CN102382242A - 一种两亲高分子及其用途 - Google Patents

一种两亲高分子及其用途 Download PDF

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CN102382242A
CN102382242A CN2011102103193A CN201110210319A CN102382242A CN 102382242 A CN102382242 A CN 102382242A CN 2011102103193 A CN2011102103193 A CN 2011102103193A CN 201110210319 A CN201110210319 A CN 201110210319A CN 102382242 A CN102382242 A CN 102382242A
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formula
amphiphilic macromolecule
amphiphilic
structural unit
macromolecule
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CN102382242B (zh
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王金本
徐晓慧
史学峰
韩玉淳
王毅琳
闫海科
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Institute of Chemistry CAS
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Institute of Chemistry CAS
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Priority to MYPI2014700161A priority patent/MY166452A/en
Priority to PCT/CN2011/001576 priority patent/WO2013013354A1/zh
Priority to EP11869894.3A priority patent/EP2738189B1/en
Priority to EA201490338A priority patent/EA025931B1/ru
Priority to DK11869894.3T priority patent/DK2738189T3/en
Priority to US14/235,016 priority patent/US9738741B2/en
Priority to ES11869894.3T priority patent/ES2630738T3/es
Priority to CA2842783A priority patent/CA2842783C/en
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Abstract

本发明提供了一种两亲高分子及该高分子的用途。该两亲高分子具有重复结构单元：调节分子量与分子量分布以及荷电特性作用的结构单元、高空间位阻结构单元和两亲结构单元，适用于油田钻井、固井、压裂、原油集输、污水处理、污泥处理和造纸等领域，可用作强化采油驱油剂、稠油降粘剂、压裂液、粘土稳定剂、污水处理剂、造纸用助留助滤剂或补强剂等。

Description

一种两亲高分子及其用途
技术领域
本发明涉及一种两亲高分子及其用途，该两亲高分子适用于油田钻井、固井、压裂、原油集输、污水处理、污泥处理和造纸等领域，可用作强化采油驱油剂、稠油降粘剂、压裂液、粘土稳定剂、污水处理剂、造纸用助留助滤剂或补强剂等。
背景技术
三次采油用聚合物的溶液粘度和粘度稳定性是衡量其使用效果的重要指标。油藏温度、地层水和注入水矿化度的高低，直接影响聚合物溶液的增粘能力。对于部分水解聚丙烯酰胺而言，虽然其在淡水中具有明显的增粘作用，但随着油田温度、地层水或注入水矿化度的增加，聚合物大分子流体力学半径减小，同时聚合物在岩石表面的吸附量增大也使溶液有效浓度降低，导致溶液粘度不断下降。两亲高分子是一类重要的水溶性聚合物，通过在亲水性大分子链上引入少量的疏水基团，产生分子内或分子间疏水相互作用，使大分子在溶液中形成空间网状结构，因而具有显著的增粘效果。通过增加高分子链上疏水基团含量或增大分子量可以在一定程度上抵御高温、高盐度的影响，但也可能导致聚合物溶解能力变差、溶解时间大幅增加以及大分子链容易剪切降解和容易吸附于岩层等问题。随着地层温度和水矿化度的增大，这些问题尤为严重。
