CN109799528A - Oxidation gel and preparation method thereof for the sampling of radioactive pollution metal shallow-layer - Google Patents
Oxidation gel and preparation method thereof for the sampling of radioactive pollution metal shallow-layer Download PDFInfo
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- CN109799528A CN109799528A CN201910043151.8A CN201910043151A CN109799528A CN 109799528 A CN109799528 A CN 109799528A CN 201910043151 A CN201910043151 A CN 201910043151A CN 109799528 A CN109799528 A CN 109799528A
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- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
Abstract
The invention belongs to the field of radiation detection technology, it is related to the oxidation gel and preparation method thereof sampled for radioactive pollution metal shallow-layer.The oxidation gel contains by weight percentage: the gel base as gelatum skeleton material of 5-15%, the surfactant of 5-10%, the thixotroping multiplication agent of 0.5-5%, the strong oxidizer of 3-20%, the acid of 3-20% and the water of surplus.Using the oxidation gel for the sampling of radioactive pollution metal shallow-layer of the invention, the shallow-layer sampling that more acurrate, smooth, controllable, intuitive can be used for radioactive pollution metal, and reduce radiation injury of the sampling process to operator.
Description
Technical field
The invention belongs to the field of radiation detection technology, be related to for radioactive pollution metal shallow-layer sample oxidation gel and
Preparation method.
Background technique
China's nuclear industry after decades of development, has large quantities of nuclear facilities and enters or will enter retirement phase.It takes
Sample detection is the important link of elimination of nuclear facilities work, and the metal sampler method in existing nuclear facilities is to wipe sampling or thermal cutting
Based on sampling, drilling sampling, but limit by nuclear facilities type, polluting property, operating space, manage require to limit etc. it is many because
The influence of element, these existing sampling methods are usually unable to satisfy actual use demand, show: wiping sampling can not be acquired effectively
Activated metal shallow-layer sample, and thermal cutting and drilling will cause radioaerosol quickly increases, radioactive metal bits splash etc.
Problem.Therefore, it is necessary to develop and apply some novel metal sampler technologies for nuclear facilities.
Gel is a kind of with good thixotropic non-newtonian fluid, its apparent viscosity reduction under shearing force, and
After shearing force is removed, apparent viscosity increases rapidly again.Also, the above-mentioned performance of inorganic gel will not be by strong acid, highly basic and strong
Oxidative attack.In addition, strong oxidizer is obvious to corrosion of metal effect, the uniform and rate of corrosion is very fast, especially suitable for gold
Belong to sampling.
Summary of the invention
Primary and foremost purpose of the invention is to provide the oxidation gel for the sampling of radioactive pollution metal shallow-layer, with can be more quasi-
Really, it smoothly, controllably, is intuitively sampled for the shallow-layer of radioactive pollution metal, and reduces sampling process to the spoke of operator
Shoot evil wounded.
In order to achieve this, the present invention is provided to the samplings of radioactive pollution metal shallow-layer in the embodiment on basis
Oxidation gel, the oxidation gel contains by weight percentage: the gel base as gelatum skeleton material of 5-15%,
The surfactant of 5-10%, the thixotroping of 0.5-5% are doubled agent, the strong oxidizer of 3-20%, the acid of 3-20% and surplus
Water.
Surface tension of the surfactant to adjust oxidation gel in oxidation gel of the invention, improves oxidation gel
Wetting property, so that the sampling to tiny slit can be realized.
Thixotroping multiplication agent in oxidation gel of the invention can quickly improve the thixotropic property of oxidation gel.Good thixotropy
It can make to aoxidize gel viscosity reduction when by shear action, it is easily operated (in such as spraying process, to be dropped by shearing force viscosity
It is low, Gu and the performance requirement to spray coating mechanical can be reduced), thixotroping multiplication agent mainly controls oxidation gel under low shear condition
Viscosity.
Strong oxidizer in oxidation gel of the invention is main corrosion reagent, is formed and is corroded to metal surface, reached
Sample purpose.
