CN111500861A - Method for extracting technetium from neutral molybdenum solution by using activated carbon fiber - Google Patents

Method for extracting technetium from neutral molybdenum solution by using activated carbon fiber Download PDF

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CN111500861A
CN111500861A CN202010261503.XA CN202010261503A CN111500861A CN 111500861 A CN111500861 A CN 111500861A CN 202010261503 A CN202010261503 A CN 202010261503A CN 111500861 A CN111500861 A CN 111500861A
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technetium
activated carbon
neutral
solution
molybdenum
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CN111500861B (en
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宋志浩
张蕴瀚
王宁
邓雪松
赵海龙
高翔
郭宏利
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Atom High Tech Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B61/00—Obtaining metals not elsewhere provided for in this subclass
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The invention discloses a method for extracting technetium from a neutral molybdenum solution by using activated carbon fibers, which comprises the following steps: (1) before molybdenum-technetium solution adsorption, washing the activated carbon fiber with water until effluent liquid is neutral; (2) preparing a neutral mixed solution containing molybdenum and technetium, wherein the mixed solution contains a high-concentration neutral salt compound; (3) adsorbing technetium in the molybdenum-technetium mixed solution obtained in the step (2) by using activated carbon fibers; (4) washing the molybdenum of the activated carbon fiber adhesive tape by using a washing solution; (5) the technetium adsorbed by the activated carbon fiber is desorbed by using a low-concentration leacheate or a leacheate without a neutral salt compound. The method has the following advantages: the solid phase separation material has good radiation resistance and low price and is easy to obtain; the obtained final solution containing technetium is neutral solution, and the preparation method is used for preparing the solution containing technetium99mTc]The subsequent process of the radiopharmaceutical does not require adjustment of the acidity of the solution.

Description

Method for extracting technetium from neutral molybdenum solution by using activated carbon fiber
Technical Field
The invention belongs to the field of radionuclide separation, and particularly relates to a method for extracting technetium from a neutral molybdenum solution by using activated carbon fibers.
Background
99Mo-99mTc generators were originally invented by Walter Tucker and Margret Greens in 1958 in an isotope project at the Brookhaven national laboratory. 80-85% of nuclear drugs used in medical imaging diagnosis in the world are used at present99mTc. The radioactive isotope is mainly from99mMother nuclide in Tc generator99β -decay of Mo.99Mo decays to99mThe efficiency of Tc is about 88.6%, the remaining 11.4% decays directly to99Tc。
99Mo-99mIn Tc Generator eluate99mThe concentration of Tc largely determines the image quality in Single Photon Emission Computed Tomography (SPECT) diagnostics and, therefore, in99Mo-99mIn the development of the Tc generator, it is known,99mthe concentration of Tc in the eluate is always the focus of most concern.
Due to different production methods99mFor use in Tc generators99The specific activity of Mo is different.
High specific activity at present99Mo (100-50000 Ci/g Mo) is obtained by uranium fission production. Fission in commercial use today99Mo-99mThe main component of the Tc generator is an acidic alumina column, using MoO4 2-The affinity with acid alumina is far greater than that of TcO4 -And (4) designing the characteristics of the light source. The generator can obtain the high technetium which meets the requirements of pharmacopoeia99mTc]Sodium acid injection. High specific activity in the world99Mo is mainly provided by reactors in the Netherlands, Belgium, France, south Africa, Australia and Russia, and is fissile when events such as reactor shutdown overhaul or decommissioning occur in major production countries99Mo supply may face a shortage.
Non-fission process production99Mo is usually represented by98Mo and100mo is used as a raw material and is obtained by irradiation or accelerator preparation by using a reactor. Prepared by non-fission processes99The Mo activity is low (1-10 Ci/g)Mo), non-radioactive Mo dominates the overwhelming majority. Loading Mo with low specific activity into normal fission99Mo-99mTc generator structure, obtained99mTc in the eluate99mThe Tc concentration is low and cannot meet the requirements of pharmacopoeia. Therefore, it is necessary to develop a low specific activity99Enrichment in Mo feed liquid99mTc.
