WO2015076688A1 - Procédé d'obtention d'engrais à partir de vinasse - Google Patents

Procédé d'obtention d'engrais à partir de vinasse Download PDF

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Publication number
WO2015076688A1
WO2015076688A1 PCT/RO2013/000023 RO2013000023W WO2015076688A1 WO 2015076688 A1 WO2015076688 A1 WO 2015076688A1 RO 2013000023 W RO2013000023 W RO 2013000023W WO 2015076688 A1 WO2015076688 A1 WO 2015076688A1
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WO
WIPO (PCT)
Prior art keywords
vinasse
bio
mixture
yeast
char
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PCT/RO2013/000023
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English (en)
Inventor
Florin Oancea
Emanuel Corneliu DOBRONAUTEANU
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Sc Transproiect Organic Srl
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Publication of WO2015076688A1 publication Critical patent/WO2015076688A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F11/00—Other organic fertilisers
    • C05F11/02—Other organic fertilisers from peat, brown coal, and similar vegetable deposits
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D9/00—Other inorganic fertilisers
    • C05D9/02—Other inorganic fertilisers containing trace elements
    • 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
    • C05F5/006—Waste from chemical processing of material, e.g. diestillation, roasting, cooking
    • C05F5/008—Waste from biochemical processing of material, e.g. fermentation, breweries
    • 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

