CN107129560A - 一种颗粒暂堵剂的制备方法 - Google Patents
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Abstract
本发明涉及一种颗粒暂堵剂的制备方法,属于油田开采技术领域。本发明首先将玉米淀粉、茯苓多糖等进行搅拌混合,并在低温下滴加氢氧化钠溶液进行反应后,滴加氯乙酸溶液进行加热混合并过滤,将滤液进行透析后浓缩,得到浓缩液,接着将浓缩液与无水乙醇在低温下混合并过滤,将滤渣干燥后,与水等进行混合,得混合液A,再以丙烯酸、氨水等为原料进行混合,得混合液B,并将其加入混合液A中,同时加入表面活性剂等,制得粘稠液,最后将粘稠液降温放置后干燥并粉碎即可。本发明制备的暂堵剂耐温性能好,在高温条件下具有较好的封堵效果,同时大大提高了封堵层的强度,具有广阔的应用前景。
Description
技术领域
本发明涉及一种颗粒暂堵剂的制备方法,属于油田开采技术领域。
背景技术
随着大批成熟油田陆续进入枯产期,即使是经过注水开发也仅能获得25~35%的地下原油,油层中仍有大量未动用的储层或动用程度较低的油层存在。注水开采不仅采收效率低,而且随着注水油田的长期不断开发,进入开发中后期阶段以后,出现油田综合含水率上升,修井、压井、冲砂等作业频繁,修井液漏入地层造成污染,以及油田开采效益逐年变差等严重问题。因此,大多数油田采取通过对作业井某些层面进行短期暂堵,从而对目的层原油进行开采,以提高原油的采收率。
目前所采用的暂堵剂有水溶性暂堵剂,其中水溶性暂堵剂多为高分子聚合物的复配产物,其使用时优先进入不含油的孔道,即使有少量进入含油的孔道,也难自行解堵,而且使用的无固相盐水滤失量大,对设备管线腐蚀性也较大。同时水溶性暂堵剂溶解速度快,不适合温度高120℃的油井环境,温度高导致暂堵剂的封堵性降低等,无法发挥正常的封堵作用,强度也会大大降低,导致堵水作业的失败,最终影响石油产出量。
发明内容
本发明所要解决的技术问题:针对传统的暂堵剂在高温油井环境下,封堵性能降低,无法发挥正常的封堵作用,且封堵强度降低,影响堵水作用的问题,提供了一个颗粒暂堵剂的制备方法。
为解决技术问题,本发明采用的技术方案是:
(1)称取玉米淀粉、茯苓多糖、纤维素和异丙醇加入三口烧瓶中,在低温下向三口烧瓶中滴加氢氧化钠溶液,搅拌反应后将三口烧瓶置于室温下,加入氯乙酸溶液,加热反应,反应后冷却,出料,得反应物,将反应物过滤得反应液;
(2)用盐酸调节反应液pH值为7.0,将调节后的反应液置于透析袋中透析,得透析液,旋转蒸发得浓缩液,将浓缩液与无水乙醇混合,低温放置后过滤得滤渣,并干燥,得干燥物;
(3)称取干燥物和去离子水加入反应釜中,加热后加入过硫酸铵溶液,搅拌得混合液A,备用;
(4)称取丙烯酸和氨水加入烧杯中,向烧杯中加入丙烯酰胺和N,N'-亚甲基双丙烯酸胺,搅拌后得混合液B;
(5)将混合液B滴加到步骤(4)备用的混合液A中,滴加结束后加热反应得反应物,向反应物中加入醇醚磺基琥珀酸单酯二钠盐、十二烷基硫酸钠和L-乳酸,并设置反应釜的温度和真空度,搅拌反应,出料,得粘稠液;
(6)将粘稠液降温后密封放置,得冻胶,将冻胶干燥,粉碎,过筛,收集颗粒,即可得到耐高温高强度颗粒暂堵剂。
本发明与其他方法相比,有益技术效果是:
(1)本发明将玉米淀粉、茯苓多糖和纤维素混合后进行羧甲基化处理,经过羧甲基化处理后得到具有水溶性增稠物,再将水溶性增稠物在引发剂和交联剂的作用下与丙烯酸和丙烯酰胺进行交联反应,交联得到的产物中加入表面活性剂和L-乳酸,在减压和高温条件下L-乳酸会进行脱水反应,生成L-乳酸低聚物,并进一步与丙烯酰胺交联产物进行反应,从而可以提高丙烯酰胺交联产物的耐高温性能和强度,使用传统的水溶性暂堵剂耐温温度达到80~120℃,本发明制备的颗粒暂堵剂耐温温度达到125~190℃,在暂堵层厚度为3~4cm时,使用传统的水溶性暂堵剂使得暂堵层强度达到2~4MPa,本发明制备的颗粒暂堵剂使得暂堵层强度达到5~8MPa;
