WO2016034042A1 - 油砂萃取分离工艺方法 - Google Patents

油砂萃取分离工艺方法 Download PDF

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WO2016034042A1
WO2016034042A1 PCT/CN2015/087228 CN2015087228W WO2016034042A1 WO 2016034042 A1 WO2016034042 A1 WO 2016034042A1 CN 2015087228 W CN2015087228 W CN 2015087228W WO 2016034042 A1 WO2016034042 A1 WO 2016034042A1
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organic solvent
oil
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weight
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张国柱
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张国柱
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/04Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction

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  • the invention relates to an oil sand extraction and separation process method, which is a process method for extracting and separating petroleum components contained in pure solid oil sands.
  • the method comprises the following steps: heating the oil sand with hot water or steam, adding alkaline substances and other industrial additives to assist solid-liquid separation, and the generated wastewater cannot be discharged to the standard during the processing; the separated solid material contains petroleum components and cannot be utilized.
  • the resource recovery is not complete.
  • the technical problem to be solved by the present invention is to provide an oil sands extraction and separation process method, which overcomes the problems of low resource utilization rate and environmental pollution, and solves the problem of continuous large-scale production.
  • an oil sands extraction and separation process method comprising the following steps:
  • step 5 The solid phase material separated in step 5 is heated and steamed by steaming in a steaming line, the heating temperature is 95-110 ° C, and the steaming off steaming pressure is 0.1-0.23 MPa, and solid matter is discharged from the outlet, and the organic solvent is discharged. After steaming off, return it as solvent oil Received
  • step 3 and step 5 The liquid phase materials separated by centrifugation in step 3 and step 5 are merged into the rising film evaporator and the thin film evaporator, the evaporation temperature is 80-120 ° C, and the evaporation pressure is 0.1-0.2 MPa, mainly asphalt.
  • the petroleum component product is discharged from the outlet of the thin film evaporator, and the organic solvent is distilled off and recovered as a solvent oil;
  • the organic solvent is one or a mixture of two or more of an alcohol, an acid, a lipid, an alkane or a cycloalkane.
  • the organic solvent is composed by volume percentage, hexane 70% and benzene 30%.
  • the organic solvent is composed of 5% by weight, 5% by weight of benzene and 70% by weight of hexane.
  • the organic solvent is composed of 5% by volume, 5% by weight of benzene and 70% by weight of hexane.
  • the organic solvent was composed by volume percentage, ethyl acetate 30%, benzene 20%, and hexane 50%.
  • the organic solvent is composed by volume percent, cyclohexene 50% and hexane 50%.
  • the oil sand extraction and separation process method can fully separate and extract the active components in the oil sand by the above steps, and the process is simple, and the separation efficiency is high, and the solvent can be reused, the environment is protected, and the production cost is saved;
  • the product can be further processed to produce building materials or cement fillers, while liquid products can produce diesel, asphalt or water repellents.
  • the organic solvent is a mixture of alcohols, acids, lipids, alkanes or naphthenes.
  • the extraction has strong penetrating power and good extraction effect, and the distillation range is usually short at 60-95 ° C. It is easy to recycle, economical and practical, and toxic. small.
  • Figure 1 is a flow chart of the oil sands extraction separation process.
  • Oil sands are solid black materials rich in petroleum, with a weight of 0.68-1.0 tons/ m3 and a petroleum content of more than 20%. At the same time, it contains a certain amount of metal elements. The oil sands are rich in resources and easy to mine, and have a broad prospect for development and utilization.
  • an oil sands extraction separation process includes the following steps:
  • step 5 The solid phase material separated in step 5 is heated and steamed by steaming in a steaming line, the heating temperature is 95-110 ° C, and the steaming off steaming pressure is 0.1-0.23 MPa, and solid matter is discharged from the outlet, and the organic solvent is discharged. After steaming off, it is recovered as a solvent oil;
  • step 3 and step 5 The liquid phase materials separated by centrifugation in step 3 and step 5 are merged into the rising film evaporator and the thin film evaporator, the evaporation temperature is 80-120 ° C, and the evaporation pressure is 0.1-0.2 MPa, mainly asphalt.
  • the petroleum component product is discharged from the outlet of the thin film evaporator to obtain a purified product, and the organic solvent is distilled off and recovered as a solvent oil;
  • the organic solvent in the step is composed of 7% by weight and 30% by weight of benzene.
  • the weight loss ratio of the oil sands to the organic solvent was 1:0.5, and the time of the two mixed extractions was 3 minutes, respectively, and the remaining steps were the same as in the first embodiment.
  • the organic solvent is composed of 5% by weight, 5% by weight of benzene and 70% by weight of hexane. After two extractions and separations in this example, the solid phase was detected and there was no soluble substance.
  • the weight ratio of the oil sands to the organic solvent was 1:0.4, the oil sand particle diameter was 1 mm ⁇ d ⁇ 3 mm, and the time of the two mixed extractions was 3 minutes, respectively, and the remaining steps were the same as in the first embodiment.
  • the organic solvent is composed of 5% by volume, 5% by weight of benzene and 70% by weight of hexane. After two extractions and separations in this example, the solid phase was detected and there was no soluble substance.
  • the weight loss ratio of the oil sands to the organic solvent was 1:0.4, the oil sand particle diameter was 3 mm ⁇ d ⁇ 6 mm, and the time of the two mixed extractions was 10 minutes, respectively, and the remaining steps were the same as in the first embodiment.
  • the organic solvent was composed by volume percentage, ethyl acetate 30%, benzene 20%, and hexane 50%. After two extractions and separations in this example, the solid phase was detected and there was no soluble substance.
  • Example 2 The same procedure as in Example 1 except that the organic solvent was composed by volume percentage of cyclohexene 50% and hexane 50%.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