稠油资源已经成为我国重要的战略接替资源之一，但开采难度很大，主要原因是稠油的粘度大，胶质、沥青质或含蜡量高，在地层、井筒及输油管线中不易流动，另外由于油水流度比大，还易造成油井见水快、含水率高、地层易出砂等严重影响生产的问题。
如何保持高分子溶液的增粘与稳粘性、提高其乳化和分散稠油、降低稠油粘度的能力，对于提高原油采收率以及最大限度挖潜地下残余原油具有重要意义。
发明内容
本发明以下内容中，除另有定义外，相同的可变基团、分子式/结构式等均具有相同的定义。
本发明涉及一种两亲高分子，所述两亲高分子具有如下所述的重复单元：起调节分子量、分子量分布以及荷电特性作用的结构单元A、高空间位阻结构单元B和两亲结构单元C。
在一个实施例中，所述调节分子量、分子量分布以及荷电特性作用的结构单元A包括(甲基)丙烯酰胺类单体单元A1和/或(甲基)丙烯酸类单体单元A2；优选同时包括(甲基)丙烯酰胺类单体单元A1和(甲基)丙烯酸类单体单元A2。在本领域中，两亲高分子的分子量通常可根据需要进行选择，使用比较多的是100-2000万之间。
优选的，所述(甲基)丙烯酰胺类单体单元A1具有如下式(1)所示的结构：
Figure BDA0000078609940000021
式(1)
式(1)中，R1为H或甲基；R2和R3各自独立的选自H、C1-C3的烷基；R2和R3优选为H。
优选的，所述(甲基)丙烯酸类单体单元A2为(甲基)丙烯酸和/或(甲基)丙烯酸盐；甲基丙烯酸盐优选为甲基丙烯酸钠。
优选的，所述(甲基)丙烯酰胺类单体单元A1在整个两亲高分子所有重复单元中所占的摩尔百分数为70-99mol％，优选为70-90mol％，更优选70-78mol％。
优选的，所述(甲基)丙烯酸类单体单元A2在整个两亲高分子所有重复单元中所占的摩尔百分数为1-30mol％，优选1-28mol％，更优选20-28mol％。
在另一个实施例中，所述起调节分子量、分子量分布以及荷电特性作用的结构单元A具有如下式(2)所示的结构：
Figure BDA0000078609940000022
式(2)
其中，R1为H或甲基；R2和R3各自独立的选自H、C1-C3的烷基；R2和R3优选为H；R4选自H或甲基；Gr为-OH或-O-Na+；m和n表示该结构单元在整个两亲高分子所有重复单元中所占的摩尔百分数；m为70-99mol％，优选为70-90mol％，更优选70-78mol％；n为1-30mol％，优选1-28mol％，更优选20-28mol％。
在另一个实施例中，式(2)中R1-R3优选为H，Gr优选为-O-Na+。
在另一个实施例中，所述高空间位阻结构单元B至少含有结构G，所述结构G为以主链相邻两个碳原子为基础形成的环状烃结构或选自式(3)表示的结构，结构单元B中任选的含有式(4)所示的结构：
Figure BDA0000078609940000031
式(3)式(4)
式(3)中，R5为H或甲基；优选为H；R6选自如下式(5)-(6)所示的基团：
Figure BDA0000078609940000032
式(5)式(6)
式(5)中，a为1-11的整数；优选为1-7；
式(4)中，R7为H；R8选自H、-SO3H及其盐、-(CH2)2CH3Cl、-CH2N+(CH3)2(CH2)ξCH3Cl-或-CH2N+(CH3)2(CH2)2N+(CH3)2(CH2)σCH32Cl-；ξ、σ分别为1-15的整数，优选1-11。
优选的，所述高空间位阻结构单元B含有结构G和式(4)所示的结构。
在另一个实施例中，所述以主链相邻两个碳原子为基础形成的环状烃结构选自：
Figure BDA0000078609940000033
优选的，上述高空间位阻结构单元B中结构G在整个两亲高分子所有重复单元中所占的摩尔百分数为0.02-2mol％，优选0.02-1.0mol％，更优选为0.1-0.5mol％。
优选的，上述高空间位阻结构单元B中式(4)所示的结构在整个两亲高分子所有重复单元中所占的摩尔百分数为0.05-5mol％，优选为0.1-2.5mol％，更优选为0.1-1.5mol％。
