CN103570199A - 一种含油污泥的高效萃取方法 - Google Patents
一种含油污泥的高效萃取方法 Download PDFInfo
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- CN103570199A CN103570199A CN201210250237.6A CN201210250237A CN103570199A CN 103570199 A CN103570199 A CN 103570199A CN 201210250237 A CN201210250237 A CN 201210250237A CN 103570199 A CN103570199 A CN 103570199A
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- oily sludge
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- 239000010802 sludge Substances 0.000 title claims abstract description 121
- 238000000605 extraction Methods 0.000 title claims abstract description 101
- 239000002904 solvent Substances 0.000 claims abstract description 71
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 69
- 238000009835 boiling Methods 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims description 57
- 239000003208 petroleum Substances 0.000 claims description 25
- 239000007790 solid phase Substances 0.000 claims description 23
- 239000007791 liquid phase Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 238000007670 refining Methods 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-butanone Chemical group 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- 239000012046 mixed solvent Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 11
- 239000012466 permeate Substances 0.000 abstract 1
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- CTQNGGLPUBDAKN-UHFFFAOYSA-N o-xylene Chemical compound 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CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 230000001698 pyrogenic Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- SLUNEGLMXGHOLY-UHFFFAOYSA-N benzene;hexane Chemical compound 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Abstract
