CN110423597A - 一种纳米封堵剂改性缩酮及其制备方法和油田钻井液 - Google Patents
一种纳米封堵剂改性缩酮及其制备方法和油田钻井液 Download PDFInfo
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Abstract
本发明公开了一种纳米封堵剂改性缩酮及其制备方法和油田钻井液,该改性缩酮由乙酰乙酸乙酯乙二醇缩酮、氯乙酸钠和氢氧化钠经羟甲基化反应后再经交联剂交联,即可得到纳米级粒径尺寸的纳米封堵剂改性缩酮。制备方法简单,反应过程无需氮气保护,加入各原料反应后所得产物直接冷却即可,无需加热干燥。流动性好,封堵地层微裂缝尤其是纳米级微裂缝效果显著,加入油田钻井液中,可有效改善泥饼,稳定井壁,防止垮塌。
Description
技术领域
本发明涉及油田钻井液材料技术领域,具体涉及一种油田钻井液用纳米封堵剂改性缩酮NAX50及其配制的油田钻井液。
背景技术
面对石油天然气勘探开发过程中日益复杂的地质条件,对井壁的稳定性提出了更高的要求,在钻井过程中,钻井液滤液在压差作用下容易通过微小孔隙进入地层内部,水力压力在微裂缝中的传递作用造成裂缝发展,使得井壁稳定性变差,严重时带来井壁垮塌等钻井事故。所以,需要在钻井液中加入封堵剂,以改善泥饼质量,封堵地层微裂缝,稳定井壁。地层微裂缝的产生,往往是从纳米级微裂缝开始,在水化、压力传递等物理化学因素作用下发展而成的,所以在纳米微裂缝开始产生时进行有效封堵,封堵防塌效果最佳。
目前常规封堵剂多为改性沥青类,包括磺化沥青与乳化沥青,这些沥青类封堵剂粒子粒径多处于微米级及微米级以上,粒径较大难以对纳米级微裂缝进行有效封堵,当初始产生的纳米级微裂缝不能及时封堵时,微裂缝发展长大导致地层强度变差,即使之后有大小匹配的粒子封堵,封堵效果依然很差,不能有效封堵防塌。油田钻井,尤其是页岩气钻井,其初始裂缝多为纳米级(1~100nm),这就要求有纳米级封堵剂封堵微裂缝以保持井壁稳定,为此,我们开发出了一种纳米封堵剂改性缩酮。
发明内容
本发明的目的是提供一种流动性好、封堵地层微裂缝尤其是纳米级微裂缝效果显著的纳米封堵剂改性缩酮。
本发明提供的纳米封堵剂改性缩酮,结构式如下:
本发明还提供了上述纳米封堵剂改性缩酮的制备方法,步骤为:
将乙酰乙酸乙酯乙二醇缩酮溶解于乙醇中,加入氯乙酸钠、氢氧化钠和水,在搅拌状态下加热至90~100℃,反应3~4h后,再加入交联剂继续反应3~4h,即可得到纳米级粒径尺寸的纳米封堵剂改性缩酮。
反应式如下:
第一步,羧甲基化反应,以乙醇为溶剂:
第二步,交联反应:
优选的,上述制备方法中,按重量份数计,各原料用量为:
优选的,上述制备方法中,所述乙酰乙酸乙酯乙二醇缩酮、乙醇、氯乙酸钠、氢氧化钠均为工业优级产品。
优选的,上述制备方法中,所述交联剂为三偏磷酸钠和/或磷酸氢二钠。
优选的,上述制备方法中,所述三偏磷酸钠和/或磷酸氢二钠为工业优级产品。
本发明还提供了一种油田钻井液,含有上述纳米封堵剂改性缩酮。
优选的,上述油田钻井液中,以钻井液的淡水用量为基数,其纳米封堵剂改性缩酮的含量为1wt%~5wt%。
优选的,上述油田钻井液中,配方为:以淡水用量为基数,分别加入0.3%Na2CO3、1.5%Visco1、4%Redu2、3%白沥青、3%聚合醇、50%Weigh2、30%Weigh3和1~5%纳米封堵剂改性缩酮。
与现有技术相比,本发明具有如下有益效果:
