聚丙烯酰胺的反相乳液聚合及其絮凝沉降性能研究
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摘要
论文采用反相乳液聚合法制备较高分子量的非离子型和阳离子型聚丙烯酰胺乳液絮凝剂,并通过对非离子型聚丙烯酰胺乳液进行“后水解处理”,制备了阴离子型聚丙烯酰胺乳液产品。
反相乳液聚合制备非离子型聚丙烯酰胺的最佳工艺条件为：反应温度为45℃,反应时间为4h,引发剂V-50用量为0.2‰,乳化剂用量为6%,HLB=6,单体浓度为40%,油水比为1.0：1.0,EDTA-2Na用量为0.5‰。聚合工艺条件具有良好的重现性,得到聚合产物相对分子质量高达1100万,通过FT-IR和DSC-TGA对产物结构和热稳定性进行了表征,证明聚合物为AM均聚产物,并且具有良好的热稳定性。
以上述乳液产品为水解原料,以NaOH为水解剂,理论水解度为30%,水解温度为60℃,水解时间为2h的条件下,得到实际水解度为24.5%,相对分子质量660万的部分水解聚丙烯酰胺乳液产品。
以丙烯酰胺(AM)和甲基丙烯酰氧乙基三甲基氯化铵(DMC)为共聚单体,通过反相乳液聚合制备高分子阳离子共聚物P(DMC-AM)的最佳工艺条件为：引发剂V-50用量为1.4‰、乳化剂用量为6%、EDTA-2Na用量为1.0‰、亲水亲油平衡值为6、单体浓度为40%、单体配比为n(DMC):n(AM)=5:95、油水质量比为1.1:1.0、pH值为5、反应温度为50℃及反应时间为4h,在上述条件下,所得产物的相对分子质量可达580万。通过FT-IR对产物结构进行了表征,证实了制备的聚合物为目标产物。
考察了上述乳液絮凝剂对铝土矿正浮选尾矿浆的沉降絮凝性能,结果表明：阴离子型聚丙烯酰胺产品显现出优异的絮凝性能,在用量20g/t时,沉降速度、固液分离及上清液澄清度均取得良好效果。
In this paper, non-ionic polyacrylamide and cationic polyacrylamide with high molecular weight were synthesized by the means of Inverse Emulsion Polymerization, anionic polyacrylamide emulsion was synthesized by the means of hydrolization of non-ionic polyacrylamide with alkali added in later process.
The optimum conditions of preparing non-ionic polyacrylamide using Inverse Emulsion Polymerization was that:reaction temperature 45℃, reaction time 4h, amount of initiator 0.2‰, amount of emulsifier 6%, HLB=6, mass fraction of monomer 40%, the mass ratio of oil to water 1.0:1.0,EDTA-2Na 1.0‰. Unde this condition, the obtained polymer with high molecular weight 1100×104 showed good reproducibility.
The above-mentioned emulsion was hydrolyzed at optimum hydrolysis conditions:the hydrolysis agent NaOH, theoretical degree of hydrolization 30%, temperature 60℃, time two hours. Under this condition, Partially hydrolyzed polyacrylamide latex was obtained with DH 24.5% and molecular weight over 660x 104.
Cationic polyacrylamide P(DMC-AM) was synthesized with acrylamide(AM) and methacrylatoethyl trimethyl ammonium chloride(DMC) as co-monomers by Inverse Emulsion Polymerization in this paper,the optimal conditions were as follows:amount of initiator 1.4%o, amount of emulsifier 6%, HLB=6, mass fraction of monomer 40%, EDTA-2Na 1.0‰, the molar ratio of DMC to AM 5:95, the mass ratio of oil to water 1.1:1.0, pH=5, reaction temperature 50℃and reaction time 4h. Under above conditions, the molecular weight of the product was 580×104. Through Fourier transform infrared spectrum (FT-IR) measurement, the product was proved to cationic copolymer P(DMC-AM).
The flocculation behavior of bauxite forward flotation tailings aqueous system was investigated by the sedimentation test, the experimental result revealed that the flocculation effect of anionic polyacrylamide flocculant was better than nonionic and cationic polyacrylamide, the sedimentation rate was higher,the liquid-solid separating effect was distinct and the up liquid was clear at the best dosage 20g/t.
