Nativa, Sinop, v. 10, n. 2, p. 277-282, 2022.
Pesquisas Agrárias e Ambientais
DOI: https://doi.org/10.31413/nativa.v10i2.13665 ISSN: 2318-7670
Effect of acetylation on technological characteristics of
Jacaranda copaia
wood: Part 1 – Physical and mechanical properties
Andressa Midori Yamauchi BAUFLEUR1, Diego Martins STANGERLIN1,2*,
Matheus Rafael FERREIRA2, Elisangela PARIZ2, Francisco RODOLFO JUNIOR3,
Edgley Alves de Oliveira PAULA4, Rafael Rodolfo de MELO4
1PostGraduated Program in Forest and Environmental Sciences, Federal University of Mato Grosso, Cuiabá, MT, Brazil.
2Institute of Agricultural and Environmental Sciences, Federal University of Mato Grosso, Sinop, MT, Brazil.
3Federal University of Piauí, Profa. Cinobelina Elvas Campus, Bom Jesus, PI, Brazil.
4Federal Rural University of the Semi-arid Region, Mossoró, RN, Brazil.
*E-mail: diego_stangerlin@yahoo.com.br
(ORCID: 0000-0003-2318-2428; 0000-0003-4336-6793; 0000-0002-3395-2142; 0000-0002-8009-9789;
0000-0001-9173-9748; 0000-0002-0258-3209; 0000-0001-6846-2496)
Received on 02/09/2022; Accepted on 06/15/2022; Published on 07/22/2022.
ABSTRACT: The objective of this work was to evaluate the effect of acetylation on the technological
characteristics of Jacaranda copaia (Aubl.) D. Don. wood. Physical (apparent and basic densities, water
absorption, and thickness swelling) and mechanical (Rockwell hardness) properties were evaluated. Wood
acetylation was carried out by immersion of samples in acetic anhydride; five treatments were evaluated: control
(no acetylation), acetylation for 2 hours, acetylation for 4 hours, acetylation for 6 hours, and acetylation for 8
hours. All reactions were carried out at a constant temperature of 90 °C. The results show that the 8-hour
acetylation treatment presented the highest weight gain (21.62%). This treatment also presented the lowest
water absorption (119.55%) and the highest Rockwell hardness (24.78 HRL). In general, the acetylation
treatment resulted in interesting improvements in wood’s physical and mechanical properties.
Keywords: chemical modification; dimensional stability; hardness.
Efeito da acetilação nas características tecnológicas da madeira
de
Jacaranda copaia
: Parte 1 – propriedades físicas e mecânicas
RESUMO: O trabalho teve como objetivo avaliar a eficiência da acetilação para madeira de Jacaranda copaia
(Aubl.) D. Don. em suas características tecnológicas. Para isso, foram avaliadas propriedades físicas (densidade
aparente e básica, absorção em água e inchamento em espessura) e a mecânica (dureza Rockwell). A acetilação
da madeira foi realizada mediante imersão de amostras em anidrido acético, sendo avaliados cinco tratamentos:
controle (não acetiladas), acetilação por 2 h, acetilação por 4 h, acetilação por 6 h e acetilação por 8 h. Todas as
reações realizadas com a temperatura constante de 90 °C. Os resultados mostram que o maior ganho de massa
foi apresentado pelo tratamento de acetilação durante 8 horas, como o valor de 21,62%. O tratamento também
apresentou o menor valor de absorção de água, sendo 119,55%, e o maior valor para dureza Rockwell, sendo
24,78 HRL. De modo geral, o tratamento de acetilação promoveu melhorias interessantes nas propriedades
físicas e mecânicas da madeira.
Palavras-chave: modificação química; estabilidade dimensional; dureza.
1. INTRODUCTION
Wood is a natural material from renewable sources which
has a high demand for applications in construction due to its
mechanical properties (BECK et al., 2018). According to
Digaitis et al. (2021), wood has been considered worldwide
as one of the most important materials for sustainable
transition.
According to Makela et al. (2021), wood structures
consist of cellulose fibrils in a matrix of lignin and
hemicellulose, which together result in a high strength-to-
weight ratio, but form a material with vulnerability to
hygroscopicity and dimensional instability.
Wood performance for some applications is directly
related to the presence of water, as it results in negative
changes to wood’s physical properties (dimensional
instability) and directly affects mechanical strength properties
and durability of the material (DIGAITIS et al., 2021). Beck
et al. (2018) reported that one of the main disadvantages of
wood is its high susceptibility to biological degradation,
which should be prevented.
