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Preparation and characterization of sorbents from food waste

  • Barbora Grycova

    Barbora Grycova studied Economics in Metallurgy and Metallurgy at VSB Technical University of Ostrava and obtained her PhD degree in 2012 at VSB Technical University of Ostrava (field of study: thermal technology and fuels in industry). She is a junior researcher and lecturer at the Institute of Environmental Technology, VSB Technical University of Ostrava and interested in the field of thermal engineering, e.g. new generation biofuels and activated carbon production by pyrolysis and gasification.

     EMAIL logo     , Adrian Pryszcz

    Adrian Pryszcz MSc studied Environmental Technology at the Institute of Chemical Technology, Prague and obtained his MSc degree in 2007. He is a PhD student at the Institute of Environmental Technology, VSB Technical University of Ostrava and interested in the field of thermal engineering, e.g. new generation biofuels and activated carbon production by pyrolysis and gasification.

         , Pavel Lestinsky

    Pavel Lestinsky studied Process Engineering at VSB Technical University and obtained his PhD in 2013. He is a senior researcher and lecturer at the Institute of Environmental Technology, VSB Technical University of Ostrava and interested in the field of chemical engineering, e.g. gas and flue gas cleaning, mathematical modeling of the transport phenomena (by Matlab, Comsol, Fluent), simulation of chemical processes (by Aspen Plus) or new generation biofuel production by pyrolysis.

         and Katerina Chamradova

    Katerina Chamradova studied at the Faculty of Mining and Geology, VSB Technical University of Ostrava and obtained her PhD degree in 2012 from VSB Technical University of Ostrava (field of study: environmental protection within industry). She is a junior researcher and lecturer at the Institute of Environmental Technology, VSB Technical University of Ostrava and a member of the anaerobic digestion team. She is interested in the field of anaerobic digestion, in particular use of food waste by anaerobic treatment.
Published/Copyright: February 28, 2017
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Green Processing and Synthesis
From the journal Green Processing and Synthesis Volume 6 Issue 3

Abstract

Waste coffee was treated by pyrolysis in the conventional laboratory apparatus at 800°C. Afterwards, a mass balance of the final yields, gas chromatographic analysis and assessment of solid and liquid residues were done. The selected waste material was also subjected to microwave pyrolysis in terms of adsorbents preparation. The solid residues were further activated with potassium hydroxide. Final characterization of prepared sorbents was made by sorption of nitrogen at 77 K. Activated sorbents had much better sorption properties. The surface area according to Brunauer-Emmett-Teller (BET) theory of activated material (from conventional pyrolysis) was measured 1794 m2·g−1.

Keywords: activated carbon; food waste; pyrolysis

1 Introduction

An enormous amount of food waste is produced in the world. These recyclable wastes threaten the localities due to depositing wastes in landfills, which are known to produce carbon dioxide, methane and other contaminated elements. In particular, methane is classified as the most plentiful greenhouse gas. Because of the Directive No. 1999/31/EC on the waste landfilling [1], pressure to decrease the quantity of recyclable waste placed in landfills until 2020 to 35 wt. % of the weight of this type of waste produced in 1995 is growing. Usually, wastes from food processing are constantly stereotypically placed in landfills; a trivial amount is utilized for fattening intents and for biogas performance [2, 3], or compost [4]. Lipid originating from these wastes could be transformed to biodiesel [5, 6]. Furthermore, a comprehensive carbohydrate such as cellulose plus starch may be hydrolyzed to glucose and fructose and these sugars may be converted to bioethanol by fermentation later on [7, 8].

