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Conceptual Design of a Kraft Lignin Biorefinery for the Production of Valuable Chemicals via Oxidative Depolymerization

Cite this: ACS Sustainable Chem. Eng. 2020, 8, 23, 8823–8829
Publication Date (Web):June 5, 2020
https://doi.org/10.1021/acssuschemeng.0c02945

Copyright © 2020 American Chemical Society. This publication is licensed under CC-BY.

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Abstract

Lignin is the most abundant aromatic biopolymer on Earth, and its aromatic structure makes it a promising platform for the production of biobased chemicals and other valuable building blocks. The valorization of lignin into chemicals currently presents a challenge, and its facilitation is key in the development of viable lignocellulosic biorefinery processes. This study presents a conceptual design for a recently demonstrated process for lignin oxidative depolymerization. Modeling, simulation, and analysis were performed based on experimental data to assess the viability of the process. Mass and energy balances and main design data were determined for a 700 t/y kraft lignin biorefinery. The production capacity of aromatic chemicals, including vanillin, vanillic acid, guaiacol, and acetovanillone, was 0.3 kg aromatics/kg net lignin use. A heat-integrated process design is suggested, and the energy demands and the CO2 emissions are evaluated and compared. Assuming an interest rate of 10% and a plant lifetime of 10 years, the return on investment was calculated to be 14%, indicating that such a biorefinery is viable. A sensitivity analysis was carried out to assess the impact of the vanillin selling price and the cost of lignin on the profitability of the process. A quantitative investigation of process sustainability resulted in an E-factor of ∼1.6 for the entire synthetic route, that is, 38% material efficiency. The findings of this study underline the need for further research to develop efficient lignin conversion technologies with attractive yields in order to increase profitability on an industrial scale.

Synopsis

The economic viability of a process for the oxidative depolymerization of lignin as a renewable resource for sustainable chemical production is analyzed.

Introduction

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Lignin is the largest source of aromatic building blocks in nature and has significant potential as a raw material for the production of biobased products, allowing the replacement of fossil-derived materials. (1,2) It is found in most terrestrial plants, constituting 15–40% dry weight, and purveys structural integrity. (3,4) Because of its heterogeneity and recalcitrance, lignin is often treated as a waste byproduct and burned to produce energy. However, the efficient valorization of lignin is key in realizing more sustainable and competitive biorefineries, and the utilization of lignin as a resource for the production of chemicals offers an attractive opportunity. (5) The development of efficient process technologies for the conversion of lignin into value-added chemicals is thus of the utmost importance in biorefinery research. (6,7)
Kraft pulping is the main process used to produce paper pulp. Wood is transformed into pulp by cooking in a solution of Na2S/NaOH, the so-called white liquor, at a temperature of 155–175 °C for several hours. (8) About 90–95% of the lignin in the starting material can be dissolved through this process. (9) It has recently been estimated that the annual production of kraft pulp worldwide is about 130 million tons, (10) from which approximately 50 million tons of degraded lignin are liberated. (11,12) Lignin from kraft black liquor also represents a large share of the bioenergy sector in Sweden and Finland, (13,14) and new product chains based on exploiting kraft lignin from black liquor as a renewable source of aromatics are being encouraged.
Techno-economic evaluation of lignocellulosic biorefineries in general, and lignin biorefinery concepts in particular, is required to assess the commercial viability of novel and emerging technologies. Examples of such technologies include bio-oil stabilization and upgrading, (15) levulinic acid conversion, (16) the production of monosugars, (17) 5-hydroxymethylfurfural, (18) butadiene from furfural, (19) biodiesel from algal oil, (20) glycerol valorization, (21) and lignocellulosic ethanol. (22) Such studies revealed considerable variability in the feedstock and products derived from different biorefinery processes.
A limited number of studies have recently been carried out on the technical design and viability of novel lignin valorization processes. Energy and exergy calculations have been performed on catechol production based on lignin extracted from olive tree pruning. (23) Process intensification has been combined with simulation to compare different strategies for the production of vanillin/methyl vanillate from kraft lignin, for example, extraction with organic solvents, nanofiltration, and adsorption with zeolite; the last alternative shows additional savings in energy and cost of 0.2 and 7.4%, respectively. (24) Capacity design and risk analysis of biophenol/resin production from kraft lignin have also been presented, (25,26) demonstrating that the viability of such a biorefinery depends on the selling price of the product on the market and variations in the cost of lignin. The techno-economics of large-scale production of colloidal lignin particles, involving solubilization with tetrahydrofuran and ethanol, has also been assessed, where an internal rate of return of 17% was reported. (27) In another study, the feasibility of synthesizing lignin micro- and nanoparticles via an aerosol/atomization method has been evaluated, where manufacturing costs were quoted as being in the range of 600–1170 $/t. (28) Three lignin conversion routes to biobased aromatics have been analyzed: noncatalytic pyrolysis, hydrothermal upgrading, and direct hydrodeoxygenation; the last route is found to be the most economically promising. (29)
Life cycle assessment (LCA) studies have also been carried out on lignin-based processes to assess their environmental impact. An LCA of catechol production from lignin contained in candlenut shells has been performed, (30) showing an overall reduction in the environmental footprint of this route, compared to the conventional production from petrochemicals. LCA of adipic acid production from lignin has also been performed, in which reductions in greenhouse gas emissions of 62–78% were predicted for the biobased route, compared to conventional production of adipic acid. (31) Techno-economic analysis and LCA are essential when introducing a developing technology onto the market, to provide information for investment purposes, and to identify whether additional research is needed prior to implementation.
In the present study, the experimental work reported by Abdelaziz et al. (32) was used as a basis for the design and techno-economic evaluation of large-scale production of valuable chemicals from lignin. The oxidative depolymerization of industrial kraft lignin, extracted using the LignoBoost technology, to provide low-molecular-weight compounds suitable for microbial conversion was described. We investigate the viability of chemical production preceding biological funneling as another possible route for lignin processing. Novel process configurations were developed using Aspen Plus software. Economic and environmental analyses were performed, and process profitability was evaluated using different price ranges of lignin and products.

