Page 202 - 精细化工2019年第9期

第 36 卷第 9 期 精 细 化 工 Vol.36, No.9
201 9 年 9 月 FINE CHEMICALS Sept. 2019

油田化学品与油品添加剂
多氨基硼交联剂的制备与性能评价

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罗攀登 1,2 ，宋志峰 1,2 ，张建贝 ，曹 杰
〔1. 中国石化西北油田分公司 石油工程技术研究院，新疆 乌鲁木齐 830011；2 .中国石化缝洞型油藏提
高采收率重点实验室，新疆 乌鲁木齐 830011；3. 中国石油大学（华东） 石油工程学院，山东 青岛
266580〕

摘要：以多胺化合物和硼酸酯为原料，合成羟丙基胍胶压裂液用有机硼交联剂，通过在交联剂中引入多个含硼
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交联位点，达到降低压裂液体系中羟丙基胍胶的用量、提升压裂液体系耐温性能的目的。采用 FTIR、 HNMR
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和 BNMR 对不同交联剂的结构进行了表征，并分析了反应机理。考察了多胺化合物的种类（二乙烯三胺、四
乙烯五胺、多乙烯多胺、聚乙烯亚胺-600）、反应物的配比、反应温度和反应时间对产物交联性能的影响，结果
表明，当硼酸酯与多乙烯多胺的质量比为 3∶2、反应时间为 4 h、反应温度为 150 ℃时，可以制备性能最优的
交联剂 BNX-1。评价了 BNX-1 配制压裂液的耐温耐剪切性能、破胶性能和静态滤失性能。结果表明，以羟丙基
胍胶质量分数 0.35%、羟丙基胍胶溶液与 BNX-1 交联质量比 100∶0.4 配制的压裂液体系，在 140 ℃、170 s –1
下剪切，120 min 后黏度为 122 mPa·s；以工业交联剂 TCB-1 作为对照（以羟丙基胍胶质量分数为 0.5%、羟丙基
胍胶溶液与 TCB-1 交联质量比为 100∶0.5 配制的压裂液体系），在同等条件下剪切，黏度为 98 mPa·s。
关键词：交联剂；多乙烯多胺；压裂液；热稳定性；油田化学品
中图分类号：TE357.12 文献标识码：A 文章编号：1003-5214 (2019) 09-1930-06

Preparation and Property Evaluation of Polyamine Boron Crosslinker

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LUO Pan-deng , SONG Zhi-feng , ZHANG Jian-bei , CAO Jie
〔1. Research Institute of Petroleum Engineering, SINOPEC Northwest Oilfield Branch, Urumqi 830011, Xinjiang, China;
2. Key Laboratory of EOR for Carbonate Fractured-Vuggy Reservoirs, SINOPEC, Urumqi 830011, Xinjiang, China; 3. School
of Petroleum Engineering, China University of Petroleum (East China), Qingdao 266580, Shandong, China〕
Abstract: Organic boron crosslinkers for hydroxypropylguar gum fracturing fluid were synthesized from
polyamine compound and borate ester. The amount of hydroxypropyl guar gum used in fracturing fluid was
reduced and the heat resistance of fracturing fluid was also enhanced due to several boron-based
crosslinking sites in this crosslinker. The structures of different crosslinkers were characterized by FTIR,
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1 HNMR and BNMR, and the reaction mechanism was discussed. The influences of polyamine compound
types (diethylenetriamine, 1,4,7,10,13-pentaazatridecane, polyethylene-polyamines and polyethylenimine-
600), mass ratio between two raw chemicals, reaction temperature and time on the properties of fracturing
fluid were studied.The results showed that when the mass ratio of borate ester to polyethylene polyamine
was 3∶2, reaction time was 4 h, reaction temperature was 150 ℃, the prepared product BNX-1 had the
best performance. The heat and shear resistance, gel-breaking performance and static fluid-loss performance
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of BNX-1 based fracturing fluid were studied. After being sheared at a shear rate of 170 s for 120 min
under 140 ℃, the viscosity of the fracturing fluid (hydroxypropyl guar gum mass fraction 0.35%, mass
ratio of hydroxypropylguar gum solution to BNX-1 100∶0.4) was up to 122 mPa·s. However, that of
industrial crosslinker (TCB-1) based system (hydroxypropyl guar gum 0.5%, mass ratio of hydroxypropyl
guanidine gum solution to TCB-1 100∶0.5) was 98 mPa·s under the same measurement conditions.
Key words: crosslinking agent; polyethyene polyamine; fracturing fluid; thermal stability; oil field
chemicals

收稿日期：2019-04-02; 定用日期：2019-07-09; DOI: 10.13550/j.jxhg.20190266
基金项目：国家科技重大专项（2016ZX05053-004）
作者简介：罗攀登（1985—），男，工程师，硕士。联系人：曹 杰（1983—），男，讲师， E-mail：jcao@upc.edu.cn。