油田污水防垢与缓蚀技术研究
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摘要
我国油田主要采用注水开发的方式。注入水通常是产出液中分离出的污水,水质复杂,含有大量无机盐、溶解气,可在油井井筒、地面系统和注水地层结垢或导致井筒、管线腐蚀,影响油田正常生产。通过加入防垢剂、缓蚀剂可以防止腐蚀、结垢的发生。木文针对油田的使用条件,系统评价了液体防垢剂的性能,改进了聚马来酸、马束酸酐-醋酸乙烯酯共聚物的合成方法,优化了膦基聚羧酸的合成条件,制备了可在井筒使用的固体防垢块;通过研究碳酸钙晶型分布与防垢率的关系、防垢剂对碳酸钙表面zeta电位影响,探讨了防垢剂作用机理;通过系列咪唑啉和聚氧乙烯烷基苯酚醚磷酸酯的合成,研究了缓蚀剂结构与性能的关系。
评价了国内15种防垢剂的钙容忍度、热稳定性能、防碳酸钙垢性能和防硫酸钡垢性能,结果表明:(1) 对碳酸钙垢,有机膦酸防垢剂质量浓度为2mg/L时防垢率大于90%,相同浓度的聚合物防垢率不到85%;对硫酸钡垢,聚合物PASP、PAA和有机膦酸EDTMP有一定抑制效果,而将PASP与EDTMP 3∶2复配后,产生明显的协同效应,质量浓度为50mg/L时,对硫酸钡垢防垢率可达到90%。(2) 有机膦酸的钙容忍度低于聚合物防垢剂。分子中含酯基、磺酸根的共聚物防垢剂具有更高的钙容忍度。(3) 除氧后的聚合物防垢剂具有较好的耐温性能,其中丙烯酸-丙烯酸酯共聚物、聚丙烯酸在150℃下加热(除氧)72h后,防碳酸钙垢率仍可达到70%。在HEDP、ATMP、PBTC、EDTMP四种有机膦酸中,HEDP的耐热性能最好;有机膦酸防垢剂可以用于90℃以下,当使用温度高于100℃时,防垢性能会受到不同程度影响。
以水为溶剂,以防垢率为主要指标,研究了聚马来酸、马来酸酐—醋酸乙烯酯共聚物、膦基聚羧酸的合成:以30%的过氧化氢为引发剂,在过渡金属离子催化作用下合成的聚马来酸,溴值低于150mg/g,防垢率达93.52%(质量浓度为8mg/L);首次在过硫酸铵中引入少量的次亚磷酸钠作为复合引发剂合成马来酸酐—醋酸乙烯酯共聚物,所得防垢剂溴值小于100mg/g,钙容忍度为1500mg/L,防垢率为91.2%(质量浓度为4mg/L);以过硫酸铵-次亚磷酸钠组成的氧化还原体系为引发剂合成的膦基聚马来酸和膦基马来酸-丙烯酸共聚物,质量浓度为2mg/L时,阻碳酸钙垢率分别为85%、90%,优于PAA、HPMA、MA-AA,但即使使用浓度高达50mg/L,对油阳污水也基本没有缓蚀性能。
制备了可悬挂于抽油泵下面使用的低温、中温、高温三个温度系列的固体防垢块,可分别在60℃、70℃、80℃井筒条件下使用。防垢块主要由防垢剂、胶结剂组成。HEDP防垢性能和热稳定性较好,可用作固体块中的防垢剂,使用前需制成HEDP-Na或Ca_2HEDP,前者易溶于水,后者在水中可缓慢溶解。固体块中的胶结剂由塑料构成。通过比较塑料的熔点和在柴油中的溶解性能,可以用1C10A作为低温防垢块的胶结剂、TN00作中温防垢块胶结剂、7042和1C10A复配作高温防垢块的胶结剂。用HEDP-Na作防垢成份时,由于防垢材料和胶结材料的极性差别较大,造成防垢剂颗粒不能被充分
Watertlood development is used widely in Chinese oilfield. Usually injected water is sewage separated from oilfield produced liquid. It contains multiple constitute such as inorganic salt and solved gas, to which scale and corrosion is ascribed in wellbore, surface equipment at al. The occurrence of scale and corrosion affected usual oilfield production. An effective way to inhibit scale and corrosion is using scale inhibitor and corrosion inhibitor. In this paper , the following research is implemented: systematically evaluation of liquid scale inhibitor, improved synthesis method of polymaleic acid and maleic anhydride-vinyl acetate copolymer, optimum synthesis method of phosphonate containing polymer, preparation of solid scale inhibitor, discuss of scale inhibition mechanism based on the influence of scale inhibitor on crystal form distributatuion and zeta potential of calcium carbonate, relationship of molecular structure and corrosion inhibitor performance.15 scale inhibitors were evaluated for their calcium tolerance, thermal stability, CaCO_3 and BaSO_4 scale inhibition performance. The results indicate: (1) CaCO_3 scale inhibition ratio of phosphonic acid type inhibitor is higher than 90% and that of polymer type scale inhibitor is lower than 85% at concentration of 2mg/L. Although PASP PAA and EDTMP are three effective BaSO_4 scale inhibitors, scale inhibition ratio of single inhibitor is lower than 70%. When PASP is compounded with EDTMP with a ratio of 3:2 , scale inhibition ratio can be improved to 90% with 50mg/L mixture for the occurrence of synergetic effect between PASP and EDTMP. (2)The calcium tolerance of phosphonic acid is lower than polymer type scale inhibitors. Higher calcium tolerance can be reached for ester-containing polymer or sulfonate-containing polymer.(3)The thermal stability of polymer type scale inhibitors is better after aeration, especially for acrylic acid/acrylic ester copolymer, polyacrylic acid ,CaCO_3 scale inhibition ratio can retain 70% after being heated at 150℃ for 72h .The evaluation of thermal stability on HEDP、 ATMP、 PBTC、 EDTMP show that performance of HEDP is best and phosphonic acid can be used at temperature lower than 90℃ .when the medium temperature is high than 100℃,scale inhibitor performance may be debilitated to diffferent extent.The synthesis method of polymaleic acid, maleic anhydride-vinyl acetate copolymer, phosphonate-containing polymer in water were studied based on scale inhibition ratio as main target: for polymaleic acid synthesized in water with a transition metal ion as catalyst and H_2O_2 as stimulant, bromine value is less than 150mg/g and inhibition ratio of calcium
