近临界水对块状油页岩中有机质的提取研究
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摘要
油页岩是一种含有有机质的沉积岩，可以通过干馏制取页岩油，属于非常规油气资源。油页岩资源在地球上储量非常丰富，折算成页岩油的储量可达目前石油探明储量的3倍以上。我国页岩油储量仅次于美国列在世界第二位，有非常大的开发前景。
油页岩资源的原位开采方法具有无需采矿、可开发较深层与高厚度的资源、产油率高、占地面积少和环境污染低等优点。目前诸多国家与大型能源公司都在积极研发各种地下原位开采技术。然而我国油页岩资源大多品位低、埋藏深，超过300m深的油页岩资源占有相当大的比例。根据传统的油页岩原位干馏技术，尚不能进行开发利用。
针对我国油页岩资源埋藏深、品位低的情况，我们提出了利用近临界水作为热传导介质和提取剂对地下油页岩资源进行原位开采的思想。本文利用高温高压反应釜研究了近临界水对大尺寸油页岩块的提取效果，考察了近临界水的提取条件、油页岩样品的质地、尺寸等因素对近临界水提取油页岩内部有机质的影响。分析了近临界水提取物的组成以及油页岩基质性状在提取过程中的变化。证明了近临界水法提取块状油页岩中有机质的可行性，为近临界水法原位提取地下油页岩的研究提供了一定的实验基础和理论依据。主要研究内容及结果如下：
（一）研究了260℃的低温近临界水对油页岩内部原有沥青化合物的萃取情况。发现在较低温度下，升高体系压强可以增强近临界水对块状油页岩的渗透作用，从而促进对有机质的提取。
萃取沥青的组成非常复杂，除了含有大量烃类物质外还存在一些环酮、茚酮、噻吩、酚类等杂原子和芳香族化合物，且其中杂原子化合物含量要比NMP-CS2混合溶剂萃取沥青中的含量高。
（二）通过对不同温度下萃取沥青的气质分析发现，升高萃取温度可以提高近临界水对油页岩内部沥青的提取能力，且获得了更多的小分子化合物。说明一些较大分子量的有机物在温度较高的近临界水中更容易转化成小分子。当提取温度高于330℃时，近临界水可以使油页岩内部的干酪根有机质分解成沥青化合物并提取出来。当近临界水的温度升至350℃时，对油页岩内部干酪根的提取效率有非常显著的提高，并且可以获得比365℃近临界水条件下更高的提取率。
（三）350℃近临界水提取出的干酪根分解沥青主要由正构烷烃、烯烃、类异戊二烯烷烃、直链的2-酮和一元羧酸组成，芳香类化合物含量相对较低。而在油页岩残渣内的残余有机质中含有较多的芳香化合物。反映出近临界水对脂肪族化合物的提取更据有倾向性。
（四）对不同尺寸的油页岩样品进行提取实验发现，当提取时间达到20h左右时，沥青的提取率几乎不再受油页岩样品尺寸影响。这是由于油页岩内部干酪根有机质在近临界水的作用下发生溶胀与分解，体积增大，产生的应力使块状油页岩样品在垂直断面上出现了许多沿着页岩层理方向的裂缝。另外，由于内部有机质的释放，油页岩样品表面与内部出现了许多毛细孔隙，并且随着提取时间的增加孔隙现象会越发显著。
油页岩块上这些裂缝与孔隙等传质通道的形成，大大提高了近临界水对块状油页岩内部有机质的提取效率。而对大尺寸油页岩内部干酪根有机质提取的可行性也为近临界水的地下油页岩原位提取设想提供了一定参考依据。
（五）根据近临界水对油页岩内部有机质作用力的变化将整个传质过程分解成：油页岩与水相对静止、近临界水的渗透、干酪根的溶胀分解、沥青质的渗出、沥青的溶解和提取物与近临界水“油水分离”6个阶段。
由于不同阶段近临界水产生作用的不同，干酪根在不同提取时间转化成沥青的速率呈现出明显的阶段性变化。在提取时间为2h之前干酪根几乎没有发生分解。2~10h是沥青生成速率最快的时间段，干酪根内部结合相对较弱的部分快速分解。10~50h时间段内干酪根中结合力相对较强部分物质开始逐渐断裂，沥青形成速率有所下降。50h后由于干酪根大分子中大部分有机质已经断裂，新沥青的生成变得很少，而释放出来的化合物越来越多的会转化成气体小分子。
干酪根在不同的提取时间段发生的化学反应也是不同的。干酪根裂解初期释放得有机物主要是小分子环烃、芳烃和类异戊二烯烷烃，然后是正构烷烃、烯烃、酮和羧酸等直链化合物的断裂，最后是干酪根亚单元核心部分的芳烃类化合物。另外干酪根的裂解产物在近临界水中还会发生二次裂解以及水解、加氢、水合、氧化、脱羧、烷基化等一系列反应。也正是通过这些反应，干酪根有机质才得以被近临界水从油页岩内部提取出来。
（六）近临界水对桦甸、抚顺、农安和扶余等不同地区油页岩的提取实验都获得了较好的提取效果。其中，近临界水对桦甸、抚顺和农安地区油页岩块的最大沥青提取率值都超过了各样品的Fischer测试含油率值。而对扶余油页岩岩芯的提取率也达到了Fischer测试含油率的90%以上。
各地区油页岩的近临界水提取物组成大体相似，主要组成为正构烷烃、异构烷烃和芳香烃化合物，另外还有一定量的环烷烃、烯烃、醇、酮、酚等化合物。抚顺、农安和扶余油页岩的提取物中异构烃和芳烃组分含量都高于桦甸油页岩的提取物，产物的流动性也比桦甸油页岩提取沥青好。
