CN110277182A - Corrosivity for iron-based material surface is from crisp type decontamination agent preparation method - Google Patents
Corrosivity for iron-based material surface is from crisp type decontamination agent preparation method Download PDFInfo
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- CN110277182A CN110277182A CN201910525642.6A CN201910525642A CN110277182A CN 110277182 A CN110277182 A CN 110277182A CN 201910525642 A CN201910525642 A CN 201910525642A CN 110277182 A CN110277182 A CN 110277182A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
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- 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
- G21F9/001—Decontamination of contaminated objects, apparatus, clothes, food; Preventing contamination thereof
-
- 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
Abstract
The invention belongs to radioactive decontamination technical field, a kind of corrosivity for iron-based material surface is disclosed from the preparation method of crisp type decontamination agent, uses silica for inorganic component, silica is modified by Silane coupling agent KH550；Using methyl methacrylate, methacrylic acid, trifluoroethyl methacrylate ternary atactic copolymer as organic component, by organic/inorganic it is compound prepare it is compound from brittleness detergent；It is compounded again with etching components such as nitric acid, preparation is obtained for the corrosivity of carbon steel and stainless steel from crisp type decontamination agent.Detergent of the present invention is directed to the strong qualitative radioactive pollutant of ferrous metals material surface, by corrosive component by ferrous metals surface damage, pollutant is adsorbed and is wrapped up by detergent, is formed crisp chip after dry embrittlement and is voluntarily removed, to realize the removal for ferrous metals surface radioactive pollutant.
Description
Technical field
The invention belongs to radioactive decontamination technical field more particularly to a kind of corrosivity for iron-based material surface from crisp
Type decontamination agent preparation method.
Background technique
Currently, the immediate prior art:
Compared to traditional energies such as coal, petroleum, nuclear energy has high energy density, and nuclear fuel is stored up with minimum volume
Huge energy and energy controlled release are deposited, therefore has just been applied rapidly since it is found.On the utilization of nuclear energy originates in
Century four the fifties, moved back so there are a large amount of nuclear facilities in worldwide at present due to reaching service life
It uses as a servant or prepares retired.Meanwhile using the production, scientific research and technological transformation of nuclear energy still in continuous carry out, therefore generate a large amount of
By the metal material of radionuclide contamination.These by the retired metal equipment of radionuclide contamination, such as: nuclear industry is set
Standby, nuclear material storage container, metallic conduit, valve, metallic weapon, instrument and tool etc. are exposed under radionuclide for a long time,
Its radioactive pollution situation is more complicated, and the radioactive contamination different from other materials is polluted, and radioactive pollutant is not only simple
It is singly attached to metal surface, is also invaded in matallic surface layer.A large amount of practical study shows: more than putting for overwhelming majority pollution
Penetrating property nucleic is present in ten micrometer depth ranges of metal surface, and within the scope of ten micrometer depth of metal surface ten to four only
In the presence of be lower than 2 percent contaminating radioactivity nucleic, the existing radionuclide in the depth bounds of metal surface deeper
It is then less, it can ignore substantially relative to nucleic total amount of pollutants discharge.Therefore the radioactive pollutant of metal material surface is gone
Except to be destroyed to metal surface, to achieve the purpose that deep-pollution-removing, in general when decontamination depth reaches 10 μm, substantially
It can be realized the decontamination for contaminated metal material surface layer.The metal surface radioactive decontamination method of mature has very at present
It is more, usually it is divided into two class of physical method and chemical method according to action principle.Physical technology of removing pollution method is primarily referred to as passing through mechanical grinding
The method that the physical means such as mill, ultrasound, laser, melting are removed metal surface radioactive pollution, common physical method
Mainly there are melting decontamination, laser decontamination, mechanical lapping decontamination, injection decontamination and supersonic wave decontamination etc..Common chemical method master
There are chemical cleaning decontamination, electrochemical decontamination, foam decontamination, gel decontamination, membrane body decontamination and supercritical fluid decontamination etc..With regard to mesh
For preceding various decontamination technologies, various technologies are had some limitations.
