CN116751336B - 一种耐温的乳液型压裂液稠化剂的制备方法 - Google Patents
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Abstract
本发明涉及压裂液技术领域,且公开了一种耐温的乳液型压裂液稠化剂的制备方法,本发明利用含有二烯基的3,5‑二丙烯基醚苯基苯酰亚胺作为交联剂,与丙烯酰胺、甲基丙烯酸甲酯,通过反相乳液聚合法,进行自交联聚合,得到耐温的乳液型压裂液稠化剂,将酰亚胺基团接枝到稠化剂中,形成的压裂液具有疏水缔合作用,提高了压裂液的粘度;并且酰亚胺基团具有刚性大,耐热性强,有利于提高压裂液的耐高温性能和抗剪切性能,经过3,5‑二丙烯基醚苯基苯酰亚胺自交联,形成的稠化剂具有交联网络结构,结构稳定性好,耐盐性优良。
Description
技术领域
本发明涉及压裂液技术领域,具体为一种耐温的乳液型压裂液稠化剂的制备方法。
背景技术
压裂液在石油化工领域有着广泛的应用,压裂液油田开采和施工过程中可以起到传递压力、形成裂缝等效果,因此需要压裂液在地层温度下需要保持一定的粘度,其中稠化剂是压裂液的重要组成部分,可以起到提高粘度,提供交接基团等作用,对压裂液的性能影响很大。目前压裂液主要有瓜尔胶类压裂液、聚丙烯酰胺类压裂液、表面活性剂压裂液等。聚丙烯酰胺类压裂液具有成本低廉,分子结构可设计等优点,具有广泛的实际应用,但是聚丙烯酰胺类压裂液存在耐温性、耐盐性、耐剪切性等性能的较差的问题,阻碍了其在石油化工和油田开采等领域的发展。文献《疏水缔合型两性聚丙烯酰胺增稠剂的制备及性能研究》,以N,N'-亚甲基双丙烯酰胺为交联剂,丙烯酸十八酯为长碳链疏水单体与丙烯酰胺、甲基丙烯酰氧乙基三甲基氯化铵等单体进行反相乳液聚合,得到疏水缔合型两性增稠剂,其综合增稠效果最佳;但是该增稠剂的耐高温性和耐剪切性不佳。
发明内容
本发明解决如下技术问题:制备了一种耐温的乳液型压裂液稠化剂,解决了传统乳液型压裂液稠化剂耐温性和耐盐性不佳的问题。
本发明通过的技术方案如下:
一种耐温的乳液型压裂液稠化剂,按照如下工艺进行制备:
S1、向白油中加入表面活性剂,高速搅拌得到油相;
S2、向水中加入反应单体:丙烯酰胺、甲基丙烯酸甲酯和3,5-二烯丙基醚苯基苯酰亚胺,高速搅拌得到水相;所述3,5-二烯丙基醚苯基苯酰亚胺的结构式为
;
S3、将水相滴加进油相中并搅拌均匀,然后在氮气气氛中加入过硫酸铵、亚硫酸氢钠,反应后,冷却,得到耐温的乳液型压裂液稠化剂。
优选的,所述表面活性剂为司盘60、司盘80或吐温80的任一种或组合。
优选的,所述S2中各反应单体的比例为丙烯酰胺:甲基丙烯酸甲酯:3,5-二烯丙基醚苯基苯酰亚胺:=1mol:(0.15-0.4)mol:(0.08-0.2)mol。
优选的,所述S3中过硫酸铵和亚硫酸氢钠的摩尔用量分别是各反应单体总摩尔量的0.5%-0.8%和0.3%-0.45%。
优选的,所述S3中反应在60-70℃的温度搅拌进行2-5h。
优选的,所述3,5-二烯丙基醚苯基苯酰亚胺按照如下工艺进行制备: (1)向二甲亚砜中加入邻苯二甲酸酐和5-氨基间苯二酚,氮气气氛中搅拌反应2-4h,然后在120-150℃的温度下,搅拌反应18-24h,冷却,加入水和乙酸乙酯,萃取后将乙酸乙酯相减压浓缩,丙酮洗涤产物,干燥,得到二羟基苯酰亚胺中间体; (2)向四氢呋喃中加入二羟基苯酰亚胺中间体、3-溴丙烯和碳酸钾,反应后冷却,减压浓缩,丙酮洗涤产物,干燥,得到3,5-二烯丙基醚苯基苯酰亚胺。
优选的,所述(1)中各反应物的比例为邻苯二甲酸酐:5-氨基间苯二酚=1mol:(1.1-1.3)mol。
优选的,所述(2)中各反应物的比例为二羟基苯酰亚胺中间体、3-溴丙烯和碳酸钾1: (9-12):(10-15)。
优选的,所述(2)中反应在65-75℃的温度下回流72-96h。
本发明具有如下技术效果:本发明利用含有二烯基的3,5-二烯丙基醚苯基苯酰亚胺作为交联剂,与丙烯酰胺、甲基丙烯酸甲酯,通过反相乳液聚合法,进行自交联聚合,得到耐