Definitions

  • This invention refers to a process for obtainment of fertilizers from vinasse, (co)product from the utilization of molasses in industrial fermentative processes, especially from the production of (bio)ethanol from molasses, respectively of an organo-mineral fertilizer which contains humic acids, and a nitrogen fertilizer with osmo-protectant action, due to the presence (glycine)betaine.
  • This cycle of methionine have a regulatory function on: (/) gene expression through methylation, including epigenetic response to environmental factors, and (//) the cascade of signal factors, at intra- and inter - cellular level, polyamines - nitric oxide - peroxynitrite. Due to this involvement in the regulation of the metabolism of some key compounds (glycine)betaine is a versatile compound, with a major function in plant response to abiotic and biotic stress (see e.g. the review Ahmad et al., 2013, Plant Biotech. Rep., 7: 49-57).
  • the osmoprotectant effect protecting plants against hydric stress due to low rainfall, drought and salinity, has significant implications in the current context of climate changes, characterized by modification of the pattern of rainfall and increased drought risk.
  • the technical problems related to the use of vinasse as fertilizers / fertigants are resulted from: (/) the microbiological instability of vinasse, due to the presence of fermentation yeast, partially inactivated by distillation, which makes vinasse difficult to be kept as it for more than 10 days; (/ ' /) clastogenicity / chromosomal breakdown with aberrations, determined by the melanoidinic / humic-like (soluble) compounds, formed and accumulated during repeated heat treatments, included into technological processes that lead to the obtainment of molasses and then to vinasse (see e.g. da Silva et al., 2013, Environ. Monit.
  • Patent US 5 851 405 describes a process of clarification and of recovery of betaine and potassium from vinasse. Clarification of vinasse is performed after pH adjustment, preferably from 6.5 to 7.5, on a centrifugal separator, at 9,000 x g. Clarified vinasse is concentrated in a circular evaporator, till a solid content of 59% to 65%. Potassium sulfate crystals, which are beginning to be formed from the 40% dry matter content in concentrated vinasse, are removed by decantation and filtration on a press filter, with diatomaceous earth as a filtration additive. The resulting concentrated vinasse is diluted and subjected to ion exchange chromatography separation for recovery of the betaine.
  • the process involves concentration operations, followed by dilution of concentrated vinasse and re-concentration of chromatographic eluat containing betaine. During the concentration process, done at high temperatures, the risk of the formation of new melanoidinic (soluble) compounds is high. In the process described by U.S. Patent 5 851 405 are not claimed steps wherein these potentially dangerous organic compounds are inactivated.
  • Patent Application WO2010/070622 describes a process of electro- flotation/oxidation, which reduce total organic carbon, oxygen consumption and total solids of vinasse, including the potentially dangerous melanoidinic compounds, which involves the following steps: introduction of vinasse into electrolytic cells equipped with galvanized steel electrodes, adjustment of vinasse pH to a value between 7 and 14, preferably between 7 and 1 1 , the application of a constant current, at a current density of between 20 and 40 mA/cm 2 , hydrogen peroxide injection, continuous or sequential, in the vinasse, in the proximity of the electrodes, in a concentration that is between 10 and 67,000 ppm H 2 0 2 per liter of vinasse, preferably between 1 ,000 and 67,000 ppm H 2 0 2 per liter of vinasse, removal of treated vinasse from electrolytic cell and separation of flocculated insoluble solids by gravity, filtration or centrifugation.
  • a drawback of the process described above is the use of relatively large quantities of hydrogen peroxide, relatively expensive compounds, which require precautions in utilization. Also the described process does not include subsequent steps of using of vinasse purified by the process of electro-flotation/oxidation.
  • a portion of the organic matter removed through the above described process of electro-flotation/oxidation is represented by melanoidinic compounds from the category of humic acids - Bengal et al., 2008, Chemosphere, 71 : 1730-1737.
  • Humic acids have a significant role in the formation of soil - Tarchitzky et al., 2000, Soil Sci. 165, 327-342, and promote plant growth and nutrition - Nardi et al., 2002, Soil Biol Biochem., 34: 1527-1536, including due to effects which are similar to phytohormones.
  • Patent Application WO 2009/129589 presents a process for obtainment of a organo- mineral granulated fertilizer, consisting of the following steps: evaporative concentration of vinasse up to 65% dry matter, mixing of the concentrated vinasse with filter cake resulted from sugar syrup fabrication from sugar cane, preferably up to 10 ...20% residual moisture, adding ash from the burning of sugar cane bagasse and/or other residue of sugar cane, adding macro-nutrients, primary (N, P, K) and secondary (Ca, Mg, S), and micro-nutrients (Zn, Fe, Cu, CI, Bo, Mn, Mo), to obtain various organo-mineral agrochemical formulations, corresponding to different types of applications, required by plants cultivation.
  • the process described above is applicable only in the factories which produce (bio)ethanol from sugar cane, and cannot apply to factories which produce (bio) ethanol from molasses, sugar cane or sugar beet, in which there is not produced filter cake from sugar syrup filtration and much less sugar cane bagasse / ash.
