CN103693825B - 一种含油污泥的资源化处理方法 - Google Patents
一种含油污泥的资源化处理方法 Download PDFInfo
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- CN103693825B CN103693825B CN201210366893.2A CN201210366893A CN103693825B CN 103693825 B CN103693825 B CN 103693825B CN 201210366893 A CN201210366893 A CN 201210366893A CN 103693825 B CN103693825 B CN 103693825B
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- extraction
- oily sludge
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- 239000003921 oil Substances 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 43
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-butanone Chemical group 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- CTQNGGLPUBDAKN-UHFFFAOYSA-N o-xylene Chemical compound 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CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 abstract description 16
- 239000002131 composite material Substances 0.000 abstract description 12
- 230000003019 stabilising Effects 0.000 abstract description 3
- 239000000446 fuel Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound 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[C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 2
- 239000003245 coal Substances 0.000 abstract 2
- 238000010304 firing Methods 0.000 abstract 1
- 238000004065 wastewater treatment Methods 0.000 description 14
- 238000011084 recovery Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000295 fuel oil Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
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- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound 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- 239000002699 waste material Substances 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N Anthracene Chemical compound 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Abstract
本发明涉及一种含油污泥资源化的处理方法，特别是发明一种复合萃取剂，处理炼油厂污水处理过程中产生的含油污泥。本发明是将经过离心脱水后含水率较高的含油污泥，在温度较高的条件下与复合萃取剂混合，破坏含油污泥中水、油、固稳定体系，进行萃取处理，对萃取后的混合物进行固液分离，分离出的固相进行干化，形成固体残渣与煤混合，可作为燃煤锅炉的燃料使用，分离出的油和萃取剂直接进入原油加工系统进行回炼。过程中生成的废水经过生化处理后达标排放，本发明的主要特点在于，萃取效率高、装置流程短，设备投资低。
Description
技术领域
[0001] 本发明涉及含油污泥的一种萃取处理方法，特别是炼油厂、炼油污水处理厂产生 的含油污泥无害化、资源化的处理工艺。
背景技术
[0002] 炼化企业在石油炼制和废水处理过程中产生大量的含油污泥，它们主要来自隔油 池、浮选池、生物活性污泥、原油脱水罐、储油罐和污油罐等。这些污泥成分复杂，属于较稳 定的多相体系，一般由水包油、油包水以及悬浮固体组成，且乳化充分，黏度较大，固相难以 彻底沉降，处理难度较大。目前，我国石油化工行业中，平均每年约产生80万吨含油污泥。 随着企业生产装置规模的不断扩大，这些企业在创造经济效益的同时，也对环境产生了巨 大的压力。相应的废渣排放总量及种类也在逐步地增加，使得企业排污总量和污染治理费 用也呈现上升的趋势。废固的无害化资源化利用已被列为建设节约性社会的重要工作内 容，按照新的法规、标准，许多企业对含油污泥的处置很难达到要求，造成企业排污负担加 重，环境污染隐患突出。
[0003] 近20年以来，虽然有多种有关含油污泥的研究报道，而含油污泥的处理技术也多 种多样，每种方法各有各自的优缺点和使用范围，现今含油污泥的处理技术难以得到推广 应用形成工业化生产。目前，含油污泥处理问题一直难以得到经济合理地解决，常常采用露 天堆放或填埋方式处理，这些污泥中一般含有烃类、苯系物、酚类和蒽类等物质，并伴随恶 臭和毒性，若直接和自然环境接触，会对土壤、水体和植被造成较大污染，同时也造成石油 资源的浪费。
[0004] CN1488591A提出了一种含油污泥的处理方法，将含油污泥进行机械脱水，然后与 萃取剂混合并预热，混合均质后进行热萃取-脱水处理，然后进行固液分离，液相进入焦化 装置，固相作为燃料。该技术在萃取过程中仅使用一种萃取剂与含油污泥中结构复杂的石 油类物质的相容性有很大的局限性，萃取效果有限。
[0005] CN101823824B、CN200910079177. 4提出含油污泥处理工艺中，所述的萃取剂为 c4~c2。中烃类中的一种，与含油污泥中结构复杂的石油类物质的相容性有很大的局限性，萃 取效果有限。
[0006] CN1526797A提出一种含油污泥萃取方法，选用萃取剂为轻质煤焦油（常压下沸点 45°C~90°C )，石油醚、轻质油或C5，仅使用一种萃取剂，含油污泥经过萃取后油萃取不易彻 底。
[0007] CN1765781A提出一种含油污泥的处理方法，采用萃取剂与含油污泥混合、萃取蒸 发脱水处理及固液分离，其特征在于多效多级或单效多级萃取蒸法系统，所述的多效多级 萃取蒸发系统的操作条件如下：其第一级采用常压，温度为95~115°C，最后一级压力为 0. 01~0. 60MPa，温度为125~175°C。该技术使用的萃取剂为单一种类萃取剂，针对含油 污泥复杂的石油类物质的相容性有很大的局限性，萃取效果有限。
[0008] CN1178777A提出一种含油污泥的处理方法，将含油污泥预脱水之后，在减压蒸馏 釜内控制一定的压力和温度，蒸出污泥中全部的水和部分油，将剩下的油和泥渣自然分离 沉降分离，泥渣加入洗涤水洗涤，洗涤水送入污水处理池，分出的渣排出后进行常规处理。 该方法生成废水量大，污泥残渣的处理不彻底。
[0009] US4990237公开了一种从含油污泥中回收油的方法，主要是采用常压或微负压下， 通过低温和高温两个蒸发段，对含油污泥中的油进行全部蒸发。该方法工艺流程长，设备复 杂，操作条件苛刻，能耗大。另外，还有部分专利文献也分别涉及含油污泥的处理，但是这些 专利文献所涉及的含油污泥处理技术存在着能量消耗高、工艺流程复杂、操作条件苛刻或 含油污泥处理不够彻底等方面的不足之处。
