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Ultrasonics - Sonochemistry
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Review
A R T I C L E I N F O A B S T R A C T
Keywords: Technologies based on cavitation, produced by either ultrasound or hydrodynamic means, are part of growing
Cavitation literature for individual refinery unit processes. In this review, we have explained the mechanism through which
Crude oil these cavitation technologies intensify individual unit processes such as enhanced oil recovery, demulsification
Desulphurisation of water in oil emulsions during desalting stage, crude oil viscosity reduction, oxidative desulphurisation/de-
Crude upgrading
metallization, and crude oil upgrading. Apart from these refinery processes, applications of this technology are
Enhanced oil recovery
Oil sand extraction
also mentioned for other potential crude oil sources such as oil shale and oil sand extraction. The relative
Oil shale advantages and current situation of each application/process at commercial scale is explained.
Petroleum industry
⁎
Corresponding author.
E-mail address: balasubrahmanyam.avvaru@ril.com (B. Avvaru).
https://doi.org/10.1016/j.ultsonch.2017.12.010
Received 6 January 2017; Received in revised form 2 November 2017; Accepted 4 December 2017
Available online 05 December 2017
1350-4177/ © 2017 Elsevier B.V. All rights reserved.
B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
enhanced oil recovery, oil extraction from unconventional sources, pi- considerably reduce the influence of capillary forces on oil percolation,
peline transport and downstream refinery processes. Finally, industrial coalescence of oil drops due to the Bjerknes forces, resulting in an in-
scale cavitation reactors, reactor configurations and their operating creased rate of migration through the porous medium. Mechanical vi-
strategy are discussed. brations destroy the surface films adsorbed on the pore boundaries,
thereby increasing the effective cross-section of pores and accelerating
2. Ultrasound enhanced oil recovery the process of the penetration of liquids into capillaries (Sono-capillary
effect) [18]. A complete analysis of oil percolation, capillary interaction
Declining production of oil from the reservoir is of major concern to and oil recovery under ultrasonic waves has been well explained with
the oil companies. The various oil production methods can be classified laboratory experiments. It is reported [19] that ultrasound irradiation
as primary, secondary and tertiary. Under primary production, the enhances surfactant solubility and capillary imbibition recovery of oil
natural well pressure in the reservoir generally allows 30 percent re- for various fluid pairs besides reducing surfactant adsorption onto the
covery of the oil present in the formation. The residual oil after primary rock matrix [20]. Venkitaraman et al. [21] studied the removal of near
production is difficult to produce because of its very low mobility well bore damage by ultrasonic radiation. Based on a laboratory study
caused by decreased permeability in the producing wellbore by the focussed on removal of mud solids on a plug, they mentioned that
deposition of scales and precipitants, increased viscosity of the oil, acoustic streaming and cavitation generated from ultrasonic waves can
blockage of pores etc. [9,10]. The secondary production methods in- remove the damages by mud particles and also increase the perme-
clude gas and brine reinjection or water flooding. The injected fluid ability several times. Substantial amount of work [22–29] has been
displaces the produced reservoir fluid directly into the production wells carried out using laboratory model systems to find the exact me-
or maintains the reservoir pressure. A most common method involves chanism. Hamidi et al. [30] revealed through laboratory experiments,
flooding the reservoir with water. The ultimate recovery factor can be that oil recovery can be improved considerably by using ultrasound-
increased to 40–50% using these secondary recovery methods [10–12]. assisted CO2 flooding compared to conventional CO2 flooding, and
However during such production, the steam or water addition to the found that the changes were more pronounced for uncontrolled tem-
reservoir may cause stable emulsion formation with the polar hydro- perature conditions of ultrasound-assisted CO2 flooding.
carbon compounds. These production methods are affected by the The first industrial tests of the ultrasonic method for reservoir sti-
disadvantages of stable water-in-oil emulsions on flow owing to higher mulation reported the treatment of several productive wells at
friction factor, viscosity and correspondingly larger pressure drop [13]. Samotlorskoye and Fedorovskoye oil fields in Western Siberia [31,32]
The tertiary production methods, also known as enhanced oil recovery with an overall success rate of about 52 percent. For a successful
(EOR) methods, focus on recovery of the remaining oil in the reservoir treatment, the effect of enhanced production may last for 3–24 months
after the primary and secondary methods. They include layer burning, with a significant increase in production. However, in some other wells
solvent and acid injection treatment by mechanical scrapers and high the enhanced oil recovery effect lasted for 1.5 months only before the
pressure fracturing. These methods may not be suitable for every type production dipped far below the initial level. During 1991 Shaw Re-
of reservoir either due to uneconomical, technical limitations, or due to source services conducted tests on seventeen wells using their patented
undesirable side effects. They may require shutting in production, or “Sona-Tool” on the wells showing declining oil and water production
may create harmful ecological consequences, and may be economically rates before the stimulation [33]. They reported a 40–50% success rate
not feasible. for three minutes of ultrasonic excitation with the duration of the effect
Before we examine various ultrasound based applications for en- lasting up to one month in most effective cases. Shaw Resource services
hanced oil recovery, it is instructive to know the possible reasons for [33] have described the criteria for the selection of wells for successful
decrease in production of oil from wells. These can be based on factors acoustic treatment. The reservoir should show declining production
that would affect the permeability of the near-well zone of the reservoir attributed to near borehole zone plugged by deposits and should not
as stated below [14]: exhibit a significant drop of internal pressure. Other reservoir char-
acteristics should include: Porosity of internal well structure should be
1. Fluid-fluid incompatibilities, for example, emulsions generated be- 5% or above, significant gas content (more than 10 m3 gas/m3 total
tween invading oil based mud filtrate and formation water. fluid) and a maximum oil viscosity of 10−2 Pa s. Abramov et al. [34]
2. Deposition of organic or inorganic scale precipitation, solid plugging reported that in wells with permeability above 20 mD and porosity
are the main causes of this problem. greater than 15%, ultrasonic treatment can increase oil production by
3. Fines migration, for example the internal movement of fine parti- 50% or even more in some cases. The effect of ultrasonic treatment lasts
culates within a rock’s pore structure resulting in the bridging and from 3 to 12 months. For wells of lower permeability and porosity,
plugging of pore throats. ultrasonic treatment alone is less successful but high production rates
4. Deposition of reaction products as a result of widely used treatments can be achieved when it is applied in conjunction with chemical re-
near-well zone of formation of chemical reagents and paraffin/as- agents. In this case, an average productivity increase of nearly threefold
phaltene deposition. can be achieved by synergistically combining ultrasound with chemical
treatment (Sono-Chemical) methods. The ultrasonic treatment not only
In addition, the physical and chemical characteristics of the impact contributes to the cleaning of the perforation zone and increasing the
of these factors on the formation are different in nature. Ultrasound mobility of oil, but also increases the penetration of the reagent into the
based applications work on improving the well production from the formation and hence accelerates the chemical reaction in the porous
adverse impact of above mentioned factors as examined further. media of formation.