It is the new development of chemical membrane body decontamination technology from crisp type decontamination technology, membrane body is sent out after detergent membrane body adsorbs pollutant
Raw embrittlement, peels off naturally and achievees the purpose that decontamination.Compared to general chemical decontamination method, waste minimization original was both met
Then, and irradiation injury to human body can be reduced by mechanical collection.Detergency mechanism from crisp type decontamination method is to pass through decontamination
The flexibility radioactive pollution on the complexing removal surface of the suction-operated and complexing agent of agent membrane body, it cannot be used for
Except the stationarity radioactive pollution of metal surface.And the organic matters such as P (MMA-co-MAA) and P (MMA-b-MAA) acid and alkali-resistance is rotten
Corrosion is poor, can not realize the function from crisp type detergent corrosion metal surface by the way that the corrosive components such as soda acid are added.
In conclusion problem of the existing technology is:
The existing stationarity radioactive pollutant that removal metal material surface is not used to from crisp type detergent, removal effect
Rate is low.
And the organic matters acid-alkali-corrosive-resisting such as P (MMA-co-MAA) and P (MMA-b-MAA) is poor, and it can not be by the way that acid be added
The corrosive components such as alkali realize the function from crisp type detergent corrosion metal surface.
There are secondary amount of waste for existing metal surface radioactive pollution decontamination method greatly, is unable to remote mechanical operation, after
The problems such as treatment process difficulty is big.
Solve the difficulty of above-mentioned technical problem:
(1) will from crisp type detergent corrode functionalization, realize to ferrous metals material surface corrosivity decontamination while,
Be able to maintain again detergent from brittleness energy, be one of difficult point of the invention.
(2) by introducing inorganic particle and the compound corrosion resistance improved from crisp type detergent of polymer, guarantee decontamination
The corrosion resistance of agent system and from brittleness can be the two of difficult point of the invention.
Solve the meaning of above-mentioned technical problem:
Corrosivity is prepared from crisp type decontamination agent by the way that functionalization will be corroded from crisp type detergent, is had both from crisp type and is gone
The dirty secondary amount of waste of method is few, can remote mechanical operation the advantages of, and the radioactive pollutant in matallic surface layer can be removed.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of corrosivity for iron-based material surface from crisp type
Decontamination agent preparation method.
The invention is realized in this way a kind of system of corrosivity for iron-based material surface from crisp type decontamination agent
Preparation Method uses silica for inorganic component, is modified by silane coupling agent to silica.
It is to have unit with methyl methacrylate, methacrylic acid, trifluoroethyl methacrylate ternary atactic copolymer
Point, by organic/inorganic it is compound prepare it is compound from brittleness detergent.
It is compounded again with etching components such as nitric acid, preparation obtains going for the corrosivity of carbon steel and stainless steel from crisp type radioactivity
Dirty agent.
Further, the compound preparation method from brittleness detergent includes: that anhydrous second is added in polytetrafluoroethylene (PTFE) ball grinder
The mixed liquor of pure and mild deionized water sequentially adds 30nm silica, Silane coupling agent KH550 and emulsifier.By ball milling zirconium
Ball milling zirconium pearl is added in pearl and silica quality ratio 10:1, and it is outstanding to obtain improved silica for separating zirconium pearl after 45~60min of ball milling
Supernatant liquid.The random copolymer solution of synthesis is added into suspension, shears 3~5min of dispersion using high-speed emulsifying machine, is made multiple
Mould assembly is from brittleness detergent.
Further, the mixed liquor dosage is 72~73 parts.30nm silica content is 14~15 parts.Random copolymer
Solution usage is 7~7.5 parts.KH550 dosage is 1~1.5 part.Emulsifier is 3~3.5 parts.
