WO2015046736A1 - Procédé pour produire directement du biodiesel à haute énergie à partir de biomasse humide - Google Patents

Procédé pour produire directement du biodiesel à haute énergie à partir de biomasse humide Download PDF

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WO2015046736A1
WO2015046736A1 PCT/KR2014/007027 KR2014007027W WO2015046736A1 WO 2015046736 A1 WO2015046736 A1 WO 2015046736A1 KR 2014007027 W KR2014007027 W KR 2014007027W WO 2015046736 A1 WO2015046736 A1 WO 2015046736A1
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Prior art keywords
catalyst
alcohol
biodiesel
biomass
wet biomass
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PCT/KR2014/007027
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English (en)
Korean (ko)
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양지원
박민성
미슈라산쥬
서인상
파루크와싶
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재단법인 탄소순환형 차세대 바이오매스 생산전환 기술연구단
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Publication of WO2015046736A1 publication Critical patent/WO2015046736A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
    • C10L1/026—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only for compression ignition
    • 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
    • Y02E50/10—Biofuels, e.g. bio-diesel
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock

Definitions

  • the present invention relates to a method for the direct production of high energy biodiesel from a wet biomass, and more particularly, the step of pretreatment by adding alcohol to the wet biomass; And adding alcohol and a catalyst to the pretreated biomass, followed by heating to perform transesterification, thereby directly producing biodiesel from the wet biomass without extracting lipids. It is about.
  • biodiesel one of the main forms of alternative energy.
  • Almost all of today's biodiesel is produced from edible crops such as wheat and corn, waste cooking oil and animal fats.
  • these will not serve as alternative energy sources for fossil fuels because of ultimate sustainability issues.
  • Daemon's research paper (Deamon, 2007, Nature, 449: 652-655) and Laurent's research paper (Laurent et al., 2009, Environ. Sci. Technol. 43: 6475-6481)
  • the debate over fuel has been raised and the need for a biomass base that does not hinder food production.
  • the 2011 study paper (D.H.Lee et al., 2011, Biores.Technol. 102: 43-49) raised the issue of the lack of arable land and replacement sites for biomass grown for fuel production.
  • Microalgae are single-cell photosynthetic organisms capable of photosynthetic growth using water, carbon dioxide and sunlight, also called phytoplankton, and are estimated to be present in about 200,000 to 800,000 species worldwide. Microalgae can be cultivated anywhere in the wasteland, the coast, and the sea as long as photosynthesis is possible. The microalgae live in freshwater or seawater, absorb carbon dioxide and release oxygen, and contain useful substances such as oil. . In particular, microalgae accumulate high quality vegetable oils in vivo through photosynthesis, and the amount of oil produced per unit area is 10 times less than conventional edible crops such as soybeans and corn for obtaining biodiesel raw oil. It is about 50-100 times higher on average.
  • the microalgae has the advantage that the growth rate is faster than the land plants, can be grown in high concentration in a large amount, and can grow even in extreme environments. Microalgae show higher fuel productivity compared to conventional crops because the available oil content amounts to 30-70% of the biomass. In addition, since microalgae do not compete with other crops in terms of land or space, the present invention has the advantage of not causing secondary environmental problems such as rising prices of food resources and deforestation.
  • microalgae uses extremely high process costs of dehydration, drying, extraction and processing when microalgae are used for biodiesel production.
  • Microalgae also have polar structures such as monoglycerides (MAGs, monoglycerides), diglycerides (DAGs, diglycerides) and triglycerides (TAGs, triglycerides), and polar structures such as phospholipids and glycolipids. Having lipids, the biochemical composition and amount of such lipids can be altered by harvesting, drying and storage techniques.
  • microalgae are known to consume stored fat through cellular respiration during long-term storage after harvesting, and contain lipases that can break down lipids into free fatty acids, resulting in significant amounts of lipids during storage at room temperature. There is a problem that the amount is lost and the quality is reduced. Thus, for this reason, it is essential that the microalgae's wet biomass be treated as soon as it is available.
  • lipids are first extracted before being converted to fuel.
  • the cell walls of microalgae composed of coarse cellulose must be destroyed.
  • Lipids can then be recovered from the microalgae by physical (cold press, French press, homogenization and cavity methods) and chemical (solvent extraction) methods.
  • Solvent extraction processes for lipids are generally carried out using other combinations of chlorine or neutral solvents such as chloroform, methanol and water, and after extraction, the neutral lipids can be obtained via hexane fractions. Since most individual methods are not sufficient for high recovery of lipids, a combination of these methods is required for effective extraction. However, all of the drying and extraction steps are energy intensive, expensive, use many solvents and require several steps.
  • Korean Patent Publication No. 2013-0037516 discloses an 'integrated non-catalyst continuous biodiesel conversion process without omission of milking and extraction'
  • Korean Patent No. 1264543 discloses 'raw material for biodiesel from microalgae'. Method of extracting and biodiesel production using the same 'is disclosed, but there is no description of the direct production process of high-energy biodiesel from the wet biomass of the present invention.
