CN108048062A - 一种堵水调剖剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种堵水调剖剂及制备方法,采用乙丙橡胶为基本树脂原料,碳酸钙和白油作为添加剂,经交联和发泡反应,得到具有均匀孔径的微发泡交联乙丙橡胶造粒后得到所述的堵水调剖剂;整个反应条件温和,操作方便,其具有吸油率和吸油速率可控的特点,吸油后树脂具有良好的力学性能和稳定性,能广泛应用于不同条件的油田二次,三次开采。
Description
技术领域
本发明属于聚合物材料领域,具体涉及一种堵水调剖剂及其制备方法。
背景技术
在油田开发的过程中,当油层原始能量开始降低后,需要向地层补注能量,即向油层注水,以提高原油采收率,然而,当油田开发进入中晚期后,特别是“二次采油”以来,就会遇到油井出水问题,给油井生产带来严重的影响。因此,油田出水问题就成了油田开采过程中的难题。目前,我国油田开采过程中已进入特高含水期。由于油藏中油水的粘度差异,油层水淹状况差异,油层结构的非均质性,导致注入水不均匀推进现象严重,大部分生产井过早见水或水淹,进一步严重影响吸水剖面,造成油藏采收率严重降低,产油量显著降低。因此,在油田开发的过程中,为了能够减少或清除水淹现象,控制产水层中水的流动方向,必须及时注意油井出水趋势,必要时对出水层段采用物理或化学方法封闭堵塞,这种工艺操作叫堵水调剖工艺,所采用的处理剂就是堵水调剖剂。目前,常用的堵水调剖剂有无机盐类(如水玻璃等)和聚合物类。其中聚合物类又分为吸水膨胀树脂和吸油膨胀树脂。如20世纪60年代开始使用聚丙烯酰胺类高分子聚合物凝胶技术,这为化学调剖堵水技术打开了新局面。20世纪90年代初,C S Mccooi等对聚丙烯酰胺/Cr3+凝胶体系引起的渗透率下降机理进行了室内研究。目前,我国水驱油田普遍进入高含水或特高含水开采期,针对单井或井组水驱问题开展的近井调剖堵水或大剂量处理技术,已不能满足解决油藏深部水驱问题的需要。新型廉价、长效深部调剖(驱)剂研究。研究廉价、长效、适应不同油藏条件(高温、高盐、深井、厚油层、水平井等)的新型深部堵水调剖材料是关键。
吸油膨胀橡胶与非极性材料表面(沥青、塑料、橡胶)和极性材料表面(水泥砂浆、钢筋水泥)均有良好的浸润密合性能,可反复快速吸收油而膨胀,且在一定的压力下有稳定的保油性能,是目前最理想的防油止漏密封材料。
二元乙丙橡胶是以乙烯、丙烯为单体共聚而制得,三元乙丙橡胶是以乙烯、丙烯及少量非共轭双烯为单体共聚而制得。乙丙橡胶(EPDM)具有优异的耐热、耐湿、耐寒、耐臭氧、耐老化和电绝缘性,可在130℃下长期使用,也可在150℃或更高的温度下间断使用,且易与聚烯烃塑料共混,硫化胶物理机械性能及压缩永久变形性能直接影响到EPDM制品的可靠性、安全性和使用寿命,因此备受关注。
本发明针对常规吸油树脂类堵水调剖剂成本高,限制了深部调剖大规模应用的问题,研制出一种新型堵水调剖剂。。
发明内容
本发明提供了一种堵水调剖剂,吸油膨胀率以及吸油成胶的速率大大得到提高,且热稳定性和抗盐性也得到改善。
为了解决上述问题,本发明采用的技术方案是这样的,一种堵水调剖剂,采用乙丙橡胶为基本树脂原料,碳酸钙和白油作为添加剂,经交联和发泡反应,得到具有均匀孔径的微发泡交联乙丙橡胶造粒后得到所述的堵水调剖剂。
优选地,以重量份数计,乙丙橡胶100份,碳酸钙50份,白油20份,交联剂0.5-5.0份,发泡剂0.1-4.0份。
