超临界CO2萃取含油污泥研究现状与进展

doi:10.16085/j.issn.1000-6613.2022-0314

摘要/Abstract

摘要：

含油污泥是一种含有大量有机物、絮状体的复杂多相稳定乳化胶体体系，主要来源于油气开采和集输过程。污泥中的含油量一般为10%~30%（体积分数），利用超临界二氧化碳（supercritical CO₂，scCO₂）提取和回收其中的油基成分可实现污泥的无害化处理，并产生可观的经济效益。本文综述了scCO₂萃取原理及工业化应用情况，分析了萃取条件及携带剂对萃取率的影响，重点论述了scCO₂萃取含油污泥的相平衡热力学及动力学机制研究进展。指出应坚持实验与理论相结合的手段，着重开展以下三方面的研究：①针对含油污泥组成复杂、极性组分含量高的特点，结合scCO₂与含油污泥多组分复杂体系相平衡实验，建立scCO₂萃取含油污泥的相平衡模型，阐明scCO₂萃取含油污泥的相平衡特征及影响因素；②考虑不同分子间的键结合能与非键结合能，从scCO₂萃取油基的微观效应出发，探究油基与污泥基质间的吸附、解吸及扩散规律，定性描述、定量揭示scCO₂萃取油的动力学特征与作用机制；③考虑萃取工艺的经济性，以萃取率最高为目标函数，建立萃取条件优化模型，为scCO₂萃取含油污泥工艺的设计、优化及工业化应用提供理论与技术支撑。

关键词: 超临界二氧化碳, 含油污泥, 溶剂萃取, 回收, 相平衡, 动力学

Abstract:

Oily sludge is a complex multiphase stable emulsified colloid system, which contains a large amount of organic matter and flocs. It mainly comes from the process of oil and gas development and transportation. The volumetric content of oil in the sludge is generally 10%—30%. Extraction and recovery of the oil in the sludge can realize the harmless treatment of the sludge and produce considerable economic benefits. Supercritical carbon dioxide (supercritical CO₂, scCO₂) can dissolve small molecules of organic matter. And its diffusion coefficient is much larger than that of liquid, approaching that of gas. And it has good flow permeability. This technology has great application prospects for extracting oil-based components in oily sludge. In this paper, the principle and industrial application of scCO₂ extraction were reviewed. Combined with experiment and theory, following three aspects of the research could be focused: ①According to the characteristics of complex composition and high content of polar components of oily sludge, combined with the multiphase equilibrium experiment of scCO₂ and oily sludge, the multiphase equilibrium model of scCO₂ extraction was established to clarify the multiphase equilibrium characteristics and influencing factors of scCO₂ extraction of oily sludge. ② Based on the microscopic effects of scCO₂ extraction of oil base, the laws of adsorption and diffusion between oil base and sludge matrix was explored, and the kinetic characteristics and mechanism of scCO₂ extraction were qualitatively described and quantitatively reveal; ③Considering the economy of the extraction process and taking the highest extraction rate as the objective function, the optimization model of extraction conditions was established to provide theoretical and technical supports for the design, optimization and industrial application of scCO₂ extraction oily sludge process.

Key words: supercritical carbon dioxide, oily sludge, solvent extraction, recovery, phase equilibria, kinetics

中图分类号:

X741

贾文龙, 宋硕硕, 李长俊, 吴瑕, 杨帆, 张员瑞. 超临界CO₂萃取含油污泥研究现状与进展[J]. 化工进展, 2022, 41(12): 6573-6585.

JIA Wenlong, SONG Shuoshuo, LI Changjun, WU Xia, YANG Fan, ZHANG Yuanrui. Progress of oily sludge extraction by supercritical CO₂[J]. Chemical Industry and Engineering Progress, 2022, 41(12): 6573-6585.

图/表 18

表1 超临界流体与其他流体物理性质比较

性质	气体（p=1.013×10⁵Pa，T=15~30℃）	超临界流体		液体（p=1.013×10⁵Pa，T=15~30℃）
性质	气体（p=1.013×10⁵Pa，T=15~30℃）	p=p_c，T=T_c	p=4p_c，T=T_c	液体（p=1.013×10⁵Pa，T=15~30℃）
密度/kg·m^-3	0.6~2	200~500	400~900	600~1600
黏度/10^-5Pa·s	1~3	1~3	3~9	20~300
扩散系数/10^-4m²·s^-1	0.1~0.4	0.7×10^-3	0.2×10^-3	(0.2~2)×10^-5

