Classifications

• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
  • F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
  • F16B33/00—Features common to bolt and nut
• • C—CHEMISTRY; METALLURGY
  • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
  • C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
  • C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
  • C12N1/20—Bacteria; Culture media therefor
• • C—CHEMISTRY; METALLURGY
  • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
  • C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
  • C12M21/00—Bioreactors or fermenters specially adapted for specific uses
  • C12M21/04—Bioreactors or fermenters specially adapted for specific uses for producing gas, e.g. biogas
• • C—CHEMISTRY; METALLURGY
  • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
  • C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
  • C12M23/00—Constructional details, e.g. recesses, hinges
  • C12M23/58—Reaction vessels connected in series or in parallel
• • C—CHEMISTRY; METALLURGY
  • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
  • C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
  • C12M41/00—Means for regulation, monitoring, measurement or control, e.g. flow regulation
  • C12M41/30—Means for regulation, monitoring, measurement or control, e.g. flow regulation of concentration
  • C12M41/32—Means for regulation, monitoring, measurement or control, e.g. flow regulation of concentration of substances in solution
• • C—CHEMISTRY; METALLURGY
  • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
  • C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
  • C12M41/00—Means for regulation, monitoring, measurement or control, e.g. flow regulation
  • C12M41/30—Means for regulation, monitoring, measurement or control, e.g. flow regulation of concentration
  • C12M41/34—Means for regulation, monitoring, measurement or control, e.g. flow regulation of concentration of gas
• • C—CHEMISTRY; METALLURGY
  • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
  • C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
  • C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
  • C12N1/26—Processes using, or culture media containing, hydrocarbons
• • 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
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
  • C23C22/82—After-treatment
  • C23C22/83—Chemical after-treatment
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
  • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
• • 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
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E50/00—Technologies for the production of fuel of non-fossil origin
  • Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel

Definitions

• the invention relates to a process for the production of biogas from predominantly starchy raw materials as biomass by a multi-stage anaerobic conversion by wet fermentation as primary fermentation (hydrolysis and acidogenesis) and secondary fermentation (acetogenesis and methanogenesis), in at least two separate fermentation stages.
• biogas is carried out in a conventional manner in one or more reactors or fermenters, the mesophilic ⁇ temperatures below 45 ° C) or thermophilic (temperatures 45 to 80 ° C) can be operated.
• biodegradation processes take place in four stages during the reaction, such as hydrolysis, acidogenesis, acetogenesis and methanogenesis.
• the first two stages of hydrolysis and acidogenesis are referred to as primary fermentation and acetogenesis and methanogenesis as secondary fermentation.
• the biological process occurs during primary fermentation by microbial bacteria and secondary fermentation by microbial archaea.
• the decomposition processes caused by bacteria can take place under aerobic or anaerobic conditions.
• the most commonly used method is wet fermentation where the dry matter content TS is ⁇ 15% and the water content is> 85%.
• biogases with a methane content of up to 65% under thermophilic conditions and mesophilic conditions of up to 53% can be obtained.
• the methane content varies by +/- 1 to 2% on average over the day.
• Purified biogas (methane) is used, among other things, for heating purposes, eg in combined heat and power plants, or as an energy source for feeding into natural gas networks.
• other impurities in particular hydrogen sulfide, nitrogen and ammonia
• still contained in biogas C0 2 must be separated to obtain a suitable for further use methane gas desired quality.
• the purification or processing of biogas is a technologically complicated process, which is associated with a high expenditure on apparatus.
• a general disadvantage of the known methods are too low yields of methane in the conversion of biomass to biogas and too low methane concentrations in a mesophilic biological reaction, and the relatively high levels of hydrogen sulfide and ammonia in the biogas produced.
• the invention has for its object to provide processes for the production of biogas from predominantly starchy raw materials as biomass, which can be achieved with a higher yield of raw or biogas and a higher content of methane in the raw gas.
• the predominantly starch-containing raw materials used as biomass are cereals, in particular corn, wheat, barley, manioc, rye, as well as potatoes, rice, grass, seeds and milk juice, individually or as a mixture, but without the addition of other starting materials, such as e.g. Manure or sewage sludge.
• the anaerobic conversion of the biomass takes place in at least two, preferably three, separate fermentation stages.