Pyrolysis is demonstrably an original form of application technique related to waste that converts less valuable material to higher value outputs [9]. Pyrolysis has been utilized for production of charcoal from biomass for thousands of years. At present, a trendy approach is rising up in the manufacture of low-cost adsorbents from biomass and numerous food waste inputs on a commercial basis. Activated carbons (ACs) are extremely permeable substances with the required surface characteristics [10], which are widely used in various fields of purification and industrial processes [11]. For that reason, the demand for ACs is constantly growing. New invention methods and the use of low-priced raw materials have been considered [12]. Conventional heating is one of the most appropriate methods used for preparation. As a substitute heating method, microwave irradiation has created hopeful results recently in this area [13, 14]. Microwave heating provides many benefits in comparison with conventional heating, such as non-contact prompt heating, energy transmission instead of heat transmission, quick start-up and stopping, advanced level of protection and mechanization [15].

Basically, physical activation and chemical activation are used to obtain ACs. The enormous interest in the research area belongs to chemical activation due to a number of benefits equated to the so called physical activation, e.g. lower temperatures for process, extremely high surface area, etc. Between the weaknesses of this procedure, the process corrosiveness and the washing phase are to be noted. The chemicals mostly used are alkali (potassium hydroxide, sodium hydroxide), alkali earth metal salts (aluminum chloride and zinc chloride) and some acids (phosphoric acid and sulfuric acid). These chemicals are dehydrating representatives supporting pyrolytic decomposition and suppressing the tar creation. KOH and ZnCl2 belong to among the most frequently used compounds for the production of sorbents [16]. Universally, physical activation covers a carbonization and activation stage. For activation, steam and carbon dioxide are the most shared elements, pronouncedly prompting the porosity of the resulting material [17]. Most predecessors which are practical for the production of ACs are organic carbon-rich materials. Natural wastes can be taken into account to be a very meaningful feedstock for this production due to their availability and renewability. During the last several years, there has been growing interest in research with the use of renewable and lower priced precursors. A significant portion of research has been stated on ACs from agricultural and food wastes, such as walnut shell [18], coconut shell [19, 20], almond shell [21], acavia mangium wood [22], rice husk [23, 24], mung bean husk [25], buriti shell [26], edible fungi residue [27], coffee husk [28], coffee ground [29, 30], tea industry waste [31, 32], olive-waste cake [33], etc.

Authors of the study [34] assessed the pyrolysis process with regard to syngas and hydrogen flow rates, complete gas and hydrogen yields, and also apparent thermal effectiveness. The outcomes prove that food waste provides a worthy potential for compact waste thermal handling with the exact target of power generation. Energy generation based on the food waste by means of digestion with subsequent pyrolysis was also evaluated [35].

In this study waste coffee was pyrolyzed in the conventional pyrolysis apparatus at a maximum temperature of 800°C and also in the microwave reactor with power of 400 W. The solid residues were further activated with KOH. Final characterization of prepared sorbents was made by sorption of nitrogen at 77 K.

2 Materials and methods

2.1 Material

For the measurement, a sample of waste coffee was selected: WaCo (Cervus Inc.)

The production of this waste is counted in tonnes per week. Most of this waste is landfilled. WaCo was analyzed by thermogravimetry and differential scanning calorimetry with the use of the unit STA 409C (Netzsch, Selb, Germany) on 18-414/4 in an atmosphere of helium, with two heating rates of 10 K·min−1 and 20 K·min−1. Thermo-analytical techniques are specific methods to determine mass loss properties which are necessary for understanding the pyrolysis kinetics in an easy way [36, 37]. Elemental analysis was performed with the use of the LECO CHSN628 (LECO, Saint Joseph, USA). The higher heating value HHV was measured based on ISO 1928 with the use of the calorimeter LECO AC-350.

2.2 Laboratory devices

Laboratory apparatuses assembled for the purpose of experiments are shown in Figure 1. In the case of conventional pyrolysis, an appropriate quantity of sample (200 g) was weighed and placed into the prepared retort. The retort with length of 30 cm and inner diameter of 5.5 cm was tightly fastened, positioned into the furnace and connected to other components of the apparatus. A gasometer was placed at the end of the apparatus. The final temperature of 800°C was chosen. Nitrogen was used for inertization.

Figure 1: Microwave and conventional apparatus.
Figure 1:

Microwave and conventional apparatus.

