CN117660981A - Supercritical CO 2 Coated microemulsion, preparation method thereof and application thereof in removing radioactive pollution on stainless steel surface - Google Patents
Supercritical CO 2 Coated microemulsion, preparation method thereof and application thereof in removing radioactive pollution on stainless steel surface Download PDFInfo
- Publication number
- CN117660981A CN117660981A CN202311461642.7A CN202311461642A CN117660981A CN 117660981 A CN117660981 A CN 117660981A CN 202311461642 A CN202311461642 A CN 202311461642A CN 117660981 A CN117660981 A CN 117660981A
- Authority
- CN
- China
- Prior art keywords
- supercritical
- stainless steel
- radioactive
- microemulsion
- molten salt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 54
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 48
- 239000010935 stainless steel Substances 0.000 title claims abstract description 48
- 238000003904 radioactive pollution Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 230000002285 radioactive effect Effects 0.000 claims abstract description 82
- 150000003839 salts Chemical class 0.000 claims abstract description 52
- 238000005202 decontamination Methods 0.000 claims abstract description 51
- 230000003588 decontaminative effect Effects 0.000 claims abstract description 47
- 239000003344 environmental pollutant Substances 0.000 claims abstract description 47
- 231100000719 pollutant Toxicity 0.000 claims abstract description 47
- KJIFKLIQANRMOU-UHFFFAOYSA-N oxidanium;4-methylbenzenesulfonate Chemical compound O.CC1=CC=C(S(O)(=O)=O)C=C1 KJIFKLIQANRMOU-UHFFFAOYSA-N 0.000 claims abstract description 32
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims abstract description 19
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 19
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 19
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims abstract description 17
- 235000019743 Choline chloride Nutrition 0.000 claims abstract description 17
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims abstract description 17
- 229960003178 choline chloride Drugs 0.000 claims abstract description 17
- 239000012466 permeate Substances 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims description 53
- 239000000356 contaminant Substances 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 33
- 238000002156 mixing Methods 0.000 claims description 29
- 229910052770 Uranium Inorganic materials 0.000 claims description 24
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- 230000015572 biosynthetic process Effects 0.000 claims description 14
- 239000012530 fluid Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 12
- 229910052712 strontium Inorganic materials 0.000 claims description 11
- 238000012546 transfer Methods 0.000 claims description 11
- 229910017052 cobalt Inorganic materials 0.000 claims description 9
- 239000010941 cobalt Substances 0.000 claims description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 9
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 9
- 239000002699 waste material Substances 0.000 abstract description 10
- 239000000839 emulsion Substances 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000001988 toxicity Effects 0.000 abstract description 2
- 231100000419 toxicity Toxicity 0.000 abstract description 2
- 239000010963 304 stainless steel Substances 0.000 description 79
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 79
- 238000001035 drying Methods 0.000 description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- 238000011109 contamination Methods 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 238000002791 soaking Methods 0.000 description 10
- 238000011068 loading method Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000002253 acid Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000002901 radioactive waste Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000010814 metallic waste Substances 0.000 description 3
- -1 paratoluenesulfonic acid monohydrate Chemical class 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004055 radioactive waste management Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/28—Treating solids
- G21F9/30—Processing
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/06—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using emulsions
-
- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
Supercritical CO 2 Coated microemulsion, a preparation method thereof and application thereof in removing radioactive pollution on the surface of stainless steel. The invention belongs to the technical field of radioactive pollution removal. The invention aims to solve the technical problems of large secondary waste liquid amount, strong corrosiveness and strong reagent toxicity of the existing radioactive metal chemical solution decontamination method. The invention reasonably regulates the proportion and the addition amount of the p-toluenesulfonic acid monohydrate, the choline chloride and the nonylphenol polyoxyethylene ether in the room-temperature molten salt to ensure that the mixture is in supercritical CO 2 The emulsion can quickly permeate to the surface of pollutants, has the high-efficiency dissolution characteristic of room-temperature molten salt, can quickly remove radionuclides on the surface of metal, and has obviously reduced demand for room-temperature molten salt. After decontamination is completed, CO is reduced 2 Temperature and pressure of (2) to convert CO 2 At room temperatureSeparating the fused salt emulsion and separating CO 2 Recycling is realized, and secondary waste minimization is realized.
Description
Technical Field
The invention belongs to the technical field of radioactive pollution removal, and in particular relates to a supercritical CO 2 Coated microemulsion, a preparation method thereof and application thereof in removing radioactive pollution on the surface of stainless steel.
Background
The sources of radioactive metal waste are diverse, including nuclear power plant waste, nuclear fuel production waste, nuclear weapon related activities waste, medical facility radioisotope and scientific research facility waste, etc. Among them, radioactive contaminants generated during the operation and retirement of nuclear power plants can be classified into three types: corrosion products (Co, mn, zr), fission products (Sr, cs, ce, zr, ru) and transuranic species (U, pu, np, am, etc.). These radioactive wastes have radiation that can cause direct damage to the organisms. In addition, radioactive metal waste may cause radiation leakage in case of improper treatment or storage, creating long-term hazards to soil, water sources and ecosystems. Therefore, safe and efficient treatment of radioactive metal waste has been an important subject. The most commonly used radioactive metal decontamination method is chemical solution decontamination, but the method has the disadvantages of large secondary waste liquid amount, strong corrosiveness and strong reagent toxicity, and the development of the technology is greatly limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a supercritical CO 2 Coated microemulsion, a preparation method thereof and application thereof in removing radioactive pollution on the surface of stainless steel.