(2)本发明在交联反应物中加入表面活性剂,其目的是为了提高反应产物的分散性和亲水性,有利于操作使用;
(3)本发明反应得到的粘稠液,降温放置一段时间后,粘稠液内部会形成网状的结构,即为冻胶,最后将冻胶干燥粉碎成颗粒,便于携带使用。
具体实施方式
本发明所需要的原料有:玉米淀粉、茯苓多糖、纤维素、异丙醇、质量分数20%氢氧化钠溶液、质量分数15%氯乙酸溶液、蒸馏水、去离子水、过硫酸铵溶液、丙烯酸、质量分数8%氨水、丙烯酰胺、N,N'-亚甲基双丙烯酸胺、醇醚磺基琥珀酸单酯二钠盐、十二烷基硫酸钠和L-乳酸。
分别称取10~15g玉米淀粉、20~30g茯苓多糖、15~20g纤维素和120~140g异丙醇加入三口烧瓶中,并将三口烧瓶置于水浴锅中,在3~5℃下向三口烧瓶中滴加60~80g质量分数20%氢氧化钠溶液,控制滴加速度为2~4g/min,滴加同时以400~500r/min转速进行搅拌,待滴加结束后继续搅拌反应50~70min,反应后将三口烧瓶移出水浴锅并置于室温下,再向三口烧瓶中滴加70~80g质量分数15%氯乙酸溶液,控制滴加速度为3~5g/min,滴加后将三口烧瓶移入水浴锅中,在60~80℃和400~500r/min条件下搅拌反应2~4h,反应后冷却至室温并出料,得反应液,得到的反应液是利用氯乙酸溶液对玉米淀粉、茯苓多糖和纤维素进行羧甲基化改性,用质量分数10%盐酸调节反应液pH值为7.0,将调节后的反应液置于截留分子量为12000~15000Da的透析袋中,使用蒸馏水透析2~4天后收集透析液,并将透析液在40~50℃下旋转蒸发30~40min,收集得浓缩液后置于烧杯中,再向烧杯中加入浓缩液质量4~6倍无水乙醇,搅拌混合10~20min后将烧杯置于冰箱中,在3~5℃条件下放置8~10h,放置后过滤得滤渣,将滤渣在-30~-20℃下冷冻干燥20~30min,得干燥物,将羧甲基化改性后得到反应液进行提纯和浓缩,得浓缩液后加入无水乙醇中进行醇沉,醇沉得到水溶性增稠物,分别称取10~12g干燥物和100~120g去离子水加入反应釜中,并设置反应釜温度为40~45℃,保温搅拌10~15min后向反应釜中加入3~5g质量分数3%过硫酸铵溶液,搅拌5~10min得混合液A,向水溶性增稠物中加入引发剂,其目的是为了得到待反应的水溶性增稠物,分别称取60~70g丙烯酸和20~25g质量分数8%氨水加入烧杯中,搅拌混合5~10min后向烧杯中加入5~7g丙烯酰胺和0.1~0.3gN,N'-亚甲基双丙烯酸胺,搅拌混合5~10min后得混合液B,混合液B是由交联剂和交联单体混合,将混合液B滴加到混合液A中,控制滴加速度为1~3g/min,滴加结束后在60~80℃下搅拌反应1~3h,反应结束后得交联反应物,向交联反应物中依次加入1~3g醇醚磺基琥珀酸单酯二钠盐、2~4g十二烷基硫酸钠和40~50gL-乳酸,并设置反应釜温度为100~110℃,真空度为0.02~0.04MPa,搅拌20~30min后出料,得粘稠液,水溶性增稠物在交联剂和引发剂的作用下进行交联反应,得到的交联反应物与脱水得到的L-乳酸低聚物进一步进行反应,得到粘稠液,将粘稠液置于烧杯中,于10~15℃温度下密封放置80~100min,得冻胶,将冻胶放入真空干燥箱中,在100~105℃下干燥8~10h,干燥后粉碎,过50~60目筛,收集过筛颗粒,即可得到颗粒暂堵剂。
实例1