The sample was also treated in the microwave reactor for 20 min at a power of 400 W and frequency of 2450 MHz, which corresponds to a temperature of 800°C. A hole was cut out in the upper part of the PANASONIC NN-SD271 microwave for placing a flask with the sample into the microwave. The flask was connected with a glass tube with a cooler. After the cooler, there were washing bottles and a gasometer placed (same as in conventional pyrolysis). Microwave heating was used only in terms of adsorbents preparation (the gas and liquid products were not subjected to other determination).

2.3 KOH activation

The sample was treated in a two-stage process which was found to be very effective for preparation of porous carbons with high surface area from biodegradable waste materials [24, 32]. The residues from conventional and microwave pyrolysis were further activated with potassium hydroxide, which is described as the best activation agent. Different activation agents such as KOH (1835 m2·g−1), NaOH (1558 m2·g−1), K2CO3 (1579 m2·g−1) and Na2CO3 (660 m2·g−1) were utilized in the study [18] to identify a suitable activation agent. The result indicated that KOH was the most suitable activation agent among those agents, with the highest porosity and surface area of AC. Also the impregnation ratio of KOH has a strong effect on the characteristics of activated char, as is disclosed by Khezami et al. [38]. The char was mixed with KOH, in a ratio of 1:4, which is suggested in literature to be the optimum [24]. According to authors [30], higher KOH concentrations consistently produce a lower yield of product with a much larger surface area.

Such prepared mixtures were then thermally treated in an inert atmosphere of nitrogen at 800°C for 1 h. Authors [39] confirm that Brunauer-Emmett-Teller (BET) surface areas of carbons increase with activation temperature. After cooling, the activated samples were neutralized, filtered and finally washed. For neutralization, hydrochloric acid was applied. After drying, the activated samples were ready for subsequent surface analysis.

2.4 Characterization of solid residues

Basic determination of solid residues of pyrolyzed samples was done to define the sorption capacity. The true density was analyzed with the use of an automatic pycnometer PYCNOMATIC ATC (Thermo Fisher Scientific, Waltham, USA) by using helium as a carrier gas. The specific surface area of the samples was evaluated using two methods; the single point measurement at P/P0=0.2 and the BET method. Final characterization of prepared sorbents was made by sorption of N2 at 77 K. Measurement was carried out on a 3Flex Surface Characterization (Micromeritics Instrument Corporation, Norcross, USA) Analyzer (Micromeritics). Ahead of the nitrogen physisorption measurements, the activated samples were degassed at 300°C for 24 h under vacuum less than 1 Pa. The iodine adsorption number according to the standard DIN 53 582 was measured for further characterization of microporous structure.

3 Results and discussion

For the sample, proximate and ultimate analyses were carried out (see Table 1); thermogravimetry (TG) and differential scanning calorimetry curves (DSC) curves are presented in Figure 2.

Table 1:

Proximate and ultimate analysis.

SampleW(r) (wt. %)A(r) (wt. %)V(r) (wt. %)C(r) (%)H(r) (%)N(r) (%)S(r) (%)O(r) (%)HHV(r) (MJ·kg−1)LHV(r) (MJ·kg−1)
WaCo2.52.975.746.76.81.20.140.320.919.5

  1. A, ash; C, carbon; H, hydrogen; HHV, higher heating value; LHV, lower heating value; N, nitrogen; O, oxygen; (r), original sample; S, sulfur; V, volatile matter; W, moisture.

Figure 2: TG and DSC.
Figure 2:

TG and DSC.

The mass balance of the pyrolysis experiment was done according to the weight of the resulting products (solid residue, liquid residue). The process temperature significantly affected the distribution of final products. Solid residue yield decreased with rising temperature; on the other side, desired properties were achieved at higher pyrolysis temperature. Solid residue yield (30 wt. %) was dependent on the working temperature and heating rate which corresponds with authors [40].

