CN108774503A - 一种钻井液用微纳米防塌封堵剂及其制备方法 - Google Patents
一种钻井液用微纳米防塌封堵剂及其制备方法 Download PDFInfo
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
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- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
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Abstract
本发明公开了一种钻井液用微纳米防塌封堵剂及其制备方法，该封堵剂由以下重量份配比的原料制成：环氧树脂5‑20份，衣康酸5‑15份，丙烯酸10‑38份，2‑丙烯酰胺基‑2‑甲基丙磺酸15‑35份，pH值调节剂2‑10份，乳化剂1‑6份，引发剂0.2‑1.0份，溶剂5‑15份，水50‑150份。本发明和现有技术相比，有纳米级及微米级可变形粒子，降低滤失量，调节流变性，抗温性能好，无荧光，配伍性良好；同时该封堵剂分子链上带有多种吸附基团，能吸附在黏土颗粒表面对钻井液中的颗粒填充形成的滤饼进行修补；通过粒径尺寸和可变形特性使其可以进入泥页岩地层孔隙和层理，阻止滤液进入地层，起到稳定井壁的作用；该封堵剂分散能力强，稳定性高，适用于各种微裂缝发育的硬脆性泥岩。
Description
技术领域
本发明涉及钻井液处理剂技术领域，具体是一种钻井液用微纳米防塌封堵剂及其制备方法。
背景技术
井壁稳定性问题是世界许多油田都普遍存在的一大难题，一直困扰着石油工业的发展。目前，水基钻井液的护壁防塌作用有多种途径和方法，总体上可归纳为三个方向，即：密度支撑、封堵防塌、抑制水化。当前常用的防塌剂如沥青类、腐殖酸类等产品，因荧光级别、环保性能等原因其应用受到一定的限制；而封堵剂乳化石蜡虽比较常用，但抗温性能差、软化点低，适用的温度范围有限，对深井泥页岩地层的井壁稳定作用效果较差。
在钻井过程中需要对井壁地层的岩石孔隙进行封堵。不同地层岩石的孔隙尺寸也不同，易发生井壁失稳的泥页岩地层的孔隙尺寸多为微纳米级别，常规的粒子无法进行有效封堵，不能有效阻止钻井液及其滤液对近井壁地层的侵蚀，进而引起泥页岩水化膨胀，造成井壁坍塌等复杂事故。钻井过程中，对井壁的微小裂缝进行有效封堵是避免井壁失稳的有效手段之一，而沥青类和乳化石蜡封堵剂材料颗粒尺寸都较大，对于裂缝缝隙尺寸较大的地层封堵效果较好，但是对泥岩泥微裂缝和层理这类纳微米孔隙(缝)不能形成很好的尺寸匹配，其井壁稳定能力受到较大限制。
综上所述，一种钻井液用微纳米防塌封堵剂将更有效的对泥页岩地层的微裂缝及层理进行封堵，有助于解决泥页岩地层的井壁失稳这一技术难题，有利于钻井液技术的发展。
发明内容
本发明的技术任务是提供一种钻井液用微纳米防塌封堵剂及其制备方法。
本发明的技术任务是按以下方式实现的：
一种钻井液用微纳米防塌封堵剂，该封堵剂由以下重量份配比的原料制成：
环氧树脂5-20份，衣康酸5-15份，丙烯酸10-38份，2-丙烯酰胺基-2-甲基丙磺酸15-35份，pH值调节剂2-10份，乳化剂1-6份，引发剂0.2-1.0份，溶剂5-15份，水50-150份。
所述的pH值调节剂是氢氧化钾、氢氧化钠、氨水中的一种。
所述的乳化剂是山梨醇酐油酸酯、辛基苯酚聚氧乙烯醚、聚氧乙烯山梨糖醇酐三油酸酯、十二烷基硫酸钠中的一种或两种的混合物。
所述的引发剂是过硫酸钾、过硫酸铵、过硫酸铵与亚硫酸氢钠氧化还原体系、叔丁基过氧化氢与亚硫酸氢钠氧化还原体系、过氧化苯甲酰、偶氮二异丁腈中的一种。
所述的溶剂是丙酮、乙醇、甲苯、二甲苯、1，4-丁二醇、正丁醇、苯甲醇、乙二醇乙醚、乙二醇丁醚、2-叔丁氧基乙醇中的一种或两种的混合物。
一种钻井液用微纳米防塌封堵剂的制备方法，该制备方法的步骤如下：
步骤1)将适量衣康酸、丙烯酸、以及2-丙烯酰胺基-2-甲基丙磺酸溶解在水中，然后用pH值调节剂将溶液调至pH＝3-10得到混合溶液一；
步骤2)称取适量环氧树脂与适量溶剂在60-120℃下溶解1h，获得料液；
步骤3)于30-100℃下，向步骤2)获得的料液中通氮气30min后，滴加步骤1)获得的混合溶液一，同时加入引发剂和乳化剂，得到混合溶液二；
步骤4)将步骤3)获得的混合溶液二送入高剪切乳化机，加入pH值调节剂调至pH＝6-10，然后进行剪切乳化，之后得到最终产物；