The acetylation process has been studied to minimize
negative effects that result in the fragilization of wood’s
physical and mechanical properties. According to Quintana
et al. (2018), this process is a chemical change in which acetyl
(CH3CO-) groups react with hydroxyl (OH) groups present
in the cellulose surface, thus resulting in a less hydrophilic
surface. Wojeicchowski et al. (2018) reported that hydroxyl
groups present different reactivity levels and, during the
acetylation process, there are reactions of addition and
removal of these groups, which are converted into acetyl.
According to Marsich et al. (2018), acetylation treatments
improved the wood capacity to support higher loads than
Effect of acetylation on technological characteristics of Jacaranda copaia wood: Part 1 – Physical and mechanical...
Nativa, Sinop, v. 10, n. 2, p. 277-282, 2022.
278
non-modified wood, as the effect of acetylation increases
mechanical strength and decreases water absorption.
Acetylation also results in wood dimensional stability.
This stability is a result of the grouping of acetate linked to
hydroxyls of polymers of the cell wall. The cell wall volume
is close to the original fresh matter volume; thus, a little
swelling occurs when water enters the wood (ROWELL,
2006).
According to Van Der Lugt et al. (2016), chemical
treatments with acetylation at as industrial scale have been
carried out in some European countries and acetylated wood
is marketed mainly for the manufacturing of products for
external use, such as doors, windows, coatings, floors, and
light structures. Despite the existence of products based on
acetylated wood, and the fact that the acetylation process has
been used by industries for decades, the distributions of
acetyl groups in the wood are still little understood
(MAKELA et al., 2021). In Brazil, the wood acetylation
process is under research, but many species were still not
studied (FIGUEIREDO et al., 2019).
Jacaranda copaia (Aubl.) D. Don is among wood species
that are native, but not endemic, to Brazil. The geographical
distribution of this species in Brazil includes several states:
Acre, Amazonas, Amapá, Pará, Rondônia, and Roraima in
the North, Maranhão in the Northeast, and Mato Grosso in
the Central-West region (FARIAS-SINGER, 2020).
J. copaia wood presents specific properties, including low
density, dimensional instability, little mechanical strength,
easy water exchange with the external medium, low resistance
to deterioration, and low market cost (ELEOTÉRIO;
SILVA, 2014). Thus, this species has been used for purposes
that do not require high technological properties, such as the
production of boxes and toys and the manufacturing of
ferries. In this context, the objective of this work was to
evaluate the physical and mechanical properties of J. copaia
wood after acetylation, and assess whether this process is
efficient and results in improvements in the material
properties.
2. MATERIAL AND METHODS
2.1. Sample collection and preparation
Jacaranda copaia wood was obtained from timber boards
stored by the Laboratory of Wood Technology (LTM) of the
Institute of Agricultural Defense of the State of Mato Grosso
(INDEA), in Cuiabá, MT, Brazil.
One-hundred samples with nominal dimensions of 2.5 ×
2.5 × 1.0 cm (width × length × thickness) were used, all free
from pronounced defects such as cracks and knots.
The samples were placed in a forced air circulation oven
at a temperature of 60±2 °C until they presented anhydrous
weight and volume. The weight was determined using an
analytical balance, and the volume was determined using a
digital caliper, at the end of the drying. The samples were then
divided into five groups (treatments) with 20 samples: four
groups with samples to be subjected to acetylation and one
control group (non-acetylated samples).
2.2. Acetylation
The acetylation treatment was applied using the adapted
methodology of Gomes et al. (2006). The wood was
subjected to acetylation treatments four different times (2, 4,
6, and 8 hours) under constant temperature (90±2 °C). The
wood samples were immersed in four glass bottles containing
1000 mL of acetic anhydride, and the material was maintained
warm in a water bath.
The samples were then withdrawn from the immersion
and washed with water for removing most of the reagent and
subjected to drying in a forced air circulation oven at 60±2
°C. The samples were then weighed in an analytical balance
and measured for width, length, and thickness using a digital
caliper, thus obtaining the anhydrous volumes.
The weight gain of the acetylated wood was determined
using the ratio between the dry weights before and after the
treatments (Equation 1):
𝑊𝐺 =
∗ 100 (01)
where: WG = weight gain (%); Wt = treated wood dry weight (g);
Wnt = non-treated wood dry weight (g).
2.3. Physical properties
The tests of physical properties followed the procedures
established by the Brazilian Association of Technical
Standards (NBR 7190) (ABNT, 1997). Twelve samples of
each treatment were immersed in containers with distilled
water at 30±2 °C, and their weights and volumes were
determined after the following times: 2, 24, and 720 hours
(total saturation).