在另一个实施例中，所述高空间位阻结构单元B具有式(7)所示的结构：
Figure BDA0000078609940000041
式(7)
式(7)中，G的定义如上所述，优选为式(3)所表示的结构、
Figure BDA0000078609940000043
R7和R8的定义如式(4)所述；x和y分别表示该结构单元在整个两亲高分子所有重复单元中所占的摩尔百分数；x为0.02-2mol％，优选0.02-1.0mol％，更优选为0.1-0.5mol％；y为0.05-5mol％，优选为0.1-2.5mol％，更优选为0.1-1.5mol％。
在另一个实施例中，所述两亲结构单元C具有式(8)所示的结构：
Figure BDA0000078609940000044
式(8)
式(8)中，R9为H或甲基，R10为-N+(CH3)2(CH2)rCH3X-、-N+((CH2)sCH3)3X-或-N+(CH3)((CH2)tCH3)2X-；r为3-21的整数，s为2-9的整数，t为3-15的整数，X-为Cl-或Br-。优选地，r为3-17，s为2-5，t为3-11。
优选的，上述两亲结构单元C在整个两亲高分子所有重复单元中所占的摩尔百分数为0.05-10mol％，优选0.1-5.0mol％，更优选0.5-1.5mol％。
在另一个实施例中，所述两亲高分子具有式(9)所示的结构：
Figure BDA0000078609940000051
式(9)
式(9)中，R4，m，n的定义如式(2)所述；R7，R8，G，x，y的定义如式(7)所述；R9，R10的定义如式(8)所述，z表示该结构单元在整个两亲高分子所有重复单元中所占的摩尔百分数，z为0.05-10mol％，优选0.1-5.0mol％，更优选0.5-1.5mol％。
本发明具体提供了如下式(I)-(X)所示的高分子化合物：
Figure BDA0000078609940000052
Figure BDA0000078609940000061
Figure BDA0000078609940000071
Figure BDA0000078609940000081
本发明上述两亲高分子的分子量为100万-2000万之间；优选为300万-1100万之间。
分子量M的测定方法：使用乌氏粘度计测定特性粘数[η]，并将测得的[η]代入下面公式中计算得到；
M＝802[η]1.25
本发明所述两亲高分子可采用本技术领域所已知的方法制备，例如：通过起调节分子量、分子量分布以及荷电特性作用的结构单元单体、高空间位阻结构单元单体和两亲结构单元单体在引发剂作用下聚合而成；聚合反应可以为悬浮聚合、乳液聚合、溶液聚合、沉淀聚合等本领域熟知的聚合方法。
典型的制备方法为：在水体系中通过搅拌的方式分散或溶解上述各单体，在氮气保护下引发聚合形成两亲性高分子。现有技术中制备两亲高分子的相关技术均可用于本发明的两亲高分子的制备。
制备两亲高分子所采用的单体均可直接商购获得，或依据现有技术直接制备得到，一些单体的合成路线在具体实施例中有详细说明。
本发明的两亲高分子的用途，其用于油田钻井、固井、压裂、原油集输、污水处理、污泥处理和造纸，或用作强化采油驱油剂、稠油降粘剂、压裂液、粘土稳定剂、污水处理剂、造纸用助留助滤剂或补强剂等。
特别适用于原油开采领域，如可用作强化采油聚合物驱油剂和稠油降粘剂。作为驱油剂使用时，溶液在高温高盐条件下仍具有显著增粘效果，能够提高原油采收率。作为稠油降粘剂时，通过有效分散和乳化稠油，显著降低稠油粘度、减小稠油在地层和井筒中流动阻力。
附图说明
图1本发明实施例1-实施例5制得的两亲高分子在1×104mg/L矿化度盐水中60℃下的粘浓关系曲线。
图2本发明实施例1-实施例5制得的两亲高分子在1×104mg/矿化度盐水中浓度为1750mg/L时的粘温关系曲线。
具体实施方式
下面结合具体实施例对本发明作进一步说明，但本发明并不限于以下实施例。
实施例1
本实施例合成的两亲高分子如式(I)所示：
Figure BDA0000078609940000101
本实施例的亲高分子的合成：
先将占总反应体系重量3/4的水加入反应釜中，再将占总反应体系重量1/4的各种单体加入反应釜，各重复单元的摩尔百分数m、n、x、y、z依次为78％、20％、0.25％、0.5％、1.25％，搅拌使它们完全溶解，并向其中加入pH值调节剂调节反应溶液，使其pH为8左右，通氮气30min除去其中的氧气。在氮气保护下加入引发剂，再通氮气10min后封口，在18℃下反应，反应约5h反应结束，反应完全。所得产品经过干燥，得到粉末状两亲高分子.两亲高分子的分子量970×104。