carbonate scale is 93.52% at concentration of 8 mg/L; for maleic anhydride-vinyl acetate copolymer synthesized with the compounded stimulant of sodium hypophosphite and ammonium persulfate, its bromine value is less than 30mg/g , calcium tolerance is 1500mg/L and inhibition ratio of calcium carbonate scale is 91.2% at concentration of 4 mg/L; for phosponate-containing polymaielic acid and phosphonate-containing maielic acid-acrylic acid copolymer, inhibition ratio of calcium carbonate scale is 85% and 90% respectively, but they exhibit ineffective on corrosion inhibition even at concentration of 50mg/L.To inhibit scale formation in oil well, three types of solid scale inhibitor, which can be hung to oil pump in well ting at low temperature, moderate temperature and high temperature respectively, was made mainly from phosphonic type inhibitors. The experiments show that, HEDP, a wide used scale inhibitor in oilfield now, can be selected as scale inhibiting material in solid scale inhibitor for its excellent scale inhibition performance and thermal stability. Before used to prepare solid inhibitor, HEDP must be made into HEDP-Na, a powder soluble in water or Ca2HEDP, a powder springly soluble in water. By comparing melting point and solubility of different plastic in diesel, 1C10A, TN00, compound of DFDA7042 and 1C10A is selected as consolidating agent for low, moderate,and high temperature solid scale inhibitor respectively. When solid scale inhibitor was made only from consolidating agent and HEDP-Na, HEDP-Na would swiftly solve in water because it wasn't not be well consolidated by consolidating agent for their great difference of polarity. After the polarity was conjusted by amphiprotic polymer ,a solid scale inhibitor with good slow releasing ability can be produced.To probe mechanism of scale inhibition, calcium carbonate scale was collected before and after the addition of scale inhibitors and analysized by SEM,FT-IR,XRD qualitatively or quantitately. The results confirm that, after addition of inhibitors, both morphology and content of vaterite is changed. Scale inhibition ratio is higher, change of morphology and increase of vaterite content is more great. It can be inferred that change of morphology is ascribed to the change of crystal form.There are three stage in crastallizing process including occurrence and disappearing of unstable phase , occurrence and disappearing of metastable phase, development of stable phase. When scale inhibitors are added, the second stage and the first stage can be controlled preceedingly to different content according to scale inhibition efficency, so crystal form is changed.To verify the effect of HEDP on surface electrical properity of calcium carbonate scale, which is one of classical scale inhibiting mechanism, zeta potential of freshly CaCC>3 originated from admixture of equimolar of Ca2+ and CO32" was measured during
precipitating process with time. The results show that the produced CaCO3 is negatively charged and IIEDP had no obvious effect on zeta potential of CaCO3 if having been added during precipitation. In addition, zeta potential of CaCO3 originated from admixture of equimolar ot Cai4 and CO3"" was also measured during dissolution. With the preceding of dissolution , zeta potentials of CaCO3 and the values of pH continuously decreased. Whether the Scale inhibitor was added or not during CaCO3 prepartation,the zeta potential had no obvious difference and whether the dispersion contained HEDP or not, zeta potential also had no obvious difference -To investigate annnelation during synthesis of imidazoline, resultants from oleic acid and diethyienetriamine at 160°C for different time were analyzed by IR and UV, produced water rate and acid value was measured, and corrosion inhibitor performance was investigated by electrochemical polarization curves. The results indicate that cyclization and amidation is developed at