The early use of sound to revitalize oil wells involved audible sound The sono-chemical method of EOR can also be applied to horizontal
i.e. sonic waves of a much longer wavelength than ultrasound, often wells. Abramov et al. [34] described the theoretical background of
termed seismic waves [15]. The use of elastic wave stimulation has applying sono-chemical technology in horizontal wells including
been suggested as an alternative or complementary tool to conventional equipment required. The ultrasound EOR equipment consisted of
EOR methods. This technique first attracted the attention of researchers downhole equipment including a sonotrode, a system for injection of
in the US and USSR in the late 1950 s. A good review on elastic wave chemicals and a probe for acquiring geophysical data (temperature,
stimulation for enhanced oil recovery has been available in the litera- pressure and flow). The equipment has a special cable with a hydraulic
ture [15]. The penetration of low frequency elastic waves through channel for injection of technological fluids (surfactant formulations)
porous medium, creates harmonics with higher frequencies [16]. Ni- and includes electrical cores to power the equipment and the geophy-
kolaevskiy [17] speculates that excitation by elastic waves may sical probe. For other than the injection of reagents directly to the zone
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B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
Table 1
World reserves of Oil shale deposits [44].
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B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
Table 2
Total world reserves of original Natural bitumen (Tar-sands) and Extra-Heavy oil [54].
solvent to reach inside the oil shale structure and thereafter the cavi-
tational events causing them to break down the insoluble cross linked
structure of kerogen. Zhao et al. [53] carried out ultrasonic extraction
of kerogen from Huadian oil shale with 60 kHz frequency of ultrasound.
They achieved a maximum extraction of 15.6% using a solvent having
60 wt% CHCl3 and 40 wt% of CS2. The optimised mass ratio of demi-
neralized oil shale to CHCl3-CS2 was found to be 1:20.
As discussed, other than a few laboratory literature available for
extraction of kerogen from oil shale using cavitation, no work has been
Fig. 2. Sono-chemical recovery of Bitumen from oil-sands Region A: Extraction of oily
reported at pilot scale. May be the high cost associated with the
fractions of bitumen Region B: Neutralisation of resinous compounds/production of in
grinding of whole rock to target size and solvent regeneration in the situ surfactants Region C: Cracking of asphaltene micelles.
process may be hampering the application to the pilot scale level.
Considering the large reserves of world oil shale resources, further
developments are needed to process them by these cavitation methods. molecules in a membrane-mimetic fashion [65–67]. Sadeghi et al. [68]
carried out kinetic studies on three different oil sand samples, and re-
vealed that formation of these in situ formed surfactants follow an
4. Oil sand extraction using ultrasound cavitation autocatalytic mechanism. For all the samples, the cumulative recovery
curves for the experiments performed so far resembled the ‘S’ shaped
Oil sand is made up of grains of quartz sand, surrounded by a layer characteristic rate curve shown in Fig. 2. Extraction of bitumen dy-
of water and clay, and then covered in a slick of heavy oil called bi- namics can be represented by three regions (A, B, and C) as shown in
tumen. Deposits of oil sand and extra heavy oils exist throughout the the Fig. 2. Region ‘A’ is where the oily fraction of bitumen is released. In
world, and as shown in Table 2 [54] most of them were found in Alberta region ‘B’, neutralization of resinous compounds occurs and production
(Canada) and in Orinoco (Venezuela) respectively [55,56]. In view of of in situ surfactants are initiated. These natural surfactants then dis-
rising oil consumption, the extraction of bitumen/residual oil from oil rupt the already exposed asphaltene micelles through the inversion
bearing sand has become increasingly important. To use bitumen as an process to form Hartley micelles. Region ‘C’ illustrates an advantage of
energy source, it must be first extracted from oil sand and then up- using the power of cavitation. In this region, actual cracking of as-
graded to light oils. Wen et al. [57] described bitumen as consisting of phaltene micelles occurs. In this way, without exhaustion these sur-
following fractions: gas oil (saturated/aromatic hydrocarbons), resin, factants can be reused by maintaining the pH of the solution in alkaline
asphaltene, and carbene/carboid (preasphaltenes). Although the bi- region. The bitumen from Athabasca oil sand has an average API
tumen saturation of tar sands may vary from 10 to 18%, the bitumen gravity of 8°. The bitumen recovered by ultrasonic process has an
content of high grade Athabasca tar sands is relatively constant, at average API gravity of 15° [68]. With the addition of radical initiators
14.5% by weight. A number of technologies are available for the ex- such as H2O2 to the in situ surfactants, it can further shorten the mi-
traction of oil from tar sands. They all use hydro-mechanical (me- cellar inversion time into a matter of minutes to extract the bitumen
chanical mixing or hydro transport), thermal (mixing with hot water or from Athabasca oil sands [69].