本发明提供了一种性能更为优良的含油污泥萃取方法，先让含油污泥与少量萃取溶剂在密闭容器中经高温和自生压力，使溶剂更大程度的渗透和替换油泥中的油分，之后在较大剂量溶剂的带动下充分分离出油分。萃取溶剂含有：主剂A，沸程为110～135℃的馏分油；副剂B，沸程为140～150℃的馏分油；助剂C，80～100℃的馏分油或者工业纯产品。所述的馏分油为石脑油、轻质油等。本发明的萃取方法在萃取过程中，萃取时间短，萃取效果突出，在更大程度上实现含油污泥的资源化目标。
Description
一种含油污泥的高效萃取方法
技术领域
[0001] 本发明涉及一种含油污泥的萃取方法，特别是对原油储运过程产生的罐底泥和炼油厂、炼油污水处理厂产生的含油污泥的萃取方法。
背景技术
[0002] 炼化企业在石油储运、炼制和废水处理过程中产生大量的含油污泥，他们主要来自隔油池、浮选池、原油脱水罐、储运罐和污油罐等。这些污泥成分复杂，含有大量的老化原油、蜡质、浙青质、胶体和固体悬浮物、细菌等，污水处理过程中还加入了大量的凝聚剂、缓蚀剂、阻垢剂、杀菌剂等水处理药剂，这给污泥处理带来很大的难度。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。并且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。近年，随着国家环保法规标准要求的不断提高，环保执法力度不断加大，生产过程中所生成固体废弃物的污染控制和资源化利用，已成为困扰石油和石油加工行业的难题。
[0003] 针对含油污泥成分复杂，处理难度大，处理成本高且难以彻底处理等问题，近20年来虽然有多种有关含油污泥的研究报道，且处理技术也多种多样，每种方法各有各的优缺点和使用范围，但至今含油污泥的处理技术也难以得到推广应形成工业化生产。含油污泥处理最终的目的是以减量化、无害化、资源化为原则。含油污泥常用的处理方法:溶剂萃取法、焚烧法、生物法、焦化法等。焦化法虽然可以利用高温条件下烃类的热裂解和热缩合反应产生液相油品、不凝气和焦碳产品，但这种方法耗能较高，且容易结焦，对工艺要求高。生物法主要是利用微生物将含油污泥中的石油烃类降解为无害的土壤成份，但对于越来越稀缺的石油资源来说是一种浪费。焚烧处理法优点是污泥经焚烧后，多种有害物几乎全部除去，减少了对环境的危害，废物减容效果好，处理比较安全，缺点是焚烧过程中产生了二次污染，同样也浪费了宝贵资源。萃取法是利用“相似相溶”原理，选择一种合适的有机溶剂作萃取剂，将含油污泥中的原油回收利用的方法。目前，萃取法处理含油污泥还在试验开发阶段。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，所以萃取法成本高，很少实际应用于炼厂含油污泥处理。
[0004] 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45~90°C )、石油醚、轻质油，利用溶剂对含油污泥中燃料油的溶解作用，对含油污泥中水、油和渣进行分离。但是，该技术的萃取工艺条件为萃取温度45~55°C，萃取过程中溶剂损耗较高，且含油污泥经过萃取后，油萃取不易彻底。
[0005] CN02133117提出一种含油污泥干化后热萃取的方法，在较高的温度下，用煤油、柴油、石蜡油等一种或几种进行萃取分离。液相进行焦化，而固相经燃烧利用热值，因为萃取后煤油很难完全回收，导致溶剂煤油或其他油将渣油在含油污泥内部进行置换，而油固相很难完全分离。
[0006] CN200410050782提出用宽沸点油(100~500°C )作为含油污泥萃取的溶剂油，并采用多效热萃取的方式对含油污泥中的油进行回收。但是，此工艺流程较长，且在较高操作温度下很难完全回收成分稳定的溶剂油，并循环利用。