Oil shale is an organic-rich fine-grained sedimentary rock which can generateshale oil after retorting. It is a kind of unconventional oil and gas resource. Oil shaleresources are abundant in the earth. Estimates of global deposits, converted into shaleoil, are3times higher than the proved oil reserves. The resource of shale oil in Chinais second in the world next after the United States. It has a very great developmentprospects.
There is no need to mining out the oil shale by the in-situ retorting technology.The in-situ technology can exploit the deep and high thickness oil shale resourceswith several advantages as high conversion rate, few occupied space and lowenvironmental pollution. Accordingly, many countries which are rich in oil shale andsome large energy companies are actively developing the in-situ retortingtechnologies of oil shale. However, the traditional in-situ retorting technology is notapplied to Chinese oil shale for the low oil content level and high bed depth resources.
Concentrating on the characteristics of the oil shale resources in our country, weput forward the concept of using sub-critical water as a heat transfer medium andextractant to the in-situ conversion of oil shale. In this paper, high temperature andhigh pressure reactor was used to simulate the sub-critical water extraction process ofoil shale underground. The impacts of the extraction conditions of sub-critical, thesize, texture and level of the oil shale sample on the organics extraction were studied.The composition of the extracts, the extraction and mass transfer mechanism ofsub-critical water were analyzed. The extraction experiments proved the feasibility ofextracting organic matter from the large-sized oil shale lumps by sub-critical waterand provided some experimental and theoretical basis for the in-situ conversionconcept.The main research contents and results are shown as follows:
(I) Sub-critical water extraction of the natural bitumen in oil shale was performed at a low temperature,260°C. The results showed that the increase of system pressurecould enlarge the infiltration of sub-critical water at this temperature and enhance theextraction of bitumen.
The composition of the extracted bitumen was very complex. The bitumen wasconsisted of hydrocarbons, ketones, indanones, thiophenes, phenol derivatives andother heteroatomic and aromatic compounds. The content of heteroatomic compoundsin the bitumen was significantly higher than that in the NMP-CS2extracted bitumenfrom oil shale.