所述的各步骤中各原料的重量份配比如下：
环氧树脂5-20份，衣康酸5-15份，丙烯酸10-38份，2-丙烯酰胺基-2-甲基丙磺酸15-35份，pH值调节剂2-10份，乳化剂1-6份，引发剂0.2-1.0份，溶剂5-15份，水50-150份。
所述的步骤3)中，引发剂和乳化剂需要缓慢加入，反应时间为4-10h。
本发明的一种钻井液用微纳米防塌封堵剂及其制备方法和现有技术相比，有纳米级及微米级可变形粒子，降低滤失量，调节流变性，抗温性能好，无荧光，配伍性良好；同时该封堵剂分子链上带有多种吸附基团，能吸附在黏土颗粒表面对钻井液中的颗粒填充形成的滤饼进行修补；通过粒径尺寸和可变形特性使其可以进入泥页岩地层孔隙和层理，阻止滤液进入地层，起到稳定井壁的作用；该封堵剂分散能力强，稳定性高，适用于各种微裂缝发育的硬脆性泥岩。
具体实施方式
实施例1：
备料：
环氧树脂5kg，衣康酸5kg，丙烯酸18kg，2-丙烯酰胺基-2-甲基丙磺酸15kg，氨水3kg，辛基苯酚聚氧乙烯醚2kg，过氧化苯甲酰0.2kg，正丁醇5kg，水50kg；
加工：
步骤1)将衣康酸、丙烯酸、以及2-丙烯酰胺基-2-甲基丙磺酸溶解在水中，然后用氨水将溶液调至pH＝4得到混合溶液一；
步骤2)称取环氧树脂与正丁醇在60℃下溶解1h，获得料液；
步骤3)于80℃下，向步骤2)获得的料液中通氮气30min后，滴加步骤1)获得的混合溶液一，同时缓慢加入过氧化苯甲酰和辛基苯酚聚氧乙烯醚，反应时间6h后，得到混合溶液二；
步骤4)将步骤3)获得的混合溶液二送入高剪切乳化机，加入氨水调至pH＝6，然后进行剪切乳化，之后得到最终产物。
实施例2：
备料：
环氧树脂8kg，衣康酸12kg，丙烯酸10kg，2-丙烯酰胺基-2-甲基丙磺酸25kg，氢氧化钾5kg，聚氧乙烯山梨糖醇酐三油酸酯3kg，过硫酸钾0.8kg，甲苯12kg，水100kg；
加工：
步骤1)将衣康酸、丙烯酸、以及2-丙烯酰胺基-2-甲基丙磺酸溶解在水中，然后用氢氧化钾将溶液调至pH＝6得到混合溶液一；
步骤2)称取环氧树脂与甲苯在100℃下溶解1h，获得料液；
步骤3)于60℃下，向步骤2)获得的料液中通氮气30min后，滴加步骤1)获得的混合溶液一，同时缓慢加入过硫酸钾和聚氧乙烯山梨糖醇酐三油酸酯，反应时间4h后，得到混合溶液二；
步骤4)将步骤3)获得的混合溶液二送入高剪切乳化机，加入氢氧化钾调至pH＝8，然后进行剪切乳化，之后得到最终产物。
实施例3：
备料：
环氧树脂18kg、衣康酸7kg、丙烯酸30kg、2-丙烯酰胺基-2-甲基丙磺酸9kg、氢氧化钠4kg、十二烷基硫酸钠和山梨醇酐油酸酯的混合物4kg、偶氮二异丁腈0.4kg、二甲苯和1，4-丁二醇的混合物10kg、水70kg；
加工：
步骤1)将衣康酸、丙烯酸、以及2-丙烯酰胺基-2-甲基丙磺酸溶解在水中，然后用氢氧化钠将溶液调至pH＝3得到混合溶液一；
步骤2)称取环氧树脂与二甲苯和1，4-丁二醇的混合物在80℃下溶解1h，获得料液；
步骤3)于70℃下，向步骤2)获得的料液中通氮气30min后，滴加步骤1)获得的混合溶液一，同时缓慢加入偶氮二异丁腈与十二烷基硫酸钠和山梨醇酐油酸酯的混合物，反应时间8h后，得到混合溶液二；
步骤4)将步骤3)获得的混合溶液二送入高剪切乳化机，加入氢氧化钠调至pH＝8，然后进行剪切乳化，之后得到最终产物。
上述三个实施例的样品粒度测试：
取实施案例1-3的样品，配制成质量百分比浓度为0.5％的溶液，在超声分散仪上超声分散5min，激光粒度分布仪测定粒径得到表1数据；
表1实施例1-3样品激光粒度分布表
| 名称 | ＜100nm(％) | ＜500nm(％) | ＜1000nm(％) | ＞1μm(％) |
| 实施例1 | 21.60 | 50.21 | 89.69 | 10.31 |
| 实施例2 | 25.72 | 59.80 | 91.20 | 8.80 |
| 实施例3 | 22.58 | 52.76 | 86.39 | 13.61 |
岩心压力传递实验：
岩心压力传递实验考察封堵后岩心压力传递情况，选用低渗透天然页岩岩心；围压为50MPa，上游压力为35MPa，监测下游压力的变化；配制4％氯化钠盐水溶液、3％实施例1-3水溶液；
表2岩心压力传递结果
| 名称 | 24h下游压力(MPa) |
| 4％氯化钠盐水 | 35 |
