超临界CO2流体环境中线路板分层实验分析

在超临界CO2流体环境下,当温度达到240℃以上时,印刷线路板就会发生分层现象。同时,在实验中发现在非超临界流体环境下,当温度达到260℃以上时,线路板也会发生分层现象。从线路板粘接材料发生热解反应的角度出发,在对比超临界CO2流体环境下与非超临界流体环境下的线路板分层效果的基础上,对超临界CO2流体环境下的线路板分层...     

超临界CO2回收线路板工艺研究

用正交试验设计进行了超临界CO2回收废弃印刷线路板的实验。以温度、压强、时间和夹带剂为实验因素,通过对实验前后样本在重量、厚度、弯曲强度和断裂强度四方面变化的分析考察了各实验因素对实验效果的影响。实验结果表明,影响超临界CO2法回收印刷线路板的最主要因素为温度、时间和夹带剂,超临界CO2法回收废弃印刷线路板的最佳工艺条件：温度270℃,压强大于7．38MPa,时间3h,夹带剂（水）160mL。实验进一步验证了压强对实验结果的非显著性影响。     

响应面法优化超临界CO_2流体处理油基钻屑工艺

采用超临界CO2流体处理油基钻屑,考察了萃取温度、萃取压力以及分离温度对油基钻屑油相回收率的影响,在单因素实验基础上,应用响应面法最终确定超临界CO2流体处理油基钻屑的最佳条件为:萃取压力21 MPa,萃取温度55℃,分离温度64℃。各因素对油相回收率的影响依次为:萃取压力分离温度萃取温度。在最佳条件下,油相回收率为99.65%,处理后废渣油相含量0.08%,满足《农用污泥中污染物控制标准》(GB 4284-84),同时达到GB18599-2001的Ⅱ类固废物要求,可安全处置。     

超临界丙酮降解废弃线路板中的溴化环氧树脂

探讨废弃线路板中溴化环氧树脂在超临界丙酮中的脱溴降解特性,重点考察了温度、反应时间和有机溶剂添加量对溴化环氧树脂降解特性的影响,确立的最佳实验条件为:温度260℃、保温时间1~2 h、丙酮添加量20~40 mL,系统压强3~6 MPa,此时溴化环氧树脂能够快速降解,脱溴率达到97.94%,降解产物主要为苯酚和异丙基苯酚,含量分别为60.99%和3.12%,降解产物中溴主要以HBr的形式存在于油相中,可以用碱液从油相中萃取脱除。线路板经超临界丙酮处理后,铜箔与玻璃纤维自动分层解离便于后续破碎回收,为废弃线路板的无害化处理和资源回收利用提供了一条新途径。     

超临界丙酮降解废弃线路板中的溴化环氧树脂简

探讨废弃线路板中溴化环氧树脂在超临界丙酮中的脱溴降解特性,重点考察了温度、反应时间和有机溶剂添加量对溴化环氧树脂降解特性的影响,确立的最佳实验条件为：温度260℃、保温时间1~2 h、丙酮添加量20~40 mL,系统压强3~6 MPa,此时溴化环氧树脂能够快速降解,脱溴率达到97.94%,降解产物主要为苯酚和异丙基苯酚,含量分别为60.99%和3.12%,降解产物中溴主要以HBr的形式存在于油相中,可以用碱液从油相中萃取脱除。线路板经超临界丙酮处理后,铜箔与玻璃纤维自动分层解离便于后续破碎回收,为废弃线路板的无害化处理和资源回收利用提供了一条新途径。     

超临界CO2回收线路板工艺研究

采用正交试验设计进行了超临界CO₂回收废弃印刷线路板的实验。以温度、压强、时间和夹带剂为实验因素,通过对实验前后样本在重量、厚度、弯曲强度和断裂强度四方面变化的分析考察了各实验因素对实验效果的影响。实验结果表明,影响超临界CO₂法回收印刷线路板的最主要因素为温度、时间和夹带剂,超临界CO₂法回收废弃印刷线路板的最佳工艺条件：温度270℃,压强大于7.38 MPa,时间3 h,夹带剂(水)160 mL。实验进一步验证了压强对实验结果的非显著性影响。     

