CN112439395A - 一种用于分析检测油井采出液中聚表剂的液相色谱柱的制备方法 - Google Patents
一种用于分析检测油井采出液中聚表剂的液相色谱柱的制备方法 Download PDFInfo
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Abstract
本发明提供了一种用于分析检测油井采出液中聚表剂的液相色谱柱的制备，是将多孔硅胶微球置于浓盐酸中活化后，加入到柠檬酸和聚乙烯醇溶于去离子水形成的前驱体溶液中混合搅拌，再加入多聚磷酸作为催化剂，使其在硅胶表面发生聚合反应，制得柠檬酸‑聚乙烯醇交联/SiO2微球；重复聚合过程，制得交联聚柠檬酸乙烯酯/SiO2微球；使用乙醇对此复合微球进行浮选，得到色谱填料，最后采用气泵将色谱填料填装进内径为4.6 mm、长度为30 mm的色谱管中，得到色谱柱。该色谱柱在特定色谱条件下，能够实现油井采出液中聚表剂和聚合物、无机盐等干扰物的有效分离，进而实现聚表剂的单独分析检测。
Description
技术领域
本发明涉及一种油井采出液中聚表剂分析检测用液相色谱柱及其制备方法，应用于油井采出液中聚表剂的液相色谱分析检测，属于高效液相色谱分析领域。
背景技术
聚表剂是近年来在聚合物驱、三元复合驱基础上研制形成的一种新型驱油剂，近年来已成为提高采收率的研究热点。由于很多油井采出液中同时含有聚表剂和普通聚合物，传统的“淀粉-碘化镉法”和“紫外分光光度法”只是针对聚合物中的酰胺基团进行检测，得到的是聚合物的总量，无法区分聚表剂和普通聚合物各自的含量。因此采用传统检测方法，由于普通聚合物的干扰，既无法了解各油井采出液中是否含有聚表剂，也不能根据采出液中聚表剂浓度适时调整开采方案。如何实现油井采出液中聚表剂单独分析检测，一直是油田近10年有待解决的问题。
高效液相色谱法是色谱法的一个重要分支，以液体为流动相，采用高压输液系统，将具有不同极性的单一溶剂或不同比例的混合溶剂、缓冲液等流动相泵入装有色谱填料的色谱柱，在柱内各成分被分离后，进入检测器进行检测，从而实现对试样的分析。借助高效液相色谱技术，可以首先采用色谱柱将普通聚合物和聚表剂进行分离，然后再对聚表剂进行单独检测。但是目前市场上并没有专门针对聚表剂和普通聚合物分离的商品化色谱柱，因此研制专门针对油井采出液中聚表剂分析检测用的色谱柱，实现油井采出液中聚表剂单独分析检测，具有非常重要的现实应用意义。
发明内容
本发明的目的是提供一种用于分析检测油井采出液中聚表剂的液相色谱柱及其制备方法。
本发明液相色谱柱的制备方法，包括以下步骤：
（1）硅胶表面活化：将粒径为4-5μm，比表面积为250-300 m2/g的多孔硅胶在浓盐酸浸泡40-48 h，水洗至中性，120℃-140℃条件下真空干燥12-18 h，得到表面活化硅胶；
（2）前驱体溶液制备：将柠檬酸、聚乙烯醇、去离子水按照1:（2~3）:（30~40）的体积比混合均匀制得前驱体溶液；
（3）表面聚合：将活化硅胶按3~5g/100mL的比例加入到前驱体溶液中混合搅拌，再加入多聚磷酸作为催化剂，于100-120℃下反应10-15 h，制得柠檬酸-聚乙烯醇交联/SiO2微球；重复表面聚合过程3-4次，制得交联聚柠檬酸乙烯酯/SiO2微球；
多聚磷酸的加入量为活化硅胶质量的0.05-0.1倍；多聚磷酸化学式为Hn+2PnO3n+1，无色透明黏稠状液体，具有腐蚀性。多聚磷酸为质子酸，能溶解多种低分子及高分子有机化合物。在有机合成中用作失水剂、环化剂、酰化剂，是缩合、环化、重排、取代等反应的催化剂或溶剂；
（4）微球浮选：将交联聚柠檬酸乙烯酯/SiO2微球以3-5g/100 mL分散于乙醇中浮选3-4h，反复浮选5-6次，最后对浮选得到的微球在80℃-100℃下真空干燥80-10 h，得到色谱填料；
（5）色谱柱填装：以水为匀浆液，以丙酮为顶替液，采用气泵在40Mpa气压下将色谱填料填装进内径为4.6 mm、长度为30 mm的色谱管中，得到色谱柱。
图1为填料的透射电镜图。图2为填料的扫描电镜图。从透射电镜上可以看到硅胶表面被包裹上了一层均匀的聚合物薄层，从扫描电镜上可以看到相对于裸硅胶，表面变粗糙度减小，变得更加平滑。色谱填料的元素分析显示，C含量为15.43%。所有这些表征均证实填料的成功合成。
