WO2017054256A1 - 利用碳纳米管海绵电控驱油技术回收油污的方法 - Google Patents

利用碳纳米管海绵电控驱油技术回收油污的方法 Download PDF

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WO2017054256A1
WO2017054256A1 PCT/CN2015/092287 CN2015092287W WO2017054256A1 WO 2017054256 A1 WO2017054256 A1 WO 2017054256A1 CN 2015092287 W CN2015092287 W CN 2015092287W WO 2017054256 A1 WO2017054256 A1 WO 2017054256A1
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carbon nanotube
oil
nanotube sponge
sponge
electrolyte
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薛亚辉
李锡英
段慧玲
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Peking University
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material

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  • the present invention relates to nanotechnology. More specifically, the present invention relates to a method for recovering oil stains using a carbon nanotube sponge electrically controlled flooding technique.
  • the present invention provides a method for recycling oil stains using a carbon nanotube sponge.
  • the method fully utilizes the good electrical conductivity of the carbon nanotube sponge and the strong oil absorption capability, and based on the principle of electrowetting, the electrolyte can be controlled by an electrolyte (for example, seawater) at a lower voltage (for example, about -1V).
  • an electrolyte for example, seawater
  • a lower voltage for example, about -1V
  • a method for recovering oil stains using the carbon nanotube sponge electronically controlled oil displacement technology of the present invention includes:
  • Step S1 placing a carbon nanotube sponge on an oil stain surface to adsorb oil stain;
  • Step S2 contacting the carbon nanotube sponge with an electrolyte, and applying a voltage to drive the adsorbed oil stain;
  • step S3 the carbon nanotube sponge is washed.
  • the electrolyte is a 1 wt% solution of dodecyltrimethylammonium bromide.
  • the electrolyte is seawater.
  • the voltage is -1.2V.
  • step S3 the carbon nanotube sponge is repeatedly washed with alcohol and pure water, and then subjected to high-temperature vacuum drying.
  • the method further comprises: repeating the processes S1-S3 using the washed and dried sponge to perform multiple and/or multiple oil recovery.
  • the oil stain comprises one or more of the following: cyclohexane, n-hexane, 12 alkane, edible oil, high speed vacuum pump oil, gasoline, and diesel.
  • FIG. 1 is a flow chart of a method for recovering oil stains using a carbon nanotube sponge electronically controlled oil displacement technique in accordance with an embodiment of the present invention.
  • the invention provides a method for recycling carbon oil by carbon nanotube sponge, which fully utilizes high specific surface area, superhydrophobicity and good electrical conductivity of carbon nanotube sponge, combined with water-soluble active agent, at a lower voltage,
  • the oil adsorbed in the sponge is driven off by the aqueous electrolyte solution, and then the carbon nanotube sponge is recycled to recover the oil stain by means of washing and high-temperature drying. This not only improves the efficiency of oil recovery, but also applies to different types of oil recovery.
  • FIG. 1 is a flow chart of a method for recovering oil stains using a carbon nanotube sponge electronically controlled oil displacement technique in accordance with an embodiment of the present invention. As shown in Figure 1, the method includes:
  • Step S1 placing a carbon nanotube sponge on an oil stain surface to adsorb oil stain;
  • Step S2 contacting the carbon nanotube sponge with an electrolyte, and applying a voltage to drive the adsorbed oil stain;
  • step S3 the carbon nanotube sponge is washed.
