CN117285913A - 一种强吸附型粘土稳定剂的制备方法 - Google Patents
一种强吸附型粘土稳定剂的制备方法 Download PDFInfo
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/06—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton from hydroxy amines by reactions involving the etherification or esterification of hydroxy groups
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C217/00—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton
- C07C217/02—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton
- C07C217/04—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated
- C07C217/28—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having one amino group and at least two singly-bound oxygen atoms, with at least one being part of an etherified hydroxy group, bound to the carbon skeleton, e.g. ethers of polyhydroxy amines
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Abstract
本发明涉及油田粘土防膨技术领域，提供了一种强吸附型粘土稳定剂的制备方法，其特征在于由多元醇在碱性条件下接枝3‑氯‑2羟基丙基三甲基氯化铵制得，具有较好的防膨效果与突出的抗水洗能力。该粘土稳定剂2%水溶液防膨率最高可达88%，耐水洗率可达90%以上，制备工艺简单，可用于油井注水过程中地层粘土矿物水化膨胀的抑制。
Description
技术领域
本发明涉及一种强吸附型粘土稳定剂的制备方法，属于石油开采技术领域。
背景技术
粘土是地层中含量很高的一类成分，主要由具有晶体结构的粘土矿物组成的颗粒聚集体。其分类主要包括高岭石、伊利石、蒙脱石、绿泥石、各混层等，它们的水敏性强度排列顺序为：蒙脱石>伊蒙混合矿物>伊利石>高岭石>绿泥石。粘土水化膨胀抑制是石油钻采领域必须要解决的问题，钻井时井壁矿物水化膨胀会造成缩颈、垮塌等意外情况，注水、注汽驱采时地层粘土矿物的水化则会严重降低储层渗透率，给原油采出带来极大的阻碍。
早期的粘土稳定剂主要为氯化钾、氯化铵、甲酸钾等盐类，由于高浓度盐类对底栖生物的影响已逐步被无机多核聚合物、阳离子表面活性剂以及阳离子有机聚合物取代。
随着油田开采过程对经济性与环保性要求的进一步提高，弱吸附性粘土稳定剂由于不耐水洗，存在起效时间短，补加周期快的问题已逐渐被强吸附性、长效高效型粘土稳定剂所替代。此类粘土稳定剂一般在分子结构中包含多个吸附位点，可与粘土颗粒发生多位点吸附，大大增强了抗水洗能力，凭借抑制粘土水化膨胀性能突出、抗水洗能力强、起效浓度低成为了研究的热点。
CN111574993A公开了一种酸化压裂用长效型粘土稳定剂配方，其组成包稳定剂、交联剂、缩膨剂、螯合稳定剂、吸附剂、引发剂、润湿反转剂。此类配方型粘土稳定剂组分较多，在现场应用过程中容易发生因地层成分复杂造成的比例失调与柱分离现象，难以完全发挥粘土稳定剂的抑制效果。CN103571449B公开了一种长效粘土稳定剂的制备方法，该方法将环氧氯丙烷和多电荷阳离子聚季铵盐按摩尔比为1～2：1进行反应，制得粘土稳定剂。该方法制备工艺较为复杂，制备过程中需严格控制产物分子量大小，并且阳离子浓度较高时容易使得粘土颗粒发生团聚堵塞地层孔隙，造成渗透率下降。
CN105950130A公开了一种共聚物复配无机盐型长效粘土稳定剂，该粘土稳定剂由二甲基二烯丙基氯化铵-丙烯酰胺共聚物与高浓度氯化铵复配组成。该粘土稳定剂抑制效果过于依赖于高浓度氯化铵，而学者发现高浓度氯化铵对地层生物群落影响较大，应尽可能减少用量。
