A Novel environmental nano-catalyst of zeolite amended with carbon nanotube/silver nanoparticles decorated carbon paste electrode for electro-oxidation of propylene glycol

doi:10.21203/rs.3.rs-1296937/v1

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A Novel environmental nano-catalyst of zeolite amended with carbon nanotube/silver nanoparticles decorated carbon paste electrode for electro-oxidation of propylene glycol

https://doi.org/10.21203/rs.3.rs-1296937/v1

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A novel environmental nano-catalyst based on zeolite (ZE) adjusted with carbon nanotube (CNT)/silver nanoparticles (AgNPS) ornamented carbon paste electrode (CPE) is used for electrochemical oxidation of propylene glycol (PG) in 0.5 M H₂SO₄ solution. The techniques like cyclic voltammetry (CV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) are utilized to achieve the catalytic performance. Surface characteristics are achieved by means of Scanning electron microscopic (SEM) and Energy dispersive X-ray analysis (EDX) techniques. Enhancing the loading magnitude of CNT into catalyst's ingredient can meaningfully develop the catalytic activity of the electrocatalyst towards propylene oxidation. The impact of altering the concentration of propylene glycol and the scanning rate on the resulting electrocatalyst performance during the oxidation cycle is considered. Chronoamperograms present an amplify of the steady state oxidation current density values after addition of these nano-catalysts. A promising catalytic stability of nano-catalyst has been achieved in electing its use for propylene glycol electro-oxidation in fuel cells applications.

Electrocatalysis

carbon paste electrode

propylene glycol oxidation

electrochemical impedance spectroscopy

cyclic voltammetry

The world has faced energy shock because fossil fuel reserves are rapidly exhausted. Also, the utilization of fossil fuels is being perceived for its harmful influences that may cause a natural and social crisis [1, 2]. Thus, it is important to look for a practical alternate fuel and make new energy conversion instruments to resolve these energy cohort difficulties [3, 4]. Direct alcohol fuel cells dependent on small organic molecules have great consideration as probable power devices, mainly for portable electronic devices and electric vehicles in view of their high energy density, efficiency, low ecological contamination and low working temperature [5, 6]. The electrocatalytic oxidations of different small organic molecules on various edited electrodes have been examined for application in fuel cells [7–13]. Most of recent reports, polyalcohol such as ethylene glycol, propylene glycol and glycerol is a good choice in fuel cells due to its high reactivity in electro-oxidation, inflammability, lower toxicity and high boiling point that allows tranquil handling and storage [14, 15]. Polyalcohol fuels are valuable due to they can be produced from renewable sources [16, 17]. Furthermore, to improve the efficacy of fuel employment, active catalysts, having enough ability to break strong C–C bond in polyalcohol are highly wanted [18–20] .The electrochemical oxidation of polyalcohol on noble metals such as platinum, palladium, and gold has been demonstrated in several recent investigations. Sadiki et al. [21] Studied the polyalcohol oxidation in alkaline media by improve the efficacy of the palladium catalysts edited by several adatoms (antimony, tin, lead). The existence of bimetallic surface leads to enhance the oxidation rate of these alcohols. Munoz et al. [22] presented that a carbon-supported Pd-Cu nanocatalyst can increase the polyalcohol oxidation rate in alkaline medium. The developments have been accredited to both electronic and bifunctional effects. Furthermore; the Cu/Pd ratio seems to have a noteworthy impression on the rate of oxidation [23, 24]. To make the electro-oxidation of polyalcohol practically valuable, novel inexpensive and selective catalysts are required. Catalyst plays a crucial role in electrochemical energy conversion in fuel cell. Carbon paste electrode (CPE) is the most popular catalytic support material due to their strong electronic conductivity, comparative stability in different media and high effective surface area [25–27].The nano-modified electrodes are substantial to improve the catalytic activity in order to reduce production costs.