3.1 Analysis of gaseous products

The pyrolysis gas was analyzed with the use of the Agilent 7890A (Agilent Technologies, Santa Clara, USA) gas chromatograph equipped with flame ionization and thermal conductivity detector. A significant amount of publications are focused on hydrogen production [41]. Hydrogen evolution was strongly influenced by increasing temperature, as expected. The maximum concentration of measured hydrogen (56 vol. %) was analyzed during the third gas sampling at a temperature from 700°C to 800°C. The amounts of measured hydrocarbons and carbon monoxide reduced with the rising temperature, as disclosed by Kalinci et al. [42]. The gas formation gradually increased and peaked in temperature around 500°C (see Figure 3).

Figure 3: Gas evolution and composition.
Figure 3:

Gas evolution and composition.

3.2 Evaluation of solid residues in terms of adsorption properties

Table 2 demonstrates the values of ultimate and proximate analysis, SBET, t-Plot Micropore Area, iodine adsorption number and true density of activated and non-activated samples after conventional and microwave pyrolysis. In the case of non-activated samples, a very low value of the surface area (below 10 m2·g−1) was achieved in comparison with commercial ACs. This conclusion conforms to Mohan et al. [43]. The iodine number of the pyrolyzed sample after conventional pyrolysis was 280 mg·g−1. This value suggests an opportunity for usage of this waste in “single-use sorbents” production. The surface area of the carbonisates was subsequently activated to improve its removal efficiency (see Figure 4).

Table 2:

Proximate and ultimate analysis, SBET, t-Plot microarea, iodine adsorption number and density of activated and non-activated samples after conventional and microwave pyrolysis.

Conventional pyrolysis
 C(d) (wt. %)H(d) (wt. %)N(d) (wt. %)S(d) (wt. %)O(d) (wt. %)Ct(d) (wt. %)A(d) (wt. %)
 83.3n/82.5a0.4n/0.3a1.4n/2.9a0.1n/0.1a2.8n/2.2a88.0n/88.0a12.0n/12.0a
 V(d) (wt. %)FC(d) (wt. %)Yield (wt. %)SBET (m²·g−1)t-Plot MicroArea (m²·g−1)I (mg·g−1)ρ (g·cm−3)
 3.3n/11.5a84.7n/76.5a30.0n/19.53.2n/1794.0a9.4n/1128.0a280.0n/1437.0a1.8n/2.5
Microwave pyrolysis
 C(d) (wt. %)H(d) (wt. %)N(d) (wt. %)S(d) (wt. %)O(d) (wt. %)Ct(d) (wt. %)A(d) (wt. %)
 74.1n/73.8a2.7n/0.5a2.2n/1.2a0.1n/0.1a7.9n/4.9a87.0n/80.6a13.0n/19.6a
 V(d) (wt. %)FC(d) (wt. %)Yield (wt. %)SBET (m²·g−1)t-Plot MicroArea (m²·g−1)I (mg·g−1)ρ (g·cm−3)
 15.3n/13.5a71.7n/67.1a41.0n/26.7a2.9n/1044.0a3.3n/882.0a55.0n/1335.0a1.8n/2.4

  1. Indexn, non-activated sample/indexa activated sample; (d), anhydrous sample; C, carbon; H, hydrogen; N, nitrogen; S, sulfur; O, oxygen; Ct, total combustible; A, ash; V, volatile matter; FC, fixed carbon; SBET, (Brunauer, Emmett and Teller) surface area; t-PlotMicroArea, t-Plot micropore area; I, jodine adsorption number; ρ, density.

Figure 4: Adsorption isotherms of activated samples.
Figure 4:

Adsorption isotherms of activated samples.

3.3 Evaluation of activated solid residues

Activated samples had much better sorption properties. The surface area according to BET of activated material (from conventional pyrolysis) was measured 1794 m2·g−1(see Table 2). Surface area of sorbents prepared by microwave pyrolysis was measured as much lower in comparison with conventional pyrolysis. This could be caused by two differences. The first is that the temperature could change throughout the entire volume; there could be spots with higher temperature (hot spots) and also with lower temperature. Secondly the activation time in a microwave is shorter than in a conventional furnace.

