抚顺油页岩残渣制备氧化铝和白炭黑研究
摘要
油页岩残渣是油页岩在工业制油、燃烧以及发电等化工过程中产生的废料,如果直接抛弃不仅会对环境造成不必要的污染和破坏,而且是对资源的浪费。本文旨在利用油页岩残渣制备氧化铝和白炭黑,探索一种适合油页岩残渣回收利用的实验方案。
实验以抚顺油页岩制油残渣为原料,先以酸溶法提取原料中的Al2O3,再通过碱溶反应将残渣中的SiO2化为Na2SiO3。考察了原料粒度、煅烧温度、煅烧时间、酸碱溶液浓度、液固比、反应温度及反应时间对油页岩残渣中Al2O3和SiO2浸出率的影响规律。结果表明,抚顺油页岩残渣最佳煅烧温度为850℃,煅烧时间为1.0h,原料粒度为0.074mm；酸溶反应最佳盐酸浓度为12%,液固比为5：1,反应温度为100℃,反应时间为1.5h；碱溶反应最佳NaOH浓度为6mol/L,液固比为5：1,反应温度为90℃,反应时间为3.0h。在上述所得最佳工艺条件下,原料中Al2O3和SiO2的浸出率分别为81.75%和80.01%。
采用均相化学沉淀法由酸溶反应得到的氯化铝滤液制备氧化铝,通过单因素考察法确定最佳工艺条件如下：反应温度为55℃,铝酸钠浓度为0.4mol/L,乙酸乙酯加入与铝离子物质的量比为1.7：1,反应时间为1.5h,活性剂的剂量为总体系质量的0.3%。各项工艺指标在最佳工艺条件下时,得到中位径(d50)为0.216μm的氧化铝白色粉末。经表征研究证实所得产品是γ-Al2O3。经醋酸分离提纯后纯度可达98.7%。
采用二氧化碳为潜伏酸化剂代替强酸,结合醋酸的高选择性分离方法,研究以油页岩制油残渣提取氧化铝后的滤渣为原料,低腐蚀低能耗条件下制备高品质白炭黑的工艺方法,并研究工艺条件对白炭黑产品的粒径分布影响规律。研究表明,采用碳化反应法,由残渣碱提取液硅酸钠溶液制备白炭黑的最佳工艺条件为：反应温度为50℃,硅酸钠溶液浓度为0.0274g/ml,CO2流量为20ml/min,表面活性剂聚乙二醇6000的用量为0.007g/ml,此工艺条件下得到的白炭黑粒径最小,为20-30nm,经醋酸分离提纯后的白炭黑纯度为98.4%。
In the processes of oil refining industry, burning system and power generation process using oil shale will produce residue of oil shale, it will not only bring unnecessary pollution and destruction to environment, but also waste of resources if directly throw away. This paper intends to preparation alumina and silica to explor a suitable way to make good use and recycle of residue.
The work take residue of Fushun oil shale as raw material, Al2O3 in material converts into AICl3 by means of acid leaching reaction at first, and then SiO2 converts into Na2SiO3 through alkali leaching reaction. Using single-factor method research influence of activation temperature, activation time, granularity of raw material, concentration of HCl and NaOH solution, liquid-solid ratio, reaction temperature and reaction period on leaching rates of Al2O3 and SiO2 were obtained. The optimum technological conditions of Al2O3 and SiO2 leaching process are as follows:the activation temperature is 850℃, the activation time is 1.0h, the granularity of raw material is 0.074mm; The optimum acid leaching conditions are listed as follows:the concentration of acid is 12%, the liquid-solid ratio is 5:1, reaction temperature is 100℃, the reaction period is 1.5h; The optimum alkaline leaching conditions are as follows:the concentration of NaOH solution is 6mol/L, the liquid-solid ratio is 5:1, the reaction temperature is 90℃, the reaction time for 3.Oh. The leaching rates of Al2O3 and SiO2 are 81.75% and 80.01% respectively.
Homogeneous chemical precipitation method was used in the alumina preparation. Optimum technological conditions of alumina preparation are determined by single-factor research method. The result is as follows:the reaction goes at 55℃for 1.5h, the concentration of sodium meta aluminate is 0.4 mol/L, the dose of surfactant is 0.3% of total system quality. the purity can be effectively improved by acetic acid solution(25%) wash,γ-Al2O3 is 0.216μm(d5o), and the degree of purity is 98.7%.
Using CO2 replacing strong acid as latent acidifier and combining highly selective separation method of acetic acid study, the silica was prepared from filter cake that gets from acid leaching process and the influence of preparation process on particle size of silica. The results show that optimum technological conditions of modification preparation silica are as follows:the reaction temperature is 50℃, the concentration of sodium silicate 0.027g/L, CO2 flow is 20ml/min, the dose of surfactant is 0.007g/ml of volume of total system. The white powder silica was spherical approximately, and the average particle size(d50) was 20-30nm. the product could be comparable with the relevant national standards, degree of purity is 98.4%. It provides a new way for the development and utilization of residue of oil shale,.
