Fabrication and characterization of Polysulphanilic acid/Borate glass Composites as Anticorrosion Coat for Mild steel in Acidic medium

doi:10.21203/rs.3.rs-5220718/v1

Polymer-glass matrix composite exhibits excellent performance as scale inhibitors and anticorrosive coatings.Polysulphanilic acid borate glass composites were chemically performed using potassium dichromate (PDC) as an oxidant in an acidic medium at room temperature. The prepared polymer composites are characterized by IR spectroscopy, XRD and SEM. The interaction between polymer and borate glass is mainly via H-bonding and electrostatic attraction. The efficiency of all the synthesized polymeric samples as anticorrosive coating on mild steel in acidic mediumwas performed by using electrochemical techniques and well compared. The morphology of the coated samples after 7 days of immersion in 1.0 M HCl and the polarization and impedance results confirmed that the composite containing glass borate with0 % CuO (Graft100) represented the best coat with an efficiency of 94.6 %.

Polysulphanilic acid

corrosion

Polysulphanilic acid grafted borate glass

Mild steel

Mild steel uses widely in industry especially in acidic media due of its various desirable characteristics like the electrical and thermal conductivity, good ductility, and high tensile strength [1–2]. As the acidic media are very aggressive for metals and alloys and could lead to corrosion, therefore, It is best to apply a protective method to stop this unwanted rusting as well[3].In many aqueous media, polymers especially the water-soluble ones are used as efficient corrosion inhibitors. The inhibition is brought about by the polymers' functional groups bonding with metal ions to form complexes on the metal surface. They have numerous points of interest, the most noteworthy of which is its simplicity to get ready and high dissolvability furthermore low thickness [4]. Previous works showed the use of various cationic polymers such as poly ethyleneimine derivatives to stop metals from corroding through blanketing the surface with large surface area complexes [5–6]. Polymers having the COOH group and that containing polyethylene oxide, polyacrylamide, and carboxymethyl cellulose (CMC) are represented as effective corrosion inhibitors [7–8]. Current research efforts are focused on discovering substitutes for both organic and inorganic chemicals in corrosion inhibitors. Naturally occurring materials have been found to readily satisfy this need due to their availability, inexpensive and a regenerative supply of resources,, and ecofriendly and ecologically acceptability [9–10].The greater 1 part of the effective natural mixes is the presence of oxygen, sulfur,

Nitrogenatoms and various bonds through which the adsorption occurred on the metal surface [11–13].The mechanisms behind corrosion inhibition are neither consistent or constant with a single inhibitor in a particular system, nor are they uniform with regard to all types of chemicals that have been studied to far.[14].The offshore industry is very 7interested in coating the surface of metallic substrates like steel, iron, magnesium, and aluminium, as well as their alloys, to avoid corrosion. Many factors can cause corrosion in offshore installations, including mud, splash, atmospheric and submerged zones [15].Stainless steel covered by polyaniline (PANI) remained in the passive state for a relatively long period in sulfuric acid solution. Poly (1,5‑diaminonaphthalene) coated on copper surface prevent it from corrosion in chloride medium [16]. The chemical makeup of the polymer determines the potentials of polymer inhibition, and the majority of polymer research is conducted without taking into consideration the chemical features of the polymers. The presence of foreign molecules with the polymer to form polymer matrix composite are strongly affected their surface and increases the physical barrier network which causes an increase in the corrosion inhibition abilityof the polymer as the mechanism of inhibition in most cases occurred through adsorption of the inhibitor molecules on the metal surface resulting in blocking the active sites [17–18]. It was reported that the presence of inorganic compounds such as Zinc phosphate can enhance the corrosion inhibition of the organic coating [19–20].Some kinds of glasses such as phosphate and borate glasses were used as corrosion inhibitors for metals and alloys in acidic medium through the adsorption of these molecules on the metal surface[21–25].desorption-mediated inhibition's effectiveness is defendant upon the mechanical, structural, and chemical properties of the layer that has been adsorbed.[26], and the presence of glass materials within this layer affect the coat properties. Therefore, in the present work, sulphanilic acid was polymerized in the presence of different borate glass samples using potassium dichromate (PDC). Polysulphanilic acid/ borate glass composites were characterized by IR, SEM and XRD to confirm the suggested structure of the formed composites. Using a variety of electrochemical and surface analytic methods, the impact of these composites' polymeric coating on the suppression of mild steel corrosion in an acidic environment was investigated.