Table 3 compares the characteristics with respect to sorption capabilities of some commercial and food/vegetable based ACs mentioned in the literature.

Table 3:

Comparison of adsorptive characteristics of activated carbons (ACs) reported in literature.

ACCommercial ACCoffee ground ACCoffee husk ACPine cone ACBuriti shell ACCoconut shell ACGrape waste AC
SBET (m²·g−1)1440925152218068435001455
References[44][29][28][44][26][20][44]
ACWalnut shell ACCoconut husk ACAcavia mangium wood ACOlive-waste cake ACEdible fungi residue ACAlmond shell ACRice husk AC
SBET (m²·g−1)1835135610401020684840516
References[18][19][22][33][27][21][23]

  1. AC, activated carbon.

These results show that WaCo could be a substitute precursor for the profitable AC production. It could be also engaged as an advantageous carbonaceous adsorbent for the removal cationic and anionic dyes from wastewater.

3.4 Rating condensates

The condensate from conventional pyrolysis (38 wt. %) was subjected to the determination of water content (76.8 wt. %) by the Karl-Fischer method on TitroLine 7500 KF (SI Analytics GmbH, Mainz, Germany). Among the most represented components analyzed in the condensate were lauric acid (29.5 rel. %), which could be used in the case of possible isolation in the manufacture of shampoos, liquid soaps and detergents, caprylic acid (9.2 rel. %), myristic acid (6.5 rel. %) and capric acid (6 rel. %). Caprylic acid could be used, for example in the treatment of bacterial infections, or in the production of esters for perfumery and myristic acid as an additive for cosmetic creams.

4 Conclusion

The selected food waste material was treated by pyrolysis in conventional laboratory apparatus at 800°C. Afterwards, a mass balance of the final yields, gas chromatographic analysis and assessment of solid and liquid residues were done. Waste coffee was also subjected to microwave pyrolysis in terms of adsorbents preparation. The final step of this work was by activation and sorption characterization on a 3Flex Surface Characterization Analyzer (Micromeritics). The measured data from BET and t-plot confirm that the surface area of activated materials had sorption properties close to higher quality AC. The non-activated samples had almost zero sorption properties. From the results, it could be concluded that waste coffee, which is a waste material that is mostly disposed of by landfilling, could be used for preparation of sorbents with surface area around 1800 m2·g−1. The surface area of sorbent prepared by microwave pyrolysis was measured as much lower in comparison with conventional pyrolysis. By contrast, it must be mentioned that the treatment time can be considerably reduced, which in many cases represents a reduction in the energy consumption as well. The preparation took only 20 min compared to several hours in the case of conventional pyrolysis, and it could be an interesting way of sorbents preparation in the future.

About the authors

Barbora Grycova

Barbora Grycova studied Economics in Metallurgy and Metallurgy at VSB Technical University of Ostrava and obtained her PhD degree in 2012 at VSB Technical University of Ostrava (field of study: thermal technology and fuels in industry). She is a junior researcher and lecturer at the Institute of Environmental Technology, VSB Technical University of Ostrava and interested in the field of thermal engineering, e.g. new generation biofuels and activated carbon production by pyrolysis and gasification.

Adrian Pryszcz

Adrian Pryszcz MSc studied Environmental Technology at the Institute of Chemical Technology, Prague and obtained his MSc degree in 2007. He is a PhD student at the Institute of Environmental Technology, VSB Technical University of Ostrava and interested in the field of thermal engineering, e.g. new generation biofuels and activated carbon production by pyrolysis and gasification.

Pavel Lestinsky

Pavel Lestinsky studied Process Engineering at VSB Technical University and obtained his PhD in 2013. He is a senior researcher and lecturer at the Institute of Environmental Technology, VSB Technical University of Ostrava and interested in the field of chemical engineering, e.g. gas and flue gas cleaning, mathematical modeling of the transport phenomena (by Matlab, Comsol, Fluent), simulation of chemical processes (by Aspen Plus) or new generation biofuel production by pyrolysis.

