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Application of Sustainable Lignin Stabilized Expansive Soils in Highway

Subgrade

Conference Paper  in  Geotechnical Special Publication · May 2021

DOI: 10.1061/9780784483435.033

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Application of Sustainable Lignin Stabilized Expansive Soils in Highway Subgrade

Debojit Sarker1; Omar Shahrear Apu2; Narendra Kumar3; Jay X. Wang4; and Joan G. Lynam5
1
Program of Civil Engineering, Louisiana Tech Univ., Ruston, LA. Email: dsa038@latech.edu
2
Program of Civil Engineering, Louisiana Tech Univ., Ruston, LA. Email:
apucekuet@gmail.com
3
Dept. of Chemical Engineering, Louisiana Tech Univ., Ruston, LA. Email: nku004@latech.edu
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4
Programs of Civil Engineering and Construction Engineering Technology, Louisiana Tech
Univ., Ruston, LA. Email: xwang@latech.edu
5
Dept. of Chemical Engineering, Louisiana Tech Univ., Ruston, LA. Email: lynam@latech.edu

ABSTRACT

A by-product of the paper and wood industries, lignin is produced abundantly worldwide due
to the increasing demand for wood and paper-based products. Improper disposal or storage of
lignin is not only a misuse of natural resources but also poses a critical hazard to public health
and the environment. Construction of highway subgrade has been identified as one of the
feasible responses for consuming vast quantities of lignin to dispose of it in an ecologically
sound manner, as it can be a low-cost and less energy-intensive chemical additive for soil
stabilization. However, studies on the performance of lignin in stabilizing expansive soils in
highway subgrade have been very constrained. Volume change resulting from seasonal moisture
variations in expansive soil subgrades damages existing highways and complicates highway
construction in expansive soil areas. To reduce expansive soil-induced geological disasters and
utilize waste resources, the use of lignin could potentially be a sustainable solution for soil
stabilization. In this research, a series of multi-scale laboratory tests were conducted to examine
the Atterberg limits, the compaction and consolidation behavior, and the Fourier-transform
infrared spectroscopy (FTIR) characteristics of lignin-stabilized expansive soils. The study
reveals that the degree of lignin content impacts the physical, mechanical, and microstructural
properties of the stabilized expansive soil. From the compression index (Cc) and swelling index
(Cs) values, it was concluded that a satisfactory level of soil stabilization could be achieved by
the application of an optimum percentage of lignin. The lignin-based cementing material bonds
soil particles firmly together and fills the pores to produce a progressively steady soil structure.

INTRODUCTION

Expansive soils exhibit significant volume changes (i.e., shrinking or swelling) associated
with moisture content fluctuations. Montmorillonite is a durable hydrophilic clay mineral that
triggers volumetric change behavior (Mitchell and Soga 2005). As a result, expansive soils
containing montmorillonite cause extreme distress and severe damage to various structures (e.g.,
embankment failure, subgrade subsidence, and differential settlement of slabs) and cause billions
of dollars of damage throughout the world (Nelson et al. 2015). In the United States, the
estimated damage to buildings and infrastructure due to the effects of shrinkage and swelling of
such soils exceeds $15 billion annually (Jones and Jefferson 2012). Researchers have studied the
field moisture content and soil suction potentials of expansive subsoils and investigated the
potentials at which soil and pavement cracking occur (Gaspard et al. 2019; Hossain et al. 2016;

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Puppala et al. 2011; Zornberg et al. 2008). As pavement is substantially impermeable, seasonal
moisture variation primarily affects the soils near pavement edges, resulting in heave or
shrinkage. However, the center remains unchanged throughout the year, causing differential
movements responsible for longitudinal cracking of the pavement structure. Figure 1 shows
typical longitudinal cracks that occur in pavements on expansive soils. Soil stabilization is one of
the practical techniques for enhancing the engineering properties of such problematic soils. For
example, a few traditional stabilizers, hydrated lime, Portland cement, and fly ash, have been
integrated to stabilize expansive soils (Khan et al. 2018; Mahedi et al. 2020; Phanikumar and
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Sharma 2007). However, the widespread utilization of such stabilizers extensively increases the
construction budget and intensifies natural resources (Seco et al. 2011). Thus, it would be
desirable to find a low cost and eco-friendly alternative to the traditional ones.

