CN105315984A - 一种用于抗高温水基压裂液的聚合物交联剂及其生产方法 - Google Patents
一种用于抗高温水基压裂液的聚合物交联剂及其生产方法 Download PDFInfo
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Abstract
一种用于抗高温水基压裂液的聚合物交联剂，该聚合物交联剂适用于180～200℃储层的压裂施工。合成方案为：在三颈烧瓶中，加入丙酮水溶液(体积比：丙酮∶水＝7∶3)，氮气保护和一定温度下，往烧瓶中投加设计比例的氯氧化锆(TiOCl2)、四氯化钛(TiCl4)、马来酸(MA)、乙酰丙酮(AAT)、异丁醇(IPA)(各单体摩尔比为：n(ZrOCl2)∶n(TiCl4)∶n(MA)∶n(AAT)∶n(IPA)＝1.20∶0.800∶0.220∶0.180∶0.440)，30～40min加完，搅拌反应1.0h；升高温度至60℃，继续搅拌恒温回流反应3h；用旋转蒸发仪蒸去丙酮溶剂，得到交联剂。
Description
技术领域
本发明涉及油田化学及压裂增产技术领域，特别涉及一种用于抗高温水基压裂液的聚合物交联剂及其生产方法，该聚合物交联剂适用于180～200℃储层的压裂施工。
背景技术
有机钛的特点是水解快、交联快，低温下有足够的交联能力，但交联压裂液的抗温、抗剪切性相对较差。有机锆的特点是水解慢、交联慢，在高温下其水解速度加快，可以弥补有机钛因温度而部分失去的交联作用，从而提高压裂液体系的抗温抗、剪切能力，其缺点是在低温下交联较慢，影响压裂液体系的悬砂性。其主要原因是交联剂中心原子的结构不同。有机钛、锆交联剂一般是中心离子与有机配体形成的络合物，其性质由中心离子的原子结构和有机配体的络合能力决定。中心原子Ti、Zr属于同族元素，外层电子构型分布为3d24s2、4d25s2，其失去4个电子的离子(Ti4+、Zr4+)的电子构型分别3d°4s°、4d°5s°，共有6个空轨道可以接纳孤对电子形成配位键，即只能形成六配位体化合物，但实际上Ti4+、Zr4+的羟桥化合物形成的是8配位体化合物，说明Ti4+、Zr4+的外层其他空轨道也参加接纳电子形成配位键。根据能量规则，只能是外层邻近的p轨道，即可以形成配位键的轨道有，3d°4s°4p°、4d°5s°5p°，但从能级差来看，Ti4+离子的4s和4p轨道能级差大于Zr4+的5s和5p轨道，因此，Ti4+形成的配位键弱于Zr4+形成的配位键，配位键的离解可能性是Ti4+＞Zr4+，即其抗温性Zr4+＞Ti4+。在高温压裂液的交联中，既需要在地面低温下有较快的交联速度，以便携砂，又需要交联剂在高温下有较强的交联性(即配位键稳定性)，以满足高温下的悬砂能力。Ti4+离子半径小、电性相对较强、能级差较大、水解较快，能和-SO3-、-COO-等酸根负离子快速形成配位键；Zr4+离子半径大、电性相对较弱、能级差小，也能和-SO3-、-COO-等酸根负离子形成配位键，但形成速度较慢；而在高温时，其形成速度会大大提高，同时其配位键稳定性高，表现出较好的高温交联性。
发明内容
压裂液中的携砂液是压裂液施工的关键工作液，在配制压裂携砂液作业中，要求压裂液基液粘度不能太高，以确保混砂能顺利进行；同时要求在混砂后要有较高的粘度，以满足压裂液的悬砂要求。压裂液基液是高分子聚合物溶液，本身具有较高的粘度，使地面混砂作业中产生混砂不均、下砂受阻等问题，交联后的压裂液粘度更高，甚至使混砂作业无法进行。因此，工程上压裂液基液要在混砂作业完成后的一定时间内交联。对于高温压裂液，要求交联剂既要在混砂阶段交联速度较慢；混砂后在输送管线及低温井筒内有较快交联速度；在高温下有较强的交联能力。
无机高价钛、锆等金属离子能通过与-CONH2、-COO-、-SO3-等的络合作用交联高分子，但其交联速度较快，如果直接使用无机钛、锆配制压裂液，将严重影响混砂作业。为解决地面混砂问题，通常是将其预先形成有机络合物，这种络合物具有一定的稳定性，但也可以在较慢的速度下与-CONH2、-COO-、-SO3-等基团较好而交联高分子，因此，设计出交联剂有机络合物适当的稳定性是研究的关键。
交联剂有机络合物的稳定性受与其作用的有机配体的络合能力、结构等有关，考虑到高温压裂液的工程普通要求和抗高温的特殊要求，本项目研究设计的交联剂为钛、锆复合交联剂。其中有机钛交联剂满足低温阶段的交联要求，有机锆满足高温下的交联要求。可以通过选择不同配位能力的配位剂种类、加量以调整有机交联剂的络合物稳定性，来控制交联剂与压裂液配位体的交换速度，从而控制交联速度。为了方便生产和使用，本研究采用“一锅煮法”进行交联剂的制备。根据文献资料和理论分析，可供选择的络合剂有：三乙醇胺、异丙醇、葡萄糖酸、乳酸、丁二酸、马来酸、乙酰丙酮等。考虑到本项目研究的为高温压裂液，为满足抗温性能要求，必须选择有较强络合能力的配体以控制增稠剂基团与其交换而交联增稠剂的速度。配位剂的选择主要从提供孤对电子能力和形成络合物结构的稳定性考虑。选择进行试验的配位剂单体是三乙醇胺、异丙醇、马来酸、乙酰丙酮，其中三乙醇胺、异丙醇主要靠羟基氧原子提供孤对电子，配位能力较弱，以满足低温交联要求；马来酸、乙酰丙酮，主要依靠羧基氧负离子、酰基酮上的氧原子提供配位键，其配位能力强，同时可以形成钳形螯合物，提高交联剂的稳定性，以满足高温交联要求。其理想结构如图1。本研究合成的交联剂的交联时间应控制在2～10min内。