Recently, Silver nano particles (AgNPs) have potentially demonstrated in electrocatalysis applications. AgNPs can act as a conduction center to improve the transmission of electrons and deliver exceptional catalytic activity [28, 29]. Carbon nanotubes (CNTS) are porous constituents with special characteristics, high efficiency of surface area, strong conductivity, and chemical stability [30]. Carbon nanotube has high electrocatalytic activity in numerous substances and therefore suitable for building various electrocatalyst with high efficiency [31–34]. Zeolites are known as microporous crystalline aluminosilicate materials with high surface area, adsorptive and molecular sieving materials. Zeolites are unique materials, which can be exploited in the development of modified electrodes with high chemical and thermal stability [35–38]. Nevertheless, the propylene glycol oxidation in acidic media is quiet not fully revealed and requires to be additional studied. It is well recognized that carbon paste electrode with nano-material showed electrocatalytic act toward propylene glycol oxidation in acidic medium due to strong adsorbability of PG molecules on the nano-material surface.

The aim of this work to produce a novel environmental nano-catalyst created from modified carbon paste electrode with zeolite, carbon nanotube and silver nanoparticles. The catalyst with large surface area, simple and low cost construction is recommended for propylene glycol oxidation in acidic medium.

2.1. Materials and reagents

The Chemicals are graphite, multi walled carbon nanotube, zeolite and silver nanoparticles powder (dispersion nanoparticles, < 100 nm), propylene glycol (99, 8%), Sigma–Aldrich (USA) and were used without further purifications. All solutions are prepared utilizing triple distilled water. All experiments were achieved at ambient temperature.

2.2. SMWZCPE modified electrode preparation

In order to develop the catalytic activity of modified electrode different weights of zeolite and silver nanoparticles were investigated. Also the loading of carbon nanotube into the catalyst (0.01–0.04 mg) was considered. The best modification for carbon paste (CPE) electrode was made by mixing 5 g graphite powder with drops of paraffin oil on a glassy mortar, then 0.04 mg of carbon nanotube, 5 mg of silver nanoparticles and 0.1 g zeolite were added to set up the catalyst (SMWZCPE), which was utilized in all experiments. The carbon paste was packed in a Teflon tube with pressing to acquire a smooth surface.

2.3. Cell and Apparatus

A three-electrode cell enclosing a platinum rode as a counter electrode (CE), saturated calomel electrode (SCE) as a reference electrode (RE) and (SMWZCPE) as the working electrode (WE) was used. Cyclic voltammetry (CV), chronoamperometry (CA) and Electrochemical impedance spectroscopic (EIS) measurements are achieved by EC-Lab SP 150 Potentiostat electrochemical workstation. EIS are done at 10 mV ac amplitude at frequency of 1.0 mHz to 100 kHz. EC-Lab software is operated for demonstrating. Scanning electron microscopic (SEM) measurements were performed by SEM Model Quanta 250 FEG (Field Emission Gun) related with EDX Unit (Energy Dispersive X-ray Analyses) (FEI company, Netherlands).

3.1. Characterization of the modified electrocatalyst

Figure 1A shows the SEM images of the SMWZCPE modified electrode which reveals that silver nanoparticles, CNT and zeolite dispersed in a uniform distribution on the graphite paste.

Figure 1B demonstrates well the EDX spectrum of SMWZCPE which approves the existence of C, O, Ag, Al and Si by a good percentage in the formed electrocatalyst. The uniform spreading of the elements along the entire catalyst surface offered an opportunity to improve the active electrochemical surface area and increasing the elecrocatalytic efficiency.

