KR101763064B1 - Method of preparing oil and sugar from spent coffee ground - Google Patents
Method of preparing oil and sugar from spent coffee ground Download PDFInfo
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- KR101763064B1 KR101763064B1 KR1020160033159A KR20160033159A KR101763064B1 KR 101763064 B1 KR101763064 B1 KR 101763064B1 KR 1020160033159 A KR1020160033159 A KR 1020160033159A KR 20160033159 A KR20160033159 A KR 20160033159A KR 101763064 B1 KR101763064 B1 KR 101763064B1
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- 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
- C12P19/00—Preparation of compounds containing saccharide radicals
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
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- 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
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/02—Monosaccharides
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- 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
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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- 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
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/16—Preparation of compounds containing saccharide radicals produced by the action of an alpha-1, 6-glucosidase, e.g. amylose, debranched amylopectin
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- 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
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/20—Preparation of compounds containing saccharide radicals produced by the action of an exo-1,4 alpha-glucosidase, e.g. dextrose
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- 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
Abstract
A method for producing oil and sugar from coffee grounds with high efficiency, comprising the steps of: adding an alkaline solution to the coffee grounds; Separating the liquid phase and the solid phase by administering a non-polar solvent to the coffee grounds; Recovering the nonpolar solvent in the separated liquid phase and separating the solvent and the oil; And a step of administering a hydrolase to the solid to produce a sugar.
Description
The present invention relates to a method for producing a sugar available for bio-refinery by hydrolyzing glucan and galactomannan contained in coffee grounds with enzymes, a method for removing hydrolysis-inhibiting substances by a thermochemical treatment method, And simultaneously extracting the oil.
Biorefinery research, which produces biomaterials and fuels based on biomass raw materials, is drawing attention as an environmentally friendly production technology of the future. Refineries based on existing fossil raw materials have problems such as limitation of petroleum resources and induction of environmental pollutants, while bio-refineries have no problem of exhaustion of resources and are environment-friendly processes.
Currently, biomass, which is mainly used in the bio-refinery process, is a food resource such as potatoes, corn, sweet potatoes, sugar cane, and edible oil, which causes social problems such as rising international food and feed prices and local starvation. Therefore, biomass should be sought not to be confronted with human food problems, and researches utilizing resources such as agricultural by-products, microalgae, and organic wastes that can replace them are underway all over the world.
Second generation woody biomass, which is a typical non-biodegradable biomass, has complicated components such as cellulose, hemicellulose, and lignin, so it is necessary to apply conversion technology suited to the raw material characteristics to increase production efficiency.
Coffee residue is an organic biomass that is different from second-generation biomass because of the carbohydrates, crude fat, crude fiber, crude protein, and ash content, including glucan and galactomannan. However, Can be improved. In the case of crude fat in the coffee grounds, it can be used as a raw material for production of biodiesel after extracting the oil by heat-chemical treatment. In the case of carbohydrate and crude fiber, it can be converted into reducing sugar such as glucose and galactose mannose which are monomers. Sugar is a carbon nutrient source essential for microbial cell growth such as yeast, and includes monosaccharides such as glucose (glucose), galactose, mannose, xylose and arabinose, and disaccharides such as sucrose, lactose and maltose, The process of producing a specific substance using biomass is included in bio-refinery.
According to the Korea Customs Service (KCS), in 2014, Korea imported about 140,000 tons of coffee, with imports steadily increasing (14.8% more than in 2013), and the amount of coffee grounds estimated to be similar. At present, coffee grounds are limited to be used as fragrance or compost, so they are distributed free of charge in coffee shops or are mostly disposed of.
On the other hand, Korean Patent Registration No. KR 10-1427179 describes a method for producing a fermentable sugar from herbal medicines residue, but the ingredients of the herbal medicine and the coffee are totally different, making it difficult to apply the content of the above patent to coffee.
Accordingly, the present inventors have completed the present invention by demonstrating bio-refineries that produce sugar with high efficiency at the same time as extracting oil from coffee grounds, converting it into a high-value substance by applying it to a microbial fermentation process.
Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made in view of the above problems, and it is an object of the present invention to provide a method for converting a waste coffee residue into a high value-added substance.
The present invention provides a method for producing oil and sugar from coffee grounds with high efficiency, comprising the steps of: adding an alkali solution to a coffee ground; Separating the liquid phase and the solid phase by administering a non-polar solvent to the coffee grounds; Recovering the nonpolar solvent in the separated liquid phase and separating the solvent and the oil; And administering a hydrolase to the solid to produce a sugar.
Generally, the amount of oil contained in the coffee grounds is about 10 to 15%, and the available carbohydrate is 20 to 30%. When introducing the high temperature alkali treatment method proposed in the present invention, oil extraction is possible quickly (within 1 hour). In addition, it was confirmed that the conversion yield of the coffee residue was improved during the enzymatic hydrolysis.
The present invention can contribute to solving environmental problems in terms of utilization of existing waste materials because it can expect new profit by converting coffee waste, which is mainly used, to a high value-added material with limited use.
Figure 1 is a flow chart outlining the overall flow of the present invention.
Figs. 2A and 2B are graphs showing constituents of a coffee bean having a general coffee bean, coffee grounds and alkali treated. Fig.
Figure 3 shows the production of a new beta mannanase from Streptomyces sp. CS147, and the two newly produced mannose hydrolysis enzymes and the two mannan hydrolysates on the market under the same conditions It is the result of evaluating the hydrolysis efficiency of LBG and coffee scraps.
FIG. 4 shows the results of ethanol content analysis using the sugar prepared according to the present invention.
FIG. 5 is a graph showing the production results of oil and sugar from coffee grounds according to the present invention using newly encountered hydrolytic enzymes. FIG.
The present invention relates to a technology for converting coffee waste, which is mainly used as general waste, into oil and sugar because utilization of fragrance, compost, etc. is low. The main components of the residue from coffee beans were 10-15% of glucan, 30-35% of galactomannan, 15-20% of crude fat, 5-10% of crude fiber, 10-15% of crude protein, 5-30%, and the hydrolysis of glucan and galactomannan with enzymes produces monosaccharides (glucose, mannose, galactose) that can be used for microbial fermentation. Accordingly, in the present invention, in order to improve enzyme hydrolysis efficiency, coffee residue was treated with an alkaline chemical and an oil component was extracted. As a result, an improved sugar conversion efficiency was confirmed. It was confirmed that ethanol was produced after using the saccharified liquid as a nutrient source of a typical ethanol fermenting microorganism Saccharomyces, and this shows that it can be utilized for microbial fermentation. Korea imports about 140,000 tons of coffee (based on the Korea Customs Service in 2014) and estimates that coffee waste will be similar. It is expected that new waste can be expected by converting mainly scrapped waste into available resources and at the same time it can help solve environmental problems in terms of waste resources.
The present inventors have experimentally confirmed that the recovery rate of oil and sugar is maximized when the alkaline solution is added to the coffee grounds for pretreatment, thereby completing the present invention.
A method for producing oil and sugar from coffee grounds with high efficiency, comprising the steps of: adding an alkaline solution to the coffee grounds; Separating the liquid phase and the solid phase by administering a non-polar solvent to the coffee grounds; Recovering the nonpolar solvent in the separated liquid phase and separating the solvent and the oil; And administering a hydrolase to the solid to produce a sugar.
Specifically, the present invention provides a process for producing a coffee beverage comprising: a) drying a coffee ground; b) adding an alkaline solution to the dried coffee grounds; c) maintaining the coffee grounds to which the alkali solution has been added at a temperature of 100 to 150 캜; d) separating the liquid phase and the solid phase by administering a non-polar solvent to the coffee grounds; e) recovering the nonpolar solvent in the separated liquid phase and separating the solvent and the oil; f) washing and neutralizing the separated solid coffee grounds; And g) adding a hydrolase to the coffee grounds after the neutralization step to produce a sugar. One or more of steps a) through g) above may be omitted or changed. FIG. 1 is a flow chart showing the process for producing an oil and a sugar of the present invention.