Further, the random copolymer solution preparation method the following steps are included:
The first step, the preparation of monomer solution: weighing methyl methacrylate and methacrylic acid in beaker, uses high speed
Mulser shearing is uniformly dispersed, and forms mixed monomer solution, then take trifluoroethyl methacrylate in another beaker.
The preparation of initiator solution: second step azodiisobutyronitrile is dissolved in beaker with hot dehydrated alcohol, with ultrasound
Wave is uniformly mixed, and forms initiator solution.
Third step, the synthesis of random copolymer: being added dehydrated alcohol in the four-hole boiling flask equipped with blender, and 75~78 DEG C
Lower stirring is added dropwise methyl methacrylate into four-hole boiling flask simultaneously with constant pressure funnel and methacrylic acid mix monomer is molten
The initiator of liquid and preparation, control time for adding react 3~4h in 30min or so after dripping off, metering system is added in property again
Sour trifluoro ethyl ester reacts 3~4h, discharges after cooling.
Monomer 1 is methyl methacrylate dosage in the first step: 60~65 parts.Monomer 2 is methacrylic acid dosage:
25~30 parts.Monomer 3 is trifluoroethyl methacrylate: 8~10 parts.
Dosage of azodiisobutyronitrile in the second step: 1~2 part, dosage is the 0.69~1.43% of monomer gross mass.Nothing
Water-ethanol dosage: 128~132 parts, dosage is the 88.28~94.62% of monomer gross mass.
Another object of the present invention is to provide a kind of utilization iron-based material surface corrosion from crisp type radioactive decontamination
The preparation method of agent is prepared compound from brittleness detergent.
Further, the preparation method of carbon steel surface corrosion from crisp type decontamination agent includes: using 65~68%
Concentrated nitric acid prepares 5mol/L dust technology, and the 5mol/L dust technology of preparation is added in beaker, adds nitric acid corrosion inhibiter, at 30 DEG C
Stirring is completely dissolved under water-bath, obtains corrosion of carbon steel agent.Take preparation it is compound from brittleness detergent in beaker, add carbon
Steel corrosion agent, 15~20min of stirring are allowed to uniformly mixed, and corrosion of carbon steel is made from crisp type decontamination agent.
Further, it is compound from brittleness detergent dosage be 85~90 parts.5mol/L dust technology dosage is 10~15 parts.Nitre
Acid inhibitor dosage is 0.4~1.2 part.
Another object of the present invention is to provide a kind of iron-based material surface corrosions from crisp type decontamination agent
Preparation method preparation corrosion of carbon steel from crisp type decontamination agent.
Further, stainless steel surface corrosivity from crisp type decontamination agent preparation method include: using 65~68%
Concentrated nitric acid prepares 5mol/L dust technology, and the 5mol/L dust technology of preparation is added in beaker, adds sodium chloride, in 30 DEG C of water-baths
Lower stirring is completely dissolved.Iron chloride is added after being cooled to room temperature, stirs to being completely dissolved, obtains faint yellow Corrosion of Stainless Steel agent.
Take preparation it is compound from brittleness detergent in beaker, add Corrosion of Stainless Steel agent, it is equal that 15~20min of stirring is allowed to mixing
It is even, Corrosion of Stainless Steel is made from crisp type decontamination agent.
It is compound from brittleness detergent dosage be 75~80 parts.5mol/L dust technology dosage is 15~20 parts.Iron chloride is used
Amount is 0.25-1.75 parts.Sodium chloride dosage is 0.1~0.35 part.
It is gone using the iron-based material surface corrosion from crisp type radioactivity another object of the present invention is to provide a kind of
The stainless steel surface corrosivity of the preparation method preparation of dirty agent is from crisp type decontamination agent.
