KR20110077722A - Effective extracts from coffee remnants and method for manufacturing the same - Google Patents

Abstract

PURPOSE: A method for manufacturing effective extracts using coffee remnants is provided to prepare bio oil and active ingredients such as antioxidant materials, and to reuse coffee remnants discarded as food waste. CONSTITUTION: A method for manufacturing effective extracts using coffee remnants comprises the steps of: (110) mixing coffee remnants with alcohol, filtering the mixture, and extracting a biomass from which alcohol extracts are removed; (120) mixing hexane with the biomass, filtering the mixture, removing solid components, and extracting crude bio oil; (130) reacting the crude bio oil with an acidic solvent to separate an aqueous solution layer and a crude bio oil layer; and (140) removing free fatty acids from the crude bio oil layer using a basic solvent to extract bio oil.

Description

Effective extracts from coffee remnants and method for manufacturing the same}

The present invention relates to an oil-soluble extract using coffee grounds, and more particularly, to a method for producing oil-soluble extract, which can be a functional cosmetic material or a pharmaceutical material, together with bio oil, which is a raw material of biodiesel, using coffee grounds. It is about.

There is research showing that coffee grounds contain many surprisingly healthy ingredients. Dr. Astridnell League of France, who specializes in the association between coffee and health, says many misconceptions, such as coffee being bad for heart health and damaging the digestive tract, have been the only stimulants of coffee for the past two centuries. It's because it's concentrated on caffeine. Astridnell League research shows that coffee contains powerful antioxidants, chlorogenic acid and melanoids, which neutralize free radicals that damage DNA (Deoxyribonucleic Acid), a harmful oxygen molecule that is produced as a by-product of our body's metabolism. Let's do it. In addition, coffee reduces the risk of cirrhosis, prevents Parkinson's disease, and can reduce the risk of type 2 (adult) diabetes by 50%. Coffee is said to be better than fruits and vegetables, especially in preventing the oxidation of DNA, which causes serious diseases such as cancer. However, there are few studies showing that coffee is carcinogenic, which suggests that coffee contains about 30 potential carcinogens.

Despite these concerns about coffee, its inherent taste and aroma have made coffee one of the most sought after beverages that people like to eat. As a result, coffee consumption continues to increase in our country and around the world. In line with this, not only the production of coffee is increasing, but also the amount of coffee grounds produced after the production of coffee is also increasing every year.

By the way, coffee residues, a by-product of making coffee, are mostly thrown away as garbage. Some people use coffee grounds as deodorant, but only for personal consumption. Coffee grounds contain many useful ingredients in addition to the caffeine component and the like contained in the coffee, an effort is being made to produce a functional material by extracting it. For example, various studies are being conducted to prepare alternative energy sources, dietary supplements, and raw medicines using coffee grounds.

One problem to be solved by the present invention is to remove the toxic substances contained in the coffee grounds and extract only useful ingredients to produce useful extracts (raw materials such as pharmaceuticals or cosmetics) showing antioxidant, whitening and anti-inflammatory effects To provide a way.

Another object of the present invention is to provide a method for producing biodiesel from coffee grounds as a raw material for producing biodiesel.

Method for producing an oil-soluble extract using coffee grounds according to an embodiment of the present invention for solving the above problems is the step of extracting the biomass (biomass) from which the alcohol extract is removed by mixing and stirring the coffee grounds and alcohol In addition, hexane is mixed with the biomass, stirred, and filtered to remove solid components to extract crude bio-oil. The crude bio-oil is reacted with an acidic solvent to form an aqueous solution layer and an unrefined bio. Separating into an oil layer, and removing the free fatty acid from the crude bio-oil layer using a basic solvent to extract the bio-oil.

According to an aspect of the embodiment, the step of esterifying the bio-oil using an alcohol under an acid catalyst, followed by extracting deoxidized bio-oil, a transesterification of the deoxidized bio-oil using alcohol under a base catalyst And then extracting the unrefined biodiesel and removing impurities from the unrefined biodiesel and synthesizing the biodiesel. In this case, the acid catalyst may comprise sulfuric acid. And the deoxidation bio-oil extraction step may include the step of separating and removing impurities after making the acidity (pH) of the esterified bio-oil to 5.5 ~ 6.5. In addition, the base catalyst may include potassium hydroxide or sodium hydroxide.

According to another aspect of the embodiment, the alcohol may include at least one of methanol, ethanol, and butanol.