Methods

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The process design was based on first-hand experimental data, obtained from a study on the oxidative depolymerization of kraft lignin as a means of pretreatment for microbial conversion. (32) Briefly, kraft lignin precipitated using the LignoBoost technology was treated with molecular oxygen under different reaction conditions to identify the best conditions for obtaining a biocompatible, oxidatively depolymerized lignin stream. The reactions were also performed under mild alkaline conditions to ensure solubilization of the lignin. However, the addition of sodium hydroxide was not included in process simulation because of the possibility of using the sodium hydroxide material stream available in a pulp mill as an active cooking chemical. The feed to the process was rather assumed to be in the form of weak black liquor. The highest yield of aromatic monomers was obtained at 160 °C and 3 bar oxygen partial pressure (Table S1), and this product slate was found to be suitable for conversion by several microbial species. Carboxylic acids were also generated from the reaction and are treated here as useful coproducts.
An opportunity for scaling up the production of biobased chemicals from the lignin material was investigated to enable assessing the economic viability of such a biorefinery. The underlying goal was to identify the process limitations and to determine whether the process would be of commercial interest. The major aromatic compounds generated by this process include vanillin, vanillic acid, acetovanillone, and guaiacol, while the carboxylic acids were primarily composed of formic and acetic acids. This process was designed to be integrated into an existing pulp and paper mill. A simplified block flow diagram of the proposed process modeled in this study is presented in Figure 1.

Figure 1

Figure 1. Simplified block flow diagram of the lignin oxidative depolymerization process.

Process Simulation

Aspen Plus V10 software was used to simulate the process of oxidative depolymerization of lignin into aromatic chemicals and carboxylic acids. Mass and energy balances were calculated in the Aspen Plus simulation environment after specifying the input streams and unit operations. The proposed biorefinery was assumed to have an input of about 700 metric tons of lignin per annum, excluding feedstock streams recovered within the process, which is almost 10% of the production from LignoBoost lignin. The RISE lignin plant (LignoDemo), located at Bäckhammar in Sweden, can produce up to 8000 t/y of high-quality LignoBoost kraft lignin (the raw material used in our experimental work), which is then used as a raw material for the production of biofuels, chemicals, and other materials.
The phenolic compound 2-methoxy-4-propylphenol (C10H14O2) was used as a model for lignin. (33) The thermodynamic model used to describe the phase equilibrium between different components of the process was the nonrandom two-liquid (NRTL) property model. Simulations included the Mixer, Pump, Compr, Heater, HeatX, Valve, RStoic, Flash2, Sep, and RadFrac modules. The main reactions defined for the stoichiometric reactor simulation were as follows
(1)
(2)
(3)
(4)
(5)
(6)
(7)

