非牛顿含蜡原油溶胶与凝胶相互转化过程特性与机理研究
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摘要
含蜡原油是一种复杂的混合体系,其流变特性对石油的开采、集输和长距离管道输送等有重大影响。本论文以物理化学和结构力学等基本理论为基础,综合利用流变测量、DSC以及显微镜观察法对非牛顿含蜡原油溶胶与凝胶相互转化过程特性及机理进行了详细的研究和探索。主要研究内容及结果如下：
通过对含蜡原油冷却胶凝过程特性的研究发现,原油种类不同,导致原油冷却过程中结构参数的变化规律也不尽相同。降温速率越小,剪切速率越小,原油开始胶凝的温度越高,同时相同温度下形成的胶凝结构越强。依据流变学原理实验并计算验证了原油中蜡晶溶剂化层的存在,根据实验现象结合结晶学原理及溶剂化层理论对含蜡原油的冷却胶凝机理做了进一步的探讨。
通过对含蜡原油等温胶凝过程特性的研究发现,静态降温条件下,随着测量温度的降低以及恒温时间的延长,原油的储能模量增大,损耗角减小。对于动态降温或经静态降温并恒温剪切的原油而言,其储能模量的变化趋势与静态降温的原油相似,但损耗角随着测量温度的降低先减小后增大。此外,在较低的温度条件下,随着静止时间的延长,原油损耗角也会表现出先减小后增加的趋势。静态降温速率越小,原油恒温过程中形成的结构越强；而动态降温速率越小,原油在恒温静止初始的结构越强,最终的平衡结构却越弱。当测量温度不同时,降温过程中的剪切速率对原油等温胶凝特性的影响也不同。较高温度下,剪切速率越大,原油恒温过程中形成的结构越强；凝点温度时,原油的等温胶凝结构强度随着剪切速率的增加先减小后增加；当温度较低时,剪切速率越大,原油恒温过程中形成的结构越弱。而恒温剪切对原油的结构总是起破坏作用的。最后对含蜡原油的等温胶凝机理进行了探索。
通过对胶凝含蜡原油在不同载荷加载方式下屈服特性的研究发现,胶凝含蜡原油在恒应力下的屈服实际上是一个蠕变过程。引入损伤变量及硬化函数,建立的胶凝含蜡原油非线性蠕变方程,能够精确的描述多种含蜡原油的3个蠕变阶段,简洁实用,可在工程中推广应用。连续增加剪切应力方式下,随着应力加载速率的增加,胶凝原油的屈服值增大,屈服时间减小。在阶梯式增加剪切应力方式下,单阶作用时间增加,胶凝原油的屈服值减小,屈服时间增加；阶段应力增加幅度增大,胶凝原油的屈服值逐渐增大并最终趋为定值,而屈服时间则逐渐减小。在连续增加剪切速率方式下,当剪切速率增加速率较小时,应力随剪切速率的增加出现波动现象；随着加载速率的增大,应力波动现象逐渐减小直至消失,同时胶凝原油的屈服值也逐渐增大。
以基于等结构参数法建立的Houska模型为基础,结合原油触变性实验数据,综合推导得出一个描述原油触变裂降曲线的新模型,该模型物理意义明确,适应性较强,使用方便。利用等结构参数法建立了第一个具有理论意义的含蜡原油静态结构恢复模型,并证明该模型可以较好的描述多种含蜡原油的静态结构恢复特性。以青海原油为例详细研究并得出了多种历史条件对上述两个模型拟合参数的影响规律。
利用流变测量技术首次对胶凝含蜡原油的熔化特性进行了详细的研究,结果表明,原油的熔化与胶凝并不是简单的逆过程。胶凝原油升温速率越大,相同测量温度下,原油的结构强度越强。终冷温度越低,原油升温过程中相同温度下的结构强度越弱,同时在较高的非牛顿流体温度条件下恒温静止形成的结构也越弱。而终冷温度下的恒温时间对原油的熔化及在较高温度下恒温结构发展特性的影响并不明显。依据实验现象结合结晶学原理提出了相应的胶凝含蜡原油熔化机理。
Waxy crude oil is a complex mixture whose rheological properties have great influence on the exploitation, storage and pipeline transportation. Basing on the theories of physical chemistry and structure mechanics, the properties and mechanism of sol-gel transformation for non-newtonian waxy crude oil were investigated in detail, using a combination of rheological methods, DSC and optical microscopy. The main contents and conclusions are the following.
The gelling properties for crude oil due to decreasing temperature were investigated.It is shown that the variation of structure parameters are distinct for different kinds of oils.The gel point of the waxy crude oil becomes higher and the strength of the gel structure increases with the decrease of cooling rate and shear stress. The existence of wax solvation layer was proved by rheological experiment and calculation.The corresponding gelling mechanism was improved by combim gexperimental phenome na and crystallography theory.
