CN110306232B - Decontamination method - Google Patents

Decontamination method Download PDF

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Publication number
CN110306232B
CN110306232B CN201910594306.7A CN201910594306A CN110306232B CN 110306232 B CN110306232 B CN 110306232B CN 201910594306 A CN201910594306 A CN 201910594306A CN 110306232 B CN110306232 B CN 110306232B
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China
Prior art keywords
decontaminated
decontamination
piece
workpiece
oxalate
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CN201910594306.7A
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CN110306232A (en
Inventor
洪振旻
王浩宇
姜磊
张宇宏
赵滢
张惠炜
何小平
秦体照
何继强
彭珍琳
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China General Nuclear Power Corp
CGN Power Co Ltd
Daya Bay Nuclear Power Operations and Management Co Ltd
Lingdong Nuclear Power Co Ltd
China Nuclear Power Operation Co Ltd
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China General Nuclear Power Corp
CGN Power Co Ltd
Daya Bay Nuclear Power Operations and Management Co Ltd
Lingdong Nuclear Power Co Ltd
China Nuclear Power Operation Co Ltd
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Application filed by China General Nuclear Power Corp, CGN Power Co Ltd, Daya Bay Nuclear Power Operations and Management Co Ltd, Lingdong Nuclear Power Co Ltd, China Nuclear Power Operation Co Ltd filed Critical China General Nuclear Power Corp
Priority to CN201910594306.7A priority Critical patent/CN110306232B/en
Publication of CN110306232A publication Critical patent/CN110306232A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/10Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00Electrolytic cleaning, degreasing, pickling or descaling
    • C25F1/02Pickling; Descaling
    • C25F1/04Pickling; Descaling in solution
    • C25F1/06Iron or steel
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F7/00Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Cleaning By Liquid Or Steam (AREA)

Abstract

The present invention relates to a decontamination method. The decontamination method comprises the following steps: placing a piece to be decontaminated in a decontamination composition, and carrying out ultrasonic and electrolytic treatment on the piece to be decontaminated, wherein the raw material for preparing the decontamination composition comprises HNO with the volume percentage of 2-5 percent310 to 30 percent of glycerol, 80 to 140g/L of nitrate and 5 to 25g/L of oxalate. The decontamination method has good decontamination effect.

Description

Decontamination method
Technical Field
The invention relates to the field of nuclear environment protection, in particular to a decontamination method.
Background
In nuclear-related equipment maintenance, stainless steel components are often contaminated with various radioactive materials. The presence of these radioactive materials can affect the normal use of the equipment, and these radioactive materials may be contaminated and amplified with the activities of people, thereby bringing about safety hazards to workers and the environment. At present, the common decontamination process has poor decontamination effect on stainless steel, and influences the normal use of stainless steel parts.
Disclosure of Invention
Therefore, a decontamination method with good decontamination effect is needed.
A method of decontamination comprising the steps of:
placing a piece to be decontaminated in a decontamination composition, and carrying out ultrasonic and electrolytic treatment on the piece to be decontaminated, wherein the raw material for preparing the decontamination composition comprises HNO with the volume percentage of 2-5 percent310 to 30 percent of glycerol, 80 to 140g/L of nitrate and 5 to 25g/L of oxalate.
In the decontamination method, the nitrate, oxalate and HNO in the raw materials for preparing the decontamination composition are selected from the specific decontamination composition3The cleaning agent is cooperated with glycerol, can remove the loose pollutants on the part to be cleaned under the action of ultrasound, can remove deep pollutants on the part to be cleaned under the action of electrolysis, and has good cleaning effect. Tests prove that Z5CND13.04 martensitic stainless steel can be removed by performing decontamination treatment on the martensitic stainless steel by the decontamination methodZ5CND13.04 martensite stainless steel has more than 90% of pollutants and good decontamination effect.
In one embodiment, the nitrate salt is selected from at least one of sodium nitrate and potassium nitrate.
