CN105481211A - 超声强化超临界萃取油泥的方法 - Google Patents
超声强化超临界萃取油泥的方法 Download PDFInfo
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- CN105481211A CN105481211A CN201410484985.XA CN201410484985A CN105481211A CN 105481211 A CN105481211 A CN 105481211A CN 201410484985 A CN201410484985 A CN 201410484985A CN 105481211 A CN105481211 A CN 105481211A
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- extraction
- supercritical extraction
- greasy filth
- supercritical
- ultrasonic
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- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 42
- 239000010802 sludge Substances 0.000 title abstract description 14
- 238000000605 extraction Methods 0.000 claims abstract description 58
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 238000005728 strengthening Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 8
- 238000002604 ultrasonography Methods 0.000 claims description 7
- OTMSDBZUPAUEDD-UHFFFAOYSA-N ethane Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N carbon dioxide Chemical compound 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O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
本发明公开了一种超声强化超临界萃取油泥的方法，油泥和萃取剂进入带有强化超声装置的超临界萃取装置，设定超临界萃取压力及超临界萃取温度，进行超临界萃取。与现有技术相比，本发明方法采用超声强化超临界萃取技术，从而降低了萃取压力和温度，缩短了萃取时间，最终提高了萃取率。
Description
技术领域
[0001] 本发明涉及对含油污泥的处理方法，特别是采用萃取方法分离油泥的方法。
背景技术
[0002] 油泥主要是指由于各种原因造成的原油或其它油品与泥土等形成的含油污泥，以 及油田正常生产中系统带出的含油泥沙等，是一种富含矿物油的固体废物，主要成分是原 油、泥和水。固体颗粒尺寸可从不足微米到几英寸，大多数在1至100微米之间，油的组成 取决于原油种类、炼油厂结构与操作条件，污泥的组成可能随时间变化而变化。通常污泥中 含有一定的原油（浓度质量5%~80%)、重金属离子（如铁、铜、镍等）与无机盐类（浓 度质量5%~20% )化合物等。这些油泥中一般含有苯系物、酚类等物质，并伴随恶臭和毒 性，若直接和自然环境接触，会使土地毒化、酸化或碱化，导致土壤及土质结构的改变，妨碍 植物根系生长并会对水体和植被造成较大污染，同时也意味着石油资源的浪费。
[0003] 按国家危险废物名录，油泥被列为危险废物，其对环境危害的长期性和潜在性， 正引起高度重视。开展油泥管理及防治技术研究是目前国家环保工作的一项重要任务。因 此，如何把这些含油污泥进行无害化和资源化利用，也是摆在炼油行业面前亟待解决的一 个重要环保问题。
[0004] 目前处理含油污泥的技术主要有资源回收、无害化处理和综合利用技术等。资源 回收处理技术包括溶剂萃取法、水洗法、微乳洗涤、破乳法等。油泥无害化处理处理技术包 括固定化处理，生物处理、焚烧等技术。综合利用技术包括热分解、制砖铺路以及其它用途。 油泥的处理技术多种多样，每种方法都有各自的优缺点和适用范围。随着环保法规的日益 严格和完善，油田含油泥砂处理技术将引起高度重视，含油污泥砂无害化、资源化、综合利 用处理技术将成为油泥砂处理技术发展的必然趋势。