steam), or/and chemical (addition of reagents) procedures. Hot water Abramov et al. [70–72] carried out series of extraction experiments
processes are currently used by Suncor and Syncrude in Alberta, Ca- using ultrasound on Athabasca oil sands using various alkaline reagents
nada, to recover the bitumen [58–61]. such as sodium silicate, NaOH and Na2CO3. They observed that bi-
Avvaru et al. [62,63] reported ultrasonic cavitation in solid slurries tumen extraction decreased with increasing alkaline reagent con-
produces micro jets, which lead to particle breakage. Ultrasound im- centration until a certain value beyond which bitumen extraction im-
proves the local transport in the pores of the suspended solids at solid- proved with increase of reagent concentration. At very low reagent
liquid interfaces. Hence ultrasound cavitation is a promising method for concentration (C < 0.01%), author has observed entrapment of sand
extraction of heterogeneous mixtures and therefore in combination along with bitumen and with increasing reagent concentration bitumen
with other methods (for e.g. chemical ones) can be an effective alter- extraction has decreased. At 1–1.2% reagent concentration the bitumen
native to conventional process of oil sand extraction. Sadeghi et al. [64] extraction was observed to be very low and thereafter it increased to
conducted a series of experiments on a wide variety of fuel sources such 95% extraction with increase in reagent concentration to 12%. Similar
as coal liquids, oil sand, oil shale, asphalt and heavy oils. These ex- improvement in the extraction yield were found with Venezuelan heavy
periments indicated that ultrasound cavitation could be a feasible up- oils as well [73]. Spent alkali solution shows initial extraction rate
grading technology. In all the above cases, upgrading (conversion) of much higher than fresh alkali solution, due to readily available sur-
asphaltenes to resins were observed, and the rate of conversion in- factant micelles for the extraction process. Recycling of spent alkali
creased with externally added surfactants. In presence of ultrasound, allows the ultrasonic oil sand extraction to be an environmentally be-
the components of bitumen in alkaline solution (e.g. sodium hydroxide) nign process. Okawa et al. [74], have carried out the effect of fre-
and the in situ formed surfactants facilitate the bitumen separation and quencies on ultrasonic oil sand extraction at 28 & 200 kHz. The bitumen
upgrading to useful components. The surfactants interact with resin
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B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
extraction rate at 200 kHz was slightly higher than compared to 28 kHz the pipeline due to high viscosity of the heavy oil makes it cost and
at 75 °C temperature. This could be due to increased cavitational events energy intensive to transport via pipeline [80]. Improved way of
at higher ultrasound frequency. In presence of small concentration of transporting the heavy crude and bitumen using pipelines can be
H2O2 recovery rate of bitumen has been observed to be maximum at achieved through pre-heating of the heavy crude alongside heating of
28 kHz ultrasound. Similarly, laboratory studies by Zhao et al. [75] on the pipeline, blending or dilution with light hydrocarbon fluids, as well
Mongolian oil sands showed improved oil extraction rate. as emulsification of heavy oil with water and reduction of viscosity of
The ultrasonic apparatus required for oil sand extraction were de- the oil by core-annular flow [81–84]. Another set of processes rely on
signed and installed at the Ultrasonic devices laboratory of Institute of the reduction of heavy crude oil viscosity by heating the crude oil by
general and inorganic chemistry, Russian academy of sciences. The partial upgrading were reported [85,86].
acoustic system was equipped with computer-aided ultrasonic gen- High energy ultrasound can induce cavitation effect in extra heavy
erators and 1–7 kW magneto-striction transformers for operation at oil. This can change large molecules in extra heavy oil into light hy-
frequencies of 25–40 kHz. The soil contaminated with a large amount of drocarbon molecules. The earliest work on viscosity reduction of heavy
fuel oil was purified at the pilot scale. The pilot trial results confirmed oils was reported by Sokolov et al. [87], who observed that viscosity is
the results obtained at the laboratory studies [70]. Petrosonic heavy oil reduced by 20–25% for 30–60 min of operation. Islam et al. [88] car-
processes [76] have shown the conversion of heavy sour oil (HSO) and ried out experiments to ascertain the relationship between asphaltene
bitumen (heavy oil and oil sands fields of Athabascan) having an API content (molecular weight) and bitumen viscosity. They showed that
gravity of 8–14° to a value added synthetic crude oil of 18–23° API high oil viscosity was due to the presence of more asphaltene heavy
gravity. The process consists of two stages: solvent de-asphalting fol- components. Using ultrasound cavitation they cracked the asphaltene
lowed by distillation. The innovation associated with the Petrosonic molecular chains, and consequently reduced the viscosity of oil.
