2023-CHEN-Experimental Optimization of Industrial Waste-Based Soil Hardening Agent...
2023-CHEN-Experimental Optimization of Industrial Waste-Based Soil Hardening Agent...
2023-CHEN-Experimental Optimization of Industrial Waste-Based Soil Hardening Agent...
A R T I C L E I N F O A B S T R A C T
Keywords: In this study, an innovative approach was proposed for developing industrial-waste-based soil
Experimental optimization curing agent mixtures using D-optimal design (DOD) and the genetic algorithm (GA). The in
Soil hardening agent fluences of blast furnace slag (BFS), steel slag (SS), phosphogypsum (PG), and 42.5-grade ordinary
Unconfined compressive strength Portland cement (P.O 42.5) on the mechanical characteristics of the solidified soil were assessed
Genetic algorithm through unconfined compressive strength (UCS) tests. The mechanism, hydrates, and ecological
Life cycle assessment
properties of the soil solidified with the optimized curing agent were also evaluated. The statis
tical analysis confirmed the precision of the fitted regression model in forecasting the mechanical
characteristics of the stabilized soil. Furthermore, the BFS and PG were found to have a positive
effect on the UCS within a certain range at a 7-day age, while the SS and P.O 42.5 exhibited the
opposite effect. The hybrid DOD-GA technique was more effective to optimize the formulation
than the DOD technique. Overall, the UCS of the new curing agent-stabilized soil cured for 7 days
with the same dosage was 46.25% higher than that of cement-stabilized soil; and the global
warming potential (GWP) of the new curing agent per ton was 70.42% lower than that of cement.
The new curing agent is more capable of achieving improved strength, microstructure, and
environmental benefits than cement is, in addition to having inherent potential in industrial
waste recycling, greenhouse buffering, and natural resource conservation. The contribution of
this research is that the proposed systematic framework is universal, and it is reasonable to
implement formulation optimization of soil hardening agents.
1. Introduction
Global warming continues to intensify due to the enormous emissions of greenhouse gases. According to the International Energy
Agency publication “Global Energy Review: Carbon Dioxide Emissions in 2021,” the global CO2 emissions of the energy field in 2021
totaled 36.3 billion tons [1]. Initial statistics suggest that 2.537 Gt of CO2 in the cement industry was produced globally in 2020 [2].
Further, treatment of industrial waste has become a major problem in the global environment and energy fields, and its utilization
rate is less than 60%. The recycling of industrial waste is essential for achieving the Net Zero Emissions by 2050 Scenario goal. The
development of civil engineering promotes cement demand, which further exacerbates environmental pollution [3]. Therefore, the
cement industry is an important determinant of CO2 emissions and energy consumption [4]. Moreover, cemented soil exhibits the
disadvantage of a low early strength. It is possible to replace cement with industrial waste as the soil curing agent. It has been reported
* Corresponding author.
E-mail addresses: [email protected] (X. Chen), [email protected] (F. Yu), [email protected] (J. Yu), [email protected] (S. Li).
https://doi.org/10.1016/j.jobe.2023.106611
Received 20 February 2023; Received in revised form 1 April 2023; Accepted 18 April 2023
Available online 19 April 2023
2352-7102/© 2023 Elsevier Ltd. All rights reserved.
X. Chen et al. Journal of Building Engineering 72 (2023) 106611
that the appropriate utilization of industrial waste benefits the strength of solidified soil but additionally effectively decreases the
environmental burden [5,6]. For example, Miraki et al. [7] adopted mechanical and microstructural tests to evaluate the durability of
stabilized clay by volcanic ash (VA) and blast furnace slag (BFS). The testing results demonstrated that a proper aggregation of VA and
BFS was superior to Portland cement in terms of the structure, strength, and environment. Liu et al. [8] conducted a series of
experimental tests on the properties of SCM (steel slag, cement, and metakaolin)-solidified soil, which included unconfined
compressive strength (UCS) tests and scanning electron microscopy (SEM). The experimental results showed that the strength of the
SCM-stabilized clay reached 1.0 MPa at the curing age of 28 days, and the relationship between the strength and binder-free water ratio
was proposed for further analysis. Jiang et al. [9] studied a binder composed of BFS, carbide slag (CS), and other materials to stabilize
soft soil instead of cement. A giant quantity of hydrate in the new binder-solidified soil supplied a greater sulfate attack resistance. Li
et al. [10] studied the effect of BFS and cement for as-contaminated soil treatment, which confirmed that the BFS had a prominent
improvement effect on the strength at 28 days. Salimi and Ghorbani [11] carried out several experiments to investigate the various
factors affecting the properties of slag- and geopolymer-stabilized soft clay. Ren et al. [12] examined the effect of
phosphogypsum-solidified silty soil, aiming to establish a linear model to analyze the association between the physical parameters and
the microstructural properties.