the same time and performance of corrosion inhibitor with cyclized structurehigher is better.For series imidazoline with different lipophilic tail and hydrophilic group ,the corrosion inhibitor performance for A3 steel in synthetic brine saturated with CO2 was investigated, and the relationship between molecular structure and performance was suggested. Results show that, in solution containing less than 5X 104mg/L salt, imidazoline with longer lipophilic tail exhibit more efficient, especially when there is double bond in the hydrophobic chain. In solution containing more than 5 X 104mg/L salt, performance of imidazoline with long hydrophobic chain, such as l-aminoethyl-2-pentadecylimidazoline,l-aminoethyl-2-septadecylimidazoline and l-aminoethyl-2-septadecylene imidazoline ,is weaken with the increase of salt content in solution, while that is slightly enhanced for short hydrophobic chain imidazolines such as 1-aminoethyl-2-unadecyl imidazoline and l-aminoethyl-2-tridecyl imidazoline.Also the performance affected by salty change, l-aminoethyl-2-septadecylene imidazoline is always most efficient in mentioned imidazoline. Aong another four imidazoline from resultants of septadecylene imidazoline with ehloroacetic acid, acetic acid and sulfaminic acid respectively, performance of l-aminoethyl-l-carboxymethyl-2-septadecylene imidazoline is best and performance of aminoethyl imidazoline is better than that of hydroxylimidazoline.Also corrosion inhibitor performance was evaluated for a series of octyl-phenol-polyoxythylene ether phosphates with different oxythylene chain length and monoester content. The results indicate that length of oxythylene chain have substantial influence on corrosion inhibitor performance,which can be improved with the change of oxythylene chain length from 10 to 4. A corrosion inhibition ratio over 90% can be
obtained at the concentration of 10 mg/L when oxythylene chain is 4(OPP4). While monoester content has slightly influence on corrosion inhibitor performance . Corrosion inhibition ratio increases by no more than 4% when mono-ester content of the product increases from 29.78% to 91.55%.
评价了国内15种防垢剂的钙容忍度、热稳定性能、防碳酸钙垢性能和防硫酸钡垢性能,结果表明:(1) 对碳酸钙垢,有机膦酸防垢剂质量浓度为2mg/L时防垢率大于90%,相同浓度的聚合物防垢率不到85%;对硫酸钡垢,聚合物PASP、PAA和有机膦酸EDTMP有一定抑制效果,而将PASP与EDTMP 3∶2复配后,产生明显的协同效应,质量浓度为50mg/L时,对硫酸钡垢防垢率可达到90%。(2) 有机膦酸的钙容忍度低于聚合物防垢剂。分子中含酯基、磺酸根的共聚物防垢剂具有更高的钙容忍度。(3) 除氧后的聚合物防垢剂具有较好的耐温性能,其中丙烯酸-丙烯酸酯共聚物、聚丙烯酸在150℃下加热(除氧)72h后,防碳酸钙垢率仍可达到70%。在HEDP、ATMP、PBTC、EDTMP四种有机膦酸中,HEDP的耐热性能最好;有机膦酸防垢剂可以用于90℃以下,当使用温度高于100℃时,防垢性能会受到不同程度影响。
以水为溶剂,以防垢率为主要指标,研究了聚马来酸、马来酸酐—醋酸乙烯酯共聚物、膦基聚羧酸的合成:以30%的过氧化氢为引发剂,在过渡金属离子催化作用下合成的聚马来酸,溴值低于150mg/g,防垢率达93.52%(质量浓度为8mg/L);首次在过硫酸铵中引入少量的次亚磷酸钠作为复合引发剂合成马来酸酐—醋酸乙烯酯共聚物,所得防垢剂溴值小于100mg/g,钙容忍度为1500mg/L,防垢率为91.2%(质量浓度为4mg/L);以过硫酸铵-次亚磷酸钠组成的氧化还原体系为引发剂合成的膦基聚马来酸和膦基马来酸-丙烯酸共聚物,质量浓度为2mg/L时,阻碳酸钙垢率分别为85%、90%,优于PAA、HPMA、MA-AA,但即使使用浓度高达50mg/L,对油阳污水也基本没有缓蚀性能。
制备了可悬挂于抽油泵下面使用的低温、中温、高温三个温度系列的固体防垢块,可分别在60℃、70℃、80℃井筒条件下使用。防垢块主要由防垢剂、胶结剂组成。HEDP防垢性能和热稳定性较好,可用作固体块中的防垢剂,使用前需制成HEDP-Na或Ca_2HEDP,前者易溶于水,后者在水中可缓慢溶解。固体块中的胶结剂由塑料构成。通过比较塑料的熔点和在柴油中的溶解性能,可以用1C10A作为低温防垢块的胶结剂、TN00作中温防垢块胶结剂、7042和1C10A复配作高温防垢块的胶结剂。用HEDP-Na作防垢成份时,由于防垢材料和胶结材料的极性差别较大,造成防垢剂颗粒不能被充分
Watertlood development is used widely in Chinese oilfield. Usually injected water is sewage separated from oilfield produced liquid. It contains multiple constitute such as inorganic salt and solved gas, to which scale and corrosion is ascribed in wellbore, surface equipment at al. The occurrence of scale and corrosion affected usual oilfield production. An effective way to inhibit scale and corrosion is using scale inhibitor and corrosion inhibitor. In this paper , the following research is implemented: systematically evaluation of liquid scale inhibitor, improved synthesis method of polymaleic acid and maleic anhydride-vinyl acetate copolymer, optimum synthesis method of phosphonate containing polymer, preparation of solid scale inhibitor, discuss of scale inhibition mechanism based on the influence of scale inhibitor on