The technical scheme of the invention is realized by the following steps:
one of the purposes of the present invention is to provide a supercritical CO 2 Coated microemulsion coated with supercritical CO 2 In the fluid, the microemulsion is composed of paratoluenesulfonic acid monohydrate, choline chloride and nonylphenol polyoxyethylene ether.
Further defined, the mass content of each component in the microemulsion is as follows: 10-50% of p-toluenesulfonic acid monohydrate, 5-45% of choline chloride and 30-70% of nonylphenol polyoxyethylene ether.
It is a second object of the present invention to provide a supercritical CO 2 The preparation method of the coated microemulsion comprises the following steps:
firstly mixing p-toluenesulfonic acid monohydrate and choline chloride for a certain time under the heating condition, then adding nonylphenol polyoxyethylene ether for continuous mixing to obtain room-temperature molten salt, and then dissolving the molten salt in supercritical CO under the stirring state 2 In the formation of supercritical CO 2 Coated microemulsions.
Further defined, the heating temperature is 30-90 ℃, and the mixing time is 2-12 hours.
Further limiting, adding the polyoxyethylene nonylphenol ether and continuously mixing for 0.1-12h.
Further defined, the stirring speed is 50-600rpm.
It is a further object of the present invention to provide a supercritical CO 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel comprises the following specific processes:
s1: placing a stainless steel sample with radioactive pollutants in a cleaning kettle, and then adding room-temperature molten salt;
s2: filling CO into the cleaning kettle 2 Heating to supercritical state, and stirringForming supercritical CO under stirring 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the stainless steel sample surface and transfers the radioactive contaminant to the supercritical CO 2 In (a) and (b);
s3: repeating the cleaning process for 0-3 times after the cleaning time is reached, and carrying the supercritical CO with radioactive pollutants 2 Introducing into a separation kettle, reducing temperature and pressure to make supercritical CO 2 And the gas state is restored, so that dissolved pollutants are released, and decontamination is completed.
Further defined, the element contained in the radioactive contaminant in S1 is one or more of uranium, strontium, and cobalt.
Further limited, the addition amount of the room temperature molten salt in the S1 is 1-50% of the inner cavity volume of the cleaning kettle.
Further defined, S2 is charged with CO 2 To 5-40MPa, and heating to 30-80 ℃.
Further defined, the stirring speed in S2 is 50-600rpm.
Further defined, the cleaning time in S3 is 30-300min.
Compared with the prior art, the invention has the remarkable effects that:
supercritical CO of the present invention 2 The coated microemulsion can be used as a cleaning agent in the field of radioactive waste treatment, thereby providing an emerging radioactive pollution removal method and providing a potential solution for radioactive waste treatment. The method has the specific advantages that:
(1) Supercritical CO of the present invention 2 The coated microemulsion is capable of rapidly separating radioactive metal ions from the waste by contact with the metal radioactive waste, reducing the radiation hazard of the waste, while producing only a very small amount of secondary waste. The method provides a feasible way for realizing the sustainable development goal of nuclear energy, and simultaneously provides a new idea for future radioactive waste management and environmental protection.
(2) The invention reasonably regulates the composition and the addition amount of the room temperature molten salt to ensure that the molten salt is in supercritical CO 2 An emulsion which can rapidly penetrate to the surface of the contaminant and which has room temperatureThe efficient dissolution characteristic of the molten salt can rapidly remove radionuclides on the metal surface, and the demand for room-temperature molten salt is obviously reduced. After decontamination is completed, CO is reduced 2 Temperature and pressure of (2) to convert CO 2 Separating from room temperature molten salt emulsion and separating CO 2 Recycling is realized, and secondary waste minimization is realized.
(3) Supercritical CO in the present invention 2 Under the decontamination process condition, 99.83% uranium-containing radioactive dirt on the stainless steel surface can be removed after the stainless steel is cleaned twice, and 95.79% cobalt-containing simulated radioactive dirt and 96.98% strontium-containing simulated radioactive dirt on the stainless steel surface can be removed after the stainless steel is cleaned once.
Drawings
FIG. 1 is an SEM image of a uranium radio-contaminated sample of example 7 prior to decontamination;
fig. 2 is an SEM image of the uranium radioactive contaminated sample of example 7 after decontamination.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, methods and apparatus used, without any particular description, are those conventional in the art and are commercially available to those skilled in the art.
The terms "comprising," "including," "having," "containing," or any other variation thereof, as used in the following embodiments, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range. In the present specification and claims, the range limitations may be combined and/or interchanged, such ranges including all the sub-ranges contained therein if not expressly stated.
The endpoints of the ranges and any values disclosed in the invention are not limited to the precise range or value, and the range or value should be understood to include values close to the range or value. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Example 1 supercritical CO 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel comprises the following specific processes:
the first step: preparation of uranium-containing 304 stainless steel sheet samples.
(1) Soaking 304 stainless steel sheet of 20×20X0.3 mm in absolute ethanol for 0.5 hr, washing with deionized water, drying in a drying oven, and measuring the background value of 304 stainless steel with CoMo-170 surface contamination instrument, denoted as A 0 ；
(2) 0.4219g UO was weighed 2 (NO 3 ) 2 ·6H 2 O, dissolving with absolute ethyl alcohol to a constant volume of 10mL, dripping 200 mu L of the solution on the 304 stainless steel sheet in the step (1), drying the solution on the surface of the 304 stainless steel sheet by using an infrared lamp, then placing the 304 stainless steel sheet in a well type furnace at 370 ℃ for 2.5 hours, obtaining the 304 stainless steel sheet with uranium-containing radioactive pollutants, and dipping the surface of the 304 stainless steel sheet by adopting CoMo-170The radioactive pollution value of the 304 stainless steel sheet before decontamination is measured by a pollution meter and is recorded as A 1 。
And a second step of: and (3) preparing the room-temperature molten salt.
