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Article(id=1190369068239650968, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1190365079976640655, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2025.07.011, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1727193600000, receivedDateStr=2024-09-25, revisedDate=1731427200000, revisedDateStr=2024-11-13, acceptedDate=null, acceptedDateStr=null, onlineDate=1761735701856, onlineDateStr=2025-10-29, pubDate=1752940800000, pubDateStr=2025-07-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1761735701856, onlineIssueDateStr=2025-10-29, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1761735701856, creator=13701087609, updateTime=1761735701856, updator=13701087609, issue=Issue{id=1190365079976640655, tenantId=1146029695717560320, journalId=1149653034449285133, year='2025', volume='58', issue='7', pageStart='1', pageEnd='150', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=null, createTime=1761734750980, creator=13701087609, updateTime=1761735924323, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1190370001430348320, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1190365079976640655, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1190370001430348321, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1190365079976640655, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=93, endPage=100, ext={EN=ArticleExt(id=1190369068474531994, articleId=1190369068239650968, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Structural optimization of attapulgite composite materials and adsorption decolorization of retired transformer oil, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=

To solve the ageing problem of transformer insulation oil after the long-term operation, three composite materials, including glucose attapulgite (GLU-APT), starch attapulgite (AL-APT), and polydopamine attapulgite (PDA-APT), were designed and prepared. The structures of the composite materials were characterized by X-ray diffractor, field emission scanning electron microscopy, Raman spectrometer, Fourier transform infrared spectrometer, and N2 adsorption-desorption test. The results show that the decolorization and acid value reduction effects of the three composite materials on retired oil improves significantly compared to APT, among which the GLU-APT shows the best regeneration effect to retired oil. When the mass ratio of GLU-APT adsorbent and retired transformer oil is 1:2, the adsorption time is 2 h, and the adsorption temperature is 90℃, the decolorization rate of regenerated oil can reach 88.2%, and the acid value is reduced to 0.010 mgKOH/g, the adsorption efficiency can maintain 90% after 5 cycles of regeneration.

, articleAbstract=

To solve the ageing problem of transformer insulation oil after the long-term operation, three composite materials, including glucose attapulgite (GLU-APT), starch attapulgite (AL-APT), and polydopamine attapulgite (PDA-APT), were designed and prepared. The structures of the composite materials were characterized by X-ray diffractor, field emission scanning electron microscopy, Raman spectrometer, Fourier transform infrared spectrometer, and N2 adsorption-desorption test. The results show that the decolorization and acid value reduction effects of the three composite materials on retired oil improves significantly compared to APT, among which the GLU-APT shows the best regeneration effect to retired oil. When the mass ratio of GLU-APT adsorbent and retired transformer oil is 1:2, the adsorption time is 2 h, and the adsorption temperature is 90℃, the decolorization rate of regenerated oil can reach 88.2%, and the acid value is reduced to 0.010 mgKOH/g, the adsorption efficiency can maintain 90% after 5 cycles of regeneration.

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针对变压器油长期运行后出现的老化问题，本文设计制备出葡萄糖碳-凹凸棒土（GLU-APT）、淀粉碳-凹凸棒土（AL-APT）以及聚多巴胺碳-凹凸棒土（PDA-APT）3种复合吸附材料，用于退役变压器油的再生研究。通过X-射线衍射、场发射扫描电子显微镜、拉曼光谱、傅里叶变换红外光谱和N2吸附-脱附测试对复合材料进行结构和形貌表征。结果表明：3种复合材料对退役油的脱色和降酸值效果较APT明显提升，其中GLU-APT对退役油的再生效果最佳。当GLU-APT吸附剂与废油质量比为1∶2、吸附时间为1 h、吸附温度为90℃时，再生油的脱色率可达到88.2%，酸值降至0.010 mgKOH/g，5次循环再生后可保持90%的吸附性能。

