Hydrogen generation by aluminum alloy corrosion in aqueous acid solutions promoted by nanometal: Kinetics study

Renewable Energy 146 (2020) 2517e2523

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Hydrogen generation by aluminum alloy corrosion in aqueous acid solutions promoted by nanometal: Kinetics study lez-Barbosa a, A.L. Martínez-Salazar a, *, J.A. Melo-Banda a, M.A. Coronel-García a, J.J. Gonza J.M. Domínguez-Esquivel b a gico Nacional de M gico de Ciudad Madero, Centro de Investigacio n en Petroquímica, Prolongacio n Bahía Adair, Blvd. de las Tecnolo exico e Instituto Tecnolo Bahías, Parque Industrial Tecnia, Altamira, Tamaulipas, 89603, Mexico b zaro Ca rdenas 152, San Bartolo Atepehuacan, Gustavo A. Madero, Ciudad de M leo, Eje Central La Instituto Mexicano del Petro exico, Distrito Federal, 07730, Mexico

a r t i c l e i n f o

a b s t r a c t

Article history: Received 26 July 2018 Received in revised form 9 August 2019 Accepted 21 August 2019 Available online 21 August 2019

A novel process to obtain H2 from flat plate aluminum corrosion in aqueous acid solutions is described. A modified traditional shrinking core model has been developed to analyze kinetics behavior by including the effect of growing and textural changes of hydroxide layer during reaction. Modified model is fitted to experimental data. Initial diffusion coefficient, magnitude of the change in its value and the ratio of volume of the produced shell to volume of consumed core during reaction were determined by parameters obtained from fitting the proposed model to experimental data. © 2019 Elsevier Ltd. All rights reserved.

Keywords: Hydrogen Production Corrosion Kinetics

1. Introduction Hydrogen has attracted attention as an environmentally friendly fuel with high calorific value. However, most of hydrogen consumed worldwide nowadays is produced by using fossil fuels with the corresponding generation of CO2. In addition, conventional methods for hydrogen production are not profitable due to the high energy requirements. This scenario encourages the research focused in innovative, sustainable and economical ways to produce hydrogen. Hydrogen production based in light metals corrosion in aqueous solutions can be considered as a promising alternative route. Among all of them, aluminum (Al) is probably the most adequate metal for energetic purposes due to its high electron density, oxidation potential, high abundance, low price and by-products safely. The main disadvantage of hydrogen production through this reaction is the exceptional aluminum metal corrosion resistance due to an oxide passive film formation on its surface [1,2]. When aluminum metal is placed in water, a hydration reaction

* Corresponding author. E-mail addresses: [email protected], (A.L. Martínez-Salazar). https://doi.org/10.1016/j.renene.2019.08.103 0960-1481/© 2019 Elsevier Ltd. All rights reserved.

occurs on surface oxide film [3]. Bunker et al. [4] used secondary ion mass spectrometry to explain the development and rate of passive film formation on aluminum surface in contact with water. They concluded that in aluminum oxide (Al2O3) hydration, AleOeAl bonds are constantly being broken via hydrolysis to form AleOH species. Continuous hydration produces, eventually, oxyhydroxide or hydroxide phases such as boehmite (AlOOH) and bayerite (Al(OH)3) that are thermodynamically more stable than Al2O3 at room temperature. Deng et al. [5] proposed a model describing the different stages in aluminum-water reaction. 1. At initial stage, on the aluminum particle surface, oxide layer is hydrated and boehmite is formed. This stage is the induction stage during which no film growth occurs: Al2O3 þ H2O / 2AlOOH

R1

2. Hydroxide phases generated are thermodynamically unstable in contact with aluminum [6] and can be removed involving redox [email protected]

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reactions at Al2O3:Al interface to regenerate the oxide and produce hydrogen: 6AlOOH þ 2Al / 4Al2O3 þ 3H2[

R2

3. Non-reacted boehmite reacts with water excess to produce bayerite: AlOOH þ H2O / Al(OH)3

behavior of hydrogen production by flat plate aluminum corrosion in HCl aqueous solutions at different concentration in presence of Na2MoO4 was developed. Seawater was used in order to increase chloride ions presence. A comparison was made between modified model and traditional shrinking core model, and mass transfer rate of species/water molecules was calculated based on the modified model. This kinetic study will allow the evaluation and prediction of hydrogen production rates and efficiencies for different HCl concentrations, providing important design criteria for hydrogen generation technologies relying on the aluminum-water reaction.