In conclusion advantages of the present invention and good effect are as follows:
Iron-based material surface corrosion provided by the invention is from the preparation method of crisp type decontamination agent, for iron-based gold
Belong to the strong qualitative radioactive pollutant of material surface, it, will by corrosive component after contaminated metal surface sprays detergent
Pollutant is adsorbed and is wrapped up by ferrous metals surface damage, detergent, is formed crisp chip after dry embrittlement and is voluntarily removed, thus realization pair
In the removal of ferrous metals surface radioactive pollutant.Corrosivity has both from crisp type decontamination agent from crisp type decontamination method two
Secondary amount of waste is few, can remote mechanical operation the advantages of, and the radioactive pollutant in matallic surface layer can be removed.The present invention carries out
Development of the iron-based material surface corrosion from crisp type decontamination agent.The detergent is quasi- by compound from brittleness detergent and rotten
Corrosion component compounds: using silica for inorganic component, is changed by Silane coupling agent KH550 to silica
Property, using P (MMA-co-MAA-co-TFEMA) random copolymer as organic component, by organic/inorganic it is compound prepare it is compound from
Brittleness detergent is improved with inorganic component from crisp type detergent acid resistance.It is compounded again with etching components such as nitric acid, preparation is used
In the corrosivity of carbon steel and stainless steel from crisp type decontamination agent.Iron-based material surface corrosion of the invention is radiated from crisp type
Property detergent by the way that functionalization will be corroded from crisp type detergent, after being coated on contaminated metal surface, etching component is by metal
Surface damage, pollutant are adsorbed by detergent and are wrapped up, and are voluntarily fallen off with the dry embrittlement of detergent, and crisp by mechanical collection
Piece, not only had many advantages, such as secondary amount of waste it is few, can remote mechanical operation, but also metal surface deep layer radioactive pollution can be carried out
Removal.
Detergent of the present invention is directed to the strong qualitative radioactive pollutant of ferrous metals material surface, will by corrosive component
Pollutant is adsorbed and is wrapped up by ferrous metals surface damage, detergent, is formed crisp chip after dry embrittlement and is voluntarily removed, thus realization pair
In the removal of ferrous metals surface radioactive pollutant.Corrosivity has both from crisp type decontamination agent from crisp type decontamination method two
Secondary amount of waste is few, can remote mechanical operation the advantages of, and the radioactive pollutant in matallic surface layer can be removed.
Detailed description of the invention
Fig. 1 is system of the corrosivity provided in an embodiment of the present invention for iron-based material surface from crisp type decontamination agent
Preparation Method flow chart.
Fig. 2 is the preparation method flow chart of random copolymer solution provided in an embodiment of the present invention.
Fig. 3 is iron-based material surface layer provided in an embodiment of the present invention corrosivity from crisp type detergent from crisp shape appearance figure.In figure:
A, carbon steel surface；B, stainless steel surface.
Fig. 4 is the carbon steel and stainless steel surface macro morphology figure of detergent corrosion provided in an embodiment of the present invention front and back.
Fig. 5 is the carbon steel and stainless steel surface topography figure of detergent corrosion provided in an embodiment of the present invention front and back.
Fig. 6 is the three-dimensional microphoto of corrosion tomography provided in an embodiment of the present invention.In figure: (a) plan view；(b) three-dimensional
Figure.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The problem of existing radioactive pollutant that removal metal material surface is not used to from crisp type detergent.
To solve the above problems, being described in detail with reference to the accompanying drawing to technical solution of the present invention.
As shown in Figure 1, the embodiment of the present invention is used for system of the iron-based material surface corrosion from crisp type decontamination agent
Preparation Method is in terms of 100 parts by the compound quality from brittleness detergent of synthesis, comprising the following steps:
S101: it is compound from brittleness detergent preparation method: polytetrafluoroethylene (PTFE) ball grinder be added dehydrated alcohol and go from
The mixed liquor (volume ratio 3:1) of sub- water, sequentially adds 30nm silica, Silane coupling agent KH550 and emulsifier, by ball
It grinds zirconium pearl and silica quality ratio 10:1 and is added ball milling zirconium pearl, 45~60min of ball milling (400 revs/min) separating zirconium pearl afterwards obtains
To improved silica suspension, the random copolymer solution of synthesis is added into suspension, uses high-speed emulsifying machine shearing point
It dissipates 3~5min (10000 revs/min), is made compound from brittleness detergent.Mixed liquor dosage: 72~73 parts.30nm titanium dioxide
Silicon dosage: 14~15 parts.Random copolymer solution dosage: 7~7.5 parts.KH550 dosage: 1~1.5 part.Emulsifier: 3-
3.5 part.
