FOAM CHARACTERIZATION USING GLASS COKER EXPERIMENTAL SET UP

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Abstract: A large number of industrial processes specially in the petroleum refinery sector undergo problems with foaming which leads to fouling and decay of the process equipments. Thus in certain cases in petroleum refineries, foaming leads to process inefficiency and higher equipment maintenance cost. A very relevant aspect of current petroleum refinery operations is the heating up of vacuum residue in a coke drum and the subsequent generation of unwanted foam. This research paper describes the foam produced by heating vacuum residue in a Glass Coker experimental set up in terms of foam over temperature. The vacuum resids for analysis were obtained from Major U.S. oil companies like Chevron, Shell, Petrobras, etc. Detailed plots are provided that illustrate the variation of foam over temperature for different vacuum resids and with different times during a Glass Coker run. The experimental results clearly lead to the fact that foaming during a Glass Coker run is dependent on the residue (feedstock) properties and run operating conditions. Keywords: Glass Coker, foam over, foam, vacuum residue, experiments, petroleum refinery

Introduction

In oil/gas production, foaming is a serious issue and if left unattended, can lead to unexpected process shutdowns. In literature [1], Callaghan et al. pointed out that the foaming tendency of crude oil is directly proportional to the concentration of asphaltenes. Kremer et al. [2] are very precise and point out that the vapor generation and the presence of natural surfactants like asphaltenes and resins are crucial towards foam growth and lead to enhanced foaming in delayed cokers. According to Guitian and Joseph [3], the foam producing capability of a hydrocarbon mixture is dependent on the surfactant and on the mixture components chosen to create the foam. Zaki et al. [4] point out that the viscosity of the feedstock and asphaltene aggregation play an important role towards foam growth. As per Joseph [5], the presence of surfactant is crucial for a gas-liquid mixture to foam. As per Kouloheris [6], the amount of surfactant added to initiate foaming has a very large effect in the generation of foam.

In the present study, a glass coker was constructed and testing was begun for the purpose of visually observing and measuring foam formation under carefully controlled coking conditions. The tests were performed in 2005 in the TUDCP Pilot Plant, Tulsa, Oklahoma, U.S.A. The experimental setup for the glass coker is shown in Figure 1.

Figure 1: Experimental setup

The setup comprised of three main components: the distilling flask, the temperature control system and the heavy liquid collection system. A Pyrex brand 250 ml distilling flask with side arm was used as the reactor. The heating mantle was a Glass-Col series STM heating mantle that had an operating temperature range from ambient to 650C. The temperature was monitored using a Digitrol temperature controller that had an operating range of 0-750C. It is used to monitor temperatures at different locations in the flask (0.5, 3.5, 6.5 inches from the bottom of the flask). The vapors are condensed in a flask that is submerged in a water bath. The entire device was wrapped in a molded

insulating blanket. The test device was surrounded by a blast shield and tests were conducted in a vent hood.

The vacuum resids tested with the Glass Coker setup are shown in Table 1. The detailed feedstock properties for the resids tested are also shown in the same table. The first 16 tests were conducted where a window was left in the insulation to observe the foaming phenomena taking place. A second series of tests were conducted where the reactor was totally insulated. The test matrix for the glass coker tests performed are depicted in Table 2 and Table 3 respectively.

Table 1: Feedstock properties of the vacuum resids tested

Property

Equilon Resid

Citgo Resid 4.6 34.2 110

Chevron Resid 5.7 17.6 193

Suncor Resid 2.9 25.2 125

Marathon Petrobras Resid 10.3 12.1 38 Resid 6.5 24.3 63

(Shell) API 0.5 Asphaltenes 39.2 wt % Metal content, Ni (ppm) Metal content, V (ppm) Sulfur wt % Sodium 5.51 8 739 142

703

148

330

57

69

3.09 8

2.16 8

5.76 30

2.62 7

1.45 23

(ppm)

Table 2: Test matrix of selected glass coker tests with partial insulation

Run ID CIT 1 CIT 2 PETR 7 CIT 9 SUNC 11 CHV 12 CHV 15 EQU 16

Resid tested Citgo Citgo Petrobras Citgo Suncor Chevron Chevron Equilon

Date tested 06/01/2005 11/01/2005 03/02/2005 02/03/2005 11/03/2005 17/03/2005 25/03/2005 29/03/2005