upgrading process, lies in the rapid de-asphalting achieved by using Chakma and Berruti [89] reported 15% viscosity reduction of heavy
ultrasound cavitation in the patented Petrosonic reactor. The process asphaltene oil samples after irradiating with ultrasonic waves. In 1993,
anticipates that 15–20% of the asphalt byproduct, can be sold in the Xianghong and Yaping [90] showed that the viscosity of 20 ml extra
asphalt market. The Sonoprocess™ filters the DAO (de-asphalted oil) heavy oil is reduced by 24% after 2 min of ultrasonic treatment. Espe-
from the hydrocarbon asphaltene and reduces the de-asphalting time cially for extra heavy oil mixed with water, its viscosity can be greatly
from 6 to 10+ h to 2 min, i.e., 50 orders of conversion rate improve- reduced after ultrasonic treatment. In 2004, Bjorndalen and Islam [91]
ment. Given the significant difference in boiling points between the found that the relative viscosity of liquid paraffin is reduced by 10%
upgraded oil and the solvent for recovery, they are easily and eco- after 2 min of ultrasonic treatment. Xianyong and Ping [92] and Jihui
nomically separated with only a solvent residual of less than 4% re- et al. [93] studied the influence of ultrasound frequency, treatment
maining in the oil. Such a small solvent residual in the oil is well within time, temperature and sound intensity on the viscosity reduction of
the quality parameters for pipeline and refinery specifications. The Binnan oil well of Shengli oil field in China. Experimental results have
process requires much lower capital expenditures, operational costs and shown that the optimum values of ultrasonic frequency, treatment time,
it also lowers the transportation cost of the refined oil. temperature and sound intensity for reducing the viscosity of crude oil
is 18.5 kHz, 30 min, 40 °C and 52 W/cm2 respectively. Abramov et al.
5. Crude oil viscosity reduction using cavitation [94] have conducted field experiments to show that a viscosity reduc-
tion by 16% after 4 h of treatment was observed and this simulta-
Heavy crude oil and bitumen exploration is faced with technical neously increased the oil production rate by 26.5%. After its recovery
challenges at all stages from recovery/production from the reservoir to when the same oil is treated in a special type of ultrasonic hydro-
transportation and refining. Transporting heavy crude oil and bitumen dynamic treatment reactor, causes not only further reduction of visc-
via pipeline to storage or refinery for downstream processing is usually osity by 30% but also changes the fractional composition of the oil. Shi
challenging due to their high density and viscosity (1000 cP). Further, et al. [95] have reported a viscosity reduction of 57% on Liaohe heavy
asphaltene deposition, heavy metals, sulphur and brine or salt content oil using ultrasonic static mixer at 360 °C temperature, with 1.8 kW
in crude oil makes it difficult to transport [77–79]. Asphaltene are power and 30 min. operating conditions. They reported ultrasonic
heavy complex molecules which are soluble in aromatics and not so- treatment requires 43% less energy compared to conventional vis-
luble in paraffin. They are the heaviest and the most polar fraction of breaking technology. Viscosity reduction of various petroleum crude
crude oil. Canada and Venezuela are the countries presently exploiting oils under ultrasonic cavitation treatment is shown in the Table 3.
heavy crude oil reserves and pipelines are used to transport 95% of the Right now, ultrasonic viscosity reduction techniques in many
heavy oil produced by them. The asphaltene portion of the heavy oils is countries emphasize field tests, with the research on theoretical models
known to be insoluble in straight chain hydrocarbons such as pentane still in its infancy, the basic theory for ultrasonic viscosity reduction
and heptane. Therefore, problems due to asphaltene precipitation due technique has still not been established. In petroleum chemistry it is
to depressurisation (below asphaltene precipitation onset pressure) may predominantly accepted that asphaltenes are suspended in micelle form
occur when transporting the heavy crude oil. High pressure drop along in petroleum and are stabilized by adsorbed resins in solutions [99].
Table 3
Viscosity reduction of petroleum oils under ultrasound cavitation conditions.
Crude oil details Time (min) % Reduction Reason for viscosity reduction Reference
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B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
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B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
Table 4
Dehydration/desalting efficiency of water in oil emulsions under ultrasonic conditions.
Emulsion system Ultrasonic irradiation time (min.) T (°C) Efficiency (%) Reference
Dehydration Desalting
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B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
Table 5 (model compound used quinoline) on UAOD process has impaired the
Companies engaged in ODS process technology during 20 years [145]. sulphur removal efficiency, however same oxidative conditions can be
used simultaneously for denitrogenation (UAODN) [156]. The opti-
Company Country Oxidant Patents
mised conditions from the batch UAOD and UAODN processes were
BP, corp., AMOCO USA H2O2 2 used to design the continuous flow reactors for energy efficient UAOD/
Exxon corp. USA H2O2 1 UAODN process [157–159].
DS2Tech ., Inc. USA H2O2 1
Carnegie-Mellon Univ. USA H2O2 2
Gul Oil corp., R&D USA HNO3 1 7.1. History of UAOD
Lyondell Chem. Comp. USA TBHP 2
Oxochem techn. Inc. USA H2O2 3 Oxidative desulphurisation process using ultrasound has been under
Petrobras Brazil H2O2 2 development since 1990. Desulfurization was carried out in basic or
PetroStar Inc. USA H2O2 3
acidic conditions by applying ultrasound frequency of 20 kHz to crude
UOP USA HCHP 4
Stanciulescu USA H2O2 1 oil. Use of transition metals, nickel and vanadium, as catalysts along
SulphCo. USA H2O2 3 with hydrogen peroxide as a chemical oxidant, assisted with ultrasound
TotalFinaElf. Corp. France H2O2 2 was developed by authors [160,161]. In the UAOD process, the Ven-
UniPureenergy Corp. USA H2O2 4
turella type of transition metal catalysts (TMC), or polyoxometalates
with Keggin structure such as phosphotungstic acid, and a quaternary
ammonium salt, tetraoctylammonium bromide, as phase transfer cata-
lyst (PTC) were introduced so as to produce highly effective and se-
lective oxidation with hydrogen peroxide to improve desulfurization
[148]. Higher than 98% desulfurization efficiency has been achieved
for diesel fuels in 10 min of ultrasonic cavitation with 30% wt hydrogen
peroxide as oxidant. However, this process has a low conversion of
benzothiophene (BT) and its derivatives and forms the brominated by-
products. Changing to phase transfer catalyst (second generation
UAOD) such as quaternary ammonium salt with fluoride instead of
bromide as anion in the catalyst eliminated the formation of by-pro-
duct, and also increased the overall desulfurization efficiency to 95%
[162]. Based on the second generation UAOD, a customized continuous
Fig. 5. Oxidation process route of various sulphur compounds. desulfurization system of 24 kg of diesel per day gave 92% desulphur-
isation efficiency [163]. To reduce hydrocarbon loss, alumina adsorp-
hence easily extractable using a suitable polar solvent. Thus basically tion was used to remove sulfones instead of liquid-liquid extraction
ODS is a two-step process, oxidation followed by either solvent ex- [164].
