Research on Preparation Technology of Temperature-Controlled Expansion Plugging Agent Based on Shape Memory Polymer
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摘要: 利用温度触发型的形状记忆材料制备温控膨胀堵漏剂，以实现堵漏液在裂缝中感应温度下的膨胀架桥。探讨了基于形状记忆聚合物型的温控膨胀堵漏剂制备工艺技术，利用低聚物树脂单体与不同高温交联剂在催化剂作用下，经不同温度和时间加热交联固化，脱模后热压成型以储备形变记忆功能，冷却后造粒制得。温控膨胀堵漏剂SDP，该堵漏玻璃化激活温度可调，粒径可调，抗拉强度大，高温高压膨胀量较大，在150 ℃、20 MPa老化后D90粒度增长率为44.71%～54.17%，能自适应裂缝架桥堵塞，经挤压变形，能够提高堵漏液的滞留能力和承压能力。Abstract: A kind of temperature-controlled expansion plugging agent based on temperature-triggered shape-memory material is prepared to achieve expansion bridging in fractured stratum after the temperature reaches the excitation temperature point. This paper discusses the preparation technology of the temperature-controlled expansion plugging agent. Firstly, an oligomer resin monomer and different high-temperature cross-linking agents are mixed to reaction by a catalyst under different heating temperature and time, then the mixture will be solidified through crosslinking. Secondly the reaction product after taking off the mold is pressed in the specific temperature in order to reserve deformation memory function. Finally the new polymer is crushed and granulated into various particle sizes according to demand at room temperature. The new plugging agent prepared has adjustable glass transition temperature, adjustable particle size, large compressive strength, large expansion at high temperature and high pressure, and the particle size growth rate of D90 after aging at 150 ℃ and 20 MPa is 44.71% ~ 54.17%. It can adapt to crack size to bridging, moreover, block leaking channels deformed by squeezing to improve the retention capacity and pressure endurance capacity of the plugging fluid.
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表 1 不同固化度下多元胺的用量
固化度/
%PJ1用量/
g多元胺/
g固化度/
%PJ1用量/
g多元胺/
g60 100 13.50 80 100 18.00 70 100 15.75 90 100 20.25 注：固化反应条件：90 ℃下加热4 h 
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表 2 单一反应温度对产品力学性能的影响
T/
℃抗拉强度/
MPa抗冲击强度/
MPaT/
℃抗拉强度/
MPa抗冲击强度/
MPa60 未固化 未固化 120 21.78 5.7 90 16.39 3.4 150 30.46 4.2
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表 3 复合反应温度对产品力学性能的影响
T/℃ 抗拉强度/MPa 抗冲击强度/MPa 110 32.87 15.3 130 40.19 20.5 150 46.27 17.2 注：固化反应条件为：90 ℃加热2 h后，然后在不同温度下加热2 h
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表 4 固化时间对产品转化温度和力学性能的影响
t/h 抗拉强度/MPa 抗冲击强度/MPa Tg/℃ 1 35.32 13.4 73.24 2 40.19 15.6 81.29 3 42.63 21.2 83.14 4 44.18 19.3 85.27 注：固化反应条件为：90 ℃加热2 h后，然后在130 ℃加热不同时间
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表 5 增韧剂加量对产品转化温度和力学性能影响
增韧剂/
%抗拉强度/
MPa抗冲击强度/
MPaTg/
℃0 40.19 21.2 83.14 5 36.78 24.3 70.43 10 30.43 26.2 63.29 15 21.65 22.7 51.37
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表 6 不同尺寸温控膨胀堵漏剂膨胀性能实验
粒径/
目T激活/
℃激活前/mm 激活后/mm △D50增
长率/%△D90增
长率/%D50 D90 D50 D90 10～20 72.86 2.48 3.12 3.41 4.81 37.50 54.17 20～40 88.90 1.42 1.98 1.91 2.98 34.50 50.50 40～80 102.35 0.60 0.85 0.80 1.23 33.33 44.71
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