WO2017132742A1 - Procédé de production d'engrais organo-minéral à partir de la carbonisation hydrothermique de la vinasse et de la bagasse de canne à sucre, et produit obtenu - Google Patents

Procédé de production d'engrais organo-minéral à partir de la carbonisation hydrothermique de la vinasse et de la bagasse de canne à sucre, et produit obtenu Download PDF

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Publication number
WO2017132742A1
WO2017132742A1 PCT/BR2017/050017 BR2017050017W WO2017132742A1 WO 2017132742 A1 WO2017132742 A1 WO 2017132742A1 BR 2017050017 W BR2017050017 W BR 2017050017W WO 2017132742 A1 WO2017132742 A1 WO 2017132742A1
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WIPO (PCT)
Prior art keywords
sugarcane
vinasse
sugarcane bagasse
mineral fertilizer
bagasse
Prior art date
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Ceased
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PCT/BR2017/050017
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English (en)
Portuguese (pt)
Inventor
Camila de Almeida MELO
Márcia Cristina BISINOTI
Odair Pastor FERREIRA
Altair Benedito MOREIRA
Rosana Lisboa SANTANA
Francisco Holanda SOARES JUNIOR
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Universidade Estadual Paulista Julio de Mesquita Filho UNESP
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Universidade Estadual Paulista Julio de Mesquita Filho UNESP
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Publication of WO2017132742A1 publication Critical patent/WO2017132742A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F5/00—Fertilisers from distillery wastes, molasses, vinasses, sugar plant or similar wastes or residues, e.g. from waste originating from industrial processing of raw material of agricultural origin or derived products thereof
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F17/00—Preparation of fertilisers characterised by biological or biochemical treatment steps, e.g. composting or fermentation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
    • Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/40—Bio-organic fraction processing; Production of fertilisers from the organic fraction of waste or refuse

