CN102549414B - 开始雾度测量设备和程序 - Google Patents
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Abstract
提供用于测量如下至少一项的设备和方法：石油产品显现出延迟光雾时的温度和光雾不存在于产品中时的温度。设备包含用于保持产品试样的容器、光源、光检测器、加热器和冷却器与用于存储和分析至少一种由试样透射或散射的光的微处理器装置组合。测量用于测定产物的光雾性能以及用于控制除雾过程以满足目标光雾性能。
Description
发明领域
本发明涉及用于测量液体中的光雾的方法和设备。特别地，本发明涉及用于通过使用光散射测量而测试液体中延迟开始光雾或光雾消失温度的方法和设备，和使用这种设备的程序。
本文所述设备和方法适于与任何能透射光的材料一起使用。然而，本发明特别适用于监控石油产品如重润滑剂基本油料，尤其是衍生自天然气合成油(GTL)材料的基本油料中的延迟开始光雾或光雾消失温度。因此，为方便起见，通过具体参考石油产品，尤其是润滑剂基本油料和GTL衍生的基本油料描述本发明。
发明背景
石油产品如燃料和润滑剂部分地通过它们在特定温度下显示出的物理变化表征。事实上，这些温度相关变化通常用作燃料和润滑剂的规格。一种这类变化为烃的浊点。如所熟知的，浊点为燃料或润滑剂中溶解的固体如石蜡开始形成并与烃分离时的温度。燃料和润滑剂的另一重要性能是它们的倾点。倾点为石油产品流动的最低温度。浊点和倾点为对于燃料或润滑剂的性能而言关键的性能。
American Society for Testing Materials(ASTM)(美国测试材料协会)已开发标准试验以测定浊点和倾点温度如ASTM D2300-91和ASTM D97-87。这些试验均要求石油产品试样的内行操作以测定浊点和倾点温度。
已开发了稍微更复杂的设备以测量石油产品的浊点，其很大程度上基于适当冷却的试样的一些光学测量。
至少从美学和经济方面看重要的石油产品的另一物理性能是它们的外观。清澈且明亮的产品比混浊的那些具有更高价值。因此，在制备石油产品如最终重润滑剂基本油料中，使脱蜡油经受除雾步骤以改善它的外观。如所知，除雾通常通过催化或吸附方法或通过过滤以除去产生混浊性的那些组分而实现。然而经验显示可制备润滑剂基本油料，所述基本油料具有令人满意的浊点和倾点且在冷却至室温以后为清澈且明亮的，但当储存时可发展光雾。该现象在本文中称为延迟开始光雾形成。由于延迟开始光雾通常本身不显示延长的时段，通常长达6个月，难以了解润滑剂在其预期搁置寿命期间是否会发展光雾。光雾不存在于石油产品中时的温度在本文中称为光雾消失温度。显然，非常理想的是能监控和控制润滑剂形成过程以确保最终润滑剂基本油料具有可接受的延迟开始光雾性能或光雾消失温度。
尽管已使用光散射技术测量各种润滑剂性能如浊点和倾点，但至今未探究或实现使用这种技术监控和控制延迟开始光雾形成或光雾消失温度。
因此，需要用于快速测定石油产品是否显现出延迟开始光雾形成和不存在光雾时的温度的设备和方法。还需要可与石油方法联机和实时使用的设备以控制过程以生产具有预定光雾性能的产品。
本发明目的在于满足前述需要以及如本文具体化和宽泛地描述的其它需要。
发明概述
在本发明一个实施方案中，提供一种用于测定石油产品显现出延迟开始光雾时的温度和反过来光雾不存在于石油产品中时的最小温度(称为光雾消失温度)的方法。
方法包括用光照射产品试样，同时将试样冷却至室温以下，至在试样浊点左右或以下的目标温度。测量通过试样透射的光并用于测定延迟光雾开始温度。其后，将试样以预选的可控速率加热至升高的温度，通常约60-80℃，并测量通过试样透射的光并用于测定光雾消失温度。
在本发明另一实施方案中，方法用于监控待生产的产品和控制工艺变量，尤其是脱蜡和除雾工艺变量，以提供具有预选光雾消失温度的产品。
本发明这些和其它实施方案用一种设备实现，所述设备包含用于保持试样的具有穿过的光路的容器。设备包含用于沿着光路投射光束的装置和用于检测离开光路的光的装置。还提供用于以可控的预选速率冷却和加热试样，同时检测通过试样透射的光的装置。
附图简述
图1为本发明设备的一个实施方案的示意图。
图2为本发明可选择实施方案的示意图，其中提供用于捕获散射的光以检测和分析的装置。
图3和4为说明根据本发明方法分析的润滑基本油料的光学行为的图。
在图3-4中，此处所用OPBU指本发明的光学相行为单元。