本发明涉及一种油砂萃取分离工艺方法,包括以下步骤:1)将筛选后的油砂进行粉碎;2)油砂颗粒输送到1号混合器内加入有机溶剂,进行封闭的防爆搅拌萃取;3)将萃取后的混合液输送至1号离心分离机中进行离心分离,得到液相物质和固相物质;4)1号离心分离机离心后的固相物质在进入2号混合器进行封闭的防爆搅拌萃取;5)2号混合器中产生的混合液送至2号离心分离机中,再次得到液相物质和固相物质;6)步骤5分离出来的固相物质通过蒸脱机内蒸汽加热和喷蒸;7)离心分离出的液相物质汇合后依次进入升膜蒸发器和薄膜蒸发器中;8)蒸发的溶剂油回收利用。该工艺方法克服资源利用率低和环境污染难题,解决连续规模化生产问题。

Description

油砂萃取分离工艺方法 技术领域
本发明涉及一种油砂萃取分离工艺方法,是针对纯固态油砂中有所含有石油成分提取分离的工艺方法。
背景技术
在国外,油砂的提取分离,采用向矿层钻井,注入高温高压蒸汽,使固态物质内的是由成分融化变为流态物质,然后在实施钻井,将流态物质抽出地面加工处理。注入蒸汽持续时间长,耗能大,施工周期长,成本高,资源利用率低。引出地面的流态物质夹带固体物质和水,无法处理,对环境造成的污染也较严重。
在国内,油砂的提取分离,只是在小作坊中进行。方法是:用热水或蒸汽对油砂进行加热,再加入碱性物质和其他工业添加剂辅助固液分离,加工过程中,产生的废水无法达标排放;分离后的固体物质含有石油成份,无法利用,资源回收不彻底。
发明内容
本发明要解决的技术问题是提供一种油砂萃取分离工艺方法,该工艺方法克服资源利用率低和环境污染难题,解决连续规模化生产问题。
为解决以上问题,本发明的具体技术方案如下:一种油砂萃取分离工艺方法,包括以下步骤:
1)将筛选后的油砂在25℃-0℃的气温条件下进行粉碎,颗粒度直径0<d≤6mm;
2)在常温下将油砂颗粒输送到1号混合器内,加入有机溶剂,油砂与有机溶剂的重量比为1:1-0.4,同时加入惰性气体,进行封闭的防爆搅拌萃取,萃取时间为3分钟;
3)将萃取后的混合液输送至1号离心分离机中,进行离心分离,得到液相物质和固相物质;
4)1号离心分离机离心后的固相物质在进入2号混合器中,加入有机溶剂,有机溶剂与油砂的重量比为1:1-0.4,同时加入惰性气体,进行封闭的防爆搅拌萃取,萃取时间为3-10分钟;
5)2号混合器中产生的混合液送至2号离心分离机中,进行离心分离,再次得到液相物质和固相物质;
6)步骤5分离出来的固相物质通过蒸脱机内蒸汽加热和喷蒸,加热温度为95-110℃,蒸脱喷蒸压力在0.1-0.23MPa,产生固体物质从出口排出,有机溶剂被蒸脱后以溶剂油形式回 收;
7)步骤3和步骤5中离心分离出的液相物质汇合后依次进入升膜蒸发器和薄膜蒸发器中,蒸发温度在80-120℃,蒸发压力在0.1-0.2MPa,以沥青为主的石油成份产品从薄膜蒸发器出口排出,有机溶剂被蒸脱后以溶剂油形式回收;
8)步骤6和步骤7中回收的溶剂油再次被步骤2和步骤4中利用。
所述的有机溶剂是醇类、酸类、脂类、烷烃类或环烷烃类的一种或两种以上的混合。
所述的有机溶剂按体积百分比组成为,己烷70%和苯30%。
所述的有机溶剂按体积百分比组成为,乙醇5%、苯25%和己烷70%。
所述的有机溶剂按体积百分比组成为,乙酸5%、苯25%和己烷70%。
所述的有机溶剂按体积百分比组成为,乙酸乙酯30%、苯20%和己烷50%。
所述的有机溶剂按体积百分比组成为,环己烃50%和己烷50%。