反相乳液聚合制备非离子型聚丙烯酰胺的最佳工艺条件为：反应温度为45℃,反应时间为4h,引发剂V-50用量为0.2‰,乳化剂用量为6%,HLB=6,单体浓度为40%,油水比为1.0：1.0,EDTA-2Na用量为0.5‰。聚合工艺条件具有良好的重现性,得到聚合产物相对分子质量高达1100万,通过FT-IR和DSC-TGA对产物结构和热稳定性进行了表征,证明聚合物为AM均聚产物,并且具有良好的热稳定性。
以上述乳液产品为水解原料,以NaOH为水解剂,理论水解度为30%,水解温度为60℃,水解时间为2h的条件下,得到实际水解度为24.5%,相对分子质量660万的部分水解聚丙烯酰胺乳液产品。
以丙烯酰胺(AM)和甲基丙烯酰氧乙基三甲基氯化铵(DMC)为共聚单体,通过反相乳液聚合制备高分子阳离子共聚物P(DMC-AM)的最佳工艺条件为：引发剂V-50用量为1.4‰、乳化剂用量为6%、EDTA-2Na用量为1.0‰、亲水亲油平衡值为6、单体浓度为40%、单体配比为n(DMC):n(AM)=5:95、油水质量比为1.1:1.0、pH值为5、反应温度为50℃及反应时间为4h,在上述条件下,所得产物的相对分子质量可达580万。通过FT-IR对产物结构进行了表征,证实了制备的聚合物为目标产物。
考察了上述乳液絮凝剂对铝土矿正浮选尾矿浆的沉降絮凝性能,结果表明：阴离子型聚丙烯酰胺产品显现出优异的絮凝性能,在用量20g/t时,沉降速度、固液分离及上清液澄清度均取得良好效果。
In this paper, non-ionic polyacrylamide and cationic polyacrylamide with high molecular weight were synthesized by the means of Inverse Emulsion Polymerization, anionic polyacrylamide emulsion was synthesized by the means of hydrolization of non-ionic polyacrylamide with alkali added in later process.
The optimum conditions of preparing non-ionic polyacrylamide using Inverse Emulsion Polymerization was that:reaction temperature 45℃, reaction time 4h, amount of initiator 0.2‰, amount of emulsifier 6%, HLB=6, mass fraction of monomer 40%, the mass ratio of oil to water 1.0:1.0,EDTA-2Na 1.0‰. Unde this condition, the obtained polymer with high molecular weight 1100×104 showed good reproducibility.
The above-mentioned emulsion was hydrolyzed at optimum hydrolysis conditions:the hydrolysis agent NaOH, theoretical degree of hydrolization 30%, temperature 60℃, time two hours. Under this condition, Partially hydrolyzed polyacrylamide latex was obtained with DH 24.5% and molecular weight over 660x 104.
Cationic polyacrylamide P(DMC-AM) was synthesized with acrylamide(AM) and methacrylatoethyl trimethyl ammonium chloride(DMC) as co-monomers by Inverse Emulsion Polymerization in this paper,the optimal conditions were as follows:amount of initiator 1.4%o, amount of emulsifier 6%, HLB=6, mass fraction of monomer 40%, EDTA-2Na 1.0‰, the molar ratio of DMC to AM 5:95, the mass ratio of oil to water 1.1:1.0, pH=5, reaction temperature 50℃and reaction time 4h. Under above conditions, the molecular weight of the product was 580×104. Through Fourier transform infrared spectrum (FT-IR) measurement, the product was proved to cationic copolymer P(DMC-AM).
The flocculation behavior of bauxite forward flotation tailings aqueous system was investigated by the sedimentation test, the experimental result revealed that the flocculation effect of anionic polyacrylamide flocculant was better than nonionic and cationic polyacrylamide, the sedimentation rate was higher,the liquid-solid separating effect was distinct and the up liquid was clear at the best dosage 20g/t.