Hereinafter, steps a) to g) will be described.
a) drying the coffee grounds
In this step, the coffee grounds can be dried in a drying oven at 40 to 60 ° C for 1 to 5 days to remove moisture.
The effect of using the recovered coffee grounds directly in the heat-alkali treatment process without removing moisture is not so different from that of the dried coffee grounds, but molds can easily occur during storage of the collected coffee grounds. This can affect the quality of raw materials when used in larger scale processes. That is, the constituent components may be changed.
b) adding an alkali solution to the dried coffee grounds
This step is a pre-stage for thermo-chemically treating dried coffee grounds to maintain storage quality. The alkali solution may be sodium hydroxide (NaOH), potassium hydroxide (KOH), ammonia (NH 3 ), or the like.
It is preferable that the alkali solution is used at a concentration of 0.5 to 30 wt%, specifically 0.5 to 10 wt% in the case of sodium hydroxide and potassium hydroxide, and 10 to 30 wt% in the case of ammonia desirable.
The ratio of the coffee grounds to the alkali solution is preferably 1:10 to 1:30 by weight and sufficiently mixed for the next high temperature and high pressure reaction.
c) maintaining the coffee residue added with the alkali solution at a high temperature
The reaction temperature of the coffee grounds and the alkali solution is in the range of 100 to 150 ° C, and a device such as a high-pressure sterilizer may be used. The reaction time varies depending on the temperature, and the reaction temperature is preferably 20 to 40 minutes based on 121 占 폚. When the temperature is in the range of 150 ° C, it is recommended that the reaction time should be 10 minutes or less, and it is confirmed that coffee residue is over-decomposed or carbonized at a higher temperature to cause a large weight loss. It is also recommended to treat the reaction time in the range of 40 to 120 minutes when the reaction temperature is in the range of 100 ° C, and it is confirmed that the yield is decreased when the reaction time is long.
d) The non-polar solvent is applied to the coffee grounds, Solid phase Separating step
After the high-temperature high-pressure reaction is completed, the internal temperature of the reactor is cooled to about 30 to 50 ° C. The nonpolar solvent is mixed to extract the oil from the coffee grounds in the reactor. The nonpolar solvent may be heptane, hexane, or the like, and it is preferable to add 100 to 400% of the total amount of the coffee grounds. And then stirred at a temperature of 30 to 50 ° C for 30 to 120 minutes at a rate of 150 to 350 rpm. If the agitation is continued for a longer period of time, further reaction with the alkali solvent is continued and the solid recovery yield is lowered. Use a sieve of 100-120 sieve (inner diameter 0.152-0.125 mm) to separate the liquid and solid phases, and transfer the liquid phase to a separating funnel.
e) recovering the nonpolar solvent in the separated liquid phase and separating the solvent and the oil
After precipitation for at least 2 hours, the lower water layer is removed and the upper nonpolar solvent layer is recovered. In this case, since it is difficult to distinguish due to the inherent black color of coffee, the amount of water that has been removed is added again (three-hand method) and then precipitated for more than 2 hours to recover the non-polar solvent layer. Since the recovered nonpolar solvent contains the coffee residue-derived oil, the solvent and the oil can be easily separated using a vacuum distillation apparatus. The recovered nonpolar solvent can then be reused for subsequent oil extraction.
f) washing and neutralizing the separated solid-phase coffee grounds
The solid coffee grounds separated in the above step are neutralized. The neutralization method is a method of washing the chemically treated coffee grounds with distilled water or tap water to remove the solvent by filtering the coffee grounds through the sieve. The amount of water to be used is sufficiently neutralized by 2 to 10 times the total volume of the solvent depending on the concentration and the volume of the solvent used in the reaction.
g) Step of producing sugar by administering hydrolytic enzyme to the coffee grounds after the neutralization step
Enzymatic saccharification, after chemical pretreatment, involves adding hydrolytic enzymes to neutralized coffee grounds to produce sugars decomposed with monosaccharides. The hydrolytic enzyme used in this case is preferably one selected from the group consisting of cellulase, beta glucosidase, amylase, zeira, and mannanase. In particular, the above mannanase may be a β-mannanase in Streptomyces sp. CS147.