The isothermal gelling properties of waxy crude oil were studied systematically. The results show that the modulus of oils after static cooling becomes higher by decreasing temperature or increasing holding time, meanwhile the loss angle decreases. For the oils after dynamic cooling or shearing under isothermal condition, the variation of modulus are similar to those of static cooled samples, but the loss angle decreases first and then increases by decreasing temperature. In addition, the loss angle also decreases first and then increases by increasing holding time at relatively lower temperatures. The isothermal structure becomes stronger with a decreasing static cooling rate.while with decreasing dynamic cooling rate, the stength of initial structure under isothermal condition increases but the strength of final structure decreases.The dependence of isothermal structure development of waxy crude oil on shear rate are also strongly influenced by temperature. At relatively high temperatures, the higher shear rates can result in stronger structure.While approaches pour point, the structure decreases first and then increases with increasing shear rate. At relatively lower temperatures, the strength of structure decreases with the increase of shear rate.
The yielding properties of waxy crude oil under different measuring methods were studied.The results show that the yielding of gelled waxy crude oil under constant stress is really a creep process. The nonlinear creep model was established by introducing damage and hardening variables, which can describe the three stages of creep process for several different oils.For the shear stress loading in a linear way, a higher stress loading rate causes a higher yield stress and a shorter yielding time.For the stress loading in a stepwise way, the yield stress decreases and the yielding time increases with increasing time duration,whilewith increasing the changing rate of stress, the yield stress increases first and finally keeps constant, meanwhile the yielding time decreases. For the shear rate loading in a linear way, the shear stress-shear rate curve will appear fluctuation phenomena with a lower loading rate. As the loading rate increases, the fluctuation phenomena will decrease gradually and until disappear, while the yiled stress also increases.
A new model was obtained basing on the Houska model, and it was proved to describe the thixotropic properties of waxy crude oil simply and accurately. A first theoretical model for recovery properties of waxy crude oil was established by using a structure parameter method, which was proved to fit well with the experimental data of several different waxy crude oils. Taking Qinghai oil for example, the influence of histories on the Correlation coefficient of the two models was also found.
The melting properties of gelled waxy crude oil were first investigated by rheological method.The results show that the melting and gelling of waxy crude oil are not simply inverse processes.With the increase of heating rate, the gel strength increases during heating process. With the decrease of final cooling temperature, both the strength of structure during heating process and isothermal process at higher non-newtonian temperature decreases. And there is nearly no influence on the melting properties during heating process and isothermal structure development on higher temperature for isothermal holding time at final cooling temperature. The melting mechanism of gelled waxy crude oil was put forward.
通过对含蜡原油冷却胶凝过程特性的研究发现,原油种类不同,导致原油冷却过程中结构参数的变化规律也不尽相同。降温速率越小,剪切速率越小,原油开始胶凝的温度越高,同时相同温度下形成的胶凝结构越强。依据流变学原理实验并计算验证了原油中蜡晶溶剂化层的存在,根据实验现象结合结晶学原理及溶剂化层理论对含蜡原油的冷却胶凝机理做了进一步的探讨。
通过对含蜡原油等温胶凝过程特性的研究发现,静态降温条件下,随着测量温度的降低以及恒温时间的延长,原油的储能模量增大,损耗角减小。对于动态降温或经静态降温并恒温剪切的原油而言,其储能模量的变化趋势与静态降温的原油相似,但损耗角随着测量温度的降低先减小后增大。此外,在较低的温度条件下,随着静止时间的延长,原油损耗角也会表现出先减小后增加的趋势。静态降温速率越小,原油恒温过程中形成的结构越强；而动态降温速率越小,原油在恒温静止初始的结构越强,最终的平衡结构却越弱。当测量温度不同时,降温过程中的剪切速率对原油等温胶凝特性的影响也不同。较高温度下,剪切速率越大,原油恒温过程中形成的结构越强；凝点温度时,原油的等温胶凝结构强度随着剪切速率的增加先减小后增加；当温度较低时,剪切速率越大,原油恒温过程中形成的结构越弱。而恒温剪切对原油的结构总是起破坏作用的。最后对含蜡原油的等温胶凝机理进行了探索。
通过对胶凝含蜡原油在不同载荷加载方式下屈服特性的研究发现,胶凝含蜡原油在恒应力下的屈服实际上是一个蠕变过程。引入损伤变量及硬化函数,建立的胶凝含蜡原油非线性蠕变方程,能够精确的描述多种含蜡原油的3个蠕变阶段,简洁实用,可在工程中推广应用。连续增加剪切应力方式下,随着应力加载速率的增加,胶凝原油的屈服值增大,屈服时间减小。在阶梯式增加剪切应力方式下,单阶作用时间增加,胶凝原油的屈服值减小,屈服时间增加；阶段应力增加幅度增大,胶凝原油的屈服值逐渐增大并最终趋为定值,而屈服时间则逐渐减小。在连续增加剪切速率方式下,当剪切速率增加速率较小时,应力随剪切速率的增加出现波动现象；随着加载速率的增大,应力波动现象逐渐减小直至消失,同时胶凝原油的屈服值也逐渐增大。
以基于等结构参数法建立的Houska模型为基础,结合原油触变性实验数据,综合推导得出一个描述原油触变裂降曲线的新模型,该模型物理意义明确,适应性较强,使用方便。利用等结构参数法建立了第一个具有理论意义的含蜡原油静态结构恢复模型,并证明该模型可以较好的描述多种含蜡原油的静态结构恢复特性。以青海原油为例详细研究并得出了多种历史条件对上述两个模型拟合参数的影响规律。