The investigations in the available scientific literature have revealed that industrial waste has been considered as an alternative soil
curing agent to cement with improved environmental sustainability [13]. In most of these studies, the optimization of the curing agents
was carried out by varying the variables one by one based on traditional control variable methods, resulting in problems of a high
number of experimental trials and a relatively long period test. However, the interactions between variables are difficult to take into
consideration in univariate approaches. Hence, mixture design is a specially constrained regression design that considers the inter
action of variables, requiring a lower number of experiments [14]. Mixture design has been applied in many fields, including civil
engineering, since it was first proposed by Scheffé in 1958 [15]. For instance, Wang et al. [16] established a quadratic mixture model to
evaluate the effects of solid particles and superplasticizers on the bulk density, confirming that the D-optimal mixture design was able
to optimize the ultra-high performance concrete (UHPC) bulk density effectively. Varanda et al. [17] conducted a constrained mixture
design to prepare bitumen blends composed of residues and aromatic extracts. Sun et al. [18] added limestone and calcined clay
tailings into cement to optimize the system of the eco-efficient UHPC through a D-optimal mixture design. The eco-efficient UHPC was
superior to the normal UHPC in the environment. However, it had a lower strength and workability. In the aforementioned studies,
mixture design was an effective and essential tool for cementitious material formulation involving numerous components. Mixture
design mainly includes experimental design, model development, model suitability evaluation and optimization. The optimization of
nonlinear model also has difficulty in selecting the optimal parameters. Hence, the metaheuristic algorithm is proposed to effectively
improve the prediction accuracy of regression model. Genetic algorithm (GA) is one of the most widely used metaheuristic algorithms
and well accepted due to its outstanding search capability, randomness as well as good compatibility [19]. Therefore, the GA is
employed in this study for formula optimization.
In this study, industrial wastes, including blast furnace slag (BFS), steel slag (SS), and phosphogypsum (PG), were attempted to be
recycled into solidified soil. More specifically, the UCS at the early stage was treated as the response to assess the mechanical properties
of the stabilized soil, and the D-optimal design (DOD) model was established. In view of the discussion above, the optimal dosages of
BFS, SS, PG, 42.5-grade ordinary Portland cement (P.O 42.5), and superplasticizer (SP) were obtained by establishing a genetic al
gorithm (GA) model with specific constraints. Then, the strengths of the cured soils obtained by the DOD and DOD-GA methods were
verified. Finally, the curing mechanisms and hydration characteristics of the optimal stabilized soil and cemented soil were studied.
The life cycle assessment (LCA) of the industrial-waste-based soil hardening agent was carried out by the economic value allocation
principle. The contribution of this research is that the proposed systematic framework is universal and reasonable to implement for the
formulation optimization of soil hardening agents, and it provides a reference for similar analyses.
2.1.2. Stabilizers
In this study, BFS, SS, PG, P.O 42.5, and SP were used as the raw materials for generating the new soil hardening agent. The SP was
the polycarboxylate type. The chemical ingredients of the inorganic materials in this study are displayed in Table 2.
Table 1
Physical characteristics of silt.
Soil Unit Weight, Moisture Void Cohesion, Internal Friction Liquid Plastic Compression
Sample kN•m− 3 Content,% Ratio kPa Angle, ◦ Limit,% Limit,% Modulus, MPa
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Table 2
Chemical compositions of inorganic materials in this study.
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Table 3
Constrained variables and responses.