超临界水氧化作用可解决污泥和有毒废水问题

得克萨斯大学的埃纳斯特·格洛那报道,超临界水氧化作用可解决污泥和有毒废水的问题。一个超临界水氧化反应器,在温度500℃以上,压力34500kPa以上运行,这些温度和压力超过水的临界点(374℃,22100kPa)。在超临界水氧化下,有机物(包括有毒物)重新达到最稳状态,例如,碳氢化     

DOC系统催化性能的仿真和分析

以Langmuire Hinshelwood机理为理论依据,基于MATLAB/Simulink建立DOC系统的数值计算模型,研究不同参数(如空速、氧气浓度、NO2/NOx比例)对氮氧化物(NOx)、一氧化碳(CO)、碳氢化合物(HC)转化效率的影响,并对部分工况进行了实验研究,从而验证数值模型的准确性。结果表明,空速的降低可以增大DOC对CO、HC、NO的氧化性能,这是由于排气在催化器内的反应时间增长。当排气温度为225~300℃时,减小空速对增大HC的氧化效率效果明显,当排气温度在175~450℃范围内,减小空速对增大NO的氧化效率影响明显;当O2浓度低于1%,排气温度在175~250℃时,CO转化效率增大,在250℃之后均接近100%。当O2浓度为10%时,温度的变化对CO的转化效率影响很小。当O2浓度大于1%时,温度的变化对NO的氧化效率影响较大;当排气温度在300~550℃时,NO2/NOx比例的变化对NO的转化效率影响较大。降低排气中NO2/NOx比例,能够在排气温度高于300℃时,明显提高NO的转化效率。     

微波超声协同处理废弃印刷线路板中非金属

在相对温和的密闭水相环境中对废印刷线路板中非金属粉末的超声微波协同降解进行了研究。考察了单水热,单微波、单超声及微波超声协同作用下,温度、时间对非金属降解特性的影响。通过对初始物料、固相产物和液相产物的分析初步讨论了超声微波协同作用对废印刷线路板非金属的降解效果。结果表明,在200℃到280℃温度范围内,超声微波协同作用下,非金属中有机组分的降解率可以达到74.11%,固相产物主要是纯度较高的玻璃纤维,液相有机产物主要是苯酚类物质。     

失效锂离子电池材料真空热处理及氨性浸出

研究了失效锂离子电池中塑料、电极隔膜等有机物的真空脱除,并以电池级纯钴酸锂(LiCoO2)为原料,与活性炭粉混合,在真空中进行热还原,还原产物用含NH3和NH4HCO3的氨性水溶液浸出。实验结果表明,当加热温度大于450℃,真空压力<400 Pa时,失效锂离子电池中有机挥发物基本被脱除。在400℃真空温度下纯LiCoO2不被炭粉还原;当还原温度达到600℃,LiCoO2转变为CoO、Co和Li2CO3;在800℃时,还原产物主要为六方相、立方相金属钴及少量的CoO。还原产物中的钴易于被氨性水溶液浸出,浸出3 h后,钴基本进入溶液中,锂的浸出率也达到97%以上。     

基于超临界技术的印刷线路板资源化方法研究

印刷线路板的回收由于其结构和组成材料的复杂性,被认为是电子电器产品回收中的重点和难点之一。提出了将超临界流体技术应用于废弃印刷线路板的回收工艺,研究出了一种环境友好的废弃印刷线路板回收方法。建立了回收模型及回收实验平台,并使用正交实验设计方法对实验进行设计,利用SPSS分析软件对实验数据进行了分析研究并结合实际实验结果得出了最佳工艺参数。通过对反应生成物进行质谱分析,推测出了生成物的主要组分,并据此对反应机理进行了研究。     

Study of the distribution of the polychlorinated biphenyls in the milk fat globule by supercritical fluid extraction

The distribution of polychlorinated biphenyls (PCBs) in the milk fat globule has been studied by sequential extraction of four different lipidic fractions from powdered full-fat milk with supercritical carbon dioxide. Extractions were carried out in the dynamic mode in the pressure range 13.6-23.3 MPa at a temperature of 50 degrees C. The levels of PCBs and short-chain triglycerides (SCT), medium-chain triglycerides (MCT) and long-chain triglycerides (LCT), as well as the cholesterol in these four supercritical fluid extraction (SFE) fractions were determined. Extracts obtained at lower pressures were found to be enriched in PCBs, SCT, MCT and cholesterol, while the concentrations of all these analytes decreased for subsequent extractions. Satisfactory quadratic correlations were found between the PCB and SCT and MCT levels (r2 in the range 0.9-0.999), and between the PCB and cholesterol levels (r2 in the range 0.8-0.999, except for PCB 105) determined in the SFE fractions. These results suggested a similar distribution of the PCBs and the cholesterol in the milk fat globule. This conclusion was also supported by the comparison of the PCBs and the cholesterol chemical structures as well as by the total PCB levels determined by SFE to those obtained by using different extraction methods. The classical requirement for the analysis of this kind of lipophilic pollutants of an exhaustive extraction of the lipids of the matrix to ensure their quantitative recovery has been revised.     