In one embodiment, the oxalate is selected from at least one of sodium oxalate and potassium oxalate.
In one embodiment, the raw material for preparing the detergent composition comprises 2.5-4.5% by volume of HNO315-25% of glycerol, 90-130 g/L of sodium nitrate and 10-20 g/L of sodium oxalate.
In one embodiment, the raw materials for preparing the detergent composition further comprise a solvent selected from at least one of deionized water and pure water.
In one embodiment, the raw materials for preparing the detergent composition further comprise a solvent with a volume percentage of 70.5-82.5%.
In one embodiment, the step of ultrasonically and electrolytically treating the workpiece to be decontaminated comprises: and carrying out ultrasonic treatment and electrolytic treatment on the piece to be decontaminated simultaneously.
In one embodiment, in the step of performing ultrasonic and electrolytic treatment on the piece to be decontaminated, the current density is 200A/m2~300A/m2The ultrasonic frequency is 40 Hz-80 Hz, and the processing temperature is 25-40 ℃.
In one embodiment, after the step of performing ultrasonic and electrolytic treatment on the piece to be decontaminated, the method further comprises the following steps: and cleaning and drying the part to be decontaminated after the ultrasonic and electrolytic treatment.
In one embodiment, the piece to be decontaminated is Z5CND13.04 martensitic stainless steel or Cr13 stainless steel.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. The following is a preferred embodiment of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
An embodiment decontamination method includes the steps of: placing a piece to be decontaminated in a decontamination composition, and carrying out ultrasonic and electrolytic treatment on the piece to be decontaminated, wherein the raw material for preparing the decontamination composition comprises HNO with the volume percentage of 2-5 percent310 to 30 percent of glycerol, 80 to 140g/L of nitrate and 5 to 25g/L of oxalate.
In the decontamination method, the nitrate, oxalate and HNO in the raw materials for preparing the decontamination composition are selected from the specific decontamination composition3Cooperate with glycerol to can get rid of under the effect of supersound and wait to decontaminate loose pollutant on the piece, can get rid of under the effect of electrolysis and wait to decontaminate the pollutant of the upper deep level of piece, decontamination effect is better, and decontamination efficiency is higher.
In one embodiment, the piece to be decontaminated is Z5CND13.04 martensitic stainless steel or Cr13 stainless steel. Further, the piece to be decontaminated is Z5CND13.04 martensitic stainless steel. The member to be cleaned is not limited to the above-mentioned members, and may be other members to be cleaned.
In one embodiment, the contaminants include radioactive contaminants. It should be noted that the contaminants are not limited to the above-mentioned contaminants, and may also include other contaminants, such as: oil stains or solid contaminants.
HNO3Namely nitric acid, a strong oxidizer, can rapidly corrode and decompose the dirt on the surface of the piece to be decontaminated, so that the contaminants such as radioactive substances are separated from the piece to be decontaminated.
In one of the examples, the stain removal composition is preparedThe raw material comprises HNO with the volume percentage content of 2.5-4.5 percent3. In some of these embodiments, the starting material from which the stain removal composition is prepared comprises 2%, 2.5%, 3%, 4.5%, or 5% HNO by volume3
The glycerol is commonly called as glycerin, has strong hygroscopicity, can be mutually soluble with water and part of organic matters, can dissolve dirt on the surface of a piece to be decontaminated to release pollutants, has small irritation, and has small influence on a base material of the piece to be decontaminated so as to ensure the reutilization of the piece to be decontaminated.
In one embodiment, the raw materials from which the stain removal composition is prepared include 15% to 25% by volume glycerol. Further, raw materials for preparing the decontamination composition comprise 18-22% of glycerol by volume percentage. In some of these embodiments, the raw materials from which the stain removal composition is made include 10%, 15%, 18%, 20%, 22%, or 25% by volume glycerol.
The nitrate is HNO3The salt formed by the reaction with the metal can be used as a strong oxidant in an acidic aqueous solution to decompose pollutants on the piece to be decontaminated, so that the influence on the piece to be decontaminated is reduced, and the piece to be decontaminated can be normally and repeatedly used after decontamination.