R3 2. Materials and methods

Finally, difference pressure between trapped hydrogen bubbles and environment results in hydrated oxide layer failure, allowing water to come into contact with aluminum core and restart reaction process [5]:

Al þ 2H2 O/AlOOH þ

3 H [ 2 2

R4

It should be mentioned that phase constituents of newly formed AlOOH layer are different (slightly loose and lower tensile strength) from those on original aluminum particle surface [7]. Hydroxide species formed are soluble in solutions with a pH higher than 8.5 or lower than 4 [1,8]. However, within a pH range of 4e8.5, hydroxide layer precipitates on aluminum surface, which makes ion species/water molecules diffusion a critical step in determining hydrogen generation kinetics. Some activation methods aimed to dissolve or remove the oxide film are used in order to carry out the aluminum/water reaction [9e13]. Some of them consider chloride ions migration through the film. Breakdown occurs when chlorides reach metal-film interface. Recently, it has been shown that primary role of the anion in the initiation of corrosion processes is chemical rather than physical. It is chemisorbed onto the oxide surface assisting dissolution via oxide-chloride complexes formation [14,15]. Another way to activate aluminum surface is adding some extra reagents which act as reaction promoters. Li et al. [16] showed that Na2MoO4 particles in 1.0 M HCl solutions accelerate aluminum corrosion. On the other hand, various mechanisms have been proposed to explain passive film breakdown by “shrinking core” model proposed by Levenspiel [17e20] who established that, for gas/solid systems, unreacted core shrinkage is about a thousand times slower than the flow rate of gas toward unreacted core; due to the differences of solid to gas densities. Therefore, considering concentration gradient of gas in shell layer at any time, steady-state assumption of unreacted core could be useful [21]. In liquid/solid systems the velocity ratio is closer to unity than to 1000, so this assumption needs to be applied cautiously. Results of fittings cannot be considered satisfactory because of the considerable deviation of theoretical values from experimental data due to natural growth behavior of hydroxide layer on aluminum surface during reaction. S. S. Razavi-Tousi et al. [22] modified the shrinking core model for describe the reaction of aluminum particles with water. They involved two main differences. First one take into account that the shell (hydroxide layer) formed has different nature physical characteristic than consumed core (aluminum) therefore, the thickness difference between both needs to be consider and calculate. The second difference was that, during reaction, the shell formed becomes thicker, lowering the water diffusion rate [23,24]. The results were satisfactory because modified model fits with an R-square of 0.994 with experimental data. In this study, a modified shrinking core model to describe the

2.1. Material preparations The material studied is aluminum beverage cans waste, specifically the can body (3104 alloy according to ASM International). It chemical composition is 95.85% Al, 0.30% Si, 0.60% Fe, 1.20% Mn, 1.25% Mg, 0.25% Cu, 0.05% Cr, 0.10% Ti and 0.20% Zn. Each sheet was 0.15 mm in thickness and was sanded and cut in flat plates as a pretreatment. HCl acid (37%, AR grade) was supplied by Fermont Company. The promoter Na2MoO4 was synthetized in laboratory by chemical reduction method in aqueous solution, using ammonium heptamolybdate as precursor, sodium formaldehyde sulfoxylate (SFS) as a reducing agent and sodium citrate to stabilize the particles, capping them. Average of 14 nm particles size was obtained. Miramar beach seawater, Gulf of Mexico, was used containing a typical superficial salinity of 2.72% NaCl, 0.38% MgCl2, 0.166% MgSO4, 0.126% CaSO4, 0.086% K2SO4, 0.012% CaCO3 and 0.0076% MgBr2 [25,26]. 2.2. Experimental procedure A series of experimental evaluations were carried out at pilot level using a stainless-steel pressurized batch reactor of 2 L, for study aluminum corrosion reaction kinetics. Promoter agent molar ratio was fixed as 0.17 M of Na2MoO4. The amount of HCl was varied (0.5, 0.75, 0.875 and 1 M). Reactor was heated to maintain an initial set point temperature of 305 K. Aluminum load added to reactor was fixed at 40.67 g for each experiment. H2 production reactions started when aluminum came into contact with 1.35 L seawater solution. Pressure and temperature variations data, during reaction development, were acquired with a Wika Xsel pressure gauge and with a Tecni-lab temperature controller, respectively, in order to measure hydrogen production rates. At these conditions of temperature and pressure, H2 gas is well describe by Soave-RedlichKwong equation [27]. 2.3. Development of the model Fig. 1 shows the flat plate shape schematic diagram of the model. As in aluminum corrosion reactions in aqueous solution, the diffusion of ion species is the controlling step when a hydroxide layer is present hence, the rate at which A atoms (water atoms) are consumed by reaction is determined by the flux of A atoms through the hydroxide layer surrounding the aluminum particle to the surface of the core. Therefore, material balance is:

H2 Otowards the core ¼ H2 Oconsumed by reaction dN  A ¼ WHQA ¼ WHQAS ¼ WHQAC ¼ constant dt

(1)

Where N, Q, and W∙H are the number of moles, flux and surface

A.L. Martínez-Salazar et al. / Renewable Energy 146 (2020) 2517e2523

C

2519

W

QAC

Q QAS A

H x

CAo

L

o L C x

Fig. 1. Schematic of particle behavior during reaction.

area, respectively. QAS ¼ flux at the surface of the particle QAC ¼ flux at the boundary of the core (aluminum) The material flux of fluid can be written by Fick's law:

QA ¼ DA

dCA dx

(2)

where CA is the concentration of A atoms and DA is the effective diffusion coefficient of A in the passive film. Combining eq. (1) and eq. (2) and integrating across passive film thickness and A atoms concentration from the surface of the particle to the core, gives:

WHDA CAo ¼ 

dNA ðL  LC Þ dt

(3)

where CAo is the concentration of A at particle surface. In this step, first modification to the model proposed by S. S. Razavi-Tousi et al. [22] will be applied. Oxide passive film composition and properties are variable with hydration time and reaction conditions hence, is necessary to calculate how particle size changes during reaction. Particle overall volume (shell þ core) can be written as:

VL ¼ VLC þ Vz

(4)

Based on one-step reaction stoichiometry shown in R4, 1 mol of aluminum consumed produce 1 mol of aluminum hydroxide. Taking account their densities and molar weights, produced hydroxide volume must be 1.98 times larger than aluminum consumed. Therefore, if “n” is introduce as ratio of volume of the produced shell to volume of consumed core, n ¼ 1.98. However, AlOOH layer continuously formed will be different from the original (higher porosity), because it is formed accompanied by H2 bubble generation; “n” needs to be determined by fitting the model to experimental data, one can write:

VZ ¼ nðVLo  VLC Þ

VLo ¼ Original particle volume. Considering eqs. (4) and (5), and expressing volume in terms of fundamental dimensions, one can write:

2ðWHLÞ ¼ 2ðWHLC Þð1  nÞ þ n 2ðWHLO Þ

(6)

And therefore:

L ¼ ð1  nÞLC þ nLo

(7)

Eq. (7) predicts particle overall length (thickness) with an initial length of Lo (original thickness: 2Lo) which after reaction the core length reduced to LC. Now that equation for the particle is establish, eq. (3) can be modified by replacing the L value from eq. (7):

dN  A ðnLo  nLC Þ ¼ WHDA CAo dt VL ¼ Particle overall volume VLC ¼ Volume of the remained core VZ ¼ Volume of the produced shell on the core

(5)

(8)

According to Levenspiel [21], the amount of water (A) consumed by reaction is related to the amount of aluminum (B) consumed. Reaction can be represented by:

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A (fluid) þ bB (solid) / C (solid) þ dD (fluid) Therefore, A moles consumption rate, can be written as:

dN r r 2WH dLC dNA ¼  B ¼  B dVC ¼  B b b b

(9)

Where rB is the density of B atoms. Replacing eq. (9) in eq. (8) gives:

dLC ðnLo  nLC Þ ¼

DA CAo b dt 2rB

(10)

In this step, the next modification in the model proposed by S. S. Razavi-Tousi et al. [22] is applied. Since shell porosity decreases over time, in an unpredictable manner, with dependency on corrosive media conditions [28,29], becoming thicken and dense, diffusion coefficient of water in the shell cannot be assume as a constant and needs to be calculated. This study considers DA changes by a hyperbolic function of time (eq. (11)):

DA ¼

Do kt þ 1

(11)

Do ¼ diffusion coefficient at the time equal to zero k ¼ constant that determines the time effect on diffusion coefficient Substituting DA term in eq. (10) and integrating:

"

nL2  nLo LC  C 2

#LC ¼ Lo

bDo CAo lnðkt þ 1Þ 2rB k

(12)

In agreement with Levenspiel, defining xB as fractional conversion:

xB ¼ 1 

volume of the remained core ðVLC Þ L ¼1 C volume of the original particle ðVL0 Þ L0

(13)

Eq. (12) can be re-written as

nð1  xB Þ2  2nð1  xB Þ þ n ¼

bDo CAo L2o rB k

lnðkt þ 1Þ

(14)

Eq. (14) infers the conversion degree for a flat plate aluminum particle with a changing size and diffusion coefficient during corrosion reactions development in aqueous solutions.

