CN109999811A - 一种生物质铁碳复合材料的制备及用于催化活化过硫酸钠降解双酚a - Google Patents
一种生物质铁碳复合材料的制备及用于催化活化过硫酸钠降解双酚a Download PDFInfo
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 title claims abstract description 23
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 title claims abstract description 22
- 239000002028 Biomass Substances 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 15
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 230000004913 activation Effects 0.000 title abstract description 21
- 229940106691 bisphenol a Drugs 0.000 title abstract description 11
- 230000003197 catalytic effect Effects 0.000 title abstract description 8
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 241000167854 Bourreria succulenta Species 0.000 claims abstract description 15
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- 238000000034 method Methods 0.000 claims abstract description 12
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- 239000000843 powder Substances 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
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- 238000001994 activation Methods 0.000 description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 5
- FHHJDRFHHWUPDG-UHFFFAOYSA-L peroxysulfate(2-) Chemical compound [O-]OS([O-])(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-L 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- 150000002338 glycosides Chemical class 0.000 description 2
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- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
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- 238000003918 potentiometric titration Methods 0.000 description 2
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- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 235000005487 catechin Nutrition 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
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- 229950001002 cianidanol Drugs 0.000 description 1
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- NHADDZMCASKINP-HTRCEHHLSA-N decarboxydihydrocitrinin Natural products C1=C(O)C(C)=C2[C@H](C)[C@@H](C)OCC2=C1O NHADDZMCASKINP-HTRCEHHLSA-N 0.000 description 1
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- 229930182470 glycoside Natural products 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
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- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229960005489 paracetamol Drugs 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- -1 sodium peroxydisulfate Phenol Chemical compound 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000007725 thermal activation Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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Abstract
本发明属于水污染物处理领域，涉及一种新型的基于樱桃核的生物质铁碳复合材料。该催化材料可通过活化过硫酸钠产生活性自由基来降解水体中的有机污染物双酚A。该催化剂制备方法简单，所采用原辅材料价格低廉，容易实现批量化制备，能够快速高效的催化过硫酸钠降解双酚A，并且该铁碳复合材料具有顺磁性，催化降解完成后可以利用磁铁很容易的将材料从溶液中分离出来。结果表明，基于樱桃核的生物质铁碳复合材料活化过硫酸钠产生活性自由基降解废水中的有机污染物是一种很有前景的污染物去除技术。
Description
技术领域
本发明属于水污染物处理领域，制备了一种基于樱桃核的生物质铁碳复合材料，将其作为一种新型的催化剂活化过硫酸钠产生活性自由基来降解水体中的有机污染物双酚A。
背景技术
基于硫酸根自由基(SO4 ·-)的高级氧化技术是近年来发展起来的一类处理难降解有机污染物的新型技术[1-4]。SO4 ·-主要通过活化过硫酸盐产生，过硫酸盐包括过一硫酸盐(PMS)和过二硫酸盐(PDS)，两者结构中均有不稳定的O-O键[5, 6]，易于接收外来电子断裂。SO4 ·-的氧化还原电位（2.5-3.1 V）较高，具有很强的氧化性，并且存在寿命高于一般的活性自由基。因此，相对于其它传统水处理技术，基于SO4 ·-的高级氧化技术具有高效、快速、彻底、选择性小且反应条件温和等优点，在环境污染修复与治理领域具有广泛的应用前景。
常见活化过硫酸盐的方式包括热活化、微波活化、超声活化、紫外光活化、过渡金属离子活化、碳材料活化、碱活化等[7, 8]。光或热的物理活化方法快速、无二次污染，但通常需要复杂的设备与较高的能耗。均相过渡金属离子催化体系反应条件温和、能耗低，传质速率高，催化剂与过硫酸盐接触充分，活化效率高，但也存在分离回收困难、易造成二次污染、碱性条件下因沉淀而降低活性等缺点。基于上述不足，开发基于过渡金属的非均相催化剂具有十分重要的意义。铁材料具有价格低廉、环境友好等优点，常被用作过硫酸盐的活化材料。纳米零价铁可以缓慢释放Fe2+，从而控制过硫酸盐的活化速度，保证体系持续高效地降解污染物[9, 10]。Tan等[11]以商品化的纳米Fe3O4活化PMS降解对乙酰氨基酚。Ji等[12]以水热-煅烧法合成多孔Fe2O3颗粒活化PMS用于罗丹明B的脱色，催化剂具有高的活性和重复利用性。这些方法取得了良好的效果，然而催化材料的制备存在方法复杂、成本较高，只能在实验室进行少量的制备的应用研究。
随着工农业的发展和人民生活水平的提高，必然会产生大量的生物质废弃物。如果这些废弃物处置不当，就会对水体、大气、土壤等造成严重的环境污染。废弃生物质的主要成分包括纤维素、半纤维素和木质素，将其在隔绝空气条件下裂解或不完全燃烧可以制备性能优良的生物质活性炭。在生物质废弃物裂解的过程中，可以通过碳热还原将过渡金属还原制备复合材料。樱桃核是一种常见的食品行业的生物质废弃物，其主要成分包括苷类、黄酮、萜类、酚类、挥发油鞣质、单宁化合物、儿茶素和表儿茶素等[13]。
本文将樱桃核粉末与无水FeCl3混合均匀，在惰性气氛下高温煅烧，Fe3+可以利用其氧化性活化樱桃核粉，本身被还原为铁纳米颗粒负载到樱桃核粉生物质活性炭上，将该材料用于催化活化过硫酸钠产生活性自由基降解内分泌干扰物双酚A。
主要参考文献：
[1] 谷得明, 郭昌胜, 冯启言, 张远, 徐建, 基于硫酸根自由基的高级氧化技术及其在环境治理中的应用, 环境化学, 37 (2018) 2489-2508.