• the first fermentation stage only biomass at temperatures in the range of 40 to 65 X, which depend on the TS content of the biomass, supplying a subset of liquid fermentation substrate, which comes from a different approach to a previous first fermentation stage and has a temperature at least as high as the temperature of the first fermentation stage, primarily fermented. In this case, heat energy is released by spontaneous propagation of the acidophilic bacteria contained in the supplied liquid fermentation substrate. This increases the temperature in this stage much faster by a few ° C.
• the resulting fermentation substrate is separated into a solid phase and a liquid phase, wherein at least a portion of the separated fermentation liquid is fed to the batch for a new first fermentation stage.
• the aqueous phase (fermentation liquor) obtained after the end of the first fermentation stage are returned to the first fermentation stage for a new batch.
• the acidophilic bacteria contained in the fermentation liquid multiply after repatriation in the first fermentation stage by bifurcation, binary cleavage or budding after just a few minutes to one hour, resulting in the new approach (first fermentation stage) to a spontaneous primary fermentation with release of heat.
• the initial pH drops from 7 to 5.3. However, the pH is not used as a parameter for the reaction.
• the microbiological anaerobic conversion takes place in the first stage of fermentation by means of anaerobic bacteria (desulphuricides), which in the first fermentation stage Substrate sulfate to reduce sulfide within a few hours.
• the sulfide obtained dissociates in water to sulfide ions (S 2 " ) and the sulfide ions formed are in equilibrium with hydrogen sulfide ions (HS) and those with undissociated hydrogen sulfide according to the following reaction equations:
• the solid hare separated off after the first fermentation stage is subjected to secondary fermentation in at least one further fermentation stage over a period of at least 10 days.
• biogas is formed with a methane content of about 60 to 85 vol .-%, which is free of elemental oxygen and sulfur.
• existing carbon sources such as carbon monoxide, formic acid, formaldehyde, methanol and other hydrocarbons, take over the role of carbon dioxide as a carbon source in methanogenesis and also formed in the fermentation substrate alcohols methane arises. This makes it possible to obtain biogas with a methane content of more than 60% from starchy raw materials.
• the biogases obtained in the respective fermentation stages are worked up or purified separately for the production of methane and fed, for example, to different uses.
• the first fermentation stage is preferably carried out in a separate fermenter in batch mode.
• the second fermentation stage is operated in a continuous flow process.
• the batch mode is again preferred.
• the TS load in the third and fourth stage is significantly lower.
• the biomass used can almost completely ferment. The accumulating digestate can thus be disposed of more easily.
• At least the sulfur compounds and ammonia contained therein should be partially removed.
• at least one of the components contained in the biogas, C0 2 , CH 4 , hydrogen and / or hydrogen sulfide is measured by means of gas probes known per se and after reaching a predetermined limit value, the first fermentation stage is terminated or terminated.
• the C0 2 content has reached at least a value of 60% by volume, or the CH 4 content of 10 to 35% by volume, preferably 15 to 20% by volume, in the non-combustible range, is, or shortly after reaching a concentration peak of the hydrogen content of less than 0.5 vol .-%, preferably 0.2 vol .-%, in the non-combustible range, or shortly after reaching a concentration peak of hydrogen sulfide with a content below 0, 2 vol .-%, preferably 0.05 vol .-%, in the non-combustible range.
• the biomass is adjusted to a TS content of 1 to 12%.
• the space load of (kg oTS / m 3 d) is of no importance in the first fermentation stage, since this process is not continuous. This parameter indicates how much organic dry matter per cubic meter of fermenter volume per day is being fed.
• the first fermentation stage is run exclusively as a function of the TS content, the residence time of the fermentation substrate in the fermenter and at least the gas concentration of one of the components contained in the biogas. The residence time is in turn dependent on the composition of the biomass used.
• the fermentation substrate in the second and subsequent fermentation stages is treated at temperatures lower than the temperature in the first fermentation stage, but should not fall below a temperature of 25 ° C.
• the second fermentation stage is operated quasi-continuously with a volume loading of 0.5 to 10 kg oTS / md, preferably 1 to 6 kg oTS / m 3 d.
• the temperature of the fermentation substrate is maintained at 35 to 45 ° C during the residence time.
• the residence time is 5 to 30 days, preferably 7 to 21 days. As adjustment parameters, only the space load and residence time are used for a desired methane concentration of the second fermentation stage.
