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WO2024134675A1 - Procédé de production de biogaz à partir d'une charge d'alimentation lignocellulosique - Google Patents

Procédé de production de biogaz à partir d'une charge d'alimentation lignocellulosique Download PDF

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Publication number
WO2024134675A1
WO2024134675A1 PCT/IN2023/051178 IN2023051178W WO2024134675A1 WO 2024134675 A1 WO2024134675 A1 WO 2024134675A1 IN 2023051178 W IN2023051178 W IN 2023051178W WO 2024134675 A1 WO2024134675 A1 WO 2024134675A1
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Prior art keywords
lignocellulosic feedstock
biogas
processed
solids
feedstock
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PCT/IN2023/051178
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English (en)
Inventor
Shaileshkumar Dhondiram Sawale
Deepak Pandurang Patil
Aamod Anil NATU
Sharad Krishnachandra LALDAS
Jitendra Hirachand AKADE
Aarohi Atul KULKARNI
Jagruti Rameshbhai TANK
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Praj Industries Limited
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Application filed by Praj Industries Limited filed Critical Praj Industries Limited
Publication of WO2024134675A1 publication Critical patent/WO2024134675A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P5/00—Preparation of hydrocarbons or halogenated hydrocarbons
    • C12P5/02—Preparation of hydrocarbons or halogenated hydrocarbons acyclic
    • C12P5/023—Methane
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12R—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES C12C - C12Q, RELATING TO MICROORGANISMS
    • C12R2001/00—Microorganisms ; Processes using microorganisms
    • C12R2001/01—Bacteria or Actinomycetales ; using bacteria or Actinomycetales

Definitions

  • lignocellulosic feedstock contributes/causes its limited biodegradability and exceptionally slow rates of sugar hydrolysis, acidolysis, and methanogenesis.
  • Figure 2 (a, b) illustrates the scanning electron microscopic (SEM) images of shredded rice straw.
  • Figure 3 illustrates the scanning electron microscopic (SEM) images of milled rice straw.
  • Figure 5 illustrates the scanning electron microscopic (SEM) image of rice straw material after pretreatment with at least one microorganism.
  • FIG. 7 illustrates effect of HRT on biogas production.
  • An aspect of the instant disclosure relates to a process for producing biogas; particularly from lignocellulosic feedstock.
  • lignocellulosic feedstock or “feedstock” pertains to conventionally known feedstock or biomass material.
  • An aspect of the instant disclosure relates to a process for producing biogas from lignocellulosic feedstock comprising, selecting lignocellulosic feedstock; processing the lignocellulosic feedstock by reducing their size to obtain processed lignocellulosic feedstock; pre -treating the processed lignocellulosic feedstock with at least one micro-organism to obtain pre -treated lignocellulosic feedstock; and anaerobically digesting the pre -treated lignocellulosic feedstock to obtain biogas; such that, yield of the biogas is improved.
  • lignocellulosic feedstock is selected from conventionally known feedstock/biomass material; and preferably selected from rice straw, wheat straw, cotton stalk, Juli flora, groundnut shell, palm oil empty fruit bunch, bagasse, and soyabean straw.
  • lignocellulosic feedstock comprises total solids (TS), total volatile solids (TVS), lignin, carbohydrates, and ash in a range of about 55- 95 % w/w, 50- 90% w/w, 11-32% w/w, 28-55%, and 3-13%, respectively.
  • Another embodiment relates to processing lignocellulosic feedstock; preferably, by reducing their size; and particularly to obtain processed lignocellulosic feedstock.
  • the processing of the lignocellulosic feedstock is carried out through at least one of shredding, milling, extrusion, and plug screw.
  • the processing of the lignocellulosic feedstock is carried out through shredding or milling with at least one of extrusion or plug screw.
  • the lignocellulosic feedstock is processed to particle size distribution of ⁇ 20 mm; and preferably, to particle size distribution of ⁇ 5 mm.
  • shredded/milled lignocellulosic feedstock having 10 - 90% w/w total solids; and preferably, around 15 - 60% w/w total solids is used as inlet.
  • Yet another embodiment relates to pre-treating the processed lignocellulosic feedstock to obtain pre-treated lignocellulosic feedstock.
  • the pre -treatment is carried out with at least one of conventionally known enzymes and/or at least one micro-organism; and preferably, at least one microorganism.