Mixing 30% of p-toluenesulfonic acid monohydrate and 10% of choline chloride for 6 hours at 60 ℃ according to mass fraction, then adding 60% of nonylphenol polyoxyethylene ether, and continuously mixing for 0.5 hour at 30 ℃ to obtain room-temperature molten salt.
And a third step of: removal of radioactive contaminants.
(1) Placing a stainless steel sample with radioactive pollutants into a cleaning kettle, and then adding room-temperature molten salt accounting for 5% of the inner cavity volume of the cleaning kettle;
(2) Filling CO into the cleaning kettle 2 Heating to 15MPa at 40deg.C to supercritical state, turning on stirrer, and dissolving in supercritical CO under stirring at 250rpm 2 In the formation of supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the surface of the stainless steel sample, reacts with the radioactive contaminant, and transfers the radioactive contaminant to the supercritical CO 2 In (a) and (b);
(3) Washing for 60min, and loading supercritical CO with radioactive pollutant 2 Introducing into a separation kettle, reducing temperature and pressure to normal temperature and normal pressure to make supercritical CO 2 And (3) recovering to the gaseous state, thereby releasing dissolved pollutants, finally opening the cleaning kettle, taking out the sample, and completing decontamination.
EXAMPLE 2 supercritical CO 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel comprises the following specific processes:
the first step: preparation of uranium-containing 304 stainless steel sheet samples.
(1) Soaking 304 stainless steel sheet of 20×20X0.3 mm in absolute ethanol for 0.5 hr, washing with deionized water, drying in a drying oven, and measuring the background value of 304 stainless steel with CoMo-170 surface contamination instrument, denoted as A 0 ；
(2) 0.4219g UO was weighed 2 (NO 3 ) 2 ·6H 2 O, dissolving with absolute ethyl alcohol, and then fixing the volume to be 10mL,dripping 200 mu L of the solution on the surface of the 304 stainless steel sheet in the step (1), drying the solution on the surface of the 304 stainless steel sheet by using an infrared lamp, then placing the 304 stainless steel sheet in a well type furnace at 370 ℃ for 2.5 hours to obtain the 304 stainless steel sheet with uranium-containing radioactive pollutants, and measuring the radioactive pollution value of the 304 stainless steel sheet before decontamination by adopting a CoMo-170 surface contamination meter, and marking the radioactive pollution value as A 1 。
And a second step of: and (3) preparing the room-temperature molten salt.
Mixing 16% of p-toluenesulfonic acid monohydrate and 24% of choline chloride for 6 hours at 60 ℃ according to mass fraction, then adding 60% of nonylphenol polyoxyethylene ether, and continuously mixing for 0.5 hour at 30 ℃ to obtain room-temperature molten salt.
And a third step of: removal of radioactive contaminants.
(1) Placing a stainless steel sample with radioactive pollutants into a cleaning kettle, and then adding room-temperature molten salt accounting for 5% of the inner cavity volume of the cleaning kettle;
(2) Filling CO into the cleaning kettle 2 Heating to 15MPa at 40deg.C to supercritical state, turning on stirrer, and dissolving in supercritical CO under stirring at 250rpm 2 In the formation of supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the surface of the stainless steel sample, reacts with the radioactive contaminant, and transfers the radioactive contaminant to the supercritical CO 2 In (a) and (b);
(3) Washing for 60min, and loading supercritical CO with radioactive pollutant 2 Introducing into a separation kettle, reducing temperature and pressure to normal temperature and normal pressure to make supercritical CO 2 And (3) recovering to the gaseous state, thereby releasing dissolved pollutants, finally opening the cleaning kettle, taking out the sample, and completing decontamination.
EXAMPLE 3 supercritical CO 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel comprises the following specific processes:
the first step: preparation of uranium-containing 304 stainless steel sheet samples.
(1) Soaking 304 stainless steel sheet of 20×20X0.3 mm in absolute ethanol for 0.5 hr, washing with deionized water, and drying in a drying ovenAfter drying, the CoMo-170 surface contamination instrument is used for measuring the background value of the 304 stainless steel, which is marked as A 0 ；
(2) 0.4219g UO was weighed 2 (NO 3 ) 2 ·6H 2 O, dissolving with absolute ethyl alcohol to a constant volume of 10mL, dripping 200 mu L of the solution on the 304 stainless steel sheet in the step (1), drying the solution on the surface of the 304 stainless steel sheet by using an infrared lamp, then placing the 304 stainless steel sheet in a well type furnace at 370 ℃ for 2.5 hours, obtaining the 304 stainless steel sheet with uranium-containing radioactive pollutants, and measuring the radioactive pollution value of the 304 stainless steel sheet before decontamination by adopting a CoMo-170 surface contamination meter, and marking as A 1 。
And a second step of: and (3) preparing the room-temperature molten salt.
Mixing 30% of p-toluenesulfonic acid monohydrate and 10% of choline chloride for 6 hours at 60 ℃ according to mass fraction, then adding 60% of nonylphenol polyoxyethylene ether, and continuously mixing for 0.5 hour at 30 ℃ to obtain room-temperature molten salt.