According to another aspect of the embodiment, the alcohol extract is distilled to remove the alcohol and then lyophilized, the non-polar material dissolved in the methylene chloride by mixing the freeze-dried raw material in methylene chloride (MC) Removing, stirring and mixing methanol with a substance not dissolved in the methylene chloride in the freeze-dried raw material, followed by extracting a liquid component from which the methanol and the solid phase component have been removed, and distilling the liquid component to distill the useful component. The method may further include extracting.

According to another aspect of the present invention, there is provided a method of preparing an oil-soluble extract using coffee grounds, comprising mixing and stirring coffee grounds and alcohol, followed by filtering to obtain an alcohol extract from which biomass has been removed. Distilling the alcohol extract to remove the alcohol and freeze drying the remaining aqueous extract; mixing the freeze-dried raw material with methylene chloride (MC) to remove the nonpolar substance dissolved in the methylene chloride, Mixing methanol with a substance which is not soluble in the methylene chloride in the freeze-dried raw material, stirring and extracting a liquid component from which the methanol and the solid phase components have been removed, and distilling the liquid component to extract a first useful component Steps.

According to one aspect of the embodiment, in the step of removing the non-polar material, the non-polar material dissolved in the methylene chloride may be separated and removed by centrifugal separation using ultrasonic cleaning. The method may further include a step of extracting the second useful component by mixing and stirring the solid component removed in the extraction of the liquid component with water, followed by extracting the liquid component.

Method for preparing an oil-soluble extract using coffee grounds according to another embodiment of the present invention for solving the above problems is a step of obtaining an alcohol extract from which biomass (biomass) is removed by mixing and stirring the coffee grounds and alcohol And distilling the alcohol extract to remove the alcohol and then freeze drying, mixing the freeze-dried raw material with methylene chloride (MC) to remove nonpolar substances dissolved in the methylene chloride, and freeze-dried. Mixing and stirring methanol to a material which is not soluble in the methylene chloride in the raw material, and then extracting the solid component from which the methanol and liquid components have been removed, and stirring the solid component into water and then extracting the liquid component to freeze-drying And extracting the useful ingredient. .

According to the present invention, since the coffee grounds discarded as food waste can be recycled to produce active ingredients as well as bio oils such as antioxidants, it can contribute not only to waste reduction but also to additional profit generation.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. The terms used are terms selected in consideration of functions in the embodiments, and the meaning of the terms may vary depending on the intention or custom of the user or operator. Therefore, the meaning of the terms used in the embodiments to be described later, according to the definition if specifically defined herein, and if there is no specific definition should be interpreted to mean generally recognized by those skilled in the art.

1 is a flow chart showing an example of a method for producing an oil-soluble extract using coffee grounds according to an embodiment of the present invention, Figures 2 and 3 is a flow chart showing in more detail the steps constituting the flow chart of FIG. to be. 1 through 3 illustrate a process of extracting bio-oil from coffee grounds, and by-products or target bio oils generated in the process of FIGS. 1 through 3. The process for preparing oil-soluble extracts (including biodiesel) from the will be described later.

Referring to FIG. 1, first, coffee remnants, which are starting materials, are mixed with alcohol, and a biomass is extracted by performing a predetermined extraction process (110). This step is to remove the components other than the materials that can be used for the extraction of bio-oil from the components contained in the coffee grounds. It is to use.

More specifically, referring to FIG. 2, first, coffee remnants are prepared. Coffee grounds may contain some moisture (eg, 60%). The alcohol may include at least one substance of methanol, ethanol, and butanol. In this process, for example, 4 kg of coffee grounds containing 60% moisture and 16 L of methanol were added, followed by stirring at 45 ° C. for 30 minutes, followed by extraction (extraction). Then, filtration is performed on the extracted solution to separate the biomass, which is a solid component, and the liquid component. The liquid component may include water and methanol in which certain useful components are dissolved. In addition, methanol is separated by distillation of liquid components, and water waste in which the remaining useful components are dissolved is used to extract other useful components (to be described later). The separated methanol can be reused in the mixing process with coffee grounds.

1 and 2, next, the biomass extracted in step 110 is mixed with hexane (Hexane), and then crude bio-oil is extracted (120). This step is a process for extracting by dissolving the crude bio-oil component that can be a raw material of the bio-oil among the components contained in the biomass in hexane. After mixing and extracting the biomass and hexane well, the biomass is filtered off and disposed of, and the remaining liquid components are distilled to remove hexane and crude bio-oil. To separate. The separated hexane can be used again to mix with biomass in step 120 (Recycle Hexane).