(II) The extract ability of sub-critical water improved with the increase oftemperature and more small molecular weight organics could be extracted compounds.It showed that some larger molecules were more likely to decomposed in sub-criticalwater at a higher temperature. When the temperature was higher than330°C, thekerogen matters in oil shale began to be decomposed in sub-critical water. And whenthe temperature was increase to350°C, the extraction efficiency of sub-critical waterwould have a significantly improvement. The maximum extract yield ofkerogen-decomposed bitumen at350°C was higher than that at365°C.
(III) The results of the GC-MS analysis of the kerogen-decomposed bitumenextracted by sub-ctitical water at350°C showed that the major components of thebitumen were n-alkanes,1-alkene, isoprenoid alkanes, alk-2-one and n-alkanoic acids.The content of aromatics was low in the extracts while it was high in the remainingbitumen which was survived in the oil shale residue. It indicated a selectivity ofsub-critical water that sub-critical water was apt to extract aliphatics relative toaromatics although it was capable of releasing the two kinds of compounds fromkerogen.
(IV) Three sizes of oil shale lumps (<1cm,2-4cm and6–10cm in diameter)were extracted by sub-critical water at350°C. The results showed that, the extractyield would not be affected by the size of oil shale when the extraction time washigher than20h. It was because that the oil shale lumps were fractured alone the shaletexture in direction parallel to bedding under the action of sub-critical water and thefractures were considered to be due to the tensile stress generated by expansion associated with kerogen conversion to bitumen. The results of the SEM and BETanalysis of shale residue showed that many micro-and macro-pores appeared on thesurface and interior of the samples. And the pore phenomenon would be more andmore significant with the increase in extraction time.
The fractures and the pores greatly improved the extraction ofkerogen-decomposed bitumen by sub-critical water. And the feasibility of extractinglarge-sized oil shale lumps by sub-critical water would provide some reference for theconception of oil shale in-situ extraction by sub-critical water.
(V) According to the changing actions of sub-critical water on kerogen, thewhole extraction and mass transfer process was divided into six stages:①Inactionof water,②Permeating of sub-critical water,③Swelling and decomposition ofkerogen,④Effusion of asphaltene and pre-asphaltene,⑤Dissolution of bitumenand⑥Self-separation of oil and water.
The formation rate of kerogen-decomposed bitumen was also affected by theactings changes of sub-critical water. At first, before2h, few kerogen wasdecomposed in oil shale because the sub-critical water was undergoing the permeatingprocess. Following that, during2-10h, weak-binding kerogen fragments had beenreleased from oil shale and it was the fastest formation phase of the bitumen products.After that, in10-50h, the tight-linked organic fragments were gradually releasedfrom kerogen. After50h extraction in sub-critical water, most of the organics had beenbroken down from kerogen and the new forming bitumen was very less. In addition,the released compounds would be converted into gaseous compounds in sub-criticalwater.
The chemical reactions of kerogen were also changed with the extension ofextraction. Small molecular weight cyclic hydrocarbons, aromatics and isoprenoidswere firstly released from kerogen. After that, the straight chain compounds such asn-alkanes,1-alkenes, alk-2-ones and n-alkanoic acids were cracked from the kerogenmacromolecule. Finally, some other aromatic compounds, which mighe be the corepart of the sub-units of kerogen, were released from kerogen. Moreover, with thecracking of kerogen in sub-critical water, there are also many reactions happen on the extracts, such as the secondary cracking, hydration, oxidation and rearrangementreactions. Through these reactions, the kerogen in oil shale were decomposed andextracted out by sub-critical water.
(VI) The oil shale lumps from Fushun, Nong’an and Fuyu were extracted bysub-critical water. The extract yields of the kerogen-decomposed bitumen from thesesamples were high. In which, the extract yields from Fushun and Nong’an oil shalewere higher than the oil yield from the Fischer analysis assay respectively and theextract yield of bitumen from Fuyu oil shale was also more than90%of the Fischeroil yield.
The compositions of the bituem from different oil shale samples were similar.The major components were n-alkanes, isohydrocarbons and aromatics with a certainamount of cyclic alkanes, n-alkenes, alcohols, ketones and phenols. The contents ofisohydrocarbons and aromatics in the bitumen from Fushun, Nongan and Fuyu oilshale were much higher and the flowability of these bitumen products were muchbetter than the Huadian oil shale bitumen.
