疏水缔合型聚丙烯酰胺的合成与性能及其与离子型表面活性剂的相互作用
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摘要
本文合成了新型芳烷基丙烯酰胺疏水单体，并采用自由基胶束共聚合方法制备新型非离子型(PBAM系列)、离子型(PBAMS)疏水缔合水溶液性共聚物。通过PBAM系列共聚物的聚合反应的研究发现，丙烯酰胺水相聚合反应动力学仍然适用于胶束共聚合过程；在聚合过程中由于胶束的存在，疏水单体在反应初期的嵌入率很高，而后期主要以丙烯酰胺均聚物为主，导致严重的微观结构非均匀性，而这种非均匀性对共聚物的增粘性能有很大的影响；首次采用正交试验多指标综合评价方法考察了AMPS、BAAM、SDS及引发剂的用量对产物增粘性能的影响，得到了同时满足多指标要求的PBAMS共聚物；IR谱图证明所合成的共聚物为目标共聚物；TG测试表明共聚物均具有较好的热稳定性，且PBAMS的热稳定性高于PBAM系列。
疏水单体BAAM的用量对PBAM系列共聚物溶液粘度的影响存在一个最佳值，而对PBAMS溶液粘度的影响较为复杂，过高的用量将使共聚物无法溶解；随AMPS用量的增加，PBAMS去离子水、盐水溶液的粘度均先有所增加，然后基本保持不变。
当共聚物浓度大于临界缔合浓度(C_p~*)后，两种溶液的表观粘度急剧增加，加入NaCl或在分子链中引入离子性基团都将使C_p~*降低：部分PBAM试样与PBAMS的溶液具有盐增稠性质；pH值对PBAMS溶液粘度的影响呈“鞍形”变化；PBAM系列共聚物可在一定温度范围内表现出增稠性质，但高温使得溶液的表观粘度下降，并且升温会引起共聚物增粘性能的降低。
在剪切作用下，共聚物的去离子水溶液表现出剪切稀释性质与触变性，通过Oswald模型拟合证明溶液为假塑性流体，PBAMS共聚物溶液还表现出屈
摘 要
服点特征，并且共聚物浓度越高，假塑性越强，触变性越强，PBAMS溶液的
屈服应力越大：多次剪切使共聚物的增粘性能降低，且粘度的恢复需要一定的
时间；适量NaCI加量的共聚物溶液的增粘性能及触变性均有所增强，共聚物
NaCI溶液在低剪速下具有剪切增稠性能，在较高剪切速率下均呈现假塑性流
体特征；研究发现剪切作用可在一定程度上抵消由盐引起的分子链收缩。
线性粘弹性研究表明，PBAM系列共聚物的去离子水溶液在一定频率之后
表现为以弹性行为主的流体，且共聚物浓度越高，粘弹性特征越明显，松弛时
间越长；较低浓度的PBAMS溶液仅在一定频率之后表现出以弹性为主，而浓
度较高的PBAMS的去离于水溶液及不同PBAMS浓度的NaCI溶液均表现为
以弹性行为主的流体；PBAM与PBAMS共聚物的NaCI溶液的损耗角正切值
均随频率增加逐渐减小，溶液的弹性特征逐步增强。
本文首次以实验证明Fedors方程对疏水缔合共聚物稀溶液适用程度最高，
而Schulz－Blaschke方程中的参数k可以描述体系中分子间的相互作用；随共
聚物浓度的增加，M增加，表现出反聚电解质效应，NaCI的加入对PBAMS
溶液的影响强于对PBAM系列的影响；随着表面活性剂加量的增加，W先下
降，然后上升并在较高表面活性剂浓度时基本保持不变，可利用“拖手”模型
较好的描述稀溶液中共聚物与表面活性剂的相互作用；共聚物稀溶液为牛顿流
体，并且随剪切速率增加，PBAMS溶液的表观粘度有微小增加。
不同表面活性剂对共聚物溶液粘度的影响与共聚物结构、浓度及溶液中微
观缔合形式密切相关。对于 PBAM系列共聚物溶液，随着 SDS、SDBS和 CTAB
加量的增加，PBAM与PBA＊3溶液的表观粘度均出现大幅增加，然后迅速
减小，在较高表面活性剂浓度时基本保持不变；对于PBAM3，表面活性剂的
影响顺序为：＊＊BS＞＊TA B＞＊＊S，而对于＊＊＊MI，三者的影响情况基本一致；
对于阴离于型PBAMS共聚物溶液，CTAB与PBAMS的作用非常明显，表现
为粘度的陡升陡降，并且伴随着白色不溶物质的出现，而SDS、SDBS的加入
对分子间疏水缔合有一定抑制作用。
两种共聚物与SDBS的混合溶液的流变行为随剪切速率增加由牛顿流体转
变为具有屈服点的假塑性流体，在较高S＊BS浓度时又转变为牛顿流体：少量
SDBS的加入体系有利于在溶液中形成强度较高的网络结构，表现出较高的剪
切屈服应力，并且触变性增强；本文发现一定的剪切作用可以使被活性剂胶束
且且
四川大学工学博士学位论文
拆散的网络结构重新恢复，表现为剪切增稠，但过强的剪切作用将仍使粘度下
降；混合体系中的结构经历剪切作用后需要较长的时间才能恢复，PBAMS与
S＊BS混合溶液的粘度具有时间依赖性：适当S＊BS加量的共聚物溶液表现为
以弹性行为主的流体，较低和较高SDBS加量的溶液则在一定频率之后才可表
现出以弹性行为为主的流体。
PBAMI和 PBAMS与 SDS混合去离于水溶液的表面张力随 SDS浓度增加
均出现双转折点，而加入NaCI后，溶液的表面张力曲线仅出现单转折点；随
共聚物浓度的增加，C。逐渐增大；PBAMS用DBS混合溶液的表面张力曲线上
仅出现单转折点；首次研究了温度对混合溶液表面张力的影响，结果表明
PBAMS溶液及其与低浓度SDS混合溶液
In this paper, the novel hydrophobic monomer, arylalkylacrylamide (BAAM), was synthesized. And then the nonionic (PBAM series) and ionic (PBAMS) hydrophobically associating water-soluble copolymers were synthesized by micellar free radical copolymerization method. After the study on the synthesis reaction of PBAM series copolymers, it was found that the polymerization kinetics of acrylamide in water system could still be used in micellar polymerization process, and that the initial incorporation of BAAM into polymer was higher and the acrylamide homopolymerization was dominant at the higher conversion period of monomer, which resulted serious micro-structure heterogeneity of copolymer and had a very important effect to the viscosity properties. It's the first time to