And a third step of: removal of radioactive contaminants.
(1) Placing a stainless steel sample with radioactive pollutants into a cleaning kettle, and then adding room-temperature molten salt accounting for 5% of the inner cavity volume of the cleaning kettle;
(2) Filling CO into the cleaning kettle 2 Heating to 15MPa at 60deg.C to supercritical state, turning on stirrer, and dissolving in supercritical CO under stirring at 250rpm 2 In the formation of supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the surface of the stainless steel sample, reacts with the radioactive contaminant, and transfers the radioactive contaminant to the supercritical CO 2 In (a) and (b);
(3) Washing for 60min, and loading supercritical CO with radioactive pollutant 2 Introducing into a separation kettle, reducing temperature and pressure to normal temperature and normal pressure to make supercritical CO 2 And (3) recovering to the gaseous state, thereby releasing dissolved pollutants, finally opening the cleaning kettle, taking out the sample, and completing decontamination.
EXAMPLE 4 supercritical CO 2 Use of coated microemulsions for removing radioactive contamination from stainless steel surfaces, e.gThe following steps:
the first step: preparation of uranium-containing 304 stainless steel sheet samples.
(1) Soaking 304 stainless steel sheet of 20×20X0.3 mm in absolute ethanol for 0.5 hr, washing with deionized water, drying in a drying oven, and measuring the background value of 304 stainless steel with CoMo-170 surface contamination instrument, denoted as A 0 ；
(2) 0.4219g UO was weighed 2 (NO 3 ) 2 ·6H 2 O, dissolving with absolute ethyl alcohol to a constant volume of 10mL, dripping 200 mu L of the solution on the 304 stainless steel sheet in the step (1), drying the solution on the surface of the 304 stainless steel sheet by using an infrared lamp, then placing the 304 stainless steel sheet in a well type furnace at 370 ℃ for 2.5 hours, obtaining the 304 stainless steel sheet with uranium-containing radioactive pollutants, and measuring the radioactive pollution value of the 304 stainless steel sheet before decontamination by adopting a CoMo-170 surface contamination meter, and marking as A 1 。
And a second step of: and (3) preparing the room-temperature molten salt.
Mixing 30% of p-toluenesulfonic acid monohydrate and 10% of choline chloride for 6 hours at 60 ℃ according to mass fraction, then adding 60% of nonylphenol polyoxyethylene ether, and continuously mixing for 0.5 hour at 30 ℃ to obtain room-temperature molten salt.
And a third step of: removal of radioactive contaminants.
(1) Placing a stainless steel sample with radioactive pollutants into a cleaning kettle, and then adding room-temperature molten salt accounting for 5% of the inner cavity volume of the cleaning kettle;
(2) Filling CO into the cleaning kettle 2 Heating to 20MPa at 60deg.C to supercritical state, turning on stirrer, and dissolving in supercritical CO under stirring at 250rpm 2 In the formation of supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the surface of the stainless steel sample, reacts with the radioactive contaminant, and transfers the radioactive contaminant to the supercritical CO 2 In (a) and (b);
(3) Washing for 60min, and loading supercritical CO with radioactive pollutant 2 Introducing into a separation kettle, reducing temperature and pressure to normal temperature and normal pressure to make supercritical CO 2 The gas phase is restored to the state of the gas,thereby releasing the dissolved pollutants, finally opening the cleaning kettle, taking out the sample, and completing decontamination.
EXAMPLE 5 supercritical CO 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel comprises the following specific processes:
the first step: preparation of uranium-containing 304 stainless steel sheet samples.
(1) Soaking 304 stainless steel sheet of 20×20X0.3 mm in absolute ethanol for 0.5 hr, washing with deionized water, drying in a drying oven, and measuring the background value of 304 stainless steel with CoMo-170 surface contamination instrument, denoted as A 0 ；
(2) 0.4219g UO was weighed 2 (NO 3 ) 2 ·6H 2 O, dissolving with absolute ethyl alcohol to a constant volume of 10mL, dripping 200 mu L of the solution on the 304 stainless steel sheet in the step (1), drying the solution on the surface of the 304 stainless steel sheet by using an infrared lamp, then placing the 304 stainless steel sheet in a well type furnace at 370 ℃ for 2.5 hours, obtaining the 304 stainless steel sheet with uranium-containing radioactive pollutants, and measuring the radioactive pollution value of the 304 stainless steel sheet before decontamination by adopting a CoMo-170 surface contamination meter, and marking as A 1 。
And a second step of: and (3) preparing the room-temperature molten salt.
Mixing 30% of p-toluenesulfonic acid monohydrate and 10% of choline chloride for 6 hours at 60 ℃ according to mass fraction, then adding 60% of nonylphenol polyoxyethylene ether, and continuously mixing for 0.5 hour at 30 ℃ to obtain room-temperature molten salt.
And a third step of: removal of radioactive contaminants.
(1) Placing a stainless steel sample with radioactive pollutants into a cleaning kettle, and then adding room-temperature molten salt accounting for 5% of the inner cavity volume of the cleaning kettle;
(2) Filling CO into the cleaning kettle 2 Heating to 15MPa at 60deg.C to supercritical state, turning on stirrer, and dissolving in supercritical CO under stirring at 250rpm 2 In the formation of supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the surface of the stainless steel sample, reacts with the radioactive contaminant, and causes the radioactive contaminant to react with the stainless steel sampleTransfer to supercritical CO 2 In (a) and (b);
(3) Washing for 30min, and loading supercritical CO with radioactive pollutant 2 Introducing into a separation kettle, reducing temperature and pressure to normal temperature and normal pressure to make supercritical CO 2 And (3) recovering to the gaseous state, thereby releasing dissolved pollutants, finally opening the cleaning kettle, taking out the sample, and completing decontamination.