S102: carbon steel surface corrosion is from crisp type decontamination agent preparation method: being matched using 65~68% concentrated nitric acid
The 5mol/L dust technology of preparation is added in beaker, adds nitric acid corrosion inhibiter, stirs under 30 DEG C of water-baths for 5mol/L dust technology processed
It mixes and is completely dissolved, obtain corrosion of carbon steel agent.Take preparation it is compound from brittleness detergent in beaker, add corrosion of carbon steel
Agent, 15~20min of stirring are allowed to uniformly mixed, and corrosion of carbon steel is made from crisp type decontamination agent.It is compound to be gone from brittleness
Dirty agent dosage: 85~90 parts.5mol/L dust technology dosage: 10~15 parts.Nitric acid inhibiter consumption: 0.4-1.2 parts.
S103: stainless steel surface corrosivity is from crisp type decontamination agent preparation method: using 65~68% concentrated nitric acid
5mol/L dust technology is prepared, the 5mol/L dust technology of preparation is added in beaker, adds sodium chloride, is stirred under 30 DEG C of water-baths
It is completely dissolved, iron chloride (FeCl is added after being cooled to room temperature3·6H2O), it is rotten to obtain faint yellow stainless steel to being completely dissolved for stirring
Lose agent.Take preparation it is compound from brittleness detergent in beaker, add Corrosion of Stainless Steel agent, 15~20min of stirring is allowed to
It is uniformly mixed, Corrosion of Stainless Steel is made from crisp type decontamination agent.It is compound from brittleness detergent dosage: 75~80 parts.
5mol/L dust technology dosage: 15~20 parts.Iron chloride dosage: 0.25-1.75 parts.Sodium chloride dosage: 0.1~0.35 part.
As shown in Fig. 2, the preparation method of the random copolymer solution in step S101, comprising the following steps:
S201: the preparation of monomer solution weighs methyl methacrylate and methacrylic acid in beaker, uses high speed cream
The shearing of change machine is uniformly dispersed, and forms mixed monomer solution, then take trifluoroethyl methacrylate in another beaker.Monomer 1
That is methyl methacrylate dosage: 60~65 parts.Monomer 2 is methacrylic acid dosage: 25~30 parts.Monomer 3 is metering system
Sour trifluoro ethyl ester: 8~10 parts.
S202: azodiisobutyronitrile is dissolved in beaker with hot dehydrated alcohol, uses ultrasonic wave by the preparation of initiator solution
It is uniformly mixed, forms initiator solution.Dosage of azodiisobutyronitrile: 1~2 part, dosage be monomer gross mass 0.69~
1.43%.Dehydrated alcohol dosage: 128~132 parts, dosage is the 88.28~94.62% of monomer gross mass.
S203: dehydrated alcohol is added in the four-hole boiling flask equipped with blender in the synthesis of random copolymer, at 75~78 DEG C
Methyl methacrylate and methacrylic acid mixed monomer solution is added dropwise with constant pressure funnel in stirring into four-hole boiling flask simultaneously
With the initiator of preparation, time for adding is controlled in 30min or so, 3~4h is reacted after dripping off, methacrylic acid is added in property again
Trifluoro ethyl ester reacts 3~4h, discharges after cooling.
Technical scheme of the present invention will be further described combined with specific embodiments below.