  • the pretreatment of the processed lignocellulosic feedstock increases total volatile acid (TVA); preferably, by 3 times.
  • the pretreatment of the processed lignocellulosic feedstock is carried out at 37°C to 55°C.
  • the pretreatment of the processed lignocellulosic feedstock is carried for 12 to 96 h; and preferably, for 24 to 96 h.
  • concentration of the micro-organism is 0.5-10%.
  • the microorganism belongs to genus Bacillus, Lactobacillus, Pediococcus, and Thermobifida-, preferably, the microorganism belongs to genus Thermobifida-, and particularly, the microorganism is Thermobifida fusca.
  • the processed lignocellulosic feedstock is added to a pretreatment section (PTR); and preferably, 0.5% - 10% Thermobifida fusca is added and mixed using aeration; particularly, at about 37-55°C and continued for about 12-96 h.
  • PTR pretreatment section
  • TVA total volatile acids
  • TVA produced with Thermobifida fusca pretreatment is about 2000-4500 ppm.
  • PTR and/or digester pertain to fermenter, generator, bioreactor, vessel, jar, tank, or any manufactured device or system that supports a biologically active environment.
  • the PTR, and/or digester is rectangular, cylindrical, or circular shaped; and preferably, cylindrical shaped. Furthermore, in a related embodiment, the PTR, and/or digester is horizontally, diagonally, or vertically angled.
  • the PTR, and/or digester is a small, medium, or large capacity apparatus.
  • volume of the PTR, and/or digester is any volume from IL to several thousands of L, as per requirements.
  • a further embodiment relates to anaerobically digesting the pre-treated lignocellulosic feedstock; preferably, to obtain biogas.
  • the anaerobic digestion of the pre-treated lignocellulosic feedstock is carried out using acclimatized cow dung.
  • cow dung pertains to commercially available cow dung diluted with water and incubated for microbial enrichment and activation.
  • cow dung is diluted to about 4-5% with water. In another related embodiment, cow dung is incubated at about 35°C to 40°C.
  • cow dung is incubated for 2.5 to 4 weeks; and preferably, for about 2 weeks.
  • the anaerobic digestion of the pre-treated lignocellulosic feedstock provides at least one of biomethanated solids and biomethanated liquid.
  • total volatile solids (TVS) of the biomethanated solids is up to 20% w/w.
  • total volatile solids (TVS) of the biomethanated liquid is up to 2% w/w.
  • the acclimatized cow dung comprises 4-5% of total solids.
  • hydraulic retention time (HRT) for producing the biogas is 10 to 28 days; and preferably, is 14 to 28 days.
  • conventionally implemented digester is filled initially with anaerobic sludge having about 15-20% total solids and acclimatized cow dung slurry containing about 4-5% total solids.
  • the anaerobic digester is allowed to stabilize for a period two to three weeks.
  • Digester temperature is maintained at about 37 ⁇ 1°C during stabilization and overall bio methanation process. pH is stabilized/maintained between 6.5 to 7.0.
  • the digestate subjected to separation; and preferably, solid liquid separation using conventionally known separation means.
  • digestate pertains to the material remaining/retentate after the anaerobic digestion of pre-treated feedstock.
  • An embodiment of the instant disclosure relates to selecting (101) and processing lignocellulosic feedstock (102), wherein, the lignocellulosic feedstock is subjected to shredding and/or milling to obtain processed lignocellulosic feedstock with particle size distribution of around ⁇ 30 mm, and preferably, ranging from 10 mm to 30 mm. Further, the shredded and/or milled lignocellulosic feedstock is subjected to extrusion or plug screw (formation) (with single/double screw) for further size reduction to obtain processed lignocellulosic feedstock with particle size distribution of around ⁇ 10 mm, and particularly ⁇ 5 mm.
  • Another embodiment relates to pre -treating lignocellulosic feedstock with at least one microorganism to obtain pre-treated lignocellulosic feedstock (103) wherein, the processed lignocellulosic feedstock is added to a PTR. To this, about 0.5 % to 10% Thermobifida fusca culture is added and mixed using agitator and aeration. The pretreatment reaction is carried out at about 37°C to 55°C and for about 24 to 96 h. Post treatment, part of pretreated lignocellulosic feedstock is transferred to anaerobic digester. For continuous pretreatment process, once the pretreated lignocellulosic feedstock is transferred, same volume of processed lignocellulosic feedstock is added to PTR.