引文
[1]方道斌,郭睿威,哈润华,等.丙烯酰胺聚合物.北京：化学工业出版社,2006.13-14
[2]刘庆普.聚丙烯酰胺及其衍生物的应用[J].石油化工,1991,20(5)：345-351
[3]李富生,胡星琪,段明,等.聚丙烯酞胺的合成技术及应用研究[J].应用化工2002,31(5)：1-4
[4]王雨华.高分子量阴离子型聚丙烯酰胺的制备[J].石油化工高等学校学报,1994,7(4)：25—29
[5]申迎华,王孟,王志忠.两性聚丙烯酞胺的合成方法及应用进展[J].化工进展,2003,22(10)：1061-1065
[6]吕生华,俞从正,章川波,等.阳离子高分子絮凝剂的制备与应用[J].西北轻工业学院学报.2000,18(4)：18-22
[7]蔡开勇,王久芬,杜栓丽,等.引发体系对聚丙烯酰胺相对分子质量的影响[J].华北工学院学报,1999,20(1)：83-87
[8]王贵江,欧阳坚,朱桌岩,等.超高相对分子质量聚丙烯酰胺的研究[J].精细化工,2003,20(5)：303-306
[9]卢红霞,刘福胜,于世涛.丙烯酰胺-DMC的水溶液共聚反应[J].青岛科技大学学报,2006,27(5)：392-395
[10]Biswajit Ray,Broja M M. Dispersion polymerization of acrylamide[J]. Langmuir, 1997,13(8):2191-2196
[11]韩磊,宁荣昌,谢钢,等.分散聚合法制备聚丙烯酰胺水包水乳液[J].功能高分子学报,2004,3(17)：493-495
[12]李强.分散聚合制备聚丙烯酰胺水包水乳液：[硕士学位论文].四川：西南石油大学,2006
[13]郭睿威,赵宗峰,金启明.AM／阳离子单体在盐水介质中的分散聚合[J].化学工业与工程,2007,24(2)：129-133
[14]潘祖仁.悬浮聚合[M].北京：化学工业出版社,1997
[15]刘海峰,薛屏.反相悬浮聚合技术的研究进展与应用[J].应用化工2005,34(8)：460-463.
[16]Vanderhoff J W. The use of high-energy irradiation in an investigation of the mechanism and kinetics of emulsion polymerization[J]. Adv Chem Ser,1962,50(154):265-286
[17]胡金生,曹同玉,刘庆普.乳液聚合[M].北京：化工出版社,1987.60-73
[18]刘戈.AM/AA反相乳液聚合研究：[博士学位论文].杭州：浙江大学,1997
[19]官建国,何平,谢洪泉.丙烯酸反相乳液聚合的研究[J].化学研究,1994,23(8)：23-25
[20]Hoar T P,Schulman J H. Transparent water-in-oil dispersions:the oleopathic hydro-micelle[J]. Nature,1943(152):102-103
[21]Wan Jiang,Wu Li Yang,Xianbao Zeng,et al. Structure and Properties of Poly(methyl methacrylate)Particles Prepared by a Modified Microemulsion [J].Polymerization Journal of polymer science:Part A:Polymer chemistry,2004(42):733-741
[22]Debuigne F,Jeunieau L,Wiame M,et al. Synthesis of organie nanoparticles in different W/O microemulsions[J]. Langmuir,2000,16(20):7605-7611
[23]Wei M,Frank N J,Fu S K. Synthesis of nanosize ploy(methyl methacrylate) microlatexes with high polymer content by a modifled microemulsion polymerization[J]. Polymer Bulltin,1998,40(6):749-756
[24]Candau F,L eong Y S,Pouyet G,et al. Inverse Microemulsion Polymerizat ion of Acrylamide:Characterization of the Water in Oil Microemulsion and the Final Microlatexes [J]. J Colloid Interface Sci,1984,101(1):167-183