[2] 杨世迎, 陈友媛, 胥慧真, 王萍, 刘玉红, 王茂东, 过硫酸盐活化高级氧化新技术, 化学进展, (2008) 1433-1438.
[3] A.-Y. Zhang, N.-H. Huang, Y.-Y. He, P.-C. Zhao, J.-W. Feng, Sulfateradicals generation and refractory pollutants removal on defective facet-tailored TiO2 with reduced matrix effects, Chem Eng J, 358 (2019) 243-252.
[4] H. Liu, T.A. Bruton, W. Li, J.V. Buren, C. Prasse, F.M. Doyle, D.L.Sedlak, Oxidation of Benzene by Persulfate in the Presence of Fe(III)- and Mn(IV)-Containing Oxides: Stoichiometric Efficiency and TransformationProducts, Environ Sci Technol, 50 (2016) 890-898.
[5] X. Lou, L. Wu, Y. Guo, C. Chen, Z. Wang, D. Xiao, C. Fang, J. Liu, J.Zhao, S. Lu, Peroxymonosulfate activation by phosphate anion for organicsdegradation in water, Chemosphere, 117 (2014) 582-585.
[6] W.-D. Oh, S.-K. Lua, Z. Dong, T.-T. Lim, A novel three-dimensionalspherical CuBi2O4 consisting of nanocolumn arrays with persulfate andperoxymonosulfate activation functionalities for 1H-benzotriazole removal,Nanoscale, 7 (2015) 8149-8158.
[7] W.-D. Oh, T.-T. Lim, Design and application of heterogeneouscatalysts as peroxydisulfate activator for organics removal: An overview,Chem Eng J, 358 (2019) 110-133.
[8] Q. Zhao, Q. Mao, Y. Zhou, J. Wei, X. Liu, J. Yang, L. Luo, J. Zhang,H. Chen, H. Chen, L. Tang, Metal-free carbon materials-catalyzed sulfateradical-based advanced oxidation processes: A review on heterogeneouscatalysts and applications, Chemosphere, 189 (2017) 224-238.
[9] R. Li, X. Jin, M. Megharaj, R. Naidu, Z. Chen, Heterogeneous Fentonoxidation of 2,4-dichlorophenol using iron-based nanoparticles and persulfatesystem, Chem Eng J, 264 (2015) 587-594.
[10] 金晓英, 李任超, 陈祖亮, 纳米零价铁活化过硫酸钠降解2,4-二氯苯酚, 环境化学, 33 (2014) 812-818.
[11] C. Tan, N. Gao, Y. Deng, J. Deng, S. Zhou, J. Li, X. Xin, Radicalinduced degradation of acetaminophen with Fe3O4 magnetic nanoparticles asheterogeneous activator of peroxymonosulfate, J Hazard Mater, 276 (2014) 452-460.
[12] F. Ji, C. Li, X. Wei, J. Yu, Efficient performance of porous Fe2O3in heterogeneous activation of peroxymonosulfate for decolorization ofRhodamine B, Chem Eng J, 231 (2013) 434-440.
[13] 甄天元, 肖军霞, 樱桃核主要成分分析及其抗氧化性研究, 食品研究与开发,35 (2014) 112-115。
发明内容
本发明制备了一种铁纳米颗粒负载的樱桃核生物质碳材料，将该材料用作催化剂活化过硫酸钠产生活性自由基来降解水体环境中的有机污染物双酚A，取得了良好的效果。
材料的制备方法为：将5.78 g无水三氯化铁与2.0 g樱桃核粉末分散到50 mL乙醇溶液中，搅拌加热至50℃蒸干。之后将固体研磨后置于管式电阻炉，保持氩气气氛，以10℃/min的速度升温到800 ℃煅烧，保持5 h后自然冷却降温，得到基于樱桃核的生物质铁碳复合材料。
以双酚A为目标物，研究制备出的复合材料催化活化过硫酸钠对其的降解性能。实验结果证明：当双酚A浓度为20 mg/L，催化材料浓度0.1 g/L，氧化剂过硫酸钠浓度1.0 g/L时，只需要5 min时间就可以将双酚A完全降解，30 min总有机碳去除率接近40%，且整个反应受溶液pH的影响不大。因此，以基于樱桃核的生物质铁碳复合材料活化过硫酸钠产生活性自由基降解废水中的有机污染物是一种很有前景的有机污染物去除技术。
该催化材料主要有以下优点：
1.制备方法简单，易于规模化生产：只需将原材料混合均匀后隔绝空气高温裂解就可以得到复合材料，裂解过程中同步实现生物质炭的活化和铁纳米颗粒的负载。
2.催化效率高，反应速率快：催化降解双酚A所需的催化剂浓度较低，在5 min之内就可以将20 mg/L双酚A完全降解。
3.成本低廉，环境友好：主要原材料为生物质废弃物樱桃核和铁盐，价格低廉，能够实现废物的资源化，并且铁盐也属于环境友好的金属材料。
4.易于磁分离，操作方便：制备的材料具有良好的顺磁性，催化降解完成后，利用外加磁场可以很容易将催化剂从溶液中分离出来。
附图说明
图1是基于樱桃核的生物质铁碳复合材料的扫描电镜图
图2是生物质铁碳复合材料对双酚A的降解效率和TOC去除率
Claims (3)
1.制备了一种基于樱桃核的生物质铁碳复合材料。
2.权利1所述的生物质铁碳复合材料是将樱桃核粉末与无水FeCl3混合均匀，在氩气气氛下高温煅烧得到。
3.将按权利2方法制备的生物质铁碳复合材料用于催化过硫酸钠降解水中的内分泌干扰物双酚A。
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