发明详述
本发明涉及用于监控液体石油产品如重润滑油的延迟光雾开始性能和光雾消失温度中至少一项的方法和设备。本发明尤其用于制备时为清澈且明亮的但经储存发展光雾的液体石油产品。根据本发明，延迟光雾开始性能或其光雾消失温度可通过在操作上与脱蜡或除雾方法控制器或二者联合的光学监控系统测定，该系统容许即时控制工艺变量以确保生产满足合适光雾性能的产品。
可有利地通过本发明方法监控的石油产品尤其包括包含天然或合成脱蜡油的重润滑剂基本油料组合物，其具有能满足目标规格或要求的低温性能且在制备时为清澈且明亮的。
在本发明一个实施方案中，基本油料为天然气合成油(GTL)基本油料，优选重润滑油GTL基本油料。重润滑油GTL基本油料应当理解为在100℃下运动粘度为大于约8cSt，优选大于约10cSt，更优选大于约12cSt的一种。如本领域中所知，GTL基本油料为具有润滑粘度的材料，其一般衍生自本身衍生自更简单的气体含碳化合物、含氢化合物和/或元素作为原料的含蜡合成烃。衍生出GTL基本油料的优选GTL材料为在费托合成法中制备的高α含蜡烃。高α意指至少0.85，优选至少0.9，更优选至少0.92的α。如本文所用，α指Schultz-Flory动力学α。
一般而言，制备天然或合成油的含蜡进料具有650-750°F的始沸点，以及优选连续沸腾至至少1050°F的终点。
由含蜡进料制备润滑剂基本油料的方法可表征为异构化方法。通常，该方法在至少一种催化剂的存在下在约150至约500℃的温度下在约500-20,000kPa的压力下进行。该方法可在氢的存在下和约600-6,000kPa的氢分压下操作。氢与烃原料之比通常为约10-3,500n.l.l·-1(56-19,660SCF/bbl)，且原料的空速通常为约0.1-20LHSV。
脱蜡步骤可使用一种或多种溶剂脱蜡、催化脱蜡或加氢脱蜡实现。
在溶剂脱蜡中，使异构化蜡产物与冷却的溶剂如丙酮、甲乙酮(MEK)、甲基异丁基酮(MIBK)、MEK/MIBK混合物等接触以使较高倾点材料作为含蜡固体沉积，然后将其与含溶剂的润滑油馏分分离。然后将溶剂汽提出并可将脱蜡油分馏，以及如果需要的话经受除雾。
催化脱蜡通常使用与至少一种催化金属组分组合的形状选择性分子筛。典型的催化脱蜡条件包括约400-600°F的温度、500-900psig的压力、对于通过反应器的流量1500-3,500SCT/B的H2处理率和0.1-10的LHSV。
任选以及优选使脱蜡基本油料经受温和除雾以改善它的颜色、外观和稳定性。
除雾通常通过本领域中熟知的以除去产生混浊性的那些组分的催化或吸附方法实现。
将参考图1讨论用于本发明方法中的设备的一个实施方案。
如图1所示，提供用于保持待测试试样的比色杯10。比色杯10可以为在顶部用盖(未显示)打开的并手动地填充或分别具有入口和出口导管11和12以用于流过模式中。比色杯10在相对侧上具有光学窗口。比色杯目前可具有在窗口之间0.5mm、1mm、2mm、5mm和10mm的标准路径长度的间距。在本发明实践中，优选使用具有10mm路径长度的比色杯。比色杯10含在优选铝的金属单元15内的比色杯固定器14内。提供光纤电缆16以使光从相关光源发射到比色杯10中所含的试样中。优选，光源发射可见光。光纤电缆17与用于接收通过比色杯10中的试样透射的光的光缆16纵向排列成行。光缆17电子连接在可编程逻辑控制器18上，所述控制器电子记录和储存通过电缆17检测的光的量。加热装置20位于金属单元15内并可与可编程逻辑控制器18连通操作。金属单元15还包含用于使用于冷却单元15的冷却液体循环的流体管道21。冷却液的循环通过可编程逻辑控制器18控制。温度传感器19在与比色杯10的充分接近处位于比色杯固定器14内以检测比色杯中试样的温度。温度传感器19还可与逻辑控制器18连通操作。由于比色杯10中的试样会被冷却至室温以下，单元15位于外壳11内，干氮气可经由导管23循环通过该外壳。该外壳提供保持单元15周围的露点在有意义的最低温度以下的能力。
设备所基于的原理在于润滑油在不存在光雾下为充分透明的这一事实。因此，光会通过润滑油而不吸收或散射，从而导致具有基本单一性的透射。通过链烷烃结晶而在润滑剂中形成的光雾片晶散射光。因此，通过光雾润滑剂透射的光的量由于光散射而降低。由于光雾形成是成核为主的方法，散射强度和透射强度的降低与光雾的浓度以及通过润滑剂的路径长度成比例。因此，如果具有给定混浊性的0.1mm路径长度将透射强度降至初始强度的0.99，则1mm路径长度会给出0.99＊＊10＝0.904，且10mm路径长度将强度降至0.99＊＊100＝0.37。使用透射几何，仪器的灵敏度可通过改变单元的路径长度而提高。