本发明制备的填料具有丰富的羧基和羟基等极性基团，表现出很强的亲水色谱的性能，由于聚表兼具聚合物和表面活性剂的双重特性，比普通聚合物具有更强的亲水性，所以在本填料所填装的色谱柱上具有更强的保留时间，在特定的流动相条件下，能够实现油井采出液中聚表剂和聚合物、无机盐等干扰物的有效分离，进而实现聚表剂的单独分析检测。
附图说明
图1为填料的透射电镜图。
图2为填料的扫描电镜图。
图3为不同流动相条件下油井采出液的色谱分离图。
具体实施方式
下面通过体实施例对本发明一种油井采出液中聚表剂分析检测用液相色谱柱及其制备方法的应用做具体说明。
实施例1、一种油井采出液中聚表剂分析检测用液相色谱柱的制备
（1）硅胶表面活化：将粒径为5 μm，比表面积为300 m2/g的多孔硅胶在浓盐酸浸泡48h，水洗至中性，真空120℃条件下干燥12h，得到表面活化硅胶；
（2）前驱体溶液制备：将柠檬酸、聚乙烯醇、去离子水按照1:3:40体积比混合均匀制得前驱体溶液；
（3）表面聚合：将4g活化硅胶加入到100 mL前驱体溶液中混合搅拌，再加入0.4g多聚磷酸作为催化剂，于110℃下反应12 h，制得柠檬酸-聚乙烯醇交联/SiO2微球，重复表面聚合过程4次，制得交联聚柠檬酸乙烯酯/SiO2微球；
（4）微球浮选：将3 g交联聚柠檬酸乙烯酯/SiO2微球分散于100 mL乙醇中浮选4 h，反复浮选6次，最后对所得到的微球真空90℃干燥10 h得到色谱填料；
（5）色谱柱填装：以水为匀浆液，以丙酮为顶替液，采用高压气泵在40Mpa气压下将色谱填料填装进内径为4.6 mm、长度为30 mm的色谱管中，得到色谱柱。
实施例2、色谱柱分离油井采出液中聚表剂
色谱分析条件：流动相：水/乙腈混合溶液；流速：1.0 mL/min；紫外检测器 200 nm，柱温度：25 ℃；进样量：20 µL。
图3为不同流动相条件下油井采出液的色谱分离图。其中，1为普通聚合物色谱峰，2为无机盐色谱峰，3为聚表剂色谱峰。从图3可以看出随着流动相中水相比例的增加，聚表剂色谱峰和普通聚合物色谱峰、无机盐色谱峰等干扰物的分离度越来越大，当水相含量增大到99%时，聚表剂色谱峰已经完全和聚合物、无机盐分离开来，最终采用水：乙腈=99:1为检测流动相，可以实现油井采出液中聚表剂的分析检测。
Claims (6)
1.一种用于分析检测油井采出液中聚表剂的液相色谱柱的制备方法，包括以下步骤：
（1）硅胶表面活化：将多孔硅胶在浓盐酸浸泡活化40-48 h，水洗至中性， 120℃-140℃条件下真空干燥12-18 h，得到表面活化硅胶；
（2）前驱体溶液制备：将柠檬酸、聚乙烯醇、去离子水混合均匀，制得前驱体溶液；
（3）表面聚合：将活化硅胶加入到前驱体溶液中混合搅拌，再加入多聚磷酸作为催化剂，于100-120℃下反应10-15 h，制得柠檬酸-聚乙烯醇交联/SiO2微球；重复表面聚合过程3-4次，制得交联聚柠檬酸乙烯酯/SiO2微球；
（4）微球浮选：将交联聚柠檬酸乙烯酯/SiO2微球分散于乙醇中浮选3-4 h，反复浮选5-6次，最后对浮选得到的微球在80℃-100℃下真空干燥80-10 h，得到色谱填料；
（5）色谱柱填装：以水为匀浆液，以丙酮为顶替液，采用气泵在40Mpa气压下将色谱填料填装进内径为4.6 mm、长度为30 mm的色谱管中，得到色谱柱。
2.如权利要求1所述一种用于分析检测油井采出液中聚表剂的液相色谱柱的制备方法，其特征在于：步骤（1）中，多孔硅胶的粒径为4-5μm，比表面积为250-300 m2/g。
3.如权利要求1所述一种用于分析检测油井采出液中聚表剂的液相色谱柱的制备方法，其特征在于：步骤（2）中，柠檬酸、聚乙烯醇、去离子水按照1:（2~3）:（30~40）的体积比混合。
4.如权利要求1所述一种用于分析检测油井采出液中聚表剂的液相色谱柱的制备方法，其特征在于：步骤（3）中，活化硅胶按3~5g/100mL的比例加入到前驱体溶液中。
5.如权利要求1所述一种用于分析检测油井采出液中聚表剂的液相色谱柱的制备方法，其特征在于：步骤（3）中，多聚磷酸的加入量为活化硅胶质量的0.05-0.1倍。
6.如权利要求1所述一种用于分析检测油井采出液中聚表剂的液相色谱柱的制备方法，其特征在于：步骤（4）中，交联聚柠檬酸乙烯酯/SiO2微球以3-5g/100 mL分散于乙醇中。
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