[25]Vaskovs V, Juranicovs V, Barton J. Polymerization in inverse microemulsion IV:1 Locus of initiation by ammonium peroxodisulfate and 2,2-azoisobutyronitril[J]. Macromolecule Chemistry and physics,1992,193(3):627-637
[26]哈润华,侯斯健.(2-甲基丙烯酰氧乙基)三甲基氯化铵-丙烯酰胺反相微乳液共聚合研究[J].高等学校化学学报,1993,14(8)：1163-1166
[27]张志成,徐相凌,张曼维.过硫酸铵引发丙烯酰胺微乳液聚合[J].高分子学报,1995(1)：23—27
[28]Snuparek J,Cermak V. Inverse Emulsion Polymerization of Acryamide and Salts of Acrylic Acid[J]. Eur. Polym J,1997,33(8):1345-1352
[29]巩冠群,尹家贵,张英杰.反相乳液聚合法制备丙烯酰胺-三氧乙基三甲基氯化铵共聚物絮凝剂[J].精细石油化工,2001(2)：16-18
[30]李东,杨静秋.ROOH-Na2S2O5体系反相乳液聚合法制备高分子量PAM[J].山东化工,1995(1)：27—28
[31]Hernandez B J,Hunkeler D. Inverse-emulsion Polymerization of Acrylamide using Block Copolymeric Surfactants:Mechanism Kinetics and Moldelling[J]. Polymer,1997,38(2):437-447
[32]Kurenkov V F,et al. Peculiarities of the preparation of copolymers of acrylamide with sodium acrylate in inverse emulsions[J]. Eur.Polym,1984,20(4):357-360
[33]王振卫,石家华,等.AM/SAMPS反相乳液聚合产物的表征[J].化学研究,2001,12(2)：21-23
[34]周春华,刘威.高分子量速溶型聚丙烯酰胺的合成[J].山东建材学院学报,1998,12(3)：262-264
[35]Roger E. Neff,Roderick G. Ryles,Milford. Water-soluble highly branchen polymeric micropangicles[P].US 5354481,1994
[36]Xuewu Ge,Qiang Ye. et al. Radiation Copolymerization of Acrylamide and Cationic Monomer in an Inverse Emulsion[J]. J. Appl. polym. Sci.,1998,39 (10):1917-1920
[37]Fu Chen,Edward J. Connors. Self Inverting water in oil emlsions[P].US 5006596,1991
[38]易昌凤,程时远,李小琴,等.丙烯酰胺/DBMA反相乳液共聚乳液粒子形态及大小的研究[J].胶体与聚合物,1999(1)：17-20
[39]赵勇,陈晓晖,等.(AM/AA/DADMAC)共聚物堵水剂的反相乳液法制备研究[J].精细化工,1997,14(6)：35-37
[40]林浩,高建村,地木拉提.丙烯酰胺系反相乳液聚合研究进展[J].新疆石油学院学报,2001,13(1)：58-60
[41]黄鹏程.二甲基二烯丙基氯化钱反相乳液聚合动力学及机理的研究[J].化学学报,1996,54(3)：209-213
[42]高青雨,王振卫.AM/SAMPS反相乳液聚合动力学[J].石油化工,2000,29(11)：841—844
[43]Benda D,Snuparek J. Inverse emulsion polymerization of acrylamide and sailts of acrylic acid[J]. European Polymer Journal,1997,33(8):1345-1352