附图说明
下面结合实施例及实施例附图对本发明做进一步的说明，但不作为本发明的限定：
图1是Ti4+、Zr4+正常配位理想结构；
图2是采用实施例中合成交联剂(编号JL-01-08)的红外谱图；
图3是采用实施例中合成交联剂(编号JL-01-08)的质子核磁共振谱；
图4是采用实施例中合成交联剂(编号JL-01-08)的x衍射图谱。
具体实施方式
下面将根据具体的实施例对本发明的交联剂及其生产过程做详细的说明。
在三颈烧瓶中，加入丙酮水水溶液(体积比：丙酮∶水＝7∶3)和设计比例的络合剂；氮气保护和0℃的冰水浴下，往烧瓶中滴加四氯化锆和(或)四氯化锆的丙酮溶液，30～40min加完，搅拌反应1.0h；升温至60℃；继续搅拌恒温回流反应3h；用旋转蒸发仪蒸去丙酮溶剂，得到不同交联剂，见表1。交联剂性能试验结果如表2、表3。
表1交联剂合成单体种类及配比表
注：表中“-”表示未加该种物质。
表2交联剂合成单体种类及配比实验性能测试数据表
表3交联剂合成单体种类及配比实验综合评分表
通过考察交联剂中各种物质比例，确定了其之间的最佳比例；考察了交联剂的合成条件，确定了最佳合成方案。交联剂的最佳合成方案为：n(ZrOCl2)∶n(TiCl4)∶n(MA)∶n(AAT)∶n(IPA)＝1.20∶0.800∶0.220∶0.180∶0.440；合成条件为初始反应温度为5℃，恒温反应温度为60℃，反应时间为3h。
Claims (8)
1.一种用于抗高温水基压裂液的聚合物交联剂，合成单体为氯氧化锆(TiOCl2)、四氯化钛(TiCl4)、马来酸(MA)、乙酰丙酮(AAT)、异丁醇(IPA)，其摩尔比为：n(ZrOCl2)∶n(TiCl4)∶n(MA)∶n(AAT)∶n(IPA)＝1.20∶0.800∶0.220∶0.180∶0.440。
2.根据权利要求1所述的高温水基压裂液的聚合物交联剂，其合成条件为初始反应温度为5℃，恒温反应温度为60℃，反应时间为3h。
3.根据权利要求1和权利要求2所述的交联剂，采用“一锅煮法”进行交联剂的制备。
4.根据权利要求1-3任一项所述交联剂的方法，其包括如下步骤：
在三颈烧瓶中，加入丙酮水溶液(体积比：丙酮∶水＝7∶3)和设计比例的络合剂；氮气保护和一定温度下，往烧瓶中滴加四氯化钛和氧氯化锆的丙酮溶液，搅拌反应1.0h；升高温度至指定温度，继续搅拌恒温回流反应一定时间；得到交联剂。
5.根据权利要求4所述的方法，其中，对溶液吹氮气以除去水中的溶解氧，然后在氮气的保护下加入四氯化锆和(或)四氯化锆的丙酮溶液，搅拌反应1.0h；升温至60℃；继续搅拌恒温回流反应3h；
6.根据权利要求5所述的方法所得产物，用旋转蒸发仪蒸去丙酮溶剂，得到交联剂。
7.根据权利要求5所述方法，在氮气的保护下加入四氯化锆和(或)四氯化锆的丙酮溶液，应控制投加速度，30～40min加完。
8.根据权利要求1-7所述的方法所得交联剂，运用红外光谱、核磁共振、x衍射等现代分析手段，对交联剂的结构进行了表征，得到了交联剂分子可能的结构如下：
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| CN102417814A (zh) * | 2011-11-16 | 2012-04-18 | 北京国海能源技术研究院 | 海水基压裂液及其制备方法 |
| CN102492413A (zh) * | 2011-12-05 | 2012-06-13 | 北京希涛技术开发有限公司 | 甲醇基压裂液可控交联剂的开发 |
| CN102618249A (zh) * | 2012-03-05 | 2012-08-01 | 中国海洋石油总公司 | 一种海水基压裂液及其制备方法 |
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| CN102417814A (zh) * | 2011-11-16 | 2012-04-18 | 北京国海能源技术研究院 | 海水基压裂液及其制备方法 |
| CN102492413A (zh) * | 2011-12-05 | 2012-06-13 | 北京希涛技术开发有限公司 | 甲醇基压裂液可控交联剂的开发 |
| CN102618249A (zh) * | 2012-03-05 | 2012-08-01 | 中国海洋石油总公司 | 一种海水基压裂液及其制备方法 |
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