Acid in oxidation gel of the invention is the solvent of strong oxidizer first, secondly also has certain corrosiveness,
Cooperate with strong oxidizer, metal erosion is sampled jointly.
Defoaming agent in oxidation gel of the invention can inhibit the generation of foam in oxidation gel manufacturing process, facilitate system
Make.
Color indicator in oxidation gel of the invention is the color for aoxidizing gel and providing convenience identification, convenient for making
With.
Thickener in oxidation gel of the invention is to adjust viscosity of the oxidation gel under high-shear state, with thixotroping
Agent double together, adjusts the overall viscosity of oxidation gel.
Strong oxidizer is introduced into inorganic gel by the present invention, creatively can be with by strong oxidizer corrosivity
The outstanding rheologic behavio(u)r of inorganic gel combines, and forms oxidation sampling gel.
Oxidation gel of the invention can be widely applied to be sampled by the surface of the metal material of radioactive pollution and shallow-layer, single
Sub-sampling depth is up to a few micrometers.The oxidation gel is main sampling substance with strong oxidizer, can lead to using inorganic gel as carrier
It crosses spraying or brushes mode and be coated on metal surface.After spraying or brushing, the thixotropy of gel carrier makes to aoxidize gel in facade
It all will not sagging with top surface；And the strong oxidizer in gel and metal reaction are aoxidized, by the radiation of metal material surface or shallow-layer
Property nucleic with metal together corrosion dissolution to oxidation gel in, after gel drying to be oxidized collect, analyze.
In a preferred embodiment, the present invention is provided to the oxidation of radioactive pollution metal shallow-layer sampling is solidifying
Glue, wherein the gel base is selected from one of lithium magnesium silicate, calcium oxide or silica or a variety of combinations.
In a preferred embodiment, the present invention is provided to the oxidation of radioactive pollution metal shallow-layer sampling is solidifying
Glue, wherein the surfactant is selected from CH3(CH2)5(OCH2CH2)2OH, AT904 (contain the limited public affairs of environment-friendly materials in Shenzhen new Asia
Department) or one of alkyl diphenyl ether disulfonate or a variety of combinations.
In a preferred embodiment, the present invention is provided to the oxidation of radioactive pollution metal shallow-layer sampling is solidifying
Glue, wherein the thixotroping multiplication agent is selected from Y1010 (Shanghai Ying Jia industry development Co., Ltd), T2-815 (Guangzhou Teng Tang
Chemical Co., Ltd.) or one of rilanit special or a variety of combinations.
In a preferred embodiment, the present invention is provided to the oxidation of radioactive pollution metal shallow-layer sampling is solidifying
Glue, wherein the strong oxidizer is selected from one of two ammino silver of Hexammine cobaltic chloride, ammonium ceric nitrate or chlorination or a variety of
Combination.
In a preferred embodiment, the present invention is provided to the oxidation of radioactive pollution metal shallow-layer sampling is solidifying
Glue, wherein the acid is selected from nitric acid and/or hydrochloric acid.
In a preferred embodiment, the present invention is provided to the oxidation of radioactive pollution metal shallow-layer sampling is solidifying
Glue, wherein defoaming agent of the oxidation gel also containing weight percent 0.1-3%, selected from XWC-7100, (Hefei is ten thousand one-tenth new
Environmental Protection Technology Co., Ltd), one of n-octyl alcohol or silicone emulsion or a variety of combinations.
In a preferred embodiment, the present invention is provided to the oxidation of radioactive pollution metal shallow-layer sampling is solidifying
Glue, wherein color indicator of the oxidation gel also containing weight percent 0.1-0.5%, is selected from methylene blue, two
Amine sodium sulfonate or pyrimidine close one of ruthenium or a variety of combinations.
In a preferred embodiment, the present invention is provided to the oxidation of radioactive pollution metal shallow-layer sampling is solidifying
Glue, wherein thickener of the oxidation gel also containing weight percent 0.1-2%, is selected from HK-315 (the green perseveranceization in Guangzhou
Work Co., Ltd) and/or diethylene glycol monohexyl ether.