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There are many approaches for mixture design, including Simplex Centroid, Simplex Lattice, Extreme Vertices, ABCD Design,
Space-Filling, and Optimal designs [20–22]. In this study, the proportions of the components were restricted through higher and lower
limits. Hence, D-optimal design was applicable [23]. D-optimal design is an iterative algorithm that maximizes the determinant of the
information matrix [24]. This method provides an effective means for formula optimization with fewer tests and high precision of the
prediction model fitting.
To evaluate the optimal proportions of BFS, SS, PG, P.O 42.5, and SP, a set of mixture experiments designed by D-optimal design
were carried out. Design-Expert 12.0 was employed for the experiment design, model development, analysis of variance (ANOVA),
diagnostics, and optimization. The design and data analysis of mixture experiments usually include the following steps (Fig. 3):
(i) Determine response and mixture components.
(ii) Select an appropriate design algorithm to solve the problem. In this investigation, the mixing proportions of BFS, SS, PG, P.O
42.5, and SP were determined based on D-optimal design, and the constrained variables and responses are introduced in
Table 3.
(iii) Obtain the matrix of the D-optimal design. A 20-run-point mixture design was generated for the five-component system by the
Scheffé quadratic model, including 10 runs for model fitting, five replicate runs, and five runs for lack of fit evaluation.
(iv) Perform experiments and collect data.
(v) Analyze and verify the fitted model adequacy to determine the correlation between the requirements and factors.
(vi) Determine the optimal mixture components of the new soil hardening agents.
2.3. Methodology
2.3.1. Specimen preparation
The specimen was prepared in accordance with the requirements in “Specification for mix proportion design of cement soil (JGJ/T
233–2011)” [25]. The curing agent content should not be less than 20% of the wet soil mass in accordance with “Technical specifi
cation for trench cutting re-mixing deep wall (JGJ∕T 303–2013)” [26]. In this study, the ratio of the curing agent mixture to the wet
soil was set to be 20% with respect of engineering practice. The raw materials BFS, SS, PG, and P.O 42.5 were weighed and mixed
uniformly according to the test groups defined in Table 4. Then, the BFS, SS, PG, P.O 42.5, and soil were poured into the mixer for
stirring at a low speed for 1 min. After the mixer stopped, the SP and water were added to the mixture, and the water–binder (W/B)
ratio was 0.8. The mixer was set to a high speed, and the mixture was stirred for 4 min. The created stabilized soil was poured into three
cubic molds with side lengths of 70.7 mm and vibrated. The specimen was demolded after 24 h, and cured film mulching was per
formed at room temperature.
Table 4
D-optimal mixture design run points and corresponding responses.
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Fig. 4. Samples and equipment of unconfined compressive strength (UCS): (a) samples and (b) WAW-300B universal testing machine.
(SEM) test, the moisture in the sample will reduce the speed of equipment to reach the vacuum and the service life of the filament.
Therefore, the testing sample was dried at a temperature of 110◦ C to evaporate the free water and crushed. The naturally broken,
relatively flat soil particles were selected to be gold-plated by the JEC-3000FC to be used in the SEM analysis. After passing through a
0.075-mm sieve, the stabilized soil powder could be used in the XRD analysis. The following parameters were selected: Cu (Kα), 40 kV,
40 mA, 10◦ –80◦ , and 3◦ /min.
Fig. 5. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) equipment: (a) Gemini 500 scanning electron microscope and (b) Thermal ARL X’TRA X-ray
diffractometer.
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Fig. 6. System boundary of life cycle assessment (LCA) of new soil hardening agent.
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Fig. 9. Two-dimensional contour and three-dimensional surface plots with variations of components: (A) blast furnace slag (BFS), (B) steel slag (SS), and (C)
phosphogypsum (PG) with fixed contents of Portland cement (P.O 42.5, D = 25.36 wt%) and superplasticizer (SP, E = 0.1 wt%).
p-value. A high F-value implies that the random error of the model is smaller than the explained variance [31]. This indicates that the
result has statistical significance with a larger F-value and a smaller p-value below 0.05 [32]. For the response of the UCS, the in
teractions AD, BC, and CD were significant (p < 0.05) and the interactions AB, AC, and BD were insignificant (p > 0.05). Hence, it was
necessary to remove insignificant items in the model through the backward elimination technique (BET) [23]. The BET was imple
mented by putting all terms into the model simultaneously and then removing one at a time until the best-term-smaller model was
obtained. The acquired final mathematical fitted model based on regression analysis is as follows:
y = − 0.089x1 + 0.158x2 + 0.466x3 − 0.275x4 + 0.008x1 x4 − 0.006x2 x3 − 0.088x3 x4 (5)
where y represents the unconfined compressive strength, x1, x2, x3, and x4 represent the BFS, SS, PG, and P.O 42.5, respectively.