Figure 1. Longitudinal cracks on pavement due to subgrade heaving.

Lignin is a paper/wood industrial waste, and it is widely produced around the world (50
Mt/annum) due to the ever-increasing demand for paper and wood products (Gandini and
Belgacem 2008). Its disposal requires consideration due to its abundance, particularly in the US,
as the US produced about 72.3 Mt of paper/cardboard in 2017, and production has been growing
in subsequent years (Statista 2019). Lignin from these industries is frequently burned, generating
air pollution such as NOx (Nichols and Lien 1993). A sustainable alternative for lignin use in
highway subgrade has been assessed recently by several researchers (Arafat et al. 2019; Kim et
al. 2012b; Li et al. 2020; Zhang et al. 2018). The subgrade stabilized with a lignin-based biofuel
coproduct led to much lower cracking of Hot-Mix Asphalt (HMA) pavements under different
traffic and climate conditions (Kim et al. 2012a). Therefore, the utilization of lignin as an
expansive soil stabilizer in highway subgrade has the potential to become a sustainable and
economical solution for the construction industry.
Some past studies have reported the improvement of various geotechnical properties in
different soils using lignin. Nonetheless, these investigations were, for the most part,
concentrated on silty sand, silt clayey soil, and low plastic clays (Athukorala et al. 2013;
Indraratna et al. 2013; Li et al. 2019; Liu et al. 2020; Zhang et al. 2017). Limited investigations
on the use of lignin-stabilized expansive soil have indicated moderate improvement in
engineering properties (e.g., volumetric change behavior, plasticity, and strength) (Alazigha et al.
2016; Ijaz et al. 2020; Ta’negonbadi and Noorzad 2018). Despite the anticipated economic
advantages for the construction industry, research on lignin as a stabilizer to enhance expansive
soil subgrade has not been well documented. Lignin stabilization depends on intermolecular
interactions instead of chemical reactions like traditional stabilization with lime or cement

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(Alazigha et al. 2018). Considering the data available on lignin as a soil stabilizer, the authors
propose that using lignin as a stabilizer could viably improve expansive soil subgrades and
provide a sustainable solution for reducing industrial waste and air pollution.
The purpose of this research is to investigate the feasibility of utilizing a lignin-based paper
and wood industry by-product to stabilize expansive soil in highway subgrades by improving its
geotechnical properties while reducing energy consumption and CO2 emissions by using
frequently-burned waste material. A series of lab tests were performed, such as the Atterberg
limits, compaction and consolidation, and Fourier-transform infrared spectroscopy (FTIR), to
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observe the behavior of lignin-stabilized expansive soils. Based on the experimental results, the
impacts of different lignin contents on physical, mechanical, and microstructural properties of
lignin-stabilized subgrade expansive soils were investigated.

MATERIALS AND METHODS

This study aims to investigate the physical, mechanical, and microstructural properties of
lignin-stabilized expansive Moreland clay. As per soil taxonomy classification of the United
States Department of Agriculture (USDA), Moreland clay is very-fine, smectitic, thermic
Oxyaquic Hapluderts, expansive in nature, and considered to be a weak construction and road fill
material (USDA 2019). The ‘series extent explorer application’ shows that the Moreland clay
covers approximately 489,690 acres (1981.7 sq. kilometers) of the land distributed mostly in
Louisiana, eastern Oklahoma, eastern Texas, and Arkansas. Figure 2 presents the Moreland clay
distribution in the USA, with a large portion of it present in Louisiana.

Figure 2. The Moreland clay map of the United States (Modified after USDA (2019)).

Soil Sample: The Moreland clay samples used in this study were excavated from the open
pit at a church construction site in Bossier City, Louisiana, in 2016, following ASTM D1452 for
disturbed soil samples (ASTM 2016). All the samples were plastic-wrapped and kept in a sealed
container. The whole collection was transported and stored in the Geotechnical Laboratory at
Louisiana Tech University, following standard practice for preserving soil samples. The basic
engineering properties of the soil are listed in Table 1. The soil was classified as Fat Clay (CH)
as per the Unified Soil Classification System. According to the Louisiana Department of

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Transportation and Development (LADOTD) standard specification of roads and bridges, soils
with a plasticity index (PI) higher than 25 (e.g., Moreland clay) cannot be used directly for
highway subgrade filling materials (LADOTD 2016). It should be removed or treated.

