CN115595130A - 一种pH响应型纳米凝胶封堵材料及其制备方法与应用 - Google Patents
一种pH响应型纳米凝胶封堵材料及其制备方法与应用 Download PDFInfo
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- CN115595130A CN115595130A CN202110777697.3A CN202110777697A CN115595130A CN 115595130 A CN115595130 A CN 115595130A CN 202110777697 A CN202110777697 A CN 202110777697A CN 115595130 A CN115595130 A CN 115595130A
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Abstract
本发明提供一种pH响应型纳米凝胶封堵材料及其制备方法与应用。按照质量份数计,该pH响应型纳米凝胶封堵材料的原料包括:水50‑70份,乳化剂2‑3份,丙烯酸类三元共聚物25‑35份,聚醇类化合物10‑15份,乙烯基吡啶类化合物10‑20份。该pH响应型纳米凝胶封堵材料能够适用于奥陶系碳酸盐岩裂缝及微溶洞地层的封堵,能够自动识别奥陶系碳酸盐岩裂缝及微溶洞漏层并进行有效封堵。
Description
技术领域
本发明属于石油勘探、岩石挖掘技术领域,涉及一种pH响应型纳米凝胶封堵材料及其制备方法与应用。
背景技术
奥陶系地层裂缝及溶洞发育,其地层水钙离子含量一般在5000mg/L以上,pH值一般在5.0-7.0之间。碳酸盐岩裂缝及溶洞主要是通过酸性地层水溶融碳酸盐岩岩石形成的。奥陶系碳酸盐岩储层段发育裂缝及溶洞,而裂缝和溶洞容易发生渗漏及中小型漏失,如何实现快速识别并迅速封堵漏层是目前尚未解决的难题。
发明内容
本发明的目的在于提供一种能够适用于奥陶系碳酸盐岩裂缝及微溶洞地层封堵的封堵材料,该封堵材料能够自动识别奥陶系碳酸盐岩裂缝及微溶洞漏层并进行有效封堵。
为了实现上述目的,本发明提供了一种pH响应型纳米凝胶封堵材料,其中,按照质量份数计,该pH响应型纳米凝胶封堵材料的原料包括:水50-70份,乳化剂2-3份,丙烯酸类三元共聚物25-35份,聚醇类化合物10-15份,乙烯基吡啶类化合物10-20份。
上述pH响应型纳米凝胶封堵材料可以在钻井液中使用。上述pH响应型纳米凝胶封堵材料在碱性流体环境下的溶胀率很低,因为钻井液通常是碱性流体,因此上述pH响应型纳米凝胶封堵材料在碱性钻井液中处于微溶胀收缩的状态;而一旦遇到奥陶系碳酸盐岩裂缝及微溶洞地层,渗透性突然加大,上述pH响应型纳米凝胶封堵材料突然从碱性环境(pH值一般>9)滤失进入酸性环境,进入酸性环境的上述纳米凝胶材料会快速溶胀膨胀,起到较好的封堵效果,从而实现自动识别奥陶系碳酸盐岩裂缝及微溶洞漏层,并起到较好的防漏堵漏效果。
在上述pH响应型纳米凝胶封堵材料中,优选地,所述水选用去离子水。
在上述pH响应型纳米凝胶封堵材料中,优选地,所述的乳化剂包括聚氧乙烯醇、聚氧乙烯醚、OP-7、OP-8、OP-9和OP-10等中的一种或两种以上的组合。
在上述pH响应型纳米凝胶封堵材料中,优选地,所述聚醇类化合物包括聚乙二醇、聚乙烯醇、聚丙二醇和聚己内酯多元醇等中的一种或两种以上的组合。
在上述pH响应型纳米凝胶封堵材料中,优选地,所述乙烯基吡啶类化合物包括反-4-芳乙烯基吡啶、2-乙烯基吡啶、苯乙烯基吡啶和4-苯乙烯基吡啶等中的一种或两种以上的组合。