Energy and Environmental Analyses

The total utility requirements to satisfy the heating and cooling demands in the process flowsheets were calculated using Aspen Energy Analyzer. In the design of the base case, the available energy savings were identified by comparing the actual energy demands with the energy targets. Furthermore, a heat integration scheme was proposed with the objective of maximizing the process-to-process heat recovery, thus minimizing the total utility requirements.
The amount of CO2 emitted corresponding to burning a certain amount of fuel, Qfuel, was estimated for the base case and the heat-integrated design using the equation below
(8)
where α is the ratio of the molar masses of CO2 and carbon (=3.67). NHV denotes the net heating value, and values of 39,771 and 51,600 kJ/kg were used for heavy fuel oil and natural gas, respectively, while the carbon contents C % (dimensionless) were set to 86.5 and 75.4, respectively. (34,35)

Economic Evaluation

Stoichiometric–economic targeting (also referred to as stoichionomic targeting) was used to provide benchmarks for the flows of reactants and products. (36) Together with chemical pricing data, this tool is useful in making early-stage decisions regarding a proposed process design. The metric for inspecting sales and reactants (MISR) was used to determine whether the process had the potential for economic viability or not, defined as
(9)
where Fp is the annual production rate of product p, Sp is the selling price of product p, Fr is the annual feed rate of reactant r, and Cr is the cost price of reactant r. If MISR >1, the process may be considered for more detailed analysis, although higher values of MISR are desirable. If MISR <1, the process is not desirable from an economic perspective.
CAPCOST, a software tool for capital cost estimation based on the equipment module costing method, (37) was used for detailed analysis to calculate the total capital and operating costs and to assess the economic viability of the proposed process designs. The direct and indirect project expenses were included in the capital cost estimates by multiplying a bare module factor by the cost of the purchased equipment. All costs were estimated in US dollars (US$) and updated to 2019 prices, considering the annual Chemical Engineering Plant Cost Index (CEPCI). As the plant was assumed to be geographically located in Sweden, a corporate tax rate of 21.4% was applied. The return on investment (ROI) and net present value (NPV) were the indices calculated to assess the profitability of the proposed process designs. The major assumptions used in the techno-economic evaluation are summarized in Table S2.

Results and Discussion

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Mass and Energy Balances

A computer simulation model was developed to perform the mass and energy balance calculations, based on the block flow diagram in Figure 1. The process includes several parts, that is, lignin conversion, gas and solid separation, membrane filtration, and product recovery. The process flow diagram is depicted in Figure 2.

Figure 2

Figure 2. Process flow diagram for the conversion of lignin to aromatics and acids via oxidative depolymerization.

The lignin, in the form of weak black liquor (stream 1 in Figure 2), is heated to 174 °C before mixing with air at a pressure of 8.5 bar (stream 5). The combined stream (stream 6) is sent to a reactor (R-101), which is operated at about 160 °C and 8 bar. The reactor effluent (stream 7) is cooled to 100 °C in a heat exchanger (E-102). The effluent stream is then flashed in two flash drums (V-101 and V-102) to separate the noncondensable gases from the liquid products, while the off-gas (stream 10) is possibly sent for purification.
The liquid product mixture (stream 16) is sent to a membrane filtration unit (ME-101), where any unreacted lignin is recovered as retentate (stream 17). The permeate is sent to a hydrophobic membrane separator (ME-102) that selectively removes the organics from the aqueous stream. Such a membrane technology concept has been a subject of interest in recent research owing to the highly efficient separation of organics and ease of operation. (29) The retentate from ME-102 (stream 20) is combined with stream 17 and recycled to the pulp mill. The remaining organic fraction in aqueous solution (stream 21) is separated from water in a distillation column (T-101), and the water is returned to the mill (stream 26). The bottoms (stream 29) are sent to a second distillation column (T-102), where the carboxylic acids (formic and acetic acid, stream 33) are separated from the low-molecular-weight aromatic products (stream 37).
Based on the simulations obtained from the model, mass and energy balances were evaluated for the oxidative lignin depolymerization process. Data related to the main process streams of the base case, including component flows, conditions, and so forth, are given in Table S3.
Heat integration was then applied to the base case, and an additional heat exchanger unit was added to recover the excess energy in the process. The location of the new heat exchanger was upstream of E-101 for the cold-side fluid and upstream of E-102 for the hot-side fluid. Consequently, E-101 could be operated at a lower heating duty requirement, and the cooling duty of E-102 was reduced.

Process Analysis and Sustainability

The energy and environmental performance of the various process configurations were analyzed and compared. A considerable proportion of the process operating costs is attributed to the heating and cooling duties, both of which can be minimized by means of heat integration. Figure 3 shows the total utility consumption of the base case and the heat-integrated case. Heat integration reduced the energy demands for heating and cooling utilities by 22% and 21%, respectively.