Table 1. Physicochemical properties of the tested expansive soil.

Property Value
Specific gravity, Gs 2.75
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a
Grain size distribution (%) -
0.075 mm passing 99
Activity of clay, Ac 1.3
b
Liquid limit, LL (%) 68
b
Plastic limit, PL (%) 22
Plasticity Index, PI (%) 46
Optimum moisture content, wopt 27
Maximum dry density, ρdmax (g/cm )
3
1.49
c
pH (water/soil = 1) 7.59
a
Data from Khan et al. (2019); Measured as per ASTM D4318 (ASTM 2017); cMeasured as per
b

ASTM D4972 (ASTM 2019)

Lignin Isolation from Black Liquor: Black liquor was collected from a softwood Kraft
processing industry in Monroe, Louisiana. The received black liquor had a pH value of ~12.9
and contained 25-30% cellulose, hemicellulose, lignin, 22-27% sulfates and carbonates, and 4-
8% sodium hydroxide, and 4-8% sodium sulfide. In this study, spent sulfuric acid (SSA) was
used to precipitate the lignin fraction from black liquor. SSA was collected from a galvanizing
facility in Covent, Louisiana. The received SSA had about 6-10 % sulfuric acid content by
weight.
The precipitation of the lignin fraction through acidification of the black liquor was
performed. First, black liquor was heated to 60˚C, and then spent sulfuric acid was added and
stirred to precipitate the lignin. The precipitated lignin fraction was then collected after
decantation and washed with deionized water seven times to remove any water-soluble impurity.
After removing the water-soluble impurities, lignin was separated using a basket centrifuge and
dried at 60˚C for 48 hours. The dried lignin was ground to a fine powder that passed through a
#100 sieve, meaning that the lignin particle size was less than 0.15 mm.
Sample Preparation: The collected soil was air-dried before it was passed through the sieve
with a 2-mm opening size for a standard Proctor compaction test. This test was carried out to
evaluate the maximum dry density ρdmax and the optimum moisture content wopt of the stabilizer-
modified soils directly after treatment. For the Atterberg limits test, the air-dried soil was crushed
and passed through a 0.5-mm sieve. The chosen amounts of lignin and deionized water
(approximately wopt) were mixed in with the air-dried soil. At that point, the lignin-soil mixtures
were sealed in plastic bags and put in ambient conditions in a controlled chamber (22 ˚C and
relative humidity of 95%) for 28 days before being tested for the Atterberg limits.
The predetermined amounts of lignin and water were added into the air-dried soil for the
consolidation test until a moisture content of approximately wopt was achieved. As shown in

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Figure 3(a), the soil and lignin were mixed together for about 5 min to get homogenous mixtures.
Subsequently, the mixtures were poured into a consolidation ring and compacted to achieve the
degree of compaction of 100±5% by multiple trials via a static compaction method. Soils of
approximately 1 cm3 were sampled from the carefully hand-broken identical consolidation
specimens for FTIR analysis. All the specimens were cured at 22 ˚C and relative humidity of
95% for 28 days before tests.
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Figure 3. Experimental setup: (a) Stabilizer modified expansive soils, (b) Porous stones on
hot-plate, (c) Prepared samples in consolidation ring, and (d) Consolidation tests.

Testing Program: The Atterberg limits of the lignin-stabilized soils were determined
following ASTM D4318 (ASTM 2017). The standard Proctor compaction test was performed
with a standard compaction effort of 600 kN-m/m3 following ASTM D698 (ASTM 2012). One
way to measure soil stabilization is to perform one-dimensional consolidation tests (Terzaghi et
al. 1996). The consolidation test was conducted following ASTM D2435 (ASTM 2020). As the
soils were highly expansive, porous disks were boiled in deionized water and dried before they
were used (Figure 3(b)). After samples were prepared, as shown in Figure 3(c), the
consolidometer was placed in the loading device. A seating load with total axial stress of about
1.5 kPa was applied, sufficiently large to prevent swelling but not causing significant
consolidation. As shown in Figure 3(d), the sample was inundated with the deionized water
shortly after applying the seating load. A load increment ratio (LIR) of one was maintained by
doubling the total axial stress on the soil to obtain values of about 50, 100, 200, 400, 800, and
1600 kPa. The compression index (Cc) and swelling index (Cs) of the untreated soil and lignin-
stabilized soils were determined from the e-log p curves. In this experiment, untreated soil was