Embodiment 1
Resins synthesis provided in an embodiment of the present invention includes:
1) methyl methacrylate (MMA) 120.00g, methacrylic acid (MAA) preparation of monomer solution: are weighed
50.00g, trifluoroethyl methacrylate (TFEMA) 15.90g, MMA and MAA high speed shear are uniformly mixed spare, and TFEMA is mono-
It is solely placed in a beaker spare.
2) preparation of initiator solution: AIBN 1.95g 100mL hot ethanol is dissolved, spare after ultrasonic disperse.
3) synthesis of resin: 900mL dehydrated alcohol being added in 2000mL four-hole boiling flask, stirs under 75 DEG C of water bath conditions,
Methyl methacrylate and methacrylic acid mixed monomer solution and system is added dropwise into four-hole boiling flask simultaneously with constant pressure funnel
Standby initiator, control time for adding react 3~4h in 30min or so after dripping off, methacrylic acid trifluoro is added in property again
Ethyl ester reacts 3~4h, discharges after cooling.
Embodiment 2
The preparation of iron-based material surface layer provided in an embodiment of the present invention corrosivity from crisp type decontamination agent includes:
1) compound from brittleness detergent preparation method: polytetrafluoroethylene (PTFE) ball grinder be added 100g dehydrated alcohol and go from
The mixed liquor (volume ratio 3:1) of sub- water sequentially adds 20g 30nm silica, 2g Silane coupling agent KH550 and 5g cream
Ball milling zirconium pearl is added by ball milling zirconium pearl and silica quality ratio 10:1 in agent, and 45~60min of ball milling (400 revs/min) divides afterwards
From zirconium pearl, improved silica suspension is obtained, the random copolymer solution of 10g synthesis is added into suspension, uses high speed
Mulser shearing dispersion 3~5min (10000 revs/min), is made compound from brittleness detergent.
2) carbon steel surface corrosion is from crisp type decontamination agent preparation method: being prepared using 65~68% concentrated nitric acid
The 5mol/L dust technology that 10mL is prepared is added in 50mL beaker, adds 0.38g nitric acid corrosion inhibiter for 5mol/L dust technology,
It stirs and is completely dissolved under 30 DEG C of water-baths, obtain corrosion of carbon steel agent.The compound of 90mL preparation is taken to burn from brittleness detergent in 250mL
In cup, the corrosion of carbon steel agent of preparation is added, 15~20min of stirring is allowed to uniformly mixed, and corrosion of carbon steel is made and puts from crisp type
Penetrating property detergent.
3) stainless steel surface corrosivity is from crisp type decontamination agent preparation method: being prepared using 65~68% concentrated nitric acid
The 5mol/L dust technology that 20mL is prepared is added in 50mL beaker, 0.17g sodium chloride is added, at 30 DEG C for 5mol/L dust technology
Stirring is completely dissolved under water-bath, and 1.89g iron chloride (FeCl is added after being cooled to room temperature3·6H2O), stirring is obtained to being completely dissolved
To faint yellow Corrosion of Stainless Steel agent.Take 80mL prepare it is compound from brittleness detergent in 250mL beaker, add stainless steel
Corrosive agent, 15~20min of stirring are allowed to uniformly mixed, and Corrosion of Stainless Steel is made from crisp type decontamination agent.
Technical effect of the invention is further described below with reference to experiment.
Detergent embrittlement performance, detergency ability and corrosion depth evaluation of the present invention: choosing 50mm × 50mm sheet metal, will
For the detergent even application of preparation in metal sheet surface, detergent membrane body thickness is about 2mm, places go in 4~8 hours at room temperature
The dry embrittlement of dirty agent, the crisp chip of formation is having a size of 0.5~2cm.