traction or solid adsorption. Many companies are actively engaged in The recent development of the third generation of UAOD using
ODS process development because of its attractive cost benefits as an room temperature ionic liquids (RTIL) as phase transfer catalyst and
alternative to conventional HDS process. During the past 20 years alone extracting solvent, has achieved greater than 99.9% desulfurization in
more than 30 process patents have been issued to the companies various diesel samples with 10 min of ultrasonic cavitation [165]. Ultra
working in the ODS technology as shown in Table 5 [145]. The oxi- low sulphur diesel (ULSD) with sulphur content less than 15 ppm can be
dation process route of the sulphide/thiophene/benzothiophene/di- produced from various diesels by this third generation UAOD process.
benzo thiophene to higher polarity (sulphone and sulphoxide) is shown Ionic liquids with alkylsulfate as anion that are relatively more stable,
in Fig. 5 [146]. With the advent of ultrasound cavitation technology the and produce non-corrosive byproducts upon degradation were used for
critical drawback associated with the slow/sluggish heterogeneous re- UAOD [166,167]. As shown in Table 6, the efficiency of sulphur re-
action between the oil phase and aqueous phase oxidant can be elimi- moval can be significantly improved by using ultrasound compared
nated, and the reaction can be carried out faster and at relatively low with stirring under identical oxidative system.
temperature and pressure. Ultrasound assisted oxidative desulphurisa-
tion (UAOD) has potential to replace the HDS to process the heavy and 7.2. Reaction conditions for UAOD
extra heavy crude oils in near future [147–150]. The extreme condi-
tions of temperature and pressure during acoustic cavitation causes the In presence of ultrasound various oxidants such as concentrated
formation of free radicals such as H% and OH% (among these OH% radi- nitric acid, peroxyacids, ozone, hydrogen peroxide, oxygen, organic
cals are strong oxidising agents) [151]. It is also reported that atomic hydro peroxides and permanganate have been used for ODS processes
oxygen can be generated from dissolved oxygen in aqueous solution [175–180]. Among them, the oxidant H2O2 is considered most pro-
upon ultrasound irradiation [152]. These radicals and atomic oxygen mising in terms of selectivity, availability, safety, cost effectiveness and
would further react with dissolved oxygen, water molecules, or other environmental friendliness [181]. Fenton's reagent is also a strong
radicals to form hydrogen peroxide and oxygen eventually. Moreover, oxidising agent, improves the hydrotreated diesel desulfurization rate
the volatile and semi-volatile thioethers and thiophenes can also di- probably by increasing the concentration of available %OH (free radi-
rectly be decomposed by sonication in aqueous solutions [153]. Bolla cals) [147]. Similar to hydrogen peroxide, superoxide anion is also
et al. [154] carried out experiments for studying the mechanism of considered as a reactive oxygen species. Callahan et al. [182] have
UAOD. Ultrasound cavitation works by creating the micro turbulence found hydrogen peroxide, the superoxide anion radical, and the hy-
which enhances the oxidation reaction between hydrocarbons such as droxyl radical are the most important reactive oxygen species. How-
thiophenes and its derivatives with the aqueous H2O2. While the exact ever, oxidising agent (H2O2) alone is not sufficient in giving the good
reaction mechanism is still under debate, the overall oxidation reaction reaction rate and requires a catalyst to work in mild temperature,
rate can be improved by ultrasound cavitation to several folds. Few pressure conditions ranging from 25 °C to less than 100 °C under am-
studies [155] mapped the acoustic field intensity with desulfurization bient pressure. Various types of ODS catalysts found include carboxylic
efficiency, suggesting that high intensity acoustic regions were giving acids, poly-oxometalate acids, aldehydes and transition metal salts
high desulfurization efficiency. The presence of nitrogen compound [183–187]. Basically, poly-oxometalate anions are capable of reversible
redox reactions to actively transfer oxygen to the targeted compounds
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B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
Table 6
Effectiveness of ultrasound cavitation over normal stirring conditions for ODS.
US Stirring
for selective oxidation [188,189]. an equivalent hydrotreater would cost. The application of SulphCo’s
It has been demonstrated that ionic liquids, especially room tem- technology for crude oil upgrading has also been studied, API gravity
perature ionic liquids (RTILs) could be used for desulfurization. increase up to 3 points and viscosity reduction up to 15% has been
Extractive desulfurization using ionic liquids are of particular interest reported [196–198].