实验以抚顺油页岩制油残渣为原料,先以酸溶法提取原料中的Al2O3,再通过碱溶反应将残渣中的SiO2化为Na2SiO3。考察了原料粒度、煅烧温度、煅烧时间、酸碱溶液浓度、液固比、反应温度及反应时间对油页岩残渣中Al2O3和SiO2浸出率的影响规律。结果表明,抚顺油页岩残渣最佳煅烧温度为850℃,煅烧时间为1.0h,原料粒度为0.074mm；酸溶反应最佳盐酸浓度为12%,液固比为5：1,反应温度为100℃,反应时间为1.5h；碱溶反应最佳NaOH浓度为6mol/L,液固比为5：1,反应温度为90℃,反应时间为3.0h。在上述所得最佳工艺条件下,原料中Al2O3和SiO2的浸出率分别为81.75%和80.01%。
采用均相化学沉淀法由酸溶反应得到的氯化铝滤液制备氧化铝,通过单因素考察法确定最佳工艺条件如下：反应温度为55℃,铝酸钠浓度为0.4mol/L,乙酸乙酯加入与铝离子物质的量比为1.7：1,反应时间为1.5h,活性剂的剂量为总体系质量的0.3%。各项工艺指标在最佳工艺条件下时,得到中位径(d50)为0.216μm的氧化铝白色粉末。经表征研究证实所得产品是γ-Al2O3。经醋酸分离提纯后纯度可达98.7%。
采用二氧化碳为潜伏酸化剂代替强酸,结合醋酸的高选择性分离方法,研究以油页岩制油残渣提取氧化铝后的滤渣为原料,低腐蚀低能耗条件下制备高品质白炭黑的工艺方法,并研究工艺条件对白炭黑产品的粒径分布影响规律。研究表明,采用碳化反应法,由残渣碱提取液硅酸钠溶液制备白炭黑的最佳工艺条件为：反应温度为50℃,硅酸钠溶液浓度为0.0274g/ml,CO2流量为20ml/min,表面活性剂聚乙二醇6000的用量为0.007g/ml,此工艺条件下得到的白炭黑粒径最小,为20-30nm,经醋酸分离提纯后的白炭黑纯度为98.4%。
In the processes of oil refining industry, burning system and power generation process using oil shale will produce residue of oil shale, it will not only bring unnecessary pollution and destruction to environment, but also waste of resources if directly throw away. This paper intends to preparation alumina and silica to explor a suitable way to make good use and recycle of residue.
The work take residue of Fushun oil shale as raw material, Al2O3 in material converts into AICl3 by means of acid leaching reaction at first, and then SiO2 converts into Na2SiO3 through alkali leaching reaction. Using single-factor method research influence of activation temperature, activation time, granularity of raw material, concentration of HCl and NaOH solution, liquid-solid ratio, reaction temperature and reaction period on leaching rates of Al2O3 and SiO2 were obtained. The optimum technological conditions of Al2O3 and SiO2 leaching process are as follows:the activation temperature is 850℃, the activation time is 1.0h, the granularity of raw material is 0.074mm; The optimum acid leaching conditions are listed as follows:the concentration of acid is 12%, the liquid-solid ratio is 5:1, reaction temperature is 100℃, the reaction period is 1.5h; The optimum alkaline leaching conditions are as follows:the concentration of NaOH solution is 6mol/L, the liquid-solid ratio is 5:1, the reaction temperature is 90℃, the reaction time for 3.Oh. The leaching rates of Al2O3 and SiO2 are 81.75% and 80.01% respectively.
Homogeneous chemical precipitation method was used in the alumina preparation. Optimum technological conditions of alumina preparation are determined by single-factor research method. The result is as follows:the reaction goes at 55℃for 1.5h, the concentration of sodium meta aluminate is 0.4 mol/L, the dose of surfactant is 0.3% of total system quality. the purity can be effectively improved by acetic acid solution(25%) wash,γ-Al2O3 is 0.216μm(d5o), and the degree of purity is 98.7%.
Using CO2 replacing strong acid as latent acidifier and combining highly selective separation method of acetic acid study, the silica was prepared from filter cake that gets from acid leaching process and the influence of preparation process on particle size of silica. The results show that optimum technological conditions of modification preparation silica are as follows:the reaction temperature is 50℃, the concentration of sodium silicate 0.027g/L, CO2 flow is 20ml/min, the dose of surfactant is 0.007g/ml of volume of total system. The white powder silica was spherical approximately, and the average particle size(d50) was 20-30nm. the product could be comparable with the relevant national standards, degree of purity is 98.4%. It provides a new way for the development and utilization of residue of oil shale,.
