WO2011049572A1 - Traitement hydrothermique (htp) d'algues qui se sont développées dans des flux de déchets htp - Google Patents

Traitement hydrothermique (htp) d'algues qui se sont développées dans des flux de déchets htp Download PDF

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Publication number
WO2011049572A1
WO2011049572A1 PCT/US2009/061656 US2009061656W WO2011049572A1 WO 2011049572 A1 WO2011049572 A1 WO 2011049572A1 US 2009061656 W US2009061656 W US 2009061656W WO 2011049572 A1 WO2011049572 A1 WO 2011049572A1
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Prior art keywords
fraction
concentrated
algae
organism
biosolid
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PCT/US2009/061656
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English (en)
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Lance Schideman
Yuanhui Zhang
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The Board Of Trustees Of The University Of Illinois
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Priority to CA 2814641 priority Critical patent/CA2814641A1/fr
Priority to BR112012009461A priority patent/BR112012009461A2/pt
Priority to PCT/US2009/061656 priority patent/WO2011049572A1/fr
Priority to MX2012004676A priority patent/MX2012004676A/es
Priority to US13/502,862 priority patent/US20120198758A1/en
Publication of WO2011049572A1 publication Critical patent/WO2011049572A1/fr

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    • 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
    • C12N1/12—Unicellular algae; Culture media therefor
    • 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
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/64—Fats; Fatty oils; Ester-type waxes; Higher fatty acids, i.e. having at least seven carbon atoms in an unbroken chain bound to a carboxyl group; Oxidised oils or fats
    • C12P7/6436—Fatty acid esters
    • C12P7/6445—Glycerides
    • C12P7/6463—Glycerides obtained from glyceride producing microorganisms, e.g. single cell oil
    • 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
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Definitions

  • This invention relates to a process for the chemical conversion of organic waste to liquid fuel.
  • the invention relates to a high temperature, high pressure conversions of organic biowastes and organisms cultivated in a wastewater stream into a biocrude oil product.
  • the biocrude oil product may be used as a fuel directly or subsequently refined into motor grade fuels, asphalt, plastics, and other products commonly made from crude petroleum.
  • First generation biofuels include corn ethanol and soy biodiesel. However, these fuels have the disadvantage that they divert food production to fuel production. Second generation biofuels were developed including cellulostic ethanol to reduce the food versus fuel concerns, but still suffered from sustainability issues such as high water input and degradation of soil nutrients. Third generation biofuels were developed including algae which also addressed the food versus fuel concerns and soil nutrient depletion. Algae can grow in water bodies and other land surfaces that are not suitable for crop production.
  • algae for biofuels are their unparalleled growth rates and the high lipid content of certain species, which have been shown to be sufficiently high that 200,000 hectares (0.1 % of arable US land) could potentially produce one quad (10 15 BTU) of fuel (Sheehan et al., 1998).
  • algae can grow in water bodies and other land surfaces that are not suitable for crop production. Given that the total US oil consumption is less than 50 quads per year, algae based biofuels could completely replace liquid petroleum fuels without significantly compromising the availability of land for food production, a critical limitation of other current bioenergy paradigms.
  • Phototrophic organisms such as cyanobacteria and algae can also produce a wide variety of higher-value co- products including food, nutritional supplements, aquacultural feedstock, and pharmaceuticals that could help support the economic viability of algae biofuels (Shimizu, Y. 1996. "Microalgal metabolites: a new perspective.” Annual Review of Microbiology 50:431 -465.; Ghirardi, M.L, L. Zhang, J.W. Lee, T. Flynn, M. Seibert, E. Greenbaum, and A. Melis. 2000. "Microalgae: a green source of renewable hydrogen.” Trends Biotechnol. 18: 506-51 1 ).
  • Cantrell Cantrell et al. Bioresource Techonology, 2008, 99, 7941 -7953. discloses a wet gasification approach for processing algal biomass.
  • gasification utilizes relatively high temperatures and pressures for and the energy input requirements may exceed the energy yielded.
  • One embodiment of the invention is directed to a process for conversion of organic biowaste to biocrude oil.
  • the process comprises providing a concentrated biosolid fraction and a bypass liquid fraction obtained from organic biowaste.
