蒸汽发生器沉积物在EDTA溶液中溶解行为

宋利君; 肖艳; 孙云; 田朝晖; 刘灿帅; 邹伟

doi:10.13832/j.jnpe.2024.04.0228

蒸汽发生器沉积物在EDTA溶液中溶解行为

doi: 10.13832/j.jnpe.2024.04.0228

宋利君^{1, 2,},
肖艳^{1, 2},
孙云^{1, 2},
田朝晖^{1, 2},
刘灿帅^{1, 2},
邹伟^{1, 2}

1.
苏州热工研究院有限公司，江苏苏州，215004
2.
国家核电厂安全及可靠性工程技术研究中心，江苏苏州，215004

详细信息

作者简介:
宋利君（1980—），女，工学博士，主要从事核电厂水化学控制与优化研究工作，E-mail: songlijun1980@163.com

中图分类号: TL38
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- 被引次数: 0
出版历程
- 收稿日期: 2023-08-28
- 修回日期: 2023-09-21
- 刊出日期: 2024-08-12

Dissolution Behavior of Steam Generator Deposit in EDTA Solution

Song Lijun^{1, 2
,},
Xiao Yan^{1, 2},
Sun Yun^{1, 2},
Tian Zhaohui^{1, 2},
Liu Canshuai^{1, 2},
Zou Wei^{1, 2}

1.
Suzhou Nuclear Power Research Institute Co., Ltd., Suzhou, Jiangsu, 215004, China
2.
National Engineering Research Center for Nuclear Power Plant Safety & Reliability, Suzhou, Jiangsu, 215004, China

摘要

摘要: 为了研究化学清洗剂乙二胺四乙酸（EDTA）对模拟沉积物Fe₃O₄和蒸汽发生器（SG）泥渣的溶解能力，以指导化学清洗工艺选择，采用X射线荧光光谱和电感耦合等离子体发射光谱分析温度、EDTA浓度、溶解时间对模拟沉积物Fe₃O₄和SG泥渣的溶解效果。采用Fe₃O₄制备化学修饰电极，采用三电极体系开展修饰电极的循环伏安测试和交流阻抗测试。结果表明，溶液温度越高，EDTA浓度越高，对Fe₃O₄的溶解能力越强；溶解时间越长，模拟沉积物Fe₃O₄和SG泥渣的溶解率越高；由于SG泥渣和模拟沉积物Fe₃O₄的差异性，EDTA溶液对SG泥渣的溶解能力弱于模拟沉积物Fe₃O₄；修饰电极在EDTA溶液中的电化学反应过程属于扩散控制过程。
- 蒸汽发生器（SG） /
- Fe₃O₄ /
- 泥渣 /
- 化学修饰电极 /
- 乙二胺四乙酸（EDTA）
Abstract: In order to explore the solubility of chemical cleaning agent EDTA on simulated deposit Fe₃O₄ and steam generator sludge, and to guide the selection of chemical cleaning processes, XRF and ICP-OES were used to analyze the dissolution effects of solution temperature, EDTA concentration, and dissolution time on simulated deposit Fe₃O₄ and SG sludge. The chemically modified electrode was prepared by Fe₃O₄, and the cyclic voltammetry test and AC impedance test of the modified electrode were carried out by using a three-electrode system. The results indicate that the higher the solution temperature, the higher the EDTA concentration, and the stronger the solubility of Fe₃O₄. The longer the dissolution time, the higher the dissolution rate of Fe₃O₄ and SG sludge. Due to the differences between SG sludge and Fe₃O₄, EDTA solution has a weaker ability to dissolve SG sludge than Fe₃O₄. The electrochemical reaction process of Fe₃O₄ modified electrode in EDTA solution is diffusion-controlled process.
- Steam generator (SG) /
- Fe₃O₄ /
- Sludge /
- Chemically modified electrode /
- EDTA