Figure 3

Figure 3. Energy demands in the lignin oxidative depolymerization process in the base case and heat-integrated design.

Furthermore, heat integration led to a reduction in CO2 emissions (Figure 4). The environmental analysis was based on the amount of CO2 emitted by the combustion of fuels powering the process. The reduction in CO2 emissions, compared to the base case, was 9500 or 14,100 kg/d, depending on whether the fuel used was natural gas or heavy fuel oil, respectively. The heat-integrated process design of this lignin biorefinery thus provides a more sustainable option from both the energy and environmental perspectives.

Figure 4

Figure 4. Daily CO2 emissions from the lignin oxidative depolymerization process in the base case and the heat-integrated design.

Sheldon’s environmental factor (E-factor) was used to quantify the sustainability and greenness of the proposed process. (38) The amount of waste generated per kg of the product produced can be calculated with the E-factor, allowing the material efficiency, a metric used for the production of commodity chemicals from biomass, to be estimated. Material efficiency is defined as the total mass of useful products divided by the total mass of useful products + waste.
The useful products in this study were defined as the carboxylic acids (formic and acetic acid) and the aromatic monomers (vanillin, vanillic acid, guaiacol, and acetovanillone). The main waste steam in the process was stream 10, the off-gas, where the CO2 emission amounted to 2138 kg/d. This corresponds to an E-factor of ∼1.6, a value in the range of a bulk chemical sector. (38) This gave a material efficiency of 38%, which is an acceptable value for a biomass-based synthetic route. (39) Other metrics, such as ozone depletion, acidification, smog formation, and societal impact, can be evaluated through a detailed LCA, but this was beyond the scope of this study. Nonetheless, it should be stressed that the use of lignin as a renewable feedstock for biobased chemical production, rather than petroleum, is encouraging from a sustainability perspective.

Profitability Assessment

To assess the economic potential of this oxidative depolymerization process based on actual stoichiometric calculations, the stoichionomic indicator MISR was used. Actual product yields and separation losses were taken into account in these stoichiometric calculations. The effect of lignin cost on the MISR for the process is shown in Figure 5.

Figure 5

Figure 5. Effect of the cost of lignin on MISR in the oxidative depolymerization process.

The value at which the process becomes economically infeasible is at a lignin cost of 5600 $/ton. Under reasonable price scenarios for kraft lignin (250–750 $/ton), high values of MISR (>8) were obtained. A more detailed economic analysis, involving other costs, that is, capital cost, utilities, and so forth, was thus undertaken. The profitability of the two process schemes was evaluated based on the ROI and NPV. The key economic results for both scenarios are summarized in Table 1.
Table 1. Summary of Key Economic Results for the Lignin Oxidative Depolymerization Process
parameterbase caseheat-integrated design
total capital cost (MM$)6.536.69
cost of raw materials (MM$/y)0.170.17
utilities (MM$/y)1.631.28
product sales (MM$/y)4.064.06
NPV (MM$)3.584.97
ROI (%)10.3613.87
The total capital cost of the heat-integrated design was estimated to be about 2.5% higher than that in the base case. Figure 6 shows a cost breakdown, illustrating the contribution from each unit operation to the fixed capital investment. The air compressor unit was the most expensive component, contributing 49% to the total capital cost, followed by the heat exchangers, which contributed 24%. The main reason for the high cost of the air compressor was that a spare unit was included in the economic evaluation to provide operational flexibility.

Figure 6

Figure 6. Contributions of various pieces of equipment to the fixed capital investment.

On the other hand, a notable reduction in the cost of utilities was achieved by applying heat integration (22% compared to the base case), which in turn affected the overall profitability of the process. The NPV and the ROI of the base case were $3.6MM and 10.4%, respectively, while the corresponding values for the heat-integrated design were $5MM and 14%, respectively. Acceptable values of ROI for forest-based biorefineries have been reported to be 10–15%. (40) The acceptable value is considerably lower in Scandinavia than in other countries, indicating the potential of establishing forest biorefinery concepts.
A sensitivity analysis was performed to assess the impact of changes in the cost of feedstock and product selling price on the profitability of the process (Figure 7). The ROI is plotted against the selling price of vanillin, ranging from $15/kg to $40/kg, and a lignin cost ranging from $0.25/kg to $0.75/kg, for the two designs considered.

Figure 7

Figure 7. Sensitivity analysis for the ROI of (a) the base case and (b) the heat-integrated design, for various lignin costs.

