新型稠化酸液的制备及其性能研究
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摘要
为了满足地层深部酸化的需要，降低稠化酸的地层伤害性、提高稠化酸的粘度，制得高性能酸液，开展了新型清洁稠化酸和高粘度稠化酸的研究工作。
采用具有特殊结构的阳离子表面活性剂和助表面活性剂配制出了高粘度的盐酸溶液，研制出了与该体系具有优良配伍性的缓蚀剂，考察了酸液组成对酸液性能的影响。在此基础上提出了用于碳酸盐地层酸化作业的FL清洁稠化酸酸液配方，研究了基本性能。结果表明，FL清洁稠化酸具有良好的剪切稳定性，对钢材腐蚀性小，与大理石的反应速度慢，无残渣。组成为4％FL4-22+2％FL4-22A+20％盐酸溶液+2％缓蚀剂的酸液在90℃下粘度可达25mPa·s，在与地层岩石反应时具有粘度先升后降的特征，残酸粘度低易于返排，可用于碳酸盐地层的深部酸化作业。
采用丙烯酰胺(AM)与阴离子单体丙烯酸(AA)和阳离子单体甲基丙烯酰氧乙基三甲基氯化铵(DMC)为共聚单体，用自由基水溶液聚合方法制备出了两性离子共聚物稠化剂P(AM-DMC-AA)。采用红外光谱、核磁共振~1H谱对共聚物结构和组成进行了表征；研究了聚合反应的pH值、温度、时间、引发剂浓度、不同单体配比以及单体浓度对共聚反应产物溶液性能的影响。研究结果表明，聚合反应条件对产物性能影响较大。酸性条件下制备的共聚物溶解性较好；随着单体浓度的增加，所得聚合物的特性粘数和溶液表观粘度先升高后下降；随着引发剂浓度的增加，共聚反应转化率提高，聚合物溶液的特性粘数和表观粘度先上升后下降；随着阳离子单体甲基丙烯酰氧乙基三甲基氯化铵(DMC)单元在共聚物中含量的减少，阴离子单体丙烯酸单元在共聚物中含量的增加，共聚物的特性粘数和表观粘度先上升后下降；当AM在共聚单体中的含量增大时，共聚物的特性粘数和表观粘度先升高后降低；随着反应温度升高，所得聚合物溶液的特性粘数先升高后下降。
研究了共聚物P(AM-DMC-AA)的溶液性能，分别考察了共聚物结构及共聚物浓度、温度、剪切速率对共聚物溶液表观粘度的影响。研究结果表明，P(AM-DMC-AA)具有明显的两性离子共聚物特征，在水或盐酸中具有良好的溶解性、热稳定性、剪切稳定性，可用作酸液增粘剂。
采用P(AM-DMC-AA)为增粘剂、具有1，5—二醛结构的化合物为交联剂配制出了交联稠化酸，研究了交联剂与共聚物P(AM-DMC-AA)交联作用机理。考察了P(AM-DMC-AA)结构与浓度、温度、交联剂用量对交联稠化酸性能的影响，在此基础上提出了交联稠化酸的酸液配方。研究结果表明，P(AM-DMC-AA)在酸液中参与交联反应的基团是丙烯酰胺结构单元的酰胺基团，交联作用可大幅度提高酸液粘度．交联剂加量及合成P(AM-DMC-AA)时AM加量对所制备的交联稠化酸的粘度及稳定性有显著影响，只有在适当加量下才能获得性能良好的交联稠化酸。交联稠化酸性能评价结果表明，交联酸液粘度高，缓速性能显著优于常规盐酸和稠化酸率，破胶后粘度低、残渣含量少，是一种具有优良综合性能的新型酸液。
Acid treatment is important measure to increase production, theperformance of acid working liquids directly affect the effect of acidtreatments. In order to prepare acid with good performance, new type ofpolymer-free acid and thickened acid has been researched.
Polymer-free acid with high viscosity was formulated by 20%HCl, acationic surfactant (FL4-22),and an organic metal surfactant (FL4—22A)with special chemical structure. The corrosion inhibitor(FL4—22B)which is of good compatibility with the retarded acid was prepared. Theeffect of acid composing on performance was studied, and the formulationof the acid (FL polymer—free viscous acid)suitable for formationacidization was recommended. The proterties of FL polymer—freeviscous acid were systematically investigated. It is concluded that thisacid system have good properties in shear stability, corrosioninhibition, and retardance performance. The viscosity of FL polymer—free viscous acid(4%FL4-22+2% FL4-22A+20%HC1+2%FL4-22B) is25mPa·s at 90℃, and rheological studies showed that the acid rapidlydeveloped viscosity as the acid was spent with carbonate minerals, Thishigh viscosity will help in diverting the live acid into otherun-stimulated zones. Once the acid stimulation is complete, the high viscosity of spent acid can be broken either by dilution with theinjection water or crude oil in the reservoir. So this new type of acidsystem can be applied in carbonate acidizing treatments.