2.1 Materials and Solutions

Glacial acetic acid ( 99.5%) and Sulphanilic acid are product of Omega Scientific Service, and dimethylformamide (DMF) is product of Sigma Aldrich Chemical Company (Germany). Ammonia solution (33%) ,Hydrochloric acid (35%), methanol, and N-methyl-pyrrolidone are of chemically pure grade products provided by Prolabo-Chemical Company (England).Twice distilled water was used as a medium for the polymerization reaction. Potassium dichromate and orthoboric acid (H₃BO₃) are products of Techno Farm chem., India. Lithium carbonate (Li₂CO₃), calcium carbonate (CaCO₃) and copper oxide (CuO) are products of (Fluka, Germany).

2.2. Fabrication of Borate glass samples

The studied glasses were prepared from pure chemicals (˃99%) including orthoboric acid (H₃BO₃) as a source of B₂O₃, Lithium carbonate (Li₂CO₃), calcium carbonate (CaCO₃) and copper oxide (CuO) as sources of Li₂O, CaO and CuO respectively. The batches were melted for approximately 60 minutes at 1250 C in porcelain crucibles. Including rotating the melts at interval times for complete homogeneity. The melting was made in a SiC heating furnace (Vecstar, UK).stainless-steel molds used to slightly heated the prepared glasses inside it, and then the samples were immediately transferred to an annealing furnace regulated at about 350 ^oC.stop the muffle after 1 hr with the samples inside and then left cool to room temperature with rete 25^oC/hr.

Table 1

the glass composition.
Sample ID	B2O3	CaO	Li2O	CuO
100	50.00	20.00	30.00	0.00
101	49.95	19.98	29.97	0.10
103	49.75	19.90	29.85	0.50
105	49.26	19.70	29.55	1.49

2.3 Optimization of grafted polysulphanilic acid borate glass composites

To optimize the preparation of high yield, the effect of sulphanilic acid quantity (from 0.25 to 1.00 gm range), potassium dichromate (from 0.25 to 1.00 gm range) and glass (from 0.05 to 0.35 gm range) was studied. In addition, the effect of reaction temperature and time was studied. The optimum conditions for the preparation of high-yield polysulphanilic acid borate glass composites are found to be 1.0 gm sulphanilic aciddissolved in 20 mL distilled water mixed with 20 mL dimethylformamide (DMF) at 25°C in the presence of 1.0 gm potassium dichromate as an oxidant dissolved in 20 mL distilled water at 25°C, and 0.10 gm glass dissolved in 20 mL distilled water with one drop hydrochloric acid then the the formed graft remain for 24 h. Then, distilled water used to filtered and washed manytimes, methanol and N-methyl-pyrrolidone and dried at 60–80°C till constant weight [27–29]

2.4 Preparation of grafted polysulphanilic acid /glass composite

The chemical oxidative grafting copolymerization reactions are carried out in a well-stoppered conical flask of 250 mL capacity containing followed by the addition of the required weight 1.0 gm of sulphanilic acid dissolved in 40 mL distilled water/DMF (1:1).then added 0.1 gm of different samples of borate glass in 20 mL distilled water and shake well, then the potassium dichromate solution 1.0 gm dissolved in 10 mL distilled water was added as oxidant with continuous shaking and complete volume to 80 mL with distilled water. In every experiment carried out, the sequence in which the chemicals were added remained consistent. 10 seconds were spent shaking the flasks 15 times. After a day, the polymerisation solutions were filtered through a Buchner funnel, carefully cleaned in distilled water, and then dried in a vacuum oven at 80 °C until their weight remained constant [30-31].

