CN106916577B - 一种油井水泥温敏性缓释促凝剂 - Google Patents
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Abstract
本发明公开了一种油井水泥温敏性缓释促凝剂，通过以下组分采用油相分离法微胶囊技术制备而成，过程如下：在三角瓶中加入3‑5重量份硬脂酸、100‑125重量份有机溶剂，充分搅拌，70‑80℃水浴加热至硬脂酸充分溶解，再加入1‑3重量份聚乙二醇4000、1‑2重量份促凝材料，1‑3min后停止搅拌，超声波震荡10‑20min，使聚乙二醇4000和促凝材料均匀分散在溶液中，重新开始搅拌的同时逐步降温至35℃以下，过滤、常温干燥24h即得。本发明在水泥浆中性能稳定，到达预设温度点后缓慢释放，缓释性能良好，促凝剂释放后能够明显缩短深井、超深井候凝时间，有效解决深井、超深井的超缓凝问题，其制备方法简单，原料常见且成本低廉，易于推广，具有广阔的市场前景。
Description
技术领域
本发明属于油气田勘探开发中固井水泥浆领域，具体涉及一种新型温敏性缓释促凝剂。
背景技术
随着油田勘探开发向深井、超深井和复杂井方向发展，井底温度和压力不断升高，致使一次性上返封固段长，封固段顶部和底部温差大，基于固井工程对固井水泥浆的特殊要求，防止在深井、超深井固井作业中水泥浆在泵送过程中快速稠化和凝结，保证施工安全顺利进行，需在水泥浆中加入大量的缓凝剂以改善高温高压下水泥浆的稠化性能和流变性，但这就造成了深井、超深井长封固段顶部水泥浆超缓凝、候凝时间过长、增加工期的问题。
为解决此类问题，现有技术公开了多种合成聚合物类油井水泥缓凝剂，如中国专利“抗高温油井水泥缓凝剂及其制备方法”(CN101967371A)公开了一种2-丙烯酰胺基-2-甲基丙磺酸、衣康酸、丙烯酰胺和N，N-二甲基丙基丙烯酰胺四元共聚物缓凝剂，耐温能力达到180℃；中国专利“一种油气井固井高温缓凝剂及其制备方法”(CN101402849A)公开了一种2-丙烯酰胺基-2-甲基丙磺酸和衣康酸的二元共聚物，耐温能力达到200℃；也有国内学者将AMPS与IA共聚后，再与有机酸SA进行复配，得到对温度敏感性小的宽温带缓凝剂KH(陈大钧,余志勇,张颖,等.适合长封固段的宽温带缓凝剂的研制[J].钻井液与完井液,2012,29(1):63-65.)，适用温度范围60℃-150℃。
目前，虽然缓凝剂的耐温能力和温度敏感性(对宽温度范围的适应性)有了显著的提高，解决了长封固段一次性注水泥安全泵送的问题，但仍然无法解决深井、超深井长封固段顶部水泥浆超缓凝、候凝时间过长、增加工期的问题。
发明内容
本发明的目的在于提供一种油井水泥温敏性缓释促凝剂，该缓释促凝剂在水泥浆中性能稳定，到达预设温度点后缓慢释放，缓释性能良好，促凝剂释放后能够明显缩短深井、超深井候凝时间，有效解决深井、超深井的超缓凝问题(长封固段顶部水泥浆超缓凝、候凝时间过长、增加工期的问题)，缩短建井周期，节约建井成本，其制备方法简单，原料常见且成本低廉，易于推广，具有广阔的市场前景。
为达到以上技术目的，本发明提供以下技术方案。
一种油井水泥温敏性缓释促凝剂，通过以下组分采用油相分离法微胶囊技术制备而成，过程如下：在三角瓶中加入3-5重量份硬脂酸、100-125重量份有机溶剂，充分搅拌，70-80℃水浴加热至硬脂酸充分溶解，再加入1-3重量份聚乙二醇4000、1-2重量份促凝材料，1-3min后停止搅拌，超声波震荡10-20min，使聚乙二醇4000和促凝材料均匀分散在溶液中，重新开始搅拌的同时逐步降温至35℃以下，过滤、常温干燥24h即得。
所述有机溶剂为无水乙醇、苯、氯仿或四氯化碳。
所述促凝材料包括盐酸盐类(如氯化钙、氯化钠)、硫酸盐类(如硫酸钠、硫酸钾或硫酸钙)、硝酸盐类和亚硝酸盐类(如亚硝酸钙、硝酸钙)及以上多类复合型促凝材料。
硬脂酸的熔点是56-70℃，加热溶于无水乙醇，在聚乙二醇4000乳化和机械搅拌的作用下，分散相与连续相向两相内部乳化界面移动，降温析出的硬脂酸包覆在不溶于无水乙醇的氯化钙小颗粒周围，形成微胶囊结构的温敏性缓释促凝剂。
与现有技术相比，本发明具有以下有益效果：
