CN102390880A - Method for performing ultrasonic separation on oily wastewater with oil-soluble ferroferric oxide nanoparticles - Google Patents

Method for performing ultrasonic separation on oily wastewater with oil-soluble ferroferric oxide nanoparticles Download PDF

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CN102390880A
CN102390880A CN2011102004696A CN201110200469A CN102390880A CN 102390880 A CN102390880 A CN 102390880A CN 2011102004696 A CN2011102004696 A CN 2011102004696A CN 201110200469 A CN201110200469 A CN 201110200469A CN 102390880 A CN102390880 A CN 102390880A
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oil
water
waste
oily
ultrasonic
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李守柱
王传义
贾汉忠
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention relates to a method for performing ultrasonic separation on oily wastewater with oil-soluble ferroferric oxide nanoparticles. The method comprises the following steps: performing ultrasonic treatment on oily wastewater while adding oil-soluble ferroferric oxide nanoparticles in the oily wastewater, performing ultrasonic dispersion to ensure that ferroferric oxide enters the microdroplets of the wastewater with the help of the hydrophobic alkyl surface and magnetic oil microdroplets with ferroferric oxide particles are formed, and then combining magnetic separation to achieve the aim of removing the oil microdroplets in the wastewater. The method can be applied to treat the oily wastewater, improve the human living environment and increase the life quality of people. The oily wastewater treated by the method, particularly the oil extraction wastewater in the oilfield has a remarkable oil-water separation effect.