  • the concentrated biosolid fraction is subjected to a hydrothermal process under conditions sufficient to obtain a biocrude oil product, an aqueous residual product, and a gaseous residual product.
  • a solid residual product may also be formed.
  • An organism is cultivated in a culturing media to obtain a cultivated mixture, and a concentrated cultivated organism fraction is recovered from the cultivated mixture.
  • the concentrated cultivated organism fraction and optionally the concentrated biosolid fraction are introduced to the hydrothermal process.
  • the culturing media may comprise the aqueous residual product and optionally further comprise the bypass liquid fraction in at least 50% by volume, for example.
  • the process may further comprise separating a concentrated biosolid fraction and a bypass liquid fraction from organic biowaste.
  • the bypass liquid fraction is at least 50 percent of the organic biowaste on a total volume basis, more preferably 80%.
  • the concentrated biosolid fraction may comprise at least 5 percent total solids by weight, preferably at least 10 percent.
  • concentrated cultivated organism fraction comprises at least 5 percent by weight total solids, preferably at least 10 percent.
  • the ratio of concentrated cultivated organism fraction to concentrated biosolid fraction introduced to the hydrothermal process may be greater than about 5 percent on a total solids basis, preferably greater than about 25 percent.
  • the process may further comprise introducing the gaseous residual product to the culturing media.
  • the organic biowaste may be animal waste, animal manure, human waste from a municipal sewage stream, or food processing waste.
  • the organism may be algae or bacterial.
  • the hydrothermal process may be carried out at a temperature less than 320 °C and at a pressure above 0.5 MPa.
  • FIG. 1 is a process schematic of hydrothermal conversion of organic biowaste and algae grown in an HTP aqueous residual waste stream.
  • FIG. 2 is representative graph of percent refined oil yield and initial lipid content for different feedstocks.
  • FIG. 3 is representative graphs of mixed algae growth with post-HTP wastewater treatment.
  • FIG. 4 is representative graphs of mixed algae growth with post-HTP wastewater treatment demonstrated by: (a) biomass increase measured as percent solids; (b) organic pollutants consumption measured as chemical oxygen demand (COD); and (c) nutrient consumption measured as total nitrogen (TN).
  • FIG. 5 is a representative graph of DNA concentration of antibiotic resistant E. coli before and after HTP treatment.
  • FIG. 6 is a representative graph product yield versus temperature for HTP conversion of Chlorella pyrenoidosa.
  • FIG. 7 is a representative graph of growth of UCSD algae (upper line) and COD levels (lower line) with regular addition of post-HTP wastewater.
  • FIG. 8 is a representative table of HTP conversion tests with algae.
  • the process of the present invention uses of waste material inputs to produce a significant quantity of biocrude oil product.
  • the process provides a loop that may recycle nutrients in the hydrothermal process (HTP) aqueous residual product and may recycle the carbon dioxide in the HTP gaseous product as it combines multiple cycles of organism cultivation with subsequent HTP conversion to biocrude oil product.
  • HTP hydrothermal process
  • the process improves the cost-effectiveness of other algae- based biofuel production approaches by eliminating several key bottlenecks.
  • the process allows multiple use cycles for aqueous residual product which comprises the nutrients for organism growth.
  • Nutrients and carbon dioxide are two of the primary input costs in conventional algae growth processes, which may be reduced or eliminated.
  • HTP conversion of algae biomass does not require high oil content algae, because HTP converts other biomass components to oil.
  • HTP provides cost-effective extraction of oil from wet algae biomass without drying, which is a major energy loss in most contemporary algae to-biofuel paradigms. In short, the present process reduces input costs, increases algae oil production capabilities and reduces the energy inputs required for extracting algae biofuel products.
  • the process of the present invention also provides environmental benefits during the fuel generation process which may include improving water quality, conserving fresh water resources, sequestering carbon dioxide, reducing solid waste quantities, and destroying residual pharmaceuticals and antibiotic resistant genetic materials in human and animal wastes.
  • a feedstock is provided which comprises organic biowaste.
  • Organic biowaste includes, for example, animal waste, human waste, food processing waste, garden or park waste, paper waste and the like or combinations thereof.