EXAMPLE 6 supercritical CO 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel comprises the following specific processes:
the first step: preparation of uranium-containing 304 stainless steel sheet samples.
(1) Soaking 304 stainless steel sheet of 20×20X0.3 mm in absolute ethanol for 0.5 hr, washing with deionized water, drying in a drying oven, and measuring the background value of 304 stainless steel with CoMo-170 surface contamination instrument, denoted as A 0 ；
(2) 0.4219g UO was weighed 2 (NO 3 ) 2 ·6H 2 O, dissolving with absolute ethyl alcohol to a constant volume of 10mL, dripping 200 mu L of the solution on the 304 stainless steel sheet in the step (1), drying the solution on the surface of the 304 stainless steel sheet by using an infrared lamp, then placing the 304 stainless steel sheet in a well type furnace at 370 ℃ for 2.5 hours, obtaining the 304 stainless steel sheet with uranium-containing radioactive pollutants, and measuring the radioactive pollution value of the 304 stainless steel sheet before decontamination by adopting a CoMo-170 surface contamination meter, and marking as A 1 。
And a second step of: and (3) preparing the room-temperature molten salt.
Mixing 30% of p-toluenesulfonic acid monohydrate and 10% of choline chloride for 6 hours at 60 ℃ according to mass fraction, then adding 60% of nonylphenol polyoxyethylene ether, and continuously mixing for 0.5 hour at 30 ℃ to obtain room-temperature molten salt.
And a third step of: removal of radioactive contaminants.
(1) Placing a stainless steel sample with radioactive pollutants into a cleaning kettle, and then adding room-temperature molten salt accounting for 5% of the inner cavity volume of the cleaning kettle;
(2) Filling CO into the cleaning kettle 2 Heating to 15MPa at 60deg.C to supercritical state, turning on stirrer, stirring at 250rpmIn the state of dissolving in supercritical CO 2 In the formation of supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the surface of the stainless steel sample, reacts with the radioactive contaminant, and transfers the radioactive contaminant to the supercritical CO 2 In (a) and (b);
(3) Washing for 75min, and loading supercritical CO with radioactive pollutant 2 Introducing into a separation kettle, reducing temperature and pressure to normal temperature and normal pressure to make supercritical CO 2 And (3) recovering to the gaseous state, thereby releasing dissolved pollutants, finally opening the cleaning kettle, taking out the sample, and completing decontamination.
EXAMPLE 7 supercritical CO 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel comprises the following specific processes:
the first step: preparation of uranium-containing 304 stainless steel sheet samples.
(1) Soaking 304 stainless steel sheet of 20×20X0.3 mm in absolute ethanol for 0.5 hr, washing with deionized water, drying in a drying oven, and measuring the background value of 304 stainless steel with CoMo-170 surface contamination instrument, denoted as A 0 ；
(2) 0.4219g UO was weighed 2 (NO 3 ) 2 ·6H 2 O, dissolving with absolute ethyl alcohol to a constant volume of 10mL, dripping 200 mu L of the solution on the 304 stainless steel sheet in the step (1), drying the solution on the surface of the 304 stainless steel sheet by using an infrared lamp, then placing the 304 stainless steel sheet in a well type furnace at 370 ℃ for 2.5 hours, obtaining the 304 stainless steel sheet with uranium-containing radioactive pollutants, and measuring the radioactive pollution value of the 304 stainless steel sheet before decontamination by adopting a CoMo-170 surface contamination meter, and marking as A 1 。
And a second step of: and (3) preparing the room-temperature molten salt.
Mixing 30% of p-toluenesulfonic acid monohydrate and 10% of choline chloride for 6 hours at 60 ℃ according to mass fraction, then adding 60% of nonylphenol polyoxyethylene ether, and continuously mixing for 0.5 hour at 30 ℃ to obtain room-temperature molten salt.
And a third step of: removal of radioactive contaminants.
(1) Placing a stainless steel sample with radioactive pollutants into a cleaning kettle, and then adding room-temperature molten salt accounting for 5% of the inner cavity volume of the cleaning kettle;
(2) Filling CO into the cleaning kettle 2 Heating to 15MPa at 40deg.C to supercritical state, turning on stirrer, and dissolving in supercritical CO under stirring at 250rpm 2 In the formation of supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the surface of the stainless steel sample, reacts with the radioactive contaminant, and transfers the radioactive contaminant to the supercritical CO 2 In (a) and (b);
(3) After 60min of cleaning, the cleaning process is repeated for 1 time, and the supercritical CO carrying the radioactive pollutants is carried 2 Introducing into a separation kettle, reducing temperature and pressure to normal temperature and normal pressure to make supercritical CO 2 And (3) recovering to the gaseous state, thereby releasing dissolved pollutants, finally opening the cleaning kettle, taking out the sample, and completing decontamination.
EXAMPLE 8 supercritical CO 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel comprises the following specific processes:
the first step: preparation of uranium-containing 304 stainless steel sheet samples.