Description

The method of oil soluble ferriferrous oxide nano-particle ultrasonic separation oily(waste)water
Technical field
Invention belongs to the crossing domain of environment and material, and the method that relates to a kind of oil soluble ferriferrous oxide nano-particle ultrasonic separation oily(waste)water is used for separating the technology of oil in water emulsion and other form micro-droplet of oils of oily(waste)water.
Background technology
Oil field waste mainly contains three kinds of sources, and the one, oil well produced liquid separates the waste water that transfers, i.e. oil extraction waste water after the degassing, processed; The 2nd, desalinization of soil by flooding or leaching waste water; The 3rd, well-flushing water.Principal pollutant wherein are crude oil.At present, the most domestic oil field has got into the middle and later periods mining phase, mainly relies on water filling, annotates the crude oil in the technological displacement stratum such as tensio-active agent and polymer injection, and these measures have produced a large amount of reluctant recovered waters.Water ratio in the extraction liquid rises year by year, is generally 70%-80%.Oil in these waste water contains multiple carcinogenic polycyclic aromatic hydrocarbons, can get into human body through food chain behind the polluted-water, brings out cancer, health risk.
Magnetic separation technique is as a novel wastewater processing technology, and it is used and almost relates to all water treatment field.Magnetic separation technique has that excellent in efficiency, energy consumption are low, easy to operate, non-secondary pollution and low cost and other advantages.As a technology that has development prospect, the relevant in recent years report that directly or indirectly utilizes magnetic technology to handle oily(waste)water is increasing.Magnetic Nano material removes as the pollution clean-up agent has the advantage that general nano material specific surface area is big, adsorption rate is fast; Also has superparamagnetism; Can directly be dispersed in enrichment target contaminant in the solution; Magnetic can be accomplished pollution clean-up after separating fast, has overcome the agent of general nanometer pollution clean-up and has been difficult to isolating shortcoming.The nanometer Fe of oleic acid modified 3O 4Particle has obtained widespread use in some fields in recent years, but when being used for the environmental water sample pollutant removal, because the Fe of oleic acid modified 3O 4Have strong-hydrophobicity, be difficult to be dispersed in the water sample, and the organic impuritys such as humic acid in the water sample are easy and the effect of oleic acid group, make it remove the decline of organism effect in its surface thereby adhere to.But nanometer Fe on the other hand 3O 4Particle surface behind oleic acid modified has a large amount of non-polar group-long chain hydrocarbon groups, combines with oil droplet easily, in conjunction with suitable dispersing method, just can make its efficient micro-droplet of oil that gets into waste water make it have magnetic, realizes that magnetic separates the micro-droplet of oil in the oilfield sewage.
Summary of the invention
The object of the invention is, for the treatment process that solves existing oily(waste)water, oil production waste water in oil field is not effectively problem, a kind of method of oil soluble ferriferrous oxide nano-particle ultrasonic separation oily(waste)water is provided.This method is carried out oily(waste)water ultrasonic earlier; Simultaneously the oil soluble ferriferrous oxide nano-particle is dropped in the oily(waste)water ultransonic; Ultra-sonic dispersion; Z 250 just can get in the waste water micro-droplet of oil by its hydrophobic alkyl surface, forms the magnetic micro-droplet of oil that carries hydrophobic Z 250 particle, combines magnetic to separate again and reaches the purpose of removing micro-droplet of oil in the sewage.
The method of a kind of oil soluble ferriferrous oxide nano-particle ultrasonic separation oily(waste)water of the present invention follows these steps to carry out:
A, oily(waste)water is carried out the ultrasonic or probe type ultrasonic of ultrasound bath formula;
B, at the ultransonic oil soluble ferriferrous oxide nano-particle that adds simultaneously of oily(waste)water, ultra-sonic dispersion 5 minutes-3 hours;
The magnetic that c, the solution with step b after ultrasonic carry out permanent magnet or EM field separates, and can reach the micro-droplet of oil of removing in the oily(waste)water.
Oily(waste)water described in the step a is oil field waste, natural-gas field waste water, mechanical workout waste water or oil-containing waste water of catering.
Ultrasonic described in step a and the step b is continuous ultrasound, intermittent type is ultrasonic or pulsating ultrasound.
The add-on of the described oil soluble ferriferrous oxide nano-particle of step b is to add 0.1-5ml in every liter of oily(waste)water.
The described oil soluble ferriferrous oxide nano-particle of step b is the ferriferrous oxide nano-particle that oleic acid, linolic acid, LAURIC ACID 99 MIN, Palmiticacid, Triple Pressed Stearic Acid, myristic acid, carnaubic acid, linolenic acid or arachidonic acid are modified.