在上述pH响应型纳米凝胶封堵材料中,优选地,所述丙烯酸类三元共聚物由第一单体、第二单体、第三单体聚合得到;其中,所述第一单体包括甲基丙烯酸、乙基丙烯酸、丙烯酸酯和甲基丙烯酸羟乙酯中的一种或两种以上的组合(其中,所述丙烯酸酯优选包括丙烯酸乙酯、丙烯酸丁酯、丙烯酸异辛酯、丙烯酸甲酯和甲基丙烯酸甲酯中的一种或两种以上的组合),所述第二单体包括乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三(2-甲氧基乙氧基)硅烷、乙烯基三异丙氧基硅烷和γ-甲基丙稀酰氧基丙基三甲氧基硅烷中的一种或两种以上的组合,所述第三单体包括丙烯酰胺、羟甲基丙烯酰胺、苯乙烯、丙烯腈、氯乙烯、醋酸乙烯酯和马来酸酐中的一种或两种以上的组合;
更优选地,以质量计,第一单体、第二单体、第三单体的用量比为40-60:20-30:10-15;
更优选地,所述丙烯酸类三元共聚物通过下述方式制备得到:第一单体水溶液在冰水浴条件下加入氢氧化钠溶液,使第一单体部分中和得到溶液A;溶液A在室温条件下加入第二单体、第三单体,然后在惰性环境下加入引发剂进行聚合反应;聚合反应完成后将产物进行干燥粉碎,密封备用;进一步优选地,所述引发剂的包括偶氮二异丁酸二甲酯、偶氮二异丙基咪唑啉盐酸盐、偶氮二异丁腈、偶氮二异庚腈、过硫酸钾、过硫酸钠、过硫酸铵和异丙苯过氧化氢中的一种或两种以上的组合;再优选地,以质量计,所述引发剂与第一单体、第二单体、第三单体的用量比为:1-5:40-60:20-30:10-15。
在一具体实施方式中,所述丙烯酸类三元共聚物通过下述方式制备得到:
将40-60质量份第一单体的水溶液置于烧杯中,在冰水浴中边搅拌边缓慢滴加10-20质量份质量浓度为20%(以氢氧化钠溶液总质量为100%计)的氢氧化钠溶液,使第一单体部分中和得到溶液A;待溶液A冷却至室温后加入20-30质量份第二单体、10-15质量份第三单体,混合均匀后通氮气30min,加入1-5质量份引发剂聚合,反应完成后取出胶体产物剪碎,放入80℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用。
本发明还提供一种上述pH响应型纳米凝胶封堵材料的制备方法,其中,该方法包括:
将水、聚醇类化合物、乙烯基吡啶类化合物混合后,加入乳化剂、丙烯酸类三元共聚物搅拌均匀得到所述pH响应型纳米凝胶封堵材料。
本发明还提供上述pH响应型纳米凝胶封堵材料在碱性钻井液中的应用。
奥陶系碳酸盐岩储层特征是其地层水钙离子含量一般在5000mg/L以上,pH值一般在5.0-7.0之间,本发明从奥陶系碳酸盐岩储层特征出发,提出了一种能够选择性在奥陶系碳酸盐岩储层pH值范围内实现封堵的封堵材料。本发明提供的pH响应型纳米凝胶封堵材料仅在pH值小于5-7时大幅溶胀起效,起到迅速封堵的作用。本发明提供的pH响应型纳米凝胶封堵材料在pH值大于9的钻井液中,呈收缩状态,pH响应型纳米凝胶封堵材料不溶胀,而一旦漏入碳酸盐岩储层中以后,pH值瞬间低于7,尤其是地层水钙离子含量一般在5000mg/L以上时,该pH响应型纳米凝胶封堵材料,会大幅溶胀起效,起到迅速封堵的作用。
附图说明
图1A为实施例1提供的pH响应型纳米凝胶封堵材料在pH=7时的凝胶状态图(放大5000倍)。
图1B为实施例1提供的pH响应型纳米凝胶封堵材料在pH=9时的凝胶状态图(放大3000倍)。
图1C为实施例1提供的pH响应型纳米凝胶封堵材料在pH=5时的凝胶状态图(放大100倍)。
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,现对本发明的技术方案进行以下详细说明,但不能理解为对本发明的可实施范围的限定。
