in described destructive distillation preparation process, employing control temperature rises to 110-130 ℃ of maintenance 9-11min, control temperature rises to 440-460 ℃ and keeps 9-11min, control temperature to rise to 590-610 ℃ of maintenance 2-4min, and temperature control program when the stage that stops heating up in the time that the actual temperature of described quartzy still tube reaches 700-720 ℃, the radioactivity making
124i ion yield significantly improves, and the rate of recovery significantly improves, and the high and "dead" gas leakage in safe preparation process;
(3) preparation radioactivity of the present invention
124in the method for I ion, selecting the tellurium target thickness making is 55mg/cm
2time, radionuclide
123i and
126it is less that the impurity such as I generate, and improved radioactivity
124the purity of I ion;
(4) preparation radioactivity of the present invention
124in the method for I ion, the p particle beam intensity of selecting incident is 19 μ A, and energy is 19MeV, when the angle of incident is 8 °, has increased its irradiated area and area of dissipation, and then has improved radioactivity
124i ion yield and the rate of recovery, also saved target has been carried out to cooling time and the consumption of water simultaneously, enhances productivity and saving water resource;
(5) preparation radioactivity of the present invention
124the method of I ion, by what prepare
124i ion successively through being equipped with NaOH ionic adsorption container and be equipped with soda-lime and charcoal trap receptacle will described in
124i ion all adsorbs, the method safety, reliable, and collect
124the yield of I ion improves, and the rate of recovery improves and "dead" gas leakage.
Accompanying drawing explanation
For content of the present invention is more likely to be clearly understood, below according to a particular embodiment of the invention and by reference to the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 is the structural representation of destructive distillation device of the present invention;
In figure, Reference numeral is expressed as: 1-surge pump, 2-trap receptacle, 3-ionic adsorption container, 4-well heater, 5-target container protecting seat, 6-quartz filtering membrane, the xeothermic well heater of 7-, 8-target sheet, 9-quartz still tube, 10-carrier gas admission port, the outlet of 11-tail gas.
Embodiment
Described in the following each embodiment of the present invention, cooled tellurium target is for the preparation of radioactivity
124the step of I ion adopts the destructive distillation device shown in Fig. 1 to be prepared.As shown in Figure 1, described destructive distillation device, according to described
124the direction of motion of I ion comprises quartzy still tube 9, ionic adsorption container 3, trap receptacle 2 and the surge pump 1 that horizontal direction is communicated with in turn.
Described quartzy still tube 9 along continuous straight runs settings, for the preparation of obtaining radioactivity
124i ion, shown in the diameter of quartzy still tube 9 be 32mm, thickness of pipe is 2mm.Described quartzy still tube 9 peripheries are provided with well heater 4, for controlling the temperature of reaction in described quartzy still tube 9.Its inside, chamber is provided with fixing target container protecting seat 5 and target sheet 8, and described target sheet 8 is fixed on described target container protecting seat 5.One end of described quartzy still tube 9 is provided with carrier gas admission port 10, and the inner position near described carrier gas admission port 10, chamber is provided with quartzy filtering membrane 6, for intercepting
124i is oppositely to carrier gas admission port 10 adverse current diffuse pollution argon gas pipelines.Described well heater 4 is lateral opening formula electric furnace, and its diameter is that 60mm, long 300mm, temperature can be adjusted to 1100 ℃.
In addition, entering pressure and the flow velocity of described quartzy still tube 9 in order to control described carrier gas, described destructive distillation device is also provided with pressure-regulator and the flow director of controlling carrier gas, the optional rare gas element of described carrier gas, and preferred argon gas.
Described ionic adsorption container 3 is 2 that are communicated with side by side, and is communicated with away from one end of described carrier gas admission port 10 with described quartzy still tube 9, and in it, is provided with the NaOH of 0.2M, for adsorbing the radioactivity of overflowing from quartzy still tube 9
124i ion.
The position of communicating pipe between described quartzy still tube 9 and described ionic adsorption container 3 is provided with the xeothermic well heater 7 for heating and thermal insulation, 200 ℃ of its set temperatures.