  • the process involves steps wherein the energy consumption is high, such as the evaporative concentration of vinasse, and does not include steps to avoid further formation of potentially toxic melanoidinic compounds.
  • the melanoidinic compounds are not differentiated according to their effect, beneficial in the case of humic acids, molecular complexes with low solubility, or (potentially) toxic for fulvic acid, melanoidins with higher solubility in water.
  • humic acids due to the new perspective of humic acids, revealed by the new techniques of investigation, described by Sutton and Sposito, 2005, Environ. Sci.
  • humic acids are complex macromolecular melanoidinic compounds, stabilized by hydrophobic interactions and hydrogen bonds, insoluble at acidic pH and dissolved in alkaline pH, due to destabilization resulted from hydrophobic interactions, and fulvic acids are melanoidinic compounds soluble in water, both on acid and alkaline pH, with a significant presence of polar residues of (5-methyl)-2-furfural, formed by thermal dehydration of carbohydrate molecules.
  • Humic acids with low solubility and more pronounced hydrophobic character, have a beneficial effect on soil fertility and structure, as well as the stimulation of plant nutrition and culture - see e.g. Schnitzer and Moreal, 2011 , Advan.
  • melanoidinic compounds with a higher water solubility, and which have a higher capacity of transportation through various permeability barriers from various organisms, are included also those soluble melanoidins, which are responsible for clastogenicity / chromosomal breakdown with aberrations, and for the toxicity to aquatic organisms of leachates from soils fertilized / fertigated with vinasse.
  • Vinasse has a high content of fulvic acids and a reduced content of humic acids - Tejada and Gonzalez, 2005, Europ. J. Agron. 23: 336-347.
  • the role of manganese in catalyzing abiotic humification process demonstrated by Jokic et al., 2001 , Geophys. Res. Lett., 28: 4019-3902, explains (partially) also the manganese depletion on soils treated with large amounts of vinasse with soluble fulvic acids / incompletely humified melanoidins, that decrease the content of bio-available manganese in soils, as a result of humification reactions till humic acids.
  • the object of this invention is to describe such a process, wherein humification reactions of fulvic acids from vinasse to humic acids are performed, allowing a full recovery of melanoidins from vinasse, by obtaining organic / organo-mineral fertilizers, with reduced risks to the various components of the environment.
  • Adjustment of the clarified vinasse pH to value 4 addition of steel slag, in a ratio of 2 parts steel slag to 98 parts vinasse, and maintainance at 60°C, with 20 rpm agitation and aeration with 0.2 liter air / liter medium/ min for 12 hours, in order to promote the catalyzation of the humification reaction, by the manganese and iron oxides present in steel slag;
  • High pressure homogenization of yeast concentrate by passing through a high pressure piston homogenizer piston fitted with a knife edge valve, 2 cycles at 150 MPa and acidification to pH 2.0 of homogenate with phosphoric acid;
  • Steel slag used to catalyze the oxidation of fulvic acids and their coagulation as complexes of humic acids contains at least 2.5% of manganese oxide and 25% iron oxides;
  • Bio-char used with a specific microporous volume, W a , of at least 0,6 cm 3 g " ⁇ and with a surface of micropores, S m i Cr o, of min. 450 m 2 g "1 , is obtained by micro-wave assisted pyrolysis, from a mixture of distiller grains, from bioethanol production, and corn stover, 25 ...50% distiller grain: 50 ... 75% corn stover, and micro-wave assisted pyrolysis is performed by exposing the above mixture for 20 minutes to micro-waves, with a power of 1000 W and an incident frequency of 2450 MHz.
  • precipitate (P) bio-char : softwood sawdust : yeast homogenate, is performed with a specific power of 1 kW for 0.015 ...0.02 m 2 surface of the matrix, maintaining the temperature of the pelletizing mixture of about 65°C.
  • nitrogen fertilizer F1 reduce the ratio C:N, increasing the bioavailability of nitrogen for plants;
  • a continuous laboratory centrifuge Westfalia Laboratory Separator, model SA 1 -02-175 (GEA Westfalia Separator Group, Germany, Oelde)
  • the yeast concentrate is homogenized into a high pressure piston homogenizer GEA Niro Soavi NS2006 Arriete (GEA Niro Soavi, Parma, Italy) with a knife edge valve, two cycles 150 MPa.
  • High pressure homogenization causes inactivation of microbial cells by disruption induced by pressure variations and passing through the knife edge valve.
  • Yeast homogenate is cooled, acidified at pH 2.0 with phosphoric acid and maintained in a container chilled at 4°C until further use.
  • Steel slag used contains at least 2.5% of manganese oxide and 25% iron oxides.
  • the content of oxides of manganese and iron oxides are determined by using an X-ray wavelength dispersive fluorescence spectrometer, e.g. PW 4025 iniPal (PANalytical, Almelo, Netherland).
  • the mixture clarified vinasse - steel slag is cooled to 25°C, the pH is adjusted to 3.5 and are added 2 kg of biochar. It is maintained, under agitation at 20 rpm, for 3 hours.
  • Biochar used in the above mixture has a specific microporous volume, W a , of at least 0.6 cm 3 g ⁇ ⁇ and a specific surface of micropores, Smicro. of min. 450 m 2 g " ⁇ and is obtained by micro-wave assisted pyrolysis of a mixture of distiller grains, from bioethanol production, and corn stover.