The water-soluble copolymer P(AM-DMC-AA) of acrylamide (AM),methacryloyloxyethyl trimethyl ammonium chloride (DMC), and acrylicacid (AA) were synthesized by free radical aqueous solutioncopolymerization. The copolymer structures were characterized via IRSpectrum and ~1H-NMR Spectrum. The effects of the reaction conditions suchas pH value, reaction temperature, time, initiator concentration andvarious monomers concentrations on the performance of the copolymersolution were studied.
The results show that the conditions of polymerization reaction havenotable effect on the performance of the product. Dissolvability ofcopolymer synthesized in acidity is better than alkalescence. Theintrinsic viscosity and apparent viscosity of copolymer increases atfirst then decreases with monomer concentration, initiatorconcentration increasing and temperature rising. When the AM monomeramount in the copolymer increases, the intrinsic viscosity and apparentviscosity of copolymer increases at first then decreases. IR and ~1H-NMRstructural symptom have been confirmed the copolymer structure unitinclude acrylamide (AM), methacryloyloxyethyl trimethyl ammoniumchloride (DMC), and acrylic acid (AA).
The influence factors(water soluble time, copolymer concentration,temperature, shear rate) on Apparent viscosity of the copolymer solutionwere studied. The transmittance at various pH has also been studied, Theshow that P (AM-DMC-AA) has the good water dissolubility and thicknessability; The apparent viscosity of copolymer solution decreased withshear rate and temperature increase. Iransmittance study showed that P(AM-DMC-AA) has distinct characteristic of zwitterion copolymer.
The rheology, heat stability, shear stability of copolymerP(AM-DMC-AA) as viscosifier also were evaluated. The results show that the thickened acid has good properties of acid dissolubility, heatstability, shear stability, can be applied in acidizing treatments.
Crosslinked acid has been prepared by cross-linker; The mechanismof cross-linker and P(AM-DMC-AA)has been studied; The apparent viscositychanges of crosslinked acid in different temperature, cross-linkerconcentration, copolymer concentration and AMcontent in P (AM-DMC-AA)were investigated. Characteristic evaluate of Crosslinked acid indicatethat crosslinked acid has good propertis of retardance performance. Theapparent viscosity and residue content of liquids after gel-breakingaccord with pertinent standard.
采用具有特殊结构的阳离子表面活性剂和助表面活性剂配制出了高粘度的盐酸溶液，研制出了与该体系具有优良配伍性的缓蚀剂，考察了酸液组成对酸液性能的影响。在此基础上提出了用于碳酸盐地层酸化作业的FL清洁稠化酸酸液配方，研究了基本性能。结果表明，FL清洁稠化酸具有良好的剪切稳定性，对钢材腐蚀性小，与大理石的反应速度慢，无残渣。组成为4％FL4-22+2％FL4-22A+20％盐酸溶液+2％缓蚀剂的酸液在90℃下粘度可达25mPa·s，在与地层岩石反应时具有粘度先升后降的特征，残酸粘度低易于返排，可用于碳酸盐地层的深部酸化作业。
采用丙烯酰胺(AM)与阴离子单体丙烯酸(AA)和阳离子单体甲基丙烯酰氧乙基三甲基氯化铵(DMC)为共聚单体，用自由基水溶液聚合方法制备出了两性离子共聚物稠化剂P(AM-DMC-AA)。采用红外光谱、核磁共振~1H谱对共聚物结构和组成进行了表征；研究了聚合反应的pH值、温度、时间、引发剂浓度、不同单体配比以及单体浓度对共聚反应产物溶液性能的影响。研究结果表明，聚合反应条件对产物性能影响较大。酸性条件下制备的共聚物溶解性较好；随着单体浓度的增加，所得聚合物的特性粘数和溶液表观粘度先升高后下降；随着引发剂浓度的增加，共聚反应转化率提高，聚合物溶液的特性粘数和表观粘度先上升后下降；随着阳离子单体甲基丙烯酰氧乙基三甲基氯化铵(DMC)单元在共聚物中含量的减少，阴离子单体丙烯酸单元在共聚物中含量的增加，共聚物的特性粘数和表观粘度先上升后下降；当AM在共聚单体中的含量增大时，共聚物的特性粘数和表观粘度先升高后降低；随着反应温度升高，所得聚合物溶液的特性粘数先升高后下降。
研究了共聚物P(AM-DMC-AA)的溶液性能，分别考察了共聚物结构及共聚物浓度、温度、剪切速率对共聚物溶液表观粘度的影响。研究结果表明，P(AM-DMC-AA)具有明显的两性离子共聚物特征，在水或盐酸中具有良好的溶解性、热稳定性、剪切稳定性，可用作酸液增粘剂。
采用P(AM-DMC-AA)为增粘剂、具有1，5—二醛结构的化合物为交联剂配制出了交联稠化酸，研究了交联剂与共聚物P(AM-DMC-AA)交联作用机理。考察了P(AM-DMC-AA)结构与浓度、温度、交联剂用量对交联稠化酸性能的影响，在此基础上提出了交联稠化酸的酸液配方。研究结果表明，P(AM-DMC-AA)在酸液中参与交联反应的基团是丙烯酰胺结构单元的酰胺基团，交联作用可大幅度提高酸液粘度．交联剂加量及合成P(AM-DMC-AA)时AM加量对所制备的交联稠化酸的粘度及稳定性有显著影响，只有在适当加量下才能获得性能良好的交联稠化酸。交联稠化酸性能评价结果表明，交联酸液粘度高，缓速性能显著优于常规盐酸和稠化酸率，破胶后粘度低、残渣含量少，是一种具有优良综合性能的新型酸液。
Acid treatment is important measure to increase production, theperformance of acid working liquids directly affect the effect of acidtreatments. In order to prepare acid with good performance, new type ofpolymer-free acid and thickened acid has been researched.