油页岩资源的原位开采方法具有无需采矿、可开发较深层与高厚度的资源、产油率高、占地面积少和环境污染低等优点。目前诸多国家与大型能源公司都在积极研发各种地下原位开采技术。然而我国油页岩资源大多品位低、埋藏深，超过300m深的油页岩资源占有相当大的比例。根据传统的油页岩原位干馏技术，尚不能进行开发利用。
针对我国油页岩资源埋藏深、品位低的情况，我们提出了利用近临界水作为热传导介质和提取剂对地下油页岩资源进行原位开采的思想。本文利用高温高压反应釜研究了近临界水对大尺寸油页岩块的提取效果，考察了近临界水的提取条件、油页岩样品的质地、尺寸等因素对近临界水提取油页岩内部有机质的影响。分析了近临界水提取物的组成以及油页岩基质性状在提取过程中的变化。证明了近临界水法提取块状油页岩中有机质的可行性，为近临界水法原位提取地下油页岩的研究提供了一定的实验基础和理论依据。主要研究内容及结果如下：
（一）研究了260℃的低温近临界水对油页岩内部原有沥青化合物的萃取情况。发现在较低温度下，升高体系压强可以增强近临界水对块状油页岩的渗透作用，从而促进对有机质的提取。
萃取沥青的组成非常复杂，除了含有大量烃类物质外还存在一些环酮、茚酮、噻吩、酚类等杂原子和芳香族化合物，且其中杂原子化合物含量要比NMP-CS2混合溶剂萃取沥青中的含量高。
（二）通过对不同温度下萃取沥青的气质分析发现，升高萃取温度可以提高近临界水对油页岩内部沥青的提取能力，且获得了更多的小分子化合物。说明一些较大分子量的有机物在温度较高的近临界水中更容易转化成小分子。当提取温度高于330℃时，近临界水可以使油页岩内部的干酪根有机质分解成沥青化合物并提取出来。当近临界水的温度升至350℃时，对油页岩内部干酪根的提取效率有非常显著的提高，并且可以获得比365℃近临界水条件下更高的提取率。
（三）350℃近临界水提取出的干酪根分解沥青主要由正构烷烃、烯烃、类异戊二烯烷烃、直链的2-酮和一元羧酸组成，芳香类化合物含量相对较低。而在油页岩残渣内的残余有机质中含有较多的芳香化合物。反映出近临界水对脂肪族化合物的提取更据有倾向性。
（四）对不同尺寸的油页岩样品进行提取实验发现，当提取时间达到20h左右时，沥青的提取率几乎不再受油页岩样品尺寸影响。这是由于油页岩内部干酪根有机质在近临界水的作用下发生溶胀与分解，体积增大，产生的应力使块状油页岩样品在垂直断面上出现了许多沿着页岩层理方向的裂缝。另外，由于内部有机质的释放，油页岩样品表面与内部出现了许多毛细孔隙，并且随着提取时间的增加孔隙现象会越发显著。
油页岩块上这些裂缝与孔隙等传质通道的形成，大大提高了近临界水对块状油页岩内部有机质的提取效率。而对大尺寸油页岩内部干酪根有机质提取的可行性也为近临界水的地下油页岩原位提取设想提供了一定参考依据。
（五）根据近临界水对油页岩内部有机质作用力的变化将整个传质过程分解成：油页岩与水相对静止、近临界水的渗透、干酪根的溶胀分解、沥青质的渗出、沥青的溶解和提取物与近临界水“油水分离”6个阶段。
由于不同阶段近临界水产生作用的不同，干酪根在不同提取时间转化成沥青的速率呈现出明显的阶段性变化。在提取时间为2h之前干酪根几乎没有发生分解。2~10h是沥青生成速率最快的时间段，干酪根内部结合相对较弱的部分快速分解。10~50h时间段内干酪根中结合力相对较强部分物质开始逐渐断裂，沥青形成速率有所下降。50h后由于干酪根大分子中大部分有机质已经断裂，新沥青的生成变得很少，而释放出来的化合物越来越多的会转化成气体小分子。
干酪根在不同的提取时间段发生的化学反应也是不同的。干酪根裂解初期释放得有机物主要是小分子环烃、芳烃和类异戊二烯烷烃，然后是正构烷烃、烯烃、酮和羧酸等直链化合物的断裂，最后是干酪根亚单元核心部分的芳烃类化合物。另外干酪根的裂解产物在近临界水中还会发生二次裂解以及水解、加氢、水合、氧化、脱羧、烷基化等一系列反应。也正是通过这些反应，干酪根有机质才得以被近临界水从油页岩内部提取出来。
（六）近临界水对桦甸、抚顺、农安和扶余等不同地区油页岩的提取实验都获得了较好的提取效果。其中，近临界水对桦甸、抚顺和农安地区油页岩块的最大沥青提取率值都超过了各样品的Fischer测试含油率值。而对扶余油页岩岩芯的提取率也达到了Fischer测试含油率的90%以上。
各地区油页岩的近临界水提取物组成大体相似，主要组成为正构烷烃、异构烷烃和芳香烃化合物，另外还有一定量的环烷烃、烯烃、醇、酮、酚等化合物。抚顺、农安和扶余油页岩的提取物中异构烃和芳烃组分含量都高于桦甸油页岩的提取物，产物的流动性也比桦甸油页岩提取沥青好。
Oil shale is an organic-rich fine-grained sedimentary rock which can generateshale oil after retorting. It is a kind of unconventional oil and gas resource. Oil shaleresources are abundant in the earth. Estimates of global deposits, converted into shaleoil, are3times higher than the proved oil reserves. The resource of shale oil in Chinais second in the world next after the United States. It has a very great developmentprospects.