use multi-indexes comprehensive evaluation method of orthogonal test to study the effect of the amount of AMPS, BAAM, SDS and initiator on the viscosity behavior of tripolymers. Then PBAMS copolymer was prepared. Polymer structure was characterized by IR. From the TG analysis, two kinds of polymers have good thermal stability, and that of PBAMS is better than that of PBAM series.
For PBAM series copolymers, there had an optimum amount of BAAM, and the relationship between the amount of BAAM and the viscosity behavior was different to monotone increasing or "saddle shape" variation. The same influence to the solution viscosity of PBAMS was complicated, and higher dosage of BAAM resulted the insolubility of copolymers. With the increasing of the amount of AMPS, the viscosity of both aqueous and NaCl solution of PBAMS was firstly increased
* Sponsored by the Major State Basic Research Project of China (G199022502).
IV
and then kept unchanged.
When polymer concentration was higher than the critical association concentration (CP*), the viscosities of two kinds of copolymers increased abruptly. The addition of NaCl and the copolymerization with ionic monomer (AMPS) would decrease CP*. The solution of PBAMS and certain PBAM samples exhibited salt-thickening behavior. The influence of pH value on the viscosity of PBAMS was "saddle shape" variation. In some low temperature range, the solution of PBAM copolymers exhibited temperature-thickening behavior. However, high temperature would decrease the viscosity, and the temperature-rising process would decrease the viscositying ability of copolymers.
The aqueous solution of two kinds of copolymers exhibited shear-thinning and thixotropy behavior. The Oswald model fitting revealed that the solution of two kinds of copolymer was pseudopalstic, especially the PBAMS solution was characteristic of yield point. The higher the polymer concentration, the stronger the pseudoplastic and the thixotropy behavior, and the higher the yield stress. The viscosity of aqueous polymer solution exhibited obvious time-dependent properties. Several times of shearing would decrease the viscosifying ability of copolymers, and the viscosity restoring needed some time. Appropriate addition of NaCl would increase the viscosifying ability and the thixotropy behavior. The NaCl solution of copolymers exhibited shear-thickening behavior at lower shear rate, and the pseudoplastic behavior under higher shear rate. It was found in this paper that to some extent the shearing could offset the molecular contraction introduced by NaCl.