  • the present invention is derived by the above requirements, the present inventors pre-treatment with alcohol to the microalgae with high moisture content, without additional lipid extraction process, the alcohol and catalyst to the pre-treated microalgae again and heat
  • the present invention was completed by developing a method for producing fatty acid ethyl ester, which is a high-energy biodiesel, by adding a transesterification reaction.
  • It provides a method for producing biodiesel directly from the wet biomass without extracting lipids, comprising the step of adding an alcohol and a catalyst to the pre-treated biomass, followed by heating to perform a transesterification reaction. .
  • the present invention relates to a manufacturing method for producing biodiesel directly from a biomass having a high moisture content, and the method of the present invention can be effectively applied to produce high energy biodiesel without using a separate milking and extraction process using microalgae. Can be.
  • the method of the present invention is more cost-effective than conventional methods because there is no lipid extraction process, and solvents such as chloroform, dichloromethane and carbon tetrachloride for separating lipids are not used, and wastes generated during the process can be reused. As it is an improved process, eco-friendly effects can be expected.
  • 1 is a process chart of the production method for producing biodiesel directly from the microalgae of the present invention.
  • FIG. 2 is a result of comparing the production of biodiesel (FAEE) according to the treatment time of alcohol pretreatment conditions.
  • FAEE biodiesel
  • Figure 3 is a result of comparing the production amount of biodiesel by the number of alcohol pretreatment treatment.
  • Figure 4 is a result of comparing the production of biodiesel according to the alcohol volume ratio to the biomass of alcohol pretreatment conditions.
  • Figure 6 is a result of comparing the biodiesel production by temperature during the transesterification reaction.
  • Figure 10 is the result of confirming the distribution of lipids in algae during the process of the present invention in three types of microalgae Atria, Nannochloropsis and Oranthiochitrium. Lipid in residual biomass; Biomass, alcohol fraction (pretreatment) remaining after conversion; Alcohol recovered after pretreatment of wet biomass, Alcohol fraction (conversion); Alcohol fractions having undergone transesterification using biomass, acid and heat.
  • a method for producing biodiesel directly from the wet biomass without extracting lipids comprising the step of performing a transesterification reaction by heating.
  • the wet biomass is a raw material capable of producing biodiesel as a living microorganism containing lipids, and may be any type of microalgae, yeast, mold, bacteria or microbial slurry, and fresh water.
  • B may be a species of seawater, preferably microalgae, but is not limited thereto.
  • the microorganism may be cultured by a heterotrophic, autotrophic or mixed nutrition.
  • the microalgae may be harvested by centrifugation, flocculation, bio-flocculation, filtration, etc., but are not limited thereto.
  • the microalgae of the present invention is Ettlia, Dunaliella, Chlorella, Nannochloropsis, Golenkinia, Spirulina, Chlamydomonas ( Chlamydomonas, Chroococcus, Chaetoceros, Achnanthes, Amphora species, and the like, preferably Ettlia oleoabundans , Nanocloc Rob cis Salina (Nannochloropsis salin a), nanno claw Rob cis Gardiner appear (Nannochloropsis gaditana), two flying it Ella right Wiltshire (Dunaliella bardawil), two flying it Ella Salina (Dunaliella salina), two flying it Ella Primo rekta (Dunaliella primolecta), chlorella Bulgari ( Chlorella vulgaris ), Chlorella emorsonii , Chlorella minutissima , Chlorella sorokiniana , S
  • the cultured microalgae is 10 to 99% by weight, preferably 60 to 90% by weight, more preferably 80 to 90% by weight when used as a raw material for biodiesel production through the production method of the present invention after harvesting. It may be, but is not limited thereto.
  • the alcohol used in the pretreatment step may have a volume ratio of biomass: alcohol of 1: 0.1 to 100, preferably 1: 1 to 100, more preferably It may be 1: 1 to 10, and most preferably 1:10, but is not limited thereto.
  • the number of pretreatment may be one or more times, preferably 1 to 10 times, but is not limited thereto.
  • the alcohol of step (1) is very hygroscopic and is not limited so long as it may cause dehydration, preferably methanol, ethanol, propanol or butanol, and the like. It may be a lower alcohol, most preferably ethanol, but is not limited thereto.
  • the alcohol may inhibit the lipase that removes excess water in the biomass, lowers the yield of biodiesel, or inhibits the activity of the inhibitor of the transesterification reaction.
  • the alcohol used in the pretreatment may preferably be recycled and used during the process for producing the biodiesel of the present invention, but is not limited thereto.
  • a catalyst of a transesterification reaction is used to produce a biodiesel of fatty acid ester from the pretreated wet biomass, wherein the catalyst is an acid catalyst, a base catalyst, a homogeneous ), A heterogeneous catalyst, an enzyme catalyst or any other catalyst, and the like, and preferably, a solid acid catalyst such as zeolite and heteropoly acid, an inorganic acid catalyst such as hydrofluoric acid, sulfuric acid and phosphoric acid, and a base catalyst such as sodium hydroxide and potassium hydroxide.
  • It may be an ion exchange resin catalyst such as Amberlyst, more preferably an acid catalyst such as sulfuric acid, hydrochloric acid, nitric acid, acetyl chloride, and more preferably sulfuric acid, but is not limited thereto.
  • Amberlyst an ion exchange resin catalyst such as Amberlyst
  • an acid catalyst such as sulfuric acid, hydrochloric acid, nitric acid, acetyl chloride, and more preferably sulfuric acid, but is not limited thereto.
  • alcohol and catalyst may be reused one or more times to increase the biodiesel content in the reaction mixture.