温的乳液型压裂液稠化剂,将酰亚胺基团接枝到稠化剂中,形成的压裂液具有疏水缔合作用,
提高了压裂液的粘度;并且酰亚胺基团具有刚性大,耐热性强,有利于提高压裂液的耐高温性能和抗剪切性能,经过3,5-二烯丙基醚苯基苯酰亚胺自交联,形成的稠化剂具有交联网络结构,结构稳定性好,耐盐性优良。
具体实施方式
实施例1
向150mL的二甲亚砜中加入10mmol的邻苯二甲酸酐和13mmol的5-氨基间苯二酚,氮气气氛中搅拌反应4h,然后在120℃的温度下,搅拌反应20h,冷却,加入水和乙酸乙酯,萃取
后将乙酸乙酯相减压浓缩,丙酮洗涤产物,干燥,得到二羟基苯酰亚胺中间体;
向200mL的四氢呋喃中加入5mmol二羟基苯酰亚胺中间体、45mmol的3-溴丙烯和62mmol碳酸钾,在65℃的温度下回流72h,冷却,减压浓缩,丙酮洗涤产物,干燥,得到
3,5-二烯丙基醚苯基苯酰亚胺;
向8mL的白油中加入0.15mL的表面活性剂司盘60和0.1mL的吐温80,高速搅拌得到油相;
向10mL的水中加入反应单体:50mmol丙烯酰胺、20mmol甲基丙烯酸甲酯和4mmol3,5-二
烯丙基醚苯基苯酰亚胺,高速搅拌得到水相;
将水相滴加进油相中并搅拌均匀,然后在氮气气氛中加入各反应单体总摩尔量的0.37mmol的过硫酸铵、0.22mmol的亚硫酸氢钠,在65℃的温度搅拌反应4h,冷却,得到耐温的乳液型压裂液稠化剂。
实施例2
向100mL的二甲亚砜中加入10mmol的邻苯二甲酸酐和12mmol的5-氨基间苯二酚,氮气气氛中搅拌反应4h,然后在130℃的温度下,搅拌反应24h,冷却,加入水和乙酸乙酯,萃取后将乙酸乙酯相减压浓缩,丙酮洗涤产物,干燥,得到二羟基苯酰亚胺中间体。
向300mL的四氢呋喃中加入5mmol二羟基苯酰亚胺中间体、60mmol的3-溴丙烯和75mmol碳酸钾,在65℃的温度下回流96h,冷却,减压浓缩,丙酮洗涤产物,干燥,得到3,5-二烯丙基醚苯基苯酰亚胺。
向15mL的白油中加入0.3mL的表面活性剂司盘60和0.2mL的吐温80,高速搅拌得到油相;
向20mL的水中加入反应单体:50mmol丙烯酰胺、15mmol甲基丙烯酸甲酯和6mmol3,5-二烯丙基醚苯基苯酰亚胺,高速搅拌得到水相;
将水相滴加进油相中并搅拌均匀,然后在氮气气氛中加入各反应单体总摩尔量的0.45mmol的过硫酸铵、0.28mmol的亚硫酸氢钠,在60℃的温度搅拌反应4h,冷却,得到耐温的乳液型压裂液稠化剂。
实施例3
向200mL的二甲亚砜中加入10mmol的邻苯二甲酸酐和13mmol的5-氨基间苯二酚,氮气气氛中搅拌反应2h,然后在150℃的温度下,搅拌反应18h,冷却,加入水和乙酸乙酯,萃取后将乙酸乙酯相减压浓缩,丙酮洗涤产物,干燥,得到二羟基苯酰亚胺中间体。
向200mL的四氢呋喃中加入5mmol二羟基苯酰亚胺中间体、50mmol的3-溴丙烯和50mmol碳酸钾,在70℃的温度下回流96h,冷却,减压浓缩,丙酮洗涤产物,干燥,得到3,5-二烯丙基醚苯基苯酰亚胺。
向10mL的白油中加入0.2mL的表面活性剂司盘80和0.15mL的吐温80,高速搅拌得到油相;
向15mL的水中加入反应单体:50mmol丙烯酰胺、12mmol甲基丙烯酸甲酯和8mmol3,5-二烯丙基醚苯基苯酰亚胺,高速搅拌得到水相;
将水相滴加进油相中并搅拌均匀,然后在氮气气氛中加入各反应单体总摩尔量的0.56mmol的过硫酸铵、0.32mmol的亚硫酸氢钠,在70℃的温度搅拌反应4h,冷却,得到耐温的乳液型压裂液稠化剂。
实施例4
向150mL的二甲亚砜中加入10mmol的邻苯二甲酸酐和12mmol的5-氨基间苯二酚,氮气气氛中搅拌反应3h,然后在150℃的温度下,搅拌反应18h,冷却,加入水和乙酸乙酯,萃取后将乙酸乙酯相减压浓缩,丙酮洗涤产物,干燥,得到二羟基苯酰亚胺中间体。