, articleAbstract=

针对变压器油长期运行后出现的老化问题，本文设计制备出葡萄糖碳-凹凸棒土（GLU-APT）、淀粉碳-凹凸棒土（AL-APT）以及聚多巴胺碳-凹凸棒土（PDA-APT）3种复合吸附材料，用于退役变压器油的再生研究。通过X-射线衍射、场发射扫描电子显微镜、拉曼光谱、傅里叶变换红外光谱和N2吸附-脱附测试对复合材料进行结构和形貌表征。结果表明：3种复合材料对退役油的脱色和降酸值效果较APT明显提升，其中GLU-APT对退役油的再生效果最佳。当GLU-APT吸附剂与废油质量比为1∶2、吸附时间为1 h、吸附温度为90℃时，再生油的脱色率可达到88.2%，酸值降至0.010 mgKOH/g，5次循环再生后可保持90%的吸附性能。

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任乔林（1969-），男（汉族），湖北武汉人，教授级高级工程师，主要从事电力油务、电气绝缘、电工流体等方面的研究。
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张逸（1986-），男（汉族），湖北武汉人，副教授，主要从事绝缘油的分离纯化、吸附材料的设计合成等方面的研究；

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张逸（1986-），男（汉族），湖北武汉人，副教授，主要从事绝缘油的分离纯化、吸附材料的设计合成等方面的研究；

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张逸（1986-），男（汉族），湖北武汉人，副教授，主要从事绝缘油的分离纯化、吸附材料的设计合成等方面的研究；

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理化性质处理前废油处理后再生油
脱色率/%087.3
酸值/(mgKOH/g)0.055 90.010 0
介质损耗因数/%1.2150.025
击穿电压/kV29.341.2
), ArticleFig(id=1190960784072131377, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1190369068239650968, language=CN, label=表1, caption=

废油吸附处理前后的理化和电气性能对比表

, figureFileSmall=null, figureFileBig=null, tableContent=
理化性质处理前废油处理后再生油
脱色率/%087.3
酸值/(mgKOH/g)0.055 90.010 0
介质损耗因数/%1.2150.025
击穿电压/kV29.341.2
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凹凸棒土碳基复合材料的结构优化与退役变压器油的吸附脱色研究
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张逸 1, 2 , 任乔林 1 , 田海朋 2 , 李芳亚 1 , 黄旦莉 1 , 杨帆 1 , 蒋晶晶 1 , 吴霞 1 , 安乐天 3 , 毛佩东 1
绝缘材料 | 材料研究 2025,58(7): 93-100
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绝缘材料 | 材料研究 2025, 58(7): 93-100
凹凸棒土碳基复合材料的结构优化与退役变压器油的吸附脱色研究
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张逸1, 2, 任乔林1, 田海朋2, 李芳亚1, 黄旦莉1, 杨帆1, 蒋晶晶1, 吴霞1, 安乐天3, 毛佩东1
作者信息
  • 1.国网湖北省电力公司孝感供电公司，湖北 孝感 432100
  • 2.武汉工程大学 化工与制药学院，湖北 武汉 430073
  • 3.国网湖北省电力公司云梦供电公司，湖北 云梦 432500

    • 张逸（1986-），男（汉族），湖北武汉人，副教授，主要从事绝缘油的分离纯化、吸附材料的设计合成等方面的研究；

通讯作者:

任乔林（1969-），男（汉族），湖北武汉人，教授级高级工程师，主要从事电力油务、电气绝缘、电工流体等方面的研究。
Structural optimization of attapulgite composite materials and adsorption decolorization of retired transformer oil
Yi ZHANG1, 2, Qiaolin REN1, Haipeng TIAN2, Fangya LI1, Danli HUANG1, Fan YANG1, Jingjing JIANG1, Xia WU1, Letian AN3, Peidong MAO1
Affiliations
  • 1. State Grid Hubei Electric Power Company Xiaogan Power Supply Company, Xiaogan 432100, China
  • 2. School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan 430073, China
  • 3. State Grid Hubei Electric Power Company Yunmeng County Power Supply Company, Yunmeng 432500, China
出版时间: 2025-07-20 doi: 10.16790/j.cnki.1009-9239.im.2025.07.011
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摘要
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针对变压器油长期运行后出现的老化问题，本文设计制备出葡萄糖碳-凹凸棒土（GLU-APT）、淀粉碳-凹凸棒土（AL-APT）以及聚多巴胺碳-凹凸棒土（PDA-APT）3种复合吸附材料，用于退役变压器油的再生研究。通过X-射线衍射、场发射扫描电子显微镜、拉曼光谱、傅里叶变换红外光谱和N2吸附-脱附测试对复合材料进行结构和形貌表征。结果表明：3种复合材料对退役油的脱色和降酸值效果较APT明显提升，其中GLU-APT对退役油的再生效果最佳。当GLU-APT吸附剂与废油质量比为1∶2、吸附时间为1 h、吸附温度为90℃时，再生油的脱色率可达到88.2%，酸值降至0.010 mgKOH/g，5次循环再生后可保持90%的吸附性能。