[44]Kallon K Ghosh, Lallan Kjumar Tiwary. Influence of sodium Bis(2-Ethyl-1-Hexyl)suflosuccinate/Isooctane/Water Microemul-sions on the Hydrolysis is of salicylhydroxamic Acid [M]. Journal of molecular liquids,2003,102(1-3):183-195
[45]刘莲英,孟晶,杨万泰.丙烯酰胺／氧化-还原引发体系的反相乳液聚合[J].北京化工大学学报,2002,29(02)：59-62
[46]胡金生,哈润华,顾汉卿.丙烯酰胺的反相乳液聚合[J].高分子材料科学与工程,1985(01)：34-42
[47]杨重愚.轻金属冶金学[M].北京：冶金工业出版社,1991
[48]刘广义.一水硬铝石型铝土矿浮选脱硅研究[D].长沙：中南工业大学,1999
[49]杨志民.我国氧化铝生产的综合回收与利用[J].世界有色金属,2002(2)：35-37
[50]陈湘清,胡秋云,陈兴华.一种铝土矿选精矿或尾矿的沉降脱水方法[P].中国发明专利,CN101181701A,2008-05-21
[51]袁明亮,李俊,胡岳华.复杂铝土矿浮选尾矿机械力化学表面改性研究[J].矿山综合利用,2005(2)：3-7
[52]陈志友,陈湘清,马俊伟.铝土矿选矿尾矿性质及沉降性能研究[J].轻金属,2007(2)：7-10
[53]张去非.絮凝剂的种类及其在尾矿沉降中的应用[J].金属矿山,2008(6)：69-72
[54]秦丽娟.有机高分子絮凝剂的研究进展及发展趋势[J].上海造纸,2004,35(1)：41-46
[55]马青山,贾瑟,孙丽氓.絮凝化学和絮凝剂(M).北京：中国环境科学出版社,1988
[56]Hahn H.H., Stumm W. Kinetics of coagulation with hydrolyzed aluminum[J]. Journal of Colloid and Interface Science,1968,28(2):133-142
[57]常青.水处理絮凝学[M].北京：化学工业出版社,2003
[58]Hahn H H,Stumm W. Kinetics of coagulation with hydrolyzed Al(Ⅲ):the rate determining step[J].Journal of Colloid and Interface Science,1968,28(1):134-144
[59]曹同玉,刘庆普,胡金生.聚合物乳液合成原理、性能及应用[M].北京：化工出版社,1997
[60]中华人民共和国国家技术监督局.GB17514—1998.中华人民共和国国家标准-水处理剂聚丙烯酰胺.北京：中国标准出版社,1999-04-01
[61]惠泉,刘福胜,于世涛,等.丙烯酰胺-甲基丙烯酰氧乙基三甲基氯化铵反相乳液聚合的工艺条件[J].精细石油化工,2008,25(2)：58—62
[62]中华人民共和国国家技术监督局.GB12005.6-89.中华人民共和国国家标准-部分水解聚丙烯酰胺水解度测定方法.北京：中国标准出版社,1990-04-01
[63]蒋巍.二甲基二烯丙基氯化铵-丙烯酰胺反相乳液聚合制备阳离子絮凝剂[J].化工科技市场,2008,31(1)：19-21
[64]张万忠,乔学亮,李绵贵.水溶性偶氮引发剂用于氯化二甲基二烯丙基铵的聚合[J].应用化学,2004,21(5)：483-487
[65]高华星,骆维刚,程树军,等.用新型水溶性偶氮引发剂引发二甲基二烯丙基氯化铵的聚合反应[J].功能高分子学报,1995,18(3)：249—258
[66]张贞浴,张凤莲.超高分子量聚丙烯酰胺的合成研究[J].化学工程师,1995(6)：4—6
[67]吴强,李晨曦,李学臣,等.红外光谱法热分析液晶相变过程[J].高等学校化学学报,2001,22(12)：2123—2125
[68]周平华,许乾慰.热分析在高分子材料中的应用[J].上海塑料,2004(1)：36-40
[69]高庆,陈正国,路国红.可交联AA/AM反相乳液聚合的稳定性研究[J].湖北大学学报,2001,923(3)：255-257
[70]徐克强,田慕川.丙烯酸-丙烯酰胺的反相乳液聚合[J].北京化纤工学院学报,1985(2)：45-51
[71]牛志刚,刘济威,白明,等.反相乳液聚合法制备丙烯酰胺-丙烯酸钠二元共聚物[J].内蒙古石油化工,2008(7)：21—23
[72]鞠耐霜,曾文江.阳离子型聚丙烯酰胺合成与絮凝特性研究[J].广州化工,2000,28(1)：65-68.
[73]吕生华,俞从正,章川波,等.阳离子高分子絮凝剂的制备与应用[J].西北轻工业学院学报,2000,18(3)：18-21.