分别称取15g玉米淀粉、30g茯苓多糖、20g纤维素和140g异丙醇加入三口烧瓶中,并将三口烧瓶置于水浴锅中,在5℃下向三口烧瓶中滴加80g质量分数20%氢氧化钠溶液,控制滴加速度为4g/min,滴加同时以500r/min转速进行搅拌,待滴加结束后继续搅拌反应70min,反应后将三口烧瓶移出水浴锅并置于室温下,再向三口烧瓶中滴加80g质量分数15%氯乙酸溶液,控制滴加速度为5g/min,滴加后将三口烧瓶移入水浴锅中,在80℃和500r/min条件下搅拌反应4h,反应后冷却至室温并出料,得反应液,再用质量分数10%盐酸调节反应液pH值为7.0,将调节后的反应液置于截留分子量为12000Da的透析袋中,使用蒸馏水透析4天后收集透析液,并将透析液在50℃下旋转蒸发40min,收集得浓缩液后置于烧杯中,再向烧杯中加入浓缩液质量6倍无水乙醇,搅拌混合20min后将烧杯置于冰箱中,在5℃条件下放置10h,放置后过滤得滤渣,将滤渣-20℃下冷冻干燥30min,得干燥物,分别称取12g干燥物和120g去离子水加入反应釜中,并设置反应釜温度为45℃,保温搅拌15min后向反应釜中加入5g质量分数3%过硫酸铵溶液,搅拌10min得混合液A,分别称取70g丙烯酸和25g质量分数8%氨水加入烧杯中,搅拌混合10min后向烧杯中加入7g丙烯酰胺和0.3gN,N'-亚甲基双丙烯酸胺,搅拌混合10min后得混合液B,将混合液B滴加到混合液A中,控制滴加速度为3g/min,滴加结束后在80℃下搅拌反应3h,反应结束后得交联反应物,向交联反应物中依次加入3g醇醚磺基琥珀酸单酯二钠盐、4g十二烷基硫酸钠和50gL-乳酸,并设置反应釜温度为110℃,真空度为0.04MPa,搅拌30min后出料,得粘稠液,将粘稠液置于烧杯中,于15℃温度下密封放置100min,得冻胶,将冻胶放入真空干燥箱中,在105℃下干燥10h,干燥后粉碎,过60目筛,收集过筛颗粒,即可得到颗粒暂堵剂。
实例2
分别称取10g玉米淀粉、20g茯苓多糖、15g纤维素和120g异丙醇加入三口烧瓶中,并将三口烧瓶置于水浴锅中,在3℃下向三口烧瓶中滴加60g质量分数20%氢氧化钠溶液,控制滴加速度为2g/min,滴加同时以400r/min转速进行搅拌,待滴加结束后继续搅拌反应50min,反应后将三口烧瓶移出水浴锅并置于室温下,再向三口烧瓶中滴加70g质量分数15%氯乙酸溶液,控制滴加速度为3g/min,滴加后将三口烧瓶移入水浴锅中,在60℃和400r/min条件下搅拌反应2h,反应后冷却至室温并出料,得反应液,再用质量分数10%盐酸调节反应液pH值为7.0,将调节后的反应液置于截留分子量为12000Da的透析袋中,使用蒸馏水透析2天后收集透析液,并将透析液在40℃下旋转蒸发30min,收集得浓缩液后置于烧杯中,再向烧杯中加入浓缩液质量4倍无水乙醇,搅拌混合10min后将烧杯置于冰箱中,在3℃条件下放置8h,放置后过滤得滤渣,将滤渣在-30℃下冷冻干燥20min,得干燥物,分别称取10g干燥物和100g去离子水加入反应釜中,并设置反应釜温度为40℃,保温搅拌10min后向反应釜中加入3g质量分数3%过硫酸铵溶液,搅拌5min得混合液A,分别称取60g丙烯酸和20g质量分数8%氨水加入烧杯中,搅拌混合5min后向烧杯中加入5g丙烯酰胺和0.1gN,N'-亚甲基双丙烯酸胺,搅拌混合5min后得混合液B,将混合液B滴加到混合液A中,控制滴加速度为1g/min,滴加结束后在60℃下搅拌反应1h,反应结束后得交联反应物,向交联反应物中依次加入1g醇醚磺基琥珀酸单酯二钠盐、2g十二烷基硫酸钠和40gL-乳酸,并设置反应釜温度为100℃,真空度为0.02MPa,搅拌20min后出料,得粘稠液,将粘稠液置于烧杯中,于10℃温度下密封放置80min,得冻胶,将冻胶放入真空干燥箱中,在100℃下干燥8h,干燥后粉碎,过50目筛,收集过筛颗粒,即可得到颗粒暂堵剂。
实例3