  • the step of the transesterification reaction may be heated for 60 to 150 °C, preferably 80 to 120 °C, and reacted for 5 to 300 minutes at a stirring speed of 10 to 300 rpm
  • the present invention is not limited thereto.
  • the present invention preferably
  • the ponds were cultured by independent, mixed or heterotrophic methods.
  • Dry cell concentration in the culture medium varied from 0.1% to 1.4% (w / v). Cell concentrations were found high in the heterotrophic state and low in the autotrophic state. Cultured cells exhibited high levels of water content both intracellularly and extracellularly. Extracellular water was dehydrated using one of the known methods in microbial production, including but not limited to membrane filtration, centrifugation, precipitation or flotation (floating). Yeast cell Cryptococcus curvatus and Cryptococcus sp. Were grown for 16 hours at 25 ° C. in organic defined medium supplemented with nitrogen and a carbon source. Since the harvested biomass shows various changes in the intracellular contents of water and lipids, the harvested biomass was stored at -80 ° C until used in the process.
  • lipid content of the dry biomass was analyzed through the following steps: Approximately 10 mg of dry algal cells were mixed with 2 ml of a 2: 1 chloroform: methanol solution and capped with a Teflon capped Pyrex tube The lipid was extracted by stirring for 10 minutes at.
  • the microbial biomass After harvesting, the microbial biomass naturally contains between about 60 and 90% moisture.
  • Wet biomass of microalgae has many inhibitors that inhibit the transesterification process during biodiesel manufacturing. Therefore, in this process, we washed the wet biomass using a microbiologically synthesized solvent to inactivate inhibitors such as water or enzymes.
  • Wet biomass was mixed with a microbiologically synthesized solvent at a rate of 1: 1-10 at a speed of 300 rpm in a vibrating machine. Solvents serve to stop the activity of enzymes that can degrade lipids and remove excess water that interferes with the process of biodiesel production.
  • the solvent is then separated from the biomass through known separation methods such as centrifugation, filtration and precipitation.
  • Microalgae cells were pretreated due to the fact that intracellular lipids were sequestered after thick cellulose structures.
  • Microalgal strains of Atria with relatively thick cell walls were cultured and microalgae were harvested by centrifugation. The moisture content of the harvested microalgal samples was in the range of 80-90%.
  • the conditions for direct in situ transesterification (conversion) from triglycerides (TAG) to fatty acid ethyl esters (FAEE) were optimized.
  • TAG triglycerides
  • FEE fatty acid ethyl esters
  • wet biomass samples were obtained from a 200 m 3 open pond, an outdoor mass culture facility.
  • the microalgae used are Nannochloropsis oceanica , a seawater aquaculture system, which has a relatively high lipid content.
  • the moisture content of the wet biomass sample was found to be in the range of 65-70%.
  • reaction temperature on conversion was checked to find the optimal conditions for transesterification reaction. It is hypothesized that higher reaction temperatures will bring higher conversion yields, and are expected to be even more energy integrated, especially above 100 ° C.
  • the transesterification reaction was performed using a wet biomass for 2 hours at a temperature section between 60 ⁇ 120 °C. As a result, 8.14 mg of fatty acid ethyl ester was produced at a temperature of 60 ° C., and 10.76 mg of biodiesel was produced at a temperature of 120 ° C., confirming an increase of about 32% (FIG. 6). However, especially after the reaction temperature was increased to 100 ° C. or more, no increase was observed as much as the conversion period experiment conducted in Example 5. This suggests the possibility of achieving high yields at low conversion temperatures while other conditions are being optimized.
  • heterogeneous catalyst Amberlyst-15 (surface area 50 m 2 / g) was used as a catalyst for the direct transesterification of Ettlia sp. Biomass instead of sulfuric acid.
  • the conversion time was 2 hours and compared with the amount of fatty acid ethyl ester of the reaction via sulfuric acid catalyst.
  • the conversion yield of the sulfuric acid catalyst was not reached, but it was confirmed that the conversion yield increased as the amount of use thereof increased (FIG. 8).
  • the biodiesel production yield was improved as in the case of Example 5 described above (FIG. 9).
  • Nannochloropsis some biomass extracts large amounts of these lipids during pretreatment. These extracted lipids in the pretreated alcohol fraction are collected and subsequently subjected to transesterification.
  • Biodiesel was produced using methanol and butanol, lower alcohols than ethanol.
  • the production method uses microalgae of Ettlia sp., which has about 75% water content, as biomass, and performs pretreatment once for 10 minutes with a biomass: alcohol volume ratio of 1:10.
  • 100 ⁇ l of sulfuric acid was used as a catalyst and transesterification was carried out at 120 ° C. for 2 hours.
  • the resulting biodiesel was analyzed for fatty acid composition using gas chromatography.
  • biodiesel could be produced in all cases using methanol, ethanol and butanol, and the yield was confirmed to be similar.
  • FEE fatty acid ethyl ester
  • Ethanol mixtures mixed with fatty acid ethyl esters (FAEE) produced from the completed reactions according to the biodiesel production process of the present invention were used in the conversion reaction for biodiesel production of the next batch of microalgal biomass.
  • 200 ml of Gorenkinia wet type biomass (74.9% water content) was treated with 2 ml of fresh ethanol as a pretreatment for dehydration, and transesterified with recycled ethanol and sulfuric acid or fresh ethanol and sulfuric acid.
  • Sulfuric acid was treated at various concentrations from 0 to 200 ⁇ l to confirm the reusability of the acid catalyst.