A second object of the present invention is to provide the preparation methods of aforementioned oxidation gel, can preferably prepare aforementioned oxygen
Change gel, the oxidation gel being prepared being capable of more acurrate, smooth, controllable, the intuitive shallow-layer for being used for radioactive pollution metal
Sampling, and reduce radiation injury of the sampling process to operator.
In order to achieve this, the present invention provides the preparation method of aforementioned oxidation gel, described in the embodiment on basis
Preparation method include the following steps:
(1) gel base of formula ratio is added in the water of formula ratio, is sufficiently stirred and emulsifies to uniform；
(2) be added gel base, water, surfactant, other formula ratios outside thixotroping multiplication agent ingredient and mix equal
It is even；
(3) it agent and is uniformly mixed using the preceding surfactant that formula ratio is added, thixotroping multiplication.
The beneficial effects of the present invention are solidifying using the oxidation for the sampling of radioactive pollution metal shallow-layer of the invention
Glue, the shallow-layer sampling that more acurrate, smooth, controllable, intuitive can be used for radioactive pollution metal, and sampling process is reduced to behaviour
Make the radiation injury of personnel.
Beneficial effects of the present invention are embodied in:
(1) oxidation gel chemistries ingredient is simple and clear and definite, framework material can be removed by the method for filtering, remaining gold
Belong to element and radionuclide clear and definite, will not influence feasibility and accuracy that subsequent physical, chemistry, radiology are analyzed；
(2) oxidation gel corrodes uniform, non-selectivity in sampling, for each metallic element, corrodes non-selectivity, from
And it can guarantee the accuracy of sampling；And sampling is without passivation phenomenon, it is ensured that sampling is gone on smoothly；
(3) oxidation gel depth selection is controllable, and depth selection is only related with its dosage and action time, and in effect
Between after abundance, depth selection is substantially linear with amount of gel, this feature ensure that the controllability of depth selection (see figure
1,2)；
(4) oxidation gel sampling result is intuitive, convenient for differentiating: for oxidation gel after acting on 2h, partial gel has discoloration existing
As occurring；After acting on 5-6h, completely, gel failure, this phenomenon can also be used to judge that gel has sampled for the gel discoloration smeared
At time；
(5) cooperate corresponding spraying equipment and collecting device, oxidation gel sampling can remotely operate, this is suitable for dosage rate
The metal sampler of higher environment works.
Detailed description of the invention
Fig. 1 is the relational graph for the sampling oxidation amount of gel and metal average corrosion thickness that measurement obtains in embodiment 1.
Fig. 2 is the relational graph for the sampling oxidation amount of gel and metal average corrosion thickness that measurement obtains in embodiment 2.
Specific embodiment
A specific embodiment of the invention is further illustrated with reference to embodiments.
Embodiment 1: the preparation of gel and its measurement (one) to stainless steel depth selection, sampling accuracy are aoxidized
The formula composition of oxidation gel manufactured in the present embodiment by weight percentage is as follows:
Gel base calcium oxide 15%, surfactant CH3(CH2)5(OCH2CH2)2OH is 5%, thixotroping multiplication agent Y1010
It is 5%, strong oxidizer ammonium ceric nitrate 20%, nitric acid 20%, surplus is that water (since ammonium ceric nitrate itself has bright-colored, blisters
Situation is slight, modest viscosity, and so there is no need to add color indicator, defoaming agent and thickener).
Aoxidize gel specific the preparation method is as follows:
(1) gel base of formula ratio is added in the water of formula ratio, is sufficiently stirred and emulsifies to uniform；
(2) be added gel base, water, surfactant, other formula ratios outside thixotroping multiplication agent ingredient and mix equal
It is even, it seals up for safekeeping stand-by；
(3) it agent and is uniformly mixed using the preceding surfactant that formula ratio is added, thixotroping multiplication.
