NEW BLACK-FILLED EPOXY COATINGS FOR REPAIRING

TRANSPORT

ISSN 1648-4142 / eISSN 1648-3480

2020 Volume 35 Issue 6: 679–690

https://doi.org/10.3846/transport.2020.14286

SURFACE OFEQUIPMENTOFMARINESHIPS

Andriy BUKETOV

, Serhiy SMETANKIN

, Pavlo MARUSCHAK

, Kyrylo YURENIN

Oleksandr SAPRONOV

, Viktor MATVYEYEV

, Abdellah MENOU

Dept of Transport Technologies, Kherson State Maritime Academy, Ukraine

Dept of Industrial Automation, Ternopil Ivan Pul’uj National Technical University, Ukraine

Moroccan Airports Authority, Mohammed V International Airport, Nouaceur, Casablanca, Morocco

Received 26 March 2020; revised 20 June 2020, 5 August 2020; accepted 9 August 2020

Abstract. e methods for ensuring long-term and safe operation of marine equipment due to comprehensive repair

technologies that use epoxy oligomers and new compositions based on them are developed. e inuence of temperature

and UltraSonic Treatment (UST) on the rheological properties of the pure epoxy matrix and compositions based on it is

explored. e compositions have dierent content of nanodispersed soot carbon black of brand PowCarbon 2419G (par-

ticle size of 24±2 nm). It is established that when nanoparticle soot (q= 0.10…15.00 pts wt) is introduced into the com-

position of the epoxy matrix treated with ultrasound, the viscosity of the composition increases gradually. Based on the

results obtained, temperature ranges are recommended, in which the viscosity of the studied compositions reaches optimal

technological parameters for the eective impregnation of threads, tows and various fabrics, and which provide for the ef-

fective application of the composition to the working surfaces of marine equipment. Technical recommendations are given

for applying the developed black-lled epoxy compositions to the working surfaces of parts, ship mechanisms and pipeline

systems of marine vessels.

Keywords: protective coating, application and inspection, nanodispersed soot, rheological behaviour, marine equipment.

*Corresponding author. E-mail: maruschak.tu.edu@gmail.com

Editor of the TRANSPORT– the manuscript was handled by one of the Associate Editors, who made all decisions related to the manuscript (including the choice of referees

and the ultimate decision on the revision and publishing).

is is an Open Access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/4.0/), which permits unre-

stricted use, distribution, and reproduction in any medium, provided the original author and source are credited.

Introduction

e globalization of international trade, in particular, the

free movement of goods is impossible without sea trans-

port with an enhanced operational reliability (Emi etal.

1993; Hellio, Yebra 2009). It is known that the technical

operation of marine vessels involves a number of techno-

logical processes (Soares etal. 2009; Abbas, Shaee 2020;

Gudze, Melchers 2008), such as technical use (ensuring

the vessel operation), maintenance (maintaining the ves-

sel in proper (working) condition), repair (restoration

of good technical condition). Each of these technologi-

cal processes ensures the reliable operation of the vessel

and requires development and improvement (Yamamoto,

Ikegami 1998).

Unfortunately, the existing methods of non-destructive

testing of the marine equipment do not allow for a full

control over the defect and damage accumulation process.

In particular, this applies to the early stage, when the iden-

tication and elimination of defects allows restoring the

full eciency of the mechanism (Emi etal. 1993; Davies

2016; Naja etal. 2019).

At present, Polymer-Composite Materials (PCMs) are

used for the repair and maintenance of marine equipment

(Naja etal. 2019; Selim etal. 2017). ey allow enhanc-

ing the durability of marine equipment and protecting the

working surfaces of marine equipment exposed to such

environmental factors as sea water, precipitation, solar ra-

diation, and a variety of mechanical loads during storms.

From the technological point of view, its main advantages

over other anticorrosive coatings include the hardening

speed, high adhesion and resistance to chemical and me-

chanical inuences. Polymer composites are easy to apply,

which allows you to quickly create an even, monolithic

coating (Mardare, Benea 2017).

One of the promising PCMs that quickly and e-

ciently protect the surfaces of marine equipment from

aggressive eects are the materials based on epoxy resins

680

A. Buketov et al. New black-lled epoxy coatings for repairing surface of equipment of marine ships

characterized by the enhanced mechanical, adhesive and

thermophysical properties, as well as low shrinkage dur-

ing curing. Examples for coating systems are given in the

Class Guideline DNVGL-CG-0288 (DNV GL 2017) and

may be modied as regards coating thickness and number

of coats, if relevant. e coating shall be epoxy or equiva-

lent, rendering adequate corrosion protection to the sur-

faces in question, considering the cargo type and mode of

operation of the ship (Summerscales 2014).

It is known that chemical or physical-chemical meth-

ods are the most eective ones for improving the prop-

erties of epoxy binders and PCMs (Davies 2016; Naja

etal. 2019). e properties of epoxy composites are also

modied by nanoparticles of various nature (Rubino etal.

