Assessment of process variables on the use of macauba pulp oil as feedstock for the continuous production of ethyl esters under pressurized conditions

Colonelli, T. A. da S.; Trentini, C. P.; Santos, K. A. dos; Oliveira, J. V. de; Cardozo-Filho, L.; Silva, E. A. da; Silva, C. da

doi:10.1590/0104-6632.20170343s20150768

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Kinetics and Catalysis, Reaction Engineering and Materials Science • Braz. J. Chem. Eng. 34 (3) • July 2017 • https://doi.org/10.1590/0104-6632.20170343s20150768 copy

Assessment of process variables on the use of macauba pulp oil as feedstock for the continuous production of ethyl esters under pressurized conditions

Authorship SCIMAGO INSTITUTIONS RANKINGS

ABSTRACT

This study evaluated the potential of macauba pulp oil (MPO) as a feedstock for continuous ester production using ethanol under pressurized conditions. Experiments were performed in order to obtain data for the effect of process variables on ethyl ester (FAEE) and free fatty acid (FFA) conversion in a catalyst-free process. From the results, it appears that the MPO to ethanol mass ratio and the pressure were the variables with more favorable effect on the evaluated response variables. The addition of n-hexane caused an increase in the production of esters; however, this had a negative effect on FFA conversion. The addition of water was unfavorable for oil processing with high acidity. In this process, esterification and transesterification occur simultaneously, and the high FFA content in MPO provides high yields (85 wt% of esters; 93% FFA conversion) at low temperature, since the esterification reaction rate is higher than the transesterification. The decomposition of fatty acids was evaluated and levels <5% were observed under the evaluated experimental conditions.

Keywords:
Acrocomia aculeata; continuous; catalyst-free; ethanol

Fatty acid	Content (wt%)
Capric	0.14 ± 0.01
Lauric	1.42 ± 0.08
Myristic	0.45 ± 0.01
Palmitic	13.54 ± 0.14
Palmitoleic	1.38 ±0.01
Stearic	3.87 ± 0.03
Oleic	69.95 ± 0.18
Linoleic	7.82 ± 0.12
Linolenic	0.52 ± 0.02
Eicosanoic	0.26 ± 0.01

Variable		Level
Variable	-1	0	1
Temperature (K), T	523	548	573
Pressure (MPa), P	10	15	20
Mass ratio (MPO: ethanol), MR	1:0.5	1:1.25	1:2
Water addition (wt%), W	0	5	10
Cosolvent addition (wt%), CS	0	10	20

Run	Variable/level					Answers
Run	T^a	P^a	MR^a	W^a	CS^a	FAEE yield (%)	FFA conversion (%)
1	1	-1	1	-1	-1	72.37±0.31	91.74±0.66
2	1	1	-1	1	-1	72.13±0.22	92.97±0.57
3	-1	1	1	-1	1	85.38±0.19	93.95±0.72
4	1	-1	1	1	-1	82.47±0.42	86.71±0.35
5	1	1	-1	1	1	77.77±0.37	69.18±0.46
6	1	1	1	-1	1	84.65±0.28	90.28±0.57
7	-1	1	1	1	-1	85.20±0.33	82.89±0.36
8	-1	-1	1	1	1	70.31±0.47	84.49±0.29
9	-1	-1	-1	1	1	76.94±0.54	65.58±0.33
10	1	-1	-1	-1	1	82.09±0.62	81.00±0.41
11	-1	1	-1	-1	-1	73.02±0.34	83.87±0.39
12	-1	-1	-1	-1	-1	73.82±0.42	84.25±0.44
13-15	0	0	0	0	0	72.55±0.36^b	87.70±0.49^b

	FAEE yield (%)		FFA conversion (%)
Variable	Effect	p-level^a	Effect	p-level^a
Mean/Intercept	76.92	<0.001	84.66	<0.001
Temperature	1.13	0.033	2.80	0.010
Pressure	3.35	0.003	3.22	0.007
MPO to ethanol mass ratio	4.10	0.002	8.86	0.001
Water addition	-1.08	0.036	-7.21	0.001
Cosolvent addition	3.02	0.004	-6.32	0.002

Oil; acidity	Conditions	FAEE (wt%)	Reference
Macauba pulp oil; 70.25 wt% of FFA	1:2 oil to ethanol mass ratio (~1:20 oil to ethanol molar ratio); 523 K; 20 MPa; 25 minutes and 20 w% of cosolvent addition	85.38	This Work
Waste fried oil; 1.5 wt% of FFA	1:30 oil to ethanol molar ratio; 598 K; 15 MPa; ~46 minutes and 5 w% of water addition	82.2	Gonzalez et al. (2013)
Castor oil; 1.4 wt% of FFA	1:40 oil to ethanol molar ratio; 623 K; 14.5 MPa; 10 minutes	56.17	Rodríguez-Guerrero et al. (2013)
Waste fried oil; 3.73 mg KOH.g^-1	1:20 oil to ethanol molar ratio; 573 K; 20 MPa; 70 minutes and 20 w% of cosolvent addition	~87	Abdala et al. (2014b)
Used palm olein oil; 11.1 mg KOH.g^-1	1:30 oil to ethanol molar ratio; 573 K; 30 MPa; ~40 minutes	70	Ngamprasertsith et al. (2014)
Macauba pulp oil; 56.3 wt% of FFA	1:30 oil to ethanol molar ratio, 598 K, 15 MPa, 35 minutes and 5 wt% of water addition	69.6	Navarro-Diaz et al. (2014)
Jatropha oil; 10.1 wt% of FFA	1:20 oil to ethanol molar ratio; 573 K; 20 MPa; 52 minutes	80	Silva et al. (2014)
Camelina oil; 1.7 wt% of FFA	1:40 oil to ethanol molar ratio; 583 K; 20 MPa; 30 minutes	86	Sun et al. (2014)
Canola oil; not reported	1:40 oil to ethanol molar ratio; 573 K; 3.54 MPa; 25 minutes	~60	Farobie and Matsumura (2015)

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