Definitions

  • the present invention describes a process from hydrothermal carbonization of vinasse and sugarcane bagasse to produce a product to be used as a water-holding organo-mineral fertilizer. More specifically, it comprises a hydrothermal carbonization process using vinasse and sugarcane bagasse, in which an acid catalyst is employed to obtain a product to be used as an organo-mineral fertilizer having water retention property.
  • Brazil is the largest producer of ethanol and sugar from sugarcane, according to the Ministry of Agriculture. According to CONAB (National Supply Company) sugarcane farming in Brazil continues to expand, with the states of Mato Grosso do Sul, S ⁇ o Paulo, Goiás and Mato Grosso (National Supply Company) standing out. of the Brazilian Crop - Sugarcane, Third Survey - Dec / 2012. Available at: http://www.conab.gov.br/OlalaCMS/uploads/arquivos/
  • the main residues that can be cited are vinasse, sugarcane bagasse and filter cake.
  • the vinasse comes from the distillation of alcohol and it is estimated that for each liter of alcohol produced 10 to 14 liters of vinasse are generated (Resende, AS; Xavier, RP; Oliveira, O.; Urquiaga, S .; Alves, BJR; Boddey, RM Long-term effects of pre-harvest burning and nitrogen and vinasse applications on yield of sugar cane and soil carbon and nitrogen stocks on a plantation in Pernambuco, NE Brazil Plant and Soil, v.281, p.339 -351, 2006). Sugarcane bagasse is also generated in large quantities.
  • vinasse is used for fertigation, ie application of fresh vinasse in soils cultivated with sugar cane. This practice has been adopted in view of the chemical composition of vinasse. Lyra et al. (Lyra, MRC C; Rolim, MM; Silva, JAA Topossequence of fertigated soils with vinasse: contribution to groundwater water quality. Brazilian Journal of Agricultural and Environmental Engineering, V.7, N.
  • CETESB regulated this practice by means of Technical Standard P4.231, which stipulates that the amount of vinasse applied in the treatment of agricultural land in sugarcane crops is calculated taking into account soil fertility as a function of potassium content, with the maximum potassium concentration not exceeding 5% of the soil Cation Exchange Rate (CTC) and not exceeding 185 kg K 2 0 per hectare per cut (Company S ⁇ o Paulo State Environmental Vinhaça - Criteria and procedures for application in agricultural soil P41.231 (Dec / 2006) Available at: http://www.cetesb.sp.gov.br/ Tecnologia / camaras / P4_231. pdf Accessed August 2, 2013).
  • CTC soil Cation Exchange Rate
  • Document BR102013006606-0 describes a process for treating vinasse which aims to reduce the potassium content of vinasse by adding a phosphorus and magnesium-containing chemical to precipitate a compound containing potassium, phosphorus and magnesium and using the precipitate as a fertilizer.
  • flocculants are added to separate the solid from the liquid, and the pH has to be corrected to increase the efficiency of the precipitation process.
  • US2013046745 describes a method for hydrothermally treating vinasse from corn fermentation at 94 to 177 ° C in order to modify the physicochemical properties of the vinasse, allowing easier separation of fractions such as: fraction of high protein solids, low solids suspended liquid effluent fraction and oil fraction which may be used for other industrial purposes and / or more easily treated.
  • US201 10271588 describes a process for producing a synthetic coal from residues generated in the fermentation of ethanol.
  • the fermentation residue used comes from the production of ethanol from corn.
  • the hydrothermal carbonization process was applied to the fermentation residue of non-lignocellulosic content using temperatures from 170 to 225 ° C, from 0.5 to 6 hours and pressures up to 2.41 MPa.
  • some acid buffers (oxalic and acetic) and catalysts may be added in advance.
  • the coal produced can be used as a fuel.
  • Document BR102015003018-5 describes a process for the conversion of vinasse into solid carbon-rich material and nutrients using hydrothermal carbonization in the presence of sulfuric acid, which entails the incorporation of sulfur into the solid obtained.
  • sugarcane bagasse has also been studied as a source for the production of second generation ethanol (Rabelo, SC; Carrere, H.; Maciel Filho, R .; Costa, AC Production of bioethanol, methane and heat from sugarcane bagasse in a biorefinery concept Bioresource Technology, V. 102, P.
  • Document BR102013006389-4 claims a process for simultaneous conversion of sugarcane bagasse using Ultra High Temperature Short Time (UHTST) reactors in order to convert sugarcane bagasse to glucose monomers and oligomers for the production of biofuels using reactors.
  • UHTST Ultra High Temperature Short Time
  • the main objective is to get more sugars to increase biofuel production such as ethanol.
  • the reactors can be heated to 350 ° C for one minute and the hydrolysed broths are cooled quickly and sent for fermentation.
  • Another alternative to the destination of vinasse is biological treatment using anaerobic reactors with biogas generation and collection to be used to generate energy.
  • This process has advantages such as the use of biogas obtained for energy generation, minimizing contamination by particulate matter and soot.