The linear viscoelastic measurement results showed that for PBAM copolymer solutions the elastic behavior was dominant after certain frequency. The higher the polymer concentration, the stronger the viscoelastic behavior, and the longer the relaxation time of molecular. The elastic behavior was dominant only after certain angular frequency for lower PBAMS concentration solution, but dominant at all test frequency range for higher PBAMS concentration solution. With the increase of frequency, the loss tangent value of copolymer NaCl solution decreased slowly, which meant that the elastic feature of salt solution was stronger gradually.
Furthermore, the PBAMS NaCl solutions were all dominant by e
疏水单体BAAM的用量对PBAM系列共聚物溶液粘度的影响存在一个最佳值，而对PBAMS溶液粘度的影响较为复杂，过高的用量将使共聚物无法溶解；随AMPS用量的增加，PBAMS去离子水、盐水溶液的粘度均先有所增加，然后基本保持不变。
当共聚物浓度大于临界缔合浓度(C_p~*)后，两种溶液的表观粘度急剧增加，加入NaCl或在分子链中引入离子性基团都将使C_p~*降低：部分PBAM试样与PBAMS的溶液具有盐增稠性质；pH值对PBAMS溶液粘度的影响呈“鞍形”变化；PBAM系列共聚物可在一定温度范围内表现出增稠性质，但高温使得溶液的表观粘度下降，并且升温会引起共聚物增粘性能的降低。
在剪切作用下，共聚物的去离子水溶液表现出剪切稀释性质与触变性，通过Oswald模型拟合证明溶液为假塑性流体，PBAMS共聚物溶液还表现出屈
摘 要
服点特征，并且共聚物浓度越高，假塑性越强，触变性越强，PBAMS溶液的
屈服应力越大：多次剪切使共聚物的增粘性能降低，且粘度的恢复需要一定的
时间；适量NaCI加量的共聚物溶液的增粘性能及触变性均有所增强，共聚物
NaCI溶液在低剪速下具有剪切增稠性能，在较高剪切速率下均呈现假塑性流
体特征；研究发现剪切作用可在一定程度上抵消由盐引起的分子链收缩。
线性粘弹性研究表明，PBAM系列共聚物的去离子水溶液在一定频率之后
表现为以弹性行为主的流体，且共聚物浓度越高，粘弹性特征越明显，松弛时
间越长；较低浓度的PBAMS溶液仅在一定频率之后表现出以弹性为主，而浓
度较高的PBAMS的去离于水溶液及不同PBAMS浓度的NaCI溶液均表现为
以弹性行为主的流体；PBAM与PBAMS共聚物的NaCI溶液的损耗角正切值
均随频率增加逐渐减小，溶液的弹性特征逐步增强。
本文首次以实验证明Fedors方程对疏水缔合共聚物稀溶液适用程度最高，
而Schulz－Blaschke方程中的参数k可以描述体系中分子间的相互作用；随共
聚物浓度的增加，M增加，表现出反聚电解质效应，NaCI的加入对PBAMS
溶液的影响强于对PBAM系列的影响；随着表面活性剂加量的增加，W先下
降，然后上升并在较高表面活性剂浓度时基本保持不变，可利用“拖手”模型
较好的描述稀溶液中共聚物与表面活性剂的相互作用；共聚物稀溶液为牛顿流
体，并且随剪切速率增加，PBAMS溶液的表观粘度有微小增加。
不同表面活性剂对共聚物溶液粘度的影响与共聚物结构、浓度及溶液中微
观缔合形式密切相关。对于 PBAM系列共聚物溶液，随着 SDS、SDBS和 CTAB
加量的增加，PBAM与PBA＊3溶液的表观粘度均出现大幅增加，然后迅速
减小，在较高表面活性剂浓度时基本保持不变；对于PBAM3，表面活性剂的
影响顺序为：＊＊BS＞＊TA B＞＊＊S，而对于＊＊＊MI，三者的影响情况基本一致；
对于阴离于型PBAMS共聚物溶液，CTAB与PBAMS的作用非常明显，表现
为粘度的陡升陡降，并且伴随着白色不溶物质的出现，而SDS、SDBS的加入
对分子间疏水缔合有一定抑制作用。
两种共聚物与SDBS的混合溶液的流变行为随剪切速率增加由牛顿流体转
变为具有屈服点的假塑性流体，在较高S＊BS浓度时又转变为牛顿流体：少量
SDBS的加入体系有利于在溶液中形成强度较高的网络结构，表现出较高的剪
切屈服应力，并且触变性增强；本文发现一定的剪切作用可以使被活性剂胶束
且且
四川大学工学博士学位论文
拆散的网络结构重新恢复，表现为剪切增稠，但过强的剪切作用将仍使粘度下
降；混合体系中的结构经历剪切作用后需要较长的时间才能恢复，PBAMS与
S＊BS混合溶液的粘度具有时间依赖性：适当S＊BS加量的共聚物溶液表现为
以弹性行为主的流体，较低和较高SDBS加量的溶液则在一定频率之后才可表
现出以弹性行为为主的流体。
PBAMI和 PBAMS与 SDS混合去离于水溶液的表面张力随 SDS浓度增加
均出现双转折点，而加入NaCI后，溶液的表面张力曲线仅出现单转折点；随
共聚物浓度的增加，C。逐渐增大；PBAMS用DBS混合溶液的表面张力曲线上
仅出现单转折点；首次研究了温度对混合溶液表面张力的影响，结果表明
PBAMS溶液及其与低浓度SDS混合溶液
In this paper, the novel hydrophobic monomer, arylalkylacrylamide (BAAM), was synthesized. And then the nonionic (PBAM series) and ionic (PBAMS) hydrophobically associating water-soluble copolymers were synthesized by micellar free radical copolymerization method. After the study on the synthesis reaction of PBAM series copolymers, it was found that the polymerization kinetics of acrylamide in water system could still be used in micellar polymerization process, and that the initial incorporation of BAAM into polymer was higher and the acrylamide homopolymerization was dominant at the higher conversion period of monomer, which resulted serious micro-structure heterogeneity of copolymer and had a very important effect to the viscosity properties. It's the first time to