[74]惠泉,刘福胜,于丽明,等.阳离子聚丙烯酰胺合成工艺研究进展[J].化工生产与技术,2007,14(5)：31-34
[75]刘焦萍,黄春成.铝土矿正浮选尾矿浆沉降新工艺研究[J].轻金属,2006(5)：8-13
[2]刘庆普.聚丙烯酰胺及其衍生物的应用[J].石油化工,1991,20(5)：345-351
[3]李富生,胡星琪,段明,等.聚丙烯酞胺的合成技术及应用研究[J].应用化工2002,31(5)：1-4
[4]王雨华.高分子量阴离子型聚丙烯酰胺的制备[J].石油化工高等学校学报,1994,7(4)：25—29
[5]申迎华,王孟,王志忠.两性聚丙烯酞胺的合成方法及应用进展[J].化工进展,2003,22(10)：1061-1065
[6]吕生华,俞从正,章川波,等.阳离子高分子絮凝剂的制备与应用[J].西北轻工业学院学报.2000,18(4)：18-22
[7]蔡开勇,王久芬,杜栓丽,等.引发体系对聚丙烯酰胺相对分子质量的影响[J].华北工学院学报,1999,20(1)：83-87
[8]王贵江,欧阳坚,朱桌岩,等.超高相对分子质量聚丙烯酰胺的研究[J].精细化工,2003,20(5)：303-306
[9]卢红霞,刘福胜,于世涛.丙烯酰胺-DMC的水溶液共聚反应[J].青岛科技大学学报,2006,27(5)：392-395
[10]Biswajit Ray,Broja M M. Dispersion polymerization of acrylamide[J]. Langmuir, 1997,13(8):2191-2196
[11]韩磊,宁荣昌,谢钢,等.分散聚合法制备聚丙烯酰胺水包水乳液[J].功能高分子学报,2004,3(17)：493-495
[12]李强.分散聚合制备聚丙烯酰胺水包水乳液：[硕士学位论文].四川：西南石油大学,2006
[13]郭睿威,赵宗峰,金启明.AM／阳离子单体在盐水介质中的分散聚合[J].化学工业与工程,2007,24(2)：129-133
[14]潘祖仁.悬浮聚合[M].北京：化学工业出版社,1997
[15]刘海峰,薛屏.反相悬浮聚合技术的研究进展与应用[J].应用化工2005,34(8)：460-463.
[16]Vanderhoff J W. The use of high-energy irradiation in an investigation of the mechanism and kinetics of emulsion polymerization[J]. Adv Chem Ser,1962,50(154):265-286
[17]胡金生,曹同玉,刘庆普.乳液聚合[M].北京：化工出版社,1987.60-73
[18]刘戈.AM/AA反相乳液聚合研究：[博士学位论文].杭州：浙江大学,1997
[19]官建国,何平,谢洪泉.丙烯酸反相乳液聚合的研究[J].化学研究,1994,23(8)：23-25
[20]Hoar T P,Schulman J H. Transparent water-in-oil dispersions:the oleopathic hydro-micelle[J]. Nature,1943(152):102-103
[21]Wan Jiang,Wu Li Yang,Xianbao Zeng,et al. Structure and Properties of Poly(methyl methacrylate)Particles Prepared by a Modified Microemulsion [J].Polymerization Journal of polymer science:Part A:Polymer chemistry,2004(42):733-741
[22]Debuigne F,Jeunieau L,Wiame M,et al. Synthesis of organie nanoparticles in different W/O microemulsions[J]. Langmuir,2000,16(20):7605-7611
[23]Wei M,Frank N J,Fu S K. Synthesis of nanosize ploy(methyl methacrylate) microlatexes with high polymer content by a modifled microemulsion polymerization[J]. Polymer Bulltin,1998,40(6):749-756
[24]Candau F,L eong Y S,Pouyet G,et al. Inverse Microemulsion Polymerizat ion of Acrylamide:Characterization of the Water in Oil Microemulsion and the Final Microlatexes [J]. J Colloid Interface Sci,1984,101(1):167-183