实施例1
本实施例提供了一种pH响应型纳米凝胶封堵材料,该pH响应型纳米凝胶封堵材料通过以下步骤制备得到的:
1)制备丙烯酸类三元共聚物
将60质量份的甲基丙烯酸置于烧杯中,在冰水浴中边搅拌边缓慢滴加16质量份质量浓度为20%(以氢氧化钠溶液总质量为100%计)的氢氧化钠溶液,使甲基丙烯酸部分中和得到溶液A;待溶液A冷却至室温后加入20质量份的乙烯基三甲氧基硅烷、15质量份的羟甲基丙烯酰胺,混合均匀后通氮气30min,加入3质量份的偶氮二异丁酸二甲酯聚合;聚合反应完成后取出胶体产物剪碎,放入80℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用;
2)制备pH响应型纳米凝胶封堵材料
将去离子水70质量份、聚乙二醇(分子量17万,醇解度88%)10质量份、苯乙烯基吡啶15质量份混拌均匀10分钟后,加入聚氧乙烯醇3质量份、步骤1)制备得到的丙烯酸类三元共聚物30质量份,继续低速(80转/min)搅拌30分钟后成品;将成品放入50℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用。
实施例2
本实施例提供了一种pH响应型纳米凝胶封堵材料,该pH响应型纳米凝胶封堵材料通过以下步骤制备得到的:
1)制备丙烯酸类三元共聚物
将40质量份的甲基丙烯酸置于烧杯中,在冰水浴中边搅拌边缓慢滴加13质量份质量浓度为20%(以氢氧化钠溶液总质量为100%计)的氢氧化钠溶液,使甲基丙烯酸部分中和得到溶液A;待溶液A冷却至室温后加入30质量份的乙烯基三乙氧基硅烷、15质量份的醋酸乙烯酯,混合均匀后通氮气30min,加入5质量份的偶氮二异丁腈聚合;聚合反应完成后取出胶体产物剪碎,放入80℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用;
2)制备pH响应型纳米凝胶封堵材料
将去离子水60质量份、聚乙烯醇(分子量12万,醇解度78%)10质量份、4-苯乙烯基吡啶20质量份混拌均匀10分钟后,加入2质量份OP-7、步骤1)制备得到的丙烯酸类三元共聚物25质量份,继续低速(80转/min)搅拌30分钟后成品;将成品放入50℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用。
实施例3
本实施例提供了一种pH响应型纳米凝胶封堵材料,该pH响应型纳米凝胶封堵材料通过以下步骤制备得到的:
1)制备丙烯酸类三元共聚物
将50质量份的乙基丙烯酸置于烧杯中,在冰水浴中边搅拌边缓慢滴加18质量份质量浓度为20%(以氢氧化钠溶液总质量为100%计)的氢氧化钠溶液,部分中和得到溶液A;待溶液A冷却至室温后加入25质量份的γ-甲基丙稀酰氧基丙基三甲氧基硅烷、15质量份的丙烯腈,混合均匀后通氮气30min,加入5质量份的过硫酸钠聚合;聚合反应完成后取出胶体产物剪碎,放入80℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用;
2)制备pH响应型纳米凝胶封堵材料
将去离子水50质量份、聚己内酯多元醇(酸值21mgKOH/g,醇解度78%,分子量1万-4万)12质量份、苯乙烯基吡啶10质量份混拌均匀10分钟后,加入3质量份OP-9、步骤1)制备得到的丙烯酸类三元共聚物25质量份,继续低速(80转/min)搅拌30分钟后成品;将成品放入50℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用。