优选地,所述的乙丙橡胶为三元乙丙橡胶,二元乙丙橡胶或者两者任意比例的混合,其中乙丙橡胶中乙烯与丙烯的比例为30:70-70:30,门尼粘度 ML(1+4)125℃)为20-70。
优选地,所述的碳酸钙为轻质碳酸钙或者重质碳酸钙,碳酸钙的目数为 300-2000。
优选地,所述的交联剂由质量比为0.5-2:0的助交联剂和交联剂组成,所述的助交联剂一为三丙烯基异氰脲酸酯(TAIC),交联剂为过氧化二异丙苯(DCP) 或双叔丁基过氧化二异丙基苯(BIPB)中的一种或者两者任一比例的混合。
优选地,所述的发泡剂由发泡剂AC与助发泡剂组成,所述的助发泡剂为氧化锌,硬脂酸等中一种或者两者任一比例的混合,发泡剂AC与助发泡剂的质量比为1-2:1。
本发明还提供了上述堵水调剖剂的制备方法,以乙丙橡胶为原料,碳酸钙和白油为填料,添加交联剂和发泡剂,通过高混机内混合均匀后,加入至开炼机内辊压塑化均匀,再经硫化机模压制备出具有均匀孔径的微发泡交联乙丙橡胶,造粒后得到所述的堵水调剖剂。
优选地,所述的开炼机的开炼温度为80-100度,时间为1-10分钟。
优选地,所述的硫化机的压力温度为150-200度,硫化时间1-10分钟。
本发明所述的堵水调剖剂吸油前的性能如表1所示:
表1
性能 | 指标 |
比重(g/cm3) | 1.6 |
100%定伸(Mpa) | 1.0-5.0 |
拉伸强度(Mpa) | 3.0-10.0 |
伸长率(%) | 200-600 |
毛细管挤出外观 | 光滑 |
常温下,吸油成胶时间为1-10天,吸油成胶温度为20-90℃,吸油(26号白油,常温,72小时)成胶后的性能如表2所示:
表2
性能 | 指标 |
体积膨胀率(%) | 200-500 |
耐温(℃) | 90-130 |
耐盐(mg/l) | 高于30000 |
100%定伸(Mpa) | 0.5-2.0 |
拉伸强度(Mpa) | 1.0-8.0 |
伸长率(%) | 100-400 |
压缩变形(60℃/72h,%) | 5-25 |
有益效果:
1、本发明所述的堵水调剖剂是通过在乙丙橡胶聚合物引入交联剂和适量发泡剂制得,大大提高了聚合物吸油膨胀率以及成胶时间速率,且热稳定性和抗盐性也有改善;通过加入碳酸钙填料,提高其强度性能,同时降低成本,但碳酸钙必须在一定范围内使用,否则成胶后力学性能下降,无法起到填堵的效果;由于乙丙橡胶在填堵剂的配方中所占成本超过80%,因此开发出了最佳的配方,减少乙丙橡胶的用量,使得乙丙橡胶能在较低的含量下,通过交联后仍然能形成性能稳定的网络结构,从而达到降低成本、扩大调剖半径和堵剂用量的目的,最终能广泛应用于不同条件的油田二次,三次开采。
2、因本发明在制备过程中交联剂和发泡剂的加入,使得所得产品具有高弹性和黏性,若采用双螺杆挤出法生产容易发生堵塞螺杆情况,导致设备报修和报废,本发明采用双辊开炼机和平板硫化机来生产,克服上述问题,而且工艺简单,易于形成规模化生产,具有广泛的应用前景。
具体实施方式
为了加深对本发明的理解,下面将结合实施例对本发明作进一步详述,该实施例仅用于解释本发明,并不构成对本发明保护范围的限定。
实施例1
一种堵水调剖剂,具体组分组成如表3所示,
表3
其制备方法具体包括以下步骤:
1、首先将称量好的颗粒状乙丙橡胶,碳酸钙,DCP,白油,TAIC,发泡剂 AC,助发泡剂在高混机内混合均匀;
2、将双辊开炼机预热至设定温度90-95度,调节辊间距7-8mm之间,加入已混合好的物料进行塑料,塑炼过程中,用钢刀不断地将料带从辊筒上拉下来折叠辊压,塑化均匀。