| 实施例1 | 1.58 |
| 实施例2 | 1.60 |
| 实施例3 | 1.55 |
上述实验数据表明，实施例1-3的产品均有较好的阻缓压力传递作用，都能较明显地降低泥页岩的渗透率，阻缓压力传递效果较为明显。这就说明了它们具有较明显的封堵阻缓压力传递和滤液传递作用，具有良好的封堵作用。
钻井液性能测定：
按水：钠土：无水碳酸钠＝100：5.0：0.2的比例配制基浆，高速搅拌20min，密闭养护24h。取一份养护后的基浆400mL，高速搅拌5min，按GB/T 16783.1的规定测定基浆的流变性和API虑失量；
取上述配好的基浆400mL，加入实施例1-3 12.0g，高速搅拌20min，放入高温滚子炉中于150℃老化16h，然后取出，降温至室温(25℃±1℃)，高速搅拌5min，在室温(25℃±1℃)条件下，按GB/T 16783.1中的规定测定150℃老化后流变性和API滤失量。
表3封堵剂对钻井液流变性及滤失量影响
由上表钻井液用微纳米防塌封堵剂性能评价结果可知，该封堵剂不仅不增加体系粘度，而且具有一定的降粘切效果；经150℃老化后的滤失量与室温条件下的相当，表明抗温效果明显。
通过上面具体实施方式，所述技术领域的技术人员可容易的实现本发明。但是应当理解，本发明并不限于上述的几种具体实施方式。在公开的实施方式的基础上，所述技术领域的技术人员可任意组合不同的技术特征，从而实现不同的技术方案。
Claims (10)
1.一种钻井液用微纳米防塌封堵剂，其特征在于，该封堵剂由以下重量份配比的原料制成：
环氧树脂5-20份，衣康酸5-15份，丙烯酸10-38份，2-丙烯酰胺基-2-甲基丙磺酸15-35份，pH值调节剂2-10份，乳化剂1-6份，引发剂0.2-1.0份，溶剂5-15份，水50-150份。
2.根据权利要求1所述的封堵剂，其特征在于，所述的pH值调节剂是氢氧化钾、氢氧化钠、氨水中的一种。
3.根据权利要求1所述的封堵剂，其特征在于，所述的乳化剂是山梨醇酐油酸酯、辛基苯酚聚氧乙烯醚、聚氧乙烯山梨糖醇酐三油酸酯、十二烷基硫酸钠中的一种或两种的混合物。
4.根据权利要求1所述的封堵剂，其特征在于，所述的引发剂是过硫酸钾、过硫酸铵、过硫酸铵与亚硫酸氢钠氧化还原体系、叔丁基过氧化氢与亚硫酸氢钠氧化还原体系、过氧化苯甲酰、偶氮二异丁腈中的一种。
5.根据权利要求1所述的封堵剂，其特征在于，所述的溶剂是丙酮、乙醇、甲苯、二甲苯、1，4-丁二醇、正丁醇、苯甲醇、乙二醇乙醚、乙二醇丁醚、2-叔丁氧基乙醇中的一种或两种的混合物。
6.一种钻井液用微纳米防塌封堵剂的制备方法，其特征在于，该制备方法的步骤如下：
步骤1)将适量衣康酸、丙烯酸、以及2-丙烯酰胺基-2-甲基丙磺酸溶解在水中，然后用pH值调节剂将溶液调至pH＝3-10得到混合溶液一；
步骤2)称取适量环氧树脂与适量溶剂在60-120℃下溶解1h，获得料液；
步骤3)于30-100℃下，向步骤2)获得的料液中通氮气30min后，滴加步骤1)获得的混合溶液一，同时加入引发剂和乳化剂，得到混合溶液二；
步骤4)将步骤3)获得的混合溶液二送入高剪切乳化机，加入pH值调节剂调至pH＝6-10，然后进行剪切乳化，之后得到最终产物；
所述的各步骤中各原料的重量份配比如下：
环氧树脂5-20份，衣康酸5-15份，丙烯酸10-38份，2-丙烯酰胺基-2-甲基丙磺酸15-35份，pH值调节剂2-10份，乳化剂1-6份，引发剂0.2-1.0份，溶剂5-15份，水50-150份。
7.根据权利要求6所述的制备方法，其特征在于，所述的步骤3)中，引发剂和乳化剂需要缓慢加入，反应时间为4-10h。
8.根据权利要求6所述的制备方法，其特征在于，所述的pH值调节剂是氢氧化钾、氢氧化钠、氨水中的一种。
9.根据权利要求6所述的制备方法，其特征在于，所述的乳化剂是山梨醇酐油酸酯、辛基苯酚聚氧乙烯醚、聚氧乙烯山梨糖醇酐三油酸酯、十二烷基硫酸钠中的一种或两种的混合物；所述的溶剂是丙酮、乙醇、甲苯、二甲苯、1，4-丁二醇、正丁醇、苯甲醇中的一种或两种的混合物。
10.根据权利要求6所述的制备方法，其特征在于，所述的引发剂是过硫酸钾、过硫酸铵、过硫酸铵与亚硫酸氢钠氧化还原体系、叔丁基过氧化氢与亚硫酸氢钠氧化还原体系、过氧化苯甲酰、偶氮二异丁腈中的一种。