  • Microporous specific volume, W a of biochar was calculated from the linear function Dubinin-Radushkevich (Stoeckli et al., 2001 , Carbon 39: 1 15-1 1 16), after determination of adsorption isotherm in liquid nitrogen at 77 K, using a physisorption analyzer (Micromeritics ASAP 2020, Micromeritics, Norcross, GA, USA). Specific surface of micropores was estimated by reporting the values obtained for the specific microporous volume to average dimensions of micropores (Stoeckli, 1996 in: Patrick, J. (ed.), Porosity in Carbons - Characterization and Applications. Arnold, London, pp. 67-92).
  • the pH of the mixture vinasse - steel slag - biochar is adjusted to 1.5 pH units, is maintained at 25°C, under 20 rpm agitation, for 20 min, to complete the humic acids precipitation, pre-existing and formed by mediated catalysis of iron and manganese oxides.
  • the mixture of vinasse- steel slag - biochar is separated on a pressure filter (RPF T01 , BHS, Sonthofen-Sonthofen, Germany), at 0.6 MPa, separating a filtrate F1 , which is further used as fertigant with high (glycine)betaine content, and precipitate (P).
  • humic acids-C determined in the agro-fertilizer F2 is 15.7 g kg "1 , well above the content of humic acids in the initial vinasse, which demonstrates humification of melanoidins by steel slag / manganese and iron oxides present in the steel slag, according to the process presented above.
  • Attenuata were used the procedures described by OECD TG201 -2006/ISO 8692-2005 [ENV/J /MONO (2008) 28], and, respectively Trottier et al. 1997, Toxicol. Water qual. 12, 265-271 .
  • the used method was OECD TG202-2004/ISO 6341 -2005 [ENV/JM/MONO (2008)].
  • Toxicity was estimated by the modified Spearman-Karber method (Hamilton et al., 1977, Environ Sci. Tech.
  • Leachate of organo-mineral fertilizer F2 was obtained by washing 100 g of fertilizer with 1 liter of deionized water, repeated five times for 5 min.
  • the toxicity that occurs in the case of the filtrate F1 is determined by pH of the growth medium reduction, and not to melanoidins.
  • Apparently toxic effects which were observed in the case of leachate from organo-mineral fertilizers F2 are determined mainly by the lack of nutrient resulting from excessive dilution of the culture medium, and not as a result of potential run-off of toxic melanoidinic compounds.
  • fertilizer F1 as osmoprotectant which protect tomatoes plants against water stress was tested.
  • Plants of tomato (Lycopersicum esculentum cv. Cristal F1 ), 60 days old transplants, were transplanted into pots of 25 cm diameter and 50 cm height, in which there were introduced 5 liters of growing substrate enriched with nutrients for the first few weeks of growth (Canna Terra Professional Plus, Canna International BV).
  • Vegetation vessels were kept in greenhouse conditions at 22 ⁇ 2°C during the day and 17 ⁇ 2°C during the night, with 12 hours photoperiod, supplemented with light intensity of 160 mcE/m 2 /s, derived from the halogen lamps, when light intensity decrease below 500 mcE/m 2 level.
  • the substrate contained reserves of nutrients, so the plants were fertilized only once, after 30 days from transplanting, by application of 55 ml of nutrient solution, 1 g/l of fertilizer 20-8-20 (N-P 2 0 5 -K 2 0 Eurofertil TimacAgro, Romania).
  • the experiment was conducted in randomized block with 4 repetitions for each treatment, every repetition including five plants.
  • As a product of reference it has been used purified glicin-betaine (99%, Sigma Aldrich, St. Louis, Mo, USA), the experimental treatments including control treated only with water, water-stressed and non-stressed.
  • V-i - control not water stressed, treated with water
  • V 6 - water stressed, treated with F1 substrate initially treated with 55 ml solution 7.5% fertilizer F1 , fertigation with 55 ml solution of 1 g l of mineral fertilizer 20-8-20 (N-P2O5-K 2 O) and 7.5% fertilizer, per kg of substrate.
  • the water non stressed treatments were watered once every five days at 100% field capacity (55 ml per 1 kg of substrate), and water stressed treatments were watered each ten days at 100% capacity.
  • the plant were harvested, and the morphological parameters of plants, plant height, root length, leaves number and surface were determined. Data were processed by analysis of variance (Statistica 10, StatSoft, Tulsa, OK, USA).
  • Fertilizer F1 obtained according to the above example of invention embodiment, applied as drench treatment of the soil, in the concentration of 7.5 percent, equiv. 1.23 g/l glycine-betaine, have an activity similar to the solution of purified 10 mM glycine-betaine, limiting the effect of the water stress effects on tomatoes plants and stimulating non-stressed plants.
  • Substrate contained initial nutrients reserve, and the plants were supplementary fertilized only after five weeks, applying 55 ml of nutrient solution, 1 g/l of fertilizer 20-8-20 (N-P 2 O 5 -K2O, Eurofertil, TimacAgro), per kg of substrate.
  • the additional fertilization treatments were the following:
  • V 2 -control treated with a reference product, obtained by pelletizing in conditions similar, of a mixture of 2 parts of steel slag, 49 kg bio-char, and 52 kg of softwood sawdust, 4 g per kg of substrate, equivalent to 21 .6 tons/ha;
  • Each treatment included 12 pots, which were arranged in blocks of three per repetition, in a Latin square randomized schedule, 4 treatments in 4 repetitions. 12 weeks after transplanting of cuttings, the fresh and dry weight of roots and aerial parts of geranium plants were weighted. Data were processed by analysis of variance (Statistica 10, StatSoft, Tulsa, OK, USA).