该油砂萃取分离工艺方法采用上述步骤可以充分将油砂中的有效成分进行分离萃取,不仅工艺简单,而且分离效率高,其中的溶剂可反复利用,保护了环境,节约了生产成本;其固体产物可以进行深加工,可以制造建筑材料或水泥填充物,而液态产物可生产柴油、沥青或防水剂。
有机溶剂采用醇类、酸类、脂类、烷烃类或环烷烃类的混合物质,其萃取渗透力强,萃取效果好,同时馏程短通常在60-95℃,回收容易,经济实用,毒性小。
附图说明
图1为油砂萃取分离工艺方法的流程图。
具体实施方式
油砂是一种富含石油成份的固态黑色物质,重度在0.68-1.0吨/米3,石油成份含量在20%以上,以沥青成份为主。同时含有一定量的金属元素,油砂的资源储量丰富,易开采,开发利用前景广阔。
实施例一
如图1所示,一种油砂萃取分离工艺方法,包括以下步骤:
1)将1000公斤的油砂在25℃-0℃的气温条件下进行粉碎,颗粒度直径0<d≤1mm;
2)在常温下将油砂颗粒输送到1号混合器内,加入有机溶剂,油砂与有机溶剂的重量比为1:1,同时加入惰性气体,进行封闭的防爆搅拌萃取,萃取时间为3分钟;
3)将萃取后的混合液输送至1号离心分离机中,进行离心分离,得到液相物质和固相物 质;
4)1号离心分离机离心后的固相物质在进入2号混合器中,加入有机溶剂,有机溶剂与油砂的重量比为1:1,同时加入惰性气体,进行封闭的防爆搅拌萃取,萃取时间为3分钟;
5)2号混合器中产生的混合液送至2号离心分离机中,进行离心分离,再次得到液相物质和固相物质;
6)步骤5分离出来的固相物质通过蒸脱机内蒸汽加热和喷蒸,加热温度为95-110℃,蒸脱喷蒸压力在0.1-0.23MPa,产生固体物质从出口排出,有机溶剂被蒸脱后以溶剂油形式回收;
7)步骤3和步骤5中离心分离出的液相物质汇合后依次进入升膜蒸发器和薄膜蒸发器中,蒸发温度在80-120℃,蒸发压力在0.1-0.2MPa,以沥青为主的石油成份产品从薄膜蒸发器出口排出,即得到提纯产品,有机溶剂被蒸脱后以溶剂油形式回收;
8)步骤6和步骤7中回收的溶剂油再次被步骤2和步骤4中利用。
其中步骤中的有机溶剂按体积百分比组成为,己烷70%和苯30%。
再次分离的固相物质,经检测,无可溶解物质。
实施例二
除油砂与有机溶剂的重量比为1:0.5,两次混合萃取的时间分别为3分钟外,其余步骤与实施例一相同。所述的有机溶剂按体积百分比组成为,乙醇5%、苯25%和己烷70%。该实施例经两次萃取、分离后,对固相物检测,无可溶解物质。
实施例三
除油砂与有机溶剂的重量比为1:0.4,油砂颗粒度直径1mm<d≤3mm,两次混合萃取的时间分别为3分钟外,其余步骤与实施例一相同。所述的有机溶剂按体积百分比组成为,乙酸5%、苯25%和己烷70%。该实施例经两次萃取、分离后,对固相物检测,无可溶解物质。
实施例四
除油砂与有机溶剂的重量比为1:0.4,油砂颗粒度直径3mm<d≤6mm,两次混合萃取的时间分别为10分钟外,其余步骤与实施例一相同。所述的有机溶剂按体积百分比组成为,乙酸乙酯30%、苯20%和己烷50%。该实施例经两次萃取、分离后,对固相物检测,无可溶解物质。
实施例五
除所述的有机溶剂按体积百分比组成为,环己烃50%和己烷50%外,其余与实施例一相同。
综上所述,该油砂萃取分离工艺方法的特点为:
1)油砂粉碎在0-25℃的条件下进行,萃取过程中无需再次筛分;
2)萃取过程在常温常压或微负压下进行,无需加热,故节省了大量的热源;
3)萃取过程中通惰性气体保护,封闭混合,溶剂气体极少外泄,操作安全;
4)溶剂油以乙烷为主要成分的烷烃混合溶剂油,回收容易,综合利用率高,毒性小,保护了周围环境,节能环保。