By blade coating after the oxidation gel defoaming of above method preparation in 304 stainless steel surfaces, to measure the pollution of its shallow-layer
Situation scratches area 50cm2.The stainless steel plate length 8m, width 5m, thickness 6mm.Oxidation gel is completely dry after effect 4 hours
It is dry, constant volume in the nitric acid (mass percent concentration 40%) of 1000ml is collected and be dissolved in, is surveyed using spectrophotometer method
Determine (the reference: Liu Guicheng, Xue An, Chen Cuihong etc., the measurement skill of higher concentration iron under the conditions of concentrated acid of iron concentration in acid solution
Art, Hebei chemical industry, in June, 2006, the 6th phase of volume 2, the 47-48 pages), according to ion concentration inverse Corrosion of Stainless Steel quality and
Corrosion depth.Field sampling environmental condition are as follows: relative humidity 65%, 10 DEG C of temperature.Sampling test carries out three groups altogether, acquired results
Data are shown in Fig. 1.As seen from Figure 1, when other conditions are identical, the corrosion thickness (i.e. depth selection) and gel of oxidation sampling gel are used
Amount is substantially linear, which is conducive to the realization of quantitative sampling.
In addition, oxidation gel prepared by the above method also to be used to sample the measurement of accuracy, the specific method is as follows.
For putting a laboratory Decommissioning engineering, to a carbon steel bucket (measurement shows that the carbon outer wall of steel drum cleaning is pollution-free)
Acid soak samples two kinds of sampling modes after the sampling of oxidation gel and cutting is respectively adopted in inner wall, analyzes its pollution condition.Oxidation
When gel samples, the carbon inner walls of steel drums of a certain amount of oxidation gel to certain area is smeared, control depth selection is 2 μm, wait fill
After dividing reaction, aoxidizing complete, color change, scraping collection, which all aoxidizes, samples gels, retains to be analyzed.Cut acidleach sampling
When, the carbon steel bucket wall of certain area is extracted using angle grinder, and the carbon steel block cut is integrally immersed in acid solution and is corroded, will be corroded
It is deep-controlled at 2 μm, corrosive liquid is retained to be analyzed.
Deliver two sample of putting lab analysis, analysis the result shows that: radionuclide amount is substantially suitable in two samples,
It is slightly lower to cut the sample radioactivity radionuclide content that the acid-hatching of young eggs obtains, it may be possible to which the reasons such as vibration when cutting cause surface loosely dirty
Dye fall off and caused by.
Embodiment 2: the preparation of gel and its measurement (two) to stainless steel depth selection, sampling accuracy are aoxidized
The formula composition of oxidation gel manufactured in the present embodiment by weight percentage is as follows:
Gel base silica 5%, surfactant A T904 are 10%, and thixotroping multiplication agent T2-815 is 0.5%, by force
Oxidant Hexammine cobaltic chloride 3%, hydrochloric acid 3%, defoaming agent n-octyl alcohol 3%, two amine sodium sulfonates 0.5% of color indicator,
Thickener diethylene glycol monohexyl ether 0.1%, surplus is water.
Aoxidize gel specific the preparation method is as follows:
(1) gel base of formula ratio is added in the water of formula ratio, is sufficiently stirred and emulsifies to uniform；
(2) be added gel base, water, surfactant, other formula ratios outside thixotroping multiplication agent ingredient and mix equal
It is even, it seals up for safekeeping stand-by；
(3) it agent and is uniformly mixed using the preceding surfactant that formula ratio is added, thixotroping multiplication.
By blade coating after the oxidation gel defoaming of above method preparation in 304 stainless steel surfaces, to measure the pollution of its shallow-layer
Situation scratches area 50cm2.The stainless steel plate length 8m, width 5m, thickness 6mm.Oxidation gel is completely dry after effect 4 hours
It is dry, constant volume in the nitric acid (mass percent concentration 40%) of 1000ml is collected and be dissolved in, is surveyed using spectrophotometer method
Determine (the reference: Liu Guicheng, Xue An, Chen Cuihong etc., the measurement skill of higher concentration iron under the conditions of concentrated acid of iron concentration in acid solution
Art, Hebei chemical industry, in June, 2006, the 6th phase of volume 2, the 47-48 pages), according to ion concentration inverse Corrosion of Stainless Steel quality and
Corrosion depth.Field sampling environmental condition is shown in Fig. 2 with embodiment 1, acquired results data.From Figure 2 it can be seen that other conditions are identical
When, the corrosion thickness (i.e. depth selection) and amount of gel of oxidation sampling gel are substantially linear, and the linear relationship is advantageous
In the realization of quantitative sampling.