In this process, for example, the biomass extracted in step 110 was hot-air dried at 100 ° C. for 60 minutes, then, 16 L of n-hexane was added thereto, stirred for 30 minutes with ultrasonic waves, extracted, filtered, and the remaining liquid component was recovered. can do. After concentrating the remaining liquid component, 120 ml of methanol and 5 g of sodium hydroxide powder were added to the concentrate, stirred at 40 ° C. for about 30 minutes, cooled to 20 ° C., and then washed twice with 10 mL of purified water, n-hexane 5 L and activated carbon. After adding 5g and stirring for 30 minutes, centrifugation with a centrifuge and vacuum distillation at 40 ° C. may proceed to recover the solvent (n-hexane).

Referring to FIG. 1, the crude bio-oil layer is extracted after reacting the crude bio-oil with an acidic solvent (130). This step, also called degumming, is the process of first removing free fatty acids or phospholipids contained in unrefined bio-oil, and removing impurities that are well dissolved in acidic solvents. Hydrochloric acid (HCl) may be used as the acidic solvent, which is merely exemplary.

More specifically, referring to FIG. 3, the crude bio-oil extracted in step 120 is mixed with hydrochloric acid (HCl) and water to react with each other. For example, 0.1-1% hydrochloric acid may be added to the crude bio-oil to supply steam at 150 ° C. for 10 minutes. Then, the extraction process is performed on the solution, and impurities such as free fatty acids dissolved in an aqueous solution (more precisely, an aqueous solution mixed with hydrochloric acid) are removed together with water. Since the water layer is separated from the unrefined bio oil layer, in this step, removing the water layer may also remove impurities.

With continued reference to FIG. 1, free fatty acids remaining from the crude bio-oil layer are removed and bio-oil is extracted (140). This step is intended to remove impurities that dissolve well in free fatty acids and other basic solvents that were not completely removed in step 130. As the basic solvent, sodium hydroxide may be used, which is merely exemplary.

More specifically, referring to FIG. 3, the crude bio-oil layer extracted as a result of step 130 is mixed well with water and sodium hydroxide (NaOH), and then the solution is extracted (Extraction). After removing the aqueous layer from the extracted solution and performing filtration on the remaining crude bio-oil layer, distillation is performed to perform bio-oil (bo- oil). Bio oil obtained through this process can be used as an eco-friendly renewable support.

4 is a flow chart showing an example of a process for obtaining biodiesel from the bio-oil extracted in FIG. 5 to 7 are flowcharts illustrating each step of FIG. 4 in more detail. This embodiment shows an example of manufacturing biodiesel, which is one of environmentally friendly energy using bio oil extracted from coffee grounds, and it will be apparent to those skilled in the art that bio oils extracted from coffee grounds can be used for other purposes.

4 and 5, a process of obtaining deoxidized bio oil from the bio oil extracted as a result of FIG. 1 is performed (150). More specifically, the bio oil obtained in step 140 is subjected to an esterification reaction with an alcohol such as methanol under an acid catalyst. For example, when mixing 1 L of methanol, for example, about 20 mL of 95% sulfuric acid may be used as an acid catalyst, and bio-oil, methanol, and sulfuric acid are added to a reactor, stirred at about 60 ° C. for 2 hours, and reduced at about 50 ° C. for 10 minutes. Methanol is distilled off by distillation. After cooling to 20 to 30 ° C., a basic solution (eg, 1% sodium hydroxide solution) may be mixed to neutralize. In this case, the acidity (pH) can be about 6 after neutralization. In addition, 500 mL of purified water is stirred for 10 minutes, and the washing process may be repeated twice for 30 minutes. The phase separation of the solution is performed to remove methanol and the aqueous layer, and the deoxidation bio Get oil.

4 and 6, the crude biodiesel is extracted by transesterifying the deoxidized biooil using alcohol under a base catalyst (160). More specifically, a transesterification reaction is performed by adding a base catalyst such as sodium hydroxide or potassium hydroxide with alcohol such as methanol to some esterified raw material (that is, deoxidized bio oil) produced as a result of step 150. Get up. For example, in this process, about 20 mL of sodium hydroxide may be added to about 1 L of methanol, and stirred for about 1 hour to allow a transesterification reaction to form an ester. Then, the resultant reaction is centrifugal separation to remove the water collected in the lower layer (waste water layer) to obtain a crude bio diesel (crude bio diesel).