Claims (7)

  1. 一种油砂萃取分离工艺方法,其特征在于包括以下步骤:
    1)将筛选后的油砂在25℃-0℃的气温条件下进行粉碎,颗粒度直径0<d≤6mm;
    2)在常温下将油砂颗粒输送到1号混合器内,加入有机溶剂,油砂与有机溶剂的重量比为1:1-0.4,同时加入惰性气体,进行封闭的防爆搅拌萃取,萃取时间为3-10分钟;
    3)将萃取后的混合液输送至1号离心分离机中,进行离心分离,得到液相物质和固相物质;
    4)1号离心分离机离心后的固相物质在进入2号混合器中,加入有机溶剂,有机溶剂与油砂的重量比为1:1-0.4,同时加入惰性气体,进行封闭的防爆搅拌萃取,萃取时间为3-10分钟;
    5)2号混合器中产生的混合液送至2号离心分离机中,进行离心分离,再次得到液相物质和固相物质;
    6)步骤5分离出来的固相物质通过蒸脱机内蒸汽加热和喷蒸,加热温度为95-110℃,蒸脱喷蒸压力在0.1-0.23MPa,产生固体物质从出口排出,有机溶剂被蒸脱后以溶剂油形式回收;
    7)步骤3和步骤5中离心分离出的液相物质汇合后依次进入升膜蒸发器和薄膜蒸发器中,蒸发温度在80-120℃,蒸发压力在0.1-0.2MPa,以沥青为主的石油成份产品从薄膜蒸发器出口排出,有机溶剂被蒸脱后以溶剂油形式回收;
    8)步骤6和步骤7中回收的溶剂油再次被步骤2和步骤4中利用。
  2. 如权利要求1所述的油砂萃取分离工艺方法,其特征在于:所述的有机溶剂是醇类、酸类、脂类、烷烃类或环烷烃类的一种或两种以上的混合。
  3. 如权利要求2所述的油砂萃取分离工艺方法,其特征在于:所述的有机溶剂按体积百分比组成为,己烷70%和苯30%。
  4. 如权利要求2所述的油砂萃取分离工艺方法,其特征在于:所述的有机溶剂按体积百分比组成为,乙醇5%、苯25%和己烷70%。
  5. 如权利要求2所述的油砂萃取分离工艺方法,其特征在于:所述的有机溶剂按体积百分比组成为,乙酸5%、苯25%和己烷70%。
  6. 如权利要求2所述的油砂萃取分离工艺方法,其特征在于:所述的有机溶剂按体积百分比组成为,乙酸乙酯30%、苯20%和己烷50%。
  7. 如权利要求2所述的油砂萃取分离工艺方法,其特征在于:所述的有机溶剂按体积百分比组成为,环己烃50%和己烷50%。
PCT/CN2015/087228 2014-09-05 2015-08-17 油砂萃取分离工艺方法 WO2016034042A1 (zh)

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CN110395857A (zh) * 2018-04-19 2019-11-01 北京中科国通环保工程技术股份有限公司 处理含油含水物质的方法和装置
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