Polymer-free acid with high viscosity was formulated by 20%HCl, acationic surfactant (FL4-22),and an organic metal surfactant (FL4—22A)with special chemical structure. The corrosion inhibitor(FL4—22B)which is of good compatibility with the retarded acid was prepared. Theeffect of acid composing on performance was studied, and the formulationof the acid (FL polymer—free viscous acid)suitable for formationacidization was recommended. The proterties of FL polymer—freeviscous acid were systematically investigated. It is concluded that thisacid system have good properties in shear stability, corrosioninhibition, and retardance performance. The viscosity of FL polymer—free viscous acid(4%FL4-22+2% FL4-22A+20%HC1+2%FL4-22B) is25mPa·s at 90℃, and rheological studies showed that the acid rapidlydeveloped viscosity as the acid was spent with carbonate minerals, Thishigh viscosity will help in diverting the live acid into otherun-stimulated zones. Once the acid stimulation is complete, the high viscosity of spent acid can be broken either by dilution with theinjection water or crude oil in the reservoir. So this new type of acidsystem can be applied in carbonate acidizing treatments.
The water-soluble copolymer P(AM-DMC-AA) of acrylamide (AM),methacryloyloxyethyl trimethyl ammonium chloride (DMC), and acrylicacid (AA) were synthesized by free radical aqueous solutioncopolymerization. The copolymer structures were characterized via IRSpectrum and ~1H-NMR Spectrum. The effects of the reaction conditions suchas pH value, reaction temperature, time, initiator concentration andvarious monomers concentrations on the performance of the copolymersolution were studied.
The results show that the conditions of polymerization reaction havenotable effect on the performance of the product. Dissolvability ofcopolymer synthesized in acidity is better than alkalescence. Theintrinsic viscosity and apparent viscosity of copolymer increases atfirst then decreases with monomer concentration, initiatorconcentration increasing and temperature rising. When the AM monomeramount in the copolymer increases, the intrinsic viscosity and apparentviscosity of copolymer increases at first then decreases. IR and ~1H-NMRstructural symptom have been confirmed the copolymer structure unitinclude acrylamide (AM), methacryloyloxyethyl trimethyl ammoniumchloride (DMC), and acrylic acid (AA).
The influence factors(water soluble time, copolymer concentration,temperature, shear rate) on Apparent viscosity of the copolymer solutionwere studied. The transmittance at various pH has also been studied, Theshow that P (AM-DMC-AA) has the good water dissolubility and thicknessability; The apparent viscosity of copolymer solution decreased withshear rate and temperature increase. Iransmittance study showed that P(AM-DMC-AA) has distinct characteristic of zwitterion copolymer.
The rheology, heat stability, shear stability of copolymerP(AM-DMC-AA) as viscosifier also were evaluated. The results show that the thickened acid has good properties of acid dissolubility, heatstability, shear stability, can be applied in acidizing treatments.
Crosslinked acid has been prepared by cross-linker; The mechanismof cross-linker and P(AM-DMC-AA)has been studied; The apparent viscositychanges of crosslinked acid in different temperature, cross-linkerconcentration, copolymer concentration and AMcontent in P (AM-DMC-AA)were investigated. Characteristic evaluate of Crosslinked acid indicatethat crosslinked acid has good propertis of retardance performance. Theapparent viscosity and residue content of liquids after gel-breakingaccord with pertinent standard.
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