(1) Soaking 304 stainless steel sheet of 20×20X0.3 mm in absolute ethanol for 0.5 hr, washing with deionized water, drying in a drying oven, and measuring the background value of 304 stainless steel with CoMo-170 surface contamination instrument, denoted as A 0 ；
(2) 0.4219g UO was weighed 2 (NO 3 ) 2 ·6H 2 O, dissolving with absolute ethyl alcohol to a constant volume of 10mL, dripping 200 mu L of the solution on the 304 stainless steel sheet in the step (1), drying the solution on the surface of the 304 stainless steel sheet by using an infrared lamp, then placing the 304 stainless steel sheet in a well type furnace at 370 ℃ for 2.5 hours, obtaining the 304 stainless steel sheet with uranium-containing radioactive pollutants, and measuring the radioactive pollution value of the 304 stainless steel sheet before decontamination by adopting a CoMo-170 surface contamination meter, and marking as A 1 。
And a second step of: and (3) preparing the room-temperature molten salt.
Mixing 30% of p-toluenesulfonic acid monohydrate and 10% of choline chloride for 6 hours at 60 ℃ according to mass fraction, then adding 60% of nonylphenol polyoxyethylene ether, and continuously mixing for 0.5 hour at 30 ℃ to obtain room-temperature molten salt.
And a third step of: removal of radioactive contaminants.
(1) Placing a stainless steel sample with radioactive pollutants into a cleaning kettle, and then adding room-temperature molten salt accounting for 3% of the inner cavity volume of the cleaning kettle;
(2) Filling CO into the cleaning kettle 2 Heating to 15MPa at 40deg.C to supercritical state, turning on stirrer, and dissolving in supercritical CO under stirring at 250rpm 2 In the formation of supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the surface of the stainless steel sample, reacts with the radioactive contaminant, and transfers the radioactive contaminant to the supercritical CO 2 In (a) and (b);
(3) Washing for 60min, and loading supercritical CO with radioactive pollutant 2 Introducing into a separation kettle, reducing temperature and pressure to normal temperature and normal pressure to make supercritical CO 2 And (3) recovering to the gaseous state, thereby releasing dissolved pollutants, finally opening the cleaning kettle, taking out the sample, and completing decontamination.
Comparative example 1: this comparative example differs from example 1 in that: the room-temperature molten salt consists of 49% of p-toluenesulfonic acid monohydrate, 18% of choline chloride and 33% of nonylphenol polyoxyethylene ether according to mass fraction.
The radioactive contamination values of the surfaces of the samples after cleaning of examples 1 to 8 and comparative example 1 were measured by using a CoMo-170 surface contamination meter and are recorded as A 2 The calculation formula of the decontamination rate is as follows, and the results are shown in Table 1:
wherein DE is decontamination rate,%;
A 0 is the background value, bq;
A 1 is the radioactive pollution value, bq, before decontamination;
A 2 is the radioactive pollution value after decontamination,Bq。
TABLE 1 detergency ratio for examples 1-8 and comparative example 1
EXAMPLE 9 supercritical CO 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel comprises the following specific processes:
the first step: preparation of uranium-containing 304 stainless steel sheet samples.
(1) Soaking a 304 stainless steel sheet with the thickness of 20 multiplied by 0.3mm in absolute ethyl alcohol for 0.5h, then washing the steel sheet with deionized water, and drying the steel sheet in a drying oven to obtain the 304 stainless steel sheet;
(2) 0.0874g Co (NO) 3 ) 2 ·6H 2 O, dissolving with deionized water, fixing the volume to be 10mL, taking 200 mu L, dripping the 200 mu L on the 304 stainless steel sheet in the step (1), drying the solution on the surface of the 304 stainless steel sheet by using an infrared lamp, and then placing the 304 stainless steel sheet in a 50 ℃ oven for Wen Yizhou, thereby obtaining the 304 stainless steel sheet with cobalt-containing simulated radioactive pollutants.
And a second step of: and (3) preparing the room-temperature molten salt.
Mixing 30% of p-toluenesulfonic acid monohydrate and 10% of choline chloride for 6 hours at 60 ℃ according to mass fraction, then adding 60% of nonylphenol polyoxyethylene ether, and continuously mixing for 0.5 hour at 30 ℃ to obtain room-temperature molten salt.
And a third step of: removal of radioactive contaminants.
(1) Placing a stainless steel sample with radioactive pollutants into a cleaning kettle, and then adding room-temperature molten salt accounting for 5% of the inner cavity volume of the cleaning kettle;
(2) Filling CO into the cleaning kettle 2 Heating to 15MPa at 60deg.C to supercritical state, turning on stirrer, and dissolving in supercritical CO under stirring at 250rpm 2 In the formation of supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the surface of the stainless steel sample, reacts with the radioactive contaminant, and changes the radioactivityTransfer of contaminants to supercritical CO 2 In (a) and (b);
(3) Washing for 75min, and loading supercritical CO with radioactive pollutant 2 Introducing into a separation kettle, reducing temperature and pressure to normal temperature and normal pressure to make supercritical CO 2 And (3) recovering to the gaseous state, thereby releasing dissolved pollutants, finally opening the cleaning kettle, taking out the sample, and completing decontamination.
Example 10 supercritical CO 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel comprises the following specific processes:
the first step: preparation of uranium-containing 304 stainless steel sheet samples.