凹凸棒土  /  退役变压器油  /  吸附  /  脱色

To solve the ageing problem of transformer insulation oil after the long-term operation, three composite materials, including glucose attapulgite (GLU-APT), starch attapulgite (AL-APT), and polydopamine attapulgite (PDA-APT), were designed and prepared. The structures of the composite materials were characterized by X-ray diffractor, field emission scanning electron microscopy, Raman spectrometer, Fourier transform infrared spectrometer, and N2 adsorption-desorption test. The results show that the decolorization and acid value reduction effects of the three composite materials on retired oil improves significantly compared to APT, among which the GLU-APT shows the best regeneration effect to retired oil. When the mass ratio of GLU-APT adsorbent and retired transformer oil is 1:2, the adsorption time is 2 h, and the adsorption temperature is 90℃, the decolorization rate of regenerated oil can reach 88.2%, and the acid value is reduced to 0.010 mgKOH/g, the adsorption efficiency can maintain 90% after 5 cycles of regeneration.

attapulgite  /  retired transformer oil  /  adsorption  /  decolorization
张逸, 任乔林, 田海朋, 李芳亚, 黄旦莉, 杨帆, 蒋晶晶, 吴霞, 安乐天, 毛佩东. 凹凸棒土碳基复合材料的结构优化与退役变压器油的吸附脱色研究. 绝缘材料, 2025 , 58 (7) : 93 -100 . DOI: 10.16790/j.cnki.1009-9239.im.2025.07.011
Yi ZHANG, Qiaolin REN, Haipeng TIAN, Fangya LI, Danli HUANG, Fan YANG, Jingjing JIANG, Xia WU, Letian AN, Peidong MAO. Structural optimization of attapulgite composite materials and adsorption decolorization of retired transformer oil[J]. Insulating Materials, 2025 , 58 (7) : 93 -100 . DOI: 10.16790/j.cnki.1009-9239.im.2025.07.011
正文
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0 引言