  • the carbon nanotube sponge in step S3, may be repeatedly washed with alcohol and pure water, and finally Perform high temperature vacuum drying.
  • the washed sponge can be repeated for the process S1-S3 to perform multiple and/or multiple oil recovery.
  • aqueous electrolyte solution such as 1M KOH
  • water-soluble active agent such as 1wt% dodecyltrimethylammonium bromide, DTAB
  • the carbon nanotube sponge of 4) is lowered into contact with the electrolyte, and a voltage of -1.2 V (relative to the Ag/AgCl reference electrode in 3M KCl) is applied, and the electrolyte is used to test the displacement of the carbon nanotube sponge.
  • Example 1 Controlled displacement of cyclohexane in carbon nanotube sponge
  • the selected carbon nanotube sponge is suspended under a microbalance, and then contacted with cyclohexane, and the mass of the carbon nanotube is absorbed when the carbon nanotube sponge is saturated, and the carbon nanotube sponge saturated with the absorption of cyclohexane is contacted.
  • the electrolyte was applied, and after applying a voltage of -1.2 V, the mass of the sponge was recorded when the electrolyte was displaced from the cyclohexane in the carbon nanotube sponge until the mass of the balance no longer changed.
  • the selected carbon nanotube sponge is suspended under a microbalance, and then contacted with n-hexane to weigh the mass of the n-hexane absorbed by the carbon nanotube sponge, and the carbon nanotube sponge saturated with n-hexane is contacted to the electrolyte. After applying a voltage of -1.2 V, the mass of the sponge was recorded when the electrolyte was displaced from the n-hexane in the carbon nanotube sponge until the mass of the balance no longer changed.
  • the selected carbon nanotube sponge is suspended under the microbalance, and then contacted with the high-speed vacuum pump oil to absorb the mass of the vacuum pump oil when the carbon nanotube sponge is saturated with oil; the carbon nanotube sponge of the saturated absorption vacuum pump oil is brought into contact with the electrolyte After applying a voltage of -1.2 V, the electrolyte was recorded to drive the vacuum pump oil in the carbon nanotube sponge until the mass of the balance no longer changed, and the mass of the sponge changed.
  • the selected carbon nanotube sponge is suspended under a microbalance, and then contacted with gasoline, and the mass of the gasoline absorbed by the carbon nanotube sponge is measured; the carbon nanotube sponge of the saturated absorption gasoline is brought into contact with the electrolyte, and -1.2 is applied. After the V voltage, the mass of the sponge was recorded when the electrolyte was displaced from the carbon nanotube sponge until the mass of the balance no longer changed.
  • the selected carbon nanotube sponge is suspended under a microbalance, and then contacted with diesel oil to weigh the mass of the diesel oil absorbed by the carbon nanotube sponge when saturated; the saturated carbon nanotube sponge of the absorbed diesel oil is contacted to the electrolyte, and -1.2 is applied. After the V voltage, the mass of the sponge was recorded when the electrolyte was displaced from the carbon nanotube sponge until the mass of the balance no longer changed.
  • Table 1 shows the oil absorption mass ratio, the oil displacement mass ratio, the displacement efficiency, and the time taken to drive the 1 cm carbon tube for the various oil stains in the above examples. It can be seen that the oil displacement method according to the present invention has high oil absorption and oil displacement efficiency and high oil displacement speed, and can obtain a very good oil pollution recovery effect in a short time.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
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Abstract

