CN115490815A - 一种以poss为中心的可膨胀复合封堵剂 - Google Patents
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Abstract
本发明提供了一种以POSS为中心的可膨胀复合封堵剂的制备方法，通过采用乙烯基三甲氧基硅烷(VTMS)经催化，在溶剂中水解后自缩合，形成笼状分子即八乙烯基笼型倍半硅氧烷，然后在引发剂、乳化剂等的作用下，引发单体发生乳液聚合制备出以POSS为中心、聚(AM‑AMPS)为臂的共聚物。解决了普通钻井液封堵剂难以在高温下继续发挥作用，对于井下不规则孔隙很难进行有效封堵的技术问题。
Description
技术领域
本发明涉及钻井液添加剂领域，尤其涉及一种以八乙烯基POSS为中心的可膨胀复合封堵剂的制备方法。
背景技术
石油天然气作为能源和基础原材料，在当今社会有着举足轻重的作用，被称为现代工业的“黑色血液”。据原国土资源部预测，我国石油可开采量预计达150亿吨，资源丰富，勘探开发前景良好。但我国油气储存条件差，地层构造复杂，有73％的资源量深埋地下，且不连续。
对于油气开发的关键技术，尤其是钻井液稳定井壁技术方面，我国有所不足。国外针对泥饼滤失量大、黏土水化膨胀等引起的井壁失稳提出了相关解决方案。其中，加强钻井液对微小孔隙的封堵是避免井壁失稳的主要措施之一。在钻井过程中，对于一些裂缝发育的地层，当钻井液与井壁地层接触，若钻井液的泥饼质量及封堵性能差，钻井液及滤液容易通过裂缝进入周围地层，造成钻井液循环消耗量增大，导致孔隙的压力上升和地层岩石的力学性质发生变化，改变围岩的应力分布，并发生粘土的水化膨胀，引起井壁岩石的强度降低，发生井壁坍塌。常规钻井液封堵剂主要以架桥和充填孔隙进行封堵，但我国油藏较深，地下温度较高，普通钻井液封堵剂难以在高温下继续发挥作用，对于井下不规则孔隙很难进行有效封堵，因此需要具有可膨胀或者可变形的粒子对不规则的孔隙进行封堵。
发明内容
为了解决背景技术中钻井液及滤液对井壁孔隙的封堵性能的不足，提供了一种以POSS为中心的可膨胀复合封堵剂。
一种以POSS为中心的可膨胀复合封堵剂的制备方法，如下：
步骤一：制备八乙烯基POSS
将20～30份的乙烯基三甲氧基硅烷(VTMS)溶于100份的有机溶剂中，并将其置于在三颈烧瓶中，搅拌加热至30～50℃，逐渐滴加80份一定浓度的盐酸溶液，反应24～48h。冷却至室温后，将白色固体产物用乙醇反复洗涤，在60℃下干燥12h，得白色固体颗粒，即八乙烯基笼型倍半硅氧烷。
步骤二：制备以POSS为中心的可膨胀复合封堵剂
以白油作为溶剂，称取一定量的乳化剂加入三颈烧瓶充分搅拌，得到油相溶液，再加入3份的八乙烯基笼型倍半硅氧烷。称取40份去离子水，添加10份2-丙烯酰胺-2-甲基丙磺酸(AMPS)，并用氢氧化钠调节pH值，再加入25份的AM，得到水相溶液。将水相逐滴加入油相中，快速分散乳化后，加热溶液至35～50℃，然后逐滴滴加引发剂溶液，通入N2，继续反应2～3h。冷却得到共聚物溶液，将该溶液抽滤后得到白色固体产物，经乙醇反复洗涤并在60℃下干燥24h，即得到了所述的以POSS为中心的可膨胀复合封堵剂。
其中所述的有机溶剂，为乙酸乙酯、乙醇、甲醇、石油醚、二氯甲烷中的一种或者几种。
其中所述的乳化剂，为非离子型表面活性剂复配使用，为司班-80和吐温-80。