3.2. Electrocatalytic oxidation of propylene glycol

Figure 2 presents the CVs obtained at the bare carbon paste electrode in 0.5 M H₂SO₄ and modified electrode SMWZCPE in 0.5 M H₂SO₄ with and without 0.5 M propylene glycol at a scan rate of 100 mVs^− 1. CV verified at the bare electrode seemed unremarkable indicated catalytic inactivity. However, the CVs of the modified electrode offered a developed electro-catalytic activity towards propylene oxidation. The oxidation of propylene at modified electrode reveals a reversible oxidation peak at 0.7 V and 0.38 V with a peak current ~ 50 times more than the bare one. This indicated that the electro catalytic activity of the modified electrode surface can be improved upon addition of zeolite, silver nanoparticles to the carbon nanotube matrix where a large effective surface area was obtained inducing higher adsorptivity of propylene through active hydroxyl function group to the modified electrode surface.

Electrochemical impedance spectroscopy technique is applied to examine the conductivity (catalytic activity) of the modified electrode towards propylene oxidation which is inversely proportional to the impedance. EIS scans distinguished at the peak potential 0.7 V for bare in 0.5 M H₂SO₄ and SMWZCPE electrode in 0.5 M H₂SO₄ with and without 0.5 M propylene glycol. Figure 3 as Nyquist plots showed a semi-circle links to a charge transfer resistance and a line links to a diffusion process at both high and low frequencies, respectively. The experimental results were fitted with one-time constant model (Fig. 3 inset) including R_s (solution resistance), R₁ (charge transfer resistance), W (Warburg impedance linked to diffuesion prcess) and Q₁ (constant phase element of capacitance). Constant phase element was attributed to microscopic roughness and surface heterogeneity [39, 40]. Bare electrode show a large semicircle diameter than that of modified SMWZCPE electrode signifing that impedance reduced and conductivity upsurges. These results support well the high oxidation peak current acquired from CVs response for modified SMWZCPE electrode.

The impedance (Z_CPE) of a constant phase element is:

Z_CPE= [C (jω) ^α]⁻¹

Where α is an exponent account for surface heterogeneity, 0 ≤ α ≤ 1, j is the imaginary number (j = (-1)^1/2), ω = 2πf is the angular frequency in rad/s, f is the frequency in Hz = S^− 1 [41–43]. The EIS outcomes have confirmed the conclusions drawn from the above cyclic voltammetry experiments. The outcomes of EIS analysis are listed in Table 1.

Table 1

Electrochemical impedance parameters.
sample	R₁/ kΩ	Q₁/ µF	α	W/ k Ω cm² s^− 1/2	Rs/ Ω
Bare	19.2	11.1	0.78	9.8	21
SMWZCPE/0.5 M H₂SO₄	10.5	14.3	0.81	7.3	37
SMWZCPE/0.5 M prop + 0.5 M H₂SO₄	7.60	17.1	0.84	2.1	35

The outecomes certified well CV data, where SMWZCPE electrode have the highest current and lowest impedance values.

3.3. Impact of carbon nanotube loading

The loading of CNT into the catalyst ingredients has a substantial influence on the catalytic activity of the modified electerode towards propylene oxidation due to growth of surface area. Figure 4 displays the CVs respone for propylene oxidation on modified electrode SMWZCPE with various loading of CNT (0.01–0.04 mg) in 0.5 M H₂SO₄ at scan rate of 100 mVs^-1. The propylene oxidation is reliant on the loading amount of CNT and anodic peak current increase with the increase in CNT loading in the synthesized electrocatalyst (direct relationship). Also, the onset potential shifts to more negative values for the best performing. As clearly interpreted, the increase in anodic peak currents indicates a corresponding increase in avaliable active sites with higher adsorption extent for hydroxyl group, which required for propylene oxidation [31–33].

3.4 Effect of scan rate

Effect of varying the potential scan rate (ν ranging from 10 to 400 mVs^− 1) was performed on modified SMWZCPE electrode in 0.5 M H₂SO₄ in absence of propylene glycol to confirm the electrochemical activity of the catalyst in aqueous solution (Fig. 5). Increasing the scan rate resulted in higher anodic peak current density and positive shift occurs in the forward peak potential. A linear relationship between the anodic peak current and square root of the scan rate was gotten as shown in the inset of the figure, with the following equation: I_p (µA) = 34.13 + 3.71 ν ^1/2 (mVs^− 1) (r² = 0.9766).