Water absorption and volumetric swelling were obtained
using Equations 2 and 3, respectively:
𝐴𝐵𝑆 =
∗ 100 (02)
VS =
∗ 100 (03)
where: ABS = water absorption (%); Ww = wet weight (g); Wd =
dry weight (g); VS = volumetric swelling (%); Vw = wet volume
(cm³); Vd = dry volume (cm³).
In addition, basic and apparent anhydrous densities were
determined, using the weight-to-volume ratio, according to
Equations 4 and 5:
𝑝𝑏 =
(04)
𝑝𝑎 =
(05)
where: pb= basic density (g cm-³); Wd = dry weight (g); Vsat =
saturated volume after 30 days of immersion in water (cm³); pa =
apparent density (g cm-³); Vd = dry volume (cm³).
2.4. Mechanical properties
The mechanical strength was evaluated using the
Rockwell hardness test (L scale), according to the adapted
methodology of Stangerlin et al. (2013). The tests were
carried out in an analog bench hardness tester with a spherical
penetrator of 0.25 inches. The load was applied to the
transversal section (2.5 × 2.5 cm) in two different phases. In
the first, a 98.1 N pre-load was applied; and in the second
phase, a 588,4 N load was applied. The results were collected
directly from the hardness tester analog gauge. Three
measurements of Rockwell hardness were carried out for
each sample, totaling 8 samples for each treatment.
Baufleur et al.
Nativa, Sinop, v. 10, n. 2, p. 277-282, 2022.
279
2.5. Statistical analysis
The results obtained for weight gain, water absorption,
volumetric swelling, and basic and apparent densities were
organized in spreadsheets, analyzed, and then applied to a
completely randomized design with 12 replications for each
one of the five treatments. The results of Rockwell hardness
were organized in spreadsheets, analyzed, and then applied to
a completely randomized design with 8 replications for each
one of the five treatments. The data were subjected to
analysis of variance (ANOVA) and the means were
compared by the Tukey's test at a 5% significance level.
3. RESULTS
3.1. Weight gain and density
The results obtained for the weight gain tests showed that
all treatments presented increases in weight due to the
acetylation process. The treatment with acetylation for 8
hours presented the highest weight gain, 21.62%, which did
not statistically differ from that of the treatment with
acetylation for 6 hours (Figure 1). The treatment with
acetylation for 2 hours presented the lowest gain weight,
18.06%, which did not statistically differ from that of the
treatment for 4 hours (Figure 1). The results showed that
treatments with shorter acetylation times (2 and 4 hours)
presented lower weight gains than treatments with longer
times (6 and 8 hours). These differences denote that the time
for the acetylation directly affects the weight gain
percentages.
Figure 1. Weight gain percentages of Jacaranda copaia wood after
different acetylation treatments.
Figura 1. Ganho de massa percentual da madeira de Jacaranda copaia
após os diferentes tratamentos de acetilação.
The results showed that the treatment with acetylation for
6 hours presented the highest basic density, 0.429 g cm-1
(Table 1), which did not statistically differ from that of the
treatment for 4 hours. The control treatment presented the
lowest basic density, 0.347 g cm-1 (Table 1). The analyses of
the results showed that the acetylation process resulted in an
increase of approximately 23% in basic density when
compared to the control treatment. This increase may be due
to the weight gain presented by the wood.
The treatment with acetylation for 6 hours presented the
highest apparent density, 0.455 g cm-3 (Table 1), and the
control treatment presented the lowest, 0.406 g cm-3 (Table
1). The analyses of the results showed that the acetylation
process resulted in an increase of approximately 12% in
apparent density when compared to the control treatment.
This increase may be due to the weight gain presented by the
wood.
Table 1. Mean basic density (ρb) and an apparent density (ρa) of
Jacaranda copaia wood subjected to acetylation.
Tabela 1. Valores médios de densidade básica (ρb) e densidade
aparente (ρa) das madeiras de Jacaranda copaia submetidas à
acetilação.
Treatments
ρ
b
(g cm
-
³)
ρ
a
(g cm
-
³)
Control
0.347 b
0.406 b
2 hours
0.416 ab
0.445 ab
4 hours
0.420 a
0.447 ab
6 hours
0.429 a
0.455 a
8 hours
0.415 ab
0.446 ab
Means followed by the same letters in the columns are not different from
each other by the Tukey's test at 5% significance level.