[0007] CN200910079177提出含油污泥干化后在萃取的工艺，使用多种成品油作为萃取溶剂，比如石脑油、溶剂油、石油醚等，但经过试验对比分析，萃取出的有机物最多才占含油污泥总有机物含量的58%。其萃取效果排序为:石脑油> 120 #溶剂油 >石油醚。 [0008] Taiwo E.ACTaiwo E.A et al.0il recovery from petroleum sludge by solventextraction.Petroleum science and technology.2009 (27): 836 ~844.)用己烧和二甲苯作为含油污泥萃取的溶剂。在优化萃取条件下可以回收含油污泥中达67%的有机化合物(含油污泥含水率约19%)。但所用溶剂的毒性较大(特别是二甲苯)，对周围环境和操作人员都有较大的安全隐患。并且低沸点己烷的用量较大，在溶剂回收阶段的损失量会较大，导致工艺经济性下降。
[0009] 综上所述，目前用作含油污泥萃取溶剂的原料主要有轻质煤焦油、石油醚、石脑油、轻质油、苯、甲苯、丁酮等工业产品或宽沸程组合溶剂，虽然可以达到一定的萃取效果，但文献数据证明用以上溶剂对含油污泥的萃取，其萃取出的有机产品很难超过含油污泥中总体有机物成分的60%，并且萃取溶剂在回收利用过程中会有较大量的损失，一般损失量可达6%以上，这样就影响了含油污泥萃取技术的经济性能，暂缓了这项技术的推广应用。单一溶剂，如苯、甲苯、丁酮等，由于其分子结构的单一性，与含油污泥中结构复杂的石油类物质有一定的相容局限性，导致萃取效果不能大幅提高。单一石油产品，如煤焦油、石油醚、石脑油、轻质油等，虽然对含油污泥中结构复杂的石油类物质有较高的溶解性，但由于这类溶剂的沸程较宽，且低沸程油的含量较高，这就需要苛刻的萃取工艺设备，以免油气泄露造成爆炸危险，同时低沸程油分很难在溶剂回收阶段回收，造成较大的溶剂损失。更宽沸程的溶剂，如CN200410050782中用宽沸点油(100~500°C )作为含油污泥萃取的溶剂油，此工艺需要500°C以上的焙烧温度才能把溶剂油与干泥渣分离，工艺复杂，能耗高，同时回收溶剂损失也较高且成份不恒定。因此，影响含油污泥萃取技术发展的关键是要开发出性能更加优良的含油污泥萃取溶剂和高效的萃取方法。
发明内容
[0010] 为了克服现有技术的不足，本发明提供了一种性能更为优良的含油污泥萃取方法。采用本发明的萃取方法，可以使萃取时间较大地缩短，并且萃取效果突出，在更大程度上实现含油污泥的资源化目标。
[0011] 下文所述的“份”均指重量份。
[0012] 本发明所述的含油污泥萃取方法，包括:
[0013] I)将1份含油污泥与0.5~2份混合萃取溶剂混合后加入密闭耐压容器中，加热到100~150°C，并保持搅拌I~10分钟，所述的混合萃取溶剂包含0.1~1.5份主剂A、
0.1~1.5份副剂B和0.1~1份助剂C ；
[0014] 2)然后将密闭耐压容器中的物料迅速与2.5~18质量份主剂A混合，使溶剂总用量最终达与含油污泥的质量比为3~20:1，搅拌I~5分钟后，最后分离固液相；所述的主剂A为沸程为110~135°C的馏分油；副剂B为沸程为140~150°C的馏分油；助剂C为沸程为80~100°C的馏分油或者工业纯产品；[0015] 3)将步骤2)分离后的固相在130~180°C下干化I~3小时后作为最终处理残渣排放，其含油率小于0.3%，可达到农用污泥标准含油率的要求；
[0016] 4)将步骤2)分离后的液相按照主剂A、副剂B和助剂C的沸程段进行精馏后复配新鲜混合溶剂，剩余渣油进入原油炼制工艺。
[0017] 本发明所述的馏分油为石脑油、轻质油等的。
[0018] 本发明所述的助剂C可以为丁酮、庚烷、1，2_ 二氯乙烷等工业纯产品。
[0019] 本发明所述的主剂A优选为沸程为120~130°C的馏分油。
[0020] 本发明密闭耐压容器的装填率为65%~85%，其中装填率为物料体积占容器总体积的百分比。
[0021] 本发明的主要特点在于，针对含油污泥的萃取过程，设计了密闭高温高压的步骤。在密闭高温高压的过程中，助剂C会完全气化，有助于增加密封体系的压力，同时主剂A在密封体系中也部分气化，也可使体系保持较高的自生压力。另外含油污泥中的水分在较高的温度下也会大部分气化，进而从稳定的油-水-固三相体系中析出，增加了含油污泥中油相的活动性。在较高的压力和温度下，没有气化的主剂A和副剂B与含油污泥中的油相会发生充分的渗透和置换，使溶剂最大程度地接近含油污泥中的固相，进而剥离包覆固相的粘性油分，让其进入溶剂相。在较高的压力和温度下，主剂A和副剂B对重油的溶解度也会有较大的增加，这更有利于吸纳较大量的含油污泥中的重油组分。
