Synthesis and Properties of an Early-Strength Retarder Based on AMPS
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摘要: 随着油气开采深度的增加，长封固段温度梯度过大，为保证水泥浆的安全泵送，需要加入大量油井水泥缓凝剂，这会导致水泥浆在井口低温段出现超缓凝、强度发展缓慢等问题，严重影响固井质量和安全。针对现有问题，基于吸附理论选择AMPS、MA、NVP、DEAA四种单体合成一种耐高温早强型缓凝剂AMND，并通过红外光谱、热稳定性测试、凝胶色谱分析、高温高压稠化等方法对缓凝剂的结构和性能进行测试。测试结果表明：缓凝剂AMND高温稠化性能优异，在150℃高温条件下水泥浆稠化时间可达316 min；缓凝剂AMND具有优异的调凝性以及较低的温度敏感性与加量敏感性，能够调节不同温度段的稠化时间，有利于水泥浆在固井施工现场的安全泵送；对水泥石力学发展影响较小，在150℃循环温度、60℃养护条件下，1 d、2 d、3 d强度分别可达6.34、8.24、14.66 MPa，满足固井施工强度要求。结论认为该缓凝剂能够缓解低温段超缓凝现象，实现高温井底缓凝，且不影响井口强度发展，成功缓解大温差长封固段井超缓凝或者不凝的难题，具有很好的应用前景。Abstract: With the increase in the depth of oil and gas exploitation, the temperature gradient in the long cementing section becomes increasingly larger. To ensure the safe pumping of cement slurries, a large amount of oil well cement retarder needs to be added, resulting in problems such as super-retardation and slow strength development of the cement slurries in the low-temperature section at the wellhead, which in turn seriously affecting the quality and safety of cementing operations. To deal with these problems, a high-temperature resistant and early-strength type retarder AMND was synthesized with four monomers, namely AMPS, MA, NVP and DEAA, based on the adsorption theory. The molecular structure and performance of the retarder were tested by methods such as infrared spectroscopy, thermal stability testing, gel permeation chromatography analysis and high temperature and high pressure thickening. The test results show that: 1) the retarder AMND has excellent thickening performance at high temperatures; the thickening time of the cement slurry can reach 316 minutes at 150℃, 2) AMND has excellent setting control performance, as well as low temperature sensitivity and dosage sensitivity. It can adjust the thickening time in different temperature ranges, which is beneficial to the safe pumping of the cement slurry at the well site, 3) it has little impact on the mechanical development of the set cement. At a circulating temperature of 150℃ and a curing temperature of 60℃, the strengths of the set cement at 1 day, 2 days, and 3 days can reach 6.34 MPa, 8.24 MPa, and 14.66 MPa respectively, satisfying the strength requirements for cementing operations. The conclusion is that this retarder can alleviate the super-retardation phenomenon in the low-temperature condition, achieve retardation at high bottom hole temperatures, and does not affect the development of the strength of the cement at the wellhead. It has successfully mitigated the super-retardation or non-setting problems in wells with large temperature differences and long cementing sections, and has a very good application prospect.
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表 1 合成缓凝剂的正交实验结果
序号 A B C D t稠化/
min单体质量比 T反应/℃ 引发剂/% pH 1 6.50︰2.00︰1.25︰0.25 55 0.8 4 292 2 6.50︰2.00︰1.25︰0.25 60 1.0 5 303 3 6.50︰2.00︰1.25︰0.25 65 1.2 6 299 4 6.75︰1.75︰1.25︰0.25 55 1.2 6 305 5 6.75︰1.75︰1.25︰0.25 60 1.0 5 316 6 6.75︰1.75︰1.25︰0.25 65 0.8 4 310 7 7.00︰1.50︰1.25︰0.25 55 1.0 4 269 8 7.00︰1.50︰1.25︰0.25 60 0.8 6 276 9 7.00︰1.50︰1.25︰0.25 65 1.2 5 221 K1 298 289 293 299 K2 310 298 296 280 K3 255 277 272 293 R 55 22 24 19 最佳
水平A2 B2 C2 D1 注：单体质量比为AMPS︰MA︰NVP︰DEAA；K1、K2、K3分别为水平一、水平二、水平三条件下的平均稠化时间；R是同种因素条件下各水平之间的极差。 
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表 2 不同缓凝剂对水泥石顶部强度的影响
缓凝剂 加量/
%t稠化/
min70℃养护强度/MPa 1 d 2 d 3 d GH-9L 1.6 291 7.02 14.50 SD210 2.2 322 10.04 AMND 2.0 276 11.44 16.36 18.96 注：实验条件为125℃×60 MPa。
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表 3 缓凝剂对不同温度段抗压强度的影响
AMND/
%T稠化/
℃P稠化/
MPaT养护/
℃△T/
℃p1 d/
MPap2 d/
MPap3 d/
MPa3 150 75 60 90 6.34 8.24 14.66 3 150 75 70 80 6.46 9.56 15.28 3 150 75 90 60 7.06 12.54 19.92 3 140 70 60 80 6.90 10.18 15.24 3 140 70 70 70 7.74 12.74 15.44 3 140 70 90 50 7.96 16.66 17.92 3 130 65 60 70 8.24 10.42 16.10 3 130 65 70 60 9.36 14.90 17.68 3 130 65 90 40 9.46 17.96 18.44 2 120 60 60 60 9.05 11.82 18.10 2 120 60 70 50 11.00 16.22 18.48 2 120 60 90 30 12.98 18.66 22.44 1 110 55 60 50 10.40 12.48 18.34 1 110 55 70 40 11.46 16.96 19.62 1 110 55 90 20 15.78 19.26 25.80
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