The impact of the potential scan rate (ν ranging from 10 to 500 mVs^-1) on the electrocatalytic anodic peak current of modified electrode SMWZCPE was also achieved in 0.5 M H₂SO₄ with 0.5 M propylene glycol and established in (Fig. 6). As the scan rate increase (10–500 mV/s), the oxidation peak current amplified constantly and the peak potential moved positively. The plot of anodic peak current and square root of the scan rate (Inset B) leads to a linear relation: I_p (µA) = 91.22 + 2.77 ν ^1/2 (mVs^-1) (r² = 0.9466), which approves that the oxidation process of propylene glycol is diffusion controlled mechanism with some adsorption [44, 45].

3.5 Effect of propylene glycol concentration

The synthesized electrode was applied to distinguish the impact of propylene concentration for fuel cells application. The oxidation of propylene in the range 0.01 to 0.5 mol/ l was considered on this electrode. Figure 7 shows the conduct of this modified electrode for various propylene concentration from 0.01 to 0.5 mol/L by CVs at the scan rate of 50 mV s ^− 1. The propylene oxidation curves expose that anodic current peaks increase with expanding propylene concentration [46, 47]. This obtained results confirm that our modified electrode SMWZCPE act as effective catalyst for the oxidation of propylene in 0.5 M H₂SO₄. Figure 7 (inset B) demonstrates a linearity by: I_p (µA) = 23.27 + 218 C (r² = 0.9956). It's suggested that the above relationship between Ip and [propylene] is owing to a diffusion-controlled mechanism.

3.6 Stability of an electrocatalyst

The stability of an electrocatalyst is an essential and evaluated by chronoamperomety. The chronoamperometric curves were obtained in the solution of 0.5 mol/l H₂SO₄ containing ( 0.01–0.5 mol/l ) propylene for 20 minutes at constant potential 0.7 V. Figure 8 demonstrate current – time relation for different concentrations of propylene glycol, in the first the modified electrode SMWZCPE reveals continous decay of anodic oxidation current and after ~ 2.5 min reached relatively stable value until the end of experiment (~ 20 mins). This denotes good mechanical and electrocatalytic constancy of the modified electrode toward PG oxidation.

Finally, based on the obtained outcomes its confirm that SMWZCPE modified electrode shows good promises to improve the activity of oxidation reaction of propylene glycol in acidic medium fuel cells.

A novel environmental nano-catalyst successfully prepared constructed by modified carbon paste electrode with zeolite, carbon nanotube and silver nanoparticles .
The characterization of the electrode SEM and EDX analysis shows that a well dispersed zeolite, CNT with the existence of silver nanoparticles occurs with a good percentage on the surface.
Electrochemical measurements discovered the exceptional electrocatalytic activity of nano-catalyst for oxidizing propylene.
Propylene oxidation progression was following diffusion – controlled process at electrocatalyst surface.
Enhancing CNT content developed the attained anodic peak current until greatest performance at the electrocatalyst comprising 0.04 mg CNT.
The proposed SMWZCPE modified electrode shows acceptable stability towards propylene glycol oxidation.

Data availability

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No competing interests reported.

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You are reading this latest preprint version

A Novel environmental nano-catalyst of zeolite amended with carbon nanotube/silver nanoparticles decorated carbon paste electrode for electro-oxidation of propylene glycol

Status:

Version 1

Abstract

Figures

1. Introduction

2. Experimental

2.1. Materials and reagents

2.2. SMWZCPE modified electrode preparation

2.3. Cell and Apparatus

3. Results And Discussion

3.2. Electrocatalytic oxidation of propylene glycol

3.3. Impact of carbon nanotube loading

3.4 Effect of scan rate

3.6 Stability of an electrocatalyst

Conclusion

Declarations

References

Additional Declarations

Status:

Version 1