Table 5
Analysis of variance (ANOVA) results of the UCS model cured for 7 days.
Source Sum of Squares Degrees of Freedom Mean Square F-value p-value Results
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Fig. 10. Diagnostic plots including (a) Box–Cox plot, (b) normal plot of residuals, (c) Cook’s distance plot, (d) leverage plot, (e) residuals vs. predicted response plot,
and (f) predicted vs. actual plot.
Cook’s distance plot was obtained by evaluating the influence of the omission of one specific group from the model to facilitate the
detection of outliers. As shown in Fig. 10(c), the points were uniformly distributed, and there were no outliers due to the experimental
error. The uniformly distributed points in Fig. 10(d) and (e) were randomly scattered, supporting the result of the Cook’s distance plot.
Moreover, the outliers were ruled out in both Fig. 10(d) and (e). Fig. 10(f) shows the predicted vs. actual value of the UCS, which
revealed that the experimental UCS varied from 1.72 to 3.61 MPa whereas the predicted UCS varied from 1.76 to 3.54 MPa. The
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analysis of the predicted vs. actual plot supported the high R2 value. Overall, the results of the ANOVA and diagnostics demonstrated
that the unconfined compressive strength model was representative of the experimental data.
The quantitative relationship that the sum of the variables equals 100% was taken into account in the last term in Eq. (6). Conse
quently, the minimum value of the fitness function demonstrated the best fitness in the study. After the establishment of the initial
population (initial population size = 1000) and the fitness function, the reproduction procedure was iterated until the optimal
chromosome was found.
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Fig. 12. Two-dimensional contours and three-dimensional surface plots with fixed contents of SP (E = 0.1 wt%) (A: BFS, B: SS, C: PG, and D: P.O 42.5): (a) A = 53.82
wt%, (b) B = 10.36 wt%, (c) C = 10.36 wt, and (d) D = 25.36 wt%.
Table 6
Optimization of composite materials in stabilized soil.
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The formula optimization of the composite materials in stabilized soils was carried out separately by the GA and HCA. The optimal
solution of composite materials formula in stabilized soil by the DOD and Hybrid DOD-GA along with validated results are shown in
Table 7. The hybrid DOD-GA approach predicted the maximum UCS of 3.46 MPa when the BFS was 56%, SS was 13.52%, PG was
14.87%, P.O 42.5 was 15.51%, and SP was 0.1%. In the contrast, the DOD predicted the maximum UCS of 3.45 MPa when the BFS was
59.75%, SS was 3.07%, PG was 14.81%, P.O 42.5 was 22.27%, and SP was 0.1%. The UCS of the optimal solution given by the DOD
technique was 3.12 MPa, with a mean absolute percentage error (MAPE) of 10.56% and a root mean square error (RMSE) of 0.34.
Furthermore, the optimal solution of the hybrid DOD-GA approach was verified, with a UCS value of 3.70 MPa, an MAPE of 6.99%, and
an RMSE of 0.24. Both the MAPE and RMSE of the experiment results of the hybrid DOD-GA technique were lower than those of the
DOD approach. Furthermore, the strength was greater than that obtained by the DOD technique. This demonstrated the better pre
diction ability of the hybrid DOD-GA technique for the UCS.
4. Evaluation
The formula from the hybrid DOD-GA technique was 56% BFS, 13.52% SS, 14.87% PG, 15.51% P.O 42.5, and 0.1% SP. A group of
cement–soil samples was prepared to evaluate the properties of the new solidified soil. The proportion of the curing agent added to the
wet silt was 20%. The experimental macroscopic and microscopic characteristics of the two types of stabilized soil were examined
based on the UCS, SEM, and XRD results, as shown in Figs. 13–15 respectively.