Removing device99β of Mo-Decay to obtain99mTc, already realized by accelerators100Mo(p,2n)99mTc nuclear reaction preparation99mTc technique. Specific activity to99Extracting from Mo material liquid99mTc faces similar problems, accelerator preparation99mTc also requires extraction from feed solutions containing large amounts of nonradioactive Mo99mTc。
Therefore, how to get from low specific activity (< 10Ci/g Mo)99Separation and extraction of Mo99mTc is to solve fission99The key problem of Mo shortage.
Low specific activity99mThe Tc extraction techniques can be divided into four categories: solvent extraction, sublimation, electrochemical, and column chromatography. The key of the column chromatography is to use a solid phase material containing Mo and99madsorption in Tc solution99mTc, and no or little adsorption of Mo, thereby achieving separation of molybdenum and technetium. The method has the characteristics of easy automation realization, stability and reliability, and thus becomes a research hotspot.
In the prior art, Dowex-1 × 8, ABEC resin and activated carbon material are used as solid phase adsorption materials to separate molybdenum and technetium, wherein the Dowex-1 × 8 anion exchange resin used as the solid phase material for separating molybdenum and technetium needs to be leached by organic solvent or perchloric acid to desorb the technetium from the solid phase material, which presents a risk for clinical use, and the U.S. Food and Drug Administration (FDA) approves a novel molybdenum-technetium separation material using the ABEC resin in 2 months of 201899Mo-99mTc generator RadioGenix. The RadioGenix system uses potassium hydroxide to dissolve Mo, uses high concentration sodium hydroxide solution to wash Mo, and then uses buffer solution or diluted sodium hydroxide solution to wash Tc. Although high technetium [ alpha ] can be obtained in a high concentration99mTc]Sodium acid solution, but the required solution types are more in the separation process, and the operation is more complicated. In US2012090431, activated carbon material is used as separation material for molybdenum and technetium, the separation process is similar to that of the system of ABEC resin, also using alkaline sodium hydroxide solution as initial solution, followed by washing of Mo with sodium hydroxide solution, and finally obtaining high concentration by hot dilute lye rinsing or electrochemical method99mTc solution. Also, the separation process requires more types of solutions and is complicated to operate.
In CN106995882A, in the process of99In Mo solution99mTc is extracted by preparing the initial solution into sodium hydroxide solution, followed by sodium hydroxide solution99And (4) leaching Mo. For99Mo-99mNeutralization of the leacheate is required to separate Tc99mTc is used for radiopharmaceuticals. The equipment manufactured based on the separation method has a complex structure and the post-treatment process of the leacheate is complex.
Disclosure of Invention
In view of the problems in the background art, the present invention provides a method for extracting technetium from a neutral molybdenum solution using activated carbon fibers. The invention uses the pretreated activated carbon fiber as the solid phase separation material of molybdenum and technetium, and can adsorb technetium from the neutral mixed solution containing molybdenum and technetium, but does not adsorb or hardly adsorb molybdenum. The use of a neutral wash allows for the desorption of technetium, thereby effecting the separation of molybdenum and technetium.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for extracting technetium from a neutral molybdenum solution using activated carbon fibers, the method comprising the steps of:
(1) before molybdenum-technetium solution adsorption, washing activated carbon fibers with water until the acidity of effluent is neutral;
(2) preparing a neutral mixed solution containing molybdenum and technetium, wherein the mixed solution contains a neutral salt compound of which the mol/L is more than or equal to 1 mol;
(3) adsorbing technetium in the molybdenum-technetium mixed solution obtained in the step (2) by using activated carbon fibers;
(4) neutral salt compound solution with the concentration of more than or equal to 1 mol/L is used as washing liquid to wash molybdenum of the activated carbon fiber adhesive tape;
(5) the technetium adsorbed by the activated carbon fiber is desorbed by using a neutral salt compound solution of less than 1 mol/L or sterilized water for injection as an eluent.
As a preferable mode, in the step (1), the activated carbon fiber is any one or more of activated carbon fibers which are treated with alkali liquor, or treated with microwave heating after alkali liquor treatment, or not treated at all.
Preferably, in the step (1), the neutral pH is 5-8.
Preferably, in the step (2), the step (4) and the step (5), the pH of the neutral mixed solution is 5-8.
In a preferable embodiment, in the step (2), the neutral salt compound is a neutral salt compound containing sodium ions or potassium ions.
In a preferred embodiment, the neutral salt compound is selected from any one of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium nitrate, and potassium nitrate. For further purification of pertechnetate, the neutral salt compound is preferably inorganic salt containing chloride ions, such as sodium chloride or potassium chloride.