一种利用碳纳米管海绵电控驱油技术回收油污的方法，包括：将碳纳米管海绵置于油污表面以吸附油污；将所述碳纳米管海绵接触电解液，加电压驱替所吸附的油污；以及清洗所述碳纳米管海绵。

Description

利用碳纳米管海绵电控驱油技术回收油污的方法 技术领域
本发明涉及纳米技术。更具体地，本发明涉及一种利用碳纳米管海绵电控驱油技术回收油污的方法。
背景技术
随着社会经济的迅速发展，人类的生产生活对环境的破坏越来越严重，水污染也是其中的一个重要问题，而油污则是水污染中重要的一部分。随着人类对于石油需求的不断增加，海上石油开采和运输所导致的石油泄漏事件频频发生，泄漏的石油漂浮在海面上迅速扩展形成油膜，油膜的形成将导致海洋生态遭到破坏，使鱼类窒息、鸟类失去飞行能力甚至是影响海洋生物的生长。
目前多种吸油材料已经被提出用于清除泄露的油污，包括天然纤维材料、高分子合成材料和无机材料等三大类。在这一应用中，材料对油污的选择性吸附能力至关重要。市场上应用较多的是天然纤维和以聚丙烯和聚亚安酯为主制成的吸附剂。例如，棉花、秸秆锯木屑等天然纤维虽然成本低廉，但是在吸收漏油的过程中电会吸收海水，导致后期回收不方便。活性炭作为吸附剂不仅饱和吸附量小，而且吸附后会沉降到水底，回收比较困难。
近来，随着纳米加工技术的进步，新型纳米材料的涌现为开发更有效的吸油材料提供了新的契机。研究表明，具有高比表面积的碳纳米管海绵和石墨烯海绵表现出很好的吸油性质，且同时不会吸收海水，降低了后期回收的难度。在海绵吸油之后，利用机械压缩和燃烧两步法或热处理法可以实现对其中油污的回收以及海绵的再利用。然而，压缩-燃烧法对油污的回收效率较低，且对海绵结构产生一定的破坏作用；而热处理法对于回收沸点较高油类具有一定的局限性。因此，需要提出新的设计方案来提高利用碳材料海绵回收油污的效率和适用性。这里以碳纳米管海绵为例，利用其良好的导电性以及较强的油污吸附能力，提出利用电浸润原理、由可控的电解液驱油技术实现对油污的有效回收和利用。
发明内容
本发明提供了一种利用碳纳米管海绵可循环回收油污的方法。该方法充分利用了碳纳米管海绵良好的导电性以及较强的吸油能力，基于电浸润原理，利用电解液(例如，海水)可控驱油技术，在较低的电压(例如，约-1V)下实现对吸附油污的回收和再利用。这样可以 很大地提高油污回收的效率，并且海绵在干燥之后，可以循环利用。该方法可适用于不同油类或油类混合物的回收。
本发明的一种利用碳纳米管海绵电控驱油技术回收油污的方法包括：
步骤S1，将碳纳米管海绵置于油污表面以吸附油污；
步骤S2，将所述碳纳米管海绵接触电解液，加电压驱替所吸附的油污；以及
步骤S3，清洗所述碳纳米管海绵。
可选地，电解液为1wt％十二烷基三甲基溴化铵溶液。
可选地，电解液为海水。
可选地，电压为-1.2V。
可选地，在步骤S3中，用酒精和纯水反复清洗该碳纳米管海绵，然后进行高温真空干燥。
可选地，该方法还包括：使用清洗干燥后的海绵重复过程S1-S3，以进行多次和/或多种油污回收。
可选地，所述油污包括以下中的一种或多种：环己烷、正己烷、12烷、食用油、高速真空泵油、汽油、和柴油。
附图说明
图1是根据本发明实施例利用碳纳米管海绵电控驱油技术回收油污的方法流程图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明白，以下结合具体实施例，并参照附图，对本发明进一步详细说明。
本发明提供了一种碳纳米管海绵可循环回收油污的方法，充分利用碳纳米管海绵的高比表面积、超疏水以及良好的导电性，结合水溶性的活性剂，在较低的电压下，利用电解质水溶液将海绵内吸附的油污驱除，然后再利用清洗和高温干燥的方法，循环利用碳纳米管海绵回收油污。这样不仅提高了油污回收的效率，而且还可以适用于不同类型的油类回收。
图1是根据本发明实施例利用碳纳米管海绵电控驱油技术回收油污的方法流程图。如图1所示，该方法包括：
步骤S1，将碳纳米管海绵置于油污表面以吸附油污；
步骤S2，将所述碳纳米管海绵接触电解液，加电压驱替所吸附的油污；以及
步骤S3，清洗所述碳纳米管海绵。
根据本发明的实施例，在步骤S3中，可以用酒精和纯水反复清洗该碳纳米管海绵，最后 进行高温真空干燥。
根据本发明的实施例，清洗干燥后的海绵可以重复过程S1-S3，以进行多次和/或多种油污回收。
下面描述测试根据本发明的实施例使用碳纳米管海绵清除油污的方法性能的具体过程，包括如下步骤：
1)配制电解质水溶液(如1M KOH)，在水溶液里加入一定比例的水溶性活性剂(如1wt％十二烷基三甲基溴化铵，DTAB)，并将混合水溶液倒入烧杯中；
2)将所使用的试验用油倒入烧杯中的水溶液表面，形成均匀的油层；
3)将所选用的碳纳米管海绵称重(不包括导线质量)；
4)将所选用的碳纳米管海绵悬挂在微天平下，然后接触试验用油，称量碳纳米管海绵吸油饱和时吸收试验用油的质量；