分别称取12g玉米淀粉、25g茯苓多糖、17g纤维素和130g异丙醇加入三口烧瓶中,并将三口烧瓶置于水浴锅中,在4℃下向三口烧瓶中滴加80g质量分数20%氢氧化钠溶液,控制滴加速度为3g/min,滴加同时以450r/min转速进行搅拌,待滴加结束后继续搅拌反应60min,反应后将三口烧瓶移出水浴锅并置于室温下,再向三口烧瓶中滴加75g质量分数15%氯乙酸溶液,控制滴加速度为4g/min,滴加后将三口烧瓶移入水浴锅中,在70℃和450r/min条件下搅拌反应3h,反应后冷却至室温并出料,得反应液,再用质量分数10%盐酸调节反应液pH值为7.0,将调节后的反应液置于截留分子量为13000Da的透析袋中,使用蒸馏水透析3天后收集透析液,并将透析液在45℃下旋转蒸发35min,收集得浓缩液后置于烧杯中,再向烧杯中加入浓缩液质量5倍无水乙醇,搅拌混合15min后将烧杯置于冰箱中,在4℃条件下放置9h,放置后过滤得滤渣,将滤渣在-25℃下冷冻干燥25min,得干燥物,分别称取11g干燥物和105g去离子水加入反应釜中,并设置反应釜温度为42℃,保温搅拌12min后向反应釜中加入4g质量分数3%过硫酸铵溶液,搅拌7min得混合液A,分别称取65g丙烯酸和23g质量分数8%氨水加入烧杯中,搅拌混合7min后向烧杯中加入6g丙烯酰胺和0.2gN,N'-亚甲基双丙烯酸胺,搅拌混合7min后得混合液B,将混合液B滴加到混合液A中,控制滴加速度为2g/min,滴加结束后在70℃下搅拌反应2h,反应结束后得交联反应物,向交联反应物中依次加入2g醇醚磺基琥珀酸单酯二钠盐、3g十二烷基硫酸钠和45gL-乳酸,并设置反应釜温度为105℃,真空度为0.03MPa,搅拌25min后出料,得粘稠液,将粘稠液置于烧杯中,于12℃温度下密封放置90min,得冻胶,将冻胶放入真空干燥箱中,在102℃下干燥9h,干燥后粉碎,过55目筛,收集过筛颗粒,即可得到颗粒暂堵剂。
Claims (7)
1.一种颗粒暂堵剂的制备方法,其特征在于具体制备步骤为:
(1)称取玉米淀粉、茯苓多糖、纤维素和异丙醇加入三口烧瓶中,在低温下向三口烧瓶中滴加氢氧化钠溶液,搅拌反应后将三口烧瓶置于室温下,加入氯乙酸溶液,加热反应,反应后冷却,出料,得反应物,将反应物过滤得反应液;
(2)用盐酸调节反应液pH值为7.0,将调节后的反应液置于透析袋中透析,得透析液,旋转蒸发得浓缩液,将浓缩液与无水乙醇混合,低温放置后过滤得滤渣,并干燥,得干燥物;
称取干燥物和去离子水加入反应釜中,加热后加入过硫酸铵溶液,搅拌得混合液A,备用;
称取丙烯酸和氨水加入烧杯中,向烧杯中加入丙烯酰胺和N,N'-亚甲基双丙烯酸胺,搅拌后得混合液B;
(3)将混合液B滴加到步骤(3)备用的混合液A中,滴加结束后加热反应得反应物,向反应物中加入醇醚磺基琥珀酸单酯二钠盐、十二烷基硫酸钠和L-乳酸,并设置反应釜的温度和真空度,搅拌反应,出料,得粘稠液;
(4)将粘稠液降温后密封放置,得冻胶,将冻胶干燥,粉碎,过筛,收集颗粒,即可得到颗粒暂堵剂。
2.根据权利要求1所述的一种颗粒暂堵剂的制备方法,其特征在于:所述的步骤(1)中低温温度为3~5℃,氯乙酸溶液为质量分数15%氯乙酸溶液,加热反应温度为60~80℃。
3.根据权利要求1所述的一种颗粒暂堵剂的制备方法,其特征在于:所述的步骤(2)中透析袋的截留分子量为12000~15000Da,使用蒸馏水进行透析,低温放置的温度为3~5℃。
4.根据权利要求1所述的一种颗粒暂堵剂的制备方法,其特征在于:所述的步骤(3)中加热温度为40~45℃,过硫酸铵溶液是为质量分数3%过硫酸铵溶液。
5.根据权利要求1所述的一种颗粒暂堵剂的制备方法,其特征在于:所述的步骤(4)中氨水为质量分数8%氨水。
6.根据权利要求1所述的一种颗粒暂堵剂的制备方法,其特征在于:所述的步骤(5)中加热反应的温度为60~80℃,反应釜的温度为100~110℃,反应釜的真空度为0.02~0.04MPa。
7.根据权利要求1所述的一种颗粒暂堵剂的制备方法,其特征在于:所述的步骤(6)中降温的温度为10~15℃,密封放置的时间为80~100min,过筛后的目数为50~60目。
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