[0022] 本发明的另一特点在于，在密闭高温高压步骤结束后，再加入另一部分主剂A。密闭高温高压步骤结束后，混合物有较高的温度，用另一份主剂A与之在短时间内接触，经过热量交换，可以使总体温度降低到低于100°C，减少安全风险。同时添加的主剂A也可以在较高温度下较短时间内与混合物混合，稀释较浓的重油成分，同时起到再次清洗含油污泥固相的作用，强化密封高温步骤的萃取效果。
[0023] 本发明的另一特点是，针对萃取含油污泥并回收溶剂工艺，选择石油产品110~135°C的懼分油作为含油污泥萃取的主溶剂,原因有三点:1、考虑到回收工艺的可操作性和安全性，选择此沸程适中的馏分产品；2、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浙青质和重油组分；3、此沸程的石油产品馏分对含油污泥中油的萃出率高于一般常见溶剂，且在溶剂回收工艺中溶剂的损失量较少，有利于工艺的经济性。
[0024] 本发明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浙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来实现在密封高温步骤增加自生压力的目的，并且在最后溶剂接触混合过 程中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] 本发明的含油污泥萃取溶剂具有高效、快速、使用量少、使用范围广等特点，在含油污泥与总溶剂质量比1:3~1:20的范围内都有优良的萃取效果。
[0027] 本发明的含油污泥萃取方法具有操作时间短，处理量大，处理效果好，溶剂易于回收复配等优点。具体实施方式
[0028] 应用本发明得到的含油污泥萃取溶剂，在含油污泥前期干化或自然干化至含水率小于30%时才与溶剂进行接触，进行萃取效果检测。
[0029] 检测标准以萃取油分占含油污泥总有机物成分的质量百分比(R%)计量，也就是总有机物萃出率。
[0030] 含油污泥总有机物成分测定方法。将含油污泥在105°C烘干至衡重，再将烘干油泥在550°C马弗炉焙烧至衡重，两重量的差值既是含油污泥总有机物成分含量。
[0031] 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。
[0032] 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0.1%为止。
[0033] 萃出油分占含油污泥总有机物含量的比例(总有机物萃出率R%):
[0034]
[0035] 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？％):
[0036]
[0037] 含油污泥萃取工艺步骤。油泥与萃取溶剂的质量比为1:5，萃取温度为751:，萃取时间为40min,萃取过程中辅助60r/min的搅拌。二次萃取与一次萃取工艺相同。
[0038] 实施例1
[0039] 原料与预处理:含油污泥采用某石化公司原油储运厂的罐底油泥，含水率约为16%。原料经自然风干7天，使含水率降为3%~5%后，用作被萃取样品。
[0040] 萃取方法:
[0041] I)密闭高温步骤:将1份含油污泥与含0.5份主剂A、0.5份副剂B和0.3份助剂C的混合萃取溶剂先在密闭容器内加热到120°C，保持9分钟，其中主剂、副剂和助剂分别选用石脑油115~130°C、140~150°C和80~100°C沸程的馏分油；
[0042] 2)稀释萃取步骤:1)步后，迅速加入8.2份主剂A使含油污泥与溶剂总质量比为1:10，搅拌5分钟，分离固液相，固相经140°C干燥2h后含油率小于0.3%，达到农用污泥含油率的标准。
[0043] 萃取结果见表1实施例1数据。
[0044] 对比例I
[0045] 原料与预处理:含油污泥采用某石化公司原油储运厂的罐底油泥，含水率约为16%。原料经自然风干7天，使含水率降为3%~5%后，用作被萃取样品。