3Ca(OH)2 + Al2 O3 +3CaSO4 · 2H2 O + 23H2 O → 3CaO · Al2 O3 · 3CaSO4 · 32H2 O (11)
It speculated that the reason for the absence of portlandite in the new curing agent-stabilized soil was that the hydration products of
P.O 42.5 and BFS reacted with PG to generate ettringite. In previous studies, the main mass loss of ettringite was concentrated in 90 ◦ C
and 450 ◦ C in the [58–60]. However, ettringite was not detected in the new curing agent stabilized soil possibly due to ettringite being
transformed into amorphous product after drying [61]. In addition, Bragg’s equation was introduced to calculate the interplanar
spacing of the C-S-H [62]. The interplanar spacing of the C-S-H in the cement silt was greater than that of the stabilized silt obtained by
the DOD-GA method, indicating a more compact structure in the optimal solidified silt.
The -COOH in the SP yielded strong adsorption, and the cement particles were dispersed due to electrostatic repulsion. The free
water trapped in the cement condensate was released. As shown in Eqs. (10) and (11), the free water was converted into bound water in
the formation of ettringite, leading to the strength increment of the new curing-agent-solidified soil. Based on Fig. 15, the clubbed
hydrate and acicular hydrate were speculated to be ettringite. Although the XRD could not detect ettringite being transformed into
amorphous product during drying, the initial form of ettringite in the cementitious matrix was retained [61]. The clubbed and acicular
ettringite embedded in the flocculent hydrate formed a spatial network structure. At 1000 × magnification, the particles of the new
curing-agent-stabilized silt were denser and more ordered than those of the cement-stabilized silt. Locally magnified to 3000 × , the
new curing-agent-stabilized silt developed a large amount of clubbed ettringite and flocculent hydrate (C-S-H) that filled the pores,
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Table 7
Optimal solution and validated results of composite material formula in stabilized soil by D-optimal design (DOD) and Hybrid D-optimal design–genetic algorithm
(DOD-GA).
A B C D E
DOD 59.75 3.07 14.81 22.27 0.1 3.45 3.12 0.34 10.56
Hybrid DOD-GA 56.00 13.52 14.87 15.51 0.1 3.46 3.70 0.24 6.99
Fig. 14. Phase identification of the stabilized soils cured for 7 days: (a) optimal stabilized soil and (b) cement-stabilized soil.
which significantly improved the integrity (Fig. 15(a)). As for the cement-stabilized silt, there were small quantities of flocculent
hydrate and acicular crystals distributed on the surface, forming a weak reticular structure. The particles were observed to be
distributed in a disordered fashion, and the cement-stabilized silt particles exhibited weak cementation with more pores (Fig. 15(b)).
In summary, the regularity of the microstructure and macroscopic strength of the two kinds of solidified soil was fairly high
consistency. The new curing agent was more successful in enhancing the microstructure and strength of the silt than the cement was.
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Fig. 15. SEM images of the solidified soils at 1000 × and 3000 × magnification: (a) optimal stabilized soil and (b) cement-stabilized soil.
of diesel was obtained from the China Energy Statistics Manual [65]. The transportation distance was defined as the distance between
the raw material sources and the factory, and GWPs in the transportation stage are shown in Table 9.
The PG was transported to the plant and calcined at a temperature of 120◦ C-180◦ C [66]. The calcination reaction equation is as
follows:
120∘ C− 180∘ C
CaSO4 ⋅ 2H2 O ̅̅̅̅̅→ CaSO4 ⋅ 1 / 2H2 O + 3 / 2H2 O (12)
The theoretical enthalpies and GWPs of the PG calcination at different temperatures are shown in Table 10. The energy conversion
rate and the calcination conditions were set to 10% and 150◦ C for 1 h in this study, respectively [66]. The BFS, SS, and P.O 42.5 were
poured into the milling equipment for processing after the calcination of PG. With the 2100 mm (diameter) × 3000 mm (length) Red
Star ball mill equipment, the required power of the 1-ton curing agent was 7.29 kW•h. According to the survey statistics of the China
National Climate Strategy Center, the grid emission factor in east China is 0.7921 t CO2/MW•h. The GWPs of the manufacturing stage
are shown in Table 11.