Described trap receptacle 2 is made up of thermal glass, and in container, is provided with soda-lime and charcoal for collecting remaining radioactivity
124i ion, and each soda-lime and the replaceable setting of charcoal.
Described surge pump 1 is for compressing the gas-holder of last waste gas to band shielding, until the nucleic in waste gas decay to there is no activity after again air draft in atmosphere, thereby prevented environmental pollution (because of
124i can not 100% be adsorbed above).Described destructive distillation device carries out
124the destructive distillation processing of I ion, and described surge pump 1 is provided with tail gas outlet 11 for discharging tail gas away from a side of described trap receptacle 2, and compress the gas-holder of last waste gas to band shielding, until the nucleic in waste gas decay to there is no activity after again air draft in atmosphere, thereby prevented environmental pollution.Pumping speed >=the 10L/min of described surge pump 1.
Following each embodiment utilizes above-mentioned destructive distillation device to carry out radioactivity
124the method that the destructive distillation of I ion is collected, specifically comprises:
(1) the tellurium target bead after practicing shooting is put into described quartzy still tube 9, and be fixed on target container protecting seat 5;
(2) open surge pump 1, it is 10L/min that its pumping speed is set, and air pressure is 8KPa; And regulate pressure-regulator and flow director, make carrier gas to make argon gas make argon gas enter described quartzy still tube 9 with the suitable pressure of the speed of 0.05MPa, 10L/min and speed with the speed of 0.05MPa, 10L/min, filter through quartzy filtering membrane 6, and gradually by emptying the air in pipe;
(3) now open xeothermic well heater 7, and 200 ℃ of its Heating temperatures are set;
(4) heater 4 now, controls to preset temp program;
(5) quartzy still tube 9 interior generations
124i ion distillation also keeps after temperature through xeothermic well heater 7, through two ionic adsorption containers 3 that 0.02MNaOH is housed, most during this time successively
124i ion all can be absorbed, and remaining
124i ion can be absorbed by soda-lime and charcoal wherein by trap receptacle 2, realizes
124whole efficient collection of I ion.
Preparation radioactivity described in the present embodiment
124the method of I ion, concrete steps are as follows:
A. the aluminium sesquioxide of getting 5mg joins in the refining tellurium powder of 90mg, stirs simultaneously, and being then pressed into thickness is 50mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed on magnetic resonance acceleator, by Te (p, n)
124i irradiation 2h, the p particle beam intensity of incident is 20 μ A, and energy is 20MeV, and the angle of incident is 6 °, and while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 6h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.25MPa, the air in the described quartzy still tube of dry helium gas displacement that the purity that flow velocity is 1000mL/min is 99.995%; The temperature of now controlling described quartzy still tube rises to 750 ℃ described tellurium target is heated, and prepares described radioactivity
124i ion is overflowed, and collects, and obtains radioactivity
124i ion.
Preparation radioactivity described in the present embodiment
124the method of I ion also comprises the step of preparing tellurium dioxide, and concrete steps are as follows:
A, get the tellurium powder of 80mg, add the 6M salpeter solution of 40mL to dissolve, described tellurium abundance >=99.0%;
B, to be neutralized to pH to the ammonium hydroxide that adds liquefaction in the lysate obtaining in above-mentioned steps A be 6.5, with solution described in post-heating to dry;
C, to get concentration be that the concentrated hydrochloric acid 15mL of 12M redissolves dried residue in above-mentioned steps;
D, again take liquefying hydrogen ammonium oxide, the solution after described redissolution is neutralized to pH as 6.5, with solution described in post-heating until approach boiling, and be 15% Hexamine solution to dripping mass concentration in solution, make tellurium dioxide precipitation, placement is filtered after spending the night, get solid dry at 150 ℃, obtain described tellurium dioxide.