The method of oil soluble ferriferrous oxide nano-particle ultrasonic separation oily(waste)water of the present invention; It is ultrasonic that this method adopts the oil soluble ferriferrous oxide nano-particle to carry out in oily(waste)water; And form the magnetic micro-droplet of oil and carry out the isolating principle of magnetic, because oil soluble Fe 3O 4The surface is oil-soluble organic alkane backbone, is oil-soluble liposoluble surface tissue, and the micro-droplet of oil in the oily(waste)water also is oil-soluble organic phase, so work as the Fe of ultra-sonic dispersion oil soluble in water 3O 4The time, can make oil-soluble Fe 3O 4Micro-droplet of oil has the chance that fully contacts in hydrophobic hydrocarbon chain and the water on surface, utilizes Fe 3O 4The hydrocarbon chain on surface and the hydrophobic interaction power of micro-droplet of oil enter into the micro-droplet of oil of oily waste water sewage, further separate making micro-droplet of oil enrichment and the aqueous phase separation in the oily(waste)water through magnetic.Oil-soluble magnetic Nano Z 250 is distributed in the micro-droplet of oil, offers micro-droplet of oil magnetic, help magnetic and separate, solved micro-droplet of oil and separated difficult problem.Oil-containing wastewater is yellow turbid solution; The oil-contaminated water of oil field of the magnetic Nano Z 250 of dispersing hydrophobic, because the adding of Z 250, oil-containing wastewater becomes black; Use magnet to carry out the oil-containing wastewater after magnetic separates; It is limpid to find out that separation back water quality becomes, and the sump oil that contains the magnetic Nano Z 250 of oil soluble is adsorbed to a side of magnet, has successfully realized the magnetic separation.
Description of drawings
Fig. 1 is a principle of the invention synoptic diagram; Wherein
Figure BSA00000539561200031
is the oil soluble Z 250; ● be the oil soluble Z 250,
Figure BSA00000539561200032
is the waste water oil droplet.
Fig. 2 is the present invention ultrasonic oil-soluble Fe in oily(waste)water 3O 4Water quality UV-Vis variation diagram before and after the separating oil, wherein 1 is oily(waste)water before handling, 2 is 0.5%Fe 3O 4Handle oily(waste)water, 3 is 0.25%Fe 3O 4Handle oily(waste)water.
Fig. 3 is the present invention ultrasonic various dose oil soluble Fe in oily(waste)water 3O 4The 550nm optical density(OD) changes comparison diagram before and after the separating oil, and wherein 1 is oily(waste)water before handling, and 2 is 0.5%Fe 3O 4Handle oily(waste)water, 3 is 0.25%Fe 3O 4Handle oily(waste)water.
Embodiment
Embodiment 1
A, oil field waste 20ml is carried out ultrasound bath formula continuous ultrasound;
B, at the ultransonic oil soluble ferriferrous oxide nano-particle that adds oleic acid modified simultaneously of oil field waste, ultra-sonic dispersion 5 minutes, wherein the add-on of the oil soluble ferriferrous oxide nano-particle of oleic acid modified is to add 0.1ml in every liter of oily(waste)water;
The magnetic that c, the solution with step b after ultrasonic carry out permanent magnet separates; Use ultraviolet spectrophotometer scanning solution; Oilfield sewage demonstrates higher visible absorption phenomenon (Fig. 2) because the existence of micro-droplet of oil has scattering process so be muddy to visible light; Can there be absorption owing to alkene at this in the ultraviolet region especially; So demonstrate very strong absorption at wavelength less than the following UV-light of 300 nanometers, no matter and, can reach the micro-droplet of oil in the removal oily(waste)water through using the water sample after ultrasonic oil soluble ferriferrous oxide nano-particle separates still to absorb and all significantly descend in the ultraviolet region at visible-range.
Use of the variation (Fig. 3) of the water sample of oil soluble ferriferrous oxide nano-particle ultrasonic separation oily(waste)water micro-droplet of oil front and back in 550nm wavelength optical density(OD); Oilfield sewage is 1.679 in 550nm wavelength optical density(OD) before handling; Is 0.036 and use the water sample behind the ultrasonic 0.05ml oil soluble ferriferrous oxide nano-particle separation micro-droplet of oil in 550nm wavelength optical density(OD); The water sample that uses ultrasonic 0.1ml oil soluble ferriferrous oxide nano-particle to separate behind the micro-droplet of oil is 0.021 in 550nm wavelength optical density(OD), and visible have through using ultrasonic oil soluble ferriferrous oxide nano-particle to separate water sample before and after the micro-droplet of oil that consumption is few, the characteristics of good separating effect.
Embodiment 2
A, that natural-gas field waste water 20ml is carried out ultrasonic probe formula intermittent type is ultrasonic;
B, add the oil soluble ferriferrous oxide nano-particle that linolic acid is modified simultaneously in that natural-gas field waste water is ultransonic, ultra-sonic dispersion 10 minutes, wherein the add-on of the oil soluble ferriferrous oxide nano-particle modified of linolic acid is to add 0.5ml in every liter of oily(waste)water;
The magnetic that c, the solution with step b after ultrasonic carry out EM field separates, and uses ultraviolet spectrophotometer scanning solution, and sewage demonstrates higher visible absorption phenomenon because the existence of micro-droplet of oil has scattering process so be muddy to visible light.And, can reach the micro-droplet of oil of removing in the oily(waste)water through using the water sample after ultrasonic oil soluble ferriferrous oxide nano-particle separates to absorb all significantly decline at visible-range and ultraviolet region.Have through using ultrasonic oil soluble ferriferrous oxide nano-particle to separate water sample before and after the micro-droplet of oil that consumption is few, the characteristics of good separating effect.
Embodiment 3
A, mechanical workout oily(waste)water 20ml is carried out ultrasound bath formula pulsating ultrasound;
B, add the oil soluble ferriferrous oxide nano-particle that LAURIC ACID 99 MIN is modified simultaneously in that the mechanical workout oily(waste)water is ultransonic; Ultra-sonic dispersion 30 minutes, wherein the add-on of the oil soluble ferriferrous oxide nano-particle of LAURIC ACID 99 MIN modification is to add 1ml in every liter of oily(waste)water;
The magnetic that c, the solution with step b after ultrasonic carry out permanent magnet separates, and uses ultraviolet spectrophotometer scanning solution, and sewage demonstrates higher visible absorption phenomenon because the existence of micro-droplet of oil has scattering process so be muddy to visible light.No matter and the water sample after the ultrasonic oil soluble ferriferrous oxide nano-particle separation of process use can reach the micro-droplet of oil in the removal oily(waste)water in visible-range or all significantly decline of ultraviolet region absorption.
Embodiment 4