crystal form distributatuion and zeta potential of calcium carbonate, relationship of molecular structure and corrosion inhibitor performance.15 scale inhibitors were evaluated for their calcium tolerance, thermal stability, CaCO_3 and BaSO_4 scale inhibition performance. The results indicate: (1) CaCO_3 scale inhibition ratio of phosphonic acid type inhibitor is higher than 90% and that of polymer type scale inhibitor is lower than 85% at concentration of 2mg/L. Although PASP PAA and EDTMP are three effective BaSO_4 scale inhibitors, scale inhibition ratio of single inhibitor is lower than 70%. When PASP is compounded with EDTMP with a ratio of 3:2 , scale inhibition ratio can be improved to 90% with 50mg/L mixture for the occurrence of synergetic effect between PASP and EDTMP. (2)The calcium tolerance of phosphonic acid is lower than polymer type scale inhibitors. Higher calcium tolerance can be reached for ester-containing polymer or sulfonate-containing polymer.(3)The thermal stability of polymer type scale inhibitors is better after aeration, especially for acrylic acid/acrylic ester copolymer, polyacrylic acid ,CaCO_3 scale inhibition ratio can retain 70% after being heated at 150℃ for 72h .The evaluation of thermal stability on HEDP、 ATMP、 PBTC、 EDTMP show that performance of HEDP is best and phosphonic acid can be used at temperature lower than 90℃ .when the medium temperature is high than 100℃,scale inhibitor performance may be debilitated to diffferent extent.The synthesis method of polymaleic acid, maleic anhydride-vinyl acetate copolymer, phosphonate-containing polymer in water were studied based on scale inhibition ratio as main target: for polymaleic acid synthesized in water with a transition metal ion as catalyst and H_2O_2 as stimulant, bromine value is less than 150mg/g and inhibition ratio of calcium
carbonate scale is 93.52% at concentration of 8 mg/L; for maleic anhydride-vinyl acetate copolymer synthesized with the compounded stimulant of sodium hypophosphite and ammonium persulfate, its bromine value is less than 30mg/g , calcium tolerance is 1500mg/L and inhibition ratio of calcium carbonate scale is 91.2% at concentration of 4 mg/L; for phosponate-containing polymaielic acid and phosphonate-containing maielic acid-acrylic acid copolymer, inhibition ratio of calcium carbonate scale is 85% and 90% respectively, but they exhibit ineffective on corrosion inhibition even at concentration of 50mg/L.To inhibit scale formation in oil well, three types of solid scale inhibitor, which can be hung to oil pump in well ting at low temperature, moderate temperature and high temperature respectively, was made mainly from phosphonic type inhibitors. The experiments show that, HEDP, a wide used scale inhibitor in oilfield now, can be selected as scale inhibiting material in solid scale inhibitor for its excellent scale inhibition performance and thermal stability. Before used to prepare solid inhibitor, HEDP must be made into HEDP-Na, a powder soluble in water or Ca2HEDP, a powder springly soluble in water. By comparing melting point and solubility of different plastic in diesel, 1C10A, TN00, compound of DFDA7042 and 1C10A is selected as consolidating agent for low, moderate,and high temperature solid scale inhibitor respectively. When solid scale inhibitor was made only from consolidating agent and HEDP-Na, HEDP-Na would swiftly solve in water because it wasn't not be well consolidated by consolidating agent for their great difference of polarity. After the polarity was conjusted by amphiprotic polymer ,a solid scale inhibitor with good slow releasing ability can be produced.To probe mechanism of scale inhibition, calcium carbonate scale was collected before and after the addition of scale inhibitors and analysized by SEM,FT-IR,XRD qualitatively or quantitately. The results confirm that, after addition of inhibitors, both morphology and content of vaterite is changed. Scale inhibition ratio is higher, change of