Preparation radioactivity described in the present embodiment
124the method of I ion, concrete steps are as follows:
A. the aluminium sesquioxide of getting 4mg joins in tellurium dioxide powder prepared by 88mg, mixes, and being then pressed into thickness is 60mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed on magnetic resonance acceleator, by Te (p, n)
124i irradiation 3h, the p particle beam intensity of incident is 18 μ A, and energy is 18.5MeV, and the angle of incident is 10 °, and while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 4h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.35MPa, the purity that flow velocity is 500mL/min is the air in the described quartzy still tube of 99.99% dry argon gas displacement; The temperature of now controlling described quartzy still tube rises to 750 ℃ described tellurium target is heated, and prepares described radioactivity
124i ion is overflowed, and collects, and obtains radioactivity
124i ion.
Embodiment 3
Preparation radioactivity described in the present embodiment
124the method of I ion, concrete steps are as follows:
A. the aluminium sesquioxide of getting 5mg joins in the refining tellurium dioxide powder of 100mg, mix, and to be pressed into thickness is 55mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed in to magnetic resonance acceleator, by Te (p, n)
124i irradiation 2.5h, wherein, the p particle beam intensity of incident is 19 μ A, and energy is 19MeV, and the angle of incident is 8
°, while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 5h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.3MPa, the air in the described quartzy still tube of dry neon displacement that the purity that flow velocity is 800mL/min is 99.995%; The temperature of now controlling described quartzy still tube rises to 750 ℃ described tellurium target is heated, the step of the quartzy still tube intensification of described control specifically comprises: control temperature rises to 110 ℃ of maintenance 9min, control temperature rises to 440 ℃ and keeps 9min, control temperature to rise to 590 ℃ of maintenance 2min, and in the time that the actual temperature of described quartzy still tube reaches 700 ℃, stop heating up, prepare described radioactivity
124i ion is overflowed, described radioactivity
124i ion absorbs by the NaOH solution of 0.02M, remaining radioactivity
124i ion adsorbs by the mixture of soda-lime and charcoal, obtains radioactivity
124i ion.
Embodiment 4
Preparation radioactivity described in the present embodiment
124the method of I ion also comprises the step of preparing tellurium dioxide, and concrete steps are as follows:
A, get the tellurium powder of 120mg, add the 6M salpeter solution of 60mL to dissolve, described tellurium abundance >=99.0%;
B, to be neutralized to pH to the ammonium hydroxide that adds liquefaction in the lysate obtaining in above-mentioned steps A be 7.5, with solution described in post-heating to dry;
C, to get concentration be that the concentrated hydrochloric acid 20mL of 12M redissolves dried residue in above-mentioned steps;
D, again take liquefying hydrogen ammonium oxide, the solution after described redissolution is neutralized to pH as 7.5, with solution described in post-heating until approach boiling, and be 25% Hexamine solution to dripping mass concentration in solution, make tellurium dioxide precipitation, placement is filtered after spending the night, get solid dry at 150 ℃, obtain described tellurium dioxide.
Preparation radioactivity described in the present embodiment
124the method of I ion, concrete steps are as follows:
A. the aluminium sesquioxide of getting 5mg joins in tellurium dioxide powder prepared by 100mg, mix, and to be pressed into thickness is 55mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed in to magnetic resonance acceleator, by Te (p, n)
124i irradiation 2.5h, wherein, the p particle beam intensity of incident is 19 μ A, and energy is 19MeV, and the angle of incident is 8 °, and while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 5h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.3MPa, the air in the described quartzy still tube of dry argon gas displacement that the purity that flow velocity is 800mL/min is 99.9999%; The temperature of now controlling described quartzy still tube rises to 750 ℃ described tellurium target is heated, the step of the quartzy still tube intensification of described control specifically comprises: control temperature rises to 130 ℃ of maintenance 11min, control temperature rises to 460 ℃ and keeps 11min, control temperature to rise to 610 ℃ of maintenance 4min, and in the time that the actual temperature of described quartzy still tube reaches 720 ℃, stop heating up, prepare described radioactivity
124i ion is overflowed, described radioactivity
124i ion absorbs by the NaOH solution of 0.02M, remaining radioactivity
124i ion adsorbs by the mixture of soda-lime and charcoal, obtains radioactivity
124i ion.