2020; Mardare etal. 2016; Buketov etal. 2018; Sapronov

etal. 2019). In this case, one of the most important con-

ditions for the successful nanomodication of polymer

composites, in addition to the chemically active surface

of the particles, is their uniform distribution in the volume

of materials, which largely depends on the viscosity of the

polymer binder (Khalina etal. 2019). e core competen-

cy of the resulting coating is that even though no abrasion

resistance, strength or robustness of the coating is lost, the

particles can reversibly act as energy storage units, absorb-

ing the acute pressure of abrasive loads. e particles are

permanently bound to the resin binder polymers, due to

the binding moieties (Fu etal. 2019). ey act like nano-

springs in the coating. eir existence does not modify

the ability of the epoxy coating to adhere on the substrate.

e polymer planes and “inclusions” remain resistant to

impact or abrasion (Arabatzis etal. 2019), however, much

of the damaging energy is absorbed before the coating

cracks, akes or fails (Maruschak etal. 2012a).

A common drawback of epoxy binders is a fairly rigid

molecular structure that leads to an increase in viscos-

ity, which complicates the application of coatings to the

surface of the equipment. To solve this problem, various

diluents are used in the form of solvents and plasticiz-

ers, which are introduced into the polymer matrix in a

wide range of concentrations (Il’ina etal. 2019). A nega-

tive eect of such operation is the impairment of physical-

mechanical properties and signicant shrinkage of PCM

associated with loosening of the structure of the polymer

binder (Brusentseva etal. 2015; Buketov etal. 2019; Geng

etal. 2016). e Glass Transition Temperature (GTT) and

the strength of the PCM obtained are also lowered. In

turn, the use of solvents causes the formation of a large

number of pores and the appearance of residual stresses in

the volume of the composites. Another method for chang-

ing the viscosity of polymer systems is the targeted inu-

ence of energy elds during their formation. It is known

that UltraSonic Treatment (UST) and heating of polymer

mixtures leads to changes in a number of their properties,

including viscosity (Ganiev 2007; Sharma, Luzinov 2011;

Buketov etal. 2014). UST does not impair the physical-

mechanical and thermophysical properties of the compos-

ites obtained. Moreover, a decrease in the viscosity of the

compositions makes it possible to simplify the technologi-

cal process of applying coatings to the surface of marine

equipment. In this article, a number of approaches to the

development of this technique are proposed.

e time, during which the polymer binder retains

the ability to bind polymer compositions to solid sur-

faces (substrates) under the inuence of various harden-

ers, is one of the most important technological properties

of thermosetting oligomers. e time interval from the

preparation of the polymer binder to the moment it passes

into a system of innite viscosity, i.e., a gel (gel point) is

called as gelatinization (Mulder 1996). e optimization of

these conditions makes it possible to optimize the coating

process and improve its physical and mechanical proper-

ties (Buketov etal. 2016).

e purpose of this work was to ensure long-term and

safe operation of the marine equipment due to compre-

hensive repair technologies that use epoxy oligomers and

new compositions based on them.

1. Materials and methods of study

A correct and timely assessment of the material eective-

ness is only possible based on determining the economic

eciency of the technical decisions made. e economic

eect is divided into actual (obtained by saving produc-

tion resources) and conditional (cost reduction in the

future). e eectiveness of applying the developed poly-

mer materials based on epoxy resin (ED-20), PolyEthyl-

ene PolyAmine (PEPA) is due to the eective protection

of marine equipment. e epoxy oligomer ED-20 (GOST

10587-93 and standard ASTM D4762-08) was investigat-

ed. e characteristics of the binder are given in Table 1.

Nanodispersed soot carbon black of brand PowCarbon

2419G– Chemical Abstracts Service (CAS) No 1333-86-4,

European Inventory of Existing Chemical Substances (EI-

NECS) No 215-609-9– manufactured by Black Diamond

Material Science Co., Ltd. (China) was used as a ller. e

particle size of the powder was determined using electron

microscopy and is 24±2 nm. e characteristics of nano-

dispersed carbon black are given in Table 2.

Epoxy PCM was formed using the following technol-

ogy: preliminary dosing of epoxy resin ED-20, heating the

resin to the temperature T= 353±2K, and holding at this

temperature over the time period τ= 20±0.1 min.

Technical Nanodispersed Gas Soot (TNGS) is a hygro-

scopic material capable of absorbing moisture depending

on the particle size (Shaitanov etal. 2013), the presence

of impurities and storage conditions. is leads to clump-

ing (sticking) of the TNGS powder and complicates its

introduction and dispersion in the polymer medium. In

addition, the powder was dried in a mue furnace heated

to the temperature Т= 383±2 K and held at this tempera-

ture over the time period τ= 60±0.1 min. Soot was then

dosed and introduced into the epoxy oligomer. e ller

was introduced in the amount from 0.10 to 25.00 pts wt

Transport, 2020, 35(6): 679–690

681

per 100 pts wt of epoxy oligomer ED-20 (hereinaer, val-

ues in parts by weight are given per 100 pts wt of epoxy

oligomer ED-20). en, hydrodynamic combination of

TNGS and epoxy oligomer ED-20 particles was applied

using UST over the time period τ = (1.5...2.0)±0.1 min

in similar temperature conditions. Aer that, the nished

compositions were poured into a Grin glass (according

to ISO 7056:1981) in order to conduct further experi-

ments.