Development of a simple selective SFE method for the determination of desorption behaviour of PCBs in two Swedish sediments

A simple selective supercritical fluid extraction (SFE) method was developed for the determination of desorption behaviour of PCBs in sediments. This method was applied to determine the distribution of individual PCB congeners among sites of differing bonding strengths in two Swedish sediments (Lake J?rnsj?n and Baltic bay Orserumsviken). Four different PCB fractions were distinguished in each sediment by applying consecutively harsher supercritical fluid extraction conditions on the same sample. Even though the two sediments had completely different textures, they showed very similar extraction behaviour. It was shown that, in both sediments, a major part of the PCBs (58% and 65%, respectively) were located at "fast sites", from which they were extractable already with the mildest extraction conditions (60 min, 40 degrees C and 120 bar). Only a small fraction of the PCBs were so tightly bound to the sediments (located at "slow sites"), that they could be extracted only under the harshest conditions (60 min, 150 degrees C and 400 bar). Information of this kind should be of great value for the determination of bioavailability of pollutants in sediments and soils, and it is the author's belief that this technique has the potential to develop into a powerful tool in environmental risk assessment.     

Development of supercritical carbon dioxide extraction with a solid phase trap for dioxins in soils and sediments

A method involving supercritical fluid extraction (SFE) with a solid phase trap containing activated alumina was investigated for the rapid analysis of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), and dioxin like polychlorinated biphenyls (DL-PCBs) in soils and sediments. The samples were extracted by using supercritical carbon dioxide with water (2% versus CO(2) flow velocity) being used as an entrainer at a pressure of 30 MPa and a temperature of 130 degrees C for 50 min. The extracts were adsorbed on an activated alumina trap that was maintained at a temperature of 150 degrees C, and then, PCDD/DFs and DL-PCBs were eluted with 20 ml of hexane at 60 degrees C. After concentration, they were measured with a high-resolution gas chromatograph interfaced to a high-resolution mass spectrometric detector. The average concentrations of PCDD/DFs and DL-PCBs corresponded to the results obtained by the conventional method, and the reproducibility of this SFE method was below 21% of the relative standard deviations for all samples. The total time required for the analysis of the pretreatment of this method was only 2 h.     

Routine analysis of hydrocarbons, PCB and PAH in marine sediments using supercritical CO2 extraction

Automated Supercritical Fluid Extraction (SFE), using CO2, was tested and optimised for routine analysis of hydrocarbons (THC), polychlorinated biphenyls (PCB) and polycyclic aromatic hydrocarbons (PAH) in marine sediments. The aim of the exercise was to reduce the amount of solvents used and to reduce the manual handling time for each sample. The sediments contained elemental sulphur, which was removed during the extraction step using activated Cu. Similar recoveries and reproducibility where found for THC when conventional solvent extractions and SFE where compared. Modifying the CO2 with methanol was necessary to obtain extraction recoveries similar to conventional extraction methods for PCB and PAH.     

Study on the effect of temperature and pressure on nickel-electroplating characteristics in supercritical CO2

In this work, it was investigated the effect of solubility in supercritical CO2 on the nickel-electroplating characteristics. The plating characteristics could be controlled by electric resistance and dispersion in emulsion as well. CO2 concentration had better be controlled at lower concentration than 50 CO2 wt% to decrease electric resistance since supercritical CO2 is non-polar material. Non-ionic surfactant with EO/PO block copolymer was more efficient than any other surfactant and the dispersion at 0.2 surfactant wt% was better than at any surfactant concentration and over-added surfactant concentration over 0.2 wt% brought to the decrease of dispersion properties. Electric resistance was constant at 20Omega in ranging from pH 2.2 to pH 3.5 and increased slowly to 50Omega at pH 4 and rapidly to 400Omega at pH 5. Characteristics of nickel film has a close relation with solubility in supercritical CO2 and solubility is dependent on pressure and temperature. Solubility at 16 MPa was higher than that any other at pressure and at constant pressure of 16 MPa, solubility in supercritical CO2 increased with an increasing temperature from 31 to 45 degrees C and decreased over 45 degrees C.     

