Synthesis and Evaluation of a High Temperature Salt-Resistant Chain Polymer Filter Loss Reducer
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摘要: 针对深井钻探中钻井液处理剂抗温抗复合盐性能不足的问题，以丙烯酰胺（AM）、2-丙烯酰胺-2-甲基丙磺酸（AMPS）、N-乙烯基己内酰胺（NVCL）、二甲基二烯丙基氯化铵（DMDAAC）、烯丙醇聚氧乙烯醚（APEG）为单体，以过硫酸钾和亚硫酸氢钠作为氧化还原体系进行自由基共聚反应，合成了一种支链型聚合物降滤失剂（PAANDA）。通过实验优化确定了最优合成条件为：n（AM）∶n（AMPS）∶n（NVCL）∶n（DMDAAC）∶n（APEG）=50∶20∶5∶10∶15，反应温度为50 ℃，反应时间为4 h，引发剂用量为0.3%。利用傅里叶红外光谱（FT-IR）和核磁共振氢谱（1H- NMR）确定了聚合产物的分子结构，通过热重分析（TGA）测得PAANDA 热分解温度大于300 ℃，表明其具有良好的热稳定性。同时，应用于水基钻井液中，进一步评价PAANDA 对水基钻井液流变和滤失性能的影响。结果显示，当PAANDA 加量为2.0%时，180 ℃老化后API滤失量为4.0 mL，高温高压滤失量为22.6 mL（180 ℃），同时具有抗复合盐能力，抗盐钙能力优于国外同类产品 Driscal D。Abstract: A branched polymer filter loss reducer PAANDA has been developed to deal with the problems of poor high-temperature stability and poor salt resistance encountered in deep well drilling. Monomers used for the synthesis include acrylamide (AM), 2-acrylamide-2-methyl propane sulfonic acid (AMPS), N-vinyl caprolactam (NVCL), dimethyl diallyl ammonium chloride (DMDAAC) and allyl alcohol polyoxyethylene ether (APEG). Potassium persulphate and sodium bisulphite was used as a redox system for the radical polymerization reaction. Laboratory experiment was conducted to determine the optimum ratio of the raw reaction materials and optimum reaction conditions ad follows:n （AM）∶ n （AMPS）∶ n （NVCL）∶ n （DMDAAC）∶ n （APEG） = 50 : 20 : 5 : 10 : 15, reaction temperature = 50 °C, reaction time = 4 hours, concentration of the initiator = 0.3%. Using FTIR and 1H-NMR, the molecular structure of the polymerization product was determined. TGA analysis showed that the PAANDA filter loss reducer degrades at above 300 °C, indicating that the product has excellent thermal stability. The filtration control property of PAANDA was evaluated in water-based drilling fluids. It was found that at a water-based drilling fluid treated with 2.0% PAANDA has API filter loss of 4.0 mL and HTHP filter loss of 22.6 mL tested at 180 °C after aging the fluid at 180 °C. The PAANDA also performed better than Driscal D in resisting contamination from compound salts and calcium.
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表 1 单体物质的量比对聚合物降滤失性能的影响
AM∶AMPS∶NVCL∶
DMDAAC∶APEGAV/
mPa·sPV/
mPa·sYP/
PaFLAPI/
mL50∶20∶10∶10∶10 12.0 7.5 4.5 13.5 40∶20∶10∶10∶20 11.5 8.5 3.0 16.2 50∶20∶5∶10∶15 13.5 9.0 4.5 10.5 50∶20∶15∶10∶5 16.0 10.5 5.5 12.8 
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表 2 在不同反应条件下的PAANDA性能
引发剂/
%T反应/
℃t反应/
h黏均分子量/
g·mol-1FLAPI/
mL0.2 60 6 1.1×105 10.8 0.3 60 6 1.3×105 9.7 0.4 60 6 8.5×104 11.2 0.3 50 6 1.5×105 8.9 0.3 40 6 7.0×104 11.4 0.3 50 5 1.6×105 8.6 0.3 50 4 1.6×105 8.0 0.3 50 3 9.2×104 10.2
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表 3 降滤失剂PAANDA加量对淡水基浆的影响
PAANDA/
%AV/
mPa·sPV/
mPa·sYP/
PaFLAPI/
mLFLHTHP/
mL0 4.0 3.0 1.0 48.0 82.0 0.5 9.0 8.0 1.0 15.8 34.2 1.0 18.0 14.0 4.0 8.0 30.6 1.5 29.5 24.0 5.5 5.4 25.8 2.0 41.5 31.0 10.5 3.0 21.6 2.5 57.0 37.0 20.0 2.9 21.0 3.0 76.0 42.0 34.0 2.9 20.8 注：老化条件为160 ℃、16 h。
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表 4 不同老化温度下含2%PAANDA淡水钻井液的性能
T老化/
℃AV/
mPa·sPV/
mPa·sYP/
PaFLAPI/
mLFLHTHP/
mL室温 48.0 28.0 20.0 2.5 150 46.5 28.0 17.5 2.8 20.8 160 41.5 31.0 10.5 3.0 21.6 170 39.0 30.0 9.0 3.3 21.8 180 35.5 27.0 8.5 4.0 22.6 190 27.0 22.0 5.0 8.1 35.1 200 24.5 20.0 4.5 9.9 40.4
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表 5 不同NaCl浓度下含2%PDAADA淡水钻井液的性能
NaCl/
%AV/
mPa·sPV/
mPa·sYP/
PaFLAPI/
mLFLHTHP/
mL0 35.5 27.0 8.5 4.0 22.6 5 26.0 18.0 8.0 4.1 23.6 10 23.0 17.0 6.0 4.5 24.0 20 19.5 15.0 4.5 4.5 24.6 30 14.5 11.0 3.5 4.8 26.0 36（饱和） 14.0 11.0 3.0 5.2 27.0 注：老化条件为180 ℃、16 h。
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表 6 2%降滤失剂在复合盐水基浆中的性能
NaCl/
%CaCl2/
%AV/
mPa·sPV/
mPa·sYP/
PaFLAPI/
mLFLHTHP/
mL15 0.5 17.5 14.0 3.5 4.6 25.6 15 1.0 12.5 10.0 2.5 6.8 28.8 15 1.5 10.0 8.0 2.0 8.1 39.0 30 0.5 12.0 10.0 2.0 6.6 32.2 30 1.0 10.5 9.0 1.5 10.8 51.8 30 1.5 11.5 9.5 2.0 13.6 68.0 注：老化条件为180 ℃、16 h。
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表 7 淡水基浆加入不同处理剂老化后的Zeta电位值
NaCl/% CaCl2/% PAANDA/% ζ/mV 0 0 0 −12.5 0 0 2 −41.2 15 1.0 0 −7.6 15 1.0 2 −33.2 15 1.5 2 −16.7
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