In one embodiment, the nitrate salt is selected from at least one of sodium nitrate and potassium nitrate. Further, the nitrate comprises sodium nitrate and potassium nitrate, and the mass ratio of the sodium nitrate to the potassium nitrate is 0.8: 1-1.2: 1. Further, the mass ratio of sodium nitrate to potassium nitrate was 1.
In one embodiment, the raw materials for preparing the detergent composition include 90g/L to 130g/L nitrate. Further, the raw materials for preparing the decontamination composition comprise 100 g/L-120 g/L nitrate. In some of these embodiments, the raw materials from which the stain removal composition is made include 80g/L, 90g/L, 100g/L, 110g/L, 115g/L, 120g/L, 130g/L, or 140g/L of nitrate.
The oxalate can decompose pollutants on the part to be decontaminated, and has small corrosion effect on the part to be decontaminated.
In one embodiment, the oxalate is selected from at least one of sodium oxalate and potassium oxalate. Furthermore, the oxalate comprises sodium oxalate and potassium oxalate, and the mass ratio of the sodium oxalate to the potassium oxalate is 0.8: 1-1.2: 1. Further, the mass ratio of sodium oxalate to potassium oxalate was 1.
In one embodiment, the starting material for preparing the stain removal composition includes from 10g/L to 20g/L of an oxalate salt. Further, the raw materials for preparing the decontamination composition comprise 13 g/L-17 g/L of oxalate. In some of these embodiments, the starting material from which the stain removal composition is prepared includes 5g/L, 7g/L, 10g/L, 12g/L, 15g/L, 17g/L, 20g/L, or 25g/L oxalate.
In one embodiment, the raw material for preparing the decontamination composition includes HNO in an amount of 2.5% to 4.5% by volume315-25% of glycerol, 90-130 g/L of sodium nitrate and 10-20 g/L of sodium oxalate. The decontamination composition can effectively remove pollutants on the piece to be decontaminated and can reduce the influence on the piece to be decontaminated so that the piece to be decontaminated can be reused.
In one embodiment, the raw materials for preparing the stain removal composition further comprise a solvent selected from at least one of deionized water and purified water. Furthermore, the raw materials for preparing the decontamination composition also comprise a solvent with the volume percentage content of 70.5-82.5%. Furthermore, the raw materials for preparing the decontamination composition also comprise 75-80% of solvent by volume percentage. In some of these embodiments, the raw materials from which the stain removal composition is prepared further include a solvent in an amount of 70.5%, 72.5%, 75%, 77.5%, 80%, or 82.5% by volume.
In one embodiment, the raw material for preparing the decontamination composition includes HNO in an amount of 2.5% to 4.5% by volume315 to 25 percent of glycerol, 90 to 130g/L of sodium nitrate, 10 to 20g/L of sodium oxalate and 70.5 to 82.5 percent of solvent. The decontamination composition can effectively remove pollutants on the piece to be decontaminated and can reduce the influence on the piece to be decontaminated so that the piece to be decontaminated can be reused.
In a common decontamination process, in order to improve decontamination effect and decontamination efficiency, the operation temperature generally needs to be increased to over 90 ℃, conditions are harsh, and higher temperature may affect a piece to be decontaminated, which is not favorable for recycling the piece to be decontaminated.
In one embodiment, the step of ultrasonically and electrolytically treating the article to be decontaminated comprises: and simultaneously carrying out ultrasonic treatment and electrolytic treatment on the workpiece to be decontaminated. Through treating decontamination piece and carrying out supersound and electrolytic treatment simultaneously, the ultrasonic wave can be got rid of the loose pollutant in surface, carries out high-efficient decontamination to the pollutant of depth through the electrochemistry method, and simultaneously, the ultrasonic wave can also promote the radioactive pollutant to drop to prevent effectively that the pollutant of being cleared from sticking once more and covering at the metal surface, make and enough reach better decontamination effect, can improve decontamination efficiency again, can also suitably reduce the operating temperature of decontamination in-process, in order to reduce the influence of treating decontamination piece.