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变压器广泛应用于电网体系中，变压器油是变压器正常运行的关键，而变压器的使用将不可避免地产生大量退役变压器油。退役变压器油的直接排放会造成严重的环境污染，因此对退役变压器油进行回收再生处理十分重要。根据GB 2536—2011，变压器油应透明澄清且没有颗粒状悬浮物，而与新油相比，废油颜色变化非常明显，油品劣化程度越高其颜色就越深[1]。退役变压器油中的致色物质一般为老化后的抗氧化剂、氧化后的大分子有机物和多环芳烃，以及金属杂质等。同时，酸值升高后油品会对变压器产生腐蚀作用，直接影响到变压器的使用寿命[2]。
目前，国内外退役变压器油的再生方法主要有吸附法、溶剂萃取法、催化加氢法等。其中，催化加氢法是通过加氢还原的方法使废油中的抗氧化剂、酸性有机物等物质转化为变压器油中的基础油成分，但是催化加氢的操作要求和成本高，存在一定的局限性[3]。溶剂萃取法是选用合适溶剂选择性地将废油中的基础油组分萃取出来获得回收油，但该法对溶剂的要求较高，需对变压器油中基础成分溶解度大且对废油中杂质离子以及抗氧化剂等溶解度小，且萃取剂的用量非常大，因此溶剂萃取法也不适合规模化的退役变压器油回收[4]。
吸附法是采用固体吸附材料，通过物理或化学吸附过程去除废油中的杂质组分，包括水、老化的添加剂、氧化物等。吸附法可有效改善退役变压器油的颜色，恢复废油的电气性能[5]。相比于其他再生方法，吸附法以高效率、易操作、低成本等特点，在众多方法中较为突出。目前，WANG T等[6]制备了锌铜双金属有机框架材料用于吸附废弃油品中常见的有机硫污染物二苯并噻吩[6]。陈虎剑等[7-8]制备了壳聚糖-海泡石以及壳聚糖-聚乙二醇等吸附剂并分别对变压器油中的金属杂质和腐蚀性硫进行脱除，其中壳聚糖-海泡石对金属铜离子的去除率为73.1%，壳聚糖-乙二醇对腐蚀性硫的脱除率达到84.6%，表明壳聚糖材料经过复合后展现出优异的吸附效果。因此，吸附法具有操作简便和高效可控等突出优点，具有较好的实际应用潜力。
凹凸棒土材料属于天然黏土材料，对有机物大分子、金属离子等具有较好的吸附效果，同时也可通过表面改性和复合提升其吸附性能。已有研究人员利用凹凸棒土制备出多种复合材料用于吸附废水中的重金属、有机物、染料等污染物。例如，XUE A等[9]制备了氨基接枝的凹凸棒土用于吸附染料，其脱色效果明显。CHEN X等[10]采用细菌纤维素和凹凸棒土制备出一种复合材料，用于吸附废水中的重金属和有机物。CHEN Y等[11]采用吡咯单体，在制备聚吡咯的过程中加入凹凸棒土材料，用于吸附重金属。尽管如此，采用凹凸棒土复合材料用于去除矿物油中的金属和有机物杂质的报道却并不多见，亟需开展相关研究工作。
在上述工作的基础上，本文拟利用葡萄糖、淀粉、聚多巴胺为碳源载体，分别承载凹凸棒土，设计并制备3种复合吸附材料，并进行结构和形貌的表征分析。其中，葡萄糖为小分子，水热反应后可为材料提供小分子碳源；淀粉为大分子，经过高温退火可形成疏松多孔的碳源；聚多巴胺为高分子聚合物，经过高温煅烧后不仅能提供碳源，还能引入丰富的氮源。而不同碳源的引入均可为吸附剂增加利于有机物杂质和金属杂质附着的吸附位点。将利用上述3种复合材料对退役变压器油进行再生处理，测定再生油的脱色率与酸值等重要指标，获得最优的复合吸附材料。在此基础上，以最优复合吸附材料为研究对象，分别探讨不同吸附操作条件对退役变压器油再生性能的影响规律，进一步优化吸附脱色的工艺条件，测试再生油的电气性能指标，为大规模处理退役变压器油提供基础数据，开拓其在废油再生领域的应用。
1 实验
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1.1 实验材料
退役变压器油，国网湖北省电力公司孝感电力公司；凹凸棒土、白土、活性炭，河北省灵寿县德航矿产品有限公司；葡萄糖（分析纯）、98%硫酸溶液（分析纯）、98%乙酸溶液（分析纯）、异丙醇溶液（分析纯）、碱蓝6B（分析纯）、硝酸钴（质量分数为99%）、邻苯二甲酸氢钾（质量分数为99%）、氢氧化钾（分析纯）、盐酸多巴胺（质量分数为98%）、玉米淀粉（质量分数为96%）、25%氨水（分析纯）、氢氧化钠（分析纯），国药集团有限公司。