e rheological properties of polymer compositions

were determined using a BROOKFIELD DV-II+Pro pro-

grammable rotational viscometer (Malkin, Isayev 2012)

according to GOST 25271-93, as well as according to

ISO2555:89. e principle of operation of the device is

based on the rotation of the measuring spindle immersed

in the test uid by means of a calibration coil spring. Each

spindle is characterized by two constants, which are used

to calculate viscosity, shear stress and shear rate. A stand-

ard set of resin viscosity spindles (6 pcs) was used. To ob-

tain the most correct results, the control of the experiment

and data collection was carried out automatically using

a computer with Brookeld Rheocalc32 soware (https://

www.brookeldengineering.com/products/soware/rheoc-

alct) installed. e average dynamic viscosity η was de-

termined in the temperature range of 25…90 °C at the

same spindle rotation speed, provided that the moment

was counted in the range of 10...95%. e thermostat-

ing time of the specimens was 15±0.2 min. e tempera-

ture values were displayed using an RTD temperature

sensor (from the instrument kit), the error of which is

±1 °C (the latter can operate in the temperature range

of–100…+149 °C). e temperature in the room at the

time of the experiment was 23±2 °C, and humidity was

64±2%. e accuracy of viscosity measurements is ±1.0%,

and the repeatability of experimental data is ±0.2%.

2. Research results and their discussion

At the initial stage, the inuence of UST and temperature

on the rheological properties of pure epoxy resin, UST-

modied resin, and compositions based on it with dier-

ent concentrations of nanodispersed soot was analysed.

When the temperature of epoxy oligomers and composi-

tions based on them with various degrees of ller con-

centration raised up to Т= 310 K, a sharp decrease in the

mean dynamic viscosity η was found in all the curves,

Figure 1. e characteristic kinks on the graphs indicate a

change in the phase state of the compositions. With fur-

ther heating of the test specimens, a monotonic decrease

in the mean dynamic viscosity was recorded, which indi-

cates the absence of phase transitions in the temperature

range (Т= 320...360 K).

Changes in dynamic viscosity η under the inuence

of temperature can be traced in greater detail taking into

account the data of Table 3. By comparing the proper-

ties of epoxy resin ED-20 in the initial state and aer the

UST according to the above method, it was found that the

UST changes the rheological properties of the oligomer.

In the range of elevated temperatures Т = 321...361 K,

the dynamic viscosity of the sonicated resin slightly de-

creased (∆η= 1.25...6.25mPa⋅s). At the same time, when

the epoxy oligomer is cooled (in the temperature range

Т= 296…316 K), the dierence between the viscosity of

the sonicated and non-sonicated resin increases: ∆η =

57.5...1462.5 mPa⋅s. In our opinion, the results obtained

are associated with high-intensity pulsed hydrodynamic

Table 1. Characteristics of nanodispersed soot carbon black

of brand PowCarbon 2419G

Characteristic

Indicator from the

developer company

Study method

Mean particle

size [nm]

24±2 electron microscopy

Specic surface

area [m

/g]

145±20 electron microscopy

Oil absorption

[cc/100 g]

85±5 GB/T 7046-2003

pH 4.9±1 GB/T 7045-2003

Staining power

[%]

≥127 GB/T 7050-2003

Volatile matter

content [%]

2.3±0.2 GB/T 7047-2006

Density [g/L] 180±20 GB/T 14853.1-2002

Physical form powder without magnication

Table 2. Characteristics of epoxy oligomer ED-20

Characteristics Value

Molecular mass M

340

Content of epoxy groups

[%]

20.0…22.5

Content of hydroxyl groups

[%]

1.25

Viscosity η [Pa·s] 13…20

Density ρ [g/cm

] 1.160

10000

15000

20000

25000

30000

35000

5000

h [mPa·s]

290 300 310 320 330 340 350

360

370

T [K]

ED-20

ED-20 + UP

ED-20 + UP + soot (q = 0.10 pts wt)

ED-20 + UP + soot (q = 1.00 pts wt)

ED-20 + UP + soot (q = 5.00 pts wt)

ED-20 + UP + soot (q = 10.00 pts wt)

ED-20 + UP + soot (q = l5.00 pts wt)

Figure 1. e eect of temperature T on the mean dynamic

viscosity η of the sonicated and non-sonicated epoxy resin

ED-20 and compositions with nanodispersed soot

682

A. Buketov et al. New black-lled epoxy coatings for repairing surface of equipment of marine ships

disturbances caused by the collapse of rapidly growing

vapour-gas bubbles in the epoxy oligomer volume. Appar-

ently, the shock waves formed upon collapse at the stage of

developed cavitation (Brennen 2013) are the main driving

factor that leads to the destruction of hydrogen bonds of

polymer macromolecules (Sharma, Luzinov 2011; Huang

etal. 2002). At the same time, the С–С, С=С, С=О bonds,

as well as other types of bonds between individual seg-

ments and groups of the main chains of macromolecules,

fragment hydrogen bonds while being destroyed them-

selves. is leads to changes in the physical-chemical

properties of the epoxy resin, in particular, a decrease in

its viscosity.