5)将4)的碳纳米管海绵下降接触到电解液，施加-1.2V电压(相对于3M KCl中的Ag/AgCl参比电极)后，称量电解液驱替碳纳米管海绵中试验用油至天平质量不再变化时的海绵质量变化；以及
6)将5)中的碳纳米管海绵用去离子水和酒精反复清洗，并在高温(200℃)下干燥5小时；以及
7)将清洗干燥后的碳纳米管海绵按照上述步骤重复试验。
将上述测试方法用于以下示例1-7，可以说明碳纳米管海绵对环己烷、正己烷、12烷、食用油、高速真空泵油、汽油、柴油的可控驱替结果。
示例1：可控驱替碳纳米管海绵中的环己烷
将所选用的碳纳米管海绵悬挂在微天平下，然后接触环己烷，称量碳纳米管海绵吸油饱和时吸收环己烷的质量；将饱和吸收环己烷的碳纳米管海绵下降接触到电解液，施加-1.2V电压后，记录电解液驱替碳纳米管海绵中环己烷至天平质量不再变化时海绵质量变化。
示例2：可控驱替碳纳米管海绵中的12烷
将所选用的碳纳米管海绵悬挂在微天平下，然后接触12烷，称量碳纳米管海绵吸油饱和时吸收12烷的质量；将饱和吸收12烷的碳纳米管海绵下降接触到电解液，施加-1.2V电压后，记录电解液驱替碳纳米管海绵中12烷至天平质量不再变化时海绵质量变化。
示例3：可控驱替碳纳米管海绵中的正己烷
将所选用的碳纳米管海绵悬挂在微天平下，然后接触正己烷，称量碳纳米管海绵吸油饱和时吸收正己烷的质量；将饱和吸收正己烷的碳纳米管海绵下降接触到电解液，施加-1.2V电压后，记录电解液驱替碳纳米管海绵中正己烷至天平质量不再变化时海绵质量变化。
示例4：可控驱替碳纳米管海绵中的食用油
将所选用的碳纳米管海绵悬挂在微天平下，然后接触食用油，称量碳纳米管海绵吸油饱和时吸收食用油的质量；将饱和吸收食用油的碳纳米管海绵下降接触到电解液，施加-1.2V电压后，记录电解液驱替碳纳米管海绵中食用油至天平质量不再变化时海绵质量变化。
示例5：可控驱替碳纳米管海绵中的高速真空泵油
将所选用的碳纳米管海绵悬挂在微天平下，然后接触高速真空泵油，称量碳纳米管海绵吸油饱和时吸收真空泵油的质量；将饱和吸收真空泵油的碳纳米管海绵下降接触到电解液，施加-1.2V电压后，记录电解液驱替碳纳米管海绵中真空泵油至天平质量不再变化时海绵质量变化。
示例6：可控驱替碳纳米管海绵中的汽油
将所选用的碳纳米管海绵悬挂在微天平下，然后接触汽油，称量碳纳米管海绵吸油饱和时吸收汽油的质量；将饱和吸收汽油的碳纳米管海绵下降接触到电解液，施加-1.2V电压后，记录电解液驱替碳纳米管海绵中汽油至天平质量不再变化时海绵质量变化。
示例7：可控驱替碳纳米管海绵中的柴油
将所选用的碳纳米管海绵悬挂在微天平下，然后接触柴油，称量碳纳米管海绵吸油饱和时吸收柴油的质量；将饱和吸收柴油的碳纳米管海绵下降接触到电解液，施加-1.2V电压后，记录电解液驱替碳纳米管海绵中柴油至天平质量不再变化时海绵质量变化。
下表1中的数据示出了以上示例中针对各种油污的吸油质量比、驱油质量比、驱替效率以及驱替1cm碳管所用时间。可以看出，根据本发明的驱油方法，吸油和驱油效率高、驱油速度快，能够在较短时间内获得非常好的油污回收效果。
表1
Figure PCTCN2015092287-appb-000001
Figure PCTCN2015092287-appb-000002
以上所述的具体实施例，对本发明的目的、技术方案和有益效果进行了进一步详细说明，所应理解的是，以上所述仅为本发明的具体实施例而已，并不用于限制本发明，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (7)

  1. 一种利用碳纳米管海绵电控驱油技术回收油污的方法，包括：
    步骤S1，将碳纳米管海绵置于油污表面以吸附油污；
    步骤S2，将所述碳纳米管海绵接触电解液，加电压驱替所吸附的油污；以及
    步骤S3，清洗所述碳纳米管海绵。
  2. 根据权利要求1所述的方法，其中，电解液为1wt％十二烷基三甲基溴化铵溶液。
  3. 根据权利要求1所述的方法，其中，电解液为海水。
  4. 根据权利要求1所述的方法，其中，电压为-1.2V。
  5. 根据权利要求1所述的方法，其中，在步骤S3中，用酒精和纯水反复清洗该碳纳米管海绵，然后进行高温真空干燥。
  6. 根据权利要求1所述的方法，还包括：使用清洗干燥后的海绵重复过程S1-S3，以进行多次和/或多种油污回收。
  7. 根据权利要求1所述的方法，其中，所述油污包括以下中的一种或多种：环己烷、正己烷、12烷、食用油、高速真空泵油、汽油、和柴油。
PCT/CN2015/092287 2015-09-29 2015-10-20 利用碳纳米管海绵电控驱油技术回收油污的方法 Ceased WO2017054256A1 (zh)

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