  • anaerobic reactors consist of large tanks occupying large areas, the residence time of the residue for methane conversion is very high, the gas phase generated presents contamination with gases other than methane, which reduces calorific value.
  • the biogas pipeline system for subsequent power generation and distribution is quite complex and costly, and a sludge that needs to be properly treated prior to disposal is generated.
  • the invention describes a process for producing water-retaining organo-mineral fertilizer from hydrothermal carbonization of vinasse and sugarcane bagasse in a single process, whereas prior art processes use or vinasse or sugarcane bagasse in separate processes, which requires investments in each process, as well as expenses with transportation to other beneficiary industries.
  • the invention describes a process for producing organo-mineral fertilizer from hydrothermal carbonization of vinasse and sugarcane bagasse with the addition of phosphoric acid, which acts as a catalyst, providing the final material with phosphorus in its composition. a macronutrient essential to plants.
  • the invention describes a process for producing organo-mineral fertilizer from hydrothermal carbonization of vinasse and sugarcane bagasse that allows the use of wet biomass and thus sugarcane bagasse can be added to the process with moisture. thus avoiding costs with drying steps.
  • the invention describes a process for producing organo-mineral fertilizer from hydrothermal carbonization of vinasse and sugarcane bagasse using closed reactors.
  • the invention describes a process for producing slow-release, water-retaining organo-mineral fertilizer providing nutrients such as nitrogen, phosphorus, potassium, calcium, magnesium and carbon, among others as required by crops.
  • Figure 1A shows the diffractograms of the hydrocarbons obtained in the reactions R2, R6, R1, R3, R7 and R8 and of the sugarcane bagasse precursors (residue diffractogram after drying in an oven at 105 ° C) within a range of 5 at 65 ° (2 theta) and Figure 1B shows the same diffractograms for the range 10 to 35 ° (2 theta).
  • Figure 2 shows the ATR-FTIR spectra of the sugarcane bagasse raw materials and the hydrocarbons R2, R6, R1, R3, R7 and R8.
  • Figure 3A shows the scanning electron microscopy image of R2 hydrocarbon (temperature 180 ° C, 13 h, 4% acid), figure 3B of hydrocarbon R6 (232 ° C, 13 h, 4%) , figure 3C of hydrocarbon R1 (180 ° C, 13h, 1%), figure 3D of hydrocarbon R3 (180 ° C, 40h, 1%), figure 3E of hydrocarbon R7 (232 ° C, 40h) 0.1%) and figure 3F of hydrocarbon R8 (232 ° C, 40 h, 4%).
  • the process for producing water-holding organo-mineral fertilizer from the hydrothermal carbonization of vinasse and sugarcane bagasse comprises, In a first step, the hydrothermal carbonization of the vinasse mixture (generated by the distillation of ethanol from the fermentation of sugarcane) and sugarcane bagasse in aqueous medium.
  • CHT Hydrothermal carbonization
  • COSSU R.
  • DIAZ LF
  • STEGMANN R. (EDTS.)
  • 2009 Sardinia 2009: Twelfth International Waste Management and Landfill Symposium, Sardinia, Italy, 05-09 October 2009, Proceedings, CISA Publisher; Hwang, IH; Aoyama, H.; Matsuto, T.; Nakagishi, T.; Matsuo, T. Recovery of solid fuel from municipal solid waste by hydrothermal treatment using subcritical water. Waste Management, V.
  • CHT is governed by exothermic processes (Funke, A.; Ziegler, F.; Hydrothermal carbonization of biomass: A summary and discussion of chemical mechanisms for process engineering. Biofuels, Bioproducts and Biorefining, V. 4, P. 160-177, 2010.) is more energy-efficient than dry carbonization processes (pyrolysis), particularly as the raw material used may contain moisture and therefore need not be completely dry.
  • the vinasse is homogenized by mechanical agitation and the sugarcane bagasse is dried at room temperature, homogenized and sieved to obtain a less heterogeneous fraction and thus to ensure the sugarcane bagasse with a particle size of less than 0.5 mm.
  • Vinasse and sugarcane bagasse, rich in carbon, potassium, nitrogen, calcium and magnesium biomass, are mixed without any previous treatment, in proportions ranging from 1: 8 to 1:80 of sugarcane bagasse: vinasse preferably being 1: 20.
  • the vinasse may be replaced by water.
  • an acid preferably concentrated phosphoric acid
  • nitric acid HNO 3
  • sulfuric acid H 2 SO 4
  • boric acid H 3 BO 3
  • other acid additives may be employed as catalysts in the hydrothermal carbonization reaction.
  • the liquid and hydrocarbon fraction are separated by a solid-liquid separation process, preferably filtration, decantation or centrifugation.
  • the hydrocarbon produced may or may not be washed with water, dried at room temperature or about 50 ° C and stored for later application.
  • R1 180 ° C temperature, 13 hours time and 1.0% acid
  • R2 180 ° C temperature, 13 hours time and 4.0% acid
  • R3 180 ° C temperature, 40 hours time and 1.0% acid
  • R4 180 ° C temperature, 40 hours time and 4.0% acid
  • R5 232 ° C temperature, 13 hours time and 1.0% acid
  • R 6 232 ° C temperature, 13 hours time and 4.0% acid
  • R7 232 ° C temperature, 40 hours time and 1.0% acid