引文
[1]张洁,李冰.非常规油气资源正在走向产业化[J].中国石化,2008,7：26-28.
[2]陈洁渝,严春杰,李子冲,等.油页岩渣的综合利用[J].矿产保护与利,2006,6：41-45.
[3]易德莲.纳米二氧化硅改性及其在丁基橡胶中的应用[J].武汉科技大学学报,2007,30(6)：640～642.
[4]孙月蓉.纳米白炭黑的表面改性及其在氯丁橡胶中的应用[J].江苏化工,2004,32(5)：36-38.
[5]王宝君,张培萍,李书法,等.白炭黑的应用与制备方法[J].世界地质[J],2006,3(1)：15-17.
[6]Jamile Brandi, Julio Cesar Ximenes, Mariselma Ferreira, et al. Gelcasting of alumina-chitosan beads[J]. Ceramics Internationa,2011,37(4):1231-1235.
[7]杨本意,段先健,李仕华,等.气相法白炭黑的应用技术[J].有机硅材料[J],2003,4：28-32
[8]钱家麟等.油页岩-石油的补充能源[M].北京：中国石化出版社,2008.
[9]陈会军,刘招君,朱建伟,等.油页岩资源开发利用经济评价[J].地质与资源,2011,20(1)：50-55.
[10]Indrek Kulaots, Jillian L. Goldfarb, Eric M. Suuberg. Characterization of Chinese, American and Estonian oil shale semicokes and their sorptive potential [J]. Fuel, 2010,89(11):3300-3306.
[11]李术元,岳长涛,王剑秋,钱家麟.世界油页岩开发利用近况—记美国第28届国际油页岩会议[J].中外能源,2009,(02)
[12]刘招君,董清水,叶松青等.中国油页岩资源现状[J].吉林大学学报(地球科学版),2006,36(6)：869-876.
[13]韩晓辉,卢桂萍,孙朝辉,等.国外油页岩干馏工艺研究开发进展[J].中外能源,2011,16(4)：69-74.
[14]陈明东,史宇亮,董良杰.油页岩热裂解产物页岩油的相关性质分析[J].矿产综合利用,2010，8：31-33.
[15]王军,梁杰,王泽等.温度对油页岩快速热解特性的影响[J].煤炭化,2010,33(1)：65-68.
[16]刘同仁,张磊.龙口矿区油页岩综合利用集成技术[J].山东煤炭科技,2011,20(1)50-55.
[17]冯宗玉.油页岩渣综合利用研究[D].沈阳：东北大学材料与冶金学院,2008.
[18]陈洁渝,严春杰,李子冲,等.油页岩渣的综合利用[J].矿产保护与利用.2006, (6)42-45.
[19]邓家平,李泽林,董艳辉,等.还原法陶粒的诞生与油页岩渣超轻陶粒的研究[J].粉煤灰,2010,4：27-32.
[20]王文颖.油页岩灰渣提取铝与纳米氧化铝粉体的制备研究[D].长春：吉林大学化学学院,2008.
[21]安佰超.油页岩灰渣提取氧化铝及其应用[D].长春：吉林大学化学学院,2008.
[22]冯宗玉,李勇,薛向欣等.利用油页岩渣制备氧化铝和白炭黑[J].矿冶工程,2008,28(4)： 53-57.
[23]Xu Yingmei, He Demin, Jiang Huiming, et al. Characterization of Oil Shale Processing Residues And Separated Products[J]. Oil Shale,2009,26(4):500-512.
[24]Xu Yingmei, He Demin, Wang Dongmei, et al. Influence of calcination temperature on leaching rate of aluminum and iron impurities in oil shale ash[J].Oil Shale, 2009,26 (2):163-168.
[25]李勇,冯宗玉,薛向欣,等.油页岩灰酸碱离解法制备白炭黑的工艺比较[J].硅酸盐通报,2008,27(1)：6-11.
[26]An Baichao, Wang Wenying, JI Guijuan, Gan Shucai, Gao Guimei, Xu Jijing, Li Guanghuan. Preparation of nano-sized α-Al2O3 from oil shale ash[J]. Energy,2010, 35(1):45-49.
[27]Liu, Q., A. Wang, et al. Synthesis, characterization and catalytic applications of mesoporous γ-alumina from boehmite sol [J]. Microporous and Mesoporous Materials, 2008,111(1-3):323-333.
[28]Arro H, Prikk A, Pihu T. Utilization of semi-coke of Estonian shale oil industry [J]. Oil shale,2002,19(2):117-125.
[29]李勇,薛向欣,冯宗玉.用油页岩渣制备白炭黑的工艺[J]..过程工程学报,2007,7(4)：751-754.
[30]Jiang, X., X. Han, et al. Progress and recent utilization trends in combustion of Chinese oil shale[J]. Progress in Energy andCombustion Science,2007,33(6): 552-579.