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used to find a baseline performance, and it was compared with the 5%, 10%, and 15% lignin
stabilized soil samples.
In this research, microstructural observational tests were additionally conducted to
understand the stabilization mechanism further. Fourier transform infrared spectroscopy (FTIR)
analysis was conducted to determine the functional groups of untreated and lignin-stabilized
soils. A Mattson Genesis II FTIR (Mattson Technology, Fremont, CA, USA) with a KBr pellet
holder was used to perform FTIR on KBr pellets prepared to contain the sample. For each
sample, 32 scans were performed from 4000 to 400 cm-1. The results of FTIR analysis were
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presented in the form of percentage transmittance versus wavenumber.

RESULTS AND DISCUSSIONS

Atterberg Limits: Figure 4 shows the results of the Atterberg limits tests for untreated soil
and lignin-stabilized soils. It can be observed that for lignin-stabilized soils, both the liquid limit
(LL) and the plasticity index (PI) are lower than those obtained for the untreated soil. However,
the plastic limit (PL) values of the lignin-stabilized soils are nearly equivalent to those of the
untreated soil, showing little lignin effect. Puppala and Hanchanloet (1999) used a mixture of
lignin (LS-40) and sulfuric acid (SA-44) to stabilize cohesive soil and found that LL and PI
dropped slightly after treatment, which is in line with this study. Due to the difference in
chemical components between lignin and traditional stabilizers (i.e., lime, cement, and fly ash),
further investigations should be conducted to understand better the mechanism of Atterberg
limits variations in lignin-stabilized soils.

80
68 67 LL
70 64 PL
57 PI
Moisture content

60
50 46 44
39
40 35
30 23 25
22 22
20
10
0
0 5 10 15
Lignin content (%)

Figure 4. Atterberg limits for untreated and lignin treated expansive soils.

Compaction Characteristics: Figure 5 shows compaction curves for untreated soil and
lignin-stabilized soils with different lignin contents. It is evident from Figure 5 that the lignin-
stabilized soils show a lower maximum dry density (MDD) or ρdmax as compared with the
untreated soil. Moreland clay's MDD value decreases from 14.6 kN/m3 to around 13.7 kN/m3
after stabilization with lignin. The decrease in MDD of expansive soils with lignin addition is
consistent with previous research (Ijaj et al. 2020). However, the optimum moisture content
(OMC) or wopt decreased from 27% to roughly 25% for 5% lignin-stabilized soils, then increased

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to 29% for 10% lignin-stabilized soils, and finally came down to roughly 27% for 15% lignin-
stabilized soils. The phenomena of lignin-stabilized soils demonstrate the increased sensitivity of
dry density to the variation of moisture content. It can be concluded that the moisture content of
the lignin-stabilized expansive soils should be controlled carefully at the highway subgrade
construction site to obtain the required degree of compaction.

15.0
Zero-Air-Void curve
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14.5 Gs = 2.75
Dry density (kN/m3)

14.0
13.5
13.0 Moreland Clay
5 % lignin
12.5 10 % lignin
15 % lignin
12.0
22 24 26 28 30 32 34
Moisture content (%)

Figure 5. Compaction curves for the expansive soils with different lignin content.