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Liquid Carbonaceous Fuels (AREA)
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Abstract

La présente invention concerne un procédé pour produire directement du biodiesel à partir de biomasse humide en effectuant un prétraitement à l'alcool et en appliquant de l'alcool, un catalyseur et de la chaleur à la biomasse prétraitée, sans procédé d'extraction de lipides séparé. Le procédé selon la présente invention est plus économique que les procédés existants car il n'emploie pas de procédé de séparation des lipides, et améliore les procédés de telle sorte que les déchets produits pendant le processus de traitement peuvent être recyclés, et que l'on peut donc espérer un effet de respect de l'environnement.
PCT/KR2014/007027 2013-09-25 2014-07-31 Procédé pour produire directement du biodiesel à haute énergie à partir de biomasse humide WO2015046736A1 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107099314A (zh) * 2017-06-27 2017-08-29 华中科技大学 一种利用农林废弃物制备长链脂肪酸和掺氮碳的方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110054200A1 (en) * 2009-09-01 2011-03-03 Catilin, Inc. Systems and Processes for Biodiesel Production
US20120065416A1 (en) * 2010-09-15 2012-03-15 Utah State University Methods for Production of Biodiesel
KR20130037516A (ko) * 2011-10-06 2013-04-16 재단법인 포항산업과학연구원 착유/추출과정을 생략한 통합형 무촉매 연속식 바이오디젤 전환 공정
KR20130094182A (ko) * 2010-04-06 2013-08-23 헬리아에 디벨롭먼트, 엘엘씨 바이오연료를 제조하기 위한 방법 및 시스템
US20130236938A1 (en) * 2012-02-16 2013-09-12 Smartflow Technologies, Inc. Biodiesel fuel production, separation methods and systems

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110054200A1 (en) * 2009-09-01 2011-03-03 Catilin, Inc. Systems and Processes for Biodiesel Production
KR20130094182A (ko) * 2010-04-06 2013-08-23 헬리아에 디벨롭먼트, 엘엘씨 바이오연료를 제조하기 위한 방법 및 시스템
US20120065416A1 (en) * 2010-09-15 2012-03-15 Utah State University Methods for Production of Biodiesel
KR20130037516A (ko) * 2011-10-06 2013-04-16 재단법인 포항산업과학연구원 착유/추출과정을 생략한 통합형 무촉매 연속식 바이오디젤 전환 공정
US20130236938A1 (en) * 2012-02-16 2013-09-12 Smartflow Technologies, Inc. Biodiesel fuel production, separation methods and systems

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107099314A (zh) * 2017-06-27 2017-08-29 华中科技大学 一种利用农林废弃物制备长链脂肪酸和掺氮碳的方法

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