油田固井用SBL的合成、应用研究及MLPNBR的制备研究
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摘要
第一部分油田固井用SBL的合成、应用研究
第一章油田固井用丁苯胶乳的研究进展介绍了聚合物用作油气田固井降滤失水剂的简史及其作用的机历,重点介绍了丁苯类胶乳所取得的成果,二十世纪九十年代GOPACKRISHNAN SKIOHAR公司和HALIBURTON公司开发出了丁苯类胶乳降滤失剂产品,耐温分别达到180℃和耐温最高达176℃,但前者还须加稳定剂才能与水泥浆配伍使用。廉价、多功能(如具有降滤失水、防窜、水泥石增韧及防腐蚀功能)的水乳(溶)型聚合物是油田外加剂的发展趋势。
第二章油气田固井用丁苯胶乳的合成及应用研究首先分析了固井工艺要求、水泥浆的特点和胶乳降滤失水、防气窜的作用机历,对乳化剂、功能单体等合成胶乳的组分和结构进行了设计。研究了乳化剂、功能单体的种类及其用量、单体加入方式等因素对聚合反应及胶乳性能的影响,确定了以非离子乳化剂为主、阴离子乳化剂为辅的复配乳化体系,以丁二烯、苯乙烯为主单体、丙烯腈为功能单体并分批加入,以过硫酸盐为引发剂在中温条件下合成油气田固井用丁苯胶乳的技术方法。在胶乳应用技术研究中,通过对影响胶乳水泥浆体系性能的水灰比、分散剂、稳定剂、缓凝剂、胶乳加量以及加重剂等因素进行分项考察,构建了正常密度胶乳水泥浆体系和高密度胶乳水泥浆固井体系。胶乳具有良好的降滤失水、防气窜、和防酸腐蚀作用,满足固井工艺的要求。
第三章油气田固井用丁苯胶乳的工业放大实验及其应用评价在21M3聚合装置上,对影响聚合反应平稳和胶乳性能稳定的主要因素引发剂用量、分子量调解剂用量和聚合反应温度进行了考察研究,确定了在21M3聚合装置制备油田固井用丁苯胶乳的最佳聚合组分和工艺技术。胶乳的应用实验系统地评价了胶乳水泥浆动态和静态特性指标。胶乳的应用评价实验和现场固井实验表明:采用第二章所建立的正常密度、高密度胶乳水泥浆体系,胶乳加量在7-11%之间,通过调整HNJ-3缓凝剂的加量,胶乳水泥浆稠化时间3-5小时内可调,最高稠化温度为170℃,滤失水量<50mL,抗窜阻力可达3.5Mpa,水泥石的抗压强度>21 Mpa,水泥石在酸液中30天损失率为10%。胶乳具有良好的降滤失水、防气窜功能,水泥石增韧及耐酸腐蚀的作用,能够满足高温深井、侧井、小眼井的固井要求。现场固井效果良好。
第二部分MLPNBR的制备研究
第四章粉末丁腈橡胶的研究进展介绍了制备粉末丁腈橡胶的主要方法,重点介绍了以丁腈胶乳为原料、经凝聚隔离、闪蒸干燥成粉的凝聚法。该法能耗较低,干燥效率较高,能减少粉尘对环境的污染。合成非交联型丁腈胶乳时,目前主要采用阴离子乳化剂,氧化-还原的引发体系,在5-8℃进行聚合反应,反应时间16-20小时,单体转化率不大于85%,残余单体需要回收,需要温度较低的冷剂撤出聚合反应热。
第五章中腈含量非交联型粉末丁腈橡胶(MLPNBR)制备研究本研究采用以丁腈胶乳为原料的凝聚法制备中腈含量非交联型粉末丁腈橡胶,该法包括丁腈胶乳合成、凝聚隔离成粉、脱水干燥三个步骤。
在丁腈胶乳的合成中,研究了过硫酸盐与活化剂组成的引发体系、乳化剂、终止剂的种类及用量、单体配比、分子量调节剂的用量及加入方式以及反应温度等要素对聚合过程以及胶乳性能指标的影响,确定了过硫酸盐与活化剂组成的引发体系在,常温条件进行下中腈含量非交联型丁腈胶乳,聚合反应时间12-14小时、单体转化率达到98%,反应平稳易控,胶乳质量稳定。在凝聚、隔离、成粉的研究中,考察了凝聚剂、隔离剂的种类及用量、凝聚温度、搅拌分散强度等要素对成粉率的影响,确定了采用复配的凝聚剂及一段凝聚法、脂肪酸盐-高聚物乳液的复合隔离体系以及凝聚隔离的工艺条件。使用了脂肪酸皂与聚合物乳液复配的隔离剂,有效地提高隔离效果。
第六章MLPNBR的工业化实验及其应用在45M~3聚合装置上进行了工业放大试验,考察了引发体系和分子量调节剂的用量对聚合反应及其胶乳性能的影响,确定了工业化生产该胶乳的配方工艺条件,现已投入正常生产。
在12M3凝聚装置和2000t/a旋转闪蒸干燥器上进行了凝聚隔离、干燥、成粉的工业放大试验,考察了凝聚温度及时间、干燥时进料速度、干燥气流的温度及速度对成粉率的影响,确定了工业生产这种PNBR工艺技术,现已投入正常生产。采用了卧式离心脱水和旋转闪蒸干燥方式,成粉率达到了95%以上,提高了效率和产能,减少了粉尘对环境的污染。应用表明该产品达到了同类产品的水平,满足PVC改性的要求。
PartⅠSynthesis and applications of styrene-butadiene latex(SBL)for well cementation in oil field
Chapter 1 Advances of studying on SBL for oil-gas field
The history of polymers as fluid loss control agents and the mechanism of controlling fluid loss were reviewed. The achievements of SBL as fluid loss control agent were emphatically introduced. In 1990s, GOPACKRISHNAN SKIOHAR Corporation developed a SBL product with thickening temperature up to 180℃. But this agent must be used together with other stabilizing agent. Halliburton Corporation also developed a SBL with thickening temperature up to 176℃. To develop of cheap emulsion or soluble polymer that possess lots of advantageous performances, such as fluid loss control, anticorrosion and the resistance of gas permeation, is a hot topic of cement additives.
