双碳背景下，有机固废资源化是我国减污降碳和无废城市建设的重要任务。在资源属性和污染属性共存的情况下，我们既要实现它的无害化，也要最大化提升它的资源属性。聚氯乙烯（PVC）作为产量第三大的合成聚合物塑料易产生二次污染对环境和公众健康构成重大风险，四溴双酚A型溴化环氧树脂（TBBPA-ER）作为常见的溴代阻燃剂长期接触会影响内分泌提高致癌风险。在各项脱卤技术中，亚临界水联合增强剂（金属、碱或其他固体废物）脱卤已发展成为有机固废脱卤重要技术。然而，几乎所有的研究都集中在脱卤行为及脱卤效率，没有对脱卤碳基材料进行研究。研究发现PVC及TBBPA-ER在亚临界水体系脱卤衍生的碳基材料，具有强催化活性，可显著催化鲁米诺+H₂O₂产生强化学发光信号。本文利用PVC/煤矸石和TBBPA-ER在亚临界水和亚临界水-CuO体系脱卤碳基材料的化学发光催化活性，建立了邻苯二甲酸酯和葡萄糖的分析检测方法。研究结果如下：

       (1) PVC/煤矸石脱氯碳基材料化学发光法检测邻苯二甲酸酯。邻苯二甲酸酯被广泛用作塑料增塑剂，会干扰生殖、内分泌系统。本研究发现亚临界水中PVC/煤矸石脱氯碳基材料（CM-dPVC）是在碳基体上负载纳米Al₂O₃、SiO₂和Fe₂O₃的复合材料，具有丰富的有机官能团和较大的比表面积，使得CM-dPVC对鲁米诺-H₂O₂化学发光反应体系具有较强的催化活性，建立了具有良好信号放大能力的鲁米诺-H₂O₂-CM-dPVC化学发光分析方法。邻苯二甲酸酯通过π-π作用、氢键作用、疏水作用在CM-dPVC上结合吸附，极大地抑制了鲁米诺-H₂O₂-CM-dPVC的化学发光反应。在此基础上，构建了检测环境中6种常见邻苯二甲酸酯混合物（PAEs）和邻苯二甲酸二（2-乙基己基）酯（DEHP）的低碳高效化学发光分析。6种不同的邻苯二甲酸酯对鲁米诺-H₂O₂-CM-dPVC化学发光反应体系的抑制效果不同，邻苯二甲酸酯的烷基链越长，抑制效果越好，这也证明疏水作用是邻苯二甲酸酯对CM-dPVC的重要作用。在最佳实验条件下，PAEs和DEHP分别在0.003 ~ 7 nM、0.007 ~ 2 nM浓度范围内与化学发光信号强度具有良好的线性相关性，检测限分别为0.16 pM和0.33 pM。将该方法用于真实样品中邻苯二甲酸酯含量的测定，加标回收率在93.20% ~ 110.33%之间，5次平行测定的相对标准偏差均≤4.35%，检测结果与标准高效液相色谱法无明显差异。构建的鲁米诺+H₂O₂+CM-dPVC化学发光传感体系具有良好的稳定性（相对标准偏差=2.7%）和重复性（相对标准偏差≤1.5%），为其在实际环境分析中的应用提供了必要的实验数据基础。此外，生命周期评价结果显示，用作化学发光传感材料的CM-dPVC全球变暖潜值相较于化学试剂专门合成的传感材料降低了91.0%。结果表明，利用CM-dPVC进行化学发光传感，既提高了PVC回收效率，又减少了化学发光传感材料获取的碳排放。

       (2) TBBPA-ER脱溴碳基材料化学发光法检测葡萄糖。过量的葡萄糖会导致肥胖和糖尿病。亚临界水-CuO体系中TBBPA-ER脱溴碳基材料（CM-dTBBPA-ER）被证实是含有-C=C-、-C=C-C=C-、Cu、CuBr和较大比表面的碳基纳米复合材料，对鲁米诺-H₂O₂化学发光反应有较强的催化活性。密度泛函理论计算结果也进一步表明，CM-TBBPA-ER中C 2p轨道与Cu 3d轨道之间的强相互作用，增强了CM-TBBPA-ER中的局部电子密度，导致碳基材料介导电子迁移的能力较强。在此基础上，结合葡萄糖和葡萄糖氧化酶的反应，构建了快速、高灵敏度检测葡萄糖的化学发光分析方法。在最佳实验条件下，过氧化氢和葡萄糖分别在6×10^-7 ~ 7×10^-9 M、2.5×10^-6 ~ 3×10^-8 M浓度范围内与化学发光信号强度具有良好的线性相关性，检测限分别低至2.2×10^-10 M和3.7×10^-9 M。构建的鲁米诺+H₂O₂+CM-dTBBPA-ER化学发光传感体系具有良好的稳定性（相对标准偏差=2.1%）和重复性（相对标准偏差≤1.1%），为其在实际环境分析中的应用提供了必要的实验数据基础。将所构建的化学发光传感体系用于人血清中葡萄糖的检测，加标回收率在102.0% ~ 105.7%之间，5次平行测定的相对标准偏差均≤3.2%，测定结果与当地医院提供的结果无明显差异。通过对生命周期评价的环境影响分析，与化学试剂合成的传感材料相比，使用CM-dTBBPA-ER进行化学发光传感分析的全球变暖潜值降低了90.4%。本方法首次将TBBPA-ER脱溴碳基材料用作化学发光传感材料，提供了一种快速、经济和环保检测葡萄糖的技术方法，并为开发其他环境友好型传感分析开辟了新的途径。