  • Animal waste may include animal feces, animal urine, manure, slaughterhouse waste, and the like.
  • Human waste may include human feces, human urine, bodily fluids, and the like.
  • Human waste may be a component of a municipal sewage stream waste.
  • Municipal sewage streamwaste is water- carried waste from a community, or the used water supply of the community.
  • Municipal sewage streamwaste may comprise food wastes, pharmaceutical waste including antibiotics and other medicines, antibiotic resistant genetic materials, and other waste products of normal living.
  • Food processing waste is waste produced from during the preparation of food for humans or animals from harvested crops or slaughtered and butchered animal products, particularly in the food processing industry.
  • a concentrated biosolid fraction and a bypass liquid fraction are provided.
  • the concentrated biosolid fraction and bypass liquid fraction are obtained from organic biowaste and may be separated from the organic biowaste as part of the present process or in a separate process.
  • the organic biowaste may separated into a concentrated biosolid fraction and a bypass liquid fraction from the organic biowaste feedstock by any suitable separation process method known to one skilled in the art, including for example, gravity settling, centrifugation, membrane filtration, etc.
  • the concentrated biosolid fraction may comprise at least 5 % total solids by weight, preferably at least 10 %.
  • the concentrated biosolid fraction is subjected to a hydrothermal process (HTP) under conditions sufficient to obtain a biocrude oil product, an aqueous residual product, a gaseous product and optionally a solid residual product.
  • a hydrothermal process (HTP) also known to one skilled in the art as liquefaction, is a process wherein a fluid stream or slurry is subjected to elevated temperature and pressure which causes chemical reactions to occur, resulting in the conversion of volatile solids into organic oils.
  • Typical temperatures for HTP conversion range from about 200 - 350 °C. Maximum pressures of 3 to 20 MPa are maintained in order to keep water in a liquid form at the elevated temperatures.
  • the hydrothermal process of the present invention uses a temperature between about 200 and about 320 °C, preferably less than 250 °C.
  • the hydrothermal process uses a pressure less than about 1 1 MPa, preferably less than 7 mPa, more preferably less than about 4 MPa.
  • the residual solid product when obtained from the hydrothermal process may be used as fertilizer.
  • the bypass liquid fraction obtained from the organic biowaste feedstock is at least 50 % of the organic biowaste on a total volume basis, preferably at least 80 % of the organic biowaste on a total volume basis.
  • the bypass liquid fraction may be combined with the aqueous residual product from the hydrothermal process, which contains most of the nutrients (such as nitrogen and phosphorous) from the organic biowaste feedstock.
  • Organisms including for example algae, bacteria and combinations thereof are cultivated in a culturing media.
  • the culturing media may be any media suitable for growing the organism.
  • the culturing media may comprise the aqueous residual product or both the bypass liquid fraction and the aqueous residual product.
  • the ratio of the bypass liquid fraction to the aqueous residual may be about 1 :1 to about 20:1 by volume, preferably about 5:1 to about 15:1 by volume.
  • organism refers to algae and microorganisms, including for example bacteria, fungi, archaea, protists, rotifers, and nematodes.
  • algae refers to microalgae, macroalgae, eukaryotic algae, prokaryotic cyanobacteria, green algae, blue-green algae, brown algae, red algae, and diatoms.
  • low lipid algae may be employed, including species of Chlorella, Spirulina, and mixed species grown in wastewater.
  • Low-lipid algae may comprise less than 20 weight % lipid content in some aspects and less than 10 weight % lipid content in other aspects.
  • photosynthetic cyanobacteria including Spirulina may be used.
  • a combination of organisms may be cultivated including a combination of algae and bacteria.
  • the gaseous product may be combined with the organism cultivation.
  • the gaseous product is mainly comprised of carbon dioxide, but may also be comprised of various other minor gases such as methane, carbon monoxide, hydrogen, hydrogen sulfide and nitrogen. Since photosynthetic bacteria and algae consume carbon dioxide, carbon dioxide present in the gaseous product will be at least partially consumed when it is introduced to the culturing media used for growing organisms.
  • Previous algae-to biofuel research focused on growing algae with high lipid content and then extracting the oil from it.