2.5 Characterization of the prepared samples

Infrared transmission spectra were carried using Shimadzu FTIR Vertex 70 Bruker Optics technique recorded by Perkin Elmer 457 spectrophotometer from 500 cm^− 1 to 4000 cm^− 1, the spectra were measured at room temperature with about 1 cm^− 1 resolution for the instrument. The set is present at Beni-Suef University. The XRD patterns of all prepared polymer samples were characterized with the help of Panalytical Empyrean X-ray diffractometer 202964. The scan range was (5°–140°). The electron microscope analysis was carried out using JSM-6510LA Scanning Electron Microscope, JEOL, Japan. Both sets are present at Beni-Suef University.

2.6 Corrosion studies

Potentiodynamic polarizations for coated 7 days of immersion.

The electrochemical impedance spectroscopy (EIS) of the electrode surface after immersion in 1.0 M HCl has been carried out with Ac voltage amplitude of 10 mV using an electrochemical impedance system. The frequency range used in the study was 0.1–10⁴ Hz. The values of the equivalent circuit parameters were analyzed by using the equivalent circuit program. All the electrochemical impedance measurements were carried out at open circuit potential.

2.7. Surface examination:

The surface morphology of the mild steel specimen specimens after 7 days of immersion in 1.0 M HCl coated and uncoated with different coats (PSA, 100, 101, 103 & 105) are performed on scanning electron microscope JEOL-JSM-5600 equipped with an energy dispersive X-ray spectrometer OXFORD Link-ISIS-300.

3.1 Characterization of the Prepared Polymeric borate glass composites

The prepared polymeric composites are polysulphanilic acid (PSA), (polysulphanilic acid/ glass100 composite (PSA/100), polysulphanilic acid with glass101 (PSA/101),) and polysulphanilic acid with glass 105 (PSA/105)

3.1.1 Infrared Spectroscopic Analysis

The infrared spectra (IR) of the prepared samples, PSA, (PSA/100) ,(PSA/101) and (PSA/105) are presented in Figure (1). The assignments of the bands are tabulated in Table (2), From the Figure and Table, it is clear that, the grafting of PAS with glass was confirmed. This confirmation is clear from:

The deconvolution peaks ranging from 1600 − 1200 cm^− 1 are mostly related to the stretching vibrations of the triangle borate groups (BO₃), where the stretching vibrations of tetra borate groups are located at about 800–1200 cm^− 1. The bands at about 690 cm-1 are belongs to bending vibrations of B-O-B bonds. The bands cited at about 499, 546 and 550 are correlated to the Cu-O vibrations.
Stretching of vibrational of free and bondedOH group appear at 3461 cm^− 1, 3554 cm^− 1, 3490 cm^− 1, and weak absorption band at 3840 cm^− 1in PSA,PSA + 100, PSA + 101 and PSA + 105 respectively.
In PSA + 101 glass,C-H deformation showing substitution in benzene ring
Shifting of C-H deformation of benzene from 850 cm^− 1 in PSA and 870 cm^− 1in PSA + 101 to 793 cm^− 1in PSA + 105.deformation of C-H aromatic or OH deformation and c = c in all samples from 1600 to 1650 cm^− 1, tabulated in Table (2) referenced from [32–41].