Embodiment 5
Preparation radioactivity described in the present embodiment
124the method of I ion also comprises the step of preparing tellurium dioxide, and concrete steps are as follows:
A, get the tellurium powder of 100mg, add the 6M salpeter solution of 50mL to dissolve, described tellurium abundance >=99.0%;
B, to be neutralized to pH to the ammonium hydroxide that adds liquefaction in the lysate obtaining in above-mentioned steps A be 7, with solution described in post-heating to dry;
C, to get concentration be that the concentrated hydrochloric acid 18mL of 12M redissolves dried residue in above-mentioned steps;
D, again take liquefying hydrogen ammonium oxide, the solution after described redissolution is neutralized to pH as 7, with solution described in post-heating until approach boiling, and be 20% Hexamine solution to dripping mass concentration in solution, make tellurium dioxide precipitation, placement is filtered after spending the night, get solid dry at 150 ℃, obtain described tellurium dioxide.
Preparation radioactivity described in the present embodiment
124the method of I ion, concrete steps are as follows:
A. the aluminium sesquioxide of getting 5mg joins in tellurium dioxide powder prepared by 100mg, mix, and to be pressed into thickness is 55mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed in to magnetic resonance acceleator, by Te (p, n)
124i irradiation 2.5h, wherein, the p particle beam intensity of incident is 19 μ A, and energy is 19MeV, and the angle of incident is 8 °, and while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 5h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.3MPa, the air in the described quartzy still tube of dry argon gas displacement that the purity that flow velocity is 800mL/min is 99.9999%; The temperature of now controlling described quartzy still tube rises to 750 ℃ described tellurium target is heated, the step of the quartzy still tube intensification of described control specifically comprises: control temperature rises to 120 ℃ of maintenance 10min, control temperature rises to 450 ℃ and keeps 10min, control temperature to rise to 600 ℃ of maintenance 3min, and in the time that the actual temperature of described quartzy still tube reaches 710 ℃, stop heating up, prepare described radioactivity
124i ion is overflowed, described radioactivity
124i ion absorbs by the NaOH solution of 0.02M, remaining radioactivity
124i ion adsorbs by the mixture of soda-lime and charcoal, obtains radioactivity
124i ion.
Preparation radioactivity described in the present embodiment
124the method of I ion also comprises the step of preparing tellurium dioxide, and concrete steps are as follows:
A, get the tellurium powder of 100mg, add the 6M salpeter solution of 50mL to dissolve, described tellurium abundance >=99.0%;
B, to be neutralized to pH to the ammonium hydroxide that adds liquefaction in the lysate obtaining in above-mentioned steps A be 7, with solution described in post-heating to dry;
C, to get concentration be that the concentrated hydrochloric acid 18mL of 12M redissolves dried residue in above-mentioned steps;
D, again take liquefying hydrogen ammonium oxide, the solution after described redissolution is neutralized to pH as 7, with solution described in post-heating until approach boiling, and be 20% Hexamine solution to dripping mass concentration in solution, make tellurium dioxide precipitation, placement is filtered after spending the night, get solid dry at 150 ℃, obtain described tellurium dioxide.
Preparation radioactivity described in the present embodiment
124the method of I ion, concrete steps are as follows:
A. the aluminium sesquioxide of getting 5mg joins in tellurium dioxide powder prepared by 100mg, mix, and to be pressed into thickness is 55mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed in to magnetic resonance acceleator, by Te (p, n)
124i irradiation 2.5h, wherein, the p particle beam intensity of incident is 19 μ A, and energy is 19MeV, and the angle of incident is 8 °, and while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 5h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.3MPa, the air in the described quartzy still tube of dry argon gas displacement that the purity that flow velocity is 800mL/min is 99.9999%; The temperature of now controlling described quartzy still tube rises to 750 ℃ described tellurium target is heated, the step of the quartzy still tube intensification of described control specifically comprises: control temperature rises to 100 ℃ of maintenance 13min, control temperature rises to 430 ℃ and keeps 11min, control temperature to rise to 550 ℃ of maintenance 5min, and in the time that the actual temperature of described quartzy still tube reaches 740 ℃, stop heating up, prepare described radioactivity
124i ion is overflowed, described radioactivity
124i ion absorbs by the NaOH solution of 0.02M, remaining radioactivity
124i ion adsorbs by the mixture of soda-lime and charcoal, obtains radioactivity
124i ion.