[0005] 溶剂萃取法是油泥处理技术中常用的一种，其利用"相似相溶"原理，选择合适的 有机溶剂作萃取剂，将有机物从油泥中被溶剂抽提出来后，通过蒸馏把溶剂从混合物中分 离出来循环使用，回收的原油则用于回炼。
[0006] US484271采用萃取氧化氧化法对含油污泥进行处理，先在污泥中加入一种轻质烃 作萃取剂，经过萃取后，油和大部分有机物被去除，残留的污泥用HN03在200~375C及常 压条件下氧化处理。
[0007] CN02133117. 0采用"热萃取-脱水-固液分离"的技术处理含油污泥，将含油污泥 进行机械脱水，然后与萃取溶剂油混合并预热，混合均匀后进行热萃取-脱水处理，然后进 行固液分离，液相进入焦化装置，固相可作为燃料，热萃取-脱水的汽相经冷凝后进行油水 分离。该方法过程简单、无需特殊设备，投资及操作费用低，不但有效处理了含油污泥，而且 其中有价值成分得到了充分的利用，同时不会给后处理装置带来不利影响。
[0008] 溶剂萃取法的优点是处理含油污泥较彻底，能够将大部分石油类物质提取回收。 但是由于萃取剂价格昂贵，而且在处理过程中有一定的损失，故萃取成本较高，这也制约了 溶剂萃取法在油泥分离上的应用。
[0009] 超临界萃取是近三十年来迅速发展起来的一种新型萃取分离技术。超临界流体是 指温度和压力处于临界温度和临界压力以上的流体。超临界流体是介于气体和液体之间的 特殊流体，兼有气体和液体的双重物性，其密度接近于液体的密度，对液体和固体的溶解能 力接近于普通的液体溶剂，而黏度和扩散速度接近于普通气体。因此，超临界流体具有较好 的渗透性和较强的溶解能力，以及很高的传质速率和很快达到萃取平衡的能力。超临界萃 取就是利用超临界流体的这种特性萃取分离物质，然后借助等温降压或等压升温的方法使 超临界流体变成普通气体，即可将萃取剂与待分离物质分离。
[0010] 超临界萃取分离技术与传统的溶剂萃取分离方法相比在溶解能力、传递性能和溶 剂回收等方面都具有许多优点：其具有与普通液体溶剂相近的溶解能力.而且拥有与气体 一样的传递特性。即比液体溶剂渗透快，能更快地达到平衡；可选用化学稳定性好、临界温 度接近常温、无毒、无腐蚀性的物质作为提取剂，替代传统的有毒溶剂，真正实现生产过程 绿色化；其提取能力取决于流体密度，可通过调节主要操作参数（温度和压力）来比较容易 地加以控制；溶剂回收简单方便.通过等温降压或等压升温.提取物就可与提取剂分离，而 提取剂只需重新压缩就可循环使用，节省能源。
[0011] AvilaCh3vezM. A[SeparationScienceandTechnology, 2007,42 (10) :2327-2345], 等利用一种特制的超临界流体萃取装置，采用超临界乙烷萃取剂从原油罐底泥中提取烃， 研究认为最大的萃取率对应于最高溶剂密度的压力和温度，萃取的烃组分明显增浓。但是 由于油泥的乳化程度高，固体杂质多，为复杂的水-油-固稳定结构，采用常规的萃取或超 临界萃取方法，需要的萃取时间长，萃取效率低，限制了其应用。
发明内容
[0012] 针对现有技术的不足，本发明提供了一种超临界萃取分离油泥的方法，本发明方 法具有萃取效率1¾的优点。
[0013] 本发明超声强化超临界萃取油泥的方法包括：油泥和萃取剂进入带有强化超声装 置的超临界萃取装置，设定超临界萃取压力及超临界萃取温度，进行超临界萃取。萃取剂选 择二氧化碳、甲烷、乙烷、丙烷或乙烯，优选为二氧化碳或乙烷。
[0014] 萃取剂与油泥用量比为每克油泥使用20~50ml萃取剂，超临界萃取压力为3~ 8MPa，超临界萃取温度为30~100°C，超临界萃取时间为2~6h。
[0015] 按照权利要求1所述的方法，其特征在于：超声波频率为20~40kHz，超声波功率 密度为40~100W/L (即每升物料使用的超声波功率），超声波连续辐照或者间歇辐照，间歇 辐照时的间歇时间为（6~12s)八6~12s)
[0016] 萃取后的物料进入一级分离器、二级分离器进行分离，溶剂气化后循环使用，萃取 物从分离器底部放出，进入油水分离器分离，水相进行污水处理。油相沉降分离后，得到油 分和固体物，固体物经脱油干燥或固化后作为燃料。所得油分可回炼厂作加工处理。
[0017] 超临界萃取可以采用连续操作，也可以采用间歇式操作。
[0018] 本发明针对油泥萃取或超临界萃取时，由于油泥结构稳定造成的萃取困难，萃取 时间长，萃取效率低的不足，在适当超临界萃取的基础上，增加超声波强化。超声强化超临 界萃取技术是在超临界萃取的同时附加超声场，从而降低萃取压力和温度，缩短萃取时间， 最终提高萃取率。对于油泥来说，由于是稳定的油-水-固结构，采用适宜的超声场，可以 使该稳定结构产生振荡、解体，加快了相间传质速度，有利于萃取的进行，进而提高了萃取 效率。
附图说明
[0019] 图1是本发明工艺流程示意图。
具体实施方式