图1 scCO2萃取含油污泥中油基的过程

表2 scCO2萃取技术应用总结

应用行业	应用方式
石油天然气^[15-16]	石油残渣的脱沥青，从残渣油及抽出油中除去重金属，原油的三次回收，各组分的连续分馏，废润滑油的再生，油砂及页岩油的萃取，提高采收率
化工^[17-18]	脱附再生，石墨烯制备，诱导结晶
环保^[9]	土壤修复，重金属去除，环境污染物回收
食品^[19]	微量成分的去除，有效成分的萃取、分离和精制，生物物质的液化，低含油量快餐食品的制取
香料^[20]	天然香料的提取，合成香料的分离精制
医药^[21]	维生素、草药、吗啡、阿托品等的提取、浓缩和精制
煤炭^[22]	煤液化油的脱灰，煤液化油的萃取，煤的液化

表3 国内主要大型scCO2萃取工业设备总结[12]

生产厂家	设备规格	工业化案例
贵州某公司	1~3500L	新疆某生物科技有限公司3500L×3；河北某生物科技有限公司3000L×3；广州某药业公司3000L×3；河南某食品厂600L×3等，印度OZONE公司400L×3，突尼斯AGRI-LAND公司700L×3等
广州某公司	1~1000L	四川某白酒集团1000L×2；石家庄某化纤厂500L×2；内蒙古某食品公司500L×2等
温州某公司	1~500L	青海某生物制药厂400L×3；重庆某制药有限公司；四川某制药有限责任公司；出口泰国

表4 不同土壤修复技术处理多氯联苯的费用对比[25]

处理技术	处理费用/USD·m^-3
超临界流体技术	122~154
生物修复	245~474
原位热解吸附	100~380
焚烧	＞360
液相萃取	250~1169

图2 scCO2萃取油基碳数及摩尔分数分布[29]

图3 含油污泥萃取前后原油四组分对比[30]

图4 scCO2萃取含油污泥工艺流程

图5 Rice提出的连续进出料萃取工艺[31]

图6 连续萃取含油固体废物中油基成分的两级撬装分离装置[32]

图7 超临界CO2萃取含油污泥影响因素[43]

表5 不同类型含油污泥最佳萃取条件

含油污泥来源	含油率/%	萃取温度/℃	萃取压力/MPa	萃取时间/min	萃取率/%
某油井钻屑^［11］	14.94	35	30.0	90	99.60
南海油基钻屑^［29］	25.00	45	14.0	60	55.46
废弃油基钻屑^［38］	13.76	50	25.0	100	99.25
Athabasca油砂^［15］	10.70	31	24.1	90	42.30
Alberta油基钻屑^［44］	8.00	40	14.5	90	90.00
胜利油田孤六联合站落地泥^［30］	12~20	55	20.0	2400	33.15
涪陵国家页岩气开发示范区某井油基钻屑^［38］	18.24	55	21.0	2400	99.65
南海某平台海上现场离心机分离后含油钻屑^［41］	18.12	60	25.0	80	99.29

图8 scCO2萃取油类过程中的相平衡

表6 考虑缔合项的CPA EOS与传统状态方程的对比

状态方程	方程基本形式	方程组成
SRK EOS	$p = R T v - b - a T v v + b$	斥力项+引力项
PR EOS	$p = R T v - b - a T v v + b + b v - b$	斥力项+引力项
CPA EOS	$p = R T v - b - a (T) (v + δ 1 b) (v + δ 2 b) - 12 × R T v 1 - v ∂ l n g ∂ v ∑ i n i ∑ A i 1 - X A i$	斥力项+引力项+缔合项

表6 考虑缔合项的CPA EOS与传统状态方程的对比

状态方程	方程基本形式	方程组成
SRK EOS	$p = R T v - b - a T v v + b$	斥力项+引力项
PR EOS	$p = R T v - b - a T v v + b + b v - b$	斥力项+引力项
CPA EOS	$p = R T v - b - a (T) (v + δ 1 b) (v + δ 2 b) - 12 × R T v 1 - v ∂ l n g ∂ v ∑ i n i ∑ A i 1 - X A i$	斥力项+引力项+缔合项

图9 H2O缔合结构示意图[52]

表7 不同状态方程CO2/H2O物质缔合参数[52]

状态方程	物质	缔合结构	Ε/bar·L·mol^-1	β
CPA-SRK	CO₂	2B	78.12	0.0568
		3B	51.68	0.0411
		4C	39.23	0.0297
	H₂O	4C	166.55	0.0692
CPA-PR	CO₂	4C	48.11	0.0457
	H₂O	4C	181.13	0.1062

图10 不同方法预测的油相中水的摩尔含量

图11 微分质量衡算模型示意图[29]

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超临界CO₂萃取含油污泥研究现状与进展

Progress of oily sludge extraction by supercritical CO₂

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