实施例4
本实施例提供了一种pH响应型纳米凝胶封堵材料,该pH响应型纳米凝胶封堵材料通过以下步骤制备得到的:
1)制备丙烯酸类三元共聚物
将55质量份的甲基丙烯酸羟乙酯置于烧杯中,在冰水浴中边搅拌边缓慢滴加17质量份质量浓度为20%(以氢氧化钠溶液总质量为100%计)的氢氧化钠溶液,部分中和得到溶液A;待溶液A冷却至室温后加入25质量份的乙烯基三异丙氧基硅烷、12质量份的氯乙烯,混合均匀后通氮气30min,加入5质量份的偶氮二异庚腈聚合;聚合反应完成后取出胶体产物剪碎,放入80℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用;
2)制备pH响应型纳米凝胶封堵材料
将去离子水60质量份、高聚合物聚乙烯醇(分子量20万,醇解度88%)2质量份、2-乙烯基吡啶10质量份混拌均匀10分钟后,加入2质量份聚氧乙烯醚:OP-10(体积比例为1:1)、步骤1)制备得到的丙烯酸类三元共聚物26质量份,继续低速(80转/min)搅拌30分钟后成品;将成品放入50℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用。
实施例5
本实施例提供了一种pH响应型纳米凝胶封堵材料,该pH响应型纳米凝胶封堵材料通过以下步骤制备得到的:
1)制备丙烯酸类三元共聚物
将40质量份的丙烯酸酯置于烧杯中,在冰水浴中边搅拌边缓慢滴加14质量份质量浓度为20%(以氢氧化钠溶液总质量为100%计)的氢氧化钠溶液,部分中和得到溶液A;待溶液A冷却至室温后加入25质量份的乙烯基三(2-甲氧基乙氧基)硅烷、15质量份的马来酸酐,混合均匀后通氮气30min,加入5质量份的异丙苯过氧化氢聚合;聚合反应完成后取出胶体产物剪碎,放入80℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用;
2)制备pH响应型纳米凝胶封堵材料
将去离子水50质量份、聚丙二醇(分子量14万,醇解度98%)15质量份、2-乙烯基吡啶10质量份混拌均匀10分钟后,加入2质量份OP-9、步骤1)制备得到的丙烯酸类三元共聚物25质量份,继续低速(80转/min)搅拌30分钟后成品;将成品放入50℃干燥箱中烘至恒重,粉碎、过100目筛,密封备用。
实验例
分别用盐酸、氢氧化钠调节配制不同pH的水溶液,分别称取一定质量的实施例1-实施例5制备得到的pH响应型纳米凝胶封堵材料放入其中,充分浸泡后,取出,用干滤纸擦去表面水分,称重,计算在不同pH值下的溶胀率。
实验结果如表1与图1A-图1C所示,pH在8-10的范围时,溶胀率在1-15g/g之间,pH值在4-6范围时,溶胀率在1000-1400g/g之间,瞬间溶胀100倍以上,聚集成团如图1C所示起到封堵的作用。
表1 PH响应型纳米凝胶在不同pH值情况下的平衡溶胀率
项目 | pH=10 | pH=9 | pH=8 | pH=7 | pH=6 | pH=5 | pH=4 |
实施例1封堵材料溶胀率(g/g) | 2 | 7 | 14 | 120 | 900 | 1200 | 1600 |
实施例2封堵材料溶胀率(g/g) | 3 | 6 | 10 | 145 | 1100 | 1400 | 1600 |
实施例3封堵材料溶胀率(g/g) | 2 | 8 | 12 | 110 | 1060 | 1250 | 1500 |
实施例4封堵材料溶胀率(g/g) | 2 | 6 | 15 | 122 | 1100 | 1400 | 1500 |