  • R8 232 ° C temperature, 40 hours time and 4.0% acid.
  • reaction yield evaluation (on dry basis), dry hydrocarbon samples were weighed.
  • Moisture, volatile matter and ash were determined according to the ASTM 1762 method.
  • the pH was measured in the resting solution after 24 hours. stirring hours of the mixture of 0,5 g hydrocarbon and 50 ml deionized water.
  • the elemental composition of C, H, N and S was determined using an EA1 108 elemental analyzer (Fisons, USA).
  • the O content was calculated by the difference between the ashes and the CHNS content.
  • the functional groups were analyzed by Fourier Transform Infrared Spectroscopy (FTIR) in a UATR-TWO accessory (Perkin Élmer, USA), in the spectral region of 4000-400 cm “1 , 20 scans and 4 cm " 1 resolution.
  • FTIR Fourier Transform Infrared Spectroscopy
  • Scanning electron microscopy (SEM) images were obtained from two INSPECT 50 and FEG Quanta 450 microscopes (FEI Company, Czech Republic). Sample composition was also estimated by X-ray dispersive energy spectroscopy (EDS) using a model 150 X-ray detector (Oxford Instruments, UK) coupled to the Quanta 450 FEG scanning electron microscope.
  • EDS X-ray dispersive energy spectroscopy
  • the samples were prepared in two distinct ways: (i) the powders as synthesized were deposited on carbon tape over aluminum sample holders; (ii) the powders were suspended in deionized water by ultrasound and the suspensions deposited directly on the previously cleaned surface of the aluminum sample holder. In this case the samples were dried at room temperature prior to analysis. In addition, to obtain the images, the samples that showed charge accumulation when interacting with the primary electron beam were coated with about 10 nm of gold thickness. Images were obtained using the secondary electron detector (SE) and the The beam voltage was between 5 and 20 kV for both imaging and EDS analysis. Hydrocarbon samples were subjected to acid decomposition according to the EPA 3050B method (EPA, 1996).
  • Potassium, sodium, calcium, magnesium, manganese, zinc, aluminum and copper were quantified in the decomposed samples using a flame atomization atomic absorption spectrophotometer and / or a graphite oven atomization atomic absorption spectrophotometer (Varian, USA ).
  • Phosphorus was quantified using the visible region spectrophotometric method by the vanadate yellow method 4500-C (APHA, AWWA, WEF, 2012).
  • Water retention was calculated by assessing the difference between the initial mass of 0.2 g hydrocarbon and the final mass after 24 hours of stirring in 200 ml of deionized water (Zhong K., Lin Z., Zheng X., Jiang G ., Fang Y., Mao X., Liao Z. Starch derivative-based superabsorbent with integration of water retaining and controlled release fertilizers, V. 92, P. 1367-1376, 2013).
  • Table 1 pH values, yield and moisture, volatile matter and ash content of the hydrocarbons produced in the reactions made with the mixture of sugarcane bagasse, vinasse and acid.
  • a characterization of the hydrocarbons and ashes of each hydrocarbon as well as vinasse and sugarcane bagasse was made using X-ray Diffractograms (XRD) and X-ray Dispersive Energy Spectroscopy (EDS) to investigate the composition. and structure of precursors (raw materials) and reaction products.
  • XRD X-ray Diffractograms
  • EDS X-ray Dispersive Energy Spectroscopy
  • EDS compositional analyzes of hydrocarbon plus EDS ash analyzes indicated the presence of C, O, N, Mg, Ca, P, K, Si and Fe (Fe is much smaller than the other elements). Therefore, such analyzes showed the presence of macro and micronutrients in the generated hydrocarbon, indicating their potential application as organo-mineral fertilizer for different crops.
  • Sugarcane bagasse has 1, 9 g of K for each kg of sugarcane bagasse;
  • the hydrocarbon produced in R6, for example, has 12.6 g of K for each kg, ie potassium was concentrated from vinasse to hydrocarbon.
  • the same behavior is observed for calcium, magnesium, phosphorus, copper, zinc and manganese.
  • Table 2 Concentrations obtained from macro (phosphorus, potassium, calcium and magnesium) and microelements (iron, copper, zinc and manganese) and aluminum and sodium in the samples of vinasse, sugarcane bagasse, hydrocarbons R1, R2, R3, R4, R5, R6, R7 and R8 and water produced from reactions R1, R2, R3, R4, R5, R6, R7 and R8.
  • Table 3 lists the elemental composition of C, H, N, S and O for the raw materials and hydrocarbons as well as the atomic ratios H / C, O / C and N / C. [066] Table 3: Elemental composition of C, H, N, S and O for raw materials and hydrocarbons as well as atomic ratios H / C, O / C and
  • H / C and O / C ratios help verify the dehydration and flavoring of the materials produced.
  • Hydrocarbons have H / C ratio between 1.00 and 1.50 and O / C ratio between 0.05 and 0.30.
  • Materials such as lignins, lignites and coal have similar reasons. For agricultural purposes these values are important since lignites and coal are already used as fertilizers.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biotechnology (AREA)
  • Health & Medical Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
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Abstract