Chapter 2 Synthesis and application of SBL on stabilizing oil-gas well
The character of cement mortar and process of stabilizing well have been analyzed. The latex should have the superior performance of chemical and shear stability. According to the mechanism of controlling fluid loss and the resistance of gas permeation,we have designed the sort of emulsify agent and functional monomer. The effects of some factors, such as the kinds and ratio of emulsify agent, monomer, initiator, chain-transfer agent, electrolyte, chain terminator, polymerized temperature and stirring speed of polymerization, on polymerizing reaction and the performance of latex are studied in detail. Through application test, we determinate the optimized process: non-ion emulsify agent as the major one, negative ion emulsify agent as auxiliary agent, acrylonitrile as functional monomer with two patches addition, persulfate as initiator with polymerizing temperature of 40-50℃. The ratios of other components of latex system have also been determined. For the application of SBL we prepared, the cement-water ratio, the latex ratio and the sort, the ratio of other additives of cement mortar, the performance of latex cement mortar, are also studied. We construct the latex-cement mortar system in high density and in low density through measuring the index of thickening rate and temperature, fluid loss, the resistance of preventing gas permeation and the compressive strength of latex-cement rock. This SBL can compound with cement and have superior performances of fluid loss control, resistance of gas permeation and anticorrosion on stabilizing oil-gas well.
Chapter 3 The industrial scale-up and performance evaluation of this SBL
The effects of three main factors, such as ratio of initiator, chain-transfer, and polymerized temperature, on polymerization process and SBL performance are investigated at 21M3 polymerizing reactor. The preparative technique of this SBL on industrial scale is determined. The application tests of the SBL indicate that the thickening rate can be adjusted within 3-5 hrs, the thickening temperature can reach 170℃, the fluid loss is less than 50ml, the compressive strength of latex-cement rock is more than 21MPa. This SBL have been succeeded well cementation at LiaoHe and ShengLi oil field. Now more than 50 oil wells have been cemented using this SBL at DaGang oil field.