Embodiment 7
Preparation radioactivity described in the present embodiment
124the method of I ion, concrete steps are as follows:
A. the aluminium sesquioxide of getting 5mg joins in tellurium dioxide powder prepared by 100mg, mix, and to be pressed into thickness is 55mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed in to magnetic resonance acceleator, by Te (p, n)
124i irradiation 2.5h, wherein, the p particle beam intensity of incident is 19 μ A, and energy is 19MeV, and the angle of incident is 8 °, and while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 5h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.3MPa, the air in the described quartzy still tube of dry argon gas displacement that the purity that flow velocity is 800mL/min is 99.9999%; The temperature of now controlling described quartzy still tube rises to 750 ℃ described tellurium target is heated, the step of the quartzy still tube intensification of described control specifically comprises: control temperature rises to 135 ℃ of maintenance 7min, control temperature rises to 480 ℃ and keeps 5min, control temperature to rise to 645 ℃ of maintenance 1min, and in the time that the actual temperature of described quartzy still tube reaches 685 ℃, stop heating up, prepare described radioactivity
124i ion is overflowed, described radioactivity
124i ion absorbs by the NaOH solution of 0.02M, remaining radioactivity
124i ion adsorbs by the mixture of soda-lime and charcoal, obtains radioactivity
124i ion.
Effect example
Below by the effect example radioactivity that better explanation embodiment of the present invention 1-7 prepares
124the yield of I ion and the rate of recovery.
1. measuring method
The measuring method of yield: adopt activity meter CRC-25R to measure.
The measuring method of the rate of recovery: record total amount R with activity meter after nuclear reaction
always, then survey activity R by collect the NaI solution obtaining with NaOH
naI, the calculation formula of the rate of recovery is R
naI/ R
always.
2. measurement result
The measurement result of embodiment of the present invention 1-7 sees the following form.
| Sequence number | Yield (mCi) | The rate of recovery (%) |
| |
63 | 74 |
| |
67 | 75 |
| Embodiment 3 | 96 | 87 |
| Embodiment 4 | 97 | 88 |
| Embodiment 5 | 100 | 90 |
| |
94 | 84 |
| Embodiment 7 | 93 | 83 |
As seen from the above table, the embodiment of the present invention 5 is prepared radioactivity
124the yield of I ion, the rate of recovery are all significantly higher than other embodiment and prepare radioactivity
124the yield of I ion, the rate of recovery, embodiment 3-4 prepares radioactivity
124the yield of I ion, the preparation radioactivity that the rate of recovery is all significantly higher than embodiment 6-7
124the yield of I ion, the rate of recovery, embodiment 3-7 prepares radioactivity
124the yield of I ion, the preparation radioactivity that the rate of recovery is all significantly higher than embodiment 1-2
124the yield of I ion, the rate of recovery.Draw thus, the present invention prepares radioactivity
124i ion method has that yield is high, the high remarkable technique effect of the rate of recovery.
Obviously, above-described embodiment is only for example is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all embodiments.And the apparent variation of being extended out thus or variation are still among the protection domain in the invention.
Claims (10)
1. prepare radioactivity for one kind
124the method of I ion, is characterized in that, comprises the steps:
A. get aluminium sesquioxide and the tellurium dioxide powder that mass ratio is 1:18-22 and mix, and to be pressed into thickness be 50-60mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed in to magnetic resonance acceleator, by Te (p, n)
124i irradiation 2-3h, wherein, the p particle beam intensity of incident is 18-20 μ A, and energy is 18.5-20MeV, and the angle of incident is 6-10 °, and while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 4-6h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.25-0.35MPa, the air in the described quartzy still tube of the dry carrier gas displacement of high purity that flow velocity is 500-1000mL/min; The temperature of now controlling described quartzy still tube rises to 750 ℃ described tellurium target is heated, and prepares described radioactivity
124i ion is overflowed, and collects, and to obtain final product.