In a preferable embodiment, in the step (4), the neutral salt compound is a neutral salt compound containing sodium ions or potassium ions.
In a preferred embodiment, the neutral salt compound is selected from any one of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium nitrate, and potassium nitrate. For further purification of pertechnetate, the neutral salt compound is preferably inorganic salt containing chloride ions, such as sodium chloride or potassium chloride.
The leacheate can only use sodium chloride solution, so that the impurity content and the pollution chance are reduced.
In a preferable embodiment, in the step (5), the neutral salt compound is a neutral salt compound containing sodium ions or potassium ions.
In a preferred embodiment, the neutral salt compound is selected from any one of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium nitrate, and potassium nitrate. For further purification of pertechnetate, the neutral salt compound is preferably inorganic salt containing chloride ions, such as sodium chloride or potassium chloride.
Compared with the prior art, the invention has the following beneficial effects:
the method has the characteristics that the radiation resistance of the solid phase separation material is good, the adsorption separation performance is stable, and the solid phase separation material is low in price and easy to obtain; the resulting final technetium-containing solution is a neutral solution and adjustment of the acidity of the solution is not necessary in the subsequent process of preparing the technetium-containing radiopharmaceutical.
The essential feature of the application is that the activated carbon fiber is treated, and a material that adsorbs technetium in a neutral solution but does not adsorb molybdenum is screened and applied to separation of molybdenum and technetium. Based on this, the process is carried out99Mo-99mAt separation of Tc, contain99mTc eluates can be used for radiopharmaceuticals without neutralization (since injection solutions require neutrality and cannot be used directly if the eluates are basic). Thus, the processing process flow and the device structure can be simplified in practical application. Therefore, there is a certain advantage to extracting technetium directly from neutral molybdenum solutions, as compared to extracting technetium from alkaline molybdenum-containing solutions.
Detailed Description
The specific embodiment of the invention provides a method for extracting technetium from a neutral molybdenum solution by using activated carbon fibers, which comprises the following steps:
(1) before molybdenum-technetium solution adsorption, activated carbon fibers were rinsed with water until the effluent acidity was neutral.
The activated carbon fiber is a mixture of the activated carbon fiber, which is treated by alkali liquor, or subjected to microwave heating treatment after alkali liquor treatment, or not subjected to any treatment in any proportion. Through alkali liquor treatment and microwave treatment, the activated carbon fiber used in the invention has the following characteristics: in a static adsorption experiment, the activated carbon fiber can adsorb a certain amount of molybdate ions in a strong acid solution, and shows a repulsive action to the molybdate ions in a solution with the pH value of more than 5, so that the molybdate ions are not adsorbed. Because the surface of the activated carbon fiber has alkaline groups, in order to ensure the smooth separation operation, a certain amount of water is needed to wash the activated carbon fiber until the effluent liquid is neutral. The specific operation can be to prepare the activated carbon into a chromatographic column, inject neutral water into the chromatographic column by using a syringe or a peristaltic pump for washing, and detect the acidity of effluent by using a pH test paper until the effluent is neutral.
(2) A neutral mixed solution containing molybdenum and technetium is prepared, and the mixed solution contains a high-concentration neutral salt compound.
The molybdenum should be present as molybdate and the technetium as pertechnetate. The ionic strength of the mixed solution can affect the adsorption of pertechnetate ions by the activated carbon fibers. Experiments show that in the solution with high ionic strength, the activated carbon fiber has stronger adsorption capacity to pertechnetate, and pertechnetate ions can not be easily eluted; in the low ionic strength solution, the activated carbon fiber has weak adsorption capacity to pertechnetate, and pertechnetate ions can be easily eluted. For further purification of pertechnetate, the neutral salt compound is preferably inorganic salt containing chloride ions, such as sodium chloride or potassium chloride.
(3) And (3) adsorbing technetium in the mixed solution of molybdenum and technetium obtained in the step (2) by using activated carbon fibers.
This step can use a dynamic method to separate the mixed solution of molybdenum and technetium. The activated carbon fiber with certain mass is used to prepare a chromatographic column for dynamic adsorption separation of molybdenum and technetium. The mixed solution of molybdenum and technetium is pumped through the activated carbon chromatography column at a flow rate, for example, using a peristaltic pump or a syringe pump, such that technetium in the mixed solution of molybdenum and technetium is adsorbed on the activated carbon chromatography column, while molybdenum is not adsorbed or is minimally adsorbed on the chromatography column. A large number of99Mo flows out after passing through the color layer column99Decay daughter of Mo99mRepeating the procedure after Tc formation, and separating the molybdenum-technetium again to obtain99mTc。
(4) And washing the molybdenum adhered to the activated carbon fiber by using a washing solution.
The activated carbon fiber surface adsorbed with technetium will have some molybdenum adhered to it, which can be removed by a washing liquid while ensuring that the adsorbed technetium is not desorbed. For activated carbon fibers that adsorb technetium using dynamic adsorption, a certain volume of wash solution can be pumped through. The washing solution may have similar composition to that of the neutral mixed solution prepared in step (2).
(5) The technetium adsorbed by the activated carbon fiber is desorbed by using a low-concentration leacheate or a leacheate without a neutral salt compound.
The activated carbon fiber for adsorbing technetium by dynamic adsorption method can be desorbed by pumping a certain volume of leacheate to obtain technetium-containing solution.
To facilitate a further understanding of the invention, the following examples are provided to illustrate it in more detail. These embodiments are merely illustrative and not restrictive of the scope or principles of the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principles of the embodiments of the invention are intended to be included within the scope of the invention.
Example 1
Preparing chromatographic column from 0.5g of activated carbon fiber treated by alkali liquor, injecting water for injection by using a syringe to wash the prepared activated carbon fiber column until the pH of effluent liquid is 6, preparing 10ml of solution with the sodium chloride concentration of 1 mol/L and the sodium molybdate concentration of 1 mol/L, and adding 10mCi99Mo-99mThe mixed solution containing molybdenum and technetium was pumped through the chromatographic column at a flow rate of 10m L/min to recover a molybdenum-containing effluent, technetium was adsorbed on the chromatographic column, sodium chloride solution of 40m L1 mol/L was used to pump through the chromatographic column at a flow rate of 10m L/min to wash a small amount of molybdenum adhering thereto, and finally, 10m L sterilized water for injection was pumped at a flow rate of 10m L/min to elute technetium on the column.
Example 2
Taking 0.5g of active carbon fiber treated by alkali liquor and then treated by microwave to preparePreparing color layer column, injecting water for injection by syringe to wash the prepared activated carbon fiber column until the pH of effluent is 7, preparing 10ml of solution with potassium chloride concentration of 1.2 mol/L and sodium molybdate concentration of 1 mol/L, and adding 10mCi99Mo-99mThe mixed solution containing molybdenum and technetium was pumped through the chromatographic column at a flow rate of 10m L/min to recover a molybdenum-containing effluent, technetium was adsorbed on the chromatographic column, sodium chloride solution of 40m L1 mol/L was used to pump through the chromatographic column at a flow rate of 10m L/min to wash a small amount of molybdenum adhering thereto, and finally, 5m L sterilized water for injection was pumped at a flow rate of 10m L/min to elute technetium on the column.
Example 3
Preparing a chromatographic column from 0.3g of activated carbon fiber treated by alkali liquor and 0.2g of untreated activated carbon fiber, injecting injection water by using a syringe to wash the prepared activated carbon fiber column until the pH of an effluent is 7, preparing 10ml of solution with the concentration of 1.1 mol/L and the concentration of 1 mol/L of potassium chloride, and adding 9.5mCi99Mo-99mThe mixed solution containing molybdenum and technetium was pumped through the chromatographic column at a flow rate of 8m L/min to recover a molybdenum-containing effluent, whereupon technetium was adsorbed on the chromatographic column, a 30m L1 mol/L potassium chloride solution was used to pump through the chromatographic column at a flow rate of 10m L/min to wash a small amount of molybdenum adhering thereto, and finally, 5m L0.9.9% sodium chloride injection was pumped at a flow rate of 10m L/min to elute technetium on the column.
Example 4
Preparing a chromatographic column from 0.5g of untreated activated carbon fiber, injecting water for injection by using a syringe to wash the prepared activated carbon fiber column until the pH of an effluent is 5, preparing 10ml of solution with the concentration of 1 mol/L of sodium sulfate and the concentration of 1 mol/L of sodium molybdate, and adding 10mCi99Mo-99mThe mixed solution containing molybdenum and technetium was pumped through a chromatographic column at a flow rate of 10m L/min to recover a molybdenum-containing effluent, whereupon technetium was adsorbed on the chromatographic column, 40m L1 mol/L of sulfur was usedAnd pumping the sodium solution through the chromatographic column at the flow rate of 10m L/min to wash a small amount of molybdenum adhered to the solution, finally, pumping the sodium sulfate injection of 5m L0.02.02 mol/L at the flow rate of 10m L/min to elute technetium on the column, wherein the obtained eluent is the solution containing technetium, and the separation of molybdenum and technetium is completed.
Example 5
Preparing chromatographic column from 0.5g of activated carbon fiber treated by alkali liquor, injecting water for injection by using a syringe to wash the prepared activated carbon fiber column until the pH of effluent is 8, preparing 10ml of solution with the potassium nitrate concentration of 1.1 mol/L and the sodium molybdate concentration of 1 mol/L, and adding 10mCi into the solution99Mo-99mThe mixed solution containing molybdenum and technetium was pumped through the chromatographic column at a flow rate of 10m L/min to recover a molybdenum-containing effluent, technetium was adsorbed on the chromatographic column, potassium nitrate solution 40m L1.1.1 mol/L was used and pumped through the chromatographic column at a flow rate of 10m L/min to wash a small amount of molybdenum stuck thereon, and finally, potassium nitrate solution 5m L0.01.01 mol/L was pumped at a flow rate of 10m L/min to elute technetium on the column.
TABLE 1 residue of molybdenum in leacheate obtained in different examples
Group of Mo residue in leacheate
Example 1 Not detected out
Example 2 1.0μg/mL
Example 3 1.3μg/mL
Example 4 3.3μg/ml
Example 5 Not detected out

Claims (9)

1. A method for extracting technetium from a neutral molybdenum solution using activated carbon fibers, the method comprising the steps of:
(1) before molybdenum-technetium solution adsorption, washing activated carbon fibers with water until the acidity of effluent is neutral;
(2) preparing a neutral mixed solution containing molybdenum and technetium, wherein the mixed solution contains a neutral salt compound of which the mol/L is more than or equal to 1 mol;
(3) adsorbing technetium in the molybdenum-technetium mixed solution obtained in the step (2) by using activated carbon fibers;
(4) neutral salt compound solution with the concentration of more than or equal to 1 mol/L is used as washing liquid to wash molybdenum of the activated carbon fiber adhesive tape;
(5) the technetium adsorbed by the activated carbon fiber is desorbed by using a neutral salt compound solution of less than 1 mol/L or sterilized water for injection as an eluent.
2. The method for extracting technetium from a neutral molybdenum solution using activated carbon fiber according to claim 1, wherein in the step (1), the activated carbon fiber is any one or more of activated carbon fiber treated with alkali solution, or treated with microwave heating after alkali solution treatment, or not treated at all.
3. The method for extracting technetium from a neutral molybdenum solution using activated carbon fiber according to claim 1, wherein the neutral pH is 5 to 8 in the step (1), the step (2), the step (4) and the step (5).
4. The method for extracting technetium from a neutral molybdenum solution using activated carbon fiber according to claim 1, wherein in the step (2), the neutral salt compound is a neutral salt compound containing sodium ions or potassium ions.
5. The method for extracting technetium from a neutral molybdenum solution using activated carbon fiber according to claim 4, wherein the neutral salt-type compound is any one selected from the group consisting of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium nitrate and potassium nitrate.
6. The method for extracting technetium from a neutral molybdenum solution using activated carbon fiber according to claim 1, wherein in the step (4), the neutral salt compound is a neutral salt compound containing sodium ion or potassium ion.
7. The method for extracting technetium from a neutral molybdenum solution using activated carbon fiber according to claim 6, wherein the neutral salt-type compound is any one selected from the group consisting of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium nitrate and potassium nitrate.
8. The method for extracting technetium from a neutral molybdenum solution using activated carbon fiber according to claim 1, wherein in the step (5), the neutral salt compound is a neutral salt compound containing sodium ion or potassium ion.
9. The method for extracting technetium from a neutral molybdenum solution using activated carbon fiber according to claim 8, wherein the neutral salt-type compound is any one selected from the group consisting of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium nitrate and potassium nitrate.
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