实施例2
本实施例合成的两亲高分子如式(II)所示：
Figure BDA0000078609940000102
单体
Figure BDA0000078609940000103
的合成路线如下：
Figure BDA0000078609940000111
本实施例两亲高分子的合成：
先将占总反应体系重量3/4的水加入反应釜中，再将占总反应体系重量1/4的各种单体加入反应釜，各重复单元的摩尔百分数m、n、x、y、z依次为75％、23％、0.25％、0.25％、1.5％，搅拌使它们完全溶解，并向其中加入pH值调节剂调节反应溶液，使其pH为8左右，通氮气40min除去其中的氧气。在氮气保护下加入引发剂，再通氮气10min后封口，在22℃下反应，反应约5h反应结束，反应完全。所得产品经过干燥，得到粉末状两亲高分子。两亲高分子的分子量为1030×104。
实施例3
本实施例合成的两亲高分子如式(III)所示：
单体
Figure BDA0000078609940000113
的合成路线如下：
本实施例两亲高分子的合成：
先将占总反应体系重量3/4的水加入反应釜中，再将占总反应体系重量1/4的各种单体加入反应釜，各重复单元的摩尔百分数m、n、x、y、z依次为73％、26％、0.1％、0.1％、0.8％，搅拌使它们完全溶解，并向其中加入pH值调节剂调节反应溶液，使其pH为9左右，通氮气30min除去其中的氧气。在氮气保护下加入引发剂，再通氮气10min后封口，在25℃下反应，反应约6h反应结束，反应完全。所得产品经过干燥，得到粉末状两亲高分子。两亲高分子的分子量为620×104。
实施例4
本实施例合成的两亲高分子如式(IV)所示：
Figure BDA0000078609940000121
单体
Figure BDA0000078609940000122
的合成路线如下：
Figure BDA0000078609940000131
本实施例两亲高分子的合成：
先将占总反应体系重量3/4的水加入反应釜中，再将占总反应体系重量1/4的各种单体加入反应釜，各重复单元的摩尔百分数m、n、x、y、z依次为75％、23％、0.1％、0.4％、1.5％，搅拌使它们完全溶解，并向其中加入pH值调节剂调节反应溶液，使其pH为9左右，通氮气30min除去其中的氧气。在氮气保护下加入引发剂，再通氮气10min后封口，在25℃下反应，反应约6h反应结束，反应完全。所得产品经过干燥，得到粉末状两亲高分子。两亲高分子的分子量为390×104。
实施例5
本实施例合成的两亲高分子如式(V)所示：
Figure BDA0000078609940000141
单体的合成路线如下：
Figure BDA0000078609940000143
本实施例两亲高分子的合成：
先将占总反应体系重量3/4的水加入反应釜中，再将占总反应体系重量1/4的各种单体加入反应釜，各重复单元的摩尔百分数m、n、x、y、z依次为78％、21％、0.1％、0.1％、0.8％，搅拌使它们完全溶解，并向其中加入pH值调节剂调节反应溶液，使其pH为8左右，通氮气30min除去其中的氧气。在氮气保护下加入引发剂，再通氮气10min后封口，在25℃下反应，反应约6h反应结束，反应完全。所得产品经过干燥，得到粉末状两亲高分子。两亲高分子的分子量为390×104。
实施例6
本实施例合成的两亲高分子如式(VI)所示：
Figure BDA0000078609940000151
本实施例两亲高分子的合成：
先将占总反应体系重量3/4的水加入反应釜中，再将占总反应体系重量1/4的各种单体加入反应釜，各重复单元的摩尔百分数m、n、x、y、z依次为73.5％、25％、0.5％、0.5％、0.5％，搅拌使它们完全溶解，并向其中加入pH值调节剂调节反应溶液，使其pH为8左右，通氮气30min除去其中的氧气。在氮气保护下加入引发剂，再通氮气10min后封口，在45℃下反应，反应约3h反应结束，反应完全。所得产品经过干燥，得到粉末状两亲高分子。两亲高分子的分子量为680×104。
实施例7
本实施例合成的两亲高分子如式(VII)所示：
Figure BDA0000078609940000152
本实施例两亲高分子的合成：