Consolidation Characteristics: The expansive soil samples for the oedometer test were set
up at the optimum moisture contents and maximum dry unit weights of the lignin-soil mixture
obtained from the standard Proctor compaction curves (Figure 5). The compression index (Cc),
which is the slope of the linear portion of the e-log p curve, shows the amount of compression
undergone by the soil. Swell index (Cs) is the slope of the rebound curve. The e-log p curves for
untreated soil and lignin-stabilized soils from which Cc and Cs were determined are shown in
Figure 6. Figure 7 shows, by comparison, the variation of Cc and Cs with increasing lignin
content. The value of Cs decreases monotonically for expansive soils with increasing lignin
content. The decrease in the swelling characteristics is fundamentally by replacing plastic fines
of clay with non-plastic fines of lignin. It is evident that when the swelling index decreases, the
heave or shrinkage of the treated expansive soil is reduced. However, the value of Cc decreased
for expansive soils with the increasing lignin content up to 10% and then increased by adding
more lignin. The reduced value of Cc up to 10% lignin content suggests that the expansive soil
mixed with optimum lignin content would resist the compressive loading better and subsequently
exhibit lesser compressibility characteristics. From the variation of Cc and Cs with increasing
lignin content, it can be concluded that satisfactory stabilization of expansive Moreland clay
could be achieved with the application of 10% of lignin. Apu et al. (2021) assessed clayey soil's
compression index using over 30 consolidation tests and found that the minimum compression
index depends on the soil samples' optimum initial void ratio. Further research is needed to
develop optimized relationships associated with dry density, plasticity index, and initial void
ratio to understand the mechanism for the compression index of lignin-stabilized expansive soils
to improve the subgrade performance.

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1
0.9 Moreland Clay
5% lignin
Void ratio, e
0.8 10% lignin
15% lignin
0.7
0.6
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0.5
0.4
10 100 1000 10000
Pressure, P (kPa)

Figure 6. Consolidation curves (e - log P) for the expansive soils with different lignin
content.

0.300 0.080
0.295 Cc
Compression Index, Cc

Cs 0.075
0.290

Swell Index, Cs
0.285 0.070
0.280 0.065
0.275 0.060
0.270
0.265 0.055
0.260 0.050
0 5 10 15
Lignin content (%)

Figure 7. Variations of Cc and Cs of the expansive soils with different lignin content.

Fourier-Transform Infrared Spectroscopy Analysis: Fourier-transform infrared

spectroscopy (FTIR) analysis was carried out to investigate the vibrational characteristics of the
–OH, H–O–H, interlayer cations, and tetrahedral silicate/aluminate anions. Figure 8 shows the
FTIR analysis results of the untreated Moreland clay and 10% lignin-stabilized soil. The
functional groups compared to the wavenumbers are also labeled in Figure 8 to aid in
understanding. Moreland clay consists of functional groups such as the –OH stretch (water
bonding directly to cations, 3620 cm-1, additional adsorbed water molecules, 3450 cm-1, and
alkali-saturated water, 1633 cm-1), and the Si–O stretch (1034 cm-1). These findings confirm the
mineral montmorillonite's presence in Moreland clay by exhibiting an H2O stretching mode near
3610-3630 cm-1 (Bishop et al. 1994). Figure 8 also shows that 10% of lignin-stabilized soil
contains the functional groups of untreated soil in addition to those of lignin. The distinction in
spectra between untreated soil and lignin-stabilized soil is found in functional groups such as C–

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H stretching (CH2, 2925 cm-1), O=C=O (CO2 derived from the environment, 2350 cm-1), and –
C=C– (aromatic skeletal vibration, 1520 cm-1) (Rashid et al. 2016). This investigation postulates
the development of ionic or hydrogen bonding between functional groups of lignin and clay
minerals in the stabilized soils. It can be concluded that the lignin-based cementing materials
could chemically bond with clay minerals to form a stable structure.

(2350)
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Transmittance (%)

(2925)

(1520)

(1633)
(3620)(3450)

Moreland Clay
(1034)
10% lignin

3600 2600 1600 600

Wavenumber (cm-1)

Figure 8. Functional group analysis of untreated and 10% lignin-stabilized soil.