发明内容
[0010] 为了克服现有技术的不足，本发明提供了一种复合萃取剂，由传统的单一种萃取 剂改用复合萃取剂，提高了含油污泥中结构复杂的石油类物质的相容性。含水率较高的含 油污泥，经过加热后，破坏了油泥中油、水、沙土之间形成的稳定体系，有利于萃取的进行。 该工艺流程短，操作温度低，能量消耗低，实现含油污泥无害化处理和资源化利用。
[0011] 本发明提供了一种含油污泥处理方法，步骤如下：
[0012] (1)将污水处理厂产生的含水率在50. 0~90.0 wt%的含油污泥送入萃取罐，在 100~180°C下，压力0. 10~0. 80MPa与萃取剂混合进行萃取，萃取时间20~60min，萃取 剂与含油污泥的质量比为（200~1) :1 ;
[0013] (2)萃取过程中产生的蒸汽经过冷凝、分离后，分离出来的水由于CODcr含量较 低，可以直接进入污水处理系统，处理达标后排放；分离出来的油可以进入原油系统，进行 回炼使用。
[0014] (3)待萃取结束后，将固液混合物送入固液分离器，分离出的液相混合物直接送往 原油加工系统，进行回炼；固相进入干化设备，在温度为110~188°C，压力为20~IOOkpa (绝压）下干化20~85min后得到固体废渣。
[0015] 适宜的工艺条件和萃取剂是含油污泥处理技术的关键。本发明含油污泥处理过程 中优选的操作范围如下：萃取处理时的温度为120~160°C，操作压力为0. 20~0. 60MPa， 萃取时间为25~45min，萃取剂与含油污泥的质量比为（20~1) :1。
[0016] 本发明所述的萃取剂是一种复合萃取溶剂，以萃取溶剂的总体积为100%计，含 有：
[0017] 主剂厶，沸程为110~135°(：的馏分油，占85%~100%^八） ；
[0018] 副剂B，沸程为140~150°C的馏分油，占0~15% (v/v);
[0019] 助剂C，沸程为80~100°C的馏分油或者工业纯产品，占0~5% (v/v)。
[0020] 本发明所述的馏分油为石脑油、轻质油等。
[0021] 本发明所述的助剂C可以为丁酮、庚烷、二甲苯等工业纯产品。
[0022] 本发明所述的主剂A优选为沸程为120~130°C的馏分油。
[0023] 本发明的主要特点在于，针对萃取含油污泥并回收溶剂工艺，选择石油产品 110~135°C的馏分油作为含油污泥萃取的主溶剂，石油产品馏分油与含油污泥中的油分 一样含有多种相类似且同源的石油类物质，相似相容效果较好，因此所选的馏分油对含油 污泥中分子量分布较宽的油分有优越的溶解能力，同时可以兼顾部分更高分子量的沥青质 和重油组分。
[0024] 本发明另一特点在于在主溶剂中加入少量的沸程较高的副剂B，含油污泥中总会 有部分重油组分很难被萃取出来，少量沸程较高的副剂B的加入会使溶剂对含油污泥中的 沥青质和重油成分的溶解能力有所加强。
[0025] 本发明同时也使用少量的低沸程助剂C来实现调整主溶剂的目的。现有技术中萃 取过程大部分在30~90°C温度下进行，少量较低沸点的油分可以在主溶剂中形成局部的 溶液错动，使溶解过程中物料的转移更顺畅。
[0026] 本发明所述的含油污泥包括油田与炼化企业所产生的含油污泥。
[0027] 本发明所述将离心脱水后的含油污泥直接加入萃取罐，萃取罐上部安装有搅拌 器，萃取剂进入萃取罐内，启动搅拌器进行搅拌混合萃取，物料混合均匀后停止搅拌，将混 合物料由罐底部打入固液分离设备，分离出的液体直接进入原油加工系统进行回炼。
[0028] 本发明所述的萃取设备，采用间壁式加热，加热介质一般采用饱和蒸汽，也可以采 用导热油、烟道气加热。
[0029] 本发明所述的固液分离采用沉降分离或离心分离。
[0030] 本发明所述的萃取设备可以是釜式间歇操作，也可以使塔式连续操作。
[0031] 本发明所述的含油污泥干化设备最好为间壁式传热干化处理设备，包括旋转窑、 各种旋转式蒸发加热器、浆叶式设备干燥机等，加热介质包括高、低压蒸气、导热油、烟道气 等。
[0032] 本发明中经萃取后的固相进入旋转蒸发器，干化后的最终固体废渣的石油类物质 含量更低。