Further, the step of carrying out ultrasonic and electrolytic treatment on the piece to be decontaminated comprises the following steps: and (3) connecting the part to be decontaminated with the anode of the power supply, punching the power supply, and simultaneously carrying out ultrasonic treatment and electrolytic treatment on the part to be decontaminated. It should be noted that, the ultrasonic treatment and the electrolytic treatment are not limited to be performed on the to-be-decontaminated member at the same time, the ultrasonic treatment and the electrolytic treatment may be performed on the to-be-decontaminated member first, and the electrolytic treatment and the ultrasonic treatment may be performed on the to-be-decontaminated member first.
In one embodiment, the current density is 200A/m in the step of ultrasonic and electrolytic treatment of the piece to be decontaminated2~300A/m2The treatment temperature is 25-40 ℃, and the ultrasonic frequency is 40-80 Hz. Furthermore, the time for ultrasonic treatment and electrolytic treatment of the workpiece to be decontaminated is 10 min-20 min.
In one embodiment, after the step of performing ultrasonic and electrolytic treatment on the workpiece to be decontaminated, the method further comprises the following steps: and cleaning and drying the part to be decontaminated after the ultrasonic and electrolytic treatment. And further, cleaning the part to be decontaminated after ultrasonic and electrolytic treatment by using deionized water. The drying mode is drying or air drying. Further, the cleaning method is soaking or spraying. The cleaning temperature is 23-27 ℃.
In the decontamination method, the nitrate, oxalate and HNO in the raw materials for preparing the decontamination composition are selected from the specific decontamination composition3The cleaning agent is cooperated with glycerol, can remove the loose pollutants on the part to be cleaned under the action of ultrasound, can remove deep pollutants on the part to be cleaned under the action of electrolysis, and has good cleaning effect. Experiments prove that the Z5CND13.04 martensitic stainless steel is decontaminated by the decontamination method, more than 90% of pollutants on Z5CND13.04 martensitic stainless steel can be removed, and the decontamination effect is good.
Common decontamination technology is mainly through adopting the decontaminant to treat that the piece that decontaminates carries out chemical treatment, and the decontamination factor is little, and the waste liquid of production is more, simultaneously, in order to improve decontamination effect, often adopts the decontaminant of strong corrosivity, seriously corrodes the piece that treats the decontamination, is unfavorable for the recycle of the piece that treats the decontamination. In addition, in order to improve the decontamination effect and decontamination efficiency, the common decontamination process generally needs to increase the operating temperature to over 90 ℃, and the conditions are harsh, and a higher temperature may affect the piece to be decontaminated, which is not favorable for recycling the piece to be decontaminated. The decontamination method selects a specific decontamination composition and combines ultrasound and electrolysis, so that only a small amount of decontamination composition is needed to remove pollutants on a piece to be decontaminated, the amount of generated waste liquid is small, and the pollution to the environment is low. Meanwhile, the decontamination method can remove the pollutants on the piece to be decontaminated at 25-40 ℃ through the synergistic effect of the ultrasound and the electrolysis, has high decontamination efficiency, has small influence on the piece to be decontaminated, and is favorable for recycling the piece to be decontaminated after decontamination.
The decontamination method has the characteristics of high decontamination efficiency, small secondary waste liquid generation amount, good decontamination effect, reusability of decontaminated workpieces and the like, not only provides a technically reliable, economically feasible technical path for nuclear facility decontamination technology, but also realizes the recycling and reutilization of metal materials and decommissioning equipment used by the nuclear facility in service, so that the radioactive waste generated by the equipment in the whole service life is kept in a practical and feasible minimum amount, the nuclear energy is efficiently and stably utilized, and the generated radioactive pollution is controlled under the safety standard, thereby ensuring the safety of personnel, environment and the public. The decontamination method can be applied to various industries of nuclear fuel cycle and has good market application prospect.