先将占总反应体系重量3/4的水加入反应釜中，再将占总反应体系重量1/4的各种单体加入反应釜，各重复单元的摩尔百分数m、n、x、y、z依次为75％、23％、0.25％、0.25％、1.5％，搅拌使它们完全溶解，并向其中加入pH值调节剂调节反应溶液，使其pH为9左右，通氮气30min除去其中的氧气。在氮气保护下加入引发剂，再通氮气10min后封口，在55℃下反应，反应约3h反应结束，反应完全。所得产品经过干燥，得到粉末状两亲高分子。两亲高分子的分子量为690×104。
实施例8
本实施例合成的两亲高分子如式(VIII)所示：
Figure BDA0000078609940000161
本实施例两亲高分子的合成：
先将占总反应体系重量3/4的水加入反应釜中，再将占总反应体系重量1/4的各种单体加入反应釜，各重复单元的摩尔百分数m、n、x、y、z依次为70％、28％、0.15％、0.75％、1.1％，搅拌使它们完全溶解，并向其中加入pH值调节剂调节反应溶液，使其pH为8左右，通氮气30min除去其中的氧气。在氮气保护下加入引发剂，再通氮气10min后封口，在55℃下反应，反应约3h反应结束，反应完全。所得产品经过干燥，得到粉末状两亲高分子。两亲高分子的分子量为390×104。
实施例9
本实施例合成的两亲高分子如式(IX)所示：
Figure BDA0000078609940000171
本实施例两亲高分子的合成：
先将占总反应体系重量3/4的水加入反应釜中，再将占总反应体系重量1/4的各种单体加入反应釜，各重复单元的摩尔百分数m、n、x、y、z依次为75％、23.5％、0.5％、0.5％、0.5％，搅拌使它们完全溶解，并向其中加入pH值调节剂调节反应溶液，使其pH为8左右，通氮气30min除去其中的氧气。在氮气保护下加入引发剂，再通氮气10min后封口，在50℃下反应，反应约2.5h反应结束，反应完全。所得产品经过干燥，得到粉末状两亲高分子。两亲高分子的分子量为430×104。
实施例10
本实施例合成的两亲高分子如式(X)所示：
Figure BDA0000078609940000172
本实施例两亲高分子的合成：
先将占总反应体系重量3/4的水加入反应釜中，再将占总反应体系重量1/4的各种单体加入反应釜，各重复单元的摩尔百分数m、n、x、y、z依次为74％、23％、0.5％、1.5％、1％，搅拌使它们完全溶解，并向其中加入pH值调节剂调节反应溶液，使其pH为8左右，通氮气30min除去其中的氧气。在氮气保护下加入引发剂，再通氮气10min后封口，在50℃下反应，反应约2h反应结束，反应完全。所得产品经过干燥，得到粉末状两亲高分子。两亲高分子的分子量为560×104。
测定实施例
测定例1
使用矿化度1×104mg/L的盐水配制不同浓度的两亲高分子溶液，测定溶液浓度、温度与溶液粘度的关系，结果见图1和图2。
图中表明，在高温和高矿化度条件下，实施例1-5的两亲高分子溶液仍具有良好的增粘能力。两亲高分子中的高空间位阻单元减小了主链内旋转自由度、增加了大分子链的刚性，使大分子链难于蜷曲而趋向伸展，导致大分子流体力学半径增大，同时，两亲结构单元通过分子内或分子间作用形成缔合微区，显著提高了高温高盐条件下的溶液增粘能力。
测定例2
测试方法：温度为25℃下，将三种油田电脱原油样品25ml加入50ml具塞试管中，继续加入25ml以蒸馏水配制的不同浓度两亲高分子的水溶液，盖紧试管塞后，采用手工方式振荡或将试管放置在振荡箱内，水平振荡80-100次，振幅应大于20cm，充分混合后，松动试管塞。原油降粘率按照下式计算：
表1实施例6-实施例10制得的两亲高分子稠油降粘实验结果(油水比1∶1，25℃)
Figure BDA0000078609940000182
Figure BDA0000078609940000191
表1说明，实施例6-10的两亲高分子对于三种油样具有很好的降粘效果。随两亲高分子溶液浓度增加，降粘率增大。溶液浓度相同时，油样粘度提高则相应降粘率增大。两亲高分子通过高空间位阻单元与两亲结构单元的协同作用，有效乳化、分散原油，显著降低了原油粘度。

Claims (12)

1.一种两亲高分子，其特征在于：具有调节分子量与分子量分布以及荷电特性作用的结构单元A、高空间位阻结构单元B和两亲结构单元C作为重复结构单元。所述高空间位阻结构单元B含有结构G和式(4)所示的结构，其中所述结构G为以主链相邻两个碳原子为基础形成的环状烃结构或选自式(3)表示的结构：
Figure FDA0000078609930000011