Further experiments showed that when the nanodis-

persed carbon black in the amount q=0.10…15.00 pts wt

is introduced into the sonicated epoxy resin, the viscosity

of the compositions increases gradually. It should be noted

that the tendency with a phase transition in the region Т=

310 K is also preserved. As is seen from the data displayed

in Table3, the dynamic viscosity of the compositions in-

creases by 9...15% compared with the oligomer even at min-

imum concentrations of the introduced ller (0.10 pts wt)

in the range of elevated temperatures Т= 321…361 K. In

the temperature range that precedes the phase transition

(Т = 296…316 K), an increase in viscosity was 7...10%.

e experimental results for a composition with the nano-

dispersed soot content q= 10.00 pts wt indicate that in the

temperature range of 321…361 K, the viscosity increases

by 92...794%, and in the temperature range of 296…316 K,

it increases by 52...108%. e maximum eect of the ller

on the rheological properties of the epoxy compositions

was observed aer a phase transition at high tempera-

tures. Moreover, the more highly lled the composition,

the more pronounced this eect. An increase in the ller

concentration enhances the viscosity of epoxy composi-

tions, Figure 1, Table 3, which is possibly associated with

an increase in the hydrodynamic and thermodynamic in-

teractions between the oligomer and nanoller molecules.

e agglomeration of nanoparticles in the volume of the

epoxy oligomer due to their highly developed surface is

also possible, which leads to a limited mobility of macro-

chains of epoxy resin.

A number of rheological studies made it possible to

evaluate the processes that occur during the formation of

nanocompositions and to develop technological recom-

mendations for their application on the surface of marine

equipment. It is known that in order to obtain a high-

quality protective layer by the “wet winding” method, and

to achieve a good impregnation of threads, bundles and

various fabrics, the viscosity of the binder should not ex-

ceed 300...500 mPa⋅s (Pahomov etal. 2016). In the paint

and varnish industry, there is an empirical rule, according

to which the viscosity of about 100...500 mPa⋅s provides

acceptable spraying, brushing or applying of a binder to

work surfaces. For the epoxy resin (ED+ UST) and the

composition (ED+ UST+ carbon black, q= 0.10 pts wt),

such viscosity values are attained in the temperature range

of 321...361 K. For the composition (ED+ UST + car-

bon black, q= 1.00 pts wt)– in the temperature range of

326...361 K, and for the composition (ED+ UST+ car-

bon black, q= 5.00 pts wt)– in the temperature range of

331...361 K. At the same time, black-lled compositions

with nanoparticles content q= 10.00 pts wt can be used for

the “impregnation work” when heated to 361 K. At the same

time, compositions with the ller content q ≥ 15.00 pts wt

are unsuitable for such application.

Table 3. Viscosity values of the epoxy composition based on epoxy resin ED-20 at various temperatures and concentrations of the ller

Т [K]

Viscosity values η [mPa⋅s]

ED-20 ED-20+ UST

ED-20+ UST+

carbon black

(q= 0.10 pts wt)

ED-20+ UST+

carbon black

(q= 1.00 pts wt)

ED-20+ UST+

carbon black

(q= 5.00 pts wt)

ED-20+ UST+

carbon black

(q= 10.00 pts wt)

ED-20+ UST+

carbon black

(q= 15.00 pts wt)

361 56.25 56.25 61.25 68.75 173.75 503.00 1825.0

356 63.75 62.50 70.00 78.75 178.75 508.00 1820.0

351 75.00 72.50 82.50 93.75 188.75 510.00 1800.0

346 90.00 87.50 100.00 113.75 206.25 511.25 1780.0

341 113.75 110.00 126.25 143.75 232.50 515.00 1760.0

336 145.00 146.25 166.25 188.75 271.25 533.75 1760.0

331 202.50 196.25 228.75 257.50 337.50 583.75 1780.0

326 295.00 291.25 335.00 373.75 557.50 673.75 1880.0

321 451.25 446.25 513.75 566.25 826.25 855.0 2125.0

316 722.50 665.00 710.00 745.00 1070.0 1340.0 2645.0

311 1292.50 1197.5 1292.5 1392.5 1825.0 1820.0 3945.0

306 1945.00 1860.0 2050.0 2465.0 2700.0 3555.0 7125.0

301 4515.00 4145.0 4565.0 4590.0 6850.0 7700.0 16150.0

296 11462.5 10000.0 10000.0 10550.0 14300.0 20800.0 31450.0

Transport, 2020, 35(6): 679–690

683

e curves showing the inuence of test temperature

on the viscosity of PCM in the coordinates (lg η– 1/T)

are analysed, Figure 2. In this case, the activation energy

of the viscous ow was determined for each temperature

range separately, i.e., we can talk about the “apparent”

or “instantaneous” activation energy of a viscous ow

(Shaitanov etal. 2013).

e activation energy is known to be inuenced by

the chain microstructure and its side branches, which de-

termines the exibility and interaction between the mol-

ecules of polymer compositions in the so-called transition

state, in which the destruction and creation of bonds are

balanced (Anpilogova etal. 2016; Ermahanova, Ismailov

2018). A decrease in the activation energy indicates the

transformation of the initial bonds in epoxy compositions

and the formation of new ones, which is also actively pro-

moted by the introduction of nanoadditives. e apparent

activation energy DE

[kJ/mol] of the viscous ow was de-

termined by the formula:

( )

2.303 ln

R TT



⋅ ⋅ ⋅⋅





−

where: Ris the universal gas constant, R=8.314 J/(mol⋅K);

, η

are the experimental values of dynamic viscosity

[Pa⋅s]; T

, T

are the temperature values, at which viscosity

is determined at a constant shear rate [K].

e calculation results indicate that the rheological

behaviour of PCM is determined not only by the modi-

cation of the oligomer, but also by temperature and the

amount of the ller introduced, Table 4.