The pretreated coffee grounds are added so as to have a concentration of 10 to 50 g / L, and the optimum amount of the enzyme in the reaction solution is 5 to 10 FPU (Filter Paper Unit), β-glucosidase (cellulase) 1 to 5 CBU (Cellobiase Unit). For amylase, it should be 10 to 20 CU (Ceralpha Unit). For xylanase, it should be 50 to 100 units. And 100 to 500 units for mannanase.
The appropriate reaction temperature after enzyme administration is 40 ~ 60, and the reaction time is 2 ~ 7 days.
The sugar produced by the present invention can be used as a substrate (carbon source) of K35 (Saccharomyces cerevisiae K35), an ethanol producing strain, to confirm microbial fermentation from the sugar.
Hereinafter, the present invention will be described in more detail with reference to Examples and Experimental Examples. These Examples and Experiments are only for illustrating the present invention, and thus the scope of the present invention is not construed as being limited by these Examples and Experimental Examples. Hereinafter, the present invention will be described in more detail with reference to the following experimental examples. However, these are only for illustrating the present invention, and the scope of the present invention is not limited by these examples.
Reference Example 1. Analysis of constituents of coffee grounds
The contents of the components were analyzed in the following manner with respect to coffee beans, coffee grounds, and coffee grounds treated with alkali according to the method of the above embodiment.
( 1) Content analysis of glucan , galactan , mannan , and arabinan
Determination of Structural Carbohydrates and Lignin in Biomass / 2010 edition of the Laboratory Analytical Procedure Technical Report (NREL / TP-510-42618) developed and published by NREL The experiment was performed with reference to FIG.
To summarize the test methods, 0.3 g of each of 5 kinds of standard samples (glucose, xylose, galactose, arabinose, mannose) and the samples to be analyzed were put into a 10 mL glass test tube, and 3 mL of 72% sulfuric acid was added. Leave in a constant-temperature water bath for 2 hours. Transfer the sample to a thermostatted glass bottle with a 250 mL volume and dilute with 84 mL of distilled water. The glass bottle is placed in a sterilizer and reacted at 121 ° C for 1 hour. After the reaction, the liquid phase was neutralized with calcium carbonate to adjust the pH to about 6 to 7, and the supernatant was analyzed under the following conditions.
Analysis of the hydrolyzed monosaccharides was carried out using high performance liquid chromatography (HPLC) equipped with a Refractive Index Detector (RID-10A, Shimadzu, Japan). The columns were Aminex HPX-87P (300 X 7.8 mm, Bio-Rad Laboratories, Japan). At this time, the temperature of the column was 80 ° C, the mobile phase was of the third distilled water, and the flow rate was 1.0 mL / min. Experimental results are shown in Figs. 2A and 2B and Table 1.
(2) Analysis of crude fat, crude protein,
Crude fat: Soxhlet extraction method (using 1043 Soxtec System HT, Japan)
After weighing 1 g of sample in a cylindrical filter paper, place the ether in the fat extraction container and attach it to the Soxtec instrument. After the fat is extracted for a certain period of time, the cylindrical filter paper is taken out, the fat extraction container is taken out, and the remaining ether is evaporated. Determine the amount of fat extracted by measuring the weight of the fat extraction container.
Crude protein: Kjeldahl method using FOSS 8100 system, Japan
Take sample in test tube, add decomposition promoter (K2SO4), add sulfuric acid and decompose for 2 hours at 420 ℃ decomposition apparatus. The dissolution liquid is placed in a distillation apparatus, and the system is distilled for 5 minutes and titrated with 0.1N hydrochloric acid. Multiply the appropriate value by 6.25 (nitrogen correction factor) and check the crude protein value.