L'invention concerne un procédé de production d'engrais organo-minéral à capacité de rétention d'eau à partir de la carbonisation hydrothermique de la vinasse et de la bagasse de canne à sucre, consistant à utiliser un catalyseur acide, de préférence de l'acide phosphorique, dans un procédé de carbonisation hydrothermique, ajoutant de la valeur à ces résidus et permettant leur utilisation dans le cycle de production lui-même, réduisant ainsi les coûts en termes de transport, d'engrais et de traitements chimiques, entre autres.
PCT/BR2017/050017 2016-02-01 2017-02-01 Procédé de production d'engrais organo-minéral à partir de la carbonisation hydrothermique de la vinasse et de la bagasse de canne à sucre, et produit obtenu Ceased WO2017132742A1 (fr)

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BR102016002221-5A BR102016002221B1 (pt) 2016-02-01 2016-02-01 Processo para produção de fertilizante organo-mineral a partir da carbonização hidrotérmica da vinhaça e do bagaço de cana e produto obtido
BRBR102016002221-5 2016-02-01

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019121876A1 (fr) 2017-12-19 2019-06-27 Afyren Vinasse comme milieu de fermentation
EP3712233A1 (fr) * 2019-03-20 2020-09-23 Nederlandse Organisatie voor toegepast- natuurwetenschappelijk Onderzoek TNO Traitement de la biomasse avec de la vinasse

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009027007A1 (de) * 2009-06-17 2010-12-23 Technische Universität Berlin Verfahren zur Herstellung von mineralischem Biodünger

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009027007A1 (de) * 2009-06-17 2010-12-23 Technische Universität Berlin Verfahren zur Herstellung von mineralischem Biodünger

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
MELO, C.A. ET AL.: "Caracterização Físico-Química De Hidrocarbonos Visando Seu Uso Como Fertilizante", IN: XI ENCONTRO BRASILEIRO DE SUBSTÂNCIAS HÚMICAS, 19 October 2015 (2015-10-19), São Carlos-SP, pages 311 - 313 *
MELO, C.A. ET AL.: "Transforming sugarcane bagasse and vinasse wastes into hydrochar in the presence of phosphoric acid: an evaluation of nutrient contents and strutural properties", WASTE AND BIOMASS VALORIZATION, no. 4, 24 August 2016 (2016-08-24), pages 1139 - 1151, XP036228536 *
NOVOTNY, E.H. ET AL.: "Biochar: Pyrogenic Carbon For Agriculture Use - A Critical Review", R. BRAS. CI. SOLO, vol. 39, 2015, pages 321 - 344 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019121876A1 (fr) 2017-12-19 2019-06-27 Afyren Vinasse comme milieu de fermentation
EP3712233A1 (fr) * 2019-03-20 2020-09-23 Nederlandse Organisatie voor toegepast- natuurwetenschappelijk Onderzoek TNO Traitement de la biomasse avec de la vinasse
WO2020188088A1 (fr) * 2019-03-20 2020-09-24 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno Traitement de biomasse avec de la vinasse
US20220169937A1 (en) * 2019-03-20 2022-06-02 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno Treatment of biomass with vinasse

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