As is seen from Table 4, the lowest activation energy of

the viscous ow is in the upper temperature range, which

indicates an active formation of a new composition struc-

ture (the interaction between macromolecules, segments,

side groups of the oligomer and additives wetted during

the introduction of nanoparticles into the composition).

Further analysis of the data obtained suggests that a de-

crease in temperature leads to a natural increase in DE

especially for black-lled compositions. is, in turn, indi-

cates that agglomerates of carbon black nanoparticles and

macrochains formed in heterogeneous centers of epoxy

compositions have a structure that is more resistant to

thermosuctuation decay. e destruction and restoration

of such structures requires more thermal energy.

Another important step in optimizing the technol-

ogy of applying PCM to the surface of marine equipment

is the stage of curing. It is known that aer mixing with

the hardener, this process goes through three stages, i.e.,

the formation of a liquid, gel and solid phases (Hou etal.

2013) (Figure 3). e rst and second stages of PCM

polymerization are most important for the formation of

high-quality coatings. ey determine the time frame for

the transition from liquid to gel– gelatinization (working

time). Within this period of time, the material retains op-

timal rheological properties for the eective completion of

all technological operations of its formation. At the end of

the second and especially the third stage of PCM curing,

the viscosity of the compositions increases signicantly.

ey become less uid, which in most cases makes them

unsuitable for further application and repair (Figure 4).

Figure 2. Dependence of viscosity of the sonicated and

non-sonicated epoxy resin ED-20 and compositions with

nanodispersed soot on the test temperature

1.50

2.00

2.50

3.00

3.50

4.00

4.50

lg h

0.00270 0.00280 0.00290 0.00300 0.00310 0.00320 0.00330 0.00340

–1

1/T [K ]

ED-20

ED-20 + UP

ED-20 + UP + soot (q = 0.10 pts wt)

ED-20 + UP + soot (q = 1.00 pts wt)

ED-20 + UP + soot (q = 5.00 pts wt)

ED-20 + UP + soot (q = 10.00 pts wt)

ED-20 + UP + soot (q = l5.00 pts wt)

Table 4. Values of the apparent activation energy of the viscous ow of compositions based on ED-20 resin at various ller concentrations

Т [K]

Apparent activation energy of the viscous ow DE

[kJ/mol]

ED-20 ED-20+ UST

ED-20+ UST+

carbon black

(q= 0.10 pts wt)

ED-20+ UST+

carbon black

(q= 1.00 pts wt)

ED-20+ UST+

carbon black

(q= 5.00 pts wt)

ED-20+ UST+

carbon black (q=

10.00 pts wt)

ED-20+ UST+

carbon black

(q= 15.00 pts wt)

361…351 30.30 26.73 31.37 32.66 8.72 1.46 1.45

351…341

41.44 41.47 42.33 42.52 20.74 0.97 2.24

341…331

54.11 54.31 55.76 54.69 34.96 11.76 1.06

331…321

70.76 72.55 71.45 69.59 79.07 33.70 15.64

321…311

87.32 81.91 76.55 74.66 65.75 62.69 51.33

311…301

97.32 96.61 98.18 92.80 102.91 112.22 109.66

684

A. Buketov et al. New black-lled epoxy coatings for repairing surface of equipment of marine ships

e dependences of the gelation time on the content of

nanodispersed soot were determined experimentally. e

curing rate of polymer compositions increases signicant-

ly with an increase in temperature (in this case, the level

of residual stress and shrinkage increases, which aects

the physical-mechanical properties of the nal product),

due to which studies were carried out at a temperature of

23±2°C and an ambient humidity of 64±2%.

e main patterns of the torque variation in the pro-

cess of curing of the epoxy resin were established as op-

posed to the content of nanodispersed soot (Figure 5).

When PEPA hardener was introduced into the epoxy oli-

gomer in the amount q= 10.00 pts wt, the torque T

[%]

increased monotonously over 49 min, aer which it in-

creased sharply, forming a characteristic kink on the

curve. is indicates the beginning of the active formation

of chemical bonds between macromolecular chains and

their branches, which facilitates the formation of a three-

dimensional polymer network with an enhanced density

(Sapronov etal. 2020). A similar eect was observed dur-

ing the curing of epoxy compositions with the content of

nanoparticles from 0.10 to 1.00 pts wt.

It should be noted that even a slight increase in the

ller content (q= 0.10 pts wt) aects the nal stage of

the PCM gelatinization appreciably. At the same time, an

increase in the ller content to q= 1.00 pts wt leads to a

slowdown of the curing process compared to the original

ED-20. Further introduction of the ller in the amount

q= 5.00...15.00 pts wt leads to a signicant reduction in

gelatinization time and accelerates the curing of PCM. Ac-

cording to the authors, such dierence in the kinetics of

the polymerization reaction of highly lled nanocompos-

ites primarily indicates a signicant interaction between

nanoparticles and epoxy resin. An increase in the content

of nanoadditives leads, rst of all, to an increase in the

polymer network density. is causes the appearance of

additional friction forces when mixing the consistency,

during which energy is released, which transforms into

heat, thus accelerating the curing of PCM.

