CN104099073B - 一种磷酸钙水泥降失水剂 - Google Patents

一种磷酸钙水泥降失水剂 Download PDF

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CN104099073B
CN104099073B CN201310114159.1A CN201310114159A CN104099073B CN 104099073 B CN104099073 B CN 104099073B CN 201310114159 A CN201310114159 A CN 201310114159A CN 104099073 B CN104099073 B CN 104099073B
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曾建国
孙富全
吕光明
高永会
李鹏晓
王翀
邹建龙
刘爱萍
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China National Petroleum Corp
CNPC Offshore Engineering Co Ltd
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Abstract

本发明涉及一种磷酸钙水泥降失水剂；是一种五元共聚物，该五元共聚物的共聚单体为不饱和的酰胺单体、2‑丙烯酰胺基‑2‑甲基丙磺酸、一元不饱和羧酸、亚甲基双丙烯酰胺和烯丙基聚氧乙烯醚；五种单体按重量份比为：不饱和的酰胺单体为20～50份，2‑丙烯酰胺基‑2‑甲基丙磺酸为30～50份，一元不饱和羧酸为1～10份，亚甲基双丙烯酰胺为0.05～0.5份，烯丙基聚氧乙烯醚1～20份；本磷酸钙水泥降失水剂在50～150℃将磷酸钙水泥浆的失水量控制在50ml/30min以内。