wherein specific ionic liquids could form relatively strong π complex A short coming of ultrasound (acoustic) cavitation is that it occurs
with organic sulphur compounds (OSC) such as thiophene as compared only in the close vicinity of the surface of the ultrasonic probe and this
to benzene and paraffin [190]. Another use of RTILs is a combination of severely limits the active volume of the reactor and leads to poor per-
oxidative and extractive desulfurization process. With water miscible formance in industrial scale operations. Hydrodynamic cavitation is an
RTILs, OSCs can be extracted from fuel and become oxidized by oxidant alternative to ultrasound (acoustic) cavitation. The technique in prin-
such as hydrogen peroxide to the corresponding sulfones in RTIL phase ciple can be used to process a large volume of materials for industrial
[191]. In modified UAOD process, ionic liquid imidazolium alkylsulfate scale applications [199]. Hydrodynamic cavitation reactors powered by
is utilised as multi-phase transfer catalyst to transfer active oxygen 5–200 kW electric motors these devices can generate sound energy in-
species from aqueous phase to organic phase. The same ionic liquid tensity in excess of 1 MW/m2. Sparse patent literature is available for
could also extract OSCs or oxidized OSCs from the fuel. In combination desulphurisation of transportation fuels by hydrodynamic cavitational
with RTILs, UAOD process can achieve more than 99% desulfurization reactors [200–202]. In order to commercialise the oxidative desul-
with various types of diesel fuel oils [165,192–194]. phurisation for ultralow sulphur diesel (ULSD), hydrodynamic cavita-
A right combination of the oxidant, catalyst and phase transfer tion along with some synergistic process aids like using ionic liquids can
catalyst needs to be found out for each petroleum feedstock of its help.
characteristic sulphur compounds or oil stream to make the UAOD
successful at the commercial scale. Also the advent of magneto-striction 8. De-Metallization using ultrasound cavitation
based transducers that can work for 24 h without much intermittent
stoppages, the UAOD technology is now ready to serve the industrial The amount of metals in petroleum crude oil varies from a few ppm
needs. to more than 1000 ppm. The metals typically found are sodium, po-
tassium, lithium, calcium, strontium, copper, silver, vanadium, man-
7.3. SulphCo process ganese, tin, lead, cobalt, titanium, gold, chromium and nickel. The
metals are usually present as soaps (in combination with naphthenic
The first commercial ultrasonic desulfurization unit has been in- acids) or complex organometallic compounds such as ‘metallopor-
stalled at the IPLOM petroleum refinery near Genoa in Italy with con- phyrins’ or ‘petroporphyrins’ [203–205]. Among these metals the most
tinuous desulfurization of diesel fuel up to 350 bbl per day [195]. The abundant and undesirable are vanadium and nickel. These metals are
proposed technology meets the 10 ppm of sulphur requirement in hy- thought to occur in petroleum in two forms; ‘metalloporphyrinic’ and
drocarbon streams. In accordance with the preliminary estimation of ‘metalnonporphyrinic’. Metalloporphyrins are typical metal complexes
Betchel Corp. Scientists, the SulphCo unit will cost about 50% of what of porphyrin ligands shown in the Fig. 6. Metalloporphyrins (Ni and V)
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B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
are concentrated in the high molecular weight fraction of the asphal- feedstock [218]. The author studied the effect of ultrasonic vibrations
tenes. Ni and V increase with the asphaltic content of the crude oil. on cracking of heavy petroleum residues at high pressure. The thermal
Removal of Ni and V from metalloporphyrins requires a very strong cracking was conducted on a continuous laboratory setup at a tem-
acid, such as methanesulfonic acid or tri-fluoroacetic acid, but also perature of 430–470 °C and pressures 20–40 MPa [218]. Ultrasonic
produces a free base porphyrin where two hydrogen ions displace one energy is used in association with various agents, such as diluents and
central metal atom. Although a variety of physical and chemical other emulsifying agents to facilitate the scission of carbon-carbon
methods were investigated with the intention to remove metals [205], bonds in various petroleum mixtures by controlling the cavitation
yet no industrially viable pre-treatment process of demetallization is phenomena. The reactions pertaining to the cracking of heavy oils in
available. Currently in catalytic hydroprocessing, hydrogenation is used presence of ultrasound cavitation can be elucidated by Rice mechanism
to remove the metals from liquid petroleum fractions. One of the most [219]. The cracking of asphaltenes into gas oil and resins can be clas-
practical and effective methods of feedstock demetallization is the use sified as free radical reactions. The bond cleavages of the asphaltenes
of hydro demetallisation (HDM) catalysts, which requires expensive (RR’) under ultrasound result into R and R’, both hydrogen and hy-
capital investment and hydrogen gas as operating cost [206]. droxyl radicals are generated during the homolytic dissociation of
There is literature on effective decomposition of metalloporphyrins water molecules under ultrasound cavitation conditions producing the
using radical induced decomposition produced by ultrasound cavita- high temperature and pressure. Thus, the hydrogen radicals may either
tion. The use of additives such as hydrogen peroxide (initiator of hy- come from dissociation of water or desorption of dissolved hydrogen
droxyl free radicals) and surfactant can enhance the efficiency in which molecules from crude oil by ultrasonic irradiation. Chain propagation
the surfactants act as phase transfer agents between the oxidants in (addition) reaction (i.e. polymerization and/or polycondensation) may
aqueous phase and the metalloporphyrins in organic phase. A pre- occur, the addition reaction can form compounds with higher mole-
liminary mechanism and kinetics for the decomposition of model me- cular weight (preasphaltene).