erefore, we studied the variation of the self-heating

temperature of epoxy compositions depending on the

intensity of the chemical reaction in the presence of na-

nodispersed soot with a hardener. e maximum tem-

perature of the exothermic reaction was observed in the

composition with the highest content of additive (q =

15.00 pts wt) (Figure 6). At the same time, PCM with

the nanodispersed soot content q= 1.00...10.00 pts wt is

characterized by a lower exothermic eect, as compared

to the materials based on the initial PCM (ED-20) and

Figure 3. Curing stages of epoxy oligomer (Hou etal. 2013)

Cure time after mixing

Open time Initial cure Final cure

Epoxy temperature

Liquid Gel Solid

I II III

Figure 4. Images of epoxy oligomer ED-20 with PEPA hardener

(a) and epoxy oligomer ED-20 with PEPA hardener and carbon

nanosoot (b); viscosity of the consistencies analysed ≥47.65 Pa⋅s

and 190.2 Pa⋅s, respectively

Figure 5. Torque variation in the process of curing of the epoxy

resin with dierent concentrations of nanodispersed soot

ED-20 (without additives)

ED-20 + carbon black in the amount of 15.00 pts wt

0:00:00 0:14:24 0:28:48 0:43:12

0:57:36

1:12:00

1:26:24

t [min]

T [%]

100

ED-20; ED-20 + UP

ED-20 + UP + soot (q = 0.10 pts wt)

ED-20 + UP + soot (q = 1.00 pts wt)

ED-20 + UP + soot (q = 5.00 pts wt)

ED-20 + UP + soot (q = 10.00 pts wt)

ED-20 + UP + soot (q = l5.00 pts wt)

Transport, 2020, 35(6): 679–690

685

PCM with a minimal content of nanoparticles (q= 0.10

pts wt). is means that additional dissipation of thermal

energy occurs in black-lled composites. us, the best

properties were obtained for an epoxy oligomer with the

gas soot content q= 1.00...5.00 pts wt, which is conrmed

by the dependence of the survivability time on the begin-

ning of PCM gelatinization, Figure 6. In this case, the low-

est exothermic eect among the PCMs tested, which was

revealed in the process of curing of the compositions (Fig-

ure 6, curves ED-20+ UST+ carbon black, q= 1.00...5.00

pts wt), should be noted. A more uniform character and

low exothermic eect of the curing reaction of the compo-

sitions should lead to the formation of a less defective and

stressed structure of the PCMs obtained. Obviously, this

case is characterized by the most active relaxation pro-

cesses during the polymerization of compositions.

e above results of investigations into the rheologi-

cal properties of epoxy composites, as well as features of

their curing, are a prerequisite for the development of

engineering methods for applying them to the surface of

ship mechanisms in order to eliminate defects.

3. Engineering use of the developed coatings

for the repair of ship mechanisms

Novel surface modication and coating techniques need

to be developed in order to successfully translate these

coatings toward commercial (large‐scale) applications.

Every day, coatings with enhanced performances and new

properties are being designed and demonstrated, but they

never nd their way outside the lab (Maan etal. 2020).

Combining simple coating techniques with a high cor-

rosion durability and crosslinkers or catch‐bonds (to en-

hance mechanical stability), could result in technologically

mature coatings with large‐scale applicability.

3.1. Properties of the developed

and known protective coatings

In this section, the authors did not consider the corrosion

types and did not make a detailed description of surface

preparation methods and surface quality requirements,

since these features are described in new recommenda-

tions, for example, in ABS (2017) and Vincent (2012),

and are relevant both for the existing and new coatings.

e basic technological operations for applying coatings

have been described. e performance check and trou-

bleshooting of marine equipment were standardized and

performed in accordance with RD 31.21.30-97. Technical

requirements for cleaning and surface preparation opera-

tions were carried out in accordance with ASTM D2093-

03(2017); ASTM D2651-01(2016); BS 7079:2009; ISO

17212:2004.

e developed PCMs were used for the repair of

equipment, mechanisms and systems of a marine vessel,

such as:

– pipeline systems characterized by corrosion damage

(Figures 7, 8), due to which the pipe wall becomes

thinner and the strength of the system decreases in

places of localization of corrosion;

– deck mechanisms (cargo devices)– during storms,

critical mechanical stresses arise, which lead to

breakdowns of the above-described elements and

structures of the vessel.

e use of the developed materials with improved

physical and mechanical characteristics (Table 5) will ex-

tend time periods between repairs and protect the surface

of these systems from corrosion more eectively (Hou

etal. 2013; Mouritz etal. 2001; Alam etal. 2013; López-

Ortega etal. 2019).

3.2. Repair of the hydraulic drive of the control

system for closing/opening the lids of holds on

SEASPAN LUMAKO 4500 TEU, ME MAN B&W

container ship

e developed PCMs and methods of their application

were tested on the container ship SEASPAN LUMAKO

4500 TEU, ME MAN B&W with a summer deadweight

of 50245 tons (Figure 7) in order to restore the surface

and improve the anticorrosion properties of the hydraulic

actuator of the control system for closing/opening the lids

of holds (Figure8, position 1). is system is used to seal

open spaces, thus ensuring safety of the transported car-

go, and is an important element of the ship’s unsinkability

system, and also makes it possible to quickly provide for

transhipment operations. is emphasizes the importance

of the above-described element of the ship’s hydraulic

drive and the need for its high-quality maintenance in a

constant working condition.