The experimental program for pressing the safe book series of GB/T14057-93, IAEA 48 carries out the clean effect evaluation of detergent in fact
It tests.Choose 3~5 pieces of 50mm × 50mm sheet metal.Sample-out count is carried out using FJ2207 α β surface pollution measuring instrument.It is choosing
Metal sheet surface lay the active fall-outs of different radioactive surface activity and (mix and put in the horizontal soil powder of size selective sampling
Penetrating property element238U) and surface contamination level is measured.Detergent is sprayed in Polluted area, removes measurement surface radiation after detergent
Property residual level, the results showed that, using detergent once-used decontaminating rate > 97% prepared by the present invention.
The present invention tests the corrosion depth of detergent using weight-loss method.Choose 50mm × 50mm sheet metal 2~3
Block is weighed after cleaning is dry using assay balance.In the metal sheet surface even application detergent of selection, coating thickness is about
2mm is cleaned and dried metal plate after removing detergent, weighs again, calculates corrosion depth according to weight loss, the results showed that, this hair
The detergent of bright preparation can reach 2~4 μm to the corrosion depth of carbon steel and stainless steel.
Below with reference to specific experiment, the invention will be further described.
Table 1 it is compound from crisp type detergent to metal sheet surface radioactive dust (238U soil removal efficiency)
Fig. 3 is iron-based material surface layer provided in an embodiment of the present invention corrosivity from crisp type detergent from crisp shape appearance figure.In figure:
A, carbon steel surface；B, stainless steel surface.
Fig. 4 is the carbon steel and stainless steel surface macro morphology figure of detergent corrosion provided in an embodiment of the present invention front and back.
Fig. 5 is the carbon steel and stainless steel surface topography figure of detergent corrosion provided in an embodiment of the present invention front and back.
Fig. 6 is the three-dimensional microphoto of corrosion tomography provided in an embodiment of the present invention.In figure: (a) plan view；(b) three-dimensional
Figure.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of corrosivity for iron-based material surface is from the preparation method of crisp type decontamination agent, which is characterized in that institute
The preparation method for stating iron-based material surface corrosion from crisp type decontamination agent uses silica for inorganic component, passes through silicon
Alkane coupling agents for silica is modified；
Using methyl methacrylate, methacrylic acid, trifluoroethyl methacrylate ternary atactic copolymer as organic component, lead to
Cross organic/inorganic it is compound prepare it is compound from brittleness detergent；
It is compounded again with etching components such as nitric acid, preparation is obtained for the corrosivity of carbon steel and stainless steel from crisp type radioactive decontamination
Agent.
2. iron-based material surface corrosion as described in claim 1 is from the preparation method of crisp type decontamination agent, feature
It is, the compound preparation method from brittleness detergent includes: that dehydrated alcohol and deionization is added in polytetrafluoroethylene (PTFE) ball grinder
The mixed liquor of water sequentially adds 30nm silica, Silane coupling agent KH550 and emulsifier；By ball milling zirconium pearl and titanium dioxide
Ball milling zirconium pearl is added in silicon mass ratio 10:1, and separating zirconium pearl after 45~60min of ball milling obtains improved silica suspension；To outstanding
The random copolymer solution of synthesis is added in supernatant liquid, shears 3~5min of dispersion using high-speed emulsifying machine, is made compound from brittleness
Detergent.
3. iron-based material surface corrosion as claimed in claim 2 is from the preparation method of crisp type decontamination agent, feature
It is, the mixed liquor dosage is 72~73 parts；30nm silica content is 14~15 parts；Random copolymer solution dosage is
7~7.5 parts；KH550 dosage is 1~1.5 part；Emulsifier is 3~3.5 parts.