[0033] 本发明采用"热萃取-油回炼"的联合处理方法。其优点在于：①将含油污泥经过 热萃取脱水后，破坏了含油污泥中"油、水、沙土"所形成的稳定体系，更有利于萃取的进行。 ②采用复合萃取剂，对于复杂的含油污泥体系相容性更好，萃取更彻底；③所采用的萃取剂 本身来源于石油的不同馏分，萃取剂不需要回收再生，大大缩短了含油污泥处理过程中因 萃取剂再生带来的一系列问题(如流程长、设备多、操作复杂、能耗高等)。
具体实施方式
[0034] 实施例和对比例所述的" ％ (v/v) "指体积百分含量，其余没标注的" ％ "为质量百 分含量。
[0035] 从含油污泥中通过萃取分离出来的油分的质量的测定方法。萃取前后含油污泥质 量的差值减去等量含油污泥的含水量既是萃取出的油分量。
[0036] 含油污泥中可萃出油分的测定方法。一定量的含油污泥在大量萃取剂的条件下， 多次萃取，直到某次萃取前后干油泥的质量差小于原质量的〇. 1 %为止。
[0037] 萃出油分占含油污泥中总可萃油分的比例(可萃油分回收率P%):
[0038]
[0039] 实施例1 :
[0040] 溶剂配方为：萃取溶剂主剂选用沸程石脑油110~125°C沸程的馏分油，占85% ;副 剂选用沸程为140~150°C的馏分油，占10%;助剂沸程为80~100°C的馏分油，占5. 0%， 组成复合萃取剂。某炼油污水处理厂产生的含油污泥经过机械脱水后，含水率为65. Owt %， 油含量为20.0 wt %。萃取剂与含油污泥的质量比为1:1，该含油污泥送入萃取罐，在120°C 下，压力0. 20MPa与萃取剂混合进行萃取，萃取时间20min，待萃取结束后，将固液混合物送 入离心分离器，分离出的液相直接进入原油加工系统装置，固相进入浆叶式污泥干化机，在 温度为180°C，压力为80KPa (绝压)下干化60min后得到最终固体废渣。分析结果表明：该 处理方法最终生成的残渣可萃油分回收率为93. 2%。
[0041] 对比例1 :
[0042] 溶剂配方为：萃取溶剂全部选用沸程石脑油110~125°C沸程的馏分油，占100%。 某炼油污水处理厂产生的含油污泥经过机械脱水后，含水率为65. Owt %，油含量为 20.0 wt%。萃取剂与含油污泥的质量比为1:1，该含油污泥送入萃取罐，在120°C下，压力 0. 20MPa与萃取剂混合进行萃取，萃取时间20min，待萃取结束后，将固液混合物送入离心 分离器，分离出的液相直接进入原油加工系统装置，固相进入浆叶式污泥干化机，在温度为 180°C，压力为SOKPa (绝压)下干化60min后得到最终固体废渣。分析结果表明：该处理方 法最终生成的残渣可萃油分回收率为90. 5%。
[0043] 实施例2 :
[0044] 溶剂配方为：萃取溶剂主剂选用沸程石脑油110~125°C沸程的馏分油，占90%;副 剂选用沸程为140~150°C的馏分油，占5% ;助剂沸程为80~100°C的馏分油，占5. 0%， 组成复合萃取剂。某炼油污水处理厂产生的含油污泥经过机械脱水后，含水率为75. Owt %， 油含量为15. Owt %。萃取剂与含油污泥的质量比为5:1，该含油污泥送入萃取罐，在140 °C 下，压力0. 40MPa与萃取剂混合进行萃取，萃取时间40min，待萃取结束后，将固液混合物送 入离心分离器，分离出的液相直接进入原油加工系统装置，固相进入浆叶式污泥干化机，在 温度为160°C，压力为60KPa (绝压)下干化40min后得到最终固体废渣。分析结果表明：该 处理方法最终生成的残渣可萃油分回收率为94. 0%。
[0045] 对比例2 :
[0046] 溶剂配方为：萃取溶剂主剂选用沸程石脑油110~125°C沸程的馏分油，占90%; 副剂选用沸程为140~150°C的馏分油，占5%;助剂沸程为80~100°C的馏分油，占5. 0%， 组成复合萃取剂。某炼油污水处理厂产生的含油污泥经过机械脱水后，含水率为75. Owt %， 油含量为15. Owt%。萃取剂与含油污泥的质量比为5:1，该含油污泥送入萃取罐，在80°C 下，常压下与萃取剂混合进行萃取，萃取时间40min，待萃取结束后，将固液混合物送入离心 分离器，分离出的液相直接进入原油加工系统装置，固相进入浆叶式污泥干化机，在温度为 160°C，压力为60KPa (绝压)下干化40min后得到最终固体废渣。分析结果表明：该处理方 法最终生成的残渣可萃油分回收率为76. 0%。
