Research on a Nano-Composite Cement Slurry System Suitable for Low-Temperature Formations
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摘要: 为解决低温地层钻探过程中的井壁坍塌和井漏问题，研制了适用于低温地层的纳米复合水泥浆。采用宏观试验与微观分析相结合的方法，研究了低温下纳米Al2O3对硅酸盐–硫铝酸盐复合水泥浆性能和水化过程的影响；以普通硅酸盐水泥与硫铝酸盐水泥复合产生的水化协同效应为基础，结合纳米Al2O3、防冻剂EG、减水剂JS-1和早强剂TEOA，配制了纳米复合水泥浆NAC；采用扫描电镜、X射线衍射和水化放热试验相结合的方法，研究了NAC的低温水化过程及水化机理。试验得知，温度为–9 ℃时，纳米复合水泥浆具有良好的初始流动性，可泵期为57 min，初、终凝时间分别为84和101 min，24 h抗压强度为6.9 MPa。研究结果表明，NAC具有直角稠化效应，低温下性能优越，能够满足钻进低温地层时的护壁堵漏要求。Abstract: In order to solve the problems of borehole wall collapse and well leakage in low-temperature drilling, a nano-composite cement slurry system suitable for low-temperature formations was designed. Combining the macroscopic test with microscopic analysis, the influence of nano-Al2O3 at low temperatures on the performance of silicate-sulphoaluminate composite cement slurry and the hydration process was studied. Based on the synergistic effect of hydration generated from the composite of ordinary silicate cement and sulphoaluminate cement, a nano-composite cement (NAC) was developed in conjunction with the nano-Al2O3, antifreeze agent EG, water reducing agent JS-1, and hardening accelerating agent TEOA. In addition, the low-temperature hydration process of NAC and its mechanism were studied through a combination of the scanning electron microscope (SEM), X-ray diffraction (XRD), and exothermic experiments of hydration. Experimental results showed that the nano-composite cement slurry had good initial fluidity at −9 ℃ with a pumpable period of 57 min, a 24-hour compressive strength of 6.9 MPa, and an initial and final setting time of 84 min and 101 min, respectively. The results of the study indicated that NAC had the right-angle thickening effect and superior performance at low temperatures, capable of meeting the requirements of borehole wall protection and loss circulation control in low-temperature formations.
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图 1 NAC与CC浆液的流动性与泵送时间对比
Figure 1. Comparison of the fluidity and pumping time of NAC and composite cement（CC）slurry
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图 2 NAC与CC在不同低温下黏度变化特性对比
Figure 2. Comparison of viscosity change characteristics of NAC and CC slurry at different low temperatures
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图 3 不同养护时间下NAC和CC样品的SEM对比
Figure 3. SEM comparison of NAC and CC samples at different curing times
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图 4 NAC养护不同时间后放大不同倍数的SEM图
Figure 4. SEM image of NAC at different magnifications after different curing times
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图 5 NAC和CC养护不同时间的XRD分析结果
Figure 5. XRD analysis of NAC and CC at different curing times
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图 6 水泥浆水化过程中的放热曲线
Figure 6. Hydration exothermic curves in the hydration process of cement slurry
表 1 纳米Al2O3对复合水泥浆性能的影响试验结果
Table 1 The effect of nano Al2O3 on the properties of composite cement slurry
纳米Al2O3
加量，%初始流动度/
cm可泵期/
min初凝时间/
min终凝时间/
min24 h抗压
强度/MPa0 21 26 40 106 3.3 0.1 23 38 65 119 5.7 0.3 22 29 51 99 6.2 0.5 20 13 50 97 5.8 
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表 2 减水剂对纳米复合水泥浆性能的影响试验结果
Table 2 The effect of water reducing agent on the properties of nano-composite cement slurry
减水剂 加量，
%初始流动度/
cm可泵期/
min初凝时间/
min终凝时间/
min22.0 29 51 99 JS-1 0.1 27.0 43 144 197 0.3 35.0 103 265 354 0.5 33.0 89 186 246 NS 0.1 26.0 97 224 641 0.3 27.0 168 1 143 1 472 0.5 29.0 229 957 1 383 PAS 0.1 28.0 53 212 517 0.3 32.0 79 267 678 0.5 34.5 81 186 450
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表 3 早强剂对纳米复合水泥浆性能的影响试验结果
Table 3 The effect of hardening accelerating agent on the properties of nano-composite cement slurry
早强剂 加量，
%初始流动
度/cm可泵期/
min初凝时
间/min终凝时
间/min24 h抗压
强度/MPa33.0 89 186 246 6.1 TEOA 0.02 32.0 75 114 135 7.8 0.06 30.0 67 94 105 8.2 0.10 33.0 81 126 172 7.6 CaCl2 1.00 32.0 184 329 457 4.6 3.00 29.5 104 231 351 5.1 5.00 30.0 117 273 364 4.8 Na2SO4 0.50 31.5 52 77 96 6.3 1.50 31.0 43 72 99 6.5 2.50 30.5 37 64 89 6.7
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表 4 NAC的正交试验结果(–9 ℃)
Table 4 Results of orthogonal test of NAC (–9 ℃)
序号 A B C D 初始流动度/cm 可泵期/min 凝结时间/min 24 h抗压强度/MPa 初凝 终凝 1 0.5 0.2% 0.05% 0.4% 27.0 52 88 121 9.3 2 0.5 0.3% 0.06% 0.5% 31.0 53 159 208 9.1 3 0.5 0.4% 0.07% 0.6% 29.5 63 75 89 9.4 4 0.6 0.2% 0.06% 0.6% 31.0 60 139 219 7.7 5 0.6 0.3% 0.07% 0.4% 30.5 58 80 154 8.1 6 0.6 0.4% 0.05% 0.5% 30.5 60 144 238 8.8 7 0.7 0.2% 0.07% 0.5% 35.0 92 156 231 6.8 8 0.7 0.3% 0.05% 0.6% 33.0 75 178 234 7.3 9 0.7 0.4% 0.06% 0.4% 31.0 52 199 226 7.5
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