• the DM content is set in the second fermentation stage to a maximum value of 3 to 12%, preferably 5 to 10% at the inlet to the fermenter. A targeted interruption of the fermentation does not take place.
• the fermenter is designed to prevent a direct short-circuit flow of fermentation substrate.
• the resulting average pH value is 6.4 to 7.5, depending on the room load and the fermentation substrate used. Biogas produced under these conditions is free of oxygen and contains only a small amount of less than 10 ppm of ammonia and hydrogen sulfide.
• Of the Level of the second fermentation stage is used as a defined buffer volume.
• fermented substrate can now be continuously or cyclically discharged from the second fermenter stage via a small solids pump and fed via a separation device to a third fermentation stage. Since the TS content is approximately halved during the residence time of the fermentation substrate in the second fermenter, the TS content of the fermentation substrate for the processing in the third fermenter stage is raised again with the separation device and thus the total amount of concentrated fermentation substrate is halved. The separated liquid phase is returned to the first and / or second fermentation stage. With this procedure, a complete fermentation is achieved in the third fermentation stage at high TS content and long residence times of 30 to 90 days.
• a second fermenter is filled analogously after about 30 days after filling of the first fermenter.
• the biogas production in this third fermentation stage is reduced daily, and if it falls below 0.5% of the total gas production of the second and third fermentation stage, the fermentation process in the first fermenter, the is in the "rest or fermentation phase” is completed and it is the fermentation substrate from this fermenter via a decanter to a TS content of up to 30% concentrated and stored in a closed digestate storage.
• the separated liquid phase is stored intermediately and returned to the first and / or second fermentation stage, for adjusting the TS content.
• the emptied fermenter is available for a next cycle of the third fermentation stage.
• a fermentation substrate based on another raw material with a starch content of less than 10% can be admixed to the fermentation substrate, for example, fats are still added to the fermentation substrate maize after separation of the liquid phase in the second fermentation stage. It should be noted that this addition does not lead to increased levels of hydrogen sulfide and ammonia.
• biogas with a methane content of 68.0% by volume is obtained.
• biogas with methane contents of 50 to 55% can be produced by means of known methods from corn silage.
• FIG. 1 is a schematic representation of a plant for carrying out the method according to the invention
• Fig. 2 is a simplified flow diagram for the operation of a system according to the inventive method.
• Fig. 3 shows the gas formations within the first fermentation stage as a diagram, based on the use of maize silage as biomass.
• FIG. 1 is explained in conjunction with Examples 1 and 2.
• a fermenter F1 is provided for the first fermentation stage and a fermenter F2 for the second fermentation stage.
• two fermenters F3A and F3B are used, which are operated batchwise.
• the fermenter F1 is also operated batchwise, the first fermentation stage is terminated after 2 days and the fermentation substrate is transported into the second fermenter F2, wherein in between a solid-liquid separation is carried out, as mentioned in the following example.
• the mean residence time of the fermentation substrate in the fermenter F2 is 7 to 20 days, whereby a quantity of fermentation substrate is continuously passed from the fermenter F2 into another fermenter F3A over a period of 20-50 days. Thereafter, the fermenter F3A is no longer supplied with fermentation substrate. Fermenter substrate F2 is then transferred to the second fermenter F3B. After another time of e.g. For 20 days, the fermentation substrate in the fermenter F3A is so far outgrown that the biogas production in this fermenter F3A is less than 0.5%, based on the sum of the biogas production in the fermenters F2 and F3B.
• the fermenters F1 to F2 are preferably round containers, which are equipped with a heating and stirring technology.
• the fermenter F2 has a foil roof, in which a flexible gas storage takes place.
• the other fermenters F1 and F3, as well as the closed digestate store, may be containers with a solid concrete or other suitable material.
• two fermenters F1A and F1B are provided for realizing the first fermentation stage.
• the desired biogas composition can be adjusted in a more targeted manner, thus achieving more even biogas production in a narrower concentration range.
• two fermenters F1A and F1B are operated in parallel in the first fermentation stage, so that the daily entry into the fermenter F2 of the second fermentation stage can be carried out continuously.
• This procedure is advantageous because the composition differs from the crop specific crop and thus fermentation substrate mixtures can be processed better.
• This variant allows for a more flexible residence time adjustment and thus switching of the process to the subsequent secondary fermentation.