The following are specific examples.
Unless otherwise specified, the following examples do not include other components except inevitable impurities. The examples, which are not specifically illustrated, employ drugs and equipment, all of which are conventional in the art. The experimental procedures, in which specific conditions are not indicated in the examples, were carried out according to conventional conditions, such as those described in the prior art or those recommended by the manufacturer.
In the following examples, HNO is not specifically shown3Added as nitric acid and glycerol as glycerol. The workpieces to be decontaminated are all plates, and the length of the plates is 50mm, the width of the plates is 10mm, and the thickness of the plates is 3 mm. The water is deionized water.
Example 1
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) According to the process parameters of Table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, the piece to be decontaminated is simultaneously subjected to ultrasonic treatment and electrolytic treatment, and the current density is X2A/m2The ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the processing time is T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 2
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) Soaking a workpiece to be decontaminated in the decontamination composition of X1mL according to the process parameters of Table 2, connecting the workpiece to be decontaminated with a power supply anode, and beatingThe power supply is switched on, the ultrasonic treatment and the electrolytic treatment are simultaneously carried out on the piece to be decontaminated, and the current density is X2A/m2The ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the processing time is T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 3
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) According to the process parameters of Table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, the piece to be decontaminated is simultaneously subjected to ultrasonic treatment and electrolytic treatment, and the current density is X2A/m2The ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the processing time is T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 4
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) According to the process parameters of Table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, the piece to be decontaminated is simultaneously subjected to ultrasonic treatment and electrolytic treatment, and the current density is X2A/m2The ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the processing time is T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 5
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) According to the process parameters of Table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, the piece to be decontaminated is simultaneously subjected to ultrasonic treatment and electrolytic treatment, and the current density is X2A/m2The ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the processing time is T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 6
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) According to the process parameters of Table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, the piece to be decontaminated is simultaneously subjected to ultrasonic treatment and electrolytic treatment, and the current density is X2A/m2The ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the processing time is T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 7
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) According to the process parameters of Table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, the piece to be decontaminated is simultaneously subjected to ultrasonic treatment and electrolytic treatment, and the current density is X2A/m2The ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the processing time is T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 8
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) According to the process parameters of Table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, the piece to be decontaminated is simultaneously subjected to ultrasonic treatment and electrolytic treatment, and the current density is X2A/m2The ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the processing time is T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 9
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) According to the process parameters of Table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, the piece to be decontaminated is simultaneously subjected to ultrasonic treatment and electrolytic treatment, and the current density is X2A/m2The ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the processing time is T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 10
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) According to the process parameters of Table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, the piece to be decontaminated is simultaneously subjected to ultrasonic treatment and electrolytic treatment, and the current density is X2A/m2Ultrasonic waveThe frequency was X3Hz, the temperature was T1 ℃ and the treatment time was T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 11
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the raw materials for preparing the stain removal composition were mixed according to table 1 to obtain the stain removal composition.
(2) According to the process parameters of Table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, the piece to be decontaminated is simultaneously subjected to ultrasonic treatment and electrolytic treatment, and the current density is X2A/m2The ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the processing time is T1 min.
(3) And taking out the workpiece subjected to ultrasonic and electrolytic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 12
The stain removal process of the piece to be decontaminated of this example was substantially the same as that of example 5, except that the stain removal composition contained no glycerin and the stain removal composition contained 20g/L of ethanol.
Example 13
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the stain removal composition of this example was the same as the stain removal composition of example 5.
(2) Soaking a workpiece to be decontaminated in the decontamination composition of X1mL according to the process parameters of Table 2, connecting the workpiece to be decontaminated with a power supply anode, turning on the power supply, and performing electrolytic treatment on the workpiece to be decontaminated at a current density of X2A/m2The temperature is T1 ℃, and the treatment time is T1 min.
(3) And taking out the workpiece after the electrolytic treatment, washing the workpiece by adopting deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 14
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the stain removal composition of this example was the same as the stain removal composition of example 5.