  • Further embodiment relates to anaerobically digesting/biomethanation the pre -treated lignocellulosic feedstock to obtain biogas (104), wherein, the digester is filled initially with anaerobic sludge having about 15-20% total solids and acclimatized cow dung slurry containing about 4-5% total solids and anaerobic digestion is carried out as described previously.
  • the entire digestate is subjected to solid liquid separation to obtain wet biomethanated solids having moisture, and biomethanated liquid having solids.
  • Raw biogas is obtained.
  • digestate obtained is further subjected to solid/liquid separation using screw press to obtain biomethanated solids and biomethanated liquid.
  • the yield of the biogas is improved.
  • the yield of the biogas is improved to > 200 AM 3 /ton; preferably, to > 250 AM 3 /ton, and particularly, to > 400 AM 3 /ton.
  • biomethanated solids and/or biomethanated liquids are applied as biofertilizers.
  • Lignocellulosic feedstock was selected from rice straw, wheat straw, cotton stalk, Juli flora, groundnut shell, palm oil empty fruit bunch, bagasse, and soyabean straw comprising total solids (TS), total volatile solids (TVS), lignin, carbohydrates, and ash in a range of about 55- 95 % w/w, 50-90% w/w, 11-32% w/w, 28-55%, and 3-13%, respectively for the purpose of the present disclosure.
  • TS total solids
  • TVS total volatile solids
  • lignin lignin
  • carbohydrates and ash in a range of about 55- 95 % w/w, 50-90% w/w, 11-32% w/w, 28-55%, and 3-13%, respectively for the purpose of the present disclosure.
  • the shredded and/or milled lignocellulosic feedstock was further subjected to at least one of extrusion or plug screw (with single/double screw) for further size reduction to obtain processed lignocellulosic feedstock with particle size distribution of around ⁇ 5 mm.
  • shredded/milled rice straw having 40 - 60% w/w total solids was used as inlet feed, and rice straw having 45 - 55% w/w total solids was used as outlet feed.
  • plug screw shredded/milled rice straw having 18 - 30% w/w total solids was used as inlet feed, and rice straw having 45 - 55% w/w total solids was used as outlet feed.
  • the processed lignocellulosic feedstock obtained from plug screw (single) was without steam and chemical. Morphological study of the processed lignocellulosic feedstock was carried out using conventionally applied field emission scanning electron microscope (see Figs. 2-6). As per Fig.
  • Microorganisms such as Bacillus subtilis (BS) MTCC 2414, Bacillus subtilis (BS) MTCC 2415, , Bacillus licheniformis (BL) NCIM 2051, Lactobacillus fermentum (LF) MTCC 9748, Lactobacillus bifermentans (LBF) MTCC 3818, Lactobacillus plantarum (LP) MTCC 9495, Pediococcus pentosaceous (PP) ATCC 43200 (USA), and Thermobifida fusca (TF) NBRC 14071 (Japan), were screened for their ability to grow in liquid media comprising 1 % carboxy methyl cellulose (CMC) as sole carbon source.
  • CMC carboxy methyl cellulose
  • Total viable count (TVC, cfu/ml) was quantified using serial dilution method on an agar plate comprising about 1 % CMC as the sole carbon source (see Table 1).
  • De Man, Rogosa and Sharpe (MRS) medium was implemented for culturing Lactobacillus and nutrient broth (NB) solid agar medium was implemented for culturing Bacillus and T. fusca.
  • Table 1 TVC medium containing 1% CMC *NT- Not tested since test microbes were not growing on minimal MRS and NB media respectively.
  • Microorganisms growing on minimal media with CMC as a carbon source were further implemented to screen strain development on minimal media supplemented with about 1% rice straw (RS) and 1% cotton stalk (CS) media.
  • the strains developed through feedstock adaption were then banked in cell bank as pretreatment microorganisms for further evaluation in bio methanation/biogas production (see Table 2).
  • Table 2 Growth of microorganisms used for pretreatment of rice straw and cotton stalk media
  • Thermobifida fusca demonstrated better proliferative and degradative activity. So, Thermobifida fusca was implemented for pre-treating the processed lignocellulosic feedstock to obtain pre -treated lignocellulosic feedstock in the present disclosure.