• the maize silage has a TS content of 32% of which 96% is organic. This processes 61. 4 kg oTS per day.
• the corn silage is fed to the fermenter F1 for carrying out the first fermentation stage, together with acidophilic fermentation liquid from the container B1.
• the fermentation liquid is heated to a temperature of 55 ° C.
• the fermenter F1 has a volume of 25 m 3 and is kept at a temperature of 50 ° C by means of integrated heating. Under these conditions, the pH of the fermentation substrate is reduced from 6.9 to 5.36 over a period of 24 hours.
• the residence time can be adjusted via the fermenter temperature.
• the concentration of biogas which depends on the concentration during this time, including the components C0 2 , CH 4 and H 2, is shown in FIG. 3.
• This biogas is removed via the line L1 and purified by means of suitable and known gas scrubbing and dried.
• H 2 S, NH 3 and C0 2 are removed.
• the biogas withdrawn via line L1 contains 22.46 Nm 3 of methane, which corresponds to a calorific value of 248 kW.
• the calorific value of the contained H 2 is only 0.9 kW and is not lost.
• the purified gas is concentrated (to 50 Vo! .-% methane).
• This purified biogas (methane gas) can be used as heating gas for a CHP with an electrical output of 3.9 kW. About 5 kW can be discharged continuously as hot water at a temperature of 90 ° C.
• the content of methane is measured by means of a gas measuring probe and when a measured value of 30% by volume is reached, the first fermentation stage is stopped, whereby already 27% of the oTS (organic dry substance) contained in the fermentation substrate has been degraded in the fermenter F1 , In addition, the value of hydrogen sulfide is controlled to fall below 1,000 ppm.
• the fermentation substrate is fed via the associated line by means of the pump P1 from the first fermenter F1 for further biological conversion (second fermentation stage) via the separation unit S1 to the second fermenter F2, in the separation unit S1 5 m 3 of fermentation liquid are separated into the container B1 arrive. If necessary, fermentation liquid is conveyed into the fermenter F1 via a corresponding line by means of the pump P2.
• the fermentation substrate coming in the separation device S1 is kept constant at a temperature of about 40.degree.
• the Fermenter F2 works as a high-performance fermenter with a mean residence time of 14 days and a TS content of 10%.
• the fermenter F2 has a volume of 80 m 3 , with 65 m 3 are available as working volume.
• the space load is 3.45 kg oTS / m 3 d.
• the fermentation substrate obtained in the fermenter F2 can either be supplied to the digestate store GRL or to another fermenter F3
• Example 2 differs from Example 1 only in that the second fermentation stage is still followed by a third fermentation stage.
• the fermented in fermenter F2 substrate is transported in an amount of 100 l / h via the associated line by the pump P3 continuously to the separator S2, by means of which a separation of the fermentation substrate is carried out in a liquid phase and solid phase.
• the liquid phase passes into the container B2 and can be returned, if necessary, via a line by means of the pump P4 in the Prozeßwasserkeislauf.
• the solid phase with a TS content of 5% passes into the fermenter F3.
• the liquid phase is supplied to the container B2.
• the fermenter F3 has a volume of 50 m 3 and is filled in 20 days.
• the fermenter F3 shown in FIG. 1 corresponds in a batch mode with two identical fermenters to the fermenter F3A (variant 2 in FIG. 2).
• the parallel fermenter F3B is handled analogously via the pump P3.
• the fermenter F3A continues to produce biogas. However, as no further fermentation substrate is supplied, the biogas production stops.
• the fermenter F3A will continue to operate until its biogas production has decreased from 45 to less than 2 Nm 3 per day. This is the case after another 20 days.
• the obtainedgorene substrate is concentrated via a decanter D1 to a solids content of 28% and spent in the digestate storage GRL.
• Separated fermentation liquid is collected in the container B3 and, if necessary, for adjusting the TS content via the associated line, is integrated into the pump P5, passed into the fermenter F1 and / or F2. No longer required quantities of fermentation liquid are disposed of.
• the Ausgärphase (20 days) still produced biogas is discharged via the line L3 of the fermenter F3B, after cleaning, an average of 11, 8 Nm 3 methane per day are obtained.
• Another advantage is that a separate purification of the individual biogas streams from the fermenters F1, F2 and F3 is much cheaper than a purification of a Rescuebiogasstromes, which is formed from the individual streams.

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