Table (2): IR bands and their assignment for the investigated samples

wave number cm-1				Assignment	Ref.
PSA	PSA + 100	PSA + 101	PSA + 105	Assignment	Ref.
			3862	stretching vibration of free OH group and Stretching vibration of intermolecular H-bond	32
		3760	3761
			3424
	3416	3407
3350 ^m				stretching vibration of N-H
3234 ^m	3228			stretching vibration of N-H
			2930	C-N overtone stretching vibration of, deformation of aliphatic C-H or NH ,OH deformation	33
		2377	2378		33
1666 ^m	1664	1683	1672	stretching vibration of C = C and or C = N in the suggested polymer structure Stretching modes of triangle borate groups (BO3)	34–35
1599 ^s	1604	1602	1602
1508 ^m	1507	1507
1397	1381	1388	1435	C-N stretching vibration or combination bands of asymmetric bending and torsional oscillation of the protonated amine group	36
1304	1298	1300	1302		36
1181	1181	1182	1184	C-N stretching vibration plane deformation of CH aromatic or OH deformation (coupled) or NH deformation Stretching modes of tetrahedral borate groups (BO4)	35–37
1123 ^w	1127	1126	1123
1033 ^w	1036	1034	1033
1033 ^w	1036	1034	1033	S-O vibration band	38
928	920	920	920	out of plane C–H deformation showing substitution in benzene ring Bending vibrations of B-OB bonds	35, 39
828	828	828	830
	702	700
697			697
	631	633	629	Torsional oscillation of protonated NH3 group	40
567 m	570	570	568	Torsional oscillation of protonated NH3 group	40
		546	499, 550	Correlated to the Cu-O vibrations	41
(s = strong, m = medium, sh = shoulder and w = weak)

3.1.2 Scanning Electron Microscope and Xray Diffraction Patterns

SEM pictures of the investigated polymer samples are present in Fig. 2 (a-d). From which it is clear that Figure. 2a for polysulphanilic acid (PSA)shows spherical and sheets shapes of particle size ranged from 0. 267 to 0.734 µm. However, the PSAsamples grafted with glass such as PSA + 100 shows small particles ranged from 0.124 to 1.14 µm, PSA + 101 showed spherical shapes ranged from 0.136 to 0.955 µm, while PSA + 105 sample showedspherical shape ranged from 0.262 to 0.496 µm.

From Figure (3), it is clear that the crystallinity of PSA increase with presence of glass structures comparing by the amorphous state of the used glass. This can be contributed to the ordering of glass particles between the PSA chains which lead to increasing the crystalline regions. The XRD patterns of PSA reveal that the amorphous regions are highly ratios than the crystalline one. On polymerization of sulphanilic acid in presence borate glass leads to the chance of bonding with the formatted PSA chains via H-bonds which increase the crystallinity.

The suggested structure of prepared samples can be presented in the Fig. 4.

3.2 Corrosion Studies

3.2.1 Open‑circuit experiment

The open-circuit potentials (E_ocpvalues) were recorded as a function of time for the coated and uncoated mild steel electrodes in 1.0 M HCl solution and were showed in Fig. 5. Comparing the initial potential value of E_ocp for the uncoated mild steel (-452 mV) with the coated samples by PSA, PSA/100, PSA/101 and PSA/105 (-435, -420, -443 and − 445) which indicated more passivity of the coated mild steel than the uncoated one especially that coated with PSA/100. This behavior provided evidence on the ability of the polymer (PSA) doped with glass to protect mild steel against the corrosion in acidic medium. At the first 5 hours of immersion of the samples, the value of E_ocp for the uncoated surface and coated with PSA/100 directed to more passive values then shifted to more negative for the uncoated, however, E_ocpfor PSA/100 coated sample still nobler than the uncoated. This result indicates that the barrier efficiency of the coat diminished during the first hours of immersion due to the deterioration of the borate glass by hydrolysis from the coatdue to the penetration by ions through it, then metal ion sites can be hydrated that passivates the sample again that appears clear from the values of E_OCPduring the 7 days of immersion[42].