其中所述的引发剂，为氧化-还原引发剂体系，所述的氧化-还原引发剂体系中氧化剂：还原剂的摩尔比为1：1。
有益效果：
以POSS为中心的可膨胀复合封堵剂兼有无机粒子强度高和有机聚合物可变形的优点，同时能够提高有机聚合物的耐温性能，且在钻井液中具有良好的分散性。在制备中未使用交联剂，八乙烯基POSS起到交联剂的作用。
附图说明
图1为本发明合成八乙烯基POSS的反应机理图；
图2为可膨胀复合微球PECMs的结构图；
图3为本发明合成可膨胀复合微球PECMs的反应机理图；
图4为POSS及PECMs添加前后的基础钻井液流变性能及滤失性能；
图5为不同条件下得到的泥饼针入强度图；
图6为不同条件下得到的泥饼粘附强度图。
具体实施例
为了使本发明更清楚明白，下面通过实施例，对一种以POSS为中心的可膨胀复合封堵剂的制备方法和说明书附图做进一步说明。
本发明的原理为：首先采用乙烯基三甲氧基硅烷(VTMS)经催化，在溶剂中水解后自缩合，形成笼状分子即八乙烯基笼型倍半硅氧烷，然后在引发剂、乳化剂等的作用下，引发单体发生乳液聚合制备出以POSS为中心、聚(AM-AMPS)为臂的共聚物。
实施例
1.钻井液配方制备
根据实验经验初步确定基础钻井液配方如下：膨润土5wt％、纯碱(土量)4wt％、两性离子聚合物包被剂0.20wt％、水解聚丙烯腈钾盐0.50wt％、聚阴离子纤维素0.60wt％、氯化钾5wt％、生石灰0.20wt％、磺化酚醛树脂 2wt％、聚合物抗温抗盐降滤失剂2wt％、超细碳酸钙2wt％。
首先配置去离子水、膨润土和纯碱质量比为100：5：0.2的基浆，充分搅拌均匀后，在室温下静置水化24小时。然后，依次按量添加配方中的各种添加剂，在高速下搅拌均匀，得到实验所需的基础钻井液。
2.八乙烯基POSS的制备
本实验使用VTMS制备八乙烯基POSS，其分子式及反应机理如图1所示。量取20～30体积份VTMS作为原料，量取共100体积份有机溶剂乙酸乙酯、乙醇、甲醇、石油醚、二氯甲烷中的一种或者几种作为溶剂，倒入三口烧瓶中，置于30～50℃的水浴锅中进行磁力搅拌。向三颈烧瓶中逐滴滴加80份一定浓度的盐酸溶液作为催化剂，反应24～48h，观察到杯壁和杯底出现白色产物。冷却至室温后，取出白色固体产物并用乙醇重复洗涤，抽滤出固体并于60℃下干燥24小时，获得白色颗粒状产物，即目标产物POSS。
3.AMPS/AM/POSS聚合物微球(PECMs)的制备
称取150重量份白油作为溶剂，并称取17体积份的乳化剂加入三颈烧瓶充分搅拌，其中两种乳化剂的质量比为司班-80：吐温-80＝10：7。使其充分搅拌得到油相溶液，再向三颈烧瓶中加入3重量份的POSS。接下来配置水相溶液，称取40重量份去离子水，添加8～12重量份AMPS，并用氢氧化钠将溶液调制中性，接着再加入20～30重量份的AM，得到水相。将水相逐滴加入油相中，并将三颈烧瓶置于35～50℃的水浴锅中，充分搅拌30min一定时间。向三颈烧瓶中逐滴滴加一定浓度的引发剂水溶液，通入氮气，反应3～4小时。反应结束后倒入大量乙醇重复洗涤产品三次，抽滤出固体并于60℃下干燥24小时，获得白色颗粒状产物，即PECMs，可膨胀复合微球PECMs的分子式及反应机理如图2-3所示。
4.钻井液常规性能评价