  • high oil content algae usually have lower yields, which is a critical limitation for economic viability.
  • the present invention is not limited to high lipid content algae or high oil content algae, because HTP converts other biomass components to biocrude oil products.
  • HTP fast-growing, high-yield but low-lipid algae may be used for biofuel production.
  • Fast-growing algae and photosynthetic bacteria have key advantages over other biofuel paradigms because they can grow at rates at or above other land based plants, can be grown on non-arable land, and have simple cell walls that may be generally easier to convert to useful oils than other crops.
  • Organism growth need not be limited to a single species of organism since HTP can convert mixtures of organisms to biocrude oil product.
  • mixed algal-bacteria cultures may be employed including those collected from sewage plants.
  • the cultivated mixture may be separated into a liquid fraction comprising clean water and a concentrated cultivated organism fraction comprising the organism growth.
  • the concentrated cultivated organism fraction is then fed back into the HTP reactor as a sole feedstock or mixed with other concentrated biosolids, to produce more biocrude oil product.
  • the ratio of concentrated cultivated organism fraction to concentrated biosolid fraction may be greater than about 5:95 on a total solids basis, preferably greater than about 10:90, more preferably greater than about 25:75.
  • a synergistic effect may be obtained for various combinations of organisms and feedstocks.
  • the refined oil yield for mixtures of swine manure with Chlorella and swine manure with Spirulina was higher than the average of two individual components indicating a synergy when mixing these feedstocks.
  • the refined oil yield is only the toluene soluble fraction of the crude oil.
  • refined oil represents anywhere from 40 to 80% of the crude oil.
  • the refined oil content usually provides a more consistent measurement of the HTP trials.
  • the biocrude oil product may be characterized by a heating value of at least 25,000 kJ/kg, preferably, 28,000 kJ/kg, more preferably 32,000 kJ/kg.
  • the process comprises separating a concentrated biosolid fraction and a bypass liquid fraction from organic biowaste and subjecting the concentrated biosolid fraction to a hydrothermal process under conditions sufficient to obtain a biocrude oil product and an aqueous residual product.
  • An organism is cultivated in a culturing media comprising the aqueous residual product, and a concentrated cultivated organism fraction is recovered from the cultivated mixture.
  • the concentrated cultivated organism fraction in introduced into the hydrothermal process with the concentrated biosolid fraction, wherein a ratio of concentrated cultivated organism fraction to concentrated biosolid fraction is greater than about 5:95 on a total solids basis.
  • the process further comprises combining the aqueous residual product and the bypass liquid fraction, wherein the culturing media in which the organism is cultivated comprises the combined aqueous residual product and the bypass liquid fraction.
  • the bypass liquid fraction is at least 50 percent of the organic biowaste on a total volume basis; in others the bypass liquid fraction is at least 80 percent of the organic biowaste.
  • the concentrated biosolid fraction comprises total solids between about 1 percent and about 50 percent of the total solids of the organic biowaste feedstock.
  • the organism may be algae or bacteria or low lipid algae.
  • the hydrothermal process may be carried out at a temperature less than 250 °C and at a pressure less than 10 MPa.
  • the biocrude oil product may be
  • Another embodiment of the present invention is directed to a process for the conversion of animal waste to biocrude oil.
  • the process comprises preparing a feedstock from animal waste.
  • a concentrated biosolid fraction and a bypass liquid fraction is separated from the feedstock and the concentrated biosolid fraction is subjected to a hydrothermal process under conditions sufficient to obtain a biocrude oil product, an aqueous residual product, and a gaseous product.
  • the aqueous residual product and the bypass liquid fraction are combined and algae is cultivated in a culturing media comprising the aqueous residual product and the bypass liquid fraction to obtain a cultivated mixture.
  • a concentrated cultivated algae fraction is recovered from the cultivated mixture, and the concentrated cultivated algae fraction is introduced into the hydrothermal process with the concentrated biosolid fraction.
  • the algae may be low lipid algae or selected from the group consisting of Chlorella and Spirulina.
  • the feedstock may be animal manure.
  • the ratio of algae growth to concentrated biosolid fraction introduced to the hydrothermal process may be between 25:75 and 75:25 on a total solids basis.