These can be confirmed by the scanning microscope analysis as shown in Fig. 6 (a-e), the morphology of the uncoated mild steel immersed for 7 days in the acidic chloride solution shows amorphous surface containing the corrosion product with spreading of some pores filled with crystals from the chloride solution Fig. 6a; however, the coated mild steel surfaces with PSA, PSA/100, and PSA/105 show an absence of the pores and the presence of new feature with needle structure as shown in Fig. 6b, that filled the pores.It was also observed that the surface of the sample became coated with PSA/105 contains urchin like structure that confirms the leaching of CuO from the glass matrix to the coat surface.

3.2.2Potentiodynamic polarization measurements

The curves of potentiodynamic polarization for uncoated mild steel compared to coated mild steel after immersion in 1.0 M HCl solution are presented in Fig. 7 The curve shows that both the cathode branch and the anode branch are offset to more noble values for all coated samples except that coated with 105, however the change in corrosion potential (E_corr) is very low which indicated that the presence of the coat affect both the cathodic and the anodic reactions. Deduction of the corrosion parameters from Tafel lines was occurred such Tafel slopes (b_c, b_a), corrosion current density (i_corr) and E_corr are presented in Table 3. The corrosion current density values of ($\:{i}_{corr}^{{\prime\:}}$) for coated mild steel samples in HCl are lower than the corrosion current density value for uncoated mild steel ($\:{i}_{corr})$. The inhibition efficiency IE% value was calculated from the corrosion current density by using this formula:

$$\:IE\%=\:\frac{{i}_{corr}-\:{i}_{corr}^{{\prime\:}}}{{i}_{o}}\:x\:100$$

1

Where, $\:{i}_{corr}$and $\:{i}_{corr}^{{\prime\:}}$are the corrosion current density for uncoated and coated mild steel.

For the coated sample, corrosion current density decreases with graftingthe PSA by glass, however presence of CuO in the glass composition decreases inhibition efficiency from 94.6% (0 CuO) to 85.9% ( 1.5 CuO) but still the corrosion behavior is better than the uncoated sample. This behavior may be due to the introduction of copper oxide as modifier to the glass network modifier and subsequently Cu atoms will occupy the intersites thatdirectedthe formation of non-bridging oxygens (NBOs) and the structure opening as (BO₃) units is dominant and as a result the decrease in the volume occurred [43]. Opening the glass network gives the chance to the reaction with the surrounding ions that decreases the corrosion inhibition.

Table 3

The Corrosion parameters for Mild steel in 1.0 M HCl without (Blank) and with coating by different coats at room temperature.
Sample	b_a mV/dec	b_c mV/dec	E_corr, mV	I_corr, mA/cm²	Rp, Ω.cm²	IE, %
Blank	110.1	-132.4	-431.4	2.0316	12.28	--
PSA	73.0	-93.8	-429.6	0.1217	148.90	94.0
100	66.8	-80.1	-426.4	0.1098	150.90	94.6
101	90.4	-89.5	-425.0	0.2018	95.85	90.0
103	84.6	-102.5	-416.7	0.2587	70.78	87.3
105	76.8	-115.3	-406.8	0.2859	67.14	85.9

Electrochemical impedance is an electrochemical technique which is extensively used to evaluate the diffusion of the ions through coats, detect the flaws in coated materials as well as to determine the effectiveness of the coat [44–46].

A typical Nyquist plots for uncoated and coated mild steel after immersion for 5 min in 1.0 M HCl were shown in Fig. 8 (a) which showed one dispersed semicircle for the coated and uncoated sample. The diameter of the circle increases in case of coating mild steel indicating more resistant of the coated samples to the electrolyte attack than the uncoated sample.

The experimental impedance data fitted to the equivalent circuits shown in Fig. 8(b) which consists of the solution resistance (R_s) in series with the charge transfer resistance (R_ct) that is parallel to the constant phase element (CPE), Q, which includes two parameters Y_o (modulus of the CPE) and n (the phase shift deviation parameter). The phase constant impedance can be given by the following relation; [47, 48]

Z_CPE = 1/Y_o (j ω)ⁿ

Where ω is the angular frequency and j is the imaginary number. The fitted parameters for both uncoated and coated mild steel are given in Table 4. It was noticed that coating containing 100 represented the higher value of resistance which indicated lower penetration of electrolyte chloride ions to the coat and higher passivity of the mild steel surface. In addition, the value of n in case of 100 coat is near to 1 which indicating more homogeneity of the surface. As shown in the polarization results, all the coats can protect mild steel from attack with electrolyte ions by different degree.