talloporphyrins is available [207]. It has been mentioned that me- Asphaltene aggregates carry negative charge, since the thickness of
talloporphyrin undergoes oxidation with hydroxyl radicals forming π- the double layer around the particles will affect the repulsive force
cation radical of porphyrin before decomposing to model paraffinics, among particles, the addition of anionic surfactant will improve the
naphthenics, aromatics and metal ions [207–209]. Literature published quality of asphaltenes suspension more than non-ionic or cationic sur-
elsewhere [210] reported the effect of ultrasound assisted demetalli- factant [160]. However they have found with limited set of surfactant
zation and the amount of demetallation agent, reaction time on de- system, under ultrasound cavitation conditions the non-ionic surfactant
metallization of gasoline stream coming from coker unit that processes works better than the anionic and followed by cationic surfactant in
the oil from Liaohe oil field. The ultrasound cavitation results show that presence of reducing agent (hydrogen) environment. It is proposed that
high metal removal efficiency was obtained in a short time. The opti- both gas-oil and resin fraction can be derived by cracking the asphal-
mised parameters are demetallation agent mass fraction of 1500 μg/g, tenes. Likewise, the resin can be converted to gas-oils. The type of
ultrasound irradiation time of 15 min and ultrasound intensity of 8 W/ surfactant used affects the selectivity of these two reactions. The hy-
cm2. The removal rate of Zn is 90% and above 80% for Ca and Ni. These droxyl functional group is a polar group and the termination of free-
studies were conducted on model metalloporphyrins (VoTPP and radical reactions by hydroxyl groups will increase the polarity of the
NiTPP) compounds in various chlorinated solvents. No studies have final compound, but with hydrogen radicals it will not. The polarity of
been reported with real asphaltene hydrocarbons. The complex nature compound (either gas oil or resins) will enhance the aggregation in the
of crude oil may decrease the decomposition rate of metalloporphyrins, asphalt system. Thus, the H% (free radical) terminator is superior to the
but decomposition mechanism remains same under the cavitation OH% (free radical) terminator for disintegration of asphaltenes. Another
conditions. study by the Dunn and Yen [220], has indicated that the asphaltenes
A review paper on this subject [204,205,211] revealed various under ultrasound cavitation undergoes simultaneously both dehy-
academic labs, oil companies and individual researchers are exploring drogenation and cracking reactions. In their study, conversion by ul-
non-conventional options for metal removal from crude and residual trasound without hydrogen sources is mostly dehydrogenation i.e., 82%
oils. These methods include chemical treatment with acids and alkali, of dehydrogenation and 18% of cracking. In presence of hydrogen
selective oxidation/solvent extraction, the photo catalytic methods, source, this condition is almost equally for both dehydrogenation and
electrochemical treatment, novel thermal and catalytic methods. In cracking i.e., 57% for dehydrogenation and 43% for cracking reaction.
general, these efforts are at the laboratory to small pilot plant stage and In a complete summary of previous literature results, Sawarker et al.
no information is available at commercial stage. However, even if the [221] mentioned the effect of ultrasound cavitation for the upgrading of
ultrasonic treatment benefits heavy oil upgrading or desulphurisation vacuum residue is high when the vacuum residue is emulsified in water
processes, the in situ demetallation can be expected to improve. with surfactants. A kinetic model has been developed based on the
constituents of the vacuum residue to get an insight into the reaction
9. Upgrading of heavy crude oils using cavitation mechanism. Gopinath et al. [222] treated the heavy gas oil using ul-
trasound energy without the use of any additives at atmospheric pres-
Number of technologies have been developed over the years for sure. They obtained lighter gas hydrocarbons such as methane, ethane,
heavy crude and residue oil upgrading, which provide an opportunity ethylene and propylene. Wang et al. [223] have studied the effect of
for those refineries which can process low grade crude oils. These ultrasound treatment on the properties of petroleum coke oil slurry.
technologies include processes that are based on carbon rejection, hy- They found that the apparent viscosity decreased with the duration of
drogen addition and combination of both, most of them with some ultrasound treatment increased. Kaushik et al. [224] studied the up-
commercial success [212–217]. Another new group of technologies also grading of vacuum residue including the effect of surfactant, irradiation
are emerging as a promising solution of the problem. These technolo- time and probe diameters of the ultrasound horn reactor. With and
gies are focused on the upgrading the properties of the heavy crudes, without surfactant, they found reduction by 48% and 40% of asphal-
i.e. improvement in API gravity/reduction of viscosity and impurities tene content respectively leading to lower viscosity and converting the
content such as sulphur, nitrogen and metals to feed the refineries. residue into more useful products. Asphaltene content reduced sharply
Ultrasound cavitation technology is among one such technologies has within 30 min of irradiation time and beyond that time it reduced very
been showing improved applications in the crude oil upgrading. slowly. Several researchers [225–227] have proposed use of hydrogen
The paper presented in 1960 at the All Union Scientific and donors like cyclohexane, methylcyclohexane, tetralin etc. for upgrading
Technical conference, was probably a pioneering one concerning the heavy oils and natural bitumens during pyrolysis. The hydrogen donor
possibility of using cavitation for enhancing the cracking of petroleum forms hydrogen free radicals that react with radicals in the crude
502
B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
leading to viscosity reduction in the products by blocking polymeriza- have been particularly used for enhanced oil recovery technique. All
tion reactions. Yang et al. [228] have proposed combination of ultra- these improved designs can work up to temperature and pressure more
sonic cavitation and introduction of hydrogen donor into the reaction than 1200 °C, 9 MPa respectively. For batch mode operation, these high
mixture as a promising technology for refining heavy oil residues. power transducers can be directly immersed into the reactor for desired
Combined treatment with a hydrogen donor i.e., tetralin and ultrasound physico-chemical transformation. However industrial processes are
cavitation results in synergistic effects for the reduction of viscosity, continuous type, these batch mode operations can be converted into
density, and pour point of Beijing Yanshan refinery vacuum residue. continuous mode with the help of flow cell arrangements. In this design
Quite a few companies are offering this technology for the pilot and an external pump is used for pumping the reaction mass to ultrasonic
commercial scale production. NexGen technology [229] sends the chamber, depending on the reaction rate residence time can be fixed by
heavy crude oil through a membrane separation process where the varying the flow rate of the pump.