PartⅡStudy on the preparation of powder acrylonitrile-butadiene rubber with medium content of combined acrylonitrile and low ML (MLPNBR)
Chapter 4 Advances of studying on the powder acrylonitrle–butadiene rubber
The major methods for the preparation of PNBR, the flocculate-drying method and some factors affecting the ratio of powder in particular, were introduced. The flocculate agent must be added into NBL to produce powder of NBR, and then dry the wet powder with flash dryer. This method has several advantages, such as low energy consumption, dust pollute and high efficiency of drying. In NBL synthesizing, negative ion emulsifier and oxidation-reduction initiator are commonly used, the polymerized temperature is within 5-8℃, polymerized period is 16-20hr with monomer polymerize less than 85%.
Chapter 5 Studying on the preparation technique of powder acrylonitrile- butadiene rubber with medium content of combined acrylonitrile and low ML (MLPNBR)
The initiator system of persulfate and activator, the sort and ratio of monomer initiator emulsify agent chain-transfer agent, ratio of monomer, chain-transfer agent, electrolyte and chain terminator, and polymerized temperature, the content of combined acrylonitrile of NBL are studied in detail. The ratio of component of synthesis NBL and technological process are determined. Due to the use of persulfate in initiator system, polymerization temperature is within 25-30℃, polymerized period is shorted within 12-14hr, monmer polymerize is more than 98%. ML of NBL can be effectively controlled by the addition of chain-transfer agent in two patches.
In NBL flocculation and wet powder drying process, we have studied the affects of some factors such as the sort and ratio of flocculating agent, isolated agent, anti-oxidant and flocculation temperature, stirring speed of flocculating reaction, adding speed of the wet powder, drying temperature,on the ratio of powder. The sort and ratio of auxiliary material and technological process are also checked and determined at 300L flocculating reactor.
Chapter 6 The industrial process and performance tests of MLPNBR
The NBL preparation technique is determined after the study of the effects of initiator system and chain-transfer agent on NBL performance at 45M3 polymerizing reactor.
At 12M3 flocculantor and spiral flash evaporation dryer of drying 2000 t/a equipments, the main factors such as flocculation temperature and time, the speed of wet power entering dryer, the temperature of drying gas, which affect the ratio of powder, have been optimized. Because of using horizontal centrifugal machine and spiral flash evaporation dryer, the ratio of the powder is more than 95% and dust pollute has been lowed. The performances of the prepared MLPNBR can satisfy with the application demands.
