SPE 130333

In Situ Upgrading Extra-heavy Oil by Catalytic Aquathermolysis Treatment

Using a New Catalyst based Anamphiphilic Molybdenum Chelate
Chuan Wu, Guanglun Lei, Chuanjin Yao, and Xiaofei Jia, China University of Petroleum

Copyright 2010, Society of Petroleum Engineers

This paper was prepared for presentation at the CPS/SPE International Oil & Gas Conference and Exhibition in China held in Beijing, China, 810 June 2010.

This paper was selected for presentation by a CPS/SPE program committee following review of information contained in an abstract submitted by the author(s). Contents of the paper have not been
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Abstract
The aquathermolysis of Shengli extra-heavy oil during steam stimulation was studied by using anamphiphilic
molybdenum chelate-aromatic sulfonic iron as catalyst for the reaction in this papers. The laboratory experiment shows
that the viscosity reduction ratio of heavy oil is over 97.15% at 200, 24 hr, 0.2 % catalyst solution. The viscosity
of upgraded heavy oil is changed from 524.5Pas to 14.95mPas at 50. The chemical and physical properties of heavy
oil both before and after reaction were studied by using Fourier transform infrared (FT-IR) spectroscopy, gas
chromatography/mass spectrometry (GC-MS), elemental analysis (EL). The percentage of saturatearomatic and H/C
increased, and resinasphalt and SON decreased after the aquathermolysis. The changes of the composition and
structure of the heavy oil can lead to the viscosity reduction and improve the quality of heavy oil. It has shown that the
mechanism of aquahtermolysis is discussed further. We found the new mechanism of catalyst not only broken C-S bond,
but also broken C-O and C-N bonds, and accelerated the reaction of aquathermolysis. The results are very useful for the
popularization and application of the new technology for the insitu upgrading of heavy oil by aquathermolysis.

Introducation
With the depletion of conventional crude oil reserves in the world, heavy oil and bitumen resources have great
potential to meet the future demand for petroleum products. Heavy oil reservoirs accounts for 15% of the total oil
reservoirs in China[1]. There are many heavy crude oil reserves in China, and it is very important to the pertroleum
industry how to effectively exploit and use the discovered heavy oils. However, it is difficult to recover heavy oil
because of its high viscosity and poor flowing ability.
Nowadays, steam stimulation is the most effective way to produce heavy oil in the world. Different versions of
thermal methods are used to upgrade heavy crude oil, among the more important methods are Steam Drive, Cycle Steam
Injection, Steam Assisted Gravity Drainage(SAGD), Conventional Fire Flood, Toe-to-Heel Air Injection Process(THAI),
Down-Hole Catalytic Processes, and Aquathermolysis[2].
The Aquathermolysis mentioned is an interesting alternative to reduce of viscosity of the heavy crude oil improving
the oil quality inside the reservoir. However, aquathermolytic technology introduced in this paper could upgrade the
2 SPE 130333