  • Another embodiment of the present invention is directed to a process for conversion of human waste from a municipal sewage stream to biocrude oil.
  • the process comprises preparing a feedstock from a municipal sewage stream.
  • a concentrated biosolid fraction and a bypass liquid fraction are separated from the feedstock, and the concentrated biosolid fraction subjected to a hydrothermal process under conditions sufficient to obtain a biocrude oil product, an aqueous residual product, and a gaseous product.
  • the aqueous residual product and the bypass liquid fraction are combined, and an organism is cultivated in a culturing media comprising the combined aqueous residual product and the bypass liquid fraction to obtain a cultivated mixture.
  • a concentrated cultivated organism fraction is recovered from the cultivated mixture, and the concentrated cultivated organism fraction is introduced to the hydrothermal process with the concentrated biosolid fraction, wherein the ratio of concentrated cultivated organism fraction to
  • the concentrated biosolid fraction is between 10:90 and 90:10 on a total solids basis.
  • the organism may be algae or algae comprising less than about 20 weight percent lipid.
  • the concentrated cultivated organism fraction comprises algae and bacteria.
  • a process for conversion of organic biowaste to biocrude oil comprises providing an organic biowaste feedstock comprising organic biowaste and separating a concentrated biosolid fraction and a bypass liquid fraction from the organic biowaste, wherein the bypass liquid fraction is at least 50 percent of the organic biowaste on a total volume basis.
  • the concentrated biosolid fraction is subjected to a hydrothermal process under conditions sufficient to obtain a biocrude oil product, an aqueous residual product, and a gaseous product.
  • the aqueous residual product and the bypass liquid fraction are combined.
  • a microorganism is cultivated in a
  • cultivating media comprising the combined aqueous residual product and the bypass liquid fraction to obtain a cultivated mixture, and the gaseous product is introduced into the cultivated mixture.
  • a concentrated cultivated microorganism fraction is recovered from the cultivated mixture, and introduced to the
  • the HTP process was run according the procedure of He and Ocfemia (He, B.J., Y. Zhang, Y. Yin, T.L. Funk and G.L. Riskowski. Transactions of Amer. Soc. Agr. Engr. 43(6): 1827-1833; He, B. J., Y. Zhang, Y. Yin, T. L. Funk and G.L. Riskowski. Transactions of Amer. Soc. Agr. Engr. 44(6): 1873-1880; He, B.J., Y. Zhang, Y. Yin, T.L. Funk and G.L. Riskowski. Transactions of Amer. Soc. Agr. Engr. 44(6): 1865-1872; He, B.J., Y. Zhang, Y. Yin, T. L. Funk and G.L. Riskowski.
  • FIG. 2 the initial lipid content and refined oil yields after hydro- thermal processing (HTP) for a variety of feedstocks including several tests with algae is shown.
  • HTP hydro- thermal processing
  • the mixed algae species were collected from the Urbana- Champaign Sanitary District- North Wastewater Treatment Plant.
  • the dry solids content of the feedstock was measured by drying in an oven at 105 °C.
  • the solids content of the feedstock was adjusted to 20% either by adding tap water or by oven drying, which generally resulted in a slurry consistency.
  • Wet feedstock slurry 800 g was loaded into an HTP reactor with a total volume of 2 L. After the reactor was carefully sealed, the reactor headspace was purged 3 times with nitrogen to remove the residual air, and then more nitrogen was added to increase the desired initial pressure, typically about 0.65 MPa.
  • the reactor was subsequently heated by an electrical heating element to achieve the desired experimental temperature, generally in the range of 200 to 320 °C.
  • the heat-up period may last up to 60 minutes, and then the reaction temperature was maintained for the desired retention time of the reaction, which was varied between 0 and 120 minutes.
  • Reactor pressure was allowed to increase over the course of the heated reaction, but once the desired temperature was reached, pressured remain fairly stable at values generally between 3 to 1 1 MPa.
  • the reaction mixture generally includes an oil phase, an aqueous phase and a solid phase which are processed as follows.
  • the oil phase of the reaction mixture self separates due to lower density and is recovered by decanting.