A, oil-containing waste water of catering 20ml is carried out ultrasonic probe formula continuous ultrasound;
B, add the oil soluble ferriferrous oxide nano-particle that Palmiticacid is modified simultaneously in that oil-containing waste water of catering is ultransonic, ultra-sonic dispersion 50 minutes, wherein the add-on of the oil soluble ferriferrous oxide nano-particle modified of Palmiticacid is to add 1.5ml in every liter of oily(waste)water;
The magnetic that c, the solution with step b after ultrasonic carry out EM field separates, and uses ultraviolet spectrophotometer scanning solution, and sewage demonstrates higher visible absorption phenomenon because the existence of micro-droplet of oil has scattering process so be muddy to visible light.No matter and the water sample after the ultrasonic oil soluble ferriferrous oxide nano-particle separation of process use can reach the micro-droplet of oil in the removal oily(waste)water in visible-range or all significantly decline of ultraviolet region absorption.
Embodiment 5
A, that oil field waste 20ml is carried out ultrasonic probe formula intermittent type is ultrasonic;
B, add the oil soluble ferriferrous oxide nano-particle that Triple Pressed Stearic Acid is modified simultaneously in that oil field waste is ultransonic, ultra-sonic dispersion 1 hour, wherein the add-on of the oil soluble ferriferrous oxide nano-particle modified of Triple Pressed Stearic Acid is to add 2ml in every liter of oily(waste)water;
The magnetic that c, the solution with step b after ultrasonic carry out EM field separates, and uses ultraviolet spectrophotometer scanning solution, and sewage demonstrates higher visible absorption phenomenon because the existence of micro-droplet of oil has scattering process so be muddy to visible light.No matter and the water sample after the ultrasonic oil soluble ferriferrous oxide nano-particle separation of process use can reach the micro-droplet of oil in the removal oily(waste)water in visible-range or all significantly decline of ultraviolet region absorption.
Embodiment 6
A, natural-gas field waste water is carried out ultrasound bath formula continuous ultrasound;
B, add the oil soluble ferriferrous oxide nano-particle that myristic acid is modified simultaneously in that natural-gas field waste water is ultransonic, ultra-sonic dispersion 1.5 hours, wherein the add-on of the oil soluble ferriferrous oxide nano-particle modified of myristic acid is to add 2.0ml in every liter of oily(waste)water;
The magnetic that c, the solution with step b after ultrasonic carry out permanent magnet separates, and uses ultraviolet spectrophotometer scanning solution, and sewage demonstrates higher visible absorption phenomenon because the existence of micro-droplet of oil has scattering process so be muddy to visible light.No matter and the water sample after the ultrasonic oil soluble ferriferrous oxide nano-particle separation of process use can reach the micro-droplet of oil in the removal oily(waste)water in visible-range or all significantly decline of ultraviolet region absorption.
Embodiment 7
A, that mechanical workout waste water is carried out ultrasonic probe formula intermittent type is ultrasonic;
B, add the oil soluble ferriferrous oxide nano-particle that carnaubic acid is modified simultaneously in that mechanical workout waste water is ultransonic; Ultra-sonic dispersion 2 hours, wherein the add-on of the oil soluble ferriferrous oxide nano-particle of carnaubic acid modification is to add 2.5ml in every liter of oily(waste)water;
The magnetic that c, the solution with step b after ultrasonic carry out EM field separates, and uses ultraviolet spectrophotometer scanning solution, and sewage demonstrates higher visible absorption phenomenon because the existence of micro-droplet of oil has scattering process so be muddy to visible light.No matter and the water sample after the ultrasonic oil soluble ferriferrous oxide nano-particle separation of process use can reach the micro-droplet of oil in the removal oily(waste)water in visible-range or all significantly decline of ultraviolet region absorption.
Embodiment 8
A, oil-containing waste water of catering is carried out ultrasound bath formula pulsating ultrasound;
B, add the oil soluble ferriferrous oxide nano-particle that linolenic acid is modified simultaneously in that oil-containing waste water of catering is ultransonic, ultra-sonic dispersion 25 minutes, wherein the add-on of the oil soluble ferriferrous oxide nano-particle modified of linolenic acid is to add 3.5ml in every liter of oily(waste)water;
The magnetic that c, the solution with step b after ultrasonic carry out permanent magnet separates, and uses ultraviolet spectrophotometer scanning solution, and sewage demonstrates higher visible absorption phenomenon because the existence of micro-droplet of oil has scattering process so be muddy to visible light.No matter and the water sample after the ultrasonic oil soluble ferriferrous oxide nano-particle separation of process use can reach the micro-droplet of oil in the removal oily(waste)water in visible-range or all significantly decline of ultraviolet region absorption.
Embodiment 9
A, natural-gas field waste water is carried out ultrasonic probe formula pulsating ultrasound;
B, add the oil soluble ferriferrous oxide nano-particle that arachidonic acid is modified simultaneously in that the natural-gas field oily(waste)water is ultransonic; Ultra-sonic dispersion 3 hours, wherein the add-on of the oil soluble ferriferrous oxide nano-particle of arachidonic acid modification is to add 5ml in every liter of oily(waste)water;
The magnetic that c, the solution with step b after ultrasonic carry out EM field separates, and uses ultraviolet spectrophotometer scanning solution, and sewage demonstrates higher visible absorption phenomenon because the existence of micro-droplet of oil has scattering process so be muddy to visible light.No matter and the water sample after the ultrasonic oil soluble ferriferrous oxide nano-particle separation of process use can reach the micro-droplet of oil in the removal oily(waste)water in visible-range or all significantly decline of ultraviolet region absorption.