式(3)    式(4)
式(3)中，R5为H或甲基；优选为H；R6选自如下式(5)-(6)所示的基团：
Figure FDA0000078609930000012
式(5)    式(6)
式(5)中，a为1-11的整数。
式(4)中，R7为H；R8选自H、-SO3H及其盐、-(CH2)2CH3Cl、-CH2N+(CH3)2(CH2)ξCH3Cl-或-CH2N+(CH3)2(CH2)2N+(CH3)2(CH2)σCH32Cl-；ξ、σ分别为1-15的整数。
其中所述两亲结构单元C具有式(8)所示的结构：
Figure FDA0000078609930000013
式(8)
式(8)中，R9为H或甲基，R10为-N+(CH3)2(CH2)rCH3X-、-N+((CH2)sCH3)3X-或-N+(CH3)((CH2)tCH3)2X-；r为3-21的整数，s为2-9的整数，t为3-15的整数，X-为Cl-或Br-。
2.如权利要求1所述的两亲高分子，其特征在于：所述起调节分子量、分子量分布以及荷电特性作用的结构单元A包括(甲基)丙烯酰胺类单体单元A1和/或(甲基)丙烯酸类单体单元A2。
3.如权利要求2所述的两亲高分子，其特征在于：以两亲高分子所有重复单元总数为100mol％计，所述(甲基)丙烯酰胺类单体单元A1在整个两亲高分子所有重复单元中所占的摩尔百分数为70-99mol％；所述(甲基)丙烯酸类单体单元A2在整个两亲高分子所有重复单元中所占的摩尔百分数为1-30mol％。
4.如权利要求1所述的两亲高分子，其特征在于：结构G在整个两亲高分子所有重复单元中所占的摩尔百分数为0.02-2mol％；式(4)所示的结构在整个两亲高分子所有重复单元中所占的摩尔百分数为0.05-5mol％。
5.如权利要求1所述的两亲高分子，其特征在于：以两亲高分子所有重复单元总数为100mol％计，所述式(8)表示的结构单元在整个两亲高分子所有重复单元中所占的摩尔百分数为0.05-10mol％。
6.如权利要求1所述的两亲高分子，其特征在于：所述调节分子量、分子量分布以及荷电特性作用的结构单元A具有如下式(2)所示的结构：
Figure FDA0000078609930000021
式(2)
式(2)中，R1为H或甲基；R2和R3各自独立的选自H、C1-C3的烷基；R4选自H或甲基；Gr为-OH或-O-Na+；m和n表示该结构单元在整个两亲高分子中所占的摩尔百分数；m为70-99mol％；n为1-30mol％。
7.如权利要求1所述的两亲高分子，其特征在于：所述以主链相邻两个碳原子为基础形成的环状烃结构选自：
Figure FDA0000078609930000031
8.如权利要求1所述的两亲高分子，其特征在于：所述高空间位阻结构单元B具有式(7)所示的结构：
Figure FDA0000078609930000032
式(7)
式(7)中，G的定义如权利要求1所述，R7和R8的定义如式(4)中所述，x和y分别表示该结构单元在整个两亲高分子所有重复单元中所占的摩尔百分数，x为0.02-2mol％，y为0.05-5mol％。
9.如权利要求1所述的两亲高分子，其特征在于：所述两亲高分子具有式(9)所示的结构：
Figure FDA0000078609930000033
式(9)
式(9)中，R4选自H或甲基；m和n表示该结构单元在整个两亲高分子中所占的摩尔百分数；m为70-99mol％；n为1-30mol％；G、R7、R8、x和y的定义如上述式(7)所述；R9，R10的定义如上述式(8)所述，z表示该结构单元在整个两亲高分子所有重复单元中所占的摩尔百分数，z为0.05-10mol％。
10.如权利要求1所述的两亲高分子，所述高分子是下述式(I)-(X)化合物：
Figure FDA0000078609930000041
Figure FDA0000078609930000051
Figure FDA0000078609930000061
11.如权利要求1-10任一项所述的两亲高分子，其特征在于：分子量为100万-2000万之间。
12.权利要求1-11任一项所述的两亲高分子的用途，其特征在于：用于油田钻井、固井、压裂、原油集输、污水处理、污泥处理和造纸，或用作强化采油驱油剂、稠油降粘剂、压裂液、粘土稳定剂、污水处理剂、造纸用助留助滤剂或补强剂。
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