Description

一种磷酸钙水泥降失水剂
技术领域
本发明涉及一种油气井固井用水泥外加剂，具体的是一种磷酸钙水泥的降失水剂。
背景技术
文献（US5,900,053,US6,796,378以及2012年固井技术研讨会论文集，108-116页）研究表明，通过酸碱反应制备的磷酸钙水泥作为一种耐CO2腐蚀的特种水泥，可用于含CO2腐蚀气体的油气田固井。但是，在固井施工时，磷酸钙水泥浆在压力下经过高渗透地层时将发生“渗滤”，水泥浆滤液大量进入地层，导致水泥浆流动性变差，危及施工安全，甚至造成固井事故。同时，滤液进入储层会对储层形成不同程度的伤害。因此，通常在固井作业时需要使用降失水剂。
磷酸钙水泥作为一种非硅酸盐基的化学结合材料，其表面性质与水化过程与硅酸盐基的油井水泥差别大，因此，常见的适用硅酸盐水泥的降失水剂对磷酸钙水泥浆失水控制能力较差。美国专利（US6,846,357B2）报道，在82.2℃（180℉）下，占水泥重量1%的降失水剂羟乙基纤维素、羧甲基羟乙基纤维素、淀粉按API（美国石油协会）标准测试的失水量均为1200ml/30min。此外，在硅酸盐油井水泥浆体系应用效果良好的丙烯酰胺/2-丙烯酰胺基-2-甲基丙磺酸/丙烯酸三元共聚物、丙烯酰胺/2-丙烯酰胺基-2-甲基丙磺酸/丙烯酸/马来酸酐四元共聚物均不能有效的控制磷酸钙水泥浆的失水。而在固井作业中，一般要求水泥浆的失水量不超过250ml/30min，特殊情况下（如尾管固井），要求水泥浆的失水量不超过50ml/30min。
发明内容
本发明的目的是提供一种适用于磷酸钙水泥的降失水剂，将本降失水剂添加到磷酸钙水泥浆中，可以在50～150℃范围内将水泥浆的失水量控制在50ml/30min以内。
本发明所述的磷酸钙水泥降失水剂是一种五元共聚物，该五元共聚物的共聚单体为不饱和酰胺、2-丙烯酰胺基-2-甲基丙磺酸、一元不饱和羧酸、亚甲基双丙烯酰胺和烯丙基聚氧乙烯醚；五种单体的按重量份为：不饱和酰胺单体为20～50份，2-丙烯酰胺基-2-甲基丙磺酸为30～50份，一元不饱和羧酸为1～10份，亚甲基双丙烯酰胺为0.05～0.5份，烯丙基聚氧乙烯醚为1～20份。
较好的五元共聚物磷酸钙水泥降失水剂五种单体按重量份为：不饱和的酰胺单体为30～50份，2-丙烯酰胺基-2-甲基丙磺酸为30～50份，一元不饱和羧酸为2～8份，亚甲基双丙烯酰胺为0.1～0.5份，烯丙基聚氧乙烯醚3～15份。
所述的不饱和酰胺单体为丙烯酰胺和N,N’－二甲基丙烯酰胺的一种。
所述的一元不饱和羧酸单体为丙烯酸和甲基丙烯酸的一种。
所述的烯丙基聚氧乙烯醚单体为CH2=C(R)CH2O(CH2CH2O)nH，其中，R为甲基或氢，n值的范围为5～20，较好的n值范围为6～12。
本发明的有益效果：本发明提供的降失水剂加入到磷酸钙水泥浆中，水泥浆在50～150℃范围内失水量在50ml/30min以内。采用本发明降失水剂对磷酸钙水泥浆体系的失水控制能力显著优于市售的羟乙基纤维素、羧甲基羟乙基纤维素、聚乙烯醇、丙烯酰胺/2-丙烯酰胺基-2-甲基丙磺酸/丙烯酸三元共聚物、丙烯酰胺/2-丙烯酰胺基-2-甲基丙磺酸/丙烯酸/马来酸酐四元共聚物以及中国专利（ZL200810226689.4）报道的降失水剂。此外，在同等条件下，本发明提供的降失水剂的失水控制能力优于美国专利（US6,846,357B2）报道的由3-氯-2-羟基三甲基氯化铵醚化淀粉而形成的阳离子淀粉（见表4）。
具体实施方式
按表1和表2配方称取丙烯酰胺（或N,N’－二甲基丙烯酰胺）、2-丙烯酰胺基-2-甲基丙磺酸、（甲基）丙烯酸、亚甲基双丙烯酰胺、烯丙基聚氧乙烯醚以及氢氧化钠溶于去离子水中，然后将上述溶液加入到四口瓶反应器内，并保持搅拌（转速170rpm）,在氮气保护下升温至75℃，加入10g重量浓度为10%的过硫酸铵溶液引发聚合反应，75℃下恒温反应4h，得到五元共聚物溶液，产物经干燥、粉碎制成粉剂。
表1磷酸钙水泥降失水剂配方
表2对比试验配方
按GB/T19139-2003标准制备水泥浆，并按该标准评价表1和对比试验配方中的1#-16#样品的失水量、游离水量和抗压强度。由于国内不存在商品化的由酸碱反应制备的磷酸钙水泥，本发明中磷酸钙水泥配方为：铝酸盐水泥（CA60）100+多聚磷酸钠10.5+粉煤灰100，以下同。评价降失水剂配方：100份磷酸钙水泥+1份本发明的降失水剂+1份缓凝剂酒石酸+1份缓凝剂柠檬酸+45份水。实验结果如表3所示。考虑到9#-16#样品在50℃时具有较差的控制失水能力，因此，没必要开展更高温度的失水量、游离水量和抗压强度实验。
表3合成降失水剂性能实验结果
从表3可以得出结论:
（1）本发明提供的降失水剂1#-8#样品在50～150℃内可将失水量控制在50ml/30min以内，水泥浆游离液少，水泥石抗压强度大于14MPa，有利于提高固井质量。
（2）按同样合成工艺合成的对比试验9#-16#样品不能有效的控制磷酸盐水泥浆体系失水量。
将7#样品与市售的油井水泥降失水剂羟乙基纤维素、羧甲基羟乙基纤维素、聚乙烯醇、丙烯酰胺/2-丙烯酰胺基-2-甲基丙磺酸/丙烯酸共聚物、丙烯酰胺/2-丙烯酰胺基-2-甲基丙磺酸/丙烯酸/马来酸酐共聚物以及按ZL200810226689.4实施例1-4合成的样品（分别记为17#、18#，19#和20#）进行同等条件下性能比较试验（按GB/T19139-2003进行失水试验），实验配方：100份磷酸钙水泥+1份降失水剂+1份缓凝剂酒石酸+1份缓凝剂柠檬酸+45份水。试验结果如表4所示。
表4本发明提供的降失水剂与常见的降失水剂性能对比试验结果
*为美国专利（US6,846,357B2）报道数据。
从表4可以得出结论，本发明提供的磷酸钙降失水剂对水泥浆的失水控制能力优于表4所列的其它类型的降失水剂。

Claims (1)

1.一种磷酸钙水泥降失水剂，是一种五元共聚物，其特征在于：该五元共聚物的共聚单体为不饱和的酰胺单体、2-丙烯酰胺基-2-甲基丙磺酸、一元不饱和羧酸、亚甲基双丙烯酰胺和烯丙基聚氧乙烯醚；五种单体按重量份比为：不饱和的酰胺单体为20～40份，2-丙烯酰胺基-2-甲基丙磺酸为30～40份，一元不饱和羧酸为1～10份，亚甲基双丙烯酰胺为0.05～0.1份，烯丙基聚氧乙烯醚1～11.9份；
所述的不饱和的酰胺单体为丙烯酰胺和N,N’－二甲基丙烯酰胺的一种；
所述的一元不饱和羧酸单体为丙烯酸和甲基丙烯酸的一种；
所述的烯丙基聚氧乙烯醚单体为CH2＝C(R)CH2O(CH2CH2O)nH，其中，R为甲基或氢，n值的范围为6～12。
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