There is no need to mining out the oil shale by the in-situ retorting technology.The in-situ technology can exploit the deep and high thickness oil shale resourceswith several advantages as high conversion rate, few occupied space and lowenvironmental pollution. Accordingly, many countries which are rich in oil shale andsome large energy companies are actively developing the in-situ retortingtechnologies of oil shale. However, the traditional in-situ retorting technology is notapplied to Chinese oil shale for the low oil content level and high bed depth resources.
Concentrating on the characteristics of the oil shale resources in our country, weput forward the concept of using sub-critical water as a heat transfer medium andextractant to the in-situ conversion of oil shale. In this paper, high temperature andhigh pressure reactor was used to simulate the sub-critical water extraction process ofoil shale underground. The impacts of the extraction conditions of sub-critical, thesize, texture and level of the oil shale sample on the organics extraction were studied.The composition of the extracts, the extraction and mass transfer mechanism ofsub-critical water were analyzed. The extraction experiments proved the feasibility ofextracting organic matter from the large-sized oil shale lumps by sub-critical waterand provided some experimental and theoretical basis for the in-situ conversionconcept.The main research contents and results are shown as follows:
(I) Sub-critical water extraction of the natural bitumen in oil shale was performed at a low temperature,260°C. The results showed that the increase of system pressurecould enlarge the infiltration of sub-critical water at this temperature and enhance theextraction of bitumen.
The composition of the extracted bitumen was very complex. The bitumen wasconsisted of hydrocarbons, ketones, indanones, thiophenes, phenol derivatives andother heteroatomic and aromatic compounds. The content of heteroatomic compoundsin the bitumen was significantly higher than that in the NMP-CS2extracted bitumenfrom oil shale.
(II) The extract ability of sub-critical water improved with the increase oftemperature and more small molecular weight organics could be extracted compounds.It showed that some larger molecules were more likely to decomposed in sub-criticalwater at a higher temperature. When the temperature was higher than330°C, thekerogen matters in oil shale began to be decomposed in sub-critical water. And whenthe temperature was increase to350°C, the extraction efficiency of sub-critical waterwould have a significantly improvement. The maximum extract yield ofkerogen-decomposed bitumen at350°C was higher than that at365°C.