  • the oil phase typically retains some water, so the moisture content of the oil phase is determined by using a distillation apparatus in accordance with ASTM Standard D95-99 (ASTM D95-99.
  • the initial lipid content of the feedstock material was analyzed by Midwest Laboratories, Inc. (Omaha, Iowa) according to the standard methods of AOAC 945.16 (Association of Official Analytical Chemists) for crude fat determination. Despite low initial lipid content in the algae (Chlorella at 2% lipid) and cyanobacteria (Spirulina below 0.5% lipid), HTP conversion of these algae samples yielded 30-40% refined oil.
  • FIG. 2 presents the results from HTP conversion of three types of algal feedstocks that represent a significant range of genetic, physiological, and environmental characteristics. Additional algal samples subjected to HTP
  • FIG. 8 shows that 12 different types of algal feedstocks were used in the HTP tests including various pure microalgae species, pure macroalgae species and mixed species samples taken from various cultures and naturally occurring samples.
  • raw oil yield varied from 12.9 % to 92.5 %
  • refined oil yields varied from 6.2 % to 47.4 %.
  • the raw oil yield may in some cases contain a fair amount of ash, which makes it a less reliable measure of HTP conversion efficiency.
  • the refined oil yield which is defined based on toluene solubility of the HTP conversion products is generally a more consistent and reliable measure of conversion efficiency.
  • FIG. 6 shows tests using Chlorella algae feedstock to investigate the effects of various HTP operational parameters.
  • HTP tests were conducted at a range of temperatures from 200 to 300 °C, while all other variables were held constant.
  • the most pronounced increase in refined oil yield (24.2 % to 28.9 %) occurs between 220 °C and 240 °C.
  • solid residue drops rapidly before 240 °C, but only changes slightly for temperatures above 240 °C.
  • Retention time was another HTP operational parameter studied using the Chlorella algae feedstock.
  • reaction time was systematically varied from 0 to 30 minutes (after the reaction temperature of 240 °C was achieved)
  • refined oil production increased slightly from 26.0 % to 28.9 %.
  • Further increases of retention time up to 120 minutes increased oil yields up to 33.4 %.
  • the sizing of the HTP reactor scales linearly with the increases in the retention time, and thus represents significant effects on the capital cost of the HTP reactor.
  • Successful algal conversions were achieved when the target reaction temperature was held even for short retention times of 10 minutes or less, which corresponds to relatively small HTP reactor sizing and reduced capital cost.
  • BG1 1 a common algae growth medium, which contained the following components (mg/L): NaNO3 (1500), K 2 HPO 4 (40),
  • the algae culture (100 mL) described above during the exponential growth phase was inoculated into two 2000 mL flasks, each containing 900 mL of BG1 1 medium.
  • 5 mL of post-HTP wastewater (pw) was added at the beginning of the experiment and after 2 days. Both of the flasks were then incubated under the same culturing conditions as listed above.
  • the pw was obtained from the reaction products of HTP conversion of swine manure into biocrude oil as described earlier. Chemical characteristics of HTP post water have been analyzed and are summarized below (Appleford, J.M., Analysis and
  • HTP pw HTP pw was obtained, filtered through Whatman glass microfiber filters (Type 934-AH) to remove any large particles, and several key characteristics (COD, Ammonia, Phosphorus, and pH) were confirmed to be within the stated ranges of Table 1 .
  • Growth in the two culturing flasks was analyzed by measuring the optical density at 680 nm (OD 680) using a visible light spectrophotometer (HACH Model 2000).
  • OD 680 targets absorbance in the range where chlorophyll absorbs light and thus was used to delineate the photosynthetic growth of algae.
  • FIG. 3 shows that the mixed species UCSD wastewater algae grew better in batch culture when a small amount of HTP pw (squares,approximately 0.5% of batch volume) was added on day zero and day two than without post-HTP water
  • HTP pw was added six times over the course of seven days with small doses the first 4 times (approximately 1 % of total volume and larger doses the last two days (approximately 3 % of the total volume).