Inquiry minutes: direct conversation method
Cool the crucible and weigh it.
Take 1 g of sample, weigh it, and preliminarily carbonize it.
Put in a painting (Korean science, Korea) and let it be at 600 degrees for 3 hours or more.
After cooling, measure the weight and weigh the remaining amount.
The above method is based on the standard analysis method presented in the Korean Food Standards Codex of the Korea Food and Drug Administration.
Figs. 2A and 2B are graphs showing constituents of a coffee bean having a general coffee bean, coffee grounds and alkali treated. Fig.
(Table 1)
As a result of the experiment, it was found that there was no overall composition change in the coffee grounds compared with the coffee beans. On the other hand, alkaline treatment did not affect carbohydrates (glucan, galactan, mannan, arabinan), but decreased 3.8 times in crude fat and 4.1 times in crude protein. Thus, the present alkaline treatment resulted in a very effective removal of the unnecessary components while preserving the sugar-convertible carbohydrate in the solid phase.
Reference Example 2. Evaluation of sugar conversion by enzyme treatment without alkali pretreatment
After producing a new β-mannanase from Streptomyces sp. CS147, two newly produced mannanase and two mannan hydrolysates on sale were treated with the standard LBG The hydrolysis efficiency of the coffee scraps was evaluated. In the experiment, a 10 mL aqueous solution was set as the reaction scale. After adding 30 units of each hydrolytic enzyme, the substrate (0.5% LBG for the standard material, 3% for the coffee grounds, The content of this figure in the coffee grounds equals the metered content of the reference material). The manose and reducing sugars produced after stirring at 50 rpm for 48 hours at 200 rpm were analyzed and shown in FIG.
The mannan hydrolase newly produced by the present inventor was denoted Mn147 at the bottom of the figure, E-BMABS as the mannase-derived hydrolyzing enzyme derived from Bacillus sp. Strain, and E-BMANN as the hydrolytic enzyme derived from Aspergillus niger strain . Two commercially available commercial enzymes were purchased from Megazyme (Chicago, USA). As a result, the ability of Mn147, a newly produced mannitolase, to decompose LBG (reducing agent) into reducing sugar was 75%, which is superior to E-BMANN (90%) or E-BMABS (60%) Respectively. Experiments to convert coffee residue to sugar showed that the conversion efficiency of all three kinds of hydrolytic enzymes was as low as 20%. This suggests that the accessibility of the enzyme-substrate reaction is reduced due to other impurities contained in the coffee grounds. Therefore, a pretreatment method for removing impurities is required to improve the conversion ratio.
Reference Example 3. Assessment of physical property change by alkali treatment
As a result of analyzing the components of the carbohydrate present in the solid phase after the alkali treatment of the present invention, the conversion efficiency after hydrolysis using the enzyme, and finally the result of calculating the mass balance based on the data are shown in Table 2.
(Table 2)
The solvent used was KOH, NaOH, and NH 3 , and the reaction was carried out under the same conditions (121 ° C for 30 min) at each concentration. The solid loss, the carbohydrate components (glucan, MG : mannan + galactan) was analyzed first. It was confirmed that the solid loss and the carbohydrate area which are preserved differ depending on the kind and concentration of the alkali solvent. In the case of KOH, the higher the concentration, the lower the solid loss, but the higher the carbohydrate decomposition rate. In the case of NaOH, the solid loss was proportional to the concentration, but the carbohydrate storage ratio was relatively high. In the case of NH 3 , about 50% of the solid loss occurred from 10 to 20% concentration, but the solid loss was reduced at the high concentration (25%). However, it can be seen that the chemical selectivity increases toward the carbohydrate at a high concentration. Therefore, the enzyme conversion efficiency should be evaluated together to select the desired alkali type and concentration. The results of the enzyme conversion were expressed as RS (Reducing sugars, reducing sugar) in the above table. Hereinafter, glucose and mannose are the results of analysis of each of the sugar equivalents present in the reducing sugar. In the present invention, the total reducing sugar amount is used as a standard. After the treatment with KOH, the enzyme conversion increased about 2 to 3 times, the NaOH increased 1.7 times and the NH 3 increased 1.4 times. Therefore, the mass balance was calculated by combining the solid recovery amount, the amount of carbohydrate present, and the conversion efficiency of reducing sugar. As a result, since the unprocessed coffee grounds showed a value of 9.8%, a treatment method showing a value lower than that was not preferable. The NaOH solvent reacted under these conditions showed undesirable results, and NH 3 gave the desired results at 5% and 25% concentrations. Overall, the most desirable solvent was KOH and the concentration range was 7%. However, at 3% concentration, the mass balance is 15.7%, approaching 93% of the 7% KOH mass balance. Considering the entire process, it may be desirable to add less than 3% of solvent, since high concentration solvent input has a direct effect on cost increase.