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

L'invention concerne un procédé d'obtention d'un engrais organo-minéral qui contient des acides humiques, et d'un engrais azoté présentant une action osmo-protectrice due à la présence de (glycine)bétaïne à partir de vinasse. Le procédé est composé des étapes suivantes : séparation d'un concentré de levure de la vinasse; homogénéisation à haute pression du concentré de vinasse; addition de laitier d'aciérie à la vinasse clarifiée et maintien de la vinasse sur un milieu aéré et agité, afin de favoriser l'action catalytique des oxydes de manganèse et de fer présents dans le laitier d'aciérie sur la réaction d'humification des acides fulviques en acides humiques; précipitation des acides humiques par addition de charbon vert et acidification; séparation du filtrat et utilisation comme engrais osmo-protecteur; pelletisation du précipité conjointement avec l'homogénat de levure, le charbon vert et de la sciure de bois tendre, afin d'obtenir un engrais organo-minéral.
PCT/RO2013/000023 2013-11-25 2013-11-27 Procédé d'obtention d'engrais à partir de vinasse WO2015076688A1 (fr)

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ROA201300897 2013-11-25
ROA201300897A RO129937B1 (ro) 2013-11-25 2013-11-25 Procedeu de obţinere a unui fertilizant din vinasă

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2673713C2 (ru) * 2015-12-17 2018-11-29 Общество с ограниченной ответственностью "МФК Точка Опоры" Способ получения жидкой гуминовой органо-минеральной подкормки для растений
CN112088748A (zh) * 2020-09-23 2020-12-18 华中师范大学 一种基于铁循环调控的定向腐殖化强化造土及制法和应用

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1303034A3 (ru) * 1978-01-31 1987-04-07 Альфа Лаваль,Аб (Фирма) Способ получени этанола
WO2007006970A2 (fr) * 2005-07-13 2007-01-18 Compagnie Gervais Danone Produits alimentaires fermentes contenant des souches probiotiques, et leur procede de preparation
WO2009129589A2 (fr) * 2008-04-23 2009-10-29 Dedini S.A. Indústrias De Base Procede de production d’engrais organo-mineral

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1303034A3 (ru) * 1978-01-31 1987-04-07 Альфа Лаваль,Аб (Фирма) Способ получени этанола
WO2007006970A2 (fr) * 2005-07-13 2007-01-18 Compagnie Gervais Danone Produits alimentaires fermentes contenant des souches probiotiques, et leur procede de preparation
WO2009129589A2 (fr) * 2008-04-23 2009-10-29 Dedini S.A. Indústrias De Base Procede de production d’engrais organo-mineral

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2673713C2 (ru) * 2015-12-17 2018-11-29 Общество с ограниченной ответственностью "МФК Точка Опоры" Способ получения жидкой гуминовой органо-минеральной подкормки для растений
CN112088748A (zh) * 2020-09-23 2020-12-18 华中师范大学 一种基于铁循环调控的定向腐殖化强化造土及制法和应用

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