利用流变测量技术首次对胶凝含蜡原油的熔化特性进行了详细的研究,结果表明,原油的熔化与胶凝并不是简单的逆过程。胶凝原油升温速率越大,相同测量温度下,原油的结构强度越强。终冷温度越低,原油升温过程中相同温度下的结构强度越弱,同时在较高的非牛顿流体温度条件下恒温静止形成的结构也越弱。而终冷温度下的恒温时间对原油的熔化及在较高温度下恒温结构发展特性的影响并不明显。依据实验现象结合结晶学原理提出了相应的胶凝含蜡原油熔化机理。
Waxy crude oil is a complex mixture whose rheological properties have great influence on the exploitation, storage and pipeline transportation. Basing on the theories of physical chemistry and structure mechanics, the properties and mechanism of sol-gel transformation for non-newtonian waxy crude oil were investigated in detail, using a combination of rheological methods, DSC and optical microscopy. The main contents and conclusions are the following.
The gelling properties for crude oil due to decreasing temperature were investigated.It is shown that the variation of structure parameters are distinct for different kinds of oils.The gel point of the waxy crude oil becomes higher and the strength of the gel structure increases with the decrease of cooling rate and shear stress. The existence of wax solvation layer was proved by rheological experiment and calculation.The corresponding gelling mechanism was improved by combim gexperimental phenome na and crystallography theory.
The isothermal gelling properties of waxy crude oil were studied systematically. The results show that the modulus of oils after static cooling becomes higher by decreasing temperature or increasing holding time, meanwhile the loss angle decreases. For the oils after dynamic cooling or shearing under isothermal condition, the variation of modulus are similar to those of static cooled samples, but the loss angle decreases first and then increases by decreasing temperature. In addition, the loss angle also decreases first and then increases by increasing holding time at relatively lower temperatures. The isothermal structure becomes stronger with a decreasing static cooling rate.while with decreasing dynamic cooling rate, the stength of initial structure under isothermal condition increases but the strength of final structure decreases.The dependence of isothermal structure development of waxy crude oil on shear rate are also strongly influenced by temperature. At relatively high temperatures, the higher shear rates can result in stronger structure.While approaches pour point, the structure decreases first and then increases with increasing shear rate. At relatively lower temperatures, the strength of structure decreases with the increase of shear rate.
The yielding properties of waxy crude oil under different measuring methods were studied.The results show that the yielding of gelled waxy crude oil under constant stress is really a creep process. The nonlinear creep model was established by introducing damage and hardening variables, which can describe the three stages of creep process for several different oils.For the shear stress loading in a linear way, a higher stress loading rate causes a higher yield stress and a shorter yielding time.For the stress loading in a stepwise way, the yield stress decreases and the yielding time increases with increasing time duration,whilewith increasing the changing rate of stress, the yield stress increases first and finally keeps constant, meanwhile the yielding time decreases. For the shear rate loading in a linear way, the shear stress-shear rate curve will appear fluctuation phenomena with a lower loading rate. As the loading rate increases, the fluctuation phenomena will decrease gradually and until disappear, while the yiled stress also increases.
A new model was obtained basing on the Houska model, and it was proved to describe the thixotropic properties of waxy crude oil simply and accurately. A first theoretical model for recovery properties of waxy crude oil was established by using a structure parameter method, which was proved to fit well with the experimental data of several different waxy crude oils. Taking Qinghai oil for example, the influence of histories on the Correlation coefficient of the two models was also found.
The melting properties of gelled waxy crude oil were first investigated by rheological method.The results show that the melting and gelling of waxy crude oil are not simply inverse processes.With the increase of heating rate, the gel strength increases during heating process. With the decrease of final cooling temperature, both the strength of structure during heating process and isothermal process at higher non-newtonian temperature decreases. And there is nearly no influence on the melting properties during heating process and isothermal structure development on higher temperature for isothermal holding time at final cooling temperature. The melting mechanism of gelled waxy crude oil was put forward.
引文
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