[0020] 超临界流体萃取影响因素主要有萃取条件，包括压力、温度、时间等；原料的性质 和超临界流体的种类。其中超临界流体的选择至关重要。在超临界流体萃取过程中，要求 超临界流体具有良好的溶解性能和良好的选择性。同时出于安全、经济和环保的考虑，对于 超临界流体还有如下要求；化学性质稳定，无毒性和无腐蚀性，不易燃和不易爆的；超临界 流体的操作温度应接近于常温，以便节约能源，并使操作温度低于待分离成分的分解温度； 超临界流体的操作压力应尽可能的低，以降低压缩机的动力消耗；来源广泛，价格便宜。结 合油泥的性质，本发明选择二氧化碳、甲烷、乙烷、丙烷及其它低分子烷烃、乙烯及其它低分 子烯烃等作为超临界萃取剂，其临界数据如表1所示。
[0021] 表1部分超临界流体溶剂的临界数据
[0022]
[0023] 萃取过程中超临界流体密度的变化直接影响萃取效果，萃取压力是影响超临界相 密度的重要参数。根据萃取压力的变化，可将超临界流体分为三类。即高压时，超临界流体 的溶解能力强，可最大限度地溶解所有成分，低压临界区仅能提取易溶解的成分或除去有 害成分，中压区的选择萃取在高低压之问，可根据物料萃取的要求选择适宜的压力进行有 效萃取。本发明针对油泥的性质，以及选择的萃取剂性质，同时考虑附加的超声强化作用， 选择的萃取压力为3~8MPa。
[0024] 在临界点附近的低压区，升高温度虽然可提高分离组分的挥发度和扩散能力，但 不足以补充超临界流体的密度随温度升高而急剧下降所导致溶解能力下降。在高压区，超 临界流体的密度大，可压缩性小，此时升高温度可以提高待分离组分的蒸汽压和扩散系数， 从而提高了溶质的溶解能力。针对油泥的性质及本发明采用超声强化，采用较低的萃取温 度30~70C。
[0025] 具体实施例1:
[0026] 以某炼厂油罐底油泥为例说明本发明具体实施例。油泥含油65wt%，含水 18wt%，其余为固体物质。选择C02作为超临界萃取剂。超声功率密度为100W/L，频率为 20kHz，辐照方式为6s/6s (超声连续辐照时间/超声间歇时间）。萃取剂与油泥的用量为 30ml/g (油泥原料）。
[0027] 油泥经机械搅拌脱水后送入超临界萃取釜。超声的强化方式采用内置插入式，超 声换能器直接置于萃取罐中，超声波发生器将转为超声频的电能传给换能器，再由换能器 把电能转化为超声频机械能。从储罐（C00出来的液态C0]经过滤系统进行净化，然后通过 高压泵输送到预热器中预热，预热至设定温度后，进入萃取釜中达到设定萃取压力和萃取 温度，萃取温度为30~50°C，萃取压力为3~6MPa，萃取时间为2h。在萃取釜中C0]与原 料相接触，被萃取成分溶解在C0]中进行萃取。萃余物进行沉降分离后，得到少许油分和固 体物，固体物固化后作为燃料。萃取物随C0]流体先后进入一级分离器和二级分离器，萃取 物与C0]分离开，通过接收系统接收；0]则从二级分离器分离出并重复利用。经强化超声 超临界萃取油泥的萃取率在不同的操作条件下为95%-99% (质量）。萃取物从分离器底 部放出，进入油水分离器分离，水相进行污水处理。油相可回炼厂，进入催化裂化或焦化工 艺。
[0028] 具体实施例2 :
[0029] 以某炼厂油罐底油泥为例说明本发明具体实施例。油泥含油65%，含水18%，其 余为固体物质。选择乙烧作为超临界萃取剂。萃取温度为30~100C，萃取压力为5~8MPa， 萃取剂与油泥的用量为40ml/g (油泥原料），萃取时间为2. 5h。超声功率密度为80W/L，频 率为20kHz，辐照方式为6s/6s (超声连续辐照时间/超声间歇时间）。工艺流程同实施例 1，油泥的萃取率为95%-99% (质量）。
Claims (6)
1. 一种超声强化超临界萃取油泥的方法，其特征在于：油泥和萃取剂进入带有强化超 声装置的超临界萃取装置，设定超临界萃取压力及超临界萃取温度，进行超临界萃取。
2. 按照权利要求1所述的方法，其特征在于：萃取剂选择二氧化碳、甲烷、乙烷、丙烷或 乙烯。
3. 按照权利要求1或2所述的方法，其特征在于：萃取剂与油泥用量比为每克油泥使 用20~50ml萃取剂，超临界萃取压力为3~8MPa，超临界萃取温度为30~100°C，超临界 萃取时间为2~6h。
4. 按照权利要求1所述的方法，其特征在于：超声波频率为20~40kHz，超声波功率 密度为40~100W/L，超声波连续辐照或者间歇辐照，间歇辐照时的间歇时间为（6~12s)/ (6 ~12s)。
5. 按照权利要求1所述的方法，其特征在于：萃取后的物料进入一级分离器、二级分离 器进行分离，溶剂气化后循环使用，萃取物从分离器底部放出，进入油水分离器分离，水相 进行污水处理。
6. 按照权利要求1所述的方法，其特征在于：超临界萃取采用连续操作，或者采用间歇 式操作。
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