1.2 实验仪器
DF-101S型恒温磁力水浴锅，武汉科尔仪器设备有限公司；HH-6型六联恒温水浴锅，江苏西城新瑞仪器厂；Gemini 300型场发射扫描电子显微镜（FESEM），德国卡尔蔡司公司；D2 PHASER型X-射线衍射仪（XRD），德国布鲁克公司；Nicolet 6700型傅里叶变换红外光谱仪（FTIR）、DXR型激光共焦纤维拉曼光谱仪（Raman），美国赛默飞世尔科技公司；Autosorb-iQ型全自动比表面积和孔径分布分析仪（BET），美国康塔仪器公司；UV-2600型紫外分光光度计，日本岛津公司；DYC-1型介损及体积电导率仪，江苏云能仪器仪科技有限公司；GJW-100E型击穿电压仪，长春智能仪器设备有限公司。
1.3 复合材料的制备
用一定浓度的硫酸对凹凸棒土（APT）进行酸洗后，将APT与葡萄糖以5∶2的质量比溶解在60 mL去离子水中，搅拌均匀后，放入100 mL水热釜中，加热到160℃并保持12 h。冷却后，将所得混合物离心处理，分别用乙醇和去离子水将固体洗涤3次后放入烘箱在60℃下干燥12 h，即可得到葡萄糖碳-凹凸棒土（GLU-APT）复合材料。
将0.4 g玉米淀粉投入装有100 mL水的烧瓶中，加入2 mL乙酸，搅拌均匀，然后加入1 g的APT，在60℃下搅拌回流6 h。将所得混合物离心洗涤后放入烘箱在60℃下干燥12 h，然后将烘干后的样品研磨均匀，放入管式炉中在300℃下退火1 h，得到淀粉碳-凹凸棒土（AL-APT）复合材料。
将90 mL去离子水、40 mL无水乙醇、0.9 mL氨水以及1 g APT混合在烧瓶中，搅拌均匀得到溶液A。向10 mL去离子水中加入0.5 g盐酸多巴胺，搅拌均匀得到溶液B。随后将溶液B逐滴加入搅拌均匀的溶液A中，在室温下反应48 h，经离心洗涤后放入烘箱在60℃下干燥12 h。最后将烘干后的样品研磨均匀，放入管式炉中在350℃下退火1 h，得到聚多巴胺碳-凹凸棒土（PDA-APT）复合材料。
1.4 退役油的吸附实验
分别取0.5 g GLU-APT、AL-APT、PDA-APT复合材料或APT、活性白土、活性炭放入烧瓶中，再分别加入4 g退役变压器油，在90℃恒温磁力油浴锅中搅拌处理2 h。随后将混合物离心分离，得到上层即为再生油。用滤纸过滤去除吸附剂颗粒后，分别测定再生油的脱色率、酸值等吸附指标。
1.4.1 脱色率的测定
采用紫外分光光度计测定退役变压器油和再生油的吸光度。以去离子水为参比，在480 nm的波长下测定油品的吸光度，通过式（1）计算脱色率。
A=(E-X)/E×100%
式（1）中：A为脱色率，%；E为退役油的吸光度；X为再生油的吸光度。
1.4.2 酸值的测定
根据GB/T 41633.2—2022测定变压器油的酸值。
1.4.3 电气性能的测定
根据GB/T 5654—2007测定再生油的介质损耗因数；根据GB/T 507—2002测定再生油的击穿电压。
2 结果与讨论
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2.1 复合材料的表征分析
2.1.1 FESEM
图1展现了APT和3种APT复合材料的微观形貌特征。从图1可以看出，APT呈现为片状结构，边缘不规则；引入葡萄糖作为碳源后，GLU-APT的片状结构表面变得更加光滑，片与片之间变得更加紧实，展现出更加规整的微观形貌；引入淀粉作为碳源后，AL-APT的片状结构明显包埋于絮状物中，分散较均匀；当聚多巴胺作为碳源时，复合材料PDA-APT的片状结构变厚、尺寸变小，且表面出现明显的负载物。因此，不同碳源的引入均会显著改变材料的微观形貌，并增加材料对有机物以及金属离子的附着位点[12]。
2.1.2 XRD