Claims (5)

1. the method for an oil soluble ferriferrous oxide nano-particle ultrasonic separation oily(waste)water is characterized in that following these steps to carrying out:
A, oily(waste)water is carried out the ultrasonic or probe type ultrasonic of ultrasound bath formula;
B, at the ultransonic oil soluble ferriferrous oxide nano-particle that adds simultaneously of oily(waste)water, ultra-sonic dispersion 5 minutes-3 hours;
The magnetic that c, the solution with step b after ultrasonic carry out permanent magnet or EM field separates, and can reach the micro-droplet of oil of removing in the oily(waste)water.
2. method according to claim 1 is characterized in that the oily(waste)water described in the step a is oil field waste, natural-gas field waste water, mechanical workout waste water or oil-containing waste water of catering.
3. method according to claim 2, it is characterized in that described in step a and the step b ultrasonic for continuous ultrasound, intermittent type is ultrasonic or pulsating ultrasound.
4. method according to claim 3, the add-on that it is characterized in that the described oil soluble ferriferrous oxide nano-particle of step b is to add 0.1-5ml in every liter of oily(waste)water.
5. method according to claim 4 is characterized in that the described oil soluble ferriferrous oxide nano-particle of step b is the ferriferrous oxide nano-particle that oleic acid, linolic acid, LAURIC ACID 99 MIN, Palmiticacid, Triple Pressed Stearic Acid, myristic acid, carnaubic acid, linolenic acid or arachidonic acid are modified.
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Cited By (7)

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CN104014163A (en) * 2014-06-19 2014-09-03 中国科学院新疆理化技术研究所 Preparation method and application of aminoethyl aminopropyl modified ferroferric oxide
CN104830367A (en) * 2015-05-25 2015-08-12 哈尔滨工业大学 Method for separating shale oil and water mixture by using paraffin and magnetic iron
CN105294908A (en) * 2015-11-20 2016-02-03 云南健牛生物科技有限公司 Synthesis method and applications of magnetic nano high-molecular polymer
CN107417922A (en) * 2017-05-08 2017-12-01 苏州科技大学 A kind of mixed with polymers graft modification magnetic Nano silica and its application
CN108421533A (en) * 2018-03-22 2018-08-21 清华大学 A kind of magnetic nanoparticle of surface modification, preparation method, application and regeneration method
CN111635050A (en) * 2019-12-16 2020-09-08 江苏久吾高科技股份有限公司 Method and device for treating high-salinity mine water
CN112408537A (en) * 2020-11-11 2021-02-26 江南大学 Composition, preparation and application of pH/magnetic dual-responsiveness nanoparticles

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Publication number Priority date Publication date Assignee Title
CN104014163A (en) * 2014-06-19 2014-09-03 中国科学院新疆理化技术研究所 Preparation method and application of aminoethyl aminopropyl modified ferroferric oxide
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CN104830367A (en) * 2015-05-25 2015-08-12 哈尔滨工业大学 Method for separating shale oil and water mixture by using paraffin and magnetic iron
CN105294908A (en) * 2015-11-20 2016-02-03 云南健牛生物科技有限公司 Synthesis method and applications of magnetic nano high-molecular polymer
CN107417922A (en) * 2017-05-08 2017-12-01 苏州科技大学 A kind of mixed with polymers graft modification magnetic Nano silica and its application
CN107417922B (en) * 2017-05-08 2020-07-14 苏州科技大学 Polymer mixed graft modified magnetic nano-silica and application thereof
CN108421533A (en) * 2018-03-22 2018-08-21 清华大学 A kind of magnetic nanoparticle of surface modification, preparation method, application and regeneration method
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CN111635050A (en) * 2019-12-16 2020-09-08 江苏久吾高科技股份有限公司 Method and device for treating high-salinity mine water
CN112408537A (en) * 2020-11-11 2021-02-26 江南大学 Composition, preparation and application of pH/magnetic dual-responsiveness nanoparticles

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