[31]Trikkel, A, R. Kuusik, et al. Utilization of Estonian oil shale semi coke [J]. Fuel Processing Technology,2008,89(8):756-763.
[32]Gao Gui-mei, Zou Haifeng, Gan Shucai, et al. Preparation and properties of silica nanoparticles from oil shale ash[J]. Powder Technology,2009,191:47-51.
[33]伏耀龙,王永健,王益权,等.油页岩栽培基质脱盐技术及其效果研究[J].干旱地区农业研究,2009,27(6)：223-227.
[34]侯顺,程程.关于利用改性油页岩残渣处理含Pb2+、Cd2-废水的研究[J].中国环境管理丛书,2010,6：24-26.
[35]李勇,薛向欣,冯宗玉.改性油页岩灰吸附Cu2+的研究[J].材料与冶金学报,2007,6(4)：302-305.
[36]张晓锋,于国强,姜林文.氧化铝陶瓷的应用[J].佛山陶瓷,2010,20(2)：38-42.
[37]王爱军.准气相反应法制备多孔氧化铝球形颗粒[D].北京：北京交通大学理学院,2010.
[38]夏雪梅.纳米氧化铝制备研究[D].长春：长春工业大学,2009.
[39]卢伟光,龙军,田辉平.镧和铈改性对氧化铝性质的影响[J].催化学报,2003,24(8)：574-578.
[40]张义,高中良,陈永生,等.锰/γ-氧化铝催化剂的制备研究[J].无机盐工业,2010,42(4)：33-35.
[41]于闽.新型片状氧化铝材料的合成及在珠光颜料中的应用[D].上海：复旦大学化学系,2010.
[42]吴铭敏.高岭土制备纳米氧化铝工艺研究[D].苏州：苏州大学,2009.
[43]饶拴民.对高铝粉煤灰生产氧化铝技术及工业化生产技术路线的思考[J].轻金属,20101：15-19.
[44]田祯.拜耳法氧化铝生产后加矿增浓溶出技术应用分析[J].轻金属,2008,4：19-25.
[45]Greg Power, Joanne Loh. Organic compounds in the processing of lateritic bauxites to alumina:Part 1:Origins and chemistry of organics in the Bayer process[J]. Hydrometallurgy,2010,105(1-2):1-29.
[46]郑朝付,李民菁,史智慧,等.低苛性比溶出在拜耳法氧化铝生产中的应用[J].矿产保护与利用,2009,3：37-40.
[47]李波.拜耳法氧化铝管道溶出及平盘过滤清洁生产技术研究[D].济南：山东大学,2009.
[48]丁宏娅.采用改进酸碱联合法从高铝粉煤灰中提取氧化铝的研究[D].武汉：中国地质大学,2007.
[49]Xun Liu, Tianyou Peng, Jinchun Yao, et al. Synthesis and textural evolution of alumina particles with mesoporous structures [J]. Journal of Solid State Chemistry,2010,183(6):1448-1456.
[50]F. Mirjalili, M. Hasmaliza, L. Chuah Abdullah. Size-controlled synthesis of nano α-alumina particles through the sol-gel method[J]. Ceramics International,2010,36(4):1253-1257.
[51]曹亚鹏,郭奋,梁磊,等.高浓度水热法制备改性纳米氢氧化铝及流变性能[J].化工进展,2007,,2(5)：674-678.
[52]Jeremy P. Wu, Ian W. M. Brown, Mark E. Bowden, et al. Palladium coated porous anodic alumina membranes for gas reforming processes[J]. Solid State Sciences,2010,12(11):1912-1916.
[53]Tiberiu Popa, Guoqing Xu, Thomas F. Barton, et al. High temperature water gas shift catalysts with alumina[J]. Applied CatalysisA:General,397(1-2):15-23.
[54]B. S. Yilbas, C. Karatas, A. F. M. Arif, et al. Laser control melting of alumina surfaces and thermal stress analysis[J]. Optics & Laser Technology,2011,43(3): 858-865.
[55]商连弟,武换荣,张艳红.中国化学品氧化铝生产现状及发展趋势[J].无机盐工业,2009,41(12)：11-13.
[56]白炭黑生产工艺及应用[J].中国粉体工业.2007(02)：42-43.
[57]Daniela E. Achatz, Florian J. Heiligtag, Xiaohua Li, et al. Colloidal silica nanoparticles for use in click chemistry-based conjugations and fluorescent affinity assays[J]. Sensors and Actuators B:Chemical,2010,150(1):211-219.
[58]M. Jafarzadeh, I.A. Rahman, C. S. Sipaut. Optical properties of amorphous organo-modified silica nanoparticles produced via co-condensation method[J]. Ceramics International,2010,36 (1):333-338.
[59]Katherine Kho, Kunn Hadinoto. Aqueous re-dispersibility characterization of spray-dried hollow spherical silica nano-aggregates[J]. Powder Technology, 2010,198(3):354-363.