(2) According to the process parameters of the table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, and the piece to be decontaminated is subjected to ultrasonic treatment, wherein the ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the treatment time is T1 min.
(3) And taking out the workpiece after ultrasonic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 15
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the stain removal composition of this example was the same as the stain removal composition of example 5.
(2) Soaking a workpiece to be decontaminated in the decontamination composition of X1mL according to the process parameters of Table 2, connecting the workpiece to be decontaminated with a power supply anode, turning on the power supply, and performing electrolytic treatment on the workpiece to be decontaminated at a current density of X2A/m2The temperature is T1 ℃, and the treatment time is T1 min. And (3) carrying out ultrasonic treatment on the workpiece to be decontaminated after the electrolytic treatment, wherein the ultrasonic frequency is X3Hz, and the treatment time is t2 min.
(3) And taking out the workpiece after ultrasonic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 16
The decontamination process of the piece to be decontaminated of this example is as follows:
(1) the stain removal composition of this example was the same as the stain removal composition of example 5.
(2) According to the process parameters of the table 2, a piece to be decontaminated is soaked in the decontamination composition of X1mL, the workpiece to be decontaminated is connected with a power supply anode, the power supply is switched on, and the piece to be decontaminated is subjected to ultrasonic treatment, wherein the ultrasonic frequency is X3Hz, the temperature is T1 ℃, and the treatment time is T2 min. Electrolyzing the ultrasonically treated part to be decontaminated at a current density of X2A/m2The temperature is T1 ℃, and the treatment time is T1 min.
(3) And taking out the workpiece after ultrasonic treatment, washing the workpiece by using deionized water at normal temperature, and drying the washed workpiece to obtain the decontaminated workpiece.
Example 17
The stain removal process for the article to be decontaminated of this example was substantially the same as that of example 5, except that the stain removal composition of this example was a commercially available IMC-03 lot stain removal agent.
TABLE 1 parts to be decontaminated and raw materials for preparing a decontamination composition of examples 1-11
Figure BDA0002117135600000141
TABLE 2 Process parameters for the decontamination procedure of the items to be decontaminated of examples 1 to 16
Figure BDA0002117135600000151
Wherein "- -" in table 2 indicates that this period is not set.
And (3) testing:
(1) the stain removal effect and the effect on the stain to be removed of the pieces to be cleaned of examples 1 to 17 were measured.
Wherein, the corrosion speed of the piece to be decontaminated is measured by a mass difference method in the decontamination process;
measuring the decontamination efficiency (namely decontamination rate) of the piece to be decontaminated by adopting an energy spectrum detection method;
measuring the roughness change condition of the workpiece to be decontaminated obtained before and after decontamination by adopting a laser confocal method, wherein the roughness change refers to the difference value of the roughness before decontamination and the roughness after decontamination;
measuring the removal effect of radioactive Co pollutants on a piece to be decontaminated by adopting a radioactive isotope pollutant simulation method;
the results are shown in Table 3.
TABLE 3 decontamination Effect and Effect of the pieces to be decontaminated of examples 1 to 17
Figure BDA0002117135600000161
As can be seen from table 3, the decontamination efficiency of the decontamination methods of examples 1 to 7 is 90% to 95%, that is, the decontamination methods of examples 1 to 7 can remove 90% to 95% of the pollutants on the workpiece to be decontaminated, which is significantly higher than example 17 (83%), and the decontamination methods of examples 1 to 7 can remove 89% to 95% of the Co pollutants on the workpiece to be decontaminated, which is significantly higher than example 17 (80%), which indicates that the decontamination method of the above embodiments has a good decontamination effect and can better remove the radioactive pollutants on the workpiece to be decontaminated. Meanwhile, the corrosion rate of the to-be-decontaminated part in examples 1 to 7 is 0.065 to 0.125 μm/min, which is lower than that in example 17(0.133 μm/min), which shows that the decontamination method in the embodiment can reduce the corrosion effect on the to-be-decontaminated part and reduce the influence on the metal substrate. Among them, example 6 has the highest decontamination efficiency, low corrosion rate, and minimal effect on the surface of the workpiece to be decontaminated. The decontamination efficiency of example 14 was the lowest, and it was found that the ultrasonic decontamination alone did not achieve a good decontamination effect for deep-level surface contamination.