(1)本发明温敏性缓释促凝剂包衣为硬脂酸，不溶于水、耐碱且有较高的机械强度，在水泥浆中性能稳定，不会出现泄漏导致过早稠化、从而改变流变性的现象，不影响配浆、打浆。
(2)本发明温敏性缓释促凝剂到达预设温度80-90℃时能缓慢释放，水泥浆上返到位后，促凝剂发挥作用，明显缩短深井、超深井(长封固段顶部水泥浆)侯凝时间，节约成本。
(3)本发明温敏性缓释促凝剂使用方便，与常规外加剂的加入方式相同，不需特殊的加入方式。
(4)本发明温敏性缓释促凝剂制备工艺简单，原料常见且成本低廉，有实现工业化生产的可能性。
具体实施方式
下面结合具体实施例对本发明温敏性缓释促凝剂的实施方式、特征、功效及其配制方法进行详细说明。
实施例1
一种油井水泥温敏性缓释促凝剂，制备过程如下：
在三角瓶中加入5重量份硬脂酸、100重量份无水乙醇，充分搅拌，75℃水浴加热至硬脂酸充分溶解，再加入1.5重量份聚乙二醇4000、1.5重量份氯化钙，3min后停止搅拌，超声波震荡20min，使聚乙二醇4000和氯化钙均匀分散在溶液中，重新开始搅拌的同时降温至35℃以下，过滤，常温干燥24h即得。
实施例2
(1)水泥浆配置与性能测试
按照油井水泥浆制备的现行标准——GB/T19139-2012《油井水泥试验方法》制备漂珠低密度水泥浆，并测试其常规工程性能，结果见表1。
空白样：油井水泥100份，25份3M漂珠，25份微硅，5份降失水剂(2-丙烯酰胺-2-甲基丙磺酸)，3份缓凝剂(木质素磺酸钠)，混合搅拌均匀即得干混材料；1份分散剂(聚苯乙烯磺酸钠)，0.2份的消泡剂(二甲基硅油)溶于44份水中搅拌均匀，即得湿混材料；在4000转/min转速的搅拌条件下，将干混材料匀速加入湿混材料中(用时15s)，然后以12000转/min的转速搅拌35s并消泡，即得到对比组水泥浆体系。
配方1：在空白样的基础上增加缓释促凝剂0.3份。
配方2：在空白样的基础上增加缓释促凝剂0.6份。
表1空白样、配方1、配方2的水泥浆综合性能
注：API失水条件为90℃×7.1MPa×30min
常温稠化条件为30℃×15MPa×5min
高温稠化条件为100℃×60MPa×40min
(2)水泥石抗压强度测试
将配置好的水泥浆倒入钢模中置于水浴锅中养护，养护至测试龄期。将养护好的水泥石试样通过液压式万能试验机测试抗压强度。养护温度为30℃的水泥石养护时间为24h、36h；养护温度为60℃、90℃的水泥石养护时间为24h、72h。结果见表2。
表2空白样、配方1、配方2在不同温度下的抗压强度
注：30℃抗压强度测试时，先将水泥浆升温至90℃再降温至30℃
由表1、表2可明显看出，温敏性缓释促凝剂不影响水泥浆流动性、失水量、游离液、常温稠化时间、水泥石抗压强度等常规工程性能，由此可推断出温敏性缓释促凝剂在水泥浆中能够稳定存在。
水泥石养护温度为30℃时，采取先将水泥浆升温至90℃再降温至30℃的措施，是为了达到缓释促凝剂生效的温度点，缓慢释放微胶囊内部促凝剂，从表2中30℃的抗压强度对比以及表1中高温条件下稠化时间的变化可以看出，只有当温度达到预设的作用温度点后才开始缓慢释放内部的促凝剂，从而加快水泥浆稠化时间，解决大温差长封固段顶部水泥浆超缓凝的问题。
以上所述仅是为了便于本领域的技术人员理解本发明的技术方案，并不能用以限制本发明。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (2)
1.一种油井水泥温敏性缓释促凝剂，通过以下组分采用油相分离法微胶囊技术制备而成，过程如下：在三角瓶中加入3-5重量份硬脂酸、100-125重量份有机溶剂，充分搅拌，70-80℃水浴加热至硬脂酸充分溶解，再加入1-3重量份聚乙二醇4000、1-2重量份促凝材料，1-3min后停止搅拌，超声波震荡10-20min，使聚乙二醇4000和促凝材料均匀分散在溶液中，重新开始搅拌的同时逐步降温至35℃以下，过滤、常温干燥24h即得；所述促凝材料包括盐酸盐类、硫酸盐类、硝酸盐类、亚硝酸盐类及以上多类复合型促凝材料。
2.如权利要求1所述的一种油井水泥温敏性缓释促凝剂，其特征在于，所述有机溶剂为无水乙醇、苯、氯仿或四氯化碳。
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