向300mL的四氢呋喃中加入5mmol二羟基苯酰亚胺中间体、60mmol的3-溴丙烯和62mmol碳酸钾,在75℃的温度下回流72h,冷却,减压浓缩,丙酮洗涤产物,干燥,得到3,5-二烯丙基醚苯基苯酰亚胺。
向15mL的白油中加入0.3mL的表面活性剂司盘60和0.2mL的吐温80,高速搅拌得到油相;
向15mL的水中加入反应单体:50mmol丙烯酰胺、7.5mmol甲基丙烯酸甲酯和10mmol3,5-二烯丙基醚苯基苯酰亚胺,高速搅拌得到水相;
将水相滴加进油相中并搅拌均匀,然后在氮气气氛中加入各反应单体总摩尔量的0.5mmol的过硫酸铵、0.28mmol的亚硫酸氢钠,在70℃的温度搅拌反应2h,冷却,得到耐温的乳液型压裂液稠化剂。
对比例1:和实施例3的区别在于,不加入3,5-二烯丙基醚苯基苯酰亚胺,制备得到乳液型压裂液稠化剂。
分别将实施例和对比例制备的耐温的乳液型压裂液稠化剂或乳液型压裂液稠化剂加入到水中,配置成不同固含量的压裂液。
压裂液的性能参考SY/T5107-2016进行测试。
表1压裂液黏度测试
将压裂液在不同温度下进行剪切,控制剪切速率为200s-1,剪切时间30min,测定粘度。测试结果如下表:
表2压裂液高温黏度测试
向压裂液中加入氯化钠,控制压裂液中氯化钠的质量分数为0.2%,在不同温度下进行剪切,控制剪切速率为200s-1,剪切时间30min。测试结果如下表:
表3压裂液耐盐性能测试
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 (8)
1.一种耐温的乳液型压裂液稠化剂的制备方法,其特征在于,所述耐温的乳液型压裂液稠化剂按照如下工艺进行制备:
S1、向白油中加入表面活性剂,高速搅拌得到油相;
S2、向水中加入反应单体:丙烯酰胺、甲基丙烯酸甲酯和3,5-二烯丙基醚苯基苯酰亚胺,高
速搅拌得到水相;所述3,5-二烯丙基醚苯基苯酰亚胺的结构式为
;
S3、将水相滴加进油相中并搅拌均匀,然后在氮气气氛中加入过硫酸铵、亚硫酸氢钠,反应后,冷却,得到耐温的乳液型压裂液稠化剂;
其中,所述S2中各反应单体的比例为丙烯酰胺:甲基丙烯酸甲酯:3,5-二烯丙基醚苯基苯酰亚胺:=1mol:(0.15-0.4)mol:(0.08-0.2)mol。
2.根据权利要求1所述的耐温的乳液型压裂液稠化剂的制备方法,其特征在于,所述表面活性剂为司盘60、司盘80或吐温80的任一种或组合。
3.根据权利要求1所述的耐温的乳液型压裂液稠化剂的制备方法,其特征在于,所述S3中过硫酸铵和亚硫酸氢钠的摩尔用量分别是各反应单体总摩尔量的0.5%-0.8%和0.3%-0.45%。
4.根据权利要求1所述的耐温的乳液型压裂液稠化剂的制备方法,其特征在于,所述S3中反应在60-70℃的温度搅拌进行2-5h。
5.根据权利要求1所述的耐温的乳液型压裂液稠化剂的制备方法,其特征在于,所述3,5-二烯丙基醚苯基苯酰亚胺按照如下工艺进行制备:
(1)向二甲亚砜中加入邻苯二甲酸酐和5-氨基间苯二酚,氮气气氛中搅拌反应2-4h,然后在120-150℃的温度下,搅拌反应18-24h,冷却,加入水和乙酸乙酯,萃取后将乙酸乙酯
相减压浓缩,丙酮洗涤产物,干燥,得到二羟基苯酰亚胺中间体;
(2)向四氢呋喃中加入二羟基苯酰亚胺中间体、3-溴丙烯和碳酸钾,反应后冷却,减压浓缩,丙酮洗涤产物,干燥,得到3,5-二烯丙基醚苯基苯酰亚胺。
6.根据权利要求5所述的耐温的乳液型压裂液稠化剂的制备方法,其特征在于,所述(1)中各反应物的比例为邻苯二甲酸酐:5-氨基间苯二酚=1mol:(1.1-1.3)mol。
7.根据权利要求5所述的耐温的乳液型压裂液稠化剂的制备方法,其特征在于,所述(2)中各反应物的比例为二羟基苯酰亚胺中间体、3-溴丙烯和碳酸钾1:(9-12):(10-15)。
8.根据权利要求5所述的耐温的乳液型压裂液稠化剂的制备方法,其特征在于,所述(2)中反应在65-75℃的温度下回流72-96h。
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