[60]陈平,晏美娟,黄自华.特种气相法白炭黑R300在天然橡胶中的应用[J].橡胶科技市场2010.1：11-13.
[61]G. Serensen, A.L. Nielsen, Morten Mφller Pedersen,et al. Controlled release of biocide from silica microparticles in wood paint[J]. Progress in Organic Coatings,2010,68(4):299-306.
[62]牟秋红.导热硅橡胶的制备及性能研究[J].材料导报：研究篇,2009年3月(下)第23卷第三期.
[63]尹进华,于航,孙培宾,等.具有二次微粒结构的高分散型白炭黑的应用测试[J].化工新型材料,2011,39(1)：117-118.
[64]T. Nema, E. C. Y. Chan, P. C. Ho. Application of silica-based monolith as solid phase extraction cartridge for extracting polar compounds from urine[J]. Talanta,2010,82 (2); 488-494.
[65]Young-Jae Kang, Y. Nagendra Prasad, In-Kwon Kim,et al. Synthesis of Fe metal precipitated colloidal silica and its application to W chemical mechanical polishing (CMP) slurry[J]. Journal of Colloid and Interface Science,2010,349 (1):402-407.
[66]Raffaele Ricco, Anna Meneghello, Francesco Enrichi. Signal enhancement in DNA microarray using dye doped silica nanoparticles:Application to Human Papilloma Virus (HPV) detection[J]. Biosensors and Bioelectronics,2011,26(5):2761-2765.
[67]严大洲,汤传斌,谢正和.气相法白炭黑生产技术的研究[J].有色冶金节能,2010,6：33-35.r
[68]陈霞.影响气相法白炭黑质量的因素及处理措施[J].河南化工,2010,27(10)：37-38.
[69]李建芳.硅烷偶联剂对超细沉淀法白炭黑表面改性的研究[J].江西化工,20102：52-53.
[70]Kyomin Shin, Jin-Joo Kim, Kyung-Do Suh. A facile process for generating monolithic-structured nano-silica/polystyrene multi-core/shell microspheres by a seeded sol-gel process method[J]. Journal of Colloid and Interface Science,2010,350(2):581-585.
[71]关鲁雄,区叶秀.常压溶胶-凝胶法合成SiO2气凝胶的研究[J].硅酸盐通报,2010,29(2)：334-339.
[72]骆锋,阮建明,万千.微乳液法制备纳米二氧化硅粉末工艺的研究[J].硅酸盐通报,2004,5：48-52.
[73]刘欣梅,潘正鸿,李国,等.用煤系高岭土制取白炭黑的研究[J].石油大学学报(自然科学版).2005,29(2)：121-124.
[74]Vuk Uskokovic, Miha Drofenik. Reverse micelles:Inert nano-reactors or Physico-chemicallyactive guides of the capped reactions[J]. Advances in Colloid and Interface Science,2007(133):23-34.
[75]Teofil Jesionowski, et al. The influence of filler modification on its aggregation and dispersion behaviour in silica/PBT composite[J].Composite Interfaces,2003,10 (2-3):225-242.
[76]徐子芳,张明旭,李新运.用低温煅烧法从粉煤灰中提取纳米Al2O3和SiO2[J].非金属矿,2009,32(1)：27-30.
[77]孔德顺,肖杰,吴红,等.煤矸石碱熔提取白炭黑的研究[J].化工新型材料,2011,39(20)：114-116.
[78]任肖冬.哈密硅灰石制备白炭黑工艺及性能表征[D].乌鲁木齐：新疆大学,2010.
[79]文焱炳, 杨建安, 唐波, 朱建国. 改性白炭黑制备工艺研究进展[J].2008,38(1)：12-14.
[80]王艳 李光明 朱辉.高硬度有机硅橡胶耐热性能与回弹性能的改善[J].化工新型材料,2005,33(8)：35.
[81]M. Owezarek, M. Zaborski. Chlorsulfonated Polyethylene Elastomers Containing Zinc Oxide Ineorporated on Si02 [J]. Kautschuk Gummi Kunststoffe,2004,57(5):218-223.
[82]姚英.表面活性剂对碳化法制备白炭黑的影响研究[J].天津化工,2006,20(4)：36-37.
[83]于欣伟,陈姚.白炭黑的表面改性技术[J].广州大学学报(自然科学版),2002,6：12-16.
[84]李来时,翟玉春,秦晋国,吴艳.以粉煤灰为原料制各高纯氧化铝[J].化工学报,2006,57(9)：2189--2193.
[85]崔运成,李丹丹,孙顺丹.用不同原料制备白炭黑的工艺研究[J].吉林师范大学学报：自然科学版,2005,3：33-36.
[86]王冬梅.桦甸油页岩残渣制备白炭黑及改性研究[D].大连：大连理工大学化工环境与生命学部,2009.