本发明的纳米封堵剂改性缩酮流动性好,封堵地层微裂缝尤其是纳米级微裂缝效果显著,加入油田钻井液中,可有效改善泥饼,稳定井壁,防止垮塌。本发明提供的制备方法简单,反应过程无需氮气保护,加入各原料反应后所得产物直接冷却即可,无需加热干燥。
具体实施方式
为了对本发明的技术特征、目的和有益效果有更加清楚的理解,现结合具体实例对本发明的技术方案进行以下详细说明,应理解这些实例仅用于说明本发明而不用于限制本发明的范围。
实施例1
按重量比取30份工业优级无水乙醇加入到反应釜中,在搅拌状态下加入10份工业优级乙酰乙酸乙酯乙二醇缩酮、12份工业优级氯乙酸钠、3份工业优级氢氧化钠、25份水,缓慢升温至90℃,反应3h,之后加入5份磷酸氢二钠,将温度升高至95℃,并保持95℃在搅拌状态下继续反应3小时,冷却,即得到本实施例的纳米封堵剂改性缩酮。
实施例2
按重量比取32份工业优级无水乙醇加入到反应釜中,在搅拌状态下加入18份工业优级乙酰乙酸乙酯乙二醇缩酮、12份工业优级氯乙酸钠、3份工业优级氢氧化钠、30份水,缓慢升温至90℃,反应3h,之后加入5份磷酸氢二钠,将温度升高至95℃,并保持95℃在搅拌状态下继续反应3.5小时,冷却,即得到本实施例的纳米封堵剂改性缩酮。
实施例3
按重量比取32份工业优级无水乙醇加入到反应釜中,在搅拌状态下加入18份工业优级乙酰乙酸乙酯乙二醇缩酮、12份工业优级氯乙酸钠、4份工业优级氢氧化钠、35份水,缓慢升温至90℃,反应3h,之后加入6份磷酸氢二钠,将温度升高至92℃,并保持92℃在搅拌状态下继续反应4小时,冷却,即得到本实施例的纳米封堵剂改性缩酮。
实施例4
按重量比取30份工业优级无水乙醇加入到反应釜中,在搅拌状态下加入20份工业优级乙酰乙酸乙酯乙二醇缩酮、13份工业优级氯乙酸钠、5份工业优级氢氧化钠、30份水,缓慢升温至90℃,反应3h,之后加入10份磷酸氢二钠,将温度升高至100℃,并保持100℃在搅拌状态下继续反应3小时,冷却,即得到本实施例的纳米封堵剂改性缩酮。
将上述各实施例1~4得到的纳米封堵剂改性缩酮按照企业标准Q/HDJPK0035-2017进行各项性能测试,其结果如表1所示。
表1实施例1~4得到的纳米封堵剂改性缩酮性能指标测试数据(常温)
上述实验数据表明,在常温条件下,向钻井液体系中加入本发明制得的钻井液用纳米封堵剂,滤失量大幅下降,说明本发明提供的纳米封堵剂具有填充泥饼孔隙的作用,并形成一层致密膜结构,封堵效果显著。
(1)对钻井液滤失性能的影响评价
配制六份高密度钻井液,以淡水用量作为基数,钻井液配方为:淡水+0.3%Na2CO3+1.5%Visco1+4%Redu2+3%白沥青+3%聚合醇+50%Weigh2+30%Weigh3。其中一份不加封堵剂作为基浆,另一份加入市售磺化沥青封堵剂,其余四份分别加入实施例1~4中得到的纳米封堵剂,封堵剂加量均为2wt%,六份均用重晶石调整密度至2.2g/cm3,于180℃热滚老化16h后测试钻井液的各项性能,结果如表2所示:
表2不同种类封堵剂配制的钻井液180℃热滚16h后性能测试结果
从上述表格中数据可看出,经180℃热滚16h后,与未加封堵剂的基浆相比,加入封堵剂后常温中压和高温高压滤失量都有不同程度的降低,但是加入实施例1~4制备的纳米封堵剂配制成的钻井液,滤失量降低更加显著,与市售磺化沥青类封堵剂相比,本发明提供的油田钻井液用纳米封堵剂填充泥饼孔隙效果更强,可以形成一层致密膜结构,封堵性能更加优良。
配方中,Visco1:市售钻井液用提切剂改性硅酸盐Visco1;Redu2:市售钻井液用降滤失剂羧羟基烷烯共聚物Redu2;白沥青:市售钻井液用抑制防塌剂无荧光白沥青NFA-25;Weigh2和Weigh3:市售钻井液用水溶性加重抑制剂有机盐Weigh2和钻井液用水溶性加重抑制剂有机盐Weigh3。