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Address after: 257000 east of jingsan road and north of Weishi Road, new material industrial park, dongyinggang Economic Development Zone, Dongying City, Shandong Province Patentee after: SHANDONG DESHUNYUAN PETROLEUM SCI.AND TECH. CO.,LTD. Address before: 257091 complex building, No. 69, Dengzhou Road, Dongying Economic and Technological Development Zone, Dongying City, Shandong Province Patentee before: SHANDONG DESHUNYUAN PETROLEUM SCI.AND TECH. CO.,LTD. |
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Date of cancellation: 20230222 Granted publication date: 20210910 Pledgee: Bank of China Limited Dongying North 2nd Road sub branch Pledgor: SHANDONG DESHUNYUAN PETROLEUM SCI.AND TECH. CO.,LTD. Registration number: Y2022980001911 |
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Denomination of invention: A micro-nano anti-sloughing plugging agent for drilling fluid and its preparation method Effective date of registration: 20230224 Granted publication date: 20210910 Pledgee: Bank of China Limited Dongying North 2nd Road sub branch Pledgor: SHANDONG DESHUNYUAN PETROLEUM SCI.AND TECH. CO.,LTD. Registration number: Y2023980033321 |
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Date of cancellation: 20231227 Granted publication date: 20210910 Pledgee: Bank of China Limited Dongying North 2nd Road sub branch Pledgor: SHANDONG DESHUNYUAN PETROLEUM SCI.AND TECH. CO.,LTD. Registration number: Y2023980033321 |
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Denomination of invention: A micro nano anti collapse plugging agent for drilling fluid and its preparation method Effective date of registration: 20231228 Granted publication date: 20210910 Pledgee: Bank of China Limited Dongying North 2nd Road sub branch Pledgor: SHANDONG DESHUNYUAN PETROLEUM SCI.AND TECH. CO.,LTD. Registration number: Y2023980075120 |
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