asphaltenes are separated from the lighter crude oil. Once the asphal- Researchers [240–243] working on hydrodynamic cavitation tech-
tenes and heavy oil have been partially cracked by the process, they are nology, developed the most economical way of producing the cavitation
sent to the next cracking process which has great control on the type of by hydrodynamic means. Researchers [244–246] have proved the hy-
hydrocarbon formed. The key points of this process is that it converts drodynamic cavitation is more energy efficient in the generation of
low cost heavy oil into valuable light oil, the process operates at a low cavities whereas cavity collapse in ultrasound cavitation was much
temperature and pressure, without any catalyst and the foot print is more violent. The combination of the above two techniques yields sy-
small as compared to any other current method of refining or heavy oil nergistic cavitation effects, the operating parameters for the optimised
upgrading today. The technology can process feedstock such as bot- design have been proposed.
toms, heavy oil and extra-heavy oil (bitumen). It considerably improves Another successful design of hydrodynamic cavitation reactor is
oil quality before the oil refining takes place; significantly improves shockwave power reactorTM (SPR) system that was constructed by
yields and reduces coking reactions. Hydrodynamics Inc., [247]. The unit consists of concentric cylinders
SulphCo was founded in 1999, has developed an economic process with an annular space separating the stationary outer cylinder from the
employing ultra-sound technology for desulfurization, hydrogenation of inner, rotating cylinder. The rotating cylinder is driven by a motor and
crude oil and other oil related products. The technology upgrades sour generates cavitation in the fluid in the annular space when fluid enters
heavy crude oils into sweeter, lighter crudes, producing more gallons of and exit cavities on the surface of the spinning cylinder. The inner,
oil per barrel. SulphCo has conducted four separate series of sono- rotating cylinder houses multiple cavities where fluid is pressurized and
cracking trials since 2002, and has five U.S. patents issued for their high depressurized many times, causing hydrodynamic cavitation to occur.
powered ultrasound technology [196–198,230–232]. SulphCo’s Sono- As cavitation occurs, the fluid bulk receives energy dissipated by the
cracking technology has lower cost and low environmental impact than bubbles in the vapor phase as the bubble collapses. This type of cavi-
conventional HDS (Hydro-Desulphurization) units, which allows the tation is deemed to be ‘vortex’ cavitation and occurs in the cavities of
refinery to optimize its crude and feedstock mix for greatest economic the inner rotor. This novel design allows for a continuous flow of fluid
gain. The hydrogen addition technologies have higher investment and to replenish multiple cavities as the rotor spins, facilitating cavitation
operating costs. Ultrasound cavitation technologies have definitively and product flow through the system. Pressurizing the system during
attracted the attention of the refiners. Feasibility studies are being operation ensures continuous product contact with the inner rotor re-
carried out by many petroleum companies to make proper decision to sulting in the fluid undergoing controlled cavitation. As product enters
adopt these technologies. the SPR annular space with the rotor set at a specified operational
speed, the mass flow rate of product dictates the frequency of cavitation
10. Industrial scale cavitation reactors events and ultimately the exit temperature.
In 2001, the US department of energy successfully developed a vi- 11. Concluding remarks
brational transducer particularly for enhanced oil production, but it has
lower ultrasonic frequency and lower energy density [233]. In 2007, Since the first application of cavitation technology for petroleum
Germany’s Hielscher company successfully operated high power cy- crude oil recovery (1930), the subject of ultrasonic application to pet-
lindrical transducer [234], the most notable feature is that it can work roleum refinery processes has moved a long way from academic re-
continuously under humid and high pressure conditions. Various de- search to industrial applications. For EOR, the technology has got more
signs with different rated power capacities are available for various attention due to its simplicity, lower expenses, good applicability and
physico-chemical operations, but they cannot work at high tempera- no reservoir pollution. The technology has shown improvement in all of
tures. Edward H. Phillips proposed in their patent that piezoelectric the sites operated at Western Siberia, Samara regions and as well as in
elastomer can be used to generate high power ultrasound for enhanced China. With continuous improvement, it is likely to have more success
oil production [235]. In 2006, China has developed first generation in all of the wells it is applied.
high power transducer based on piezoelectric ceramic material. This The promise shown by oil shale extraction processes at the labora-
design further modified in 2013 and named it as second generation high tory scale is not replicated at industrial scale. The economic viability of
power transducer [236]. The successful development of the second these processes at industrial scale needs to be established. The advent of
generation transducer has greater strategic significance and this light recent high power transducers such as Lithium niobate piezo-electric
weight transducer was successfully tested in Daqing oil field, Changqing transducers may improve the economic feasibility at industrial scale
oil field, Shengli oil field and Liaohe oil fields for enhanced oil recovery. operations.
Recently, the research teams working on improving the ultrasonic oil As per literature, ultrasonic demulsification and dehydration were
production technique have developed a new high power ultrasonic mainly reported in China compared to other parts of world. The de-
transducer, the piezoelectric vibrator made of a new piezoelectric ma- mulsification of water-in-oil type emulsified crudes, the combined ul-
terial lithium-niobate crystal [237–239]. One transducer has many li- trasonic and chemical demulsification methods show better perfor-
thium niobate piezoelectric vibrators, and are all having same emission mance when they are applied together compared to each alone.
frequency and vibration phase, ultrasound field emitted by these li- However comparison should be made with the present conventional
thium niobate piezoelectric vibrators are coherent wave fields. Lithium technology of high voltage electric desalting techniques generally
niobate has good mechanical performance and chemical stability, its practised at the refinery site, if not at industrial scale level but at least at
mechanical quality factor (about 105 magnitude) is much higher than the pilot scale operations. A complete report of the same in terms of
common piezo electric transducer. These lithium niobate transducers economic feasibility and ease of operation, definitely enable the refiners
503
B. Avvaru et al. Ultrasonics - Sonochemistry 42 (2018) 493–507
to choose this technology at commercial scale. Presented at the XIII Session of the Russian Acoustical Society, Moscow, 2003.
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