In addition, oxidation gel prepared by the above method also to be used to sample the measurement of accuracy, method and result are the same as real
Apply example 1.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.If in this way, belonging to the model of the claims in the present invention and its equivalent technology to these modifications and changes of the present invention
Within enclosing, then the present invention is also intended to include these modifications and variations.Above-described embodiment or embodiment are only to the present invention
For example, the present invention can also be implemented with other ad hoc fashions or other particular form, without departing from of the invention
Main idea or substantive characteristics.Therefore, the embodiment of description is regarded as illustrative and non-limiting in any way.This
The range of invention should be illustrated that any variation equivalent with the intention and range of claim also should include by appended claims
Within the scope of the invention.
Claims (10)
1. the oxidation gel for the sampling of radioactive pollution metal shallow-layer, which is characterized in that the oxidation gel by weight hundred
Ratio is divided to contain: the gel base as gelatum skeleton material of 5-15%, the surfactant of 5-10%, the thixotroping of 0.5-5%
Double agent, the strong oxidizer of 3-20%, the acid of 3-20% and the water of surplus.
2. oxidation gel according to claim 1, it is characterised in that: the gel base is selected from lithium magnesium silicate, oxidation
One of calcium or silica or a variety of combinations.
3. oxidation gel according to claim 1, it is characterised in that: the surfactant is selected from CH3(CH2)5
(OCH2CH2)2One of OH, AT904 or alkyl diphenyl ether disulfonate or a variety of combinations.
4. oxidation gel according to claim 1, it is characterised in that: the thixotroping multiplication agent is selected from Y1010, T2-815
Or one of rilanit special or a variety of combinations.
5. oxidation gel according to claim 1, it is characterised in that: the strong oxidizer is selected from six ammino of tri-chlorination
One of two ammino silver of cobalt, ammonium ceric nitrate or chlorination or a variety of combinations.
6. oxidation gel according to claim 1, it is characterised in that: the acid is selected from nitric acid and/or hydrochloric acid.
7. oxidation gel according to claim 1, it is characterised in that: the oxidation gel also contains weight percent
The defoaming agent of 0.1-3%, selected from one of XWC-7100, n-octyl alcohol or silicone emulsion or a variety of combinations.
8. oxidation gel according to claim 1, it is characterised in that: the oxidation gel also contains weight percent
The color indicator of 0.1-0.5% closes one of ruthenium or a variety of groups selected from methylene blue, two amine sodium sulfonates or pyrimidine
It closes.
9. oxidation gel according to claim 1, it is characterised in that: the oxidation gel also contains weight percent
The thickener of 0.1-2% is selected from HK-315 and/or diethylene glycol monohexyl ether.
10. the preparation method of gel is aoxidized described in any one of -9 according to claim 1, which is characterized in that the system
Preparation Method includes the following steps:
(1) gel base of formula ratio is added in the water of formula ratio, is sufficiently stirred and emulsifies to uniform；
(2) be added gel base, water, surfactant, thixotroping multiplication agent outside other formula ratios ingredient and be uniformly mixed；
(3) it agent and is uniformly mixed using the preceding surfactant that formula ratio is added, thixotroping multiplication.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112760659A (en) * | 2020-12-02 | 2021-05-07 | 中国辐射防护研究院 | Oxidation decontamination gel and preparation method and application thereof |
| CN113481065A (en) * | 2021-06-18 | 2021-10-08 | 中国辐射防护研究院 | Foam gel and preparation method thereof |
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