[2]陈洁渝,严春杰,李子冲,等.油页岩渣的综合利用[J].矿产保护与利,2006,6：41-45.
[3]易德莲.纳米二氧化硅改性及其在丁基橡胶中的应用[J].武汉科技大学学报,2007,30(6)：640～642.
[4]孙月蓉.纳米白炭黑的表面改性及其在氯丁橡胶中的应用[J].江苏化工,2004,32(5)：36-38.
[5]王宝君,张培萍,李书法,等.白炭黑的应用与制备方法[J].世界地质[J],2006,3(1)：15-17.
[6]Jamile Brandi, Julio Cesar Ximenes, Mariselma Ferreira, et al. Gelcasting of alumina-chitosan beads[J]. Ceramics Internationa,2011,37(4):1231-1235.
[7]杨本意,段先健,李仕华,等.气相法白炭黑的应用技术[J].有机硅材料[J],2003,4：28-32
[8]钱家麟等.油页岩-石油的补充能源[M].北京：中国石化出版社,2008.
[9]陈会军,刘招君,朱建伟,等.油页岩资源开发利用经济评价[J].地质与资源,2011,20(1)：50-55.
[10]Indrek Kulaots, Jillian L. Goldfarb, Eric M. Suuberg. Characterization of Chinese, American and Estonian oil shale semicokes and their sorptive potential [J]. Fuel, 2010,89(11):3300-3306.
[11]李术元,岳长涛,王剑秋,钱家麟.世界油页岩开发利用近况—记美国第28届国际油页岩会议[J].中外能源,2009,(02)
[12]刘招君,董清水,叶松青等.中国油页岩资源现状[J].吉林大学学报(地球科学版),2006,36(6)：869-876.
[13]韩晓辉,卢桂萍,孙朝辉,等.国外油页岩干馏工艺研究开发进展[J].中外能源,2011,16(4)：69-74.
[14]陈明东,史宇亮,董良杰.油页岩热裂解产物页岩油的相关性质分析[J].矿产综合利用,2010，8：31-33.
[15]王军,梁杰,王泽等.温度对油页岩快速热解特性的影响[J].煤炭化,2010,33(1)：65-68.
[16]刘同仁,张磊.龙口矿区油页岩综合利用集成技术[J].山东煤炭科技,2011,20(1)50-55.
[17]冯宗玉.油页岩渣综合利用研究[D].沈阳：东北大学材料与冶金学院,2008.
[18]陈洁渝,严春杰,李子冲,等.油页岩渣的综合利用[J].矿产保护与利用.2006, (6)42-45.
[19]邓家平,李泽林,董艳辉,等.还原法陶粒的诞生与油页岩渣超轻陶粒的研究[J].粉煤灰,2010,4：27-32.
[20]王文颖.油页岩灰渣提取铝与纳米氧化铝粉体的制备研究[D].长春：吉林大学化学学院,2008.
[21]安佰超.油页岩灰渣提取氧化铝及其应用[D].长春：吉林大学化学学院,2008.
[22]冯宗玉,李勇,薛向欣等.利用油页岩渣制备氧化铝和白炭黑[J].矿冶工程,2008,28(4)： 53-57.
[23]Xu Yingmei, He Demin, Jiang Huiming, et al. Characterization of Oil Shale Processing Residues And Separated Products[J]. Oil Shale,2009,26(4):500-512.
[24]Xu Yingmei, He Demin, Wang Dongmei, et al. Influence of calcination temperature on leaching rate of aluminum and iron impurities in oil shale ash[J].Oil Shale, 2009,26 (2):163-168.
[25]李勇,冯宗玉,薛向欣,等.油页岩灰酸碱离解法制备白炭黑的工艺比较[J].硅酸盐通报,2008,27(1)：6-11.
[26]An Baichao, Wang Wenying, JI Guijuan, Gan Shucai, Gao Guimei, Xu Jijing, Li Guanghuan. Preparation of nano-sized α-Al2O3 from oil shale ash[J]. Energy,2010, 35(1):45-49.
[27]Liu, Q., A. Wang, et al. Synthesis, characterization and catalytic applications of mesoporous γ-alumina from boehmite sol [J]. Microporous and Mesoporous Materials, 2008,111(1-3):323-333.
[28]Arro H, Prikk A, Pihu T. Utilization of semi-coke of Estonian shale oil industry [J]. Oil shale,2002,19(2):117-125.
[29]李勇,薛向欣,冯宗玉.用油页岩渣制备白炭黑的工艺[J]..过程工程学报,2007,7(4)：751-754.
[30]Jiang, X., X. Han, et al. Progress and recent utilization trends in combustion of Chinese oil shale[J]. Progress in Energy andCombustion Science,2007,33(6): 552-579.