Assessing supercritical fluid extraction for the analysis of fipronil, kresoxim-methyl, acrinathrin, and pyridaben residues in melon

An analytical method, using supercritical fluid extraction (SFE), was assessed for residue analysis of the insecticides fipronil, acrinathrin and pyridaben and the fungicide kresoxim-methyl in melons. Extraction conditions were optimized on glass beads, as inert material, evaluating different pressures, temperatures, and CO(2) volumes. Also, the extractability of pesticides from hydromatrix and anhydrous magnesium sulfate was evaluated. Both adsorbents were evaluated for the preparation of SFE-spiked melon samples. Extractions of fortified samples were done using 20 mL of CO(2), 300 atm, and 50 degrees C. Different extraction conditions, including the addition of water and methanol as a static modifier, were used to assess the extractability of these pesticides, and the addition of methanol was demonstrated to improve the extraction of all the studied pesticides.     

Selective supercritical fluid extraction as a tool for determining the PCB fraction accessible for uptake by chironomid larve in a limnic sediment

Selective supercritical fluid extraction (SFE) at 40 degrees C, 400 bar and 60 min was used to selectively remove bioavailable PCBs from a naturally contaminated limnic sediment. The extraction decreased the sediment concentrations of the nine studied PCBs by 54% (on average). Chironomid larvae were thereafter cultured in pre-extracted sediment as well as in untreated sediment to study the differences in uptake of PCBs in the two cultures. While the prevailing equilibrium partitioning (EqP) theory predicts a 54% decrease in PCB uptake by the chironomids in the pre-extracted sediment, with a maintained biota-to-sediment accumulation factor (BSAF), a decrease in PCB uptake by 91% was observed. For all investigated PCBs the BSAFs were on average 81% lower in the cultures with pre-extracted sediment than in the untreated systems. The data allowed for a calculation of the bioavailable fraction, which was estimated to 60%. This is very close to the 54% removed by selective SFE, demonstrating the possibility of using SFE as a tool to determine the bioavailable PCB fraction in a polluted sediment.     

Comparison of supercritical fluid extraction and Soxhlet extraction for the determination of PCBs in seaweed samples

The efficiency of supercritical fluid extraction for the determination of 12 polychlorinated biphenyls from algae samples is compared to Soxhlet extraction. Analytical detection limits for the individual congeners ranged from 0.62 microgl(-1) to 19 microgl(-1). Recovery was tested for both methods using standard addition procedure. At maximum spike level of concentration, the mean recoveries were not significantly different (P>0.05) of all PCBs studied, with the exception of PCBs 28, 52, 77 and 169. Method precision for Soxhlet extraction (< or =3.9%) was slightly better than for SFE (< or =9.2%). Although both methods yield comparable results, SFE offers the advantage of detecting all PCBs studied at lower concentrations, reducing extraction time, and reducing the amount of solvents needed. The optimized methods were applied to the analysis of three real seaweed samples, except for PCB101 the concentrations of all PCBs were low or below the detection limits. The levels of PCB101 found in sample 1 were 6.6+/-0.54 ng g(-1) d.w., in sample 2 the levels were 8.2+/-0.86 ng g(-1) d.w. and in sample 3 they were 7.7+/-0.08 ng g(-1) d.w.     

The relation between levels of selected PCB congeners in human serum and follicular fluid

Individual congener and total PCB concentrations were determined in serum and follicular fluid obtained from women undergoing assisted reproductive technologies (in-vitro fertilization and embryo replacement). Although the mean individual PCB levels revealed varying degrees of contamination, the results fall in the same range as that observed by other investigators. Except for PCB 118, correlations between levels in serum and follicular fluid were strong, and statistically significant at p < 0.05. Moreover PCB 153, a major and very stable PCB congener has been shown to correlate to the total amount of PCBs (r = 0.994, and r = 0.987, for serum and follicular fluid, respectively). The same accumulation patterns of PCBs for serum and follicular fluid have been observed.