2. preparation radioactivity according to claim 1
124the method of I ion, is characterized in that, comprises the steps:
A. get aluminium sesquioxide and the tellurium dioxide powder that mass ratio is 1:20 and mix, and to be pressed into thickness be 55mg/cm
2tellurium target, for subsequent use;
B. the tellurium target of above-mentioned preparation is placed in to magnetic resonance acceleator, by Te (p, n)
124i irradiation 2.5h, wherein, the p particle beam intensity of incident is 19 μ A, and energy is 19MeV, and the angle of incident is 8 °, and while water carries out cooling to the tellurium target in irradiation, after irradiation finishes, tellurium target is placed to cooling 5h;
C. get the quartzy still tube that above-mentioned cooled tellurium target is placed in destructive distillation device, and take air pressure as 0.3MPa, the air in the described quartzy still tube of the dry carrier gas displacement of high purity that flow velocity is 800mL/min; The temperature of controlling subsequently described quartzy still tube rises to 750 ℃ described tellurium target is heated, and prepares described radioactivity
124i ion is overflowed, and collects, and to obtain final product.
3. preparation radioactivity according to claim 1 and 2
124the method of I ion, is characterized in that:
In described step c, the step of the quartzy still tube intensification of described control specifically comprises: control temperature rises to 110-130 ℃ of maintenance 9-11min, control temperature rises to 440-460 ℃ and keeps 9-11min, control temperature to rise to 590-610 ℃ of maintenance 2-4min, and in the time that the actual temperature of described quartzy still tube reaches 700-720 ℃, stops intensification.
4. preparation radioactivity according to claim 3
124the method of I ion, is characterized in that:
In described step c, the step of the quartzy still tube intensification of described control specifically comprises: control temperature rises to 120 ℃ of maintenance 10min, control temperature rises to 450 ℃ and keeps 10min, control temperature to rise to 600 ℃ of maintenance 3min, and in the time that the actual temperature of described quartzy still tube reaches 710 ℃, stops intensification.
5. according to the arbitrary described preparation radioactivity of claim 1-4
124the method of I ion, is characterized in that:
In described step c, described collection radioactivity
124the step of I ion, comprises and controls described radioactivity
124the step that I ion absorbs by the NaOH solution of 0.02M.
6. preparation radioactivity according to claim 5
124the method of I ion, is characterized in that:
In described step c, described collection radioactivity
124after the step of I ion is also included in NaOH solution and absorbs, by remaining radioactivity
124the step that I ion adsorbs by the mixture of soda-lime and charcoal.
7. according to the arbitrary described preparation radioactivity of claim 1-6
124the method of I ion, is characterized in that:
In described step c, described carrier gas is helium, argon gas or the neon of purity more than 99.99%.
8. according to the arbitrary described preparation radioactivity of claim 1-7
124the method of I ion, is characterized in that, before described step a, also comprises the step of preparing described tellurium dioxide, specifically comprises:
A, get the tellurium powder of 8-12 weight part, add the 6M salpeter solution of 40-60 parts by volume to dissolve, described tellurium abundance >=99.0%;
B, to be neutralized to pH to the ammonium hydroxide that adds liquefaction in the lysate obtaining in above-mentioned steps A be 6.5-7.5, with solution described in post-heating to dry;
C, the concentrated hydrochloric acid 15-20 parts by volume of getting 12M are redissolved dried residue in above-mentioned steps;
D, again with liquefying hydrogen ammonium oxide, the solution after described redissolution is neutralized to pH6.5-7.5, with solution described in post-heating until approach boiling, and drip the Hexamine solution that mass concentration is 15-25% in solution, make tellurium dioxide precipitation, placement is filtered after spending the night, get solid dry at 150 ℃, obtain described tellurium dioxide.