随着新型粘土稳定剂的逐步应用，一些新的问题也在使用过程中暴露出来，但从分子结构上考虑，好的粘土稳定剂应具备分子量适当、包含多个吸附位点、结构中同时包含适当间距的亲水亲油基团、合成工艺简单的共性特点。
发明内容
本发明利用含多个羟基的多元醇在碱催化作用下与3-氯-2-羟基丙基三甲基氯化铵发生亲核取代反应，在多元醇羟基位点接枝3-氯-2-羟基丙基三甲基氯化铵从而形成含多个吸附位点的粘土稳定剂，增强了粘土稳定剂与粘土颗粒之间的吸附强度。
本发明所述的一种强吸附型粘土稳定剂，其特征在于，制备过程包含以下步骤：多元醇与3-氯-2-羟基丙基三甲基氯化铵在四口烧瓶中按一定比例分散于水中，再加入一定量碱并在一定温度下反应一段时间，反应产物经过加酸中和、蒸馏除水后制得。
本发明所述的粘土稳定剂，其特征在于反应物多元醇可以是乙二醇、丙三醇、丁二醇、丁三醇、戊二醇、己二醇中的一种或多种混合物。
本发明所述的粘土稳定剂，其特征在于反应用碱可以是NaOH、KOH、氨水以及固体碱催化剂中的一种或多种混合物。
本发明所述的粘土稳定剂，其特征在于制备过程中多元醇与3-氯-2-羟基丙基三甲基氯化铵加量的摩尔比在1:2~1:3。
本发明所述的粘土稳定剂，其特征在于反应温度在40~90℃。
本发明所述的粘土稳定剂，其特征在于反应过程中碱的摩尔加量为多元醇的2~2.5倍。
本发明所述的粘土稳定剂，其特征在于产物中和用酸可以是盐酸、硫酸、硝酸、甲酸、乙酸中的一种或多种混合物。
本发明方法制备的强吸附型粘土稳定剂，具有较好的防膨效果与突出的抗水洗能力。该粘土稳定剂2%水溶液防膨率最高可达88%，耐水洗率可达90%以上，制备工艺简单，可用于油井注水过程中地层粘土矿物水化膨胀的抑制。
具体实施方式
下面结合实施例对本发明加以详细描述
实施例1
称取乙二醇5.0g，3-氯-2-羟基丙基三甲基氯化铵30.0g，去离子水50.0g，NaOH6.5g釜中65℃反应4h，反应结束加入少量盐酸中和并将产物进行减压蒸馏去除多余水分，制得粘土稳定剂。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，结果如表1所示。
实施例2
称取丙二醇5.0g，3-氯-2-羟基丙基三甲基氯化铵25.0g，去离子水50.0g，NaOH5.3g于水热釜中75℃反应4h，反应结束加入少量盐酸中和并将产物进行减压蒸馏去除多余水分，制得粘土稳定剂。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，结果如表1所示。
实施例3
称取丙三醇5.0g，3-氯-2-羟基丙基三甲基氯化铵20.5g，去离子水50.0g，NaOH4.5g于水热釜中75℃反应4h，反应结束加入少量盐酸中和并将产物进行减压蒸馏去除多余水分，制得粘土稳定剂。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，结果如表1所示。
实施例4
称取丁二醇5.0g，3-氯-2-羟基丙基三甲基氯化铵21.0g，去离子水50.0g，KOH6.3g于水热釜中75℃反应4h，反应结束加入少量盐酸中和并将产物进行减压蒸馏去除多余水分，制得粘土稳定剂。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，结果如表1所示。
实施例5
称取丁三醇5.0g，3-氯-2-羟基丙基三甲基氯化铵18.0g，去离子水50.0g，NaOH3.8g于水热釜中75℃反应4h，反应结束加入少量盐酸中和并将产物进行减压蒸馏去除多余水分，制得粘土稳定剂。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，结果如表1所示。
实施例6
称取戊二醇5.0g，3-氯-2-羟基丙基三甲基氯化铵18.5g，去离子水50.0g，NaOH3.9g于水热釜中75℃反应4h，反应结束加入少量盐酸中和并将产物进行减压蒸馏去除多余水分，制得粘土稳定剂。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，结果如表1所示。
实施例7
称取己二醇5.0g，3-氯-2-羟基丙基三甲基氯化铵16.0g，去离子水50.0g，NaOH3.4g于水热釜中75℃反应4h，反应结束加入少量盐酸中和并将产物进行减压蒸馏去除多余水分，制得粘土稳定剂。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，结果如表1所示。
实施例8