各个表中的缩写表示如下意义:
API:常温中压滤失量;
HTHP:高温高压滤失量。
(2)封堵性能评价
参考专利CN107974243A中提到的一种纳米封堵剂封堵性能评价方法(参见说明书第0063段),利用GGS42-2A型高温高压滤失仪(青岛海通达专用仪器有限公司),以膨润土、处理剂和重晶石为原料,制取一定厚度的人造岩芯,来模拟纳微米级地层。配制六份钻井液,以淡水用量作为基数,钻井液配方为:淡水+0.3%NaCO3+8%评价土,其中一份不加封堵剂作为空白基浆,另一份加入市售磺化沥青封堵剂,其余四份加入实施例1~4得到的纳米封堵剂,封堵剂加量均为3wt%,通过测定加入不同种类封堵剂的钻井液通过模拟地层的平均流量,根据达西公式(岩芯厚度,渗滤压力3.5MP),可以计算出封堵前后模拟地层的渗透率,从而评价封堵效果,结果表3所示:
表3不同种类封堵剂在模拟地层中封堵效果评价
封堵剂类别 | 渗透率(10<sup>-2</sup>mD) | 封堵率,% |
空白基浆 | 586 | / |
磺化沥青 | 327 | 44.20 |
实施例1 | 12.8 | 97.82 |
实施例2 | 12.0 | 97.95 |
实施例3 | 12.6 | 97.85 |
实施例4 | 11.2 | 98.09 |
从表3中可以看出,加入封堵剂后,模拟地层的渗透率都有不同程度的下降,与市售磺化沥青相比,加入实施例1~4制备的纳米封堵剂后的钻井液渗透率降幅显著,可以说明市售磺化沥青在纳微米级地层中封堵效果较差,本发明提供的油田钻井液用纳米封堵剂在加量为3wt%时封堵率可达97%以上,说明本发明在纳微米级地层中封堵性能优良。
配方中,评价土:市售钻井液配浆用英国评价土。
本文中应用了具体个例对发明构思进行了详细阐述,以上实施例的说明只是用于帮助理解本发明的核心思想。应当指出,对于本技术领域的普通技术人员来说,在不脱离该发明构思的前提下,所做的任何显而易见的修改、等同替换或其他改进,均应包含在本发明的保护范围之内。
Claims (9)
1.一种纳米封堵剂改性缩酮,其特征在于,结构式如下:
2.权利要求1所述纳米封堵剂改性缩酮的制备方法,其特征在于,步骤为:
将乙酰乙酸乙酯乙二醇缩酮溶解于乙醇中,加入氯乙酸钠、氢氧化钠和水,在搅拌状态下加热至90~100℃,反应3~4h后,再加入交联剂继续反应3~4h,即可得到纳米级粒径尺寸的纳米封堵剂改性缩酮。
3.根据权利要求2所述的制备方法,其特征在于,按重量份数计,各原料用量为:
4.根据权利要求2所述的的制备方法,其特征在于,所述乙酰乙酸乙酯乙二醇缩酮、乙醇、氯乙酸钠、氢氧化钠均为工业优级产品。
5.根据权利要求2所述的的制备方法,其特征在于,所述交联剂为三偏磷酸钠和/或磷酸氢二钠。
6.根据权利要求5所述的的制备方法,其特征在于,所述三偏磷酸钠和/或磷酸氢二钠为工业优级产品。
7.一种油田钻井液,其特征在于,含有权利要求1所述的纳米封堵剂改性缩酮。
8.根据权利要求7所述的油田钻井液,其特征在于,以钻井液的淡水用量为基数,其纳米封堵剂改性缩酮的含量为1wt%~5wt%。
9.根据权利要求8所述的油田钻井液,其特征在于,配方为:以淡水用量为基数,分别加入0.3%Na2CO3、1.5%Visco1、4%Redu2、3%白沥青、3%聚合醇、50%Weigh2、30%Weigh3和1~5%纳米封堵剂改性缩酮。
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