use multi-indexes comprehensive evaluation method of orthogonal test to study the effect of the amount of AMPS, BAAM, SDS and initiator on the viscosity behavior of tripolymers. Then PBAMS copolymer was prepared. Polymer structure was characterized by IR. From the TG analysis, two kinds of polymers have good thermal stability, and that of PBAMS is better than that of PBAM series.
For PBAM series copolymers, there had an optimum amount of BAAM, and the relationship between the amount of BAAM and the viscosity behavior was different to monotone increasing or "saddle shape" variation. The same influence to the solution viscosity of PBAMS was complicated, and higher dosage of BAAM resulted the insolubility of copolymers. With the increasing of the amount of AMPS, the viscosity of both aqueous and NaCl solution of PBAMS was firstly increased
* Sponsored by the Major State Basic Research Project of China (G199022502).
IV
and then kept unchanged.
When polymer concentration was higher than the critical association concentration (CP*), the viscosities of two kinds of copolymers increased abruptly. The addition of NaCl and the copolymerization with ionic monomer (AMPS) would decrease CP*. The solution of PBAMS and certain PBAM samples exhibited salt-thickening behavior. The influence of pH value on the viscosity of PBAMS was "saddle shape" variation. In some low temperature range, the solution of PBAM copolymers exhibited temperature-thickening behavior. However, high temperature would decrease the viscosity, and the temperature-rising process would decrease the viscositying ability of copolymers.
The aqueous solution of two kinds of copolymers exhibited shear-thinning and thixotropy behavior. The Oswald model fitting revealed that the solution of two kinds of copolymer was pseudopalstic, especially the PBAMS solution was characteristic of yield point. The higher the polymer concentration, the stronger the pseudoplastic and the thixotropy behavior, and the higher the yield stress. The viscosity of aqueous polymer solution exhibited obvious time-dependent properties. Several times of shearing would decrease the viscosifying ability of copolymers, and the viscosity restoring needed some time. Appropriate addition of NaCl would increase the viscosifying ability and the thixotropy behavior. The NaCl solution of copolymers exhibited shear-thickening behavior at lower shear rate, and the pseudoplastic behavior under higher shear rate. It was found in this paper that to some extent the shearing could offset the molecular contraction introduced by NaCl.
The linear viscoelastic measurement results showed that for PBAM copolymer solutions the elastic behavior was dominant after certain frequency. The higher the polymer concentration, the stronger the viscoelastic behavior, and the longer the relaxation time of molecular. The elastic behavior was dominant only after certain angular frequency for lower PBAMS concentration solution, but dominant at all test frequency range for higher PBAMS concentration solution. With the increase of frequency, the loss tangent value of copolymer NaCl solution decreased slowly, which meant that the elastic feature of salt solution was stronger gradually.
Furthermore, the PBAMS NaCl solutions were all dominant by e
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