3、调节辊间距3-4mm之间辊隙使料温和料带厚度得以控制,辊压约2min 后,当物料变得色泽均匀,且表面有光泽和有一定强度时,结束辊压过程,将混炼好的料带切割剥离辊轴,放置在切割板上,按压膜框的尺寸剪裁;
4、将平板硫化机工作温度设置为160-168度。将装好料的模具放入压板机上层的两块压板之间,启动油压开关,使压机上、下板与模具紧密接触传热。高温高压3min后,将模具换到下层压板,上升压板冷却2min,模具温度会下降,板材得以固化,然后解除压力,取出模具脱模修剪得到板材。
5、用切粒机将乙丙橡胶板材切粒。得到乙丙橡胶颗粒,即为吸油堵水调剖剂。
实施例2~实施例6
与实施例1基本相同,不同之处见表4。
表4
实施例1-6所制备得到的堵水调剖剂分别为堵水调剖剂1-6,经检测,其吸油成胶时间分别为3-10天,吸油成胶温度均为20-90℃,吸油(26号白油,常温,72小时)成胶后的性能后如表5所示:
表5
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种堵水调剖剂,其特征在于,采用乙丙橡胶为基本树脂原料,碳酸钙和白油作为添加剂,经交联和发泡反应,得到具有均匀孔径的微发泡交联乙丙橡胶造粒后得到所述的堵水调剖剂。
2.根据权利要求1所述的一种堵水调剖剂,其特征在于,以重量份数计,乙丙橡胶100份,碳酸钙40-70份 、白油10-40份,交联剂0.5-5.0份,发泡剂0.1-4.0份。
3.根据权利要求1所述的堵水调剖剂,其特征在于,所述的乙丙橡胶为三元乙丙橡胶,二元乙丙橡胶或者两者任意比例的混合,其中乙丙橡胶中乙烯与丙烯的比例为30:70-70:30,门尼粘度ML(1+4)125℃)为20-70。
4.根据权利要求1所述的堵水调剖剂,其特征在于,所述的碳酸钙为轻质碳酸钙或者重质碳酸钙,碳酸钙的目数为300-2000。
5.根据权利要求1所述的堵水调剖剂,其特征在于:所述的交联剂由质量比为0.5-2:0的助交联剂和交联剂组成,所述的助交联剂一为三丙烯基异氰脲酸酯,交联剂为过氧化二异丙苯或双叔丁基过氧化二异丙基苯中的一种或者两者任一比例的混合。
6.根据权利要求1所述的堵水调剖剂,其特征在于,所述的发泡剂由发泡剂AC与助发泡剂组成,所述的助发泡剂为氧化锌,硬脂酸等中一种或者两者任一比例的混合,发泡剂AC与助发泡剂的质量比为1-2:1。
7.权利要求1-6任一权利要求所述的堵水调剖剂的制备方法,其特征在于,以乙丙橡胶为原料,碳酸钙和白油为填料, 添加交联剂和发泡剂,通过高混机内混合均匀后,加入至开炼机内辊压塑化均匀,再经硫化机模压制备出具有均匀孔径的微发泡交联乙丙橡胶,造粒后得到所述的堵水调剖剂。
8.权利要求7所述的堵水调剖剂,其特征在于: 所述的开炼机的开炼温度为80-100度,时间为1-10分钟。
9.根据权利要求1所述的堵水调剖剂,其特征在于: 所述的硫化机的压力温度为150-200度,硫化时间1-10分钟。
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CN114456778A (zh) * | 2020-10-21 | 2022-05-10 | 中国石油化工股份有限公司 | 一种钻井液堵漏材料 |
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