4. iron-based material surface corrosion as claimed in claim 2 is from the preparation method of crisp type decontamination agent, feature
Be, the preparation method of the random copolymer solution the following steps are included:
The first step, the preparation of monomer solution: weighing methyl methacrylate and methacrylic acid in beaker, is emulsified using high speed
Machine shearing is uniformly dispersed, and forms mixed monomer solution, then take trifluoroethyl methacrylate in another beaker；
Second step, the preparation of initiator solution: azodiisobutyronitrile is dissolved in beaker with hot dehydrated alcohol, mixed with ultrasonic wave
It closes uniformly, forms initiator solution；
The synthesis of random copolymer: third step is added dehydrated alcohol in the four-hole boiling flask equipped with blender, stirs at 75~78 DEG C
Mix, be added dropwise simultaneously into four-hole boiling flask with constant pressure funnel methyl methacrylate and methacrylic acid mixed monomer solution and
The initiator of preparation, control time for adding react 3~4h in 30min or so after dripping off, methacrylic acid three is added in property again
Fluorine ethyl ester reacts 3~4h, discharges after cooling；
Monomer 1 is methyl methacrylate dosage in the first step: 60~65 parts；Monomer 2 is methacrylic acid dosage: 25~
30 parts；Monomer 3 is trifluoroethyl methacrylate: 8~10 parts；
Dosage of azodiisobutyronitrile in the second step: 1~2 part, dosage is the 0.69~1.43% of monomer gross mass；Anhydrous second
Alcohol dosage: 128~132 parts, dosage is the 88.28~94.62% of monomer gross mass.
5. it is a kind of using iron-based material surface corrosion described in claim 2~4 any one from crisp type decontamination agent
Preparation method is prepared compound from brittleness detergent.
6. iron-based material surface corrosion as described in claim 1 is from the preparation method of crisp type decontamination agent, feature
It is, the preparation method of carbon steel surface corrosion from crisp type decontamination agent includes: to be prepared using 65~68% concentrated nitric acid
The 5mol/L dust technology of preparation is added in beaker, adds nitric acid corrosion inhibiter, stirs under 30 DEG C of water-baths for 5mol/L dust technology
It is completely dissolved, obtains corrosion of carbon steel agent；Take preparation it is compound from brittleness detergent in beaker, add corrosion of carbon steel agent,
15~20min of stirring is allowed to uniformly mixed, and corrosion of carbon steel is made from crisp type decontamination agent.
7. iron-based material surface corrosion as claimed in claim 6 is from the preparation method of crisp type decontamination agent, feature
Be, it is compound from brittleness detergent dosage be 85~90 parts；5mol/L dust technology dosage is 10~15 parts；Nitric acid corrosion inhibiter is used
Amount is 0.4~1.2 part.
8. a kind of iron-based material surface corrosion as claimed in claim 6 is prepared from the preparation method of crisp type decontamination agent
Corrosion of carbon steel is from crisp type decontamination agent.
9. iron-based material surface corrosion as described in claim 1 is from the preparation method of crisp type decontamination agent, feature
It is, stainless steel surface corrosivity includes: to be prepared using 65~68% concentrated nitric acid from crisp type decontamination agent preparation method
The 5mol/L dust technology of preparation is added in beaker, adds sodium chloride for 5mol/L dust technology, stirs under 30 DEG C of water-baths complete
Dissolution；Iron chloride is added after being cooled to room temperature, stirs to being completely dissolved, obtains faint yellow Corrosion of Stainless Steel agent；Take answering for preparation
Mould assembly in beaker, adds Corrosion of Stainless Steel agent from brittleness detergent, and 15~20min of stirring is allowed to uniformly mixed, is made not
Steel corrosion become rusty from crisp type decontamination agent；
It is compound from brittleness detergent dosage be 75~80 parts；5mol/L dust technology dosage is 15~20 parts；Iron chloride dosage is
0.25-1.75 parts；Sodium chloride dosage is 0.1~0.35 part.
10. it is a kind of using iron-based material surface corrosion described in claim 9 from the preparation method system of crisp type decontamination agent
Standby stainless steel surface corrosivity is from crisp type decontamination agent.
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| CN113957259A (en) * | 2021-10-25 | 2022-01-21 | 湖南核工业宏华机械有限公司 | Radioactive pollution waste metal smelting detergent |
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