3. Results and discussion 3.1. HCl contents effect on hydrogen generation Fig. 2 shows the effect of the chloride ions quantity variation in hydrogen production rate and the temperature behavior throughout the reaction. In general, a greater chloride ions concentration, the anodic dissolution velocity increases. As can be seen in Fig. 2; as HCl molar concentrations decrease, the induction period increase. Induction period is defined as the time that oxide layer on the surface of aluminum is dissolved/hydrated by water [4,29,30]. As it is observed, there is no reaction between aluminum and water during the induction period and no hydrogen is generated, therefore, this stage was excluded from the fitting in kinetic analysis. Also shown, at low HCl molar concentration (0.5, 0.75 M), higher temperatures are needed to achieve

reaction start. Once reaction started, highest corrosion rate was obtained in a short period of time because initially, a porous and thin hydroxide film was formed on aluminum surface, allowing water to come easily into contact with aluminum surface. As the reaction continues, the pH increases gradually due to OH ions release of cathodic reactions involved in a common corrosion process. This phenomenon corresponds to a hydroxide layer densified and less porous, which causes the decrease in water diffusion coefficient. Consequently, hydrogen production rate decreases and finally stop, being evident in Fig. 2 for low HCl molar concentration (0.5 and 0.75 M) where, after around fifty and 60 min reaction, respectively, hydrogen production was negligible. Therefore, although 0.75 HCl molar concentration sample shows the higher hydrogen production rate, it generates a narrow gaussian curve which indicate low conversion degree in compare with 0.875 and 1 M samples due their increment of chloride ions and, hence, lower initial pH. The pH of solutions, initial and after reaction, are shown in Table 1. 3.2. Fitting the model Equation (14) was fitted to the experimental data. rB is the number of aluminum moles in unit volume of a particle, which equals to 0.1 mol/cm3. CAo is water molecules concentration at particle surface equal to 0.056 mol/cm3. b is the ratio of aluminum to water for reaction (b ¼ 0.5) obtained from the condition of aluminum and water reaction stoichiometry. Lo is the initial half thickness of aluminum plate equals to 0.015 cm. The results of fitting, for all the concentrations tested, are presented in Fig. 3. Table 2 provides the parameters obtained from fitting developed model to experimental data (Do, k and n) using nonlinear regression in Polymath software. Results shows high fit with an R-square above of 0.944. The main discrepancy was at the initial period. Values of n > 1.98 was obtained from the fitting. Although diffusivities obtained for the four HCl concentrations are similar, for 0.5 HCl molar concentration sample, hydroxide layer formed on particle surface is thicker (n ¼ 9.47) due to pores presence, incrementing the ion species/water molecules diffusion surface (cm2) to reach Al2O3:Al interface. Diffusion surface diminishes with respect the increase of chloride ions (n ¼ 2.84 at 1 M). Do and k values confirm the observed in experimental tests results. The highest value for water diffusion coefficient in hydroxide layer at the time zero, Do, was obtained for 0.75 M HCl concentration reflected in Fig. 2 by the peak of highest hydrogen production rate. Further, this molar concentration also obtained the highest value for k, which determines how fast diffusion coefficient of the hydroxide layer decreases because of densification, corresponding to the narrow gaussian curve obtained and low conversions. Bunker et al. [4] obtained diffusion coefficients, Do, in the order of 1016 e 1017 cm2/s for describe corrosion and pitting of aluminum in water. This research achieved diffusion coefficients of 107 e 108 cm2/s, suggesting that reaction media studied (varying HCl molar concentrations) enhances aluminum-water reaction. Chloride ions are bonded chemically in the interface, reacting with the compounds of passive layer producing different mixed oxo-, hydro- and chlorocomplexes, migrating from surface into solution; breaking down, consequently, the passive film. As mentioned before, contrary to traditional shrinking model where the diffusion coefficient is constant and different stages of the reaction cannot be adopted, the current model allows formulating transitions using eq. (11) and Do and k obtained from fitting to the experimental results. On average, in HCl concentration variations test for hydrogen production, diffusion coefficient decreased