Example 1. Production of oils and sugars from coffee grounds
Oils and sugars were produced according to the method of the present invention. Specifically, the collected coffee grounds containing the constituents of the coffee grounds were dried in an oven at 50 캜 for 3 days or more to remove moisture.
1, 3, 5, 7, 10 wt% ammonia (NH3) 5, 10, 15, 20 25 wt% sodium hydroxide (NaOH) Was mixed with the dried coffee grounds. The ratio of the coffee grounds to the alkali solvent was 1:10 by weight and sufficiently mixed for high temperature and high pressure reaction.
The reaction temperature between the coffee grounds and the alkali solvent was 121 ° C, and a high-pressure sterilizer was used, and the reaction time was 30 minutes.
After the high-temperature high-pressure reaction is completed, the internal temperature of the reactor is cooled to about 30 to 50 ° C. To extract the oil from the coffee grounds in the reactor, the nonpolar solvent heptanes or hexane is added twice the weight of the total weight of the reacted coffee. Thereafter, the mixture was stirred at 40 rpm for 1 hour at 200 rpm. To separate the liquid and solid phases, a sieve of 100-120 sieve (inner diameter 0.152-0.125 mm) was used, and the liquid phase was transferred to a separating funnel.
After at least 2 hours of precipitation until the water and nonpolar solvent were sufficiently separated, the lower water layer was removed and the upper nonpolar solvent layer was recovered. At this time, due to the inherent black color of the coffee grounds, it is difficult to distinguish the water, so the amount of water removed was added again (three-hand method) and then precipitated again to recover the non-polar solvent layer.
The solid coffee grounds separated from the above were neutralized. The neutralization method is a method of washing the chemically treated coffee grounds with distilled water or tap water to remove the solvent by filtering the coffee grounds through the sieve. The amount of water to be used is sufficiently neutralized by about 3 times the total volume of the solvent depending on the solvent concentration and the volume of the solvent used in the reaction.
Enzymatic saccharification was performed by adding hydrolytic enzyme complex to 30 g / L neutralized coffee grounds after chemical pretreatment. The enzymes used were cellulase 60 FPU / g-glucan, β-
Experimental Example 1. Analysis of ethanol content using the sugar prepared according to the present invention
The sugar produced from the coffee grounds of the present invention prepared according to the above examples was used as a carbon source of Sacharomyces cerevisiae K35, an ethanol producing strain, and its efficiency was analyzed by the following method.
The ethanol content was determined by high performance liquid chromatography (HPLC) equipped with a Refractive Index Detector (RID-10A, Shimadzu, Japan). Columns were Aminex HPX-87H (300 x 7.8 mm, Bio-Rad Laboratories, USA) was used. At this time, the temperature of the column was 50 ° C, the mobile phase was 5N H 2 SO 4 , and the flow rate was 0.8 mL / min. The experimental results are shown in Fig.
Experimental Example 2. New Meta hydrolysis Production of oils and sugars from coffee grounds according to the invention using enzymes
Hydrolysis experiments of locust bean gum (LBG) and spent coffee ground (SCG) using newly encountered hydrolytic enzymes were performed as follows. That is, a new β-mannanase was produced from Streptomyces sp. CS147, which was used for the biochemical characterization of the enzyme and the sugar conversion from the coffee grounds.