Figure 6. Torque variation relative to the temperature

of exoeect during the curing of epoxy composites with

dierent concentrations of nanodispersed soot

T [K]

0 10 20 30 40 50

70 80 90

100

T [%]

294

296

298

300

302

304

306

308

ED-20; ED-20 + UP

ED-20 + UP + soot (q = 0.10 pts wt)

ED-20 + UP + soot (q = 1.00 pts wt)

ED-20 + UP + soot (q = 5.00 pts wt)

ED-20 + UP + soot (q = 10.00 pts wt)

ED-20 + UP + soot (q = l5.00 pts wt)

686

A. Buketov et al. New black-lled epoxy coatings for repairing surface of equipment of marine ships

e surface was restored using black-lled epoxy com-

posite coatings (ED+ UST+ carbon black, q= 1.00...5.00

pts wt) (Figure 9). To apply the binder to the damaged sur-

face more eciently and quickly, the mechanized method

is used with help of pneumatic spray guns or airless spray

guns. To ensure the correct work of the above equipment

(the viscosity of the binder should not exceed 500 mPa⋅s),

as well as uniform spraying of the PC with a thickness of

0.1...0.3mm, the composite must be preheated to a temper-

ature of 326...361 K and 331...361 K, respectively (Table 3).

A PC that consists of berglass impregnated with the de-

veloped polymer binder was also formed on the surface

of the low-pressure valves (Figure 8, position 2) of this

system (Figure 9).

3.3. Repair of the outboard water pipe

of the cooling LT contour of container

ship MERWE TRADER

Damage to the outboard water pipe of the cooling (LT)

contour was detected. is important line ensures the sup-

ply of liquid to the freshwater cooler and further cool-

ing of the ship’s power plant. e resulting damage, in

our opinion, is due to cyclic loads, temperature changes,

mechanical damage during operation, as well as the cor-

rosive eect of the medium (Maruschak et al. 2012b).

Repair of permanent type was carried out according to

the “wet winding” technique (Figure10). e coating was

applied manually using hair brushes. For a more eec-

tive impregnation of reinforcing bers, the viscosity of the

developed compositions did not exceed 300...500 mPa⋅s.

Recommended values for the compositions ED+ UST+

carbon black, q= 1.00...5.00 pts wt were attained by pre-

heating the binder to a temperature of 331...361 K (Ta-

ble3). Similar corrosion damage was detected on the side

wall of the ange seat of the freshwater cooler of the LT

contour (Figure 11, position 1), which serves to cool aux-

iliary mechanisms.

e side wall of the freshwater cooler (Figure 11, posi-

tion 1) was restored by using a composition ED+ UST+

carbon black q= 1.00...5.00 pts wt. e restoration fol-

Table 5. Comparison of properties of the developed and known Protective Coatings (PC)

Indicator PC 1 PC 2 PC 3 PC 4 PC 5

Ultimate bending stresses σ

bend

[MPa] 73…75 58.6 34…36 65…68 24…32

Modulus of elasticity E [GPa] 2.1 1.5…1.8 2.6 2.2 1.8…2.0

Impact toughness W [J/cm

] 0.9…1.0 0.7…0.8 0.2…0.5 0.4…0.9 0.1…0.4

Film thickness t

[µm] 0.1…0.2 0.1…0.3 0.1…0.2 0.1…0.3 0.2…0.5

Total polymerization time t

[h] 72 72±3 168 124 92

Covering cost c

[$/kg] 6.1 6.3 12.4 10.2 9.6

Notes: PC 1– the developed nanocomposite coating with the NS content q= 1.00 pts wt;

PC 2– the developed nanocomposite coating with the NS content q=5.00pts wt;

PC 3– a coating developed by Kronocoat Universal (UK);

PC 4– a coating developed by Marine Service Jaroszewicz s.c. (Poland);

PC 5– a coating developed by ordon Bearings Inc. (Canada).

Figure 7. Container ship SEASPAN LUMAKO with the

deadweight of 50245 tons (photo by Johnny Verhulst,

https://www.marinetrac.com)

Figure 8. Types of damage hydraulic system for open/ close the

cover for cargo holds on a container ship SEASPAN LUMAKO:

1– damage to the surface of the pipeline hydraulic actuator;

2– damage to the containment and surface low pressure line

Transport, 2020, 35(6): 679–690

687

lowed the preliminary cleaning with a sandblasting appa-

ratus and degreasing of the wall surface, aer which a re-

storing layer of binder was applied to the prepared surface

without heating (ASTM D2093-03(2017); ASTM D2651-

01(2016); BS 7079:2009; ISO 17212:2004). is procedure

was followed because a composite with a reduced viscosity

can drain, forming an uneven layer of PC on the inner

surface of the wall.

A variant of restoration and repair is proposed, which

is designed for structural elements of the ship crane shown

in Figure 12.

Mounting techniques for slewing bearings are shown

in Figure 13 A-1 and A-2. Since the PCM is used during

installation works (Figure 13, A-2), the connected surfaces

t well enough and are regulated by sliding on a polymer

binder, the remains of which are removed from the sides

of the connected surfaces. is accounts for signicant la-

bour savings during tting of parts, and also provides for

corrosion protection of the internal surfaces of the con-

nected xtures.

us, the basic technological methods for applying

the developed PC to marine structures and mechanisms

are described. When the binder preparation conditions

(heating to the desired viscosity) are observed, it can be

applied mechanically using pneumatic spray guns and air-

less sprayers. is makes it possible to evenly apply the de-

veloped coatings of any thickness (including 0.1...0.3 mm)

to signicantly larger surfaces, both at and rough, with

corrosive cavities and other types of damage. e recom-

mended temperature-time conditions for heat treatment

of the developed composites are shown in Figure 13.