(1) Soaking a 304 stainless steel sheet with the thickness of 20 multiplied by 0.3mm in absolute ethyl alcohol for 0.5h, then washing the steel sheet with deionized water, and drying the steel sheet in a drying oven to obtain the 304 stainless steel sheet;
(2) Weigh 0.0800g SrCl 2 ·6H 2 O, dissolving with deionized water to a constant volume of 10mL, dripping 200 mu L of the solution on the 304 stainless steel sheet in the step (1), drying the solution on the surface of the 304 stainless steel sheet by using an infrared lamp, and then placing the 304 stainless steel sheet in a 50 ℃ oven for Wen Yizhou to obtain the 304 stainless steel sheet with the strontium-containing simulated radioactive pollutant.
And a second step of: and (3) preparing the room-temperature molten salt.
Mixing 30% of p-toluenesulfonic acid monohydrate and 10% of choline chloride for 6 hours at 60 ℃ according to mass fraction, then adding 60% of nonylphenol polyoxyethylene ether, and continuously mixing for 0.5 hour at 30 ℃ to obtain room-temperature molten salt.
And a third step of: removal of radioactive contaminants.
(1) Placing a stainless steel sample with radioactive pollutants into a cleaning kettle, and then adding room-temperature molten salt accounting for 5% of the inner cavity volume of the cleaning kettle;
(2) Filling CO into the cleaning kettle 2 Heating to 15MPa at 60deg.C to supercritical state, turning on stirrer, and dissolving in supercritical CO under stirring at 250rpm 2 In the formation of supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 Penetration of fluid to stainless steel sample surfaceChemically react with the radioactive contaminants and transfer the radioactive contaminants to supercritical CO 2 In (a) and (b);
(3) Washing for 75min, and loading supercritical CO with radioactive pollutant 2 Introducing into a separation kettle, reducing temperature and pressure to normal temperature and normal pressure to make supercritical CO 2 And (3) recovering to the gaseous state, thereby releasing dissolved pollutants, finally opening the cleaning kettle, taking out the sample, and completing decontamination.
To measure the decontamination effect of examples 9-10, first 0.1M nitric acid and 0.1M hydrochloric acid were mixed in a volume ratio of 1:3, mixing to prepare mixed acid, then using the mixed acid to completely soak and dissolve cobalt and strontium simulated radioactive dirt on the surface of the decontaminated stainless steel sample, measuring the concentration of cobalt and strontium in the mixed acid by ICP, thereby measuring the residual simulated radioactive nuclide on the surface of the decontaminated sample, wherein the calculation formula of the decontamination rate is as follows, and the result is shown in Table 2:
wherein DE is decontamination rate,%;
c 1 the concentration of cobalt or strontium in the sample surface pollution liquid is added dropwise before decontamination, mg/L;
V 1 the volume L of cobalt or strontium pollution liquid is dripped on the surface of a sample before decontamination;
c 2 is the concentration of cobalt or strontium dissolved in the mixed acid after decontamination, mg/L;
V 2 is the volume of the mixed acid used, L.
Table 2 decontamination rates for examples 9-10
| Sample of | Example 9 | Example 10 |
| Decontamination rate (%) | 95.79 | 96.98 |
As can be seen from a comparison of examples 1-2 and comparative example 1 in Table 1, the appropriate polyoxyethylene nonylphenol ether content can be found in supercritical CO 2 Providing proper hydrophilic-lipophilic balance with the room temperature molten salt interface layer, thereby promoting supercritical CO 2 Formation of the decontamination microemulsion, when the nonylphenol polyoxyethylene ether content is below the range of the present invention, it is difficult to promote supercritical CO 2 The formation of the decontamination emulsion and thus the decontamination effect is poor.
As can be seen from a comparison of example 1 and example 3 in table 1, the decontamination effect of the method is also improved with increasing decontamination temperature at a certain pressure, probably because the increase in temperature results in a decrease in the viscosity of the room temperature molten salt polar core in the emulsion, improving the mass transfer efficiency and the dissolution rate of the soil. In addition, as can be seen from a comparison of example 1 and example 4 in Table 1, the decontamination effect of the method is also improved with increasing pressure, which can be attributed to the increase in pressure resulting in an increase in density, thereby improving the supercritical CO of the room temperature molten salt 2 Solubility in supercritical CO is promoted 2 And (3) forming a decontamination emulsion. As can be seen from a comparison of examples 3, 5-7 in Table 1, the detergency effect was improved with an increase in detergency time, and a detergency ratio of 99.83% was achieved after two detergency, demonstrating supercritical CO 2 High-efficiency decontamination performance of room temperature molten salt emulsion.
As is clear from examples 9 and 10 in Table 2, the decontamination method has excellent decontamination effects on simulated radionuclides such as Co and Sr on the surface of stainless steel, and the decontamination rate is more than 95%, further demonstrating the feasibility of the method.
In the foregoing, the present invention is merely preferred embodiments, which are based on different implementations of the overall concept of the invention, and the protection scope of the invention is not limited thereto, and any changes or substitutions easily come within the technical scope of the present invention as those skilled in the art should not fall within the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (10)
1. Supercritical CO 2 Coated microemulsion, characterized in that the microemulsion is coated with supercritical CO 2 In the fluid, the microemulsion consists of 10-50% of p-toluenesulfonic acid monohydrate, 5-45% of choline chloride and 30-70% of nonylphenol polyoxyethylene ether according to mass fraction.
2. The supercritical CO of claim 1 2 A method for preparing a coated microemulsion, characterized in that the method comprises:
firstly mixing p-toluenesulfonic acid monohydrate and choline chloride for a certain time under the heating condition, then adding nonylphenol polyoxyethylene ether for continuous mixing to obtain room-temperature molten salt, and then dissolving the molten salt in supercritical CO under the stirring state 2 In the formation of supercritical CO 2 Coated microemulsions.