A comparison of the properties of expansive soils (i.e., Moreland clay) stabilized with
different lignin content is presented in Table 2. The vast majority of the expansive soils in
northern Louisiana are Moreland clay with a high plasticity index (Khan et al. 2017, 2019).
Though LADOTD, Louisiana Transportation Research Center (LTRC), and Southern Plain
Transportation Center (SPTC) have supported a limited number of research projects on
expansive soils used as subgrade, stabilization of the Moreland clay has still not been well
addressed, or related research has not been well documented in Louisiana (Gaspard et al. 2019;
Wang et al. 2018). Recently, mechanistic-based methods have been developed to identify
pavement distresses caused by expansive soil-induced heave or shrinkage deformations of the
subgrade (Khan et al. 2020; Sarker et al. 2019; Sarker and Wang 2021a). Indeed, these models
predict the realistic structural performance of pavement on lignin-stabilized expansive soils when
the engineering properties of the subsoils are known. The results presented in this study will be
useful in formulating strategies for stabilization of expansive soils by lignin-based industrial by-
products if engineering properties are used as input parameters.
Although the research shows evidence that the use of lignin as an additive for the treatment
of the expansive Moreland soils is very promising and is in line with previous research shown in
literature, it is limited to one sampling point testing. The saturated moisture content (at zero
suction) of Moreland clay is much higher, and such soil undergoes a more considerable swelling
when hydrated (Sarker and Wang 2021b). Based on theoretical considerations, it may be
demonstrated that suction would be reduced in lignin-stabilized expansive clay samples, and
consequently, the swelling would be reduced. Additional research is needed not only for lab
testing such as soil-water retention properties, consolidation swelling, X-ray Fluorescence

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(XRF), X-ray diffraction (XRD), and Scanning Electron Microscope (SEM) but also for field
testing of stabilized soil to understand better the properties of lignin and its mechanism to
stabilize clay.

Table 2. Comparison of properties of lignin stabilized expansive soils.

LL PI wopt ρdmax
Conditions Cc Cs
(%) (%) (%) (gm/cc)
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Soil
68 46 27 1.488 0.296 0.0754
(Moreland clay)
5% lignin + soil 67 44 25 1.422 0.282 0.0679
10% lignin + soil 64 39 29 1.409 0.262 0.0652
15% lignin + soil 57 35 27 1.397 0.292 0.0547

CONCLUSIONS

Based on the experimental results, it can be concluded that Moreland clay is highly
expansive soil, and lignin may be an acceptable material for sustainable stabilization of such soil.
Atterberg limits of Moreland clay with lignin resulted in a moderate decrease in the liquid limit
LL and plasticity index PI, but the plastic limit PL remains relatively constant; therefore, the PI
is essentially a reflection of the LL. Lignin stabilized expansive soils showed increased
sensitivity of dry density to the variation of moisture content. The stabilization effect of lignin on
expansive soils was measured using the swelling index, which is a reasonable indicator of the
degree of swelling or shrinkage when moisture content of stabilized expansive soils fluctuates.
The swelling index Cs of Moreland clay decreased with an increase in lignin content, which may
improve a pavement section's performance by reducing the heave or shrinkage in the subgrade.
The study shows that a satisfactory level of stabilization of expansive soils could be achieved by
adding 10% lignin content. In other words, the optimum percentage of lignin content for
Moreland clay in this study was found to be approximately 10%. The FTIR analyses reveal that
the functional groups of lignin-stabilized soil are equivalent to the functional groups of lignin in
addition to those of untreated soil. The fundamental mechanism for the lignin-stabilized
expansive soils' enhanced engineering properties is likely the development of lignin-based
cementing materials during the curing period. Preliminary results of this research should
encourage LADOTD and the DOTs of other states to investigate the potential of lignin as a
sustainable alternative to traditional stabilizers (i.e., cement, lime, and fly ash) to stabilize
expansive soils.

ACKNOWLEDGEMENTS

The authors would like to express their gratitude to Mr. Gary Hubbard at Greater Bossier
Economic Development Foundation and Dr. Shams Arafat for their assistance in soil sampling
works in the field. We thank Swarajit Sarker for assistance with Figure 1. We are also immensely
grateful to Graphic Packaging International Inc. for kindly proving black liquor and Millennium
Galvanizing for kindly providing SSA. The authors want to sincerely acknowledge the

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competitive research subprogram of the Louisiana Board of Regents for funded project
LEQSF(2017-20)-Rd-A11 and Region 6 Environmental Protection Agency P2 for grant NP -
01F55301 – 0. The two grants provided financial support for conducting the research presented
in this paper.

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