第一章油田固井用丁苯胶乳的研究进展介绍了聚合物用作油气田固井降滤失水剂的简史及其作用的机历,重点介绍了丁苯类胶乳所取得的成果,二十世纪九十年代GOPACKRISHNAN SKIOHAR公司和HALIBURTON公司开发出了丁苯类胶乳降滤失剂产品,耐温分别达到180℃和耐温最高达176℃,但前者还须加稳定剂才能与水泥浆配伍使用。廉价、多功能(如具有降滤失水、防窜、水泥石增韧及防腐蚀功能)的水乳(溶)型聚合物是油田外加剂的发展趋势。
第二章油气田固井用丁苯胶乳的合成及应用研究首先分析了固井工艺要求、水泥浆的特点和胶乳降滤失水、防气窜的作用机历,对乳化剂、功能单体等合成胶乳的组分和结构进行了设计。研究了乳化剂、功能单体的种类及其用量、单体加入方式等因素对聚合反应及胶乳性能的影响,确定了以非离子乳化剂为主、阴离子乳化剂为辅的复配乳化体系,以丁二烯、苯乙烯为主单体、丙烯腈为功能单体并分批加入,以过硫酸盐为引发剂在中温条件下合成油气田固井用丁苯胶乳的技术方法。在胶乳应用技术研究中,通过对影响胶乳水泥浆体系性能的水灰比、分散剂、稳定剂、缓凝剂、胶乳加量以及加重剂等因素进行分项考察,构建了正常密度胶乳水泥浆体系和高密度胶乳水泥浆固井体系。胶乳具有良好的降滤失水、防气窜、和防酸腐蚀作用,满足固井工艺的要求。
第三章油气田固井用丁苯胶乳的工业放大实验及其应用评价在21M3聚合装置上,对影响聚合反应平稳和胶乳性能稳定的主要因素引发剂用量、分子量调解剂用量和聚合反应温度进行了考察研究,确定了在21M3聚合装置制备油田固井用丁苯胶乳的最佳聚合组分和工艺技术。胶乳的应用实验系统地评价了胶乳水泥浆动态和静态特性指标。胶乳的应用评价实验和现场固井实验表明:采用第二章所建立的正常密度、高密度胶乳水泥浆体系,胶乳加量在7-11%之间,通过调整HNJ-3缓凝剂的加量,胶乳水泥浆稠化时间3-5小时内可调,最高稠化温度为170℃,滤失水量<50mL,抗窜阻力可达3.5Mpa,水泥石的抗压强度>21 Mpa,水泥石在酸液中30天损失率为10%。胶乳具有良好的降滤失水、防气窜功能,水泥石增韧及耐酸腐蚀的作用,能够满足高温深井、侧井、小眼井的固井要求。现场固井效果良好。
第二部分MLPNBR的制备研究
第四章粉末丁腈橡胶的研究进展介绍了制备粉末丁腈橡胶的主要方法,重点介绍了以丁腈胶乳为原料、经凝聚隔离、闪蒸干燥成粉的凝聚法。该法能耗较低,干燥效率较高,能减少粉尘对环境的污染。合成非交联型丁腈胶乳时,目前主要采用阴离子乳化剂,氧化-还原的引发体系,在5-8℃进行聚合反应,反应时间16-20小时,单体转化率不大于85%,残余单体需要回收,需要温度较低的冷剂撤出聚合反应热。
第五章中腈含量非交联型粉末丁腈橡胶(MLPNBR)制备研究本研究采用以丁腈胶乳为原料的凝聚法制备中腈含量非交联型粉末丁腈橡胶,该法包括丁腈胶乳合成、凝聚隔离成粉、脱水干燥三个步骤。
在丁腈胶乳的合成中,研究了过硫酸盐与活化剂组成的引发体系、乳化剂、终止剂的种类及用量、单体配比、分子量调节剂的用量及加入方式以及反应温度等要素对聚合过程以及胶乳性能指标的影响,确定了过硫酸盐与活化剂组成的引发体系在,常温条件进行下中腈含量非交联型丁腈胶乳,聚合反应时间12-14小时、单体转化率达到98%,反应平稳易控,胶乳质量稳定。在凝聚、隔离、成粉的研究中,考察了凝聚剂、隔离剂的种类及用量、凝聚温度、搅拌分散强度等要素对成粉率的影响,确定了采用复配的凝聚剂及一段凝聚法、脂肪酸盐-高聚物乳液的复合隔离体系以及凝聚隔离的工艺条件。使用了脂肪酸皂与聚合物乳液复配的隔离剂,有效地提高隔离效果。
第六章MLPNBR的工业化实验及其应用在45M~3聚合装置上进行了工业放大试验,考察了引发体系和分子量调节剂的用量对聚合反应及其胶乳性能的影响,确定了工业化生产该胶乳的配方工艺条件,现已投入正常生产。
在12M3凝聚装置和2000t/a旋转闪蒸干燥器上进行了凝聚隔离、干燥、成粉的工业放大试验,考察了凝聚温度及时间、干燥时进料速度、干燥气流的温度及速度对成粉率的影响,确定了工业生产这种PNBR工艺技术,现已投入正常生产。采用了卧式离心脱水和旋转闪蒸干燥方式,成粉率达到了95%以上,提高了效率和产能,减少了粉尘对环境的污染。应用表明该产品达到了同类产品的水平,满足PVC改性的要求。
PartⅠSynthesis and applications of styrene-butadiene latex(SBL)for well cementation in oil field
Chapter 1 Advances of studying on SBL for oil-gas field
The history of polymers as fluid loss control agents and the mechanism of controlling fluid loss were reviewed. The achievements of SBL as fluid loss control agent were emphatically introduced. In 1990s, GOPACKRISHNAN SKIOHAR Corporation developed a SBL product with thickening temperature up to 180℃. But this agent must be used together with other stabilizing agent. Halliburton Corporation also developed a SBL with thickening temperature up to 176℃. To develop of cheap emulsion or soluble polymer that possess lots of advantageous performances, such as fluid loss control, anticorrosion and the resistance of gas permeation, is a hot topic of cement additives.