为测定脱蜡的清澈且明亮润滑剂基本油料的延迟开始光雾形成温度，将基本油料试样放入比色杯固定器14内的比色杯10中。这可通过手动地将试样放入比色杯10中或通过将料流如来自脱蜡或除雾方法的滑流流入比色杯10中而实现。当将试样放入比色杯中时，重要的是它已保持在足以防止任何成雾组分成核的条件下。因此，放置于比色杯中时的试样应已在约80-120℃的升高温度下保持约10-30分钟。任选，但优选在将试样放入比色杯10中以后，通过加热器20将试样加热至约90℃保持约20分钟以确保任何成雾组分去核。成雾组分的去核可通过任何便利的装置测定，例如测量通过试样的光透射。然后在数据采集冷却倾斜以前，通过冷却液循环通过导管21而将试样的温度经约10分钟降至约40℃。
试样还可以，以及优选经受足以确保试样均匀性的条件。这种条件可包括在比色杯10中摇动或搅拌。作为选择，可将试样在分开的容器中加热并搅拌，然后转移至比色杯10中。
接着，将试样在室温以下冷却至在试样浊点温度左右或以下的目标温度。一般而言，目标温度为约-10℃。冷却以一般约1-0.1度/分钟，优选0.5度/分钟的恒定速率进行。
当将试样冷却至目标温度时，光通过光纤电缆16连续地发射到试样中，且透射的光通过光纤电缆17接收并通过可编程逻辑控制器18处理。
在其它功能中，将控制器18编程以将透射强度相对于时间(I原始(t))的原始数据转化成强度相对于温度(I原始(T))。然后将强度标准化成当不存在光雾时程开始时的强度(I(T)＝I原始(T)/IO)。这与单一性之间的差为散射强度和光雾量的尺度(H(T)＝1-I(T))。当试样的温度降低时，H(T)会从0提高至阈值Ht，其中H(T)＝Ht的温度为T光雾。
为测定光雾可显现于试样中时的最大温度，颠倒升温，并优选将试样以固定速率加热，所述速率任选可以为与冷却速率相同的速率，同时监控通过试样透射的光。H(T)降至基线的点或H(T)至基线的最快下降段的外延被认为是光雾消失温度。光雾消失温度表示光雾的平衡消失温度和在其以上永不形成光雾的温度。
现在参考图2，其阐述本发明的优选实施方案。该实施方案不同于图1之处在于提供检测和测量通过试样散射的光的装置。如图2所示，光纤电缆25相对于比色杯10中光学窗口以一定角度放置，其与光纤电缆16相对。在图2实施方案中，光缆25显示于45°角，但可使用其它有限角。该角度的选择取决于所需的仪器灵敏度，其中认为较小的角更灵敏。在该实施方案中，在比色杯10中的试样冷却和加热期间，存储并分析通过试样散射的光。光纤电缆25可以在操作上连接在光电倍增管(未显示)或类似器件上以用于检测和测量通过可编程逻辑控制器检测到的散射光的量。任选，该实施方案的设备还可包含光纤电缆17用于测量透射光以及可用于校准和一致性检验。
在本发明一个实施方案中，可根据本发明监控提供最终基本油料的润滑剂基本油料的脱蜡或除雾，以测定最终基本油料的光雾消失温度，并可实时控制脱蜡或除雾工艺条件以提供具有预定光雾消失温度的最终基本油料。
现在参考图3，提供在脱蜡GTL基本油料上用图2的设备得到的结果的图。所用基本油料为清澈且明亮的，且具有150的VI，在40℃下139的Kv，和在100℃下18.5的Kv。试验以40℃的试样开始。将试样以0.5℃/分钟的速率冷却。当冷却时，光散射在约-8℃下开始并随着进一步冷却持续。当加热时，散射光的量降低直至达到光雾消失温度。
图4为图3的放大尺度，其中HDT通过返回到基线而读出。图4所示NTU通过将8NTU的NTU浊度标准放入比色杯中并测量光散射而校准。因此，散射计数可涉及工业上公认的标准化浊度单位。
从前文中了解到本发明具有大量重要特征和优点。它容许测量细微光雾的开始和消失。这些测量可快速地进行。事实上，测量可实时进行以监控待生产的石油产品的质量和控制工艺变量以满足产品规格。
尽管本文已详细描述了本发明的不同实施方案，但本领域技术人员应当理解可在本文所述和要求保护的本发明宽度和范围内开发对该实施方案的各种改进和选择。
Claims (4)
1.一种由高αGTL含蜡烃制备重润滑剂基本油料的方法，其中基本油料具有预选的光雾消失温度，所述方法包括：
将GTL含蜡烃在异构化条件下异构化以形成异构化进料；