称取乙二醇5.0g，3-氯-2-羟基丙基三甲基氯化铵45.5g，去离子水100.0g，NaOH6.5g于水热釜中90℃反应4h，反应结束加入少量盐酸中和并将产物进行减压蒸馏去除多余水分，制得粘土稳定剂。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，结果如表1所示。
实施例9
称取丙三醇5.0g，3-氯-2-羟基丙基三甲基氯化铵20.5g，去离子水50.0g，NaOH8.1g于水热釜中75℃反应4h，反应结束加入少量盐酸中和并将产物进行减压蒸馏去除多余水分，制得粘土稳定剂。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，结果如表1所示。
实施例10
称取戊二醇5.0g，3-氯-2-羟基丙基三甲基氯化铵18.5g，去离子水50.0g，NaOH4.5g于水热釜中85℃反应4h，反应结束加入少量盐酸中和并将产物进行减压蒸馏去除多余水分，制得粘土稳定剂。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，结果如表1所示。
对比例1
称取4.0g乙二醇于烧杯中并加去离子水至200g，充分搅拌后评价其性能。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，耐水洗率以文献常用离心法进行评价，结果如表1所示。
对比例2
称取4.0g 3氯2羟基丙基三甲基氯化铵于烧杯中并加去离子水至200g，充分搅拌后评价其性能。防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行评价，耐水洗率以文献常用离心法进行评价，结果如表1所示。
防膨率按照《SY/T5971-2016注水用粘土稳定剂性能评价方法》进行试验，步骤如下：称取0.5g钠膨润土，加入10mL离心管中，加入去离子水至10mL刻度，充分摇匀，在室温下静置2h，装入离心机内，在转速为1500r/min下离心15min，读出钠膨润土在水中的体积V2。采用相同步骤以一定浓度的粘土稳定剂水溶液代替清水，测得离心后土的体积V1。以煤油代替水测得土的体积V0。
式中：η—防膨率，%；V0—钠膨润土在煤油中的体积，mL；V1—钠膨润土在粘土稳定剂中的体积，mL；V2—钠膨润土在清水中的体积，mL；
耐水洗性能测试步骤如下：
先采用离心法评价完样品防膨率，然后将离心管中的上层清液倒出，加去离子水至10mL，充分搅匀静置2h后在离心机中以1500r/min转速离心15min，最终读出离心管中膨润土的最终体积V1’。
耐水洗率计算公式：
式中：V1为膨润土在粘土稳定剂水溶液中的膨胀体积，mL；
V1’为膨润土水洗后的膨胀体积，mL；V2为膨润土在清水中的膨胀体积，mL。
表1 粘土稳定剂性能评价试验
| 样品 | 防膨率/% | 耐水洗率/% | |
| 实施例1 | 81 | 92 | |
| 实施例2 | 80 | 91 | |
| 实施例3 | 78 | 95 | |
| 实施例4 | 86 | 93 | |
| 实施例5 | 75 | 95 | |
| 实施例6 | 88 | 93 | |
| 实施例7 | 87 | 91 | |
| 实施例8 | 85 | 92 | |
| 实施例9 | 75 | 95 | |
| 实施例10 | 88 | 94 | |
| 对比例1 | 24 | 53 | |
| 对比例2 | 58 | 68 |
通过以上实施例与对比例可以看出，本发明制备的含多吸附位点的粘土稳定剂防膨性能优秀，抗水洗能力突出，制备工艺简单，具有较好的应用前景。
Claims (7)
1.一种强吸附型粘土稳定剂的制备方法，其特征在于包含以下步骤：多元醇与3-氯-2-羟基丙基三甲基氯化铵分散于去离子水中，再加入反应，反应产物经过加酸中和、蒸馏除水后制得强吸附型粘土稳定剂。
2.根据权利要求1所述的制备方法，其特征在于多元醇为乙二醇、丙三醇、丁二醇、丁三醇、戊二醇、己二醇中的一种或多种混合物。
3.根据权利要求1所述的制备方法，其特征在于反应用碱为NaOH、KOH、氨水以及固体碱催化剂中的一种或多种混合物。
4.根据权利要求1所述的制备方法，其特征在于多元醇与3-氯-2-羟基丙基三甲基氯化铵加量的摩尔比在1:2~1:3。
5.根据权利要求1所述的制备方法，其特征在于反应温度在40~90℃。
6.根据权利要求1所述的制备方法，其特征在于反应过程中碱的摩尔加量为多元醇的2~2.5倍。
7.根据权利要求1所述的制备方法，其特征在于反应产物中和用酸为盐酸、硫酸、硝酸、甲酸、乙酸中的一种或多种混合物。
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