Chapter 2 Synthesis and application of SBL on stabilizing oil-gas well
The character of cement mortar and process of stabilizing well have been analyzed. The latex should have the superior performance of chemical and shear stability. According to the mechanism of controlling fluid loss and the resistance of gas permeation,we have designed the sort of emulsify agent and functional monomer. The effects of some factors, such as the kinds and ratio of emulsify agent, monomer, initiator, chain-transfer agent, electrolyte, chain terminator, polymerized temperature and stirring speed of polymerization, on polymerizing reaction and the performance of latex are studied in detail. Through application test, we determinate the optimized process: non-ion emulsify agent as the major one, negative ion emulsify agent as auxiliary agent, acrylonitrile as functional monomer with two patches addition, persulfate as initiator with polymerizing temperature of 40-50℃. The ratios of other components of latex system have also been determined. For the application of SBL we prepared, the cement-water ratio, the latex ratio and the sort, the ratio of other additives of cement mortar, the performance of latex cement mortar, are also studied. We construct the latex-cement mortar system in high density and in low density through measuring the index of thickening rate and temperature, fluid loss, the resistance of preventing gas permeation and the compressive strength of latex-cement rock. This SBL can compound with cement and have superior performances of fluid loss control, resistance of gas permeation and anticorrosion on stabilizing oil-gas well.
Chapter 3 The industrial scale-up and performance evaluation of this SBL
The effects of three main factors, such as ratio of initiator, chain-transfer, and polymerized temperature, on polymerization process and SBL performance are investigated at 21M3 polymerizing reactor. The preparative technique of this SBL on industrial scale is determined. The application tests of the SBL indicate that the thickening rate can be adjusted within 3-5 hrs, the thickening temperature can reach 170℃, the fluid loss is less than 50ml, the compressive strength of latex-cement rock is more than 21MPa. This SBL have been succeeded well cementation at LiaoHe and ShengLi oil field. Now more than 50 oil wells have been cemented using this SBL at DaGang oil field.
PartⅡStudy on the preparation of powder acrylonitrile-butadiene rubber with medium content of combined acrylonitrile and low ML (MLPNBR)
Chapter 4 Advances of studying on the powder acrylonitrle–butadiene rubber
The major methods for the preparation of PNBR, the flocculate-drying method and some factors affecting the ratio of powder in particular, were introduced. The flocculate agent must be added into NBL to produce powder of NBR, and then dry the wet powder with flash dryer. This method has several advantages, such as low energy consumption, dust pollute and high efficiency of drying. In NBL synthesizing, negative ion emulsifier and oxidation-reduction initiator are commonly used, the polymerized temperature is within 5-8℃, polymerized period is 16-20hr with monomer polymerize less than 85%.
Chapter 5 Studying on the preparation technique of powder acrylonitrile- butadiene rubber with medium content of combined acrylonitrile and low ML (MLPNBR)
The initiator system of persulfate and activator, the sort and ratio of monomer initiator emulsify agent chain-transfer agent, ratio of monomer, chain-transfer agent, electrolyte and chain terminator, and polymerized temperature, the content of combined acrylonitrile of NBL are studied in detail. The ratio of component of synthesis NBL and technological process are determined. Due to the use of persulfate in initiator system, polymerization temperature is within 25-30℃, polymerized period is shorted within 12-14hr, monmer polymerize is more than 98%. ML of NBL can be effectively controlled by the addition of chain-transfer agent in two patches.
In NBL flocculation and wet powder drying process, we have studied the affects of some factors such as the sort and ratio of flocculating agent, isolated agent, anti-oxidant and flocculation temperature, stirring speed of flocculating reaction, adding speed of the wet powder, drying temperature,on the ratio of powder. The sort and ratio of auxiliary material and technological process are also checked and determined at 300L flocculating reactor.
Chapter 6 The industrial process and performance tests of MLPNBR
The NBL preparation technique is determined after the study of the effects of initiator system and chain-transfer agent on NBL performance at 45M3 polymerizing reactor.
At 12M3 flocculantor and spiral flash evaporation dryer of drying 2000 t/a equipments, the main factors such as flocculation temperature and time, the speed of wet power entering dryer, the temperature of drying gas, which affect the ratio of powder, have been optimized. Because of using horizontal centrifugal machine and spiral flash evaporation dryer, the ratio of the powder is more than 95% and dust pollute has been lowed. The performances of the prepared MLPNBR can satisfy with the application demands.
引文
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