[0047] 实施例3 :
[0048] 溶剂配方为：萃取溶剂主剂选用沸程石脑油110~125°C沸程的馏分油，占95%;副 剂选用沸程为140~150°C的馏分油，占2. 5%;助剂沸程为80~100°C的馏分油，占2. 5%， 组成复合萃取剂。某炼油污水处理厂产生的含油污泥经过机械脱水后，含水率为85. Owt %， 油含量为9. Owt %。萃取剂与含油污泥的质量比为15:1，该含油污泥送入萃取罐，在160°C 下，压力0. 50MPa与萃取剂混合进行萃取，萃取时间60min，待萃取结束后，将固液混合物送 入离心分离器，分离出的液相直接进入原油加工系统装置，固相进入浆叶式污泥干化机，在 温度为120°C，压力为20KPa (绝压)下干化20min后得到最终固体废渣。分析结果表明：该 处理方法最终生成的残渣可萃油分回收率为93. 0%。
[0049] 对比例3 :
[0050] 溶剂配方为：萃取溶剂全部选用沸程为80~100°C的馏分油。某炼油污水处理厂 产生的含油污泥经过机械脱水后，含水率为85. Owt %，油含量为9. Owt %。萃取剂与含油污 泥的质量比为15: 1，该含油污泥送入萃取罐，在60°C下，常压下与萃取剂混合进行萃取，萃 取时间60min，待萃取结束后，将固液混合物送入离心分离器，分离出的液相直接进入原油 加工系统装置，固相进入浆叶式污泥干化机，在温度为120°C，压力为20KPa (绝压）下干化 20min后得到最终固体废渣。分析结果表明：该处理方法最终生成的残渣可萃油分回收率 为 65.0%。
[0051] 实施例4:
[0052] 溶剂配方为：萃取溶剂主剂选用沸程石脑油110~125°C沸程的馏分油，占85%;副 剂选用沸程为140~150°C的馏分油，占10%;助剂沸程为80~100°C的馏分油，占5. 0%， 组成复合萃取剂。某炼油污水处理厂产生的含油污泥经过机械脱水后，含水率为70. Swt %， 油含量为15. 2wt %。萃取剂与含油污泥的质量比为8:1，该含油污泥送入萃取罐，在120°C 下，压力0. 20MPa与萃取剂混合进行萃取，萃取时间20min，待萃取结束后，将固液混合物送 入离心分离器，分离出的液相直接进入原油加工系统装置，固相进入浆叶式污泥干化机，在 温度为180°C，压力为80KPa (绝压)下干化60min后得到最终固体废渣。分析结果表明：该 处理方法最终生成的残渣可萃油分回收率为94. 5%。
[0053] 对比例4:
[0054] 溶剂配方为：萃取溶剂全部选用沸程石脑油110~125°C沸程的馏分油，占90%，副 剂选用沸程为140~150°C的馏分油，占10%。某炼油污水处理厂产生的含油污泥经过机 械脱水后，含水率为70. 8wt%，油含量为15. 2wt%。萃取剂与含油污泥的质量比为8:1，该 含油污泥送入萃取罐，在120°C下，压力0. 20MPa与萃取剂混合进行萃取，萃取时间20min， 待萃取结束后，将固液混合物送入离心分离器，分离出的液相直接进入原油加工系统装置， 固相进入浆叶式污泥干化机，在温度为180°C，压力为SOKPa (绝压)下干化60min后得到最 终固体废渣。分析结果表明：该处理方法最终生成的残渣可萃油分回收率为90. 6%。
[0055] 实施例5 :
[0056] 溶剂配方为：萃取溶剂主剂选用沸程石脑油110~125°C沸程的馏分油，占85%;副 剂选用沸程为140~150°C的馏分油，占10%;助剂沸程为80~100°C的馏分油，占5. 0%， 组成复合萃取剂。某炼油污水处理厂产生的含油污泥经过机械脱水后，含水率为82. Owt %， 油含量为8. Owt%。萃取剂与含油污泥的质量比为5:1，该含油污泥送入萃取罐，在120°C 下，压力0. 20MPa与萃取剂混合进行萃取，萃取时间20min，待萃取结束后，将固液混合物送 入离心分离器，分离出的液相直接进入原油加工系统装置，固相进入浆叶式污泥干化机，在 温度为180°C，压力为80KPa (绝压)下干化60min后得到最终固体废渣。分析结果表明：该 处理方法最终生成的残渣可萃油分回收率为94. 1%。