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图 1 模拟沉积物Fe₃O₄和SG泥渣的XRD图谱

Figure 1. XRD Patterns of Simulated Deposit Fe₃O₄and SG Sludge

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图 2 模拟沉积物Fe₃O₄的微观形貌

Figure 2. Macroscopic Morphology of Simulated Deposit Fe₃O₄

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图 3 模拟沉积物在EDTA溶液中的溶解率

Figure 3. Dissolution Rate of Simulated Deposit in EDTA Solution

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图 4 SG泥渣在EDTA溶液中的溶解率

Figure 4. Dissolution Rate of SG Sludge in EDTA Solution

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图 5 SG泥渣在95℃的10% EDTA溶液中溶解前后微观形貌

Figure 5. Macroscopic Morphology of SG Sludge before and after Dissolution in 10% EDTA Solution at 95℃

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图 6 在95℃的10% EDTA溶液中溶解8 h后照片

Figure 6. Photos of Simulated Deposit and Sludge Dissolved in 10% EDTA Solution at 95℃ for 8 h

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图 7 修饰电极在15%EDTA溶液中的CV曲线和还原峰峰电流与扫速平方根的关系曲线图

Figure 7. CV Curves and Relationship Curve Between Reduction Peak Currents and Scan Rate Square Root of Modified Electrode in 15% EDTA Solution

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图 8 修饰电极在EDTA溶液中CV循环前后的EIS图

R_s—工作电极与对电极之间的电解质溶液电阻，对应电阻值为R_s；C—界面电容，对应电容值为C；R_p—极化电阻，对应电阻值为R_p；R_ct—电荷转移电阻，对应电阻值为R_ct；C_PE1—恒相位元件电容，对应电容值为C_PE1

Figure 8. EIS Diagram of Modified Electrode Before and After CV Cycling in EDTA Solution

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表 1 实验仪器

Table 1. Experimental Instruments

仪器名称	型号
XRD	PANalytical X' PERT PRO
SEM	ZEISS Sigma 300
XRF	Bruke S2 PUMA
ICP-OES	SPECTRO ARCOS EOP
电化学工作站	CHI 660E

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表 2 SG泥渣的XRF分析结果

Table 2. XRF Analysis Results of SG Sludge

元素	Fe	Cr	Mn	Ti	Ni	Zn
质量分数/%	94.91	0.79	0.69	0.54	0.52	0.33

元素	Mg	Cu	Si	Pb	Cl	Mo
质量分数/%	0.76	0.27	0.61	0.26	0.11	0.05
注：因XRF测量原理限制，原子序数在Na之前的元素无法检出

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表 3 SG泥渣在10% EDTA溶液中溶解8 h后滤液中金属元素含量

Table 3. Metal Element Content in the Filtrate of SG Sludge Dissolved in 10% EDTA Solution for 8 h

元素	Fe	Cu	Pb	Zn	Na
浓度/(mg·kg⁻¹)	3044.4	80.4	17.3	11.9	20.0

元素	K	Ca	Mg	Al
浓度/(mg·kg⁻¹)	35.5	3.0	0.4	35.0

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表 4 修饰电极在EDTA溶液中CV循环前后的EIS拟合数据

Table 4. EIS Fitting Data of Modified Electrode Before and After CV Cycling in EDTA Solution

测试条件	EDTA 浓度/%	R_s/Ω	C/10⁻⁵F	R_p/Ω	C_PE1/10⁻⁵ F	R_ct/Ω
CV循环前	2	56.23	4.31	191.7	3.12	4308
	5	32.47	4.63	197.8	2.90	3696
	10	22.27	4.93	189.5	2.93	3228
	15	20.77	2.92	101.9	9.04	1740
CV循环后	2	66.71	3.68	153.0	3.47	4501
	5	39.73	3.99	134.8	3.26	4474
	10	28.51	4.48	148.8	2.89	3433
	15	21.30	4.78	158.8	2.92	3589

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