extra-heavy oil (viscosity is 524.5Pas at 50) in situ by adding catalyst under aqueous and thermal conditions. As a
result, the amount of saturate and aromatic are increased, resin and asphaltene are decreased, viscosity reduced. The
percentage of resinasphalt and SON decreased, and H/C increased after the up grading process.
Hyne et al. in 1982 researched the details of the chemical reaction between steam, heavy oil and minerals, and
described all of these reactions as aquathermolysis [3]. They found that the injection steam can not only reduced the
viscosity of heavy oil but also reacted with some components of the heavy oil and of the reservoir minerals, and the
properties and compositions of the heavy oil were changed[46]. Subsequently, scientists studied the aquathermolysis
further, they added various catalysts to catalyze the aquathermolysis[724]. Upon catalytic aquathermolysis, more heavy
components of the heavy oil pyrolyzed and the structure changed to a larger degree, especially some heteroatom
containing structure, and these changes could hardly regress and eventually lead to the reduction of the viscosity of
heavy oil, thereby benefiting the oil exploitation, transportation and upgrading. All the reactions between heavy oil,
steam and catalysts were described as catalytic aquathermolysis[19].
The key factor of the catalytic aquathermolysis is the choise of the appropriate catalyst. Firstly, Hyne et al. studied
the metal ions of Ni2+Fe2+Cu2+Zn2+ and so on as catalyst, then pointed out that the percentage of saturatearomatic
increased and resinasphalt and S decreased after the catalytic aquathermolysis[7]. Rivas et al. studied the nickel salt
as additive under aqueous and thermal conditions, and found that viscosity of heavy oil decreased and the quantity of
H2 CO2 and C2+ increased after the reaction[8]. Clark et al. used Fe ( II) as additive, and found it accelerated the
cleavage of the C-S bonds[9]. The patents introduced the metal ion salts as catalysts under steam injection
conditions[10-12]. LiuFanChen et al. studied the transition metal ion salts, transition metal compounds and organo
metallic compounds as the catalysts, and conducted the field experiments in Liaohe oilfield and Henan oilfield of
China[13-20]. Some researchers used solid superacids as the catalysts in heavy oil, including Strausz[21], Babcock[22],
Wen[23], Jing et al.[24], they did a large amount of experiments in the laboratory, but not reported the applied in the
oilfield. Meanwhile, some scientists studied the mechanism of catalytic aquathermolysis. Firstly, Clark, Hyne et al.
studied on the mechanism of catalytic aquathermolysis, which chose thiophene and tetrahydrothiophene as model
compounds. They pointed out that the critical factor in aquathermolysis is S-containing compounds, and the cleavage of
the C-S bonds were the key reaction. Some metal ions accelerated the cleavage of the C-S bonds and the others
reaction[25-29]. Subsequently, Clough[10]Rivas[8]Clark [9] Pelrine[30]Richard[31]Strausz[32-34]Liu
Fan et al [13,35-37]. studied the mechanism of catalytic aquathermolysis, and all these supported the mechanism that
catalysts mainly catalyzed the cleavage of the CS bonds as the main reason why the viscosity of heavy oil was at last
reduced. But in our later research, it was found that besides the cleavage of a few CS bonds, the catalyst mainly caused
changes in oxygen-containing groups such as the cleavage of CO bonds in phenolic, ethereal molecules, etc. from the
heavy oil.
Overall, there exist three gaps about the catalytic aquathermolysis between the laboratory and the field. Firstly, the
catalysts usually applied in aquathermalysis are not oilsoluable. It is mean that the catalysts and the heavy oil cannot
fully mix up, so the catalytic effect is relatively low. Secondly, the temperature on the oil floor after steam injection
gradually lowered with the increasing depth of the oil floor and is difficult to keep above 240; so, there is not enough
energy supplied for catalysis. Thirdly, the catalysts are effectively functions to moderate heavy oil, but not get a good
viscosity reduction efficiency to the extra-heavy oil which viscosity exceeds 300Pa.s at 50. Hence, synthesizing a
catalyst which can sufficiently contact the heavy oil and maximize its catalysis at 200 would be a great advance for
catalytic aquathermolysis even for the exploitation of extra-heavy oil.
SPE 130333 3

