Synthesis and Properties of High Temperature Resistant Environmental Protection Shear Strength Improving Agent
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摘要: 为提高水基钻井液用提切剂抑黏提切效果和环保性能，以低黏聚阴离子纤维素钠盐（PAC-LV）和十六烷基异氰酸酯为原料，二丁基二月桂酸锡（DBTDL）为催化剂，合成了一种疏水缔合型天然改性产物作为抗高温环保型低增黏提切剂LVHY-1。通过正交实验确定了最佳合成条件：PAC-LV与十六烷基异氰酸酯的质量比为4∶1、反应温度为60 ℃、反应时间为12 h、DBTDL浓度为0.4%。借助核磁共振光谱仪（1H-NMR）进行了分子结构表征。流变性能测试结果显示，在120 ℃老化实验中，动塑比随LVHY-1加量的增大而提高。加量为0.2% LVHY-1的钻井液经170 ℃老化16 h后，其动塑比仍可达0.5 Pa/mPa·s，高温作用时间达64 h后仍保持良好的提切效果，表现出良好的抗温性和耐候性。透射电镜（TEM）观测结构显示，LVHY-1在溶液中可形成立体的网络结构，这是其具备提切效果的原因。环保性能测试结构显示，LVHY-1的半致死浓度EC50为30 100 mg/L，生物降解性评价指标（Y）为18.25，达到排放标准，易被微生物降解。Abstract: In order to improve the anti-viscosity and environmental performance of the extractant used for water-based drilling fluid, LVHY-1 was synthesized by using low viscosity anionic cellulose sodium salt (PAC-LV) and hexadecyl isocyanate as raw materials, and dibutyltin dilaurate (DBTDL) as catalyst. The optimum synthesis conditions were determined by orthogonal experiment: mass ratio of PAC-LV to cetyl isocyanate 4:1, reaction temperature 60 ℃, reaction time 12 h, DBTDL concentration 0.4%. The molecular structure was characterized by 1H-NMR. Rheological property test results showed that the dynamic plastic ratio (RYP) increased with the increase of LVHY-1 after hot aging test at 120 ℃. After hot aging at 170 ℃ for 16 h, the RYP of 0.2% LVHY-1 drilling fluid still reached 0.5 Pa/mPa·s, and kept good effect after hot aging for 64 h, showing excellent temperature and weather resistance. Transmission electron microscopy (TEM) observation showed that LVHY-1 could form a three-dimensional network structure in solution, which was the reason for the effect of LVHY-1. The test structure of environmental performance showed that the semi-maximum effective concentration (EC50) of LVHY-1 was 30 100 mg/L, and the biodegradability evaluation index (Y) was 18.25, which met the emission standard and was easy to be degraded by microorganisms.
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表 2 L9（34）正交实验结果
实验号 A B C D YP/PV/
Pa/mPa·s1# 3∶1 50 8 0.2 0.59 2# 3∶1 60 12 0.4 0.65 3# 3∶1 70 16 0.8 0.58 4# 4∶1 50 12 0.8 0.59 5# 4∶1 60 16 0.2 0.65 6# 4∶1 70 8 0.4 0.63 7# 5∶1 50 16 0.4 0.55 8# 5∶1 60 8 0.6 0.50 9# 5∶1 70 12 0.2 0.58 均值1 0.607 0.577 0.573 0.607 均值2 0.623 0.600 0.607 0.610 均值3 0.543 0.597 0.593 0.557 极差（R） 0.080 0.023 0.034 0.053 
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表 3 不同LVHY-1浓度下钻井液的流变性能
LVHY-1/% 实验条件 AV/
mPa·sPV/
mPa·sYP/
PaYP/PV /
Pa/mPa·s0.05 老化前 9.5 7.0 2.5 0.36 老化后 8.0 6.0 2.0 0.33 0.10 老化前 10.5 7.5 3.0 0.40 老化后 10.5 7.5 3.0 0.40 0.15 老化前 14.5 10.0 4.5 0.45 老化后 14.0 9.5 4.5 0.47 0.20 老化前 19.0 11.0 8.0 0.72 老化后 18.5 11.0 7.5 0.68 0.25 老化前 23.5 13.5 10.0 0.74 老化后 22.0 13.0 9.0 0.69 0.30 老化前 27.5 15.5 12.0 0.77 老化后 26.0 15.0 11.0 0.73 注：实验条件为120 ℃×16 h
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表 4 热滚温度对钻井液流变性能的影响
T/
℃AV/
mPa·sPV/
mPa·sYP/
PaYP/PV /
Pa/mPa·s100 20.5 12.0 8.5 0.71 110 19.5 11.5 8.0 0.70 120 18.5 11.0 7.5 0.68 130 18.5 11.0 7.5 0.68 140 18.0 11.0 7.0 0.64 150 18.0 11.0 7.0 0.64 160 17.0 10.5 6.5 0.62 170 15.0 10.0 5.0 0.50 180 6.5 5.5 1.0 0.18
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表 5 LVHY-1和常规处理剂的生物毒性和生物降解性
试剂 EC50/（mg/L） Y LVHY-1 30 100 18.25 XG 52 400 28.85 FHG 54 100 26.17 CTS 51 770 25.50 HV-CMC 30 020 19.20 PAC-HV 31 000 18.77 HEC 30 430 18.52
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