  • Thermobifida fusca glycerol stock was added to about 100 ml nutrient broth and incubated at about 45 °C for about 48 h to obtain pre -grown culture which was used as the inoculum for carrying out optimization studies.
  • Example 1 About 8% w/w processed rice straw achieved through Example 1 was pretreated with varying Thermobifida fusca inoculum percentage of 0.5 to 10% at about 45°C for 48 h (see Table 5). Acclimatized cow dung as inoculum, Thermobifida fusca pretreated rice straw and water was added to make 3L reaction volume. The anaerobic biomethanation process was carried out at 37 ⁇ 1°C and 70 rpm agitation. Methane and carbon dioxide were analysed by biogas analyser. Biogas volume was measured by water displacement method (see Table 3).
  • Example 1 About 8% w/w processed rice straw achieved through Example 1 was pretreated with about 2% Thermobifida fusca at varying temperatures ranging from 37°C to 55°C (see Table 4). Acclimatized cow dung as inoculum, Thermobifida fusca pretreated rice straw, and water was added to make 3L reaction volume. The anaerobic biomethanation process was carried out at 37 ⁇ 1°C and 70 rpm agitation. Methane and carbon dioxide were analyzed by biogas analyzer. Biogas volume was measured by water displacement method (see Table 4).
  • Example 1 Optimization of Thermobifida fusca pretreatment time
  • About 8% w/w processed rice straw achieved through Example 1 was pretreated with about 2% Thermobifida fusca at varying time intervals from 12 h to 96 h (see Table 5), and total volatile acids (TVA) were analyzed.
  • Thermobifida fusca pretreatment time was optimized to 48 hours.
  • Processed lignocellulosic feedstock obtained in Example 1 was added to pretreatment reactor (PTR). To this, about 2% Thermobifida fusca culture screened through Example 2, and optimized through Example 3 was added using agitator and aeration. The pretreatment reaction was carried out at about 45 °C for about 48 h, as optimized through Example 3.
  • Example 1 About 8% w/w of processed rice straw achieved through Example 1 was pre-treated with and without Thermobifida fusca at about 45 ⁇ 2°C for about 48 h and analyzed for TVA (see
  • Table 6 Total TVA with and without Thermobifida fusca pretreatment As per Table 6, TVA produced without Thermobifida fusca pretreatment was about 300- 1500 ppm and with Thermobifida fusca pretreatment was about 3000-4500 ppm; thereby deducing that the pretreatment of the processed lignocellulosic feedstock with Thermobifida fusca increases total volatile acid (TVA) by 3 times.
  • TVA total volatile acid
  • Example 1 About 8% w/w of processed rice straw achieved through Example 1 was pretreated with cellulase enzyme sourced from Novozymes, India at a dose of about 30 mg/g of cellulose at about 37°C for about 24 h.
  • the processed rice straw achieved through Example 1 was pretreated with about 2% Thermobifida fusca culture at about 45°C for about 48 h.
  • Acclimatized cow dung as inoculum, Thermobifida fusca pretreated rice straw and water was added to make 3L reaction volume.
  • the anaerobic biomethanation process was carried out at 37 ⁇ 1 °C and 70 rpm agitation.
  • the pretreated rice straw was analysed for total volatile acids (TVA) and biogas generation (see Table 7).
  • the digester was filled initially with anaerobic sludge having about 15-20% total solids and acclimatized cow dung slurry containing about 4-5% total solids.
  • the anaerobic digester was allowed to stabilize for a period two to three weeks.
  • Digester temperature was maintained at about 37 ⁇ 1°C during stabilization and overall bio methanation process.
  • Digester pH was stabilized/maintained between 6.5 to 7.0.
  • Digester was stabilized within 10-12 days of inoculum addition.
  • biogas yield of about 350 - 420M 3 /DMT was achieved through about 14-25 days HRT with an average methane concentration of about 55% v/v and carbon dioxide concentration of about 40% v/v.
  • Table 10 Particle size, PTR TVA and biogas yield after shredding and milling with particle size.
  • Table 11 Effect of extrusion and plug screw mechanical treatment using shredded and milled material and its impact on PTR TVA and biogas yield of rice straw.