[25]Vaskovs V, Juranicovs V, Barton J. Polymerization in inverse microemulsion IV:1 Locus of initiation by ammonium peroxodisulfate and 2,2-azoisobutyronitril[J]. Macromolecule Chemistry and physics,1992,193(3):627-637
[26]哈润华,侯斯健.(2-甲基丙烯酰氧乙基)三甲基氯化铵-丙烯酰胺反相微乳液共聚合研究[J].高等学校化学学报,1993,14(8)：1163-1166
[27]张志成,徐相凌,张曼维.过硫酸铵引发丙烯酰胺微乳液聚合[J].高分子学报,1995(1)：23—27
[28]Snuparek J,Cermak V. Inverse Emulsion Polymerization of Acryamide and Salts of Acrylic Acid[J]. Eur. Polym J,1997,33(8):1345-1352
[29]巩冠群,尹家贵,张英杰.反相乳液聚合法制备丙烯酰胺-三氧乙基三甲基氯化铵共聚物絮凝剂[J].精细石油化工,2001(2)：16-18
[30]李东,杨静秋.ROOH-Na2S2O5体系反相乳液聚合法制备高分子量PAM[J].山东化工,1995(1)：27—28
[31]Hernandez B J,Hunkeler D. Inverse-emulsion Polymerization of Acrylamide using Block Copolymeric Surfactants:Mechanism Kinetics and Moldelling[J]. Polymer,1997,38(2):437-447
[32]Kurenkov V F,et al. Peculiarities of the preparation of copolymers of acrylamide with sodium acrylate in inverse emulsions[J]. Eur.Polym,1984,20(4):357-360
[33]王振卫,石家华,等.AM/SAMPS反相乳液聚合产物的表征[J].化学研究,2001,12(2)：21-23
[34]周春华,刘威.高分子量速溶型聚丙烯酰胺的合成[J].山东建材学院学报,1998,12(3)：262-264
[35]Roger E. Neff,Roderick G. Ryles,Milford. Water-soluble highly branchen polymeric micropangicles[P].US 5354481,1994
[36]Xuewu Ge,Qiang Ye. et al. Radiation Copolymerization of Acrylamide and Cationic Monomer in an Inverse Emulsion[J]. J. Appl. polym. Sci.,1998,39 (10):1917-1920
[37]Fu Chen,Edward J. Connors. Self Inverting water in oil emlsions[P].US 5006596,1991
[38]易昌凤,程时远,李小琴,等.丙烯酰胺/DBMA反相乳液共聚乳液粒子形态及大小的研究[J].胶体与聚合物,1999(1)：17-20
[39]赵勇,陈晓晖,等.(AM/AA/DADMAC)共聚物堵水剂的反相乳液法制备研究[J].精细化工,1997,14(6)：35-37
[40]林浩,高建村,地木拉提.丙烯酰胺系反相乳液聚合研究进展[J].新疆石油学院学报,2001,13(1)：58-60
[41]黄鹏程.二甲基二烯丙基氯化钱反相乳液聚合动力学及机理的研究[J].化学学报,1996,54(3)：209-213
[42]高青雨,王振卫.AM/SAMPS反相乳液聚合动力学[J].石油化工,2000,29(11)：841—844
[43]Benda D,Snuparek J. Inverse emulsion polymerization of acrylamide and sailts of acrylic acid[J]. European Polymer Journal,1997,33(8):1345-1352