Table 3: Test matrix of selected glass coker tests with complete insulation

Run ID MARA 18 MARA 19 SUNC 20

Resid tested Marathon Marathon Suncor

Date tested 05/04/2005 08/04/2005 15/04/2005

Experimental Procedure

The following operating procedure was followed for all the runs except MARA 19 and SUNC 20 runs: Before the resid is poured, 1 gm of boiling stones was added to the flask and then the resid to be tested was poured into the flask (61gms). The flask was placed into the heating mantle, was wrapped with insulation on the sides and the thermocouples were inserted into it after closing the top with a stopper. The heating mantle was connected with the temperature controller which was connected to a power source. The tubing was connected with the side arm and was sent to a liquid collecting receiver placed inside a stainless steel beaker containing cold water. The area around the flask and the mantle was covered with the insulation jacket. The blast shield was then put in front of the distillation flask. The first stage of heating was achieved by heating the resids to 600F with the output clamped at 25%. The ramping during the second stage of heating from 600F to 850F was started after the stabilization of the bottom temperatures for each resid. Also the ramping was done non-uniformly on an as-needed basis in order to reach 850F as efficiently as possible. At the end of the run, the ramping was stopped and the power settings were kept constant.

For MARA 19 and SUNC 20 runs, the same operating procedure was followed, the only difference being that at 42 mins into the run, the ramping was started by gradually increasing the power settings 3% every 5 mins.

Results & Discussion

The bottom thermocouple temperature was recorded carefully versus time for the glass coker runs. A foam over used to take place at a particular period of the runs with extensive foaming. The bottom thermocouple temperature rose from 800F and exceeded 1000F within a couple of minutes. The side arm of the distillation flask was found to be coated with resid. Table 4 and Table 5 provide the foam over data recorded for the partially insulated and completely insulated glass coker runs.

Table 4: Observations for selected partially insulated runs

Run ID PETR 7 CIT 9 SUNC 11 CHV 15 EQU 16

Foam over TB (F) 846 833 833 854 825

First Foam over time during a run (mins) 117 94 80 88 78

Table 5: Observations for selected completely insulated runs

Run ID

MARA 19 SUNC 20

860

Foam over TB (F) 889 864

First Foam over time during a run (mins) 69 70

855

Figure 2: Foam over Temperature variations for different partially insulated glass coker runs Figure 2 and Figure 3 illustrate the variation of the foam over temperatures for different resids versus time during the run when foam over took place the first time.

895

Figure 3: Foam over Temperature variations for 2 different completely insulated glass coker runs

Conclusions

For the partially insulated glass coker runs, the vacuum resids containing higher concentration (wt%) of Asphaltenes (example-Equilon, Citgo resids), the foam over temperatures are lower (820-840F) as well as the time taken to produce foam for the first time (70-100 mins). So foam is readily and quickly produced from the tests using vacuum resids with high content of Asphaltenes. For the completely insulated glass coker runs, the foam over temperatures are significantly lower for the resids with greater wt% of Asphaltenes (refer to Figure 3- Suncor vs Marathon resid). In general foaming tendencies were found dictated by variation in feedstock property (wt% Asphaltenes) and run operating conditions (total or partial insulation, non-uniform or uniform ramping for heating the resid).

Nomenclature

CIT- Citgo resid PETR- Petrobras resid SUNC- Suncor resid CHV- Chevron resid EQU- Equilon (Shell) resid MARA- Marathon resid Foam over TB- Bottom thermocouple temperature (F) at the foam over stage

Acknowledgements

I would like to thank The University Of Tulsa Delayed Coking Project Team, U.S.A. for their generous support and help regarding the successful conduction of the experimental work. I would also like to specially thank Dr. Keith Wisecarver and Dr. Volk (The University Of Tulsa Delayed Coking Project Team, U.S.A.) for their active suggestions during the pilot plant experimental work.

References

1. Callaghan et al., Identification of Crude Oil Components Responsible for Foaming, SPE Journal, 25(2), pp. 171-175 (1985). 2. Kremer et al., Foam Control Methods in Delayed Cokers, Petroleum Technology Quarterly, pp. 65-69 (2002).

3. Guitian J., Joseph D., Foaminess Measurements Using A Shaker Bottle, University of Minnesota (1996). 4. Zaki et al., Factors Contributing to Petroleum Foaming. 2. Synthetic Crude Oil Systems, Energy Fuels, 16(3), pp. 711-717 (2002). 5. Joseph D.D., Understanding Foams and Foaming, Journal Of Fluids Engineering, 119(3), pp. 497-498 (1997). 6. Kouloheris A.P., Foam-friend and foe, Chemical Engineering, 94(15), pp. 8897 (1987).

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