3.2. Water absorption and thickness swelling
The results of the water absorption tests showed that the
acetylation process resulted in decreases in wood
hydrophilicity in all acetylated treatments (Table 2). No
significant statistical differences were found between
treatments with 2 and 24 hours of absorption. However, after
reaching stability after 720 hours, the acetylation treatment
for 8 hours presented better performance, with water
absorption of 119.55%; and the control treatment presented
the worse performance, 220.17%.
The thickness swelling caused by the treatments showed
that the acetylation contributed positively to preventing
wood swelling, after water absorption. Treatments with
acetylation presented the lowest thickness swelling for all
immersion times and presented no statistically significant
differences from each other. Nonetheless, the treatment with
acetylation for 8 hours presented the lowest swelling values
at the stability time (720 hours): 7.13%. The control
treatment presented the highest swelling values at the stability
time (720 hours): 20.50% (Table 3). The analysis of the results
showed that the decrease in hydrophilicity caused by the
acetylation treatments also improved the wood’s dimensional
stability.
Table 2. Mean water absorption of samples of Jacaranda copaia wood
subjected to acetylation.
Tabela 2. Valores médios de absorção de água das amostras de
madeira de Jacaranda copaia submetidas à acetilação.
Treatments
Immersion time
2 hours (%)
24 hours (%)
720 hours (%)
Control
98.25 a
138.80 a
220.17 a
2 hours
61.56 b
88.87 b
159.04 b
4 hours
59.63 b
83.39 b
158.50 b
6 hours
53.22 b
75.90 b
149.34 b
8 hours
61.10 b
76.04 b
119.55 c
Means followed by the same letters in the columns are not different from
each other by the Tukey's test at 5% significance level.
Table 3. Mean volumetrically swelling of Jacaranda copaia wood
subjected to acetylation.
Tabela 3. Valores médios de inchamento volumétrico das madeiras
de Jacaranda copaia submetidas à acetilação.
Treatments
Immersion time
2
hours (%)
24 hours (%)
720 hours (%)
Control
12.02 a
16.74 a
20.50 a
2 hours
4.42 b
6.80 b
8.26 b
4 hours
4.11 b
6.70 b
8.82 b
6 hours
3.43 b
6.08 b
7.34 b
8 hours
3.79 b
5.84 b
7.13 b
Means followed by the same letters in the columns are not different from
each other by the Tukey's test at a 5% significance level.
18,06 b 18,70 b
21,57 a 21,62 a
0
5
10
15
20
25
30
2 4 6 8
Weight gain (%)
Time (hours)
Effect of acetylation on technological characteristics of Jacaranda copaia wood: Part 1 – Physical and mechanical...
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280
3.3. Hardness Rockwell
The results of the Rockwell hardness test showed that the
acetylation process increased the hardness of all treated
samples in all evaluation times, and presented no statistically
significant differences from each other. Despite the non-
significant differences, the treatment with acetylation for 8
hours presented the highest hardness (24.78 HRL) and the
control treatment presented the lowest hardness (5.05 HRL)
(Table 4). Considering these results, hardness increases as the
time of the acetylation process is increased.
Table 4. Mean Rockwell hardness of samples of Jacaranda copaia
wood subjected to acetylation.
Tabela 4. Valores médios de dureza Rockwell L das amostras da
madeira de Jacaranda copaia submetidas à acetilação.
Treatments
Rockwell hardness (HRL)
Control
5.05 b
2 hours
21.65 a
4 hours
22.61 a
6 hours
23.42 a
8
hours
24.78 a
Means followed by the same letters in the columns are not different from
each other by the Tukey's test at 5% significance level.
4. DISCUSSION
4.1. Physical properties
The weight gain of wood samples of Jacaranda copaia
(Aubl.) D. Don. after the acetylation treatment is probably
due to the reaction of hemicellulose to acetylation. Brum et
al. (2012) reported that one or more hydroxyl groups of the
wood chain are exchanged by acetyl groups during the
material acetylation process, thus, an increase in the material
weight is expected. According to Elrhayam and Elharfi
(2019), the chemical composition of hydroxyl groups present
in the wood is strongly dependent on electronic chemical
parameters, which makes it very important to the material
weight gain.
According to Brum et al. (2012), during the material
acetylation process, the higher the weight gain, the higher the
acetylation rate. Hunt et al. (2018) evaluated acetylation for
Pinus taeda and reported that the weight gain occurs because
the atomic weight of the hydroxyl group (17u) is lower than
that of the acetate group (59u), which substitutes it during the
chemical changes.
Ajdinaj et al. (2013) reported that acetyl molecules easily
penetrate low-density wood, making it possible to block a
greater number of free hydroxyl groups. Thus, the low
density of J. copaia wood may explain the expressive weight
gain after acetylation.