实施例5封堵材料溶胀率(g/g) | 1 | 7 | 17 | 138 | 1150 | 1200 | 1500 |
以上参照附图描述了本发明的优选实施方式。这些实施方式的许多特征和优点根据该详细的说明书是清楚的,因此权利要求旨在覆盖这些实施方式的落入其真实精神和范围内的所有这些特征和优点。此外,由于本领域的技术人员容易想到很多修改和改变,因此不是要将本发明的实施方式限于所例示和描述的精确结构和操作,而是可以涵盖落入其范围内的所有合适修改和等同物。
Claims (13)
1.一种pH响应型纳米凝胶封堵材料,其中,按照质量份数计,该pH响应型纳米凝胶封堵材料的原料包括:水50-70份,乳化剂2-3份,丙烯酸类三元共聚物25-35份,聚醇类化合物10-15份,乙烯基吡啶类化合物10-20份。
2.根据权利要求1所述的封堵材料,其中,所述乳化剂包括聚氧乙烯醇、聚氧乙烯醚、OP-7、OP-8、OP-9和OP-10中的一种或两种以上的组合。
3.根据权利要求1所述的封堵材料,其中,所述聚醇类化合物包括聚乙二醇、聚乙烯醇、聚丙二醇和聚己内酯多元醇中的一种或两种以上的组合。
4.根据权利要求1所述的封堵材料,其中,所述乙烯基吡啶类化合物包括反-4-芳乙烯基吡啶、2-乙烯基吡啶、苯乙烯基吡啶和4-苯乙烯基吡啶中的一种或两种以上的组合。
5.根据权利要求1所述的封堵材料,其中,所述丙烯酸类三元共聚物由第一单体、第二单体、第三单体聚合得到;其中,
所述第一单体包括甲基丙烯酸、乙基丙烯酸、丙烯酸酯和甲基丙烯酸羟乙酯中的一种或两种以上的组合;
所述第二单体包括乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三(2-甲氧基乙氧基)硅烷、乙烯基三异丙氧基硅烷和γ-甲基丙稀酰氧基丙基三甲氧基硅烷中的一种或两种以上的组合;
所述第三单体包括丙烯酰胺、羟甲基丙烯酰胺、苯乙烯、丙烯腈、氯乙烯、醋酸乙烯酯和马来酸酐中的一种或两种以上的组合。
6.根据权利要求5所述的封堵材料,其中,所述丙烯酸酯包括丙烯酸乙酯、丙烯酸丁酯、丙烯酸异辛酯、丙烯酸甲酯和甲基丙烯酸甲酯中的一种或两种以上的组合。
7.根据权利要求5或6所述的封堵材料,其中,以质量计,第一单体、第二单体、第三单体的用量比为40-60:20-30:10-15。
8.根据权利要求5-7任一项所述的封堵材料,其中,所述丙烯酸类三元共聚物通过下述方式制备得到:第一单体水溶液在冰水浴条件下加入氢氧化钠溶液,使第一单体部分中和得到溶液A;溶液A在室温条件下加入第二单体、第三单体,然后在惰性环境下加入引发剂进行聚合反应;聚合反应完成后将产物进行干燥粉碎,密封备用。
9.根据权利要求8所述的封堵材料,其中,所述引发剂包括偶氮二异丁酸二甲酯、偶氮二异丙基咪唑啉盐酸盐、偶氮二异丁腈、偶氮二异庚腈、过硫酸钾、过硫酸钠、过硫酸铵和异丙苯过氧化氢中的一种或两种以上的组合。
10.根据权利要求9所述的封堵材料,其中,以质量计,所述引发剂与第一单体、第二单体、第三单体的用量比为:1-5:40-60:20-30:10-15。
11.根据权利要求9所述的封堵材料,其中,所述水为去离子水。
12.权利要求1-11任一项所述的pH响应型纳米凝胶封堵材料的制备方法,其中,该方法包括:
将水、聚醇类化合物、乙烯基吡啶类化合物混合后,加入乳化剂、丙烯酸类三元共聚物搅拌均匀得到所述pH响应型纳米凝胶封堵材料。
13.权利要求1-11任一项所述的pH响应型纳米凝胶封堵材料在碱性钻井液中的应用。
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