Laboratory Experiment
Preparation of catalyst. Molybdenum salt dissolves in distilled water firstly, and put into a bottle with three necks.
Then put quantitative sodium hydroxide and sulfonic acid solution into the solution and keep the mixture boiling for 4
hours at 8590. Finally, separating the mixture and get the molybdenum after the mixture is cooled.
Properties of heavy oil samples. The extra-heavy oil samples used in this study were taken from in Shengli oil
field. The properties and composition of the samples are given in table 1.
Experiment process.
In the aquathermolytic process, 100g heavy oil sample, 0.35g catalyst and 50g water were put into
autoclave(internal volume 500mL),and then the system was heated to 200 kept for 24h. At the end of heating period,
the autoclave was cooled slowly to room temperature. Then the viscosity, element analysis and the compositions of the
oil samples were analyzed according to the following processes.
Viscosity determinations
Oil viscosities were determined using a programmable viscometer (Briekfield DV-, made in American). For the
measurement, a sensor system and about 11g of oil were used. Approximately, 1112 g of the oil was placed in the
sample cup and allowed to equilibrate to 50 over 20 min. The torque be about 50% before and after the reaction.The
rate of viscosity reduction was calculated by the method =0-/0100where the (%) was the
rate of viscosity reduction, 0 (mPas), the viscosity of oil before the reaction,and(mPa. s), the viscosity of oil after
the reaction.
Element analysis.
The elements in heavy oil were determined by model element analysis instrument(Elementar Vario EL , made in
Germany), 1g sample was used for auto sampling. Firstly, heavy oil sample was broken into CO2, H2O, NO and CO in
the furnace at high temperature, and the gases injected into injection valve are brought into the column by nitrogen, all
ingredients are separated in the column and entered into the tester by order, chromatographic signals of which will be
recorded by recorder, integrator or data processing system. Then calculate the content of the elements.
SARA composition analysis
The compositions of oil samples were determined by column chromatography (CC) analysis of the deasphaltened
separated oil. The asphaltenes were removed by precipitation with addition of 40-volume excess of heptane to the
solution of the oil sample (about 12 g), boiling 1 hour and and standing for 12 hours, filter and concentrate the filtrate.
The filtrate can then be used directly for column chromatography (CC) analysis, which packed by alumina and silica gel.
The saturate fractions were obtained by elution with petroleum aether, and after collection of the aromatic fractions
which eluated by toluene. Finally, the resins were obtained by back-flushing the column with with toluene / alcohol
(1:1,V/V). The fractions were quantified gravimetrically after removal of solvent. A mass balance in the range 99101%
was considered acceptable.
Gas collection and analysis
The compositions of the gas after the reaction by GC-MS(Varian Saturn 2000, made in American). The test samples
injected into injection valve are brought into the column by mobile phase; all ingredients are separated in the column and
entered into the tester by order, chromatographic signals of which will be recorded by recorder, integrator or data
processing system.

Results and discussion

Composition changes of the oil samples after rection
Table 2, which presents the composition changes of the oil samples after catalytic aquathermolysis treatment, shows
that the saturated and aromatic hydrocarbons increased, while the resin and asphaltene decreased. The saturated
4 SPE 130333

hydrocarbons increased from 26.87 to 31.12. Compared with samples before reaction, resin decressed by 5.19%, and
asphaltene reduced to 13.91 %. The results indicate that the heavy components were converted into light components
result of catalytic aquathermolysis reaction, it was an important factor for the viscosity reduction of the heavy oils.
Structure change of the oil samples
The infrared spectrum of the asphaltene and resin before reaction are shown in Figure 1 and Figure 3. It show that
there were absorption peaks at 10601123 cm-1, which indicates the resin sample contains C=O and SO, One
absorption peak at 3207 cm-1, which indicates the resin samples contained alcohol group. The adsorption peak at 1040
cm-1, which indicates asphaltene samples contained aromatic sulfur compound , another adsorption peaks at 650900
cm-1, which indicates the length of side alkyl chain in the oil larger than 4.
Figure 2 and Figure 4 are the infrared spectrum of the asphaltene and resin after reaction, it show that there were no
absorption peaks at 10601123 cm-1, which indicate there existed hydrodesulfurization during reaction. The absorption
peak at 3207cm-1 obviously become weak, which indicates there existed alcohol group reaction in the effect of high
temperature water and catalyst. The absorption peak at 1040cm-1 was disappeared, which indicates there existed
hydrocracking reaction, and aromatic sulfur compounds were converted into mercaptans and decomposition. The peaks
at 650900cm-1 obviously become weak, it mean that long and linear alkyl chains broke off.
Elemental analysis
The elemental composition of the samples were determined by a Elementar Vario EL model elemental analysis
instrument. Through the analysis, 1g sample sizes were used for auto sampling. The results are given in Table 3, we can
see that the amount of the hetero-atom, such as S, O and N are decreased after treatment. The hetero-atoms, mainly
located at condensed aromatic structure of heavy oils, were removed during catalytic aquathermolysis process and thus
reduced the total ring number, the intermolecular forces reduction can result in decreasing viscosity of heavy oil. At the
same time, the ratio of hydrogen increased and carbon decreased, H/C increased, and the quality of the heavy oil
inproved after the upgrading process. All of these results proved that the composition of the heavy oil samples were
changed under the catalytic aquathermolysis treatment.
The viscosity of samples before and after reaction
The viscosity of the heavy oils was determined using a rotary viscometer (Briekfield DV- , made in American).
The results are presented in Table 2. Its shown that the viscosity reduction rate was over 97.15% at 200, the reaction
time was 24 hours, the ratio of added water was 30%, with catalyst accounting for 0.2 %,the viscosity of upgraded heavy
oil is changed from 524.5Pas to 14.95mPas at 50. We can find that the viscosity of heavy oils reduced differently
after catalytic aquathermolysis, which also indicates the composition of the oils changed.
Analysis of generated gas
Figure 5, which shows that some gases were produced when water or water and catalyst were added into the
reaction system after one day reaction at 200, the compositions of the gas after the reaction by GC-MS. Only water
was added into the heavy oil, the main compositions of the gas are C4C9 alcohololefins ethersalkanes and
hydrocarbon of NO-containing compounds. When water and catalyst were added into the heavy oil, the quantity of the
gas large more than before, and the variety was increased. The added gas are C10C20 alcohololefins ethersalkanes
and NO hydrocarbon compounds. The most added gas were C4C6 hydrocarbon of O -containing compounds. All of
these results proved that the reaction of aquathermolytic was accelerated by the catalyst, and the chains contained
hetero-atom were broke off, not only broken C-S bond, but also broken C-O and C-N bonds. The amount of saturate and
aromatic increased, resin and asphaltene decreased.
SPE 130333 5