Table 4

Equivalent circuit parameters for Mild steel uncoated and coated by different coats after steady state of immersion in 1.0 M HCl at room temperature.
Type of Coat	R_s (Ω)	R_ct (Ω cm²)	Q_ads
Type of Coat	R_s (Ω)	R_ct (Ω cm²)	Y (mΩ⁻¹cm⁻²)	n
Blank	2.69	7.86	2.1	0.72
PSA	3.07	15.78	52.0	0.90
100	3.05	48.51	423.0	0.96
101	3.25	18.25	312.0	0.83
103	2.83	16.17	309.0	0.90
105	2.26	13.87	889.0	0.78

Over 7 days, EIS were performed for mild steel coated with PSA/100 in 1.0 M HCl and a typical Nyquist plots are shown in Fig. 9 (a). As shown from the figure, the radius of the semicircle increased with time of immersion until reaching 120 min then a notable decrease was detected but the semicircle diameter after 7 days of immersion in HCl is still larger than the uncoated mild steel indicating passivation of the coat even after 7 days of immersion. The increase in the coat resistance all over the first 120 min indicates that the formed corrosion products due to the high attack of electrolyte ions can work also as barrier against attacking corrosive materials therefore the resistance increases.

Comparison of polarization curves of uncoated and coated mild steel after immersion in 1.0 M HCl for 7 days shows in Fig. 9(b), which indicated a shift of both the cathodic and anodic branches of Tafel curves to more noble values indicating passivation of mild steel due to coating even after long immersion. It was also observed that the corrosion current density decreased (Table 5).

The detected passivation data of the coated mild steel in aggressive acidic chloride solution from OCP, polarization and EIS measurements can be rendered to the duel effect of polymer and glass in the coat structure, revealing that the presence of glass grafted in the polymer PSA can help in improving the corrosion resistance of the coat

Table 5

The Corrosion parameters for Mild steel coated and uncoated by different coats at room temperature after 7 days of immersion in 1.0 M HCl.
Sample	b_a mV/dec	b_c mV/dec	E_corr, mV	I_corr, mA/cm²
uncoated	103.1	-98.2	-434.63	1.5700
PSA	89.3	-102.1	-473.93	0.5687
100	65.8	-118.9	-451.99	0.4862
101	84.0	-74.5	-422.17	0.6248
103	101.2	-143.5	-447.33	0.6679
105	105.7	-193.3	-407.51	0.7108

The polymer chain with borate glass chains may be chemically bonded via hydrogen bond besides the electrostatic attraction.
The increase of CuO contentof polymeric grafted glass composites leads to slightly The effectiveness of polymer glass composites as corrosion protection coatings for mild steel is reduced due to openings in the network structureof glass that leads to decrease the stability of the coat on the mild steel surface.
An increase in the inhibition efficiency of the PSA/100 coat with time during the first hours of immersion then it decreases but still more protected than the uncoated.

Author Contribution

M. A. Azooz , M. M. El-Deeb make introduction and experimentalA. M. Fathi , Emad H M Kamal make Tables and figresH. M. Abd El-Salam,M. S.Ibrahim make Results and Discussions

Acknowledgement

“This paper is based upon work supported by Science, Technology & Innovation Funding Authority (STDF) under grant”

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No competing interests reported.

material.docx

Fabrication and characterization of Polysulphanilic acid/Borate glass Composites as Anticorrosion Coat for Mild steel in Acidic medium

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Abstract

Figures

1. Introduction

2. Experimental