Under pessimistic conditions, that is, a lignin cost of $0.75/kg and a vanillin selling price of $15/kg, rather low, but still positive, ROIs were obtained: 1.6% for the base case and 5.3% for the heat-integrated design. The selling price of vanillin had a strong influence on the ROIs of both process configurations. In a favorable scenario (a lignin cost of $0.25/kg and a vanillin selling price of $40/kg), the ROI was quite high for both configurations (≥29%). The heat-integrated design exhibited an average increase in ROI of approximately 3.4% compared to the base case at the higher lignin cost.
The process described in this study is still in its infancy, and there is a rather high degree of uncertainty concerning the value of the products generated. The commercial application of lignin depolymerization and upgrading technologies is still limited, which can lead to uncertainties in the modeling and investment cost calculations. (29,41) However, the assessment of such early-stage technologies is desirable as this could provide insights into potential drivers, barriers, targets, and impacts on further technological development. The present work contributes to the knowledge on the thermochemical transformation of lignin to value-added chemicals, which will be useful in the subsequent improvement of the process in the context of environmental and economic sustainability.

Conclusions

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The substitution of nonrenewable fossil resources with renewable biomass as the principal raw material for producing chemicals is a crucial goal of green chemistry and engineering. In this study, we have evaluated the techno-economic viability of biochemical production from kraft lignin as a renewable feedstock via oxidative depolymerization. Process synthesis, simulation, and integration formed the basis of the analysis and the assessment of the potential viability with respect to vanillin production. The process was evaluated on a scale of 700 t/y of fresh lignin feed. After heat integration, and assuming a cost of lignin of $250/ton, the process was deemed economically viable, with values of ROI in the range of 9–32%, based on the product selling price. It is suggested that the process be colocated and integrated with an existing pulp and paper mill, as this will significantly reduce the overall operating costs. Work is ongoing to improve the yield and selectivity toward vanillin employing different catalytic systems. This early-stage process analysis provides a sounder base for the practical realization of an integrated facility for valorizing lignin waste streams into value-added chemicals, which also speaks for providing environmental benefits.

Supporting Information

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The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acssuschemeng.0c02945.

  • Data related to the product parameters, the techno-economic assumptions, and the various streams in the lignin oxidative depolymerization process (PDF)

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Most electronic Supporting Information files are available without a subscription to ACS Web Editions. Such files may be downloaded by article for research use (if there is a public use license linked to the relevant article, that license may permit other uses). Permission may be obtained from ACS for other uses through requests via the RightsLink permission system: http://pubs.acs.org/page/copyright/permissions.html.

Author Information

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  • Corresponding Author
  • Authors
    • Omar Y. Abdelaziz - Department of Chemical Engineering, Lund University, Naturvetarvägen 14, 221 00 Lund, SwedenOrcidhttp://orcid.org/0000-0002-3530-3509
    • Abdulrahman A. Al-Rabiah - Department of Chemical Engineering, King Saud University, 3 King Khalid Rd, Riyadh 11421, Saudi Arabia
    • Mahmoud M. El-Halwagi - The Artie McFerrin Department of Chemical Engineering, Texas A&M University, 100 Spence Street, College Station, Texas 77843-3122, United StatesOrcidhttp://orcid.org/0000-0002-0020-2281
  • Notes
    The authors declare no competing financial interest.

Acknowledgments

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This work was supported by the Swedish Foundation for Strategic Research (RBP14-0052), the Swedish Energy Agency (45241-1 and 49701-1), and the Södra Research Foundation (2019-149). A.A.A. acknowledges financial support from the Research Center at the College of Engineering, Deanship of Scientific Research, King Saud University.

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  • Abstract

    Figure 1

    Figure 1. Simplified block flow diagram of the lignin oxidative depolymerization process.

    Figure 2

    Figure 2. Process flow diagram for the conversion of lignin to aromatics and acids via oxidative depolymerization.

    Figure 3

    Figure 3. Energy demands in the lignin oxidative depolymerization process in the base case and heat-integrated design.

    Figure 4

    Figure 4. Daily CO2 emissions from the lignin oxidative depolymerization process in the base case and the heat-integrated design.

    Figure 5

    Figure 5. Effect of the cost of lignin on MISR in the oxidative depolymerization process.

    Figure 6

    Figure 6. Contributions of various pieces of equipment to the fixed capital investment.

    Figure 7

    Figure 7. Sensitivity analysis for the ROI of (a) the base case and (b) the heat-integrated design, for various lignin costs.

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