根据美国石油学会(API)的测试方案对钻井液性能进行了评估。首先，利用中压泥浆过滤装置(7NS-2A，中国青岛通春石油仪器有限公司)对160 ℃老化前后钻井液的常温滤失量(FLAPI)进行评价，计时30min。采用高温高压过滤装置(GGS42-2A，青岛恒泰达机电设备有限公司)测定含聚合物基浆在160℃老化16h后的高温高压滤失量(FLAPI)。FLAPI和FLAPI分别在25℃和0.7MPa和160℃和4.5MPa下进行测量。
采用六速旋转粘度计(ZNN-D6B)测定160℃老化16h前后钻井液的室温流变性能。在300rpm和600rpm时分别测定了表面粘度AV(mPa·s)和塑性粘度PV\左(mPa·s)和屈服点YP(Pa)。使用的公式如下:
AV＝1/2Φ600(mPa·s)
PV＝Φ600-Φ300(mPa·s)
YP＝1/2(Φ300-PV)(Pa)
其中，
和
分别是六速旋转粘度计在300rpm和600rpm时的转速读数。
添加POSS以及可膨胀复合微球处理前后的基础钻井液的常规性能据图4所示。
5.泥饼针入度的测定
根据图5所示，按照上述的基础钻井液滤失量的测定步骤压制泥饼。将泥饼置于中心有孔的圆盘上，铺展平整后放于万能力学试验机上，将钢针固定在万能力学试验机的上夹具中。启动仪器，记录钢针穿破泥饼的极限突破力，即为泥饼的针入强度(N)。
6.泥饼粘附强度的测定
根据图6所示，按照上述的基础钻井液滤失量的测定步骤压制泥饼。将泥饼涂抹在实验室自制的模具上，并将模具置于力学试验机上，进行拉伸实验，记录拉伸过程最大拉力，即为泥饼的粘附强度(kPa)。
最后应说明的是：以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (4)
1.一种以POSS为中心的可膨胀复合封堵剂的制备方法，其特征在于，包括如下步骤：
步骤一：制备八乙烯基POSS
将20～30份的乙烯基三甲氧基硅烷溶于100份的有机溶剂中，并将其置于在三颈烧瓶中，搅拌加热至30～50℃，逐渐滴加80份一定浓度的盐酸溶液，反应24～48h，冷却至室温后，将白色固体产物用乙醇反复洗涤，在60℃下干燥12h，得白色固体颗粒，即八乙烯基笼型倍半硅氧烷；
步骤二：制备以POSS为中心的可膨胀复合封堵剂
以白油作为溶剂，称取一定量的乳化剂加入三颈烧瓶充分搅拌，得到油相溶液，再加入3份的八乙烯基笼型倍半硅氧烷，称取40份去离子水，添加10份2-丙烯酰胺-2-甲基丙磺酸，并用氢氧化钠调节pH值，再加入25份的AM，得到水相溶液，将水相逐滴加入油相中，快速分散乳化后，加热溶液至35～50℃，然后逐滴滴加引发剂溶液，通入N2，继续反应2～3h，冷却得到共聚物溶液，将该溶液抽滤后得到白色固体产物，经乙醇反复洗涤并在60℃下干燥24h，即得到了所述的以POSS为中心的可膨胀复合封堵剂。
2.根据权利要求1所述的一种以POSS为中心的可膨胀复合封堵剂的制备方法，其特征在于，步骤一中所述的有机溶剂，为乙酸乙酯、乙醇、甲醇、石油醚、二氯甲烷中的一种或者几种。
3.根据权利要求1所述的一种以POSS为中心的可膨胀复合封堵剂的制备方法，其特征在于，步骤二中所述的乳化剂，为非离子型表面活性剂复配使用，为司班-80和吐温-80。
4.根据权利要求1所述的一种以POSS为中心的可膨胀复合封堵剂的制备方法，其特征在于，步骤二中所述的引发剂，为氧化-还原引发剂体系，氧化-还原引发剂体系中，氧化剂：还原剂的摩尔比为1：1。
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