采用X-射线衍射仪对APT及其3种复合材料进行结构鉴定，结果如图2所示。从图2可以看出，3种APT复合材料的主要衍射峰与APT的谱图基本一致，其主要的衍射特征峰对应于黏土矿物中常见的物质。例如，在2θ为21.7°和35.7°处的特征峰对应于二氧化硅的衍射峰，在19.7°处的特征峰对应于镁铝硅酸盐的衍射峰[13]。此外，3种APT复合材料的衍射峰位置相比APT未发生显著的变化，表明不同碳源的引入对APT的原有结构未产生明显影响。
2.1.3 FTIR
图3为APT以及3种APT复合材料的FTIR谱图。从图3可以看出，波数为3 625 cm-1和3 424 cm-1处的红外峰分别对应于Al-OH和Mg-OH的拉伸振动峰，1 641 cm-1处的红外峰对应于沸石水的拉伸振动峰[14]。同时，上述4种材料均在1 087～1 041 cm-1处出现了明显红外峰，对应于Si-O键的拉伸振动峰，表明3种APT复合材料与APT一样均存在Si-O键[14]。另外，792 cm-1处的红外峰对应于C-H的拉伸振动峰，表明在APT复合材料中引入碳源后，其主体结构没有发生变化。APT材料在约1 500 cm-1处的红外峰为碳酸盐的拉伸振动峰，在材料复合后该峰消失，意味着制备的3种复合材料中APT材料孔道中的碳酸盐消失。4种材料在518 cm-1处均出现Si-O-Si键的拉伸振动峰，表明材料复合过程未改变APT的结构。
2.1.4 拉曼光谱
通过拉曼光谱进一步研究APT复合材料的碳质结构，比较不同碳源在复合材料中的结构特征，结果如图4所示。从图4可以看出，3种复合材料在1 381 cm-1和1 570 cm-1处均可分别观察到D带和G带，D带对应复合材料中的无序碳，G带对应复合材料的石墨碳[15]。而APT中由于不含碳材料无法表现出特征带，这也证明了3种复合材料的成功合成。根据文献[15]，D带与G带的峰面积比值（ID/IG）可反映复合材料中碳的无序度，ID/IG越大表明复合材料中碳的无序度越大。通过拟合对比，发现GLU-APT（ID/IG=1.41）中碳的无序度大于PDA-APT（ID/IG=1.39）和AL-APT（ID/IG=1.03），表明在复合材料的制备过程中碳源不同以及添加碳源的方式不同，会改变复合材料中无序碳与石墨碳的占比。由于GLU-APT内无序碳的占比更高，其吸附性能相比AL-APT和PDA-APT将更为优异。
2.1.5 N2吸附-脱附等温线和孔径分布
通过测试不同复合材料N2吸附-脱附等温曲线来获得材料的比表面积和孔径分布，结果如图5所示。从图5可以看出，葡萄糖、淀粉的引入明显改善了复合材料的比表面积和孔径，这主要是无定形碳在APT材料表面的附着导致。通过Brunauer-Emmett-Teller（BET）方法计算得到，在这4种材料中GLU-APT材料的BET比表面积为71.006 m2/g，明显高于其他3种材料的比表面积。同时，GLU-APT材料的孔径也最大，为13.66 nm。
2.2 不同APT复合材料的废油处理效果
利用紫外分光光度计测定废油和再生油在 480 nm波长下的吸光度，并计算出APT及其复合吸附材料对退役变压器油的脱色效果，同时还选取了活性白土和活性炭等常见吸附材料开展对比分析，结果如图6所示。从图6可以看出，GLU-APT对退役变压器油的脱色率达到了87.0%，相较于APT的5.8%脱色率有了明显的提升，展现出优异的吸附除杂效果。而AL-APT、PDA-APT、活性白土、活性炭处理后的再生油脱色率分别为51.8%、11.0%、8.2%、16.5%，其脱色效果明显低于GLU-APT。吸附脱色效果与不同的APT复合材料的结构特点与本征活性密切相关，同时还取决于吸附剂与致色物质的吸附关系，具体吸附过程可分为致色物质在材料表面扩散、致色物质与吸附剂的相互作用以及在吸附剂表面或孔道内部的附着[16]。从图6还可以看出，退役变压器油的初始酸值为0.055 9 mgKOH/g，经过APT处理后的再生油酸值为0.049 9 mgKOH/g，酸值降低量较小。当利用PDA-APT、AL-APT、活性白土、活性炭处理后，再生油的酸值分别为0.049 2、0.026 7、0.049 3、0.045 1 mgKOH/g，而利用GLU-APT处理后，再生油的酸值降至0.010 mgKOH/g，酸值降幅达到82.1%，展现出优异的降酸值效果，并且再生油的酸值已基本符合GB 2536—2011中酸值不高于0.010 mgKOH/g的要求。因此，下面将采用GLU-APT为复合吸附材料，继续研究不同吸附操作条件对退役变压器油脱色和降酸值效果的影响，达到工艺条件优化的目的。