If the heat treatment process is not used, the pre-

liminary polymerization of the adhesive layer is carried

out at a temperature Т= 293...323 K over a time period

τ = 100...120 min, which provides for a high degree of

crosslinking of macromolecules with the formation of a

spatial grid. For the relaxation of residual stresses and im-

provement of service characteristics, the total polymeriza-

tion time is 72 h.

Figure 9. Repair pipe SW (sea water) line for cooling LT (low temperature) contour by comp. materials as Wet Wrap technology of

container ship MERWE TRADER (in this case, berglass impregnated with compositions based on modied epoxy resins was used)

a) c)b)

Figure 10. Container ship MERWE TRADER with the summer

DeadWeight Tonnage (DWT) of 11842 tons

Figure 11. Seat of the ange of the freshwater cooler of the LT

contour for cooling auxiliary mechanisms on a container ship

MERWE TRADER (position 1– side wall)

Figure 12. Use of epoxy composites for the maintaining the

cargo crane on ship columns– simplied diagram of a slewing

crane: A-1– mounting of a rotary bearing in the traditional

way; A-2– bearing mount using a thin layer of epoxy

A–1 A–2

688

A. Buketov et al. New black-lled epoxy coatings for repairing surface of equipment of marine ships

Conclusions

Based on experimental studies, new black-lled epoxy

coatings for the repair of surfaces of marine equipment

are developed, and the conditions for their application

are substantiated based on comprehensive studies of their

rheological properties.

It is found that the viscosity of the sonicated epoxy

matrix is not much lower than that of the initial epoxy

oligomer ED-20. In the range of elevated temperatures

(Т= 321…361 K), the dynamic viscosity ∆η of the soni-

cated resin slightly decreases from 1.25 to 6.25 mPa⋅s. At

the same time, when the epoxy oligomer is cooled, the

dierence between the sonicated and non-sonicated resin

increases signicantly and is ∆η= 57.5...1462.5 mPa⋅s in

the temperature range Т= 296…316 K.

When nanodispersed soot in the amount q =

0.10…15.00 pts wt is introduced into the sonicated epoxy

resin, the viscosity of the composition increases gradually.

It should be noted that with minimum concentrations of

the introduced ller (0.10 pts wt) in the range of elevat-

ed temperatures Т= 321…361 K, the dynamic viscosity

of the composition increases signicantly (by 9...15%)

compared to the oligomer. At the same time, in the tem-

perature range that precedes the phase transition (Т =

296…316 K), an increase in viscosity was 7...10%. e ex-

perimental results obtained for the composition with the

nanodispersed soot content q= 10.00 pts wt demonstrate

that in the temperature range of 321…361K, the viscosity

increases from 92 to 794%, and in the temperature range

of 296…316 K, an increase is 52...108%. Based on the data

obtained, we can state that the rheological properties of

epoxy compositions are inuenced by the ller to a greater

extent aer a phase transition at high temperatures.

Temperature ranges are recommended, in which the

viscosity of the studied compositions reaches the accept-

able technological parameters for the eective impregna-

tion of threads, tows and fabrics, as well as for applying

the compositions to the working surfaces of objects under

repair. For the epoxy resin (ED+ UST) and the composi-

tion (ED+ UST+ carbon black, q= 0.10 pts wt), such vis-

cosity values are attained at a temperature of 321...361 K,

for the composition (ED + UST + carbon black, q =

1.00 pts wt) – at a temperature range of 326... 61 K,

and for the composition (ED + UST + carbon black,

q= 5.00ptswt)– at a temperature range of 331...361 K.

Black-lled compositions (q= 10.00 pts wt) can be used

for the “impregnation works” when heated to 361 K. At

the same time, compositions with a higher ller content

(q= 15.00pts wt or more) are not suitable for the above-

mentioned works.

e dependences of the gelation time on the content

of nanodispersed carbon black in the developed PCMs

are established. e most pronounced eect on the com-

position curing was obtained with the ller content q=

1.00...5.00 pts wt, which provides for a more uniform

character of the time dependence on the gelation process.

In particular, at a temperature of 23±2ºС and an ambient

humidity of 64±2%, the survivability time for composi-

tions with the nanodispersed soot content q= 1.00 pts wt

is 47±1 min, and when the content of nanoadditives is q=

5.00 pts wt, survivability decreases to 29±1 min.

Variation of the self-heating temperature of the epoxy

binder depending on the intensity of chemical reactions

in the volume of the studied compositions was studied. In

the process of curing, the smallest exothermic eect was

observed in the compositions with the additive content

q= 1.00 pts wt (Т= 296...302.1 K) and 5.00 pts wt (Т=

296...301.3 K), respectively. is suggests that the mini-

mum exothermic eect and a more uniform nature of the

curing reaction should lead to the formation of a less de-

fective and stressed structure of the obtained material. In

this case, relaxation processes occur with maximum speed

during the polymerization of compositions.

e results obtained made it possible to test the coat-

ing technique on a number of marine mechanisms, which

made it possible to carry out in-line repairs and restore the

performance of marine equipment.

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