[0046] 萃取方法:其它条件及步骤与实施例1相同，不同之处在于萃取过程中的密封高温步骤不加助剂C，增大主剂A的含量到0.8份，固液分离后的固相经140°C干燥2h后含油率为0.5%，达不到农用污泥含油率的标准。[0047] 萃取结果见表1对比例I数据。
[0048] 实施例2
[0049] 原料与预处理:含油污泥采用某石化公司原油储运厂的罐底油泥，含水率约为16%。原料经自然风干7天，使含水率降为3%~5%后，用作被萃取样品。
[0050] 萃取方法:
[0051] 1)密闭高温步骤:将1份含油污泥与含1份主剂A、0.5份副剂B和0.5份助剂C的混合萃取溶剂先在密闭容器内加热到140°C，保持6分钟，其中主剂、副剂和助剂分别选用石脑油115~130°C、140~150°C和80~100°C沸程的馏分油；
[0052] 2)稀释萃取步骤:1)步后，迅速加入13份主剂A使含油污泥与溶剂总质量比为1:15，搅拌5分钟，分离固液相，固相再经150°C干燥2h后含油率小于0.3%，达到农用污泥含油率的标准。
[0053] 萃取结果见表1实施例2数据。
[0054] 对比例2
[0055] 原料与预处理:含油污泥采用某石化公司原油储运厂的罐底油泥，含水率约为16%。原料经自然风干7天，使含水率降为3%~5%后，用作被萃取样品。
[0056] 萃取方法:其它条件及步骤与实施例1相同，不同之处在于萃取过程中的不经历密封高温高压步骤，而在常压下进行。萃取后，固液分离后的固相经150°C干燥2h后含油率为0.8%，达不到农用污泥含油率的标准。
[0057] 萃取结果见表1对比例2数据。
[0058] 实施例3
[0059] 原料与预处理:含油污泥采用某石化公司原油储运厂的罐底油泥，含水率约为16%。原料经自然风干7天，使含水率降为3%~5%后，用作被萃取样品。
[0060] 萃取方法:
[0061] 1)密闭高温步骤:将1份含油污泥与含0.6份主剂A、0.8份副剂B和0.3份助剂C的混合萃取溶剂先在密闭容器内加热到140°C，保持8分钟，其中主剂、副剂和助剂分别选用石脑油115~130°C、140~150°C和80~100°C沸程的馏分油；
[0062] 2)稀释萃取步骤:1)步后，迅速加入16.3份主剂A使含油污泥与溶剂总质量比为1:18，搅拌3分钟，分离固液相，固相再经150°C干燥2h后含油率小于0.3%，达到农用污泥含油率的标准。
[0063] 萃取结果见表1实施例3数据。
[0064] 对比例3
[0065] 原料与预处理:含油污泥采用某石化公司原油储运厂的罐底油泥，含水率约为16%。原料经自然风干7天，使含水率降为3%~5%后，用作被萃取样品。
[0066] 萃取方法:其它条件及步骤与实施例1相同，不同之处在于萃取过程中所用萃取剂为常减压装置煤油馏分。萃取后，固液分离后的固相经180°C干燥4h后依然有煤油残余，这种残渣只有再做燃料燃烧后才可考虑排放。
[0067] 萃取结果见表1对比例3数据。
[0068] 实施例4
[0069] 原料与预处理:含油污泥采用某石化公司原油储运厂的罐底油泥，含水率约为16%。原料经自然风干7天，使含水率降为3%~5%后，用作被萃取样品。
[0070] 萃取方法:
[0071] I)密闭高温步骤:将1份含油污泥与含0.6份主剂A、0.3份副剂B和0.1份助剂C的混合萃取溶剂先在密闭容器内加热到130°C，保持5分钟，其中主剂、副剂和助剂分别选用石脑油115~130°C、140~150°C和80~100°C沸程的馏分油；
[0072] 2)稀释萃取步骤:1)步后，迅速加入11份主剂A使含油污泥与溶剂总质量比为1:12，搅拌4分钟，分离固液相，固相再经150°C干燥2h后含油率小于0.3%，达到农用污泥含油率的标准。
[0073] 萃取结果见表1实施例4数据。
[0074] 对比例4
[0075] 原料与预处理:含油污泥采用某石化公司原油储运厂的罐底油泥，含水率约为16%。原料经自然风干7天，使含水率降为3%~5%后，用作被萃取样品。
[0076] 萃取方法:其它条件及步骤与实施例1相同，不同之处在于萃取过程中的不经历密封高温高压步骤，只在常压下进行萃取，并且另一不同之处为萃取剂为常减压装置煤油馏分。萃取后，固液分离后的固相经180°C干燥4h后依然有煤油残余，这种残渣只有再做燃料燃烧后才可考虑排放。