Fig. 16 shows the environmental impact data of the new curing agent in each stage. It demonstrates that the GWP value of the raw
material production stage of the new curing agent was the largest proportion of the total LCA (i.e., 92.2%), followed by the
manufacturing stage (i.e., 4.2%). The P.O 42.5 and BFS made a significant contribution to the GWP of the raw material production
stage. As can be seen from Table 12, the GWP of the 1-ton new curing agent was 221.853 kg, while that of 1 ton of cement was 3.38
times that of the former at 750 kg.
Overall, the environmental impact of the new curing agent production was mainly from the raw material production stage, ac
counting for 92.2%, which was much less than that of cement production. Furthermore, the strength of the new curing-agent-stabilized
soil was 3.70 MPa at the curing age of 7 days, compared to 2.53 MPa for cement, further demonstrating the superiority of the new
curing-agent-stabilized soil over cement soil in terms of the strength and environmental benefits.
Table 8
Global warming potentials (GWPs) of the production of the raw materials.
Raw materials 1 ton of optimal soil hardening agent/kg GWP/kg CO2-eq References
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Table 9
GWPs of the transportation stage.
Raw 1 ton of optimal soil Distance/ Fuel consumption of 100-km truck Default value of Calorific value of GWP/kg
materials hardening agent/kg km with 30-ton load CO2/kg•GJ− 1 China/kcal•L− 1 CO2-eq
Table 10
Theoretical enthalpies and GWPs of PG calcination at different temperatures.
Raw Calcination Theory of enthalpy/ Energy exchange Calorific value of CO2 default value of GWP/kg
materials temperature/◦ C kJ•mol− 1 efficiency anthracite/kg•GJ− 1
anthracite/kcal•L− 1 CO2-eq
Table 11
GWPs of the manufacturing stage.
Raw materials 1 ton of optimal soil hardening agent/kg GWP of calcination/kg CO2 eq Grinding and mixing/kg CO2 eq GWP/kg CO2 eq
Fig. 16. Environmental impact data of each stage of the new curing agent.
5. Conclusions
In this study, 20 groups of mixture designs were prepared by the D-optimal method to explore the effects of BFS, SS, PG, and P.O
42.5 on the solidified soil’s UCS. The following conclusions can be drawn:
(1) The BFS and PG exhibited a positive effect on the UCS within a certain range, and the SS made little contribution to the sta
bilized soil’s UCS in the early stage. The maximum UCS was achieved at an optimal content ratio of the blast furnace slag to the
cement. The ANOVA results and diagnostics demonstrated that the Scheffé quadratic regression model was competitive in
predicting the UCS of the stabilized soil.
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Table 12
GWPs of 1 ton of curing agent.
(2) The verified strength of the solidified soil optimized by the hybrid DOD-GA technique was greater than that by the DOD
technique (UCS = 3.70 MPa for DOD-GA and UCS = 3.12 MPa for DOD), with a lower MAPE and RMSE (MAPE = 6.99% and
RMSE = 0.24 for the DOD-GA; MAPE = 10.56% and RMSE = 0.34 for the DOD).
(3) The optimal stabilized soil exhibited a greater compressive strength and breaking strain than the cemented soil. The soil
particles stabilized by the new curing agent were denser and filled more orderly, with a large amount of clubbed ettringite and
flocculent hydrate (C-S-H) in the pores, which significantly improved the integrity. The features of the microstructure and
macroscopic strengths of the two kinds of solidified soil showed fairly high consistency.
(4) The GWP of 1 ton of cement was 3.38 times that of 1 ton of the new curing agent. The new curing agent is more capable of
achieving improved strength, microstructure, and environmental benefits than cement is.
Overall, the observed industrial waste can be considered to be a substitute for cement to mitigate global warming. The optimized
curing agent has significant potential for industrial waste recycling, greenhouse buffering, and natural resource conservation.
This study examined the early strengths of solidified soils. However, the long-term strength is also essential to guarantee the en
gineering safety. In the future, the impact of the curing age, dosage, organic content, and soil properties on the stabilized soil will be
investigated systematically to provide more scientific guidance for engineering.
Data availability
Acknowledgment
This work was supported by the National Natural Science Foundation of China (52178365) and the provincial research grant of
Zhejiang, China (2023C03142).
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