[44]Kallon K Ghosh, Lallan Kjumar Tiwary. Influence of sodium Bis(2-Ethyl-1-Hexyl)suflosuccinate/Isooctane/Water Microemul-sions on the Hydrolysis is of salicylhydroxamic Acid [M]. Journal of molecular liquids,2003,102(1-3):183-195
[45]刘莲英,孟晶,杨万泰.丙烯酰胺／氧化-还原引发体系的反相乳液聚合[J].北京化工大学学报,2002,29(02)：59-62
[46]胡金生,哈润华,顾汉卿.丙烯酰胺的反相乳液聚合[J].高分子材料科学与工程,1985(01)：34-42
[47]杨重愚.轻金属冶金学[M].北京：冶金工业出版社,1991
[48]刘广义.一水硬铝石型铝土矿浮选脱硅研究[D].长沙：中南工业大学,1999
[49]杨志民.我国氧化铝生产的综合回收与利用[J].世界有色金属,2002(2)：35-37
[50]陈湘清,胡秋云,陈兴华.一种铝土矿选精矿或尾矿的沉降脱水方法[P].中国发明专利,CN101181701A,2008-05-21
[51]袁明亮,李俊,胡岳华.复杂铝土矿浮选尾矿机械力化学表面改性研究[J].矿山综合利用,2005(2)：3-7
[52]陈志友,陈湘清,马俊伟.铝土矿选矿尾矿性质及沉降性能研究[J].轻金属,2007(2)：7-10
[53]张去非.絮凝剂的种类及其在尾矿沉降中的应用[J].金属矿山,2008(6)：69-72
[54]秦丽娟.有机高分子絮凝剂的研究进展及发展趋势[J].上海造纸,2004,35(1)：41-46
[55]马青山,贾瑟,孙丽氓.絮凝化学和絮凝剂(M).北京：中国环境科学出版社,1988
[56]Hahn H.H., Stumm W. Kinetics of coagulation with hydrolyzed aluminum[J]. Journal of Colloid and Interface Science,1968,28(2):133-142
[57]常青.水处理絮凝学[M].北京：化学工业出版社,2003
[58]Hahn H H,Stumm W. Kinetics of coagulation with hydrolyzed Al(Ⅲ):the rate determining step[J].Journal of Colloid and Interface Science,1968,28(1):134-144
[59]曹同玉,刘庆普,胡金生.聚合物乳液合成原理、性能及应用[M].北京：化工出版社,1997
[60]中华人民共和国国家技术监督局.GB17514—1998.中华人民共和国国家标准-水处理剂聚丙烯酰胺.北京：中国标准出版社,1999-04-01
[61]惠泉,刘福胜,于世涛,等.丙烯酰胺-甲基丙烯酰氧乙基三甲基氯化铵反相乳液聚合的工艺条件[J].精细石油化工,2008,25(2)：58—62
[62]中华人民共和国国家技术监督局.GB12005.6-89.中华人民共和国国家标准-部分水解聚丙烯酰胺水解度测定方法.北京：中国标准出版社,1990-04-01
[63]蒋巍.二甲基二烯丙基氯化铵-丙烯酰胺反相乳液聚合制备阳离子絮凝剂[J].化工科技市场,2008,31(1)：19-21
[64]张万忠,乔学亮,李绵贵.水溶性偶氮引发剂用于氯化二甲基二烯丙基铵的聚合[J].应用化学,2004,21(5)：483-487
[65]高华星,骆维刚,程树军,等.用新型水溶性偶氮引发剂引发二甲基二烯丙基氯化铵的聚合反应[J].功能高分子学报,1995,18(3)：249—258
[66]张贞浴,张凤莲.超高分子量聚丙烯酰胺的合成研究[J].化学工程师,1995(6)：4—6
[67]吴强,李晨曦,李学臣,等.红外光谱法热分析液晶相变过程[J].高等学校化学学报,2001,22(12)：2123—2125
[68]周平华,许乾慰.热分析在高分子材料中的应用[J].上海塑料,2004(1)：36-40
[69]高庆,陈正国,路国红.可交联AA/AM反相乳液聚合的稳定性研究[J].湖北大学学报,2001,923(3)：255-257
[70]徐克强,田慕川.丙烯酸-丙烯酰胺的反相乳液聚合[J].北京化纤工学院学报,1985(2)：45-51
[71]牛志刚,刘济威,白明,等.反相乳液聚合法制备丙烯酰胺-丙烯酸钠二元共聚物[J].内蒙古石油化工,2008(7)：21—23
[72]鞠耐霜,曾文江.阳离子型聚丙烯酰胺合成与絮凝特性研究[J].广州化工,2000,28(1)：65-68.
[73]吕生华,俞从正,章川波,等.阳离子高分子絮凝剂的制备与应用[J].西北轻工业学院学报,2000,18(3)：18-21.
[74]惠泉,刘福胜,于丽明,等.阳离子聚丙烯酰胺合成工艺研究进展[J].化工生产与技术,2007,14(5)：31-34
[75]刘焦萍,黄春成.铝土矿正浮选尾矿浆沉降新工艺研究[J].轻金属,2006(5)：8-13