[0077] 萃取结果见表1对比例4数据。
[0078] 实施例5
[0079] 原料与预处理:含油污泥采用某石化公司污水处理厂隔油池和浮选池排放的含油油泥，含水率约83%。原泥样在105°C下烘干3小时，使含水率降为10%~20%后，用作被萃取样品。
[0080] 萃取方法:
[0081] I)密闭高温步骤:将1份含油污泥与含0.5份主剂A、0.5份副剂B和0.3份助剂C的混合萃取溶剂先在密闭容器内加热到120°C，保持3分钟，其中主剂、副剂和助剂分别选用石脑油115~130°C、140~150°C和80~100°C沸程的馏分油；
[0082] 2)稀释萃取步骤:1)步后，迅速加入8.2份主剂A使含油污泥与溶剂总质量比为1:10，搅拌5分钟，分离固液相，固相再经150°C干燥2h后含油率小于0.3%，达到农用污泥含油率的标准。
[0083] 萃取结果见表1实施例5数据。
[0084] 对比例5
[0085] 原料与预处理:含油污泥采用某石化公司污水处理厂隔油池和浮选池排放的含油油泥，含水率约83%。原泥样在105°C下烘干3小时，使含水率降为10%~20%后，用作被萃取样品。
[0086] 萃取方法:其它条件及步骤与实施例1相同，不同之处在于萃取过程中的密封高温步骤不加助剂C，增大主剂A的含量到0.8份，萃取后，固液分离后的固相经150°C干燥2h后含油率为0.6%，达不到农用污泥含油率的标准。
[0087] 萃取结果见表1对比例5数据。
[0088] 实施例6
[0089] 原料与预处理:含油污泥采用某石化公司污水处理厂隔油池和浮选池排放的含油油泥，含水率约83%。原泥样在105°C下烘干3小时，使含水率降为10%~20%后，用作被萃取样品。
[0090] 萃取方法:
[0091] I)密闭高温步骤:将1份含油污泥与含1份主剂A、0.5份副剂B和0.5份助剂C的混合萃取溶剂先在密闭容器内加热到140°C，保持7分钟，其中主剂、副剂和助剂分别选用石脑油115~130°C、140~150°C和80~100°C沸程的馏分油；
[0092] 2)稀释萃取步骤:1)步后，迅速加入13份主剂A使含油污泥与溶剂总质量比为1:15，搅拌3分钟，分离固液相，固相再经150°C干燥2h后含油率小于0.3%，达到农用污泥含油率的标准。
[0093] 萃取结果见表1实施例6数据。
[0094] 对比例6
[0095] 原料与预处理:含油污泥采用某石化公司污水处理厂隔油池和浮选池排放的含油油泥，含水率约83%。原泥样在105°C下烘干3小时，使含水率降为10%~20%后，用作被萃取样品。
[0096] 萃取方法:其它条件及步骤与实施例1相同，不同之处在于萃取过程中所用的萃取剂为市售工业成品环己烧O萃取后，固液分离后的固相经150 V干燥2h后含油率为0.9%,达不到农用污泥含油率的标准。
[0097] 萃取结果见表1对比例6数据。
[0098] 实施例7
[0099] 原料与预处理:含油污泥采用某石化公司污水处理厂隔油池和浮选池排放的含油油泥，含水率约83%。原泥样在105°C下烘干3小时，使含水率降为10%~20%后，用作被萃取样品。
[0100] 萃取方法:
[0101] I)密闭高温步骤:将1份含油污泥与含0.6份主剂A、0.8份副剂B和0.3份助剂C的混合萃取溶剂先在密闭容器内加热到140°C，保持8分钟，其中主剂、副剂和助剂分别选用石脑油115~130°C、140~150°C和80~100°C沸程的馏分油；
[0102] 2)稀释萃取步骤:1)步后，迅速加入16.3份主剂A使含油污泥与溶剂总质量比为1:18，搅拌4分钟，分离固液相，固相再经130°C干燥2h后含油率小于0.3%，达到农用污泥含油率的标准。
[0103] 萃取结果见表1实施例7数据。
[0104] 对比例7
[0105] 原料与预处理:含油污泥采用某石化公司污水处理厂隔油池和浮选池排放的含油油泥，含水率约83%。原泥样在105°C下烘干3小时，使含水率降为10%~20%后，用作被萃取样品。