(III) The results of the GC-MS analysis of the kerogen-decomposed bitumenextracted by sub-ctitical water at350°C showed that the major components of thebitumen were n-alkanes,1-alkene, isoprenoid alkanes, alk-2-one and n-alkanoic acids.The content of aromatics was low in the extracts while it was high in the remainingbitumen which was survived in the oil shale residue. It indicated a selectivity ofsub-critical water that sub-critical water was apt to extract aliphatics relative toaromatics although it was capable of releasing the two kinds of compounds fromkerogen.
(IV) Three sizes of oil shale lumps (<1cm,2-4cm and6–10cm in diameter)were extracted by sub-critical water at350°C. The results showed that, the extractyield would not be affected by the size of oil shale when the extraction time washigher than20h. It was because that the oil shale lumps were fractured alone the shaletexture in direction parallel to bedding under the action of sub-critical water and thefractures were considered to be due to the tensile stress generated by expansion associated with kerogen conversion to bitumen. The results of the SEM and BETanalysis of shale residue showed that many micro-and macro-pores appeared on thesurface and interior of the samples. And the pore phenomenon would be more andmore significant with the increase in extraction time.
The fractures and the pores greatly improved the extraction ofkerogen-decomposed bitumen by sub-critical water. And the feasibility of extractinglarge-sized oil shale lumps by sub-critical water would provide some reference for theconception of oil shale in-situ extraction by sub-critical water.
(V) According to the changing actions of sub-critical water on kerogen, thewhole extraction and mass transfer process was divided into six stages:①Inactionof water,②Permeating of sub-critical water,③Swelling and decomposition ofkerogen,④Effusion of asphaltene and pre-asphaltene,⑤Dissolution of bitumenand⑥Self-separation of oil and water.
The formation rate of kerogen-decomposed bitumen was also affected by theactings changes of sub-critical water. At first, before2h, few kerogen wasdecomposed in oil shale because the sub-critical water was undergoing the permeatingprocess. Following that, during2-10h, weak-binding kerogen fragments had beenreleased from oil shale and it was the fastest formation phase of the bitumen products.After that, in10-50h, the tight-linked organic fragments were gradually releasedfrom kerogen. After50h extraction in sub-critical water, most of the organics had beenbroken down from kerogen and the new forming bitumen was very less. In addition,the released compounds would be converted into gaseous compounds in sub-criticalwater.
The chemical reactions of kerogen were also changed with the extension ofextraction. Small molecular weight cyclic hydrocarbons, aromatics and isoprenoidswere firstly released from kerogen. After that, the straight chain compounds such asn-alkanes,1-alkenes, alk-2-ones and n-alkanoic acids were cracked from the kerogenmacromolecule. Finally, some other aromatic compounds, which mighe be the corepart of the sub-units of kerogen, were released from kerogen. Moreover, with thecracking of kerogen in sub-critical water, there are also many reactions happen on the extracts, such as the secondary cracking, hydration, oxidation and rearrangementreactions. Through these reactions, the kerogen in oil shale were decomposed andextracted out by sub-critical water.
(VI) The oil shale lumps from Fushun, Nong’an and Fuyu were extracted bysub-critical water. The extract yields of the kerogen-decomposed bitumen from thesesamples were high. In which, the extract yields from Fushun and Nong’an oil shalewere higher than the oil yield from the Fischer analysis assay respectively and theextract yield of bitumen from Fuyu oil shale was also more than90%of the Fischeroil yield.
The compositions of the bituem from different oil shale samples were similar.The major components were n-alkanes, isohydrocarbons and aromatics with a certainamount of cyclic alkanes, n-alkenes, alcohols, ketones and phenols. The contents ofisohydrocarbons and aromatics in the bitumen from Fushun, Nongan and Fuyu oilshale were much higher and the flowability of these bitumen products were muchbetter than the Huadian oil shale bitumen.
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