The Synthesis and Application of an Environmentally Friendly High Temperature Graft Oligosaccharide Filter Loss Reducer
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摘要: 以淀粉衍生物低聚糖为原料,丙烯酰胺、2-丙烯酰胺-2-甲基丙磺酸和N-乙烯基吡咯烷酮为接枝单体,AIBN为引发剂,利用反相乳液法聚合得到低聚糖接枝物降滤失剂CG-FL。通过FTIR、扫描电镜、热失重分析等手段表征了接枝物结构,检测了低聚糖接枝物的生物毒性EC50、生物降解率及重金属离子含量,通过单剂对比测试、实验室配制环保钻井液对比测试及现场井浆性能测试,评价了低聚糖接枝物的钻井液性能。室内评价结果表明,低聚糖接枝物降滤失剂CG-FL抗温超过180 ℃,抗盐达15%,分散性和配伍性较好,性能优于对比产品。现场试验应用证明,加入CG-FL后能够降低钻井液滤失量,现场钻井液性能稳定,无起泡或者处理剂碳化现象发生。Abstract: A graft oligosaccharide filter loss reducer CG-FL was developed through inverse emulsion with starch derivative oligosaccharide as the raw material, acrylamide, 2-acrylamide-2-methapropyl sulfonic acid and N-vinyl pyrrolidone as the graft monomers and AIBN as the initiator. The molecular structure of the filter loss reducer CG-FL was characterized by FTIR, SEM and TGA etc. The biotoxicity EC50, biodegradation capacity and heavy metal contents of CG-FL were examined. The performance of CG-FL in drilling fluids was evaluated by performance comparison of single additive, performance comparison of different drilling fluids formulated in laboratory with CG-FL and other additives, as well as field application. Laboratory evaluation of CG-FL showed that CG-FL functions normally at temperatures up to 180 ℃, it is resistant to contamination by 15% salt. CG-FL has good dispersibility and compatibility with other additives. In comparison experiment, CG-FL showed better properties than the counter additives. Field application showed that CG-FL reduced the filtration rate of the drilling fluids, and the drilling fluids, after treatment, showed stable properties, no foaming or carbonization of the additive has occurred.
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表 1 低聚糖接枝物环保性能检测结果
检测项目 检测结果 指标 单位 检测方法 生物毒性
EC50>1×105 ≥30000 mg/L SY/T 6788—2020 总铬 13 ≤1000 mg/kg HJ 491—2019 总镍 <3 ≤200 mg/kg HJ 491—2019 总铜 <1 ≤1500 mg/kg HJ 491—2019 总锌 2 ≤3000 mg/kg HJ 491—2019 总铅 <10 ≤1000 mg/kg HJ 491—2019 总镉 <0.01 ≤15 mg/kg GB/T 17141—1997 总砷 <0.01 ≤75 mg/kg HJ 680—2013 生物降解率
BOD5/COD34 ≥5 % SY/T 6788—2020 表 2 不同降滤失剂单剂性能对比
降滤失剂 加量/
%AV/
mPa·sPV/
mPa·sYP/
PaFLAPI/
mLFLHTHP/
mLCG-FL 0 6.0 5.5 0.5 32.5 66.7 1.0 13.5 9.0 4.5 19.8 56.1 1.5 18.0 11.0 7.0 11.2 34.2 2.0 24.0 15.0 9.0 7.8 21.9 2.5 31.0 18.0 13.0 6.6 19.8 Driscal-D 0 6.0 5.0 1.0 33.0 66.4 1.0 11.5 9.0 2.5 20.9 44.2 1.5 17.5 12.0 5.5 15.3 35.8 2.0 22.0 13.0 9.0 9.9 29.1 2.5 29.5 18.0 11.5 7.2 25.9 POLYPAC R 0 5.5 5.0 0.5 32.8 67.0 1.0 24.5 15.0 9.5 17.5 65.9 1.5 31.0 19.0 12.0 13.4 64.1 2.0 44.5 25.0 19.5 8.9 55.4 2.5 65.0 38.0 27.0 6.8 45.9 注:在200 ℃老化16 h后测定性能;FLHTHP实验条件为3.5 MPa、150 ℃。 表 3 不同降滤失剂在盐水环保钻井液中的性能
降滤失剂 实验条件 AV/
mPa·sPV/
mPa·sYP/
PaGel/
Pa/PaFLAPI/
mLFLHTHP/
mL泥饼厚度/
mmζ/
mV空白 热滚前 30.5 23.0 7.5 1.50/4.50 11.5 68 8.5 −21.4 CG-FL 热滚前 61.5 41.0 20.5 2.00/11.50 4.5 −29.8 热滚后 44.5 34.0 10.5 1.00/6.00 3.3 17.2 2.0 −28.3 POLYPAC R 热滚前 33.5 24.0 9.5 3.50/7.50 4.0 −23.2 热滚后 16.5 16.5 0 0.25/0.75 3.8 36.4 4.0 −21.9 Driscal-D 热滚前 46.5 33.0 13.5 2.00/10.50 4.0 −27.9 热滚后 26.5 23.0 3.5 0.25/2.00 3.6 24.0 2.5 −27.1 注:FLHTHP实验条件为3.5 MPa、150 ℃;热滚条件为180 ℃、16 h;测试温度为50 ℃。 表 4 CG-FL降滤失剂在现场井浆中性能
钻井液 实验条件 ρ/
g·cm−3AV/
mPa·sPV/
mPa·sYP/
PaGel/
Pa/PaFLAPI/
mLFLHTHP/
mL泥饼厚度/
mm井浆+10 %水 50 ℃ 1.31 43.5 31 12.5 2.00/5.5 6.2 25.9 3.5 井浆+10 %水+2 %CG-FL 50 ℃ 1.31 51.5 36 15.5 2.00/9.5 4.5 180 ℃热滚16 h 1.31 44.5 34 10.5 1.00/6.0 3.3 17.2 2.5 180 ℃热滚48 h 1.32 37.5 30 7.5 1.25/6.5 2.7 15.8 2.0 180 ℃热滚72 h 1.32 40.0 32 8.0 1.25/6.5 2.9 15.0 2.0 注:FLHTHP实验条件为3.5 MPa、150 ℃。 表 5 应用井现场井浆性能
井深/
mCG-FL/
tFV/
sn K/
Pa·snGel/
Pa/PaAV/
mPa·sPV/
mPa·sYP/
PaFLAPI/
mLFLHTHP/
mL泥饼厚度/
mm4778 0 56 0.58 553 3.0/6.0 31.5 21.0 10.5 5.0 18.5 5.0 4815 5 59 0.52 612 4.5/9.5 33.0 20.0 13.0 4.0 14.5 3.0 4953 0 57 0.53 578 3.5/6.0 32.0 21.0 11.0 5.0 15.2 4.5 5116 6.9 60 0.55 552 3.0/7.0 32.5 22.0 10.5 5.0 13.2 3.5 5236 0 56 0.56 559 3.0/6.5 31.0 20.0 11.0 4.5 18.0 4.0 5450 5.0 58 0.55 599 4.0/7.0 31.5 19.5 12.0 4.0 14.0 3.0 注:FLHTHP在3.5 MPa、150 ℃下测定。 -
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