[0106] 萃取方法:其它条件及步骤与实施例1相同，不同之处在于萃取过程中的密封高温步骤不加主剂A，增大副剂 的含量到1.4份。萃取后，固液分离后的固相经130°C干燥2h后含油率为0.4%，达不到农用污泥含油率的标准。
[0107] 萃取结果见表1对比例7数据。
[0108] 实施例8[0109] 原料与预处理:含油污泥采用某石化公司污水处理厂隔油池和浮选池排放的含油油泥，含水率约83%。原泥样在105°C下烘干3小时，使含水率降为10%~20%后，用作被萃取样品。
[0110] 萃取方法:
[0111] I)密闭高温步骤:将1份含油污泥与含0.6份主剂A、0.3份副剂B和0.1份助剂C的混合萃取溶剂先在密闭容器内加热到130°C，保持9分钟，其中主剂、副剂和助剂分别选用石脑油115~130°C、140~150°C和80~100°C沸程的馏分油；
[0112] 2)稀释萃取步骤:1)步后，迅速加入11份主剂A使含油污泥与溶剂总质量比为1:12，搅拌3分钟，分离固液相，固相再经160°C干燥2h后含油率小于0.3%，达到农用污泥含油率的标准。
[0113] 萃取结果见表1实施例8数据。
[0114] 对比例8
[0115] 原料与预处理:含油污泥采用某石化公司污水处理厂隔油池和浮选池排放的含油油泥，含水率约83%。原泥样在105°C下烘干3小时，使含水率降为10%~20%后，用作被萃取样品。
[0116] 萃取方法:其它条件及步骤与实施例1相同，不同之处在于萃取过程中的密封高温步骤只加1份主剂A，不加副剂和助剂。萃取后，固液分离后的固相经160°C干燥2h后含油率为0.5%，达不到农用污泥含油率的标准。
[0117] 萃取结果见表1对比例8数据。
[0118] 表1各实施例和对比例数据总表
[0119]
[0120]
[0121] *注:由于残渣中煤油残留较多，180°C干化后依然无法测量实际含油率。
Claims (5)
1.一种含油污泥的萃取方法，其特征在于包括以下步骤: 1)将I质量份含油污泥与0.5~2质量份混合萃取溶剂混合后加入密闭耐压容器中，加热到100~150°C，并在溶剂自生压力下保持搅拌I~10分钟，所述的混合萃取溶剂包含0.1~1.5质量份主剂A、0.1~1.5质量份副剂B和0.1~I质量份助剂C ； 2)然后将密闭耐压容器中的物料迅速与2.5~18质量份主剂A混合，使混合溶剂总用量最终达与含油污泥的质量比为3~20:1，搅拌I~5分钟后，最后分离固液相； 3)将步骤2)分离后的固相在130~180°C下干化I~3小时后作为最终处理残渣排放； 4)将步骤2)分离后的液相按照主剂A、副剂B和助剂C的沸程段进行精馏后复配新鲜混合溶剂，剩余渣油进入原油炼制工艺； 所述的主剂A为沸程为110~135°C的馏分油；副剂B为沸程为140~150°C的馏分油；助剂C为沸程为80~100°C的馏分油或者工业纯产品。
2.如权利要求1所述的萃取方法，其特征在于所述的馏分油为石脑油、轻质油的。
3.如权利要求1所述的萃取方法，其特征在于所述的工业纯产品为丁酮、庚烷、1，2_二氯乙烷。
4.如权利要求1所述的萃取方法，其特征在于所述的主剂A为沸程为120~130°C的懼分油。
5.如权利要求1所述的萃取方法，其特征在于所述的密闭耐压容器的装填率为65%~85%。
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| CN107099320A (zh) * | 2017-05-18 | 2017-08-29 | 辽宁石油化工大学 | 一种油泥油砂共混萃取回收原油的方法 |
| CN107129824A (zh) * | 2017-05-23 | 2017-09-05 | 重庆理工大学 | 一种回收油泥中石油的方法 |
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| WO2020233510A1 (zh) * | 2019-05-17 | 2020-11-26 | 东南大学 | 一种常年污染深度含油和水的污泥、废渣或自然油矿中的油砂的处理方法及其处理系统 |
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