[0057] 对比例5 :
[0058] 溶剂配方为：萃取溶剂全部选用沸程石脑油110~125°C沸程的馏分油，占90%，副 剂选用沸程为80~100°C的馏分油，占10% ;。某炼油污水处理厂产生的含油污泥经过机 械脱水后，含水率为82. Owt%，油含量为8. Owt%。萃取剂与含油污泥的质量比为5:1，该含 油污泥送入萃取罐，在120°C下，压力0. 20MPa与萃取剂混合进行萃取，萃取时间20min，待 萃取结束后，将固液混合物送入离心分离器，分离出的液相直接进入原油加工系统装置，固 相进入浆叶式污泥干化机，在温度为180°C，压力为SOKPa (绝压)下干化60min后得到最终 固体废渣。分析结果表明：该处理方法最终生成的残渣可萃油分回收率为90. 9%。
[0059] 实施例6:
[0060] 溶剂配方为：萃取溶剂主剂选用沸程石脑油110~125°C沸程的馏分油，占85% ;副 剂选用沸程为140~150°C的馏分油，占10%;助剂沸程为80~100°C的馏分油，占5. 0%， 组成复合萃取剂。某炼油污水处理厂产生的含油污泥经过机械脱水后，含水率为75. Owt %， 油含量为12. Owt %。萃取剂与含油污泥的质量比为2:1，该含油污泥送入萃取罐，在120°C 下，压力0. 20MPa与萃取剂混合进行萃取，萃取时间20min，待萃取结束后，将固液混合物送 入离心分离器，分离出的液相直接进入原油加工系统装置，固相进入浆叶式污泥干化机，在 温度为180°C，压力为80KPa (绝压)下干化60min后得到最终固体废渣。分析结果表明：该 处理方法最终生成的残渣可萃油分回收率为92. 4%。
[0061] 对比例6:
[0062] 溶剂配方为：萃取溶剂全部选用沸程石脑油60~200°C沸程的市售石脑油，占 100%。某炼油污水处理厂产生的含油污泥经过机械脱水后，含水率为75. Owt %，油含量为 12. Owt%。萃取剂与含油污泥的质量比为2:1，该含油污泥送入萃取罐，在120°C下，压力 0. 20MPa与萃取剂混合进行萃取，萃取时间20min，待萃取结束后，将固液混合物送入离心 分离器，分离出的液相直接进入原油加工系统装置，固相进入浆叶式污泥干化机，在温度为 180°C，压力为SOKPa (绝压)下干化60min后得到最终固体废渣。分析结果表明：该处理方 法最终生成的残渣可萃油分回收率为80. 6%。
Claims (6)
1. 一种含油污泥的处理方法，步骤如下： (1)将污水处理厂产生的含水率在50.0 ~90.0 wt%的含油污泥送入萃取罐，在100~ 180°C下，压力0. 10~0. 80MPa与萃取剂混合进行萃取，萃取时间20~60min，萃取剂与含 油污泥的质量比为（200~I) : 1 ;(2)萃取过程中产生的蒸汽经过冷凝、分离出来的水进 入污水处理系统，处理达标后排放；分离出来的油进入原油系统，进行回炼使用；（3)待萃 取结束后，将固液混合物送入固液分离器，分离出的液相混合物直接送往原油加工系统，进 行回炼；固相进入干化设备，在温度为110~188°C，压力为20~IOOKPa下干化20~85min 后得到固体废渣；以萃取溶剂的总体积为100%计，所述的萃取剂含有： 主剂：沸程为11〇~135°(：的馏分油，占85%~95%^八） ； 副剂：沸程为140~150°C的馏分油，占2. 5%~10% (v/v); 助剂：沸程为80~100°C的馏分油，占2. 5%~5% (v/v)。
2. 如权利要求1所述的处理方法，其特征在于所述的馏分油为石脑油、轻质油。
3. 如权利要求1所述的处理方法，其特征在于所述的助剂为丁酮、庚烷、二甲苯。
4. 如权利要求1所述的处理方法，其特征在于所述的主剂为沸程为120~130°C的馏 分油。
5. 如权利要求1所述的处理方法，其特征在于萃取处理时的温度为120~160°C，操 作压力为〇. 20~0. 60MPa，萃取时间为25~45min，萃取剂与含油污泥的质量比为（20~ 1) ： 1〇
6. 如权利要求1所述的处理方法，其特征在于所述的固液分离采用沉降分离或离心分 离。
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