  • OD 680 was measured regularly during this test, and showed steady algae growth while HTP pw was being added, but algae growth peaked shortly after HTP pw dosing was stopped. During the period shown in FIG. 7, the total amount of HTP pw added accounted for about 15 % of the culture media. This batch culture was allowed to grow for another 40 days without further addition of
  • FIG. 1 dilution of HTP pw is shown by the combination of HTP pw with the biowaste decant liquid that bypasses the HTP process.
  • FIG. 4(a) shows an example of a onetime dose of post-HTP wastewater.
  • the biomass increase was monitored as percent solids, which showed a rapid growth of cells in response to the post-HTP wastewater addition at time zero.
  • FIG. 4(b) shows that the algae consumed organic pollutants measured as chemical oxygen demand (COD).
  • FIG. 4(c) shows that the algae consumed nutrients measured as total nitrogen (TN) to demonstrate clean up of the post-HTP
  • the data in FIG. 4 was generated in a batch test using algae to degrade post-HTP wastewater. Specifically, 10 ml_ filtered of post-HTP wastewater was added into 990 ml_ BG1 1 medium and 100 ml_ of a mixed algae culture grown up from a seed taken at the USCD wastewater treatment plant as described earlier. Algae growth was quantified in terms of dry weight, which was measured by filtration of aliquots on Millipore mixed cellulose ester 0.45 ⁇ filter that were subsequently dried at 105 °C for 24 h. This dry weight data is presented on the left side of FIG. 4. Algae growth was also measured by OD 680, and there was a direct correlation between OD 680 and dry cell weight.
  • FIG. 4(b) shows the chemical oxygen demand (COD) as determined by visible light absorbance after dichromate digestion according to standard methods. Total nitrogen and total phosphorous were measured in the filtrate according to standard methods approved the Environmental Protection Agency.
  • COD chemical oxygen demand
  • E. coli strain S17-1 lambda pir
  • GFP green fluorescent protein
  • phenol:chloroform:isoamyl alcohol 25:24:1
  • the upper aqueous phase was transferred to a fresh tube and mixed with an equal volume of chloroform: isoamyl alcohol (24:1 ) and centrifuged at 12,000*g for 2 min.
  • the upper aqueous phase was transferred to a fresh tube and mixed with 2.5 volume of ice-cold 100 % ethanol and allowed to precipitated 5 min on dry ice.
  • the test tube was centrifuged at 12,000*g, the supernatant was removed, and the pellet was rinsed with 70 % ethanol.
  • the pellet was dried under vacuum and dissolved in 50 ⁇ _ of Nuclease-free water or TE buffer and kept at -20 °C before use.
  • the supernatant was discarded, and the DNA pellet was placed on the bench for 10-20 minutes to allow the ethanol to evaporate, and dissolved in 10:0.1 TE buffer (pH 8).
  • the yield of plasmid DNA extracted from liquid culture before and after running through the HTP were further verified by electrophoresis on an agarose gel, which separates DNA fragments by size.
  • the elevated heat and pressure of HTP treatment is believed to effectively degrade genetic materials (plasmid DNA) so that there is less potential for transfer of antibiotic resistance from human and animal wastes.
  • the elemental mass balance of the initial dry chlorella algae feedstock and HTP reaction products for this algae were determined using a rapid elemental analyzer that combines combustion with thermal conductivity detection (TCD) to measure the weight fraction of several primary elements including carbon, hydrogen, nitrogen and oxygen.
  • TCD thermal conductivity detection
  • the initial feedstock, the refined oil, and solid residue product were analyzed using the rapid elemental analyzer.
  • the gas product was analyzed by a Varian CP-3600 Gas Chromatograph coupled with TCD to determine the amount of several typical gasses (carbon dioxide, hydrogen, nitrogen, oxygen, carbon monoxide, and methane).
  • the GC analysis of gas products used a Haysep D 100/120 column (20-ft, 1/8-in diam), with an injection temperature of 120 °C, and a filament temperature of 140 °C.
  • the carrier gas was Helium at 30 mL/ min.
  • Most of the elemental components of the aqueous product were calculated by subtraction of the quantities measured in the other products from the quantity measured in the initial feedstock. The one exception was phosporus, which was measured in the aqueous phase product by standard methods.
  • the phosphorus quantity in the initial feedstock was determined by ICP-MS (Inductively coupled plasma-mass spectrometry), and it was not measured in the other reaction products.
