Preparation of A 240 ℃ Cement Slurry Filter Loss Reducer Prepared through Thermal Initiation Polymerization
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摘要: 针对现有水泥浆降失水剂耐高温性能不足的问题，以高温热引发聚合方法替代传统水溶液引发剂聚合方法，设计并合成了抗温为240 ℃的三元水泥浆降失水剂HTFLA-A。通过实验确定了HTFLA-A的最佳合成条件：水与单体总质量比1∶1，控制温度为150 ℃，体系pH值为9，反应时间为32 h。并采用红外光谱（FT-IR）、热重分析（DSC/TGA）及核磁共振谱对HTFLA-A进行了表征。结果表明，HTFLA-A为目标预期产物，在439 ℃时的热失重仅为23.80%，这是由于高温合成过程中去除了单体中不稳定结构和有机合成过程中副反应产物,提升了高分子材料的抗温性能。对HTFLA-A的性能评价结果表明，当HTFLA-A加量为1.2%，可将水泥浆在180 ～ 240 ℃、6.9 MPa时API失水量控制在50 mL以内。Abstract: A terpolymer cement slurry filter loss reducer HTFLA-A is developed to deal with the poor thermal stability of the cement slurry filter loss reducers presently in use. HTFLA-A is designed and synthesized through high temperature thermally induced polymerization instead of the conventional water solution initiation polymerization. HTFLA-A works normally at temperatures up to 240 ℃. The optimal synthesis condition of HTFLA-A is: mass ratio of water to the monomers is 1:1, reaction temperature is 150 ℃, pH of the reaction system is 9, and the reaction time is 32 h. The molecular structure of HTFLA-A is characterized with FT-IR, DSC/TGA and NMR. The results of the study show that the final synthesis product HTFLA-A is the expected product. Weight loss on heating of HTFLA-A at 439 ℃ is only 23.80%. The reason for this low weight loss on heating is because in the high temperature synthesis, the unstable structures in the monomer molecules and the by-products of the synthesis process are all removed from the final product, thus improving the high temperature stability of the target product. Performance evaluation of HTFLA-A shows that at a concentration of 1.2%, HTFLA-A can control the API filtration rate of a cement slurry to below 50 mL at test condition of 180-240 ℃ and 6.9 MPa.
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表 1 不同温度下AMPS/AM/SSS三元聚合物分子量的变化
T/ ℃ t聚合/h 分子量/104 Da FLAPI /mL 100 48 41 13.0 110 45 44 13.0 120 43 49 10.4 130 39 54 10.0 140 36 65 7.0 150 34 72 5.8 160 33 70 5.6 170 32 71 5.6 180 29 68 5.8 190 26 64 6.8 200 24 58 9.6 
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