       Under the background of double carbon, organic solid waste recycling is an important task for China's pollution reduction, carbon reduction and waste-free city construction. In the case of coexistence of resource attributes and pollution attributes, we must not only achieve its harmlessness, but also maximize its resource attributes. Polyvinyl chloride (PVC), as the third largest synthetic polymer plastic, is prone to secondary pollution and poses a major risk to the environment and public health. Tetrabromobisphenol A brominated epoxy resin (TBBPA-ER), as a common brominated flame retardant, long-term exposure will affect endocrine and increase carcinogenic risk. Among various dehalogenation technologies, subcritical water combined with enhancer (metal, alkali or other solid waste) dehalogenation has developed into an important technology for organic solid waste dehalogenation. However, almost all studies have focused on dehalogenation behavior and dehalogenation efficiency, and no research has been conducted on dehalogenated carbon-based materials. It was found that the carbon-based materials derived from the dehalogenation of PVC and TBBPA-ER in subcritical water system have strong catalytic activity and can significantly catalyze luminol+H₂O₂ to produce strong CL signal. In this paper, CL catalytic activity of PVC/coal gangue and TBBPA-ER in subcritical water and subcritical water-CuO system dehalogenated carbon-based materials was used to establish an analytical method for phthalates and glucose. The results of the study are as follows:

        (1)PVC/coal gangue dechlorinated carbon-based material CL method for the detection of phthalates. Phthalate esters are widely used as plastic plasticizers, which can interfere with the reproductive and endocrine systems. In this study, it was found that the PVC/coal gangue dechlorination carbon-based material (CM-dPVC) in subcritical water is a composite material loaded with nano-Al₂O₃, nano-SiO₂ and nano-Fe₂O₃ on the carbon matrix. It has rich organic functional groups and large specific surface area, which makes CM-dPVC have strong catalytic activity for the luminol-H₂O₂ CL reaction system. A luminol-H₂O₂-CM-dPVC CL analysis method with good signal amplification ability was established. The CL reaction of luminol-H₂O₂-CM-dPVC was greatly inhibited by the adsorption of phthalic acid ester on CM-dPVC through π-π interaction, hydrogen bonding and hydrophobic interaction. On this basis, a low-carbon and high-efficiency CL analysis of six common phthalate mixtures (PAEs) and di (2-ethylhexyl) phthalate (DEHP) in the detection environment was constructed. The inhibitory effects of six different phthalates on CL reaction system of luminol-H₂O₂-CM-dPVC were different. The longer the alkyl chain of phthalates, the better the inhibitory effect, which also proved that hydrophobic interaction was an important role of phthalates on CM-dPVC. Under the optimal experimental conditions, PAEs and DEHP have a good linear correlation with CL signal intensity in the concentration range of 0.003~7 nM and 0.007~2 nM, and the detection limits are 0.16 pM and 0.33 pM, respectively. The method was applied to the determination of phthalate esters in real samples. The spiked recoveries were 93.20%~110.33%, and the relative standard deviations of five parallel determinations were less than 4.35%. There was no significant difference between the test results and the standard high performance liquid chromatography. The constructed luminol+H₂O₂+CM-dPVC CL sensing system has good stability (Relative Standard Deviation=2.7%) and repeatability (Relative Standard Deviation≤1.5%), which provides the necessary experimental data for its application in actual environmental analysis. In addition, the life cycle assessment results showed that the global warming potential of CM-dPVC as CL sensing material was 91.0% lower than that of the sensing material specially synthesized by chemical reagents. The results show that the use of CM-dPVC for CL sensing not only improves the recovery efficiency of PVC, but also reduces the carbon emissions obtained by CL sensing material.

       (2) TBBPA-ER debrominated carbon-based material CL detection of glucose. Excessive glucose can lead to obesity and diabetes. In the subcritical water-CuO system, TBBPA-ER debrominated carbon-based materials (CM-dTBBPA-ER) were confirmed to be carbon-based nanocomposites containing-C=C-, -C=C-C=C-, Cu, CuBr and larger specific surface, which had strong catalytic activity for luminol-H₂O₂ CL reaction. The results of density functional theory calculations further show that the strong interaction between the C 2p orbital and the Cu 3d orbital in CM-TBBPA-ER enhances the local electron density in CM-TBBPA-ER, resulting in a strong ability of carbon-based materials to mediate electron migration. On this basis, combined with the reaction of glucose and glucose oxidase, a rapid and highly sensitive CL analysis method for the detection of glucose was constructed. Under the optimal experimental conditions, hydrogen peroxide and glucose had a good linear correlation with CL signal intensity in the concentration range of 6×10^-7~7×10^-9 M and 2.5×10^-6~3×10^-8 M, and the detection limits were as low as 2.2×10^-10 M and 3.7×10^-9 M, respectively. The constructed luminol+H₂O₂+CM-dTBBPA-ER CL sensing system has good stability (Relative Standard Deviation=2.1%) and repeatability (Relative Standard Deviation ≤1.1%), which provides the necessary experimental data for its application in actual environmental analysis. The constructed CL sensing system was used for the detection of glucose in human serum. The spiked recovery wa 102.0%~105.7%, and the relative standard deviation of 5 parallel measurements was ≤3.2%. There was no significant difference between the determination results and the results provided by local hospitals. Through the environmental impact analysis of life cycle assessment, the global warming potential of CL sensing analysis using CM-dTBBPA-ER was reduced by 90.4% compared with the sensing material synthesized by chemical reagents. This method is the first time to use TBBPA-ER debrominated carbon-based material as CL sensing material, providing a rapid, economical and environmentally friendly technical method for the detection of glucose, and opening up a new way for the development of other environmentally friendly sensing analysis.

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