[31]Trikkel, A, R. Kuusik, et al. Utilization of Estonian oil shale semi coke [J]. Fuel Processing Technology,2008,89(8):756-763.
[32]Gao Gui-mei, Zou Haifeng, Gan Shucai, et al. Preparation and properties of silica nanoparticles from oil shale ash[J]. Powder Technology,2009,191:47-51.
[33]伏耀龙,王永健,王益权,等.油页岩栽培基质脱盐技术及其效果研究[J].干旱地区农业研究,2009,27(6)：223-227.
[34]侯顺,程程.关于利用改性油页岩残渣处理含Pb2+、Cd2-废水的研究[J].中国环境管理丛书,2010,6：24-26.
[35]李勇,薛向欣,冯宗玉.改性油页岩灰吸附Cu2+的研究[J].材料与冶金学报,2007,6(4)：302-305.
[36]张晓锋,于国强,姜林文.氧化铝陶瓷的应用[J].佛山陶瓷,2010,20(2)：38-42.
[37]王爱军.准气相反应法制备多孔氧化铝球形颗粒[D].北京：北京交通大学理学院,2010.
[38]夏雪梅.纳米氧化铝制备研究[D].长春：长春工业大学,2009.
[39]卢伟光,龙军,田辉平.镧和铈改性对氧化铝性质的影响[J].催化学报,2003,24(8)：574-578.
[40]张义,高中良,陈永生,等.锰/γ-氧化铝催化剂的制备研究[J].无机盐工业,2010,42(4)：33-35.
[41]于闽.新型片状氧化铝材料的合成及在珠光颜料中的应用[D].上海：复旦大学化学系,2010.
[42]吴铭敏.高岭土制备纳米氧化铝工艺研究[D].苏州：苏州大学,2009.
[43]饶拴民.对高铝粉煤灰生产氧化铝技术及工业化生产技术路线的思考[J].轻金属,20101：15-19.
[44]田祯.拜耳法氧化铝生产后加矿增浓溶出技术应用分析[J].轻金属,2008,4：19-25.
[45]Greg Power, Joanne Loh. Organic compounds in the processing of lateritic bauxites to alumina:Part 1:Origins and chemistry of organics in the Bayer process[J]. Hydrometallurgy,2010,105(1-2):1-29.
[46]郑朝付,李民菁,史智慧,等.低苛性比溶出在拜耳法氧化铝生产中的应用[J].矿产保护与利用,2009,3：37-40.
[47]李波.拜耳法氧化铝管道溶出及平盘过滤清洁生产技术研究[D].济南：山东大学,2009.
[48]丁宏娅.采用改进酸碱联合法从高铝粉煤灰中提取氧化铝的研究[D].武汉：中国地质大学,2007.
[49]Xun Liu, Tianyou Peng, Jinchun Yao, et al. Synthesis and textural evolution of alumina particles with mesoporous structures [J]. Journal of Solid State Chemistry,2010,183(6):1448-1456.
[50]F. Mirjalili, M. Hasmaliza, L. Chuah Abdullah. Size-controlled synthesis of nano α-alumina particles through the sol-gel method[J]. Ceramics International,2010,36(4):1253-1257.
[51]曹亚鹏,郭奋,梁磊,等.高浓度水热法制备改性纳米氢氧化铝及流变性能[J].化工进展,2007,,2(5)：674-678.
[52]Jeremy P. Wu, Ian W. M. Brown, Mark E. Bowden, et al. Palladium coated porous anodic alumina membranes for gas reforming processes[J]. Solid State Sciences,2010,12(11):1912-1916.
[53]Tiberiu Popa, Guoqing Xu, Thomas F. Barton, et al. High temperature water gas shift catalysts with alumina[J]. Applied CatalysisA:General,397(1-2):15-23.
[54]B. S. Yilbas, C. Karatas, A. F. M. Arif, et al. Laser control melting of alumina surfaces and thermal stress analysis[J]. Optics & Laser Technology,2011,43(3): 858-865.
[55]商连弟,武换荣,张艳红.中国化学品氧化铝生产现状及发展趋势[J].无机盐工业,2009,41(12)：11-13.
[56]白炭黑生产工艺及应用[J].中国粉体工业.2007(02)：42-43.
[57]Daniela E. Achatz, Florian J. Heiligtag, Xiaohua Li, et al. Colloidal silica nanoparticles for use in click chemistry-based conjugations and fluorescent affinity assays[J]. Sensors and Actuators B:Chemical,2010,150(1):211-219.
[58]M. Jafarzadeh, I.A. Rahman, C. S. Sipaut. Optical properties of amorphous organo-modified silica nanoparticles produced via co-condensation method[J]. Ceramics International,2010,36 (1):333-338.
[59]Katherine Kho, Kunn Hadinoto. Aqueous re-dispersibility characterization of spray-dried hollow spherical silica nano-aggregates[J]. Powder Technology, 2010,198(3):354-363.