2.3 吸附操作条件的优化
2.3.1 吸附温度
选用不同吸附温度（30、60、90、120℃），研究GLU-APT复合吸附材料与废油质量比为1∶8、吸附时间为4 h时的吸附过程，在每种吸附温度条件下均分别进行3次实验，实验结果取平均值，结果如图7所示。从图7可知，随着吸附温度从30℃上升至90℃，吸附效果越来越好，当吸附温度达到90℃时，再生油的脱色率上升至82.7%，酸值降至0.012 5 mgKOH/g，表明升高温度有利于提高吸附材料活性，提升其对致色杂质的去除能力。而当吸附温度继续上升至120℃时，再生油的脱色率稍有降低，酸值也稍有升高，主要原因可能是当温度达到120℃时，高温加速退役变压器油的老化，使得废油中致色杂质成分增加，导致脱色率下降，油品酸值升高[17]。为了探究吸附温度对退役变压器油再生效果影响的显著性，分别对脱色率和酸值数据进行单因素方差分析的F检验，结果显示两组实验的P-value值均远小于0.01，表明吸附温度对退役变压器油的脱色和降酸值效果均具出非常显著的影响。
2.3.2 吸附剂用量
选取不同吸附剂与废油质量比作为研究因素，探讨吸附剂用量对吸附性能的影响。具体来说，保持吸附温度为90℃、吸附时间为4 h，分别在吸附剂与废油的质量比为1∶2、1∶4、1∶8、1∶16下进行吸附研究，每种吸附剂用量条件下均分别进行3次实验，结果如图8所示。
从图8可以看出，随着吸附剂用量的减少，材料的吸附性能逐渐下降。当吸附剂与废油的质量比为1∶2时，再生油脱色率为87.1%，酸值为0.010 3 mgKOH/g。但是当吸附剂与废油的质量比降低到 1∶16时，再生油的脱色率已降至56.1%，酸值上升至0.0263 mgKOH/g。主要原因是废油中吸附剂用量的增加，可使有机物、金属离子等杂质与吸附剂的接触频率显著提升，强化了液固界面之间的传质效率，增强了GLU-APT复合材料对变压器废油的吸附除杂效果。对脱色率和酸值数据分别进行单因素方差分析，其P-value值也均小于0.01，表明吸附剂用量对退役变压器油的吸附除杂效果也具有非常显著的影响。
2.3.3 吸附时间
为了研究不同吸附时间对吸附效果的影响，在吸附温度为90℃、吸附剂与废油质量比为1∶2的条件下，分别在吸附0.5、1、4、6、8 h后测定油品的脱色率和酸值，每种吸附时间条件下均分别进行3次实验，结果如图9所示。
从图9可以看出，吸附时间为1 h时，复合吸附剂的吸附效果最好，脱色率为88.2%，酸值降至0.010 mgKOH/g。随着吸附时间的继续增加，脱色率缓慢下降，酸值缓慢上升，表明进一步延长吸附时间并不能提升吸附性能，可能是因为在90℃高温环境下，变压器油会发生进一步劣化，生成新的氧化杂质，使吸附效果变差。因此，吸附时间控制在 1 h可使吸附过程达到最佳的吸附效果。采用F检验的方法对脱色率和酸值数据分别进行单因素方差分析，其P-value值也均小于0.01，表明吸附时间也对吸附除杂效果具有非常显著的影响。
2.4 吸附-脱附循环实验
利用1 mol/L的硫酸溶液和50%体积分数的乙醇溶液为洗脱剂，分别在超声协助下洗脱15 min，经过离心分离后得到脱附后的材料。随后，在吸附温度为90℃、吸附时间为1 h、吸附剂与废油的质量比为1∶2的条件下，对变压器废油进行连续5次吸附-脱附循环实验，结果如图10所示。从图10可以看出，第一次吸附处理后的再生油脱色率为86.6%，酸值为0.010 5 mgKOH/g；通过第一次洗脱后的吸附剂再用于处理废油时，再生油的脱色率为93.1%，酸值为0.007 4 mgKOH/g。吸附性能指标的提高主要是因为复合材料通过酸洗后，其孔道结构中的杂质物质得到深度洗脱，暴露出更多的吸附位点，提高了吸附性能。随着循环次数的继续增加，吸附性能逐渐降低。经过连续5次循环后，吸附剂对再生油脱色率降至77.3%，酸值达到0.015 3 mgKOH/g。尽管如此，其吸附性能仍保持初始脱色率的90%左右，表明GLU-APT的吸附稳定性较好，具有较好的可重复使用性。