将异构化进料脱蜡至预选的浊点和倾点以提供脱蜡进料；
使脱蜡进料经受除雾步骤以提供除雾进料，所述除雾进料为清澈和明亮的，其中除雾步骤包括冷却和过滤；
测量延迟光雾开始温度和除雾进料的光雾消失温度中的至少一种，且需要时调整除雾条件以提供具有预选光雾消失温度的除雾进料，其中延迟光雾开始温度和光雾消失温度通过如下步骤测量：
(a)将基本油料试样加热至约90℃保持约20分钟；
(b)将所加热的试样经约10分钟冷却至约40℃；
(c)然后以约0.5度/分钟的速率将试样进一步冷却至-10℃；
(d)其后以恒定速率加热试样；同时
(e)沿着试样中的光路投射光束；
(f)通过光电倍增管检测以与光路成45°角散射的光；
(g)测量冷却和加热期间试样的温度；
(h)分析检测的光以测定延迟光雾开始温度和光雾消失温度中的至少一种。
2.根据权利要求1的方法，其中实时测量延迟光雾开始温度和光雾消失温度中的至少一种。
3.根据权利要求2的方法，其中在基本油料的滑流上测量延迟光雾开始温度和光雾消失温度中的至少一种。
4.一种通过将异构化的含蜡烃脱蜡至预选浊点和倾点并将脱蜡烃除雾以提供最终基本油料而制备最终润滑基本油料的方法，所述方法包括：当其制备时测定基本油料的延迟光雾开始温度和光雾消失温度中的至少一种以及需要时，调整除雾条件以提供具有预定光雾消失温度的基本油料。
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| US12/587,710 US8236168B2 (en) | 2009-10-13 | 2009-10-13 | Onset haze measurement apparatus and procedure |
| PCT/US2010/052125 WO2011046850A1 (en) | 2009-10-13 | 2010-10-11 | Onset haze measurement apparatus and procedure |
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| US8394256B2 (en) * | 2009-10-13 | 2013-03-12 | Exxonmobil Research And Engineering Company | Method for haze mitigation and filterability improvement for base stocks |
| US8730472B2 (en) | 2011-07-22 | 2014-05-20 | Exxonmobil Research And Engineering Company | Method for predicting haze in lubricant base stocks |
| GB2526772B (en) * | 2014-03-27 | 2017-07-26 | Analytical Tech & Control Ltd | Cloud point measurement in fuels |
| AT517729B1 (de) | 2015-09-29 | 2017-06-15 | Grabner Instr Messtechnik Gmbh | Verfahren und Vorrichtung zur Bestimmung der Niedertemperatureigenschaften |
| EP3260146A1 (en) | 2016-06-23 | 2017-12-27 | TecPharma Licensing AG | A coupling mechanism for a medication delivery device |
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| EP2488858B1 (en) | 2016-12-21 |
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| KR20120084759A (ko) | 2012-07-30 |
| US20110083994A1 (en) | 2011-04-14 |
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