In summary, the decontamination method of the above embodiment has a good decontamination effect, can better decontaminate the radioactive pollutants on the piece to be decontaminated, has a good corrosion effect on the piece to be decontaminated, and can avoid the influence on the piece to be decontaminated.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A method of decontamination, comprising the steps of:
placing a piece to be decontaminated in a decontamination composition, and carrying out ultrasonic and electrolytic treatment on the piece to be decontaminated, wherein the raw material for preparing the decontamination composition comprises HNO with the volume percentage of 2-5 percent310-30% of glycerol, 80-140 g/L of nitrate and 5-25 g/L of oxalate;
the step of performing ultrasonic and electrolytic treatment on the piece to be decontaminated comprises the following steps of: and carrying out ultrasonic treatment and electrolytic treatment on the piece to be decontaminated simultaneously.
2. The decontamination method of claim 1, wherein the nitrate salt is selected from at least one of sodium nitrate and potassium nitrate.
3. The decontamination method of claim 1, wherein the oxalate is selected from at least one of sodium oxalate and potassium oxalate.
4. The decontamination method of claim 1, wherein the raw material from which the decontamination composition is prepared comprises 2.5% to 4.5% HNO by volume315-25% of glycerol, 90-130 g/L of sodium nitrate and 10-20 g/L of sodium oxalate.
5. The decontamination method of claim 1, wherein the raw materials for preparing the decontamination composition further comprise a solvent selected from at least one of deionized water and purified water.
6. The decontamination method of claim 5, wherein the raw materials used to prepare the decontamination composition further comprise a solvent present in an amount ranging from 70.5% to 82.5% by volume.
7. The decontamination method of claim 1, wherein the nitrate salt comprises sodium nitrate and potassium nitrate, and the mass ratio of sodium nitrate to potassium nitrate is 0.8: 1-1.2: 1; the oxalate comprises sodium oxalate and potassium oxalate, and the mass ratio of the sodium oxalate to the potassium oxalate is 0.8: 1-1.2: 1.
8. The decontamination method of claim 1, wherein in the step of subjecting the item to be decontaminated to ultrasonic and electrolytic treatment, the current density is 200A/m2~300A/m2The ultrasonic frequency is 40 Hz-80 Hz, and the processing temperature is 25-40 ℃.
9. The decontamination method of claim 1, wherein the step of ultrasonically and electrolytically treating the item to be decontaminated is followed by the step of: and cleaning and drying the part to be decontaminated after the ultrasonic and electrolytic treatment.
10. The decontamination method of claim 1, wherein the item to be decontaminated is Z5CND13.04 martensitic stainless steel or Cr13 stainless steel.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101394942A (en) * 2006-02-28 2009-03-25 细胞生物工程有限公司 Polymer composition and method for removing contaminates from a substrate
US7713402B2 (en) * 2000-12-21 2010-05-11 Kabushiki Kaisha Toshiba Method for treating a chemical decontamination solution
CN205943483U (en) * 2016-08-23 2017-02-08 中国工程物理研究院核物理与化学研究所 Get rid of radioactivity surface pollution's automatic decontamination system of supersound electrolysis

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7713402B2 (en) * 2000-12-21 2010-05-11 Kabushiki Kaisha Toshiba Method for treating a chemical decontamination solution
CN101394942A (en) * 2006-02-28 2009-03-25 细胞生物工程有限公司 Polymer composition and method for removing contaminates from a substrate
CN205943483U (en) * 2016-08-23 2017-02-08 中国工程物理研究院核物理与化学研究所 Get rid of radioactivity surface pollution's automatic decontamination system of supersound electrolysis

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