Conclusion
1.The anamphiphilic molybdenum chelate-aromatic sulfonic iron is an effective catalyst for aquathermolytic. The
laboratory experiment shows that the viscosity reduction ratio of heavy oil is over 97.15% at 200, 24 hr, 0.2 % catalyst
solution. The viscosity of upgraded heavy oil is changed from 524.5Pas to 14.95mPas at 50.
2.The percentage of saturatearomatic and H/C increased, and resinasphalt and SON decreased after the
catalytic aquathermolysis. The heavy components were converted into light components, and the quality of the heavy oil
was improved. It is beneficial to heavy oil production and transportation.
3.It was found the new mechanism of catalyst not only broken C-S bond, but also broken C-O and C-N bonds, and
accelerated the reaction of aquathermolysis. The results are very useful for the popularization and application of the new
technology for the insitu upgrading of heavy oil by aquathermolysis.

Acknowledgements
The authors thank the financial supports from ministry of science and technology of China(fund No. 50774070)
and Graduate School of China University of Petroleum.

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Table 1. The properties and composition of the heavy oil

Analysis item Data
Viscosity/Pa.s,at 50 524.5
Water/wt% 5.84
SARA Saturate 26.87
composition/% Aromati 28.31
c
Resin 29.75
Asphalte 15.07
ne
Elemental C 57.645
composition/wt% H 17.495
S 0.619
N 5.743
O 18.498

Table 2. SARA composition changes in heavy oil

Item Saturated /% Aromatic/% Resin/% Asphalt/% Viscosity reduction ratio/%
Before reaction 26.87 28.31 29.75 15.07
After reaction 31.12 30.41 24.56 13.91 97.15

Table 3. The element changes in the oil samples

Item C/% H/% O/% N/% S/% NH/NC
Before reaction 57.645 17.495 18.498 5.743 0.619 3.642
After reaction 54.327 18.972 22.86 3.523 0.3182 4.191
8 SPE 130333

Figure 1. IR spectrum of asphaltene before the aquathermalysis reaction

Figure 2. IR spectrum of asphaltene after the aquathermalysis reaction

Figure 3. IR spectrum of the resin before the aquathermalysis reaction

SPE 130333 9

Figure 4. IR spectrum of the resin after the aquathermalysis reaction

Figure 5. GC-MS of the gas after aquathermal cracking without catalyst and with catalyst in heavy oil