A.L. Martínez-Salazar et al. / Renewable Energy 146 (2020) 2517e2523

370

350

(b)

360

300 0.5 M

250

0.75 M

200

0.875 M

Temperature (K)

Hydrogen produciton rate (ml/min)

2521

1M

150 100

(a)

350 340 330 0.5 M 0.75 M 0.875 M 1M

320 310

50

300

0 0

10

20

30

40

50

60

70

80

0

90

10

20

30

40

50

60

70

80

90

Time (min)

Time (min)

Fig. 2. (a)Hydrogen production rate vs time and (b)temperature history, for different HCl molar concentrations in seawater (40.67 g aluminum, 0.17 M Na2MoO4).

Table 2 Parameters obtain from fitting modified model to experimental data.

Table 1 The pH of solutions, initial and after reaction. HCl (M)

pH initial

pH after reaction

Concentration (M)

Do x 107 (cm2/s)

k x 104 (s1)

n

R2

0.5 0.75 0.875 1

1.38 1.32 1.27 1.24

3.03 2.98 2.93 2.91

0.5 0.75 0.875 1

0.464 1.295 0.870 1.101

0.98 2.41 1.02 0.94

9.47 8.16 3.26 2.84

0.944 0.979 0.997 0.994

27% with respect time. Fifty minutes reaction time interval was established for results analysis. This agrees with experimental results where hydroxide layer grows and densified which causes the decrease in the diffusion coefficient and reducing hydrogen generation rate. In order to compare the behavior of model proposed by Levenspiel versus the modified model, eqs. (15) and (16) were applied:

t

t

¼ x2B

t¼

(15)

rB L20

(16)

2bDA CA0

Experimental results of 1 M HCl concentration in seawater were

Experimental data 0.25

Modified Model (eq. 14)

0.12

Degree of conversion

Degree of conversion

0.14

0.1 0.08 0.06

a)

0.04 0.02

0.2 0.15 0.1

b)

0.05

0

0 10

20

30

40

50

60

10

20

30

40

50

60

Time (min)

0.6

0.7

0.5

0.6

Degree of conversion

Degree of conversion

Time (min)

0.4 0.3 0.2

c)

0.1 0

0.5 0.4 0.3 0.2

d)

0.1 0

0

10

20

30

40

50

Time (min)

60

70

80

90

0

10

20

30

40

50

60

70

80

90

Time (min)

Fig. 3. Results of developed model fitting, eq. (14), on the data obtained from reaction of HCl aqueous solution a)0.5 M, b)0.75 M, c)0.875 M and d)1 M and flat plates aluminum.

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A.L. Martínez-Salazar et al. / Renewable Energy 146 (2020) 2517e2523

0.7

Degree of conversion

0.6 0.5 0.4 0.3 Experimental data Modified model Levenspiel model

0.2 0.1 0 0

10

20

30

40

50

60

70

80

90

Time (min) Fig. 4. Fitting results of Levenspiel's shrinking core model and modified model (eq. (14)) on data obtained from 1 M HCl concentration in seawater.

taken as an example to fitting with Levenspiel model, obtaining: DA ¼ 2:377x108 cm2/s and R2 ¼ 0.942 (see Fig. 4). As can be seen, traditional model results in a poor fit to experimental data, while modified model fits with a much higher R2.

[8]

[9]

4. Conclusion [10]

At low HCl concentrations, diffusion of ion species/water molecules from particle surface to substrate aluminum controls kinetics. Reaction behavior suggests a predominance of water in the reaction system based on the reaction: Al þ 2H2O / AlOOH þ1.5 H2. Diffusion coefficient of the shell (hydroxide layer) formed on the core (aluminum) changes with time. A significant diminish was detected due to densification. Shell thickness is not the same as that of consumed core otherwise, is bigger than that of consumed core. Results show the increase of thickness at lower HCl concentrations. Acknowledgements We gratefully acknowledge the financial support of this work by gico Nacional de Me xico; research project 6057.17-P. Tecnolo

[11]

[12]

[13]

[14]

[15]

[16] [17]

[18]

[19]

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