Katerina Chamradova

Katerina Chamradova studied at the Faculty of Mining and Geology, VSB Technical University of Ostrava and obtained her PhD degree in 2012 from VSB Technical University of Ostrava (field of study: environmental protection within industry). She is a junior researcher and lecturer at the Institute of Environmental Technology, VSB Technical University of Ostrava and a member of the anaerobic digestion team. She is interested in the field of anaerobic digestion, in particular use of food waste by anaerobic treatment.

Acknowledgments

This work was financially supported by the Ministry of Education, Youth and Sports of the Czech Republic in the “National Feasibility Program I”, project LO1208 “TEWEP” and also by EU structural funding Operational Programme Research and Development for Innovation project no. CZ.1.05/2.1.00/19.0388.

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Received: 2016-10-27
Accepted: 2017-1-17
Published Online: 2017-2-28
Published in Print: 2017-5-24

©2017 Walter de Gruyter GmbH, Berlin/Boston

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  6. Screening of catalysts and reaction conditions for the direct conversion of corncob xylan to xylitol
  7. The influence of biomass agitation on biogas and methane production using the high-solids thermophilic anaerobic digestion
  8. Hydrogenation of levulinic acid using Ru-containing catalysts based on hypercrosslinked polystyrene
  9. Preparation and characterization of sorbents from food waste
  10. A more sustainable membrane preparation using triethyl phosphate as solvent
  11. Effective one-pot synthesis of (E)-poly(vinyl arylenes) via trans-borylation/Suzuki coupling protocol
  12. Green synthesis of copper nanoparticles with ultrasound assistance
  13. Green synthesis and antimicrobial activity of ZnO nanostructures Punica granatum shell extract
  14. Sonochemistry production of ZnO and zero-valent Fe nanoparticles from solutions of electric arc furnace dust leaching
  15. Original articles
  16. Optimization of UV irradiation mutation conditions for cellulase production by mutant fungal strains of Aspergillus niger through solid state fermentation
  17. The castor oil based water borne polyurethane dispersion; effect of -NCO/OH content: synthesis, characterization and properties
  18. Removal of benzaldehyde from a water/ethanol mixture by applying scavenging techniques
https://doi.org/10.1515/gps-2016-0182
Keywords for this article
activated carbon; food waste; pyrolysis
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BY-NC-ND 3.0

Articles in the same Issue

  1. Frontmatter
  2. In this issue
  3. GreenChemSE 2016
  4. 2nd International Conference on Green Chemistry and Sustainable Engineering (GreenChemSE16), Rome, Italy, 20–22 July, 2016
  5. Direct conversion of cellulose to α-hydroxy acids (AHAs) over Nb2O5-SiO2-coated magnetic nanoparticles
  6. Screening of catalysts and reaction conditions for the direct conversion of corncob xylan to xylitol
  7. The influence of biomass agitation on biogas and methane production using the high-solids thermophilic anaerobic digestion
  8. Hydrogenation of levulinic acid using Ru-containing catalysts based on hypercrosslinked polystyrene
  9. Preparation and characterization of sorbents from food waste
  10. A more sustainable membrane preparation using triethyl phosphate as solvent
  11. Effective one-pot synthesis of (E)-poly(vinyl arylenes) via trans-borylation/Suzuki coupling protocol
  12. Green synthesis of copper nanoparticles with ultrasound assistance
  13. Green synthesis and antimicrobial activity of ZnO nanostructures Punica granatum shell extract
  14. Sonochemistry production of ZnO and zero-valent Fe nanoparticles from solutions of electric arc furnace dust leaching
  15. Original articles
  16. Optimization of UV irradiation mutation conditions for cellulase production by mutant fungal strains of Aspergillus niger through solid state fermentation
  17. The castor oil based water borne polyurethane dispersion; effect of -NCO/OH content: synthesis, characterization and properties
  18. Removal of benzaldehyde from a water/ethanol mixture by applying scavenging techniques
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