[60]陈平,晏美娟,黄自华.特种气相法白炭黑R300在天然橡胶中的应用[J].橡胶科技市场2010.1：11-13.
[61]G. Serensen, A.L. Nielsen, Morten Mφller Pedersen,et al. Controlled release of biocide from silica microparticles in wood paint[J]. Progress in Organic Coatings,2010,68(4):299-306.
[62]牟秋红.导热硅橡胶的制备及性能研究[J].材料导报：研究篇,2009年3月(下)第23卷第三期.
[63]尹进华,于航,孙培宾,等.具有二次微粒结构的高分散型白炭黑的应用测试[J].化工新型材料,2011,39(1)：117-118.
[64]T. Nema, E. C. Y. Chan, P. C. Ho. Application of silica-based monolith as solid phase extraction cartridge for extracting polar compounds from urine[J]. Talanta,2010,82 (2); 488-494.
[65]Young-Jae Kang, Y. Nagendra Prasad, In-Kwon Kim,et al. Synthesis of Fe metal precipitated colloidal silica and its application to W chemical mechanical polishing (CMP) slurry[J]. Journal of Colloid and Interface Science,2010,349 (1):402-407.
[66]Raffaele Ricco, Anna Meneghello, Francesco Enrichi. Signal enhancement in DNA microarray using dye doped silica nanoparticles:Application to Human Papilloma Virus (HPV) detection[J]. Biosensors and Bioelectronics,2011,26(5):2761-2765.
[67]严大洲,汤传斌,谢正和.气相法白炭黑生产技术的研究[J].有色冶金节能,2010,6：33-35.r
[68]陈霞.影响气相法白炭黑质量的因素及处理措施[J].河南化工,2010,27(10)：37-38.
[69]李建芳.硅烷偶联剂对超细沉淀法白炭黑表面改性的研究[J].江西化工,20102：52-53.
[70]Kyomin Shin, Jin-Joo Kim, Kyung-Do Suh. A facile process for generating monolithic-structured nano-silica/polystyrene multi-core/shell microspheres by a seeded sol-gel process method[J]. Journal of Colloid and Interface Science,2010,350(2):581-585.
[71]关鲁雄,区叶秀.常压溶胶-凝胶法合成SiO2气凝胶的研究[J].硅酸盐通报,2010,29(2)：334-339.
[72]骆锋,阮建明,万千.微乳液法制备纳米二氧化硅粉末工艺的研究[J].硅酸盐通报,2004,5：48-52.
[73]刘欣梅,潘正鸿,李国,等.用煤系高岭土制取白炭黑的研究[J].石油大学学报(自然科学版).2005,29(2)：121-124.
[74]Vuk Uskokovic, Miha Drofenik. Reverse micelles:Inert nano-reactors or Physico-chemicallyactive guides of the capped reactions[J]. Advances in Colloid and Interface Science,2007(133):23-34.
[75]Teofil Jesionowski, et al. The influence of filler modification on its aggregation and dispersion behaviour in silica/PBT composite[J].Composite Interfaces,2003,10 (2-3):225-242.
[76]徐子芳,张明旭,李新运.用低温煅烧法从粉煤灰中提取纳米Al2O3和SiO2[J].非金属矿,2009,32(1)：27-30.
[77]孔德顺,肖杰,吴红,等.煤矸石碱熔提取白炭黑的研究[J].化工新型材料,2011,39(20)：114-116.
[78]任肖冬.哈密硅灰石制备白炭黑工艺及性能表征[D].乌鲁木齐：新疆大学,2010.
[79]文焱炳, 杨建安, 唐波, 朱建国. 改性白炭黑制备工艺研究进展[J].2008,38(1)：12-14.
[80]王艳 李光明 朱辉.高硬度有机硅橡胶耐热性能与回弹性能的改善[J].化工新型材料,2005,33(8)：35.
[81]M. Owezarek, M. Zaborski. Chlorsulfonated Polyethylene Elastomers Containing Zinc Oxide Ineorporated on Si02 [J]. Kautschuk Gummi Kunststoffe,2004,57(5):218-223.
[82]姚英.表面活性剂对碳化法制备白炭黑的影响研究[J].天津化工,2006,20(4)：36-37.
[83]于欣伟,陈姚.白炭黑的表面改性技术[J].广州大学学报(自然科学版),2002,6：12-16.
[84]李来时,翟玉春,秦晋国,吴艳.以粉煤灰为原料制各高纯氧化铝[J].化工学报,2006,57(9)：2189--2193.
[85]崔运成,李丹丹,孙顺丹.用不同原料制备白炭黑的工艺研究[J].吉林师范大学学报：自然科学版,2005,3：33-36.
[86]王冬梅.桦甸油页岩残渣制备白炭黑及改性研究[D].大连：大连理工大学化工环境与生命学部,2009.