morphology and increase of vaterite content is more great. It can be inferred that change of morphology is ascribed to the change of crystal form.There are three stage in crastallizing process including occurrence and disappearing of unstable phase , occurrence and disappearing of metastable phase, development of stable phase. When scale inhibitors are added, the second stage and the first stage can be controlled preceedingly to different content according to scale inhibition efficency, so crystal form is changed.To verify the effect of HEDP on surface electrical properity of calcium carbonate scale, which is one of classical scale inhibiting mechanism, zeta potential of freshly CaCC>3 originated from admixture of equimolar of Ca2+ and CO32" was measured during
precipitating process with time. The results show that the produced CaCO3 is negatively charged and IIEDP had no obvious effect on zeta potential of CaCO3 if having been added during precipitation. In addition, zeta potential of CaCO3 originated from admixture of equimolar ot Cai4 and CO3"" was also measured during dissolution. With the preceding of dissolution , zeta potentials of CaCO3 and the values of pH continuously decreased. Whether the Scale inhibitor was added or not during CaCO3 prepartation,the zeta potential had no obvious difference and whether the dispersion contained HEDP or not, zeta potential also had no obvious difference -To investigate annnelation during synthesis of imidazoline, resultants from oleic acid and diethyienetriamine at 160°C for different time were analyzed by IR and UV, produced water rate and acid value was measured, and corrosion inhibitor performance was investigated by electrochemical polarization curves. The results indicate that cyclization and amidation is developed at the same time and performance of corrosion inhibitor with cyclized structurehigher is better.For series imidazoline with different lipophilic tail and hydrophilic group ,the corrosion inhibitor performance for A3 steel in synthetic brine saturated with CO2 was investigated, and the relationship between molecular structure and performance was suggested. Results show that, in solution containing less than 5X 104mg/L salt, imidazoline with longer lipophilic tail exhibit more efficient, especially when there is double bond in the hydrophobic chain. In solution containing more than 5 X 104mg/L salt, performance of imidazoline with long hydrophobic chain, such as l-aminoethyl-2-pentadecylimidazoline,l-aminoethyl-2-septadecylimidazoline and l-aminoethyl-2-septadecylene imidazoline ,is weaken with the increase of salt content in solution, while that is slightly enhanced for short hydrophobic chain imidazolines such as 1-aminoethyl-2-unadecyl imidazoline and l-aminoethyl-2-tridecyl imidazoline.Also the performance affected by salty change, l-aminoethyl-2-septadecylene imidazoline is always most efficient in mentioned imidazoline. Aong another four imidazoline from resultants of septadecylene imidazoline with ehloroacetic acid, acetic acid and sulfaminic acid respectively, performance of l-aminoethyl-l-carboxymethyl-2-septadecylene imidazoline is best and performance of aminoethyl imidazoline is better than that of hydroxylimidazoline.Also corrosion inhibitor performance was evaluated for a series of octyl-phenol-polyoxythylene ether phosphates with different oxythylene chain length and monoester content. The results indicate that length of oxythylene chain have substantial influence on corrosion inhibitor performance,which can be improved with the change of oxythylene chain length from 10 to 4. A corrosion inhibition ratio over 90% can be
obtained at the concentration of 10 mg/L when oxythylene chain is 4(OPP4). While monoester content has slightly influence on corrosion inhibitor performance . Corrosion inhibition ratio increases by no more than 4% when mono-ester content of the product increases from 29.78% to 91.55%.
引文
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