2.5 吸附前后油品的对比
当采用GLU-APT吸附剂在最佳条件下（吸附温度为90℃，吸附剂与废油质量比为1∶2，吸附时间为1 h）吸附处理废油后，油品颜色发生变化，得到吸附前和吸附后油品对比如图11所示，理化性能和电气性能对比如表1所示。
从图11可以看出，吸附前的废油呈现为黄色，主要原因是变压器油中添加有抗氧化剂2,6-二叔丁基甲酚，其在高温条件下容易变成黄色。此外，废油中还含有较多的腐蚀性硫与金属离子，这些杂质的存在也会使油品变成黄色甚至深褐色。由于葡萄糖碳和APT均为多孔结构，可通过范德华力作用下的物理吸附过程脱除废油中的致色杂质，使油品颜色从深黄色转变为无色透明状态，且无沉淀物和悬浮物，符合变压器油的质量指标。从表1可以看出，经吸附处理后，再生油的脱色率达到87.3%，酸值降低至0.010 0 mgKOH/g，介质损耗因数降低至0.025%，击穿电压上升至41.2 kV，因此，该复合吸附材料可实现变压器废油的再生，使其理化性质和电气性能得以提升。
3 结论
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（1）结构表征和吸附性能测定结果表明，GLU-APT在3种复合材料中的吸附性能最优，主要得益于其表面形貌更加规整、比表面积更大、活性位点更多。
（2）利用GLU-APT吸附处理废油，当吸附温度为90℃、吸附时间为1 h、吸附剂与废油的质量比为1∶2时，可获得最佳的再生效果，此时再生油的脱色率可达到88.2%，酸值降低至0.010 0 mg/gKOH，且经过连续5次吸附-脱附循环后仍能保持90%的吸附性能。再生油的介质损耗因数降低至0.025%，击穿电压上升至41.2 kV，电气性能获得提升。
基金
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  • 国网湖北省电力公司科技项目(5215K0160007)
文献
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参考文献 引证文献
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2025年第58卷第7期
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doi: 10.16790/j.cnki.1009-9239.im.2025.07.011
  • 接收时间：2024-09-25
  • 首发时间：2025-10-29
  • 出版时间：2025-07-20
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  • 收稿日期：2024-09-25
  • 修回日期：2024-11-13
基金
国网湖北省电力公司科技项目(5215K0160007)
作者信息
    1.国网湖北省电力公司孝感供电公司，湖北 孝感 432100
    2.武汉工程大学 化工与制药学院，湖北 武汉 430073
    3.国网湖北省电力公司云梦供电公司，湖北 云梦 432500

通讯作者:

任乔林（1969-），男（汉族），湖北武汉人，教授级高级工程师，主要从事电力油务、电气绝缘、电工流体等方面的研究。
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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