3. The method according to claim 2, wherein the heating temperature is 30-90 ℃, the mixing time is 2-12 hours, and the nonylphenol polyoxyethylene ether is added and the mixing is continued for 0.1-12 hours.
4. The method according to claim 2, wherein the stirring speed is 50-600rpm.
5. The supercritical CO produced by the process of claim 2 2 The application of the coated microemulsion in removing radioactive pollution on the surface of stainless steel is characterized by comprising the following specific processes:
s1: placing a stainless steel sample with radioactive pollutants in a cleaning kettle, and then adding room-temperature molten salt;
s2: to cleanFilling CO into the kettle 2 Heating to supercritical state, and turning on stirrer to form supercritical CO 2 Coated microemulsion, supercritical CO carrying the microemulsion 2 The fluid permeates the stainless steel sample surface and transfers the radioactive contaminant to the supercritical CO 2 In (a) and (b);
s3: repeating the cleaning process for 0-3 times after the cleaning time is reached, and carrying the supercritical CO with radioactive pollutants 2 Introducing into a separation kettle, reducing temperature and pressure to make supercritical CO 2 And the gas state is restored, so that dissolved pollutants are released, and decontamination is completed.
6. The use according to claim 5, wherein the radioactive contaminant in S1 contains one or more of uranium, strontium and cobalt.
7. The method according to claim 5, wherein the addition amount of the molten salt at room temperature in S1 is 1-50% of the volume of the inner cavity of the cleaning kettle.
8. The method according to claim 5, wherein S2 is CO-filled 2 To 5-40MPa, and heating to 30-80 ℃.
9. The method according to claim 5, wherein the stirring speed in S2 is 50-600rpm.
10. The method according to claim 5, wherein the washing time in S3 is 30-300min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311461642.7A CN117660981A (en) | 2023-11-06 | 2023-11-06 | Supercritical CO 2 Coated microemulsion, preparation method thereof and application thereof in removing radioactive pollution on stainless steel surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311461642.7A CN117660981A (en) | 2023-11-06 | 2023-11-06 | Supercritical CO 2 Coated microemulsion, preparation method thereof and application thereof in removing radioactive pollution on stainless steel surface |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117660981A true CN117660981A (en) | 2024-03-08 |
Family
ID=90079803
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311461642.7A Pending CN117660981A (en) | 2023-11-06 | 2023-11-06 | Supercritical CO 2 Coated microemulsion, preparation method thereof and application thereof in removing radioactive pollution on stainless steel surface |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117660981A (en) |
-
2023
- 2023-11-06 CN CN202311461642.7A patent/CN117660981A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TW201037730A (en) | Method for decontaminating radioactively contaminated surfaces | |
| Jayaraj et al. | Corrosion investigations on zircaloy-4 and titanium dissolver materials for MOX fuel dissolution in concentrated nitric acid containing fluoride ions | |
| CN117660981A (en) | Supercritical CO 2 Coated microemulsion, preparation method thereof and application thereof in removing radioactive pollution on stainless steel surface | |
| CA2236146C (en) | Method for decontamination of nuclear plant components | |
| Patra et al. | Understanding the Mechanism of Cs Accumulation on Stainless Steel Suspended in Nuclear High-Level Liquid Waste | |
| WO1997017146A9 (en) | Method for decontamination of nuclear plant components | |
| Tian et al. | Effect of oxidizing decontamination process on corrosion property of 304L stainless steel | |
| CN111560196A (en) | Strippable film solutions for radionuclide decontamination, methods of making and using | |
| JPH0566999B2 (en) | ||
| Nakahara et al. | Electrochemical properties of zirconium in highly concentrated plutonium nitrate solution | |
| Bray | Development of a chemical process using nitric acid-cerium (IV) for decontamination of high-level waste canisters | |
| KR102407984B1 (en) | Foam decontamination method for removal of the dense radioactive oxide layer on the metal surface | |
| Askari et al. | Experimental study of the cobalt oxide etching rate from metal surface using F2/He atmospheric pressure plasma for decontamination of nuclear components | |
| Won et al. | Dissolution of magnetite by the hydrazine base solution | |
| Ngulimi et al. | Nuclear Decommissioning and Sustainable Environment: Insights on Decontamination Processes | |
| Jung et al. | Decontamination Performance of Foam Decontaminating Agent | |
| Takeuchi et al. | Adhesive property of radionuclides on material surface in high level radioactive liquid waste | |
| Kaminski et al. | Composition suitable for decontaminating a porous surface contaminated with cesium | |
| Ueda et al. | Evaluation of Carbon-14 release from irradiated zircaloy fuel cladding through a long-term static leaching test | |
| Knecht et al. | Scoping studies to reduce ICPP high-level radioactive waste volumes for final disposal | |
| Mun et al. | Study of the ruthenium fission-product behaviour in the containment of a nuclear reactor, in case of a severe accident occurring in oxidizing conditions | |
| KR101293780B1 (en) | Leaching equipment and technology for HEPA glass fiber and Leaching method using Thereof | |
| Wedman et al. | Electrolyze radioactive contamination away | |
| Taylor-Underhill | Contamination of Stainless Steel Components with Stable Caesium and Strontium Isotopes | |
| Eliassen | Disposal of high-level radioactive wastes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |