CN105037616A - Method for preparing radioactive source by microemulsion polymerization - Google Patents
Method for preparing radioactive source by microemulsion polymerization Download PDFInfo
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- CN105037616A CN105037616A CN201510317469.2A CN201510317469A CN105037616A CN 105037616 A CN105037616 A CN 105037616A CN 201510317469 A CN201510317469 A CN 201510317469A CN 105037616 A CN105037616 A CN 105037616A
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Abstract
The invention discloses a method for preparing a radioactive source by microemulsion polymerization. The method comprises the following steps: preparing a polymerizable monomer, a cosurfactant, a radioactive liquid, an initiator, an accelerator and the like into a microemulsion system, sealing the microemulsion into a mold, and carrying out polymerization reaction. The method is simple, forms the homogeneous microemulsion at normal temperature by using the polymerizable monomer and radionuclide-containing water solution, and has the advantage of uniform radionuclide distribution. The microemulsion is low in viscosity, can be conveniently filled into the corresponding mold, and is convenient to operate. The reaction system is sealed on the corresponding mold, so the polymerization reaction temperature is lower, and the reaction process can not cause pollution. The formed high-polymer polymerisate has the advantages of high strength, favorable toughness and high radioresistance.
Description
Technical field
The invention belongs to radioactive source preparation field, be specifically related to a kind of method that micro-emulsion polymerization prepares radioactive source.
Background technology
Nuclear technique has important application at the numerous areas such as industry, agricultural, medical science, national defence, scientific research, and the ray applications technology wherein based on radioactive source is a very important aspect.Such as industrial flow monitoring, industrial flaw detection
137cs source etc.; For agriculture mutation breeding, sick worm anti-evil
60co source etc.; For therapeutic treatment tumour
125i source etc.; For smoke detector
241am source etc.Current available radionuclide reaches hundred kinds, and radioactive source reaches more than 1500 and plants.The preparation of radioactive source adopts electrochemical process (plating, electroless plating etc.), silicate technology (pottery, enamel, glass etc.), powder metallurgical technique, direct activation technique etc. mostly.Electrochemical process utilizes the electrochemical properties of impressed voltage or electrolyte solution self that radionuclide ion is moved in electrolyte solution, and finally in cathode surface reduction deposition.Electrochemical process is generally used for the preparation being easy to the metal nucleic radioactive source participating in redox reaction.Silicate technology the oxide compound of radionuclide and enamel, pottery, frit and other auxiliary materials is mixed and compression moulding, and the silicate formed containing radionuclide by high temperature sintering is active fast.Be generally used in silicate technology and easily make oxide compound and resistant to elevated temperatures radionuclide.Powder metallurgical technique is by radioactive substance salify (carbonate, phosphoric acid salt etc.), and the metal-powder (gold and silver etc.) good with ductility is blended evenly and compression moulding, forms goods through sintering, finally can rolling, be die-cut into and need shape.The same with silicate technology, powder metallurgical technique is comparatively complicated, not easy to operate.Direct activation method is first made by raw material to need form, obtains required radionuclide after then putting into reactor irradiation.This method needs reactor, uses inconvenience, and due to side reaction, impurity species is generally more.
In view of above-mentioned defect, creator of the present invention obtains the present invention finally through long research and practice.
Summary of the invention
(1) goal of the invention
The object of the invention is a kind of method preparing radioactive source in order to develop micro-emulsion polymerization.
(2) technical scheme
For achieving the above object, the invention provides following technical scheme:
Micro-emulsion polymerization prepares a method for radioactive source, comprises the following steps successively:
(1) polymerization single polymerization monomer, cosurfactant, radioactivity feed liquid are configured to microemulsion, filling with inert gas is vented; Add initiator and dissolve mixing, filling with inert gas exhaust again; Add linking agent and promotor mixes.
(2) microemulsion system is encapsulated in pressure vessel mould.
(3) leave standstill, make microemulsion carry out polyreaction.
In step (1), the polymerization single polymerization monomer of composition microemulsion is methyl methacrylate (MMA), methacrylic acid (MA), acrylamide (AM) etc., content 15-80wt%; The cosurfactant of composition microemulsion is hydroxyethyl methylacrylate (HEMA), vinylformic acid (AA), dimethylaminoethyl acrylate methyl ammonia ethyl ester (DM) etc., content 15-80wt%; Radioactivity feed liquid (including radionuclide) the content 1-10wt% of composition microemulsion; The initiator added is benzoyl peroxide (BPO), Diisopropyl azodicarboxylate (AIBN), Potassium Persulphate-S-WAT (KPS-SH) etc., and addition is the 0.2-1wt% of microemulsion; The linking agent added is Vinylstyrene (DVB), N-hydroxymethylacrylate acid amides (HAM), dicumyl peroxide (DCP) etc., and addition is the 0-2wt% of microemulsion; The promotor added is N, N-dimethyl-p-toluidine (DMT), to toluenesulfinic acid (TSA) etc., addition is the 0-0.5wt% of microemulsion; .
Preferred situation:
(1) methyl methacrylate (content is 25wt%), hydroxyethyl methylacrylate (content is 70wt%), radioactivity feed liquid (content is 5wt%) are configured to microemulsion, filling with inert gas is vented; Add benzoyl peroxide (content is the 0.5wt% of microemulsion) and dissolve mixing, filling with inert gas is vented; Add Vinylstyrene (content is the 1wt% of microemulsion) and N, N-dimethyl-p-toluidine (content is the 0.1wt% of microemulsion)
(2) microemulsion system is encapsulated in pressure vessel mould;
(3) left at room temperature 6h, makes microemulsion carry out polyreaction.
In this technical scheme, emulsifying agent can be added and polymerization single polymerization monomer, cosurfactant, radioactivity feed liquid are configured to microemulsion jointly in step (1), as sodium laurylsulfonate (SDS), cetyl trimethylammonium bromide (CTAB), alkylphenol polyoxyethylene (TX-10) etc., emulsifying agent addition is the 0-8wt% of weight of microemulsion.
In this technical scheme, described radioactivity feed liquid Radionuclide can be
3h,
18f,
22na,
32p,
55fe,
57co,
60co,
63ni,
68ge,
85kr,
90sr,
99mo,
103pd,
109cd,
125i,
137cs,
147pm,
153gd,
192ir,
198au,
210po,
226ra,
238pu,
241am,
252cf or other any nucleic, the preferred 7-8 of radioactivity material liquid pH.In this technical scheme, described radioactive source can be line source, post source, point source, source, face and other any type of radioactive sources.In this technical scheme, time of repose is preferably 1-10 hour.
In this technical scheme, described polymerization single polymerization monomer is not limited to methyl methacrylate (MMA), methacrylic acid (MA), acrylamide (AM), other vinyl monomers can also be selected, or one or more the mixture selecting other can carry out in the monomer of micro-emulsion polymerization.In this technical scheme, described cosurfactant is not limited to hydroxyethyl methylacrylate (HEMA), vinylformic acid (AA), dimethylaminoethyl acrylate methyl ammonia ethyl ester (DM), other can also be selected to contain unsaturated double-bond, polyreaction can be participated in, and can be miscible with polymerization single polymerization monomer, again can one or more mixture in the material miscible with water as cosurfactant.In this technical scheme, described initiator is not limited to benzoyl peroxide (BPO), Diisopropyl azodicarboxylate (AIBN), Potassium Persulphate-S-WAT (KPS-SH), and one or more mixture in other peralcohol, azo-compound, redox initiation system can also be selected as initiator.In this technical scheme, described promotor is not limited to N, N-dimethyl-p-toluidine (DMT), to toluenesulfinic acid (TSA), other trimethylamine can also be selected, to the mixture of one or more in methyl-sulfinic acid salt as promotor.In this technical scheme, described linking agent is not limited to Vinylstyrene (DVB), N-hydroxymethylacrylate acid amides (HAM), dicumyl peroxide (DCP), can also select the vinyl monomer containing multiple unsaturated double-bond in other molecules or other the mutual bonding cross-linking of multiple thread-like molecule can be made to reticulate one or more mixture in the material of structure at line style intermolecular bridging action.
(3) beneficial effect
In the present invention, adopt polymerization single polymerization monomer to form homogeneous phase microemulsion at normal temperatures with the aqueous solution containing radionuclide, Radio-nuclide distribution is even.Microemulsion viscosity is low, is beneficial to and loads in corresponding mould, easy to operate.Reaction system is sealed in corresponding mould, and polymeric reaction temperature is lower, and reaction process can not pollute.The high molecular polymerization product intensity formed is high, and good toughness, resistance to irradiation ability is strong.Radionuclide, with reacting by uniform curing in high molecular polymer, quantitatively utilizes.Related reagent is less demanding, is regular industrial raw material.In this method, radioactive source can be designed as any shape.
Embodiment
Below in conjunction with specific embodiments the technical program is described further.
Embodiment 1
Micro-emulsion polymerization prepares a method for radioactive source, comprises the following steps successively:
(1) by methyl methacrylate (content is 25wt%), hydroxyethyl methylacrylate (content is 70wt%), radioactivity germanium [
68ge] feed liquid (content is 5wt%) is configured to microemulsion, and filling with inert gas is vented; Add benzoyl peroxide (content is the 0.5wt% of microemulsion) and dissolve mixing, filling with inert gas is vented; Add Vinylstyrene (content is the 1wt% of microemulsion) and N, N-dimethyl-p-toluidine (content is the 0.1wt% of microemulsion)
(2) microemulsion system is encapsulated in pressure vessel mould;
(3) left at room temperature 6h, makes microemulsion carry out polyreaction.
Embodiment 2
Micro-emulsion polymerization prepares a method for radioactive source, comprises the following steps successively:
(1) by methyl methacrylate (content is 49wt%), hydroxyethyl methylacrylate (content is 49wt%), radiocesium [
137cs] feed liquid (content is 2wt%) is configured to microemulsion, and filling with inert gas is vented; Add benzoyl peroxide (content is the 0.8wt% of microemulsion) and dissolve mixing, filling with inert gas is vented; Add Vinylstyrene (content is the 2wt% of microemulsion) and N, N-dimethyl-p-toluidine (content is the 0.05wt% of microemulsion)
(2) microemulsion system is encapsulated in pressure vessel mould;
(3) left at room temperature 6h, makes microemulsion carry out polyreaction.
Embodiment 3
Micro-emulsion polymerization prepares a method for radioactive source, comprises the following steps successively:
(1) by methyl methacrylate (content is 75wt%), hydroxyethyl methylacrylate (content is 25.5wt%), radiocobalt [
60co] feed liquid (content is 0.5wt%) is configured to microemulsion, and filling with inert gas is vented; Add benzoyl peroxide (content is the 0.3wt% of microemulsion) and dissolve mixing, filling with inert gas is vented; Add Vinylstyrene (content is the 0.2wt% of microemulsion) and N, N-dimethyl-p-toluidine (content is the 0.4wt% of microemulsion)
(2) microemulsion system is encapsulated in pressure vessel mould;
(3) left at room temperature 6h, makes microemulsion carry out polyreaction.
Embodiment 4
The present embodiment reagent used is analytical pure.
Micro-emulsion polymerization prepares a method for radioactive source, comprises the following steps successively:
(1) by methacrylic acid (content is 62wt%), vinylformic acid (content is 31wt%), radioiodine [
125i] feed liquid (content is 7wt%) is configured to microemulsion, and filling with inert gas is vented; Add Potassium Persulphate-S-WAT (content is the 0.7wt% of microemulsion) and dissolve mixing, filling with inert gas is vented; Add N-hydroxymethylacrylate acid amides (content is the 0.02wt% of microemulsion);
(2) microemulsion system is encapsulated in pressure vessel mould;
Leave standstill 4h at (3) 60 DEG C, make microemulsion carry out polyreaction.
Embodiment 5
(1) by acrylamide (content is 49.5wt%), dimethylaminoethyl acrylate methyl ammonia ethyl ester (content is 49.5wt%), radioactivity molybdenum [
99mo] feed liquid (content is 1wt%) is configured to microemulsion, and filling with inert gas is vented; Add Diisopropyl azodicarboxylate (content is the 0.2wt% of microemulsion) and dissolve mixing, filling with inert gas is vented;
(2) microemulsion system is encapsulated in pressure vessel mould;
Leave standstill 1h at (3) 80 DEG C, make microemulsion carry out polyreaction.
Embodiment 6
(1) by methyl methacrylate (content is 80wt%), dimethylaminoethyl acrylate methyl ammonia ethyl ester (content is 15wt%), radioactivity palladium [
103pd] feed liquid (content is 5wt%) is configured to emulsion, and the sodium laurylsulfonate adding above-mentioned emulsion total amount 8% forms microemulsion, and filling with inert gas is vented; Add Potassium Persulphate-S-WAT (content is the 1wt% of microemulsion) and dissolve mixing, filling with inert gas is vented; Add N-hydroxymethylacrylate acid amides (content is the 0.5wt% of microemulsion) and to toluenesulfinic acid (content is the 0.3wt% of microemulsion);
(2) microemulsion system is encapsulated in pressure vessel mould;
(3) left at room temperature 10h, makes microemulsion carry out polyreaction.
Embodiment 7
(1) by methacrylic acid (content is 15wt%), hydroxyethyl methylacrylate (content is 80wt%), radioactivity cadmium [
109cd] feed liquid (content is 5wt%) is configured to microemulsion, and filling with inert gas is vented; Add benzoyl peroxide (content is the 0.6wt% of microemulsion) and dissolve mixing, filling with inert gas is vented; Add dicumyl peroxide (content is the 2wt% of microemulsion) and N, N-dimethyl-p-toluidine (content is the 0.2wt% of microemulsion);
(2) microemulsion system is encapsulated in pressure vessel mould;
(3) left at room temperature 5h, makes microemulsion carry out polyreaction.
Embodiment 8
(1) by acrylamide (content is 55wt%), vinylformic acid (content is 36wt%), radioactivity americium [
241am] feed liquid (content is 9wt%) is configured to emulsion, and the alkylphenol polyoxyethylene adding above-mentioned emulsion total amount 5% forms microemulsion, and filling with inert gas is vented; Add Potassium Persulphate-S-WAT (content is the 0.3wt% of microemulsion) and dissolve mixing, filling with inert gas is vented; Add dicumyl peroxide (content is the 1.5wt% of microemulsion) and N, N-dimethyl-p-toluidine (content is the 0.05wt% of microemulsion);
(2) microemulsion system is encapsulated in pressure vessel mould;
Leave standstill 4h at (3) 50 DEG C, make microemulsion carry out polyreaction.
Embodiment 9
(1) by methyl methacrylate (content is 40wt%), vinylformic acid (content is 57wt%), radiostrontium [
90sr] feed liquid (content is 3wt%) is configured to microemulsion, and filling with inert gas is vented; Add Diisopropyl azodicarboxylate (content is the 0.4wt% of microemulsion) and dissolve mixing, filling with inert gas is vented; Add dicumyl peroxide (content is the 0.1wt% of microemulsion) and N, N-dimethyl-p-toluidine (content is the 0.5wt% of microemulsion);
(2) microemulsion system is encapsulated in pressure vessel mould;
(3) left at room temperature 2h, makes microemulsion carry out polyreaction.
Embodiment 10
(1) by methacrylic acid (content is 32wt%), dimethylaminoethyl acrylate methyl ammonia ethyl ester (content is 58wt%), radioactivity californium [
252cf] feed liquid (content is 5wt%) is configured to emulsion, and the cetyl trimethylammonium bromide adding above-mentioned emulsion total amount 2% forms microemulsion, and filling with inert gas is vented; Add Diisopropyl azodicarboxylate (content is the 0.8wt% of microemulsion) and dissolve mixing, filling with inert gas is vented; Add Vinylstyrene (content is the 0.8wt% of microemulsion) and to toluenesulfinic acid (content is the 0.4wt% of microemulsion);
(2) microemulsion system is encapsulated in pressure vessel mould;
(3) left at room temperature 4h, makes microemulsion carry out polyreaction.
Embodiment 11
(1) by the mixture (content is 72wt%) of acrylamide and methyl methacrylate, hydroxyethyl methylacrylate and acrylic acid mixture (content is 26wt%), radioactivity iridium [
192ir] feed liquid (content is 2wt%) is configured to microemulsion, and filling with inert gas is vented; Add the mixture (content is the 1wt% of microemulsion) of benzoyl peroxide and Diisopropyl azodicarboxylate and dissolve mixing, filling with inert gas is vented; Add Vinylstyrene and N-hydroxymethylacrylate acid amides mixture (content is the 1wt% of microemulsion) and to toluenesulfinic acid (content is the 0.4wt% of microemulsion);
(2) microemulsion system is encapsulated in pressure vessel mould;
Leave standstill 4h at (3) 70 DEG C, make microemulsion carry out polyreaction.
Above content is illustrating of doing the present invention in conjunction with preferred embodiment, and can not assert that the specific embodiment of the present invention is only limitted to these explanations.Concerning general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deductions and conversion can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. micro-emulsion polymerization prepares a method for radioactive source, it is characterized in that: comprise the following steps successively:
(1) polymerization single polymerization monomer, cosurfactant, radioactivity feed liquid are configured to microemulsion, filling with inert gas is vented; Add initiator and dissolve mixing, filling with inert gas exhaust again; Add linking agent and promotor mixes;
(2) microemulsion system is encapsulated in pressure vessel mould;
(3) leave standstill, make microemulsion carry out polyreaction.
2. micro-emulsion polymerization according to claim 2 prepares the method for radioactive source, it is characterized in that: in step (1), the polymerization single polymerization monomer of composition microemulsion is vinyl monomer, and described polymerization single polymerization monomer content is 15-80wt%; Described vinyl monomer is preferably one or more the mixture in methyl methacrylate (MMA), methacrylic acid (MA), acrylamide (AM) or other vinyl monomer.
3. micro-emulsion polymerization according to claim 1 prepares the method for radioactive source, it is characterized in that: in the step (1) cosurfactant of composition microemulsion be hydroxyethyl methylacrylate (HEMA), vinylformic acid (AA), dimethylaminoethyl acrylate methyl ammonia ethyl ester (DM) or other contain one or more mixture in the cosurfactant of unsaturated double-bond, described cosurfactant content is 15-80wt%.
4. micro-emulsion polymerization according to claim 1 prepares the method for radioactive source, it is characterized in that: in step (1), the described radioactivity feed liquid content including radionuclide of composition microemulsion is 1-10wt%.
5. micro-emulsion polymerization according to claim 1 prepares the method for radioactive source, it is characterized in that: in step (1), initiator is one or more the mixture in peralcohol, azo-compound or redox initiation system; The add-on of described initiator is the 0.2-1wt% of microemulsion total amount; Described superoxide is preferably benzoyl peroxide (BPO), and azo-compound is preferably Diisopropyl azodicarboxylate (AIBN), and redox initiation system is preferably Potassium Persulphate-S-WAT (KPS-SH).
6. micro-emulsion polymerization according to claim 1 prepares the method for radioactive source, it is characterized in that: the promotor added in step (1) is trimethylamine or the mixture to one or more in methyl-sulfinic acid salt; The add-on of described promotor is at most the 0.5wt% of microemulsion total amount; Trimethylamine is preferably N, N-dimethyl-p-toluidine (DMT), is preferably toluenesulfinic acid (TSA) methyl-sulfinic acid salt.
7. micro-emulsion polymerization according to claim 1 prepares the method for radioactive source, it is characterized in that: the linking agent added in step (1) is the mutual bonding cross-linking of multiple thread-like molecule can be made to reticulate one or more mixture in the material of structure at line style intermolecular bridging action containing the vinyl monomer of multiple unsaturated double-bond or other in molecule; The add-on of described linking agent is at most the 2wt% of microemulsion total amount; Vinyl monomer containing multiple unsaturated double-bond in molecule is preferably Vinylstyrene (DVB), and other can at line style intermolecular bridging action thus the material making the mutual bonding cross-linking of multiple thread-like molecule reticulate structure is preferably N-hydroxymethylacrylate acid amides (HAM) or dicumyl peroxide (DCP).
8. micro-emulsion polymerization prepares a method for radioactive source, it is characterized in that: comprise the following steps successively:
(1) the radioactivity feed liquid that be the methyl methacrylate of 25wt% by content, content is the hydroxyethyl methylacrylate of 70wt%, content is 5wt% is configured to microemulsion, and filling with inert gas is vented; Add-on is the benzoyl peroxide of the 0.5wt% of microemulsion total amount and dissolves mixing, filling with inert gas exhaust again; Add the N that Vinylstyrene that content is the 1wt% of microemulsion total amount and content are the 0.1wt% of microemulsion total amount, N-dimethyl-p-toluidine also mixes;
(2) microemulsion system is encapsulated in pressure vessel mould;
(3) left at room temperature 6 hours, makes microemulsion carry out polyreaction.
9. the micro-emulsion polymerization according to claim 1 or 8 prepares the method for radioactive source, it is characterized in that: the pH value of radioactivity feed liquid is 7-8.
10. the micro-emulsion polymerization according to claim 1 or 8 prepares the method for radioactive source, it is characterized in that: described radioactive source is line source, post source, point source or source, face.
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