  • Pre-treating the processed lignocellulosic feedstock with at least one microorganism to obtain pre -treated lignocellulosic feedstock (103) Pretreatment was carried out in a -pretreatment reactor with approximately 3.2 M 3 capacity. Considering about 3.2 M 3 reaction volume and about 7-7.5% -total solids, the processed lignocellulosic feedstock obtained above was added to a PTR. To this, about 2% Thermobifida fusca culture was added and mixed using agitator and aeration. The pretreatment reaction was carried out at about 45°C and for about 48 h. Post pretreatment, part of pretreated lignocellulosic feedstock was transferred to anaerobic digester.
  • pretreated lignocellulosic feedstock For continuous pretreatment process, once the pretreated lignocellulosic feedstock was transferred, same volume of processed lignocellulosic feedstock was added to PTR. It was found that the pre treated rice straw comprised total solids in the range of 7.0-7.5%w/w and total volatile acids in the range of about 3000-4500ppm.
  • biogas (104) Anaerobically digesting/biomethanation the pre -treated lignocellulosic feedstock to obtain biogas (104):
  • the digester was filled initially with anaerobic sludge having about 15-20% total solids and acclimatized cow dung slurry containing about 4-5% total solids and anaerobic digestion was carried out as described in Examples 7, 8, and 9.
  • TVA biogas volume, methane and carbon dioxide concentration was analysed on daily basis. HRT of 20- 22 day was maintained for all types of rice straw material during bio methanation process. During the entire bio methanation, raw biogas composed of about 55-57% v/v methane, about 35-37% v/v carbon dioxide was obtained.
  • the digestate obtained was further subjected to solid/liquid separation using screw press to obtain biomethanated solids and biomethanated liquid that were analysed (see Table 12).
  • Wet biomethanated solids were further composted to obtain dry biomethanated solids that were further analysed (see Table 13) as per FCO norms and were certified by NOCA for its applicability as a solid fertilizer.
  • biomethanated liquid was further analysed (see Table 12).
  • the post-biomethanated solids and liquid of rice straw were found to be rich in micro and macro minerals. Due to the high C/N ratio of biomethanated solids, it can be used as soil conditioner for agriculture and horticulture industries after dilution with biomethanated spent wash of rice straw thus making it a complete biofertilizer.
  • the instant process can be implemented at small, medium, as well as large scale.

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Abstract

La présente invention concerne un procédé (100) de production de biogaz à partir d'une charge d'alimentation lignocellulosique comprenant : la sélection d'une charge d'alimentation lignocellulosique (101) ; la transformation de la charge d'alimentation lignocellulosique par réduction de la taille aux fins d'obtention d'une charge d'alimentation lignocellulosique transformée (102) ; le prétraitement de la charge d'alimentation lignocellulosique transformée à l'aide d'au moins un micro-organisme aux fins d'obtention d'une charge d'alimentation lignocellulosique prétraitée (103) ; et la digestion anaérobie de la charge d'alimentation lignocellulosique prétraitée aux fins d'obtention du biogaz (104), ledit procédé améliorant ainsi le rendement du biogaz.
PCT/IN2023/051178 2022-12-20 2023-12-13 Procédé de production de biogaz à partir d'une charge d'alimentation lignocellulosique WO2024134675A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100189706A1 (en) * 2007-01-30 2010-07-29 Cathy Chang Enzymes for the treatment of lignocellulosics, nucleic acids encoding them and methods for making and using them
CN104263778A (zh) * 2006-10-26 2015-01-07 希乐克公司 生物质加工
CN104357488A (zh) * 2014-06-27 2015-02-18 江苏省农业科学院 规模化木质纤维原料厌氧发酵产沼气的方法
WO2023209736A1 (fr) * 2022-04-27 2023-11-02 Sardar Swaran Singh National Institute Of Bio-Energy Procédé de production de biogaz à partir de biomasse lignocellulosique

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104263778A (zh) * 2006-10-26 2015-01-07 希乐克公司 生物质加工
US20100189706A1 (en) * 2007-01-30 2010-07-29 Cathy Chang Enzymes for the treatment of lignocellulosics, nucleic acids encoding them and methods for making and using them
CN104357488A (zh) * 2014-06-27 2015-02-18 江苏省农业科学院 规模化木质纤维原料厌氧发酵产沼气的方法
WO2023209736A1 (fr) * 2022-04-27 2023-11-02 Sardar Swaran Singh National Institute Of Bio-Energy Procédé de production de biogaz à partir de biomasse lignocellulosique

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