The increases in basic and apparent densities in the
treated J. copaia wood samples, compared to the control
treatment, may be due to the weight gain caused by the
acetylation process. According to Olaniran et al. (2019),
weight change is a factor that directly reflects changes in the
density of wood samples.
The results of the basic density of J. copaia wood with no
acetylation treatment was very close to 0.340 g cm-³, which
was obtained by Eleotério and Silva (2014) for the same
species with no treatment. The analysis and comparison
between the results showed that the acetylation treatment
indeed resulted in increases in basic density for the evaluated
wood.
The decreases in physical properties (water absorption
and thickness swelling) found for the J. copaia wood samples
after the acetylation treatments are due to the replacement of
hydroxyl (OH) groups by acetyl groups, which results in a
lower sensitivity of wood to water absorption and, thus, tends
to improve the mechanical properties, durability, dimensional
stability, and water absorption stability (NÉMETH et al.,
2020).
Castro; Iwakiri (2014) reported that hydrophile groups
present in the wood are blocked during the acetylation
process, resulting in a lower affinity between the water and
the acetylated wood. It generates a decrease in the water
absorption capacity of the material and, consequently, an
increase in the wood’s dimensional stability (CASTRO;
IWAKIRI, 2014).
Cermák et al. (2022) evaluated acetylation treatments in
Fagus sylvatica L. wood and found that the acetylated wood
presented an improvement of 50% in characteristics related
to the wood-water interaction. They also reported that the
acetylation contributed to decreases in the hysteresis effect
between adsorption and desorption curves and in the wood
anisotropy.
The efficiency of acetylation treatments in decreasing
water absorption was also found by Lopes et al. (2011), who
reported decreases between 54% and 72% in water
absorption rate for fibers of acetylated Neoglasiovia variegata
wood. Regarding the thickness swelling, Ajdinaj et al. (2013)
found that the acetylation treatment resulted in a 61%
decrease in swelling for the wood species Populus alba L., and
53% for the species Fagus sylvatica L.
According to Esteves et al. (2011), decreases in
volumetric swelling improve the wood dimensional stability
and, thus, reduce the formation of cracks and result in a
material with better performance. It also increases the
durability of the modified wood (ESTEVES et al., 2011).
Teaca and Tanasa (2020) reported that the wood
chemically modified by acetylation tends to present a lower
affinity to water when compared to non-modified wood. Bi
et al. (2021) reported that costs related to wood acetylation
treatments are decreasing and the material performance is
improving, which has made wood processing more
industrialized.
4.2. Mechanical properties
According to Scharf et al. (2022), hardness is a measure
of the resistance of a material to penetration by another
material of higher hardness and is very used for evaluating
the performance of wood products, mainly for analyzing the
efficiency of the densification process.
The results of the Rockwell hardness (L scale) showed
increases for all treatments with acetylation. According to
Figueiredo et al. (2019), increases in hardness after acetylation
treatments can be explained by the increase in weight during
the process.
Bongers; Beckers (2003) evaluated acetylation treatments
without catalyzer in Pinus sylvestris L. end Populus sp. wood and
found that the acetylated wood exhibited improvements in
elasticity and rupture modules, resistance to shear, parallel
compression to the grain, and Janka hardness. The
application of reactive or non-reactive chemical products to
wood cell walls/lumen may result in increases in hardness
and in compression force properties due to increases in wood
density (XIE et al., 2013).
Sydor et al. (2022) evaluated the wood species Alnus
glutinosa (L.) Gaertn, Tilia europaea L, Betula alba L, Fraxinus
excelsior L, Milicia excelsa (Welw.) CC Berg, and Fagus sylvatica
Baufleur et al.
Nativa, Sinop, v. 10, n. 2, p. 277-282, 2022.
281
L. and found that the higher the wood density, the higher the
Brindel hardness. They also found that the harder the wood,
the lower the total penetration depth during the tests. These
factors confirmed that density is essential for predicting and
evaluating wood strength properties.
5. CONCLUSIONS
The physical properties of acetylated wood improved
with the acetylation process, with an increase in densities and
reductions in water absorption and volumetric swelling
during immersion for 2h, 24h, and until full saturation in
water. Regarding Rockwell hardness, acetylation provided an
increase in surface penetration resistance of acetylated wood.
The 6 and 8h treatments showed the best results for
Jacaranda copaia wood since chemical modification occurred
in its structures, 21% mass gain, and improvement of physical
and mechanical properties.
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