9. preparation radioactivity according to claim 8
124the method of I ion, is characterized in that, the step of the described tellurium dioxide of described preparation, specifically comprises:
A, get the tellurium powder of 10 weight parts, add the 6M salpeter solution of 50 parts by volume to dissolve, described tellurium abundance >=99.0%;
B, to be neutralized to pH to the ammonium hydroxide that adds liquefaction in the lysate obtaining in above-mentioned steps A be 7, with solution described in post-heating to dry;
C, concentrated hydrochloric acid 18 parts by volume of getting 12M are redissolved dried residue in above-mentioned steps;
D, again take liquefying hydrogen ammonium oxide, the solution after described redissolution is neutralized to pH as 7, with solution described in post-heating until approach boiling, and be 20% Hexamine solution to dripping mass concentration in solution, make tellurium dioxide precipitation, placement is filtered after spending the night, get solid dry at 150 ℃, obtain described tellurium dioxide.
10. the radioactivity preparing according to the arbitrary described method of claim 1-9
124i ion.
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| CN104512913A (en) * | 2015-01-26 | 2015-04-15 | 中国工程物理研究院核物理与化学研究所 | Horizontal high-concentration Na<131>I production device |
| CN104528653A (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 | Vertical type Na131I dry distillation production device |
| 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 |
| CN104528652A (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 | Vertical type Na131I dry distillation production device |
| CN104575650A (en) * | 2015-01-26 | 2015-04-29 | 中国工程物理研究院核物理与化学研究所 | Radioactive iodine-131 steam treatment set |
| CN104616711A (en) * | 2015-01-26 | 2015-05-13 | 中国工程物理研究院核物理与化学研究所 | Self-discharging horizontal type Na131I production device |
| CN104616712A (en) * | 2015-01-26 | 2015-05-13 | 中国工程物理研究院核物理与化学研究所 | Vertical type production unit for high-concentration Na131I solution |
| CN104700916A (en) * | 2015-03-16 | 2015-06-10 | 中国工程物理研究院核物理与化学研究所 | Self discharging vertical type Na131I production device |
| CN106653134A (en) * | 2017-01-22 | 2017-05-10 | 中国核动力研究设计院 | Preparation method for carrier-free phosphorus 32 |
| CN108573321A (en) * | 2017-03-10 | 2018-09-25 | 美国西门子医疗解决公司 | The production of radiopharmaceutical |
| CN108654377A (en) * | 2018-07-18 | 2018-10-16 | 中国工程物理研究院核物理与化学研究所 | A kind of ventilation type Na131I preparation destructive distillation devices |
| CN108686608A (en) * | 2018-07-18 | 2018-10-23 | 中国工程物理研究院核物理与化学研究所 | Bushing type I-131 destructive distillation absorbers |
| CN110444312A (en) * | 2019-09-03 | 2019-11-12 | 中国科学院近代物理研究所 | Medical-isotope is separated from uranium fission product using cracking process131I |
| CN113877421A (en) * | 2021-08-20 | 2022-01-04 | 苏州爱索拓普智能科技有限公司 | Medical isotope separation and purification process |
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| CN106653134A (en) * | 2017-01-22 | 2017-05-10 | 中国核动力研究设计院 | Preparation method for carrier-free phosphorus 32 |
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| CN108654377B (en) * | 2018-07-18 | 2023-04-18 | 中国工程物理研究院核物理与化学研究所 | Air-cooled Na 131 Dry distillation device for I preparation |
| CN108686608B (en) * | 2018-07-18 | 2023-06-27 | 中国工程物理研究院核物理与化学研究所 | Sleeve type I-131 dry distillation absorber |
| CN110444312A (en) * | 2019-09-03 | 2019-11-12 | 中国科学院近代物理研究所 | Medical-isotope is separated from uranium fission product using cracking process131I |
| CN110444312B (en) * | 2019-09-03 | 2020-12-29 | 中国科学院近代物理研究所 | Separation of medical isotopes from uranium fission products by dry distillation131Method of I |
| CN113877421A (en) * | 2021-08-20 | 2022-01-04 | 苏州爱索拓普智能科技有限公司 | Medical isotope separation and purification process |
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