  • the refined oil product was analyzed and found to comprise 57.5 % of the carbon in the original feedstock, 56.0 % of the hydrogen, 23.8 % of the nitrogen and 21 .1 % of the oxygen as shown in Table 3.
  • the resulting aqueous wastewater contained 73.1 % of the nitrogen from the original feedstock and 85% of the original phosphorus. Because most of the nitrogen and phosphorus nutrients are released during the HTP process to the aqueous product, these nutrients may be recycled back to growing another round of biomass and
  • the aqueous HTP wastewater also contains 27.4% and 40.5% of the original carbon and hydrogen, respectively, which may also potentially be captured and converted to more oil by treatment of the HTP wastewater in a mixed culture bioreactor with algae and/or bacteria.

Abstract

L'invention concerne un procédé pour la conversion de déchets organiques en biocarburant comprenant la culture d'organismes dans le produit aqueux du procédé de conversion HTP.
PCT/US2009/061656 2009-10-22 2009-10-22 Traitement hydrothermique (htp) d'algues qui se sont développées dans des flux de déchets htp WO2011049572A1 (fr)

Priority Applications (5)

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CA 2814641 CA2814641A1 (fr) 2009-10-22 2009-10-22 Traitement hydrothermique (htp) d'algues qui se sont developpees dans des flux de dechets htp
BR112012009461A BR112012009461A2 (pt) 2009-10-22 2009-10-22 processo hidrotermico (htp) de crescimento de algas em uma corrente de esgoto htp
PCT/US2009/061656 WO2011049572A1 (fr) 2009-10-22 2009-10-22 Traitement hydrothermique (htp) d'algues qui se sont développées dans des flux de déchets htp
MX2012004676A MX2012004676A (es) 2009-10-22 2009-10-22 Procesamiento hidrotermal (htp) de algas cultivadas en corrientes residuales de htp.
US13/502,862 US20120198758A1 (en) 2009-10-22 2009-10-22 Hydrothermal Processing (HTP) of Algae Grown in HTP Waste Streams

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PCT/US2009/061656 WO2011049572A1 (fr) 2009-10-22 2009-10-22 Traitement hydrothermique (htp) d'algues qui se sont développées dans des flux de déchets htp

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WO2012062962A1 (fr) * 2010-11-08 2012-05-18 Neste Oil Oyj Procédé pour l'extraction de lipides à partir d'une biomasse
CN103897801A (zh) * 2014-03-18 2014-07-02 中国农业机械化科学研究院 湿法提取小球藻油脂的方法及装置
CN107879584A (zh) * 2017-11-14 2018-04-06 东华大学 一种高效削减污泥中抗性基因的方法
CN109020126A (zh) * 2018-07-13 2018-12-18 胜利油田森诺胜利工程有限公司 一种用于含油污泥生物修复的施工工艺
US10711201B2 (en) 2014-12-19 2020-07-14 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method for converting algal biomass into a gas or into biocrude by hydrothermal gasification or hydrothermal liquefaction, respectively

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US9328310B1 (en) 2012-07-06 2016-05-03 Arrowhead Center, Inc. Subcritical water extraction of lipids from wet algal biomass
EP3098318A1 (fr) 2015-01-24 2016-11-30 Indian Oil Corporation Limited Procédé à base de thraustochytrides pour le traitement d'effluents usés
CN111232949B (zh) * 2020-02-02 2022-11-25 江苏省农业科学院 一种小球藻水热炭材料的制备方法及其在水稻生产中的应用

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US10711201B2 (en) 2014-12-19 2020-07-14 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method for converting algal biomass into a gas or into biocrude by hydrothermal gasification or hydrothermal liquefaction, respectively
CN107879584A (zh) * 2017-11-14 2018-04-06 东华大学 一种高效削减污泥中抗性基因的方法
CN109020126A (zh) * 2018-07-13 2018-12-18 胜利油田森诺胜利工程有限公司 一种用于含油污泥生物修复的施工工艺

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US20120198758A1 (en) 2012-08-09
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BR112012009461A2 (pt) 2015-09-15

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