Add 0.5% of LBG as a standard substance to 30 units of newly produced hydrolysis enzyme solution and start the reaction at 50 ° C. The resulting hydrolyzate was analyzed by thin layer chromatography and the results are shown in FIG. At the bottom of the picture, Mr is a marker (marker) indicating Mn1 (mannose), Mn2 (mannobiose), Mn3 (mannotriose) indicator material. As a result of the experiment, it is confirmed that LBG, which is a meta-type standard substance generated according to time, gradually changes to the equivalent form of mannose.
Claims (6)
a) drying the coffee grounds;
b) adding an alkaline solution to the dried coffee grounds;
c) maintaining the coffee grounds to which the alkali solution has been added at a temperature of 100 to 150 캜;
d) separating the liquid phase and the solid phase by applying a non-polar solvent to the coffee ground at a temperature of 30 to 50 ° C in an amount of 100 to 400% by weight based on the total coffee grounds;
e) recovering the nonpolar solvent in the separated liquid phase and separating the solvent and the oil;
f) washing and neutralizing the separated solid coffee grounds; And
g) adding a hydrolytic enzyme to the coffee grounds after the neutralization step to produce a sugar,
Wherein the apolar solvent is heptane or hexane and the hydrolytic enzyme comprises a cellulase, beta-glucosidase, and beta-mannanase.
The alkaline solution is at least one of sodium hydroxide (NaOH), potassium hydroxide (KOH), and ammonia (NH 3), method.
And the alkali solution is 0.5 to 30 wt%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200006765A (en) | 2018-07-11 | 2020-01-21 | 전남대학교산학협력단 | Pretreatment method of coffee grounds, and producing method of functional biosugar from polysaccharides derived from pretreated coffee grounds |
| KR20200026870A (en) | 2020-03-05 | 2020-03-11 | 전남대학교산학협력단 | Polysaccharides derived from pretreated coffee grounds obtained by pretreatment method of the coffee grounds |
| KR20210069970A (en) * | 2019-12-04 | 2021-06-14 | 유한회사 축산냄새연구소 | Composition for reducing odor of livestock manure comprising coffee ground extract |
| KR20210102514A (en) | 2020-02-10 | 2021-08-20 | 부산대학교 산학협력단 | Manufacturing method for xylose using coffee grounds |
| KR20230171667A (en) | 2022-06-14 | 2023-12-21 | 전남대학교산학협력단 | An integrated process for conversion of spent coffee grounds into value-added biochemicals and biofuel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007217466A (en) * | 2006-02-14 | 2007-08-30 | Ucc Ueshima Coffee Co Ltd | Method for producing polysaccharide from coffee bean and/or coffee extraction residue |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200006765A (en) | 2018-07-11 | 2020-01-21 | 전남대학교산학협력단 | Pretreatment method of coffee grounds, and producing method of functional biosugar from polysaccharides derived from pretreated coffee grounds |
| KR20210069970A (en) * | 2019-12-04 | 2021-06-14 | 유한회사 축산냄새연구소 | Composition for reducing odor of livestock manure comprising coffee ground extract |
| KR102330177B1 (en) | 2019-12-04 | 2021-11-23 | 유한회사 축산냄새연구소 | Composition for reducing odor of livestock manure comprising coffee ground extract |
| KR20210102514A (en) | 2020-02-10 | 2021-08-20 | 부산대학교 산학협력단 | Manufacturing method for xylose using coffee grounds |
| KR20200026870A (en) | 2020-03-05 | 2020-03-11 | 전남대학교산학협력단 | Polysaccharides derived from pretreated coffee grounds obtained by pretreatment method of the coffee grounds |
| KR20230171667A (en) | 2022-06-14 | 2023-12-21 | 전남대학교산학협력단 | An integrated process for conversion of spent coffee grounds into value-added biochemicals and biofuel |
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