4 and 7, a process of extracting biodiesel by removing impurities from unrefined biodiesel is performed (170). More specifically, in order to separate glycerin and soap components, which are impurities remaining in the crude biodiesel, 0.1% hydrochloric acid is mixed to remove the residual impurities. Then, phase separation is performed to remove hydrochloric acid and only an oil layer is extracted, followed by washing with 500 mL of purified water. Then, phase separation separates the purified water layer, leaving only the oil layer. Subsequently, distillation under reduced pressure is carried out for 20 minutes at 80 to 100 ° C. with respect to the oil layer to remove water such as deionized water (DI water). Then, 5 g of sodium sulfate is added and stirred for 10 minutes, followed by centrifugal separation using a centrifugal separator. The impurities precipitated as a solid mass are filtered out and discharged through only high-purity liquid biodiesel (sodium sulfate is discharged into water). Dissolved and phase separated from biodiesel).

Through this process, high purity biodiesel may be manufactured. In addition, the manufactured biodiesel may be used alone or may be mixed with diesel and in a predetermined ratio.

Next, a method of extracting other useful substances from coffee grounds is explained. As described above, the coffee shows excellent properties in the antioxidant effect, the whitening effect, etc. Hereinafter, the process of extracting a material having such an effect from the coffee grounds will be described in detail.

8 is a flow chart showing one embodiment of preparing a useful oil extract other than bio oil from coffee grounds. FIG. 9 is a flowchart illustrating a process of preparing the oil-soluble extract of FIG. 8 from the water waste from which methanol is removed in the flowchart of FIG. 2.

Referring to FIG. 8, first, coffee remnants are prepared. Coffee grounds may contain some moisture (eg, 60%). The coffee remnants are mixed with alcohol and then subjected to a predetermined extraction process to obtain an alcohol extract from which biomass has been removed (210). This step is primarily to remove the components of the coffee grounds that can be used for the extraction of bio-oil (bio-oil). The alcohol may include, for example, at least one substance from methanol, ethanol, and butanol. In this process, for example, 4 kg of coffee grounds containing 60% moisture and 16 L of methanol were added, stirred at 45 ° C. for 30 minutes, and then extracted by extracting the alcohol solution.

8, distillation (distillation) of the liquid component (alcohol extract) is performed to separate methanol, and an aqueous extract is obtained (220). In addition to water, the water soluble extract contains other useful ingredients to be extracted. The methanol separated in this step may be reused in the mixing process with coffee grounds in step 210. More specifically, 2% (weight) of activated powder of dry powder sample is added to the alcohol extract and stirred, and the sample solution is filtered twice with 5 μm filter paper, and then the filtrate is recovered and n-hexane After the liquid-liquid extraction is added in equal amounts (Hexane), the layers are separated.

8 and 9, a freeze dry process is performed on the water-soluble extract. For example, the lower layer (aqueous solution) may be separated from the above-mentioned fraction, distilled under reduced pressure at 60 ° C. for 30 minutes, and freeze-dried at −80 ° C. The freeze-dried raw material is mixed with methylene chloride (MC) to remove the nonpolar material dissolved in the MC (230). For example, MC 2L may be mixed with a freeze-dried raw material and stirred using ultrasonic waves twice for 10 minutes, and then non-polar substances dissolved in MC may be removed by centrifugation with a centrifuge. MC may be recovered by performing a distillation process on the MC solution, and the remaining nonpolar material may be disposed of as waste material. The recovered MC can be reused for step 230.

In the freeze-dried raw material, methanol that is not dissolved in MC is mixed and stirred, and then the liquid component from which the methanol and the solid phase components are removed is extracted (240). That is, in step 240, an aqueous solution obtained by removing the solid phase component and the methanol solution is obtained. More specifically, the process of mixing and stirring methanol may be performed by using ultrasonic waves for 30 minutes. The solution is then subjected to extraction and filtering processes (also centrifugation if necessary) to first remove the solid phase. The solid component removed here can be used to prepare other oil soluble extracts, which will be described later. Subsequently, a distillation process is performed on the solution from which the solid phase component has been removed to remove methanol to obtain the remaining aqueous solution.

8 and 9, useful materials are extracted 250 from the aqueous solution obtained in step 240. More specifically, the aqueous solution obtained in step 240 may be distilled under reduced pressure at 60 ° C. for 30 minutes to extract useful substances (first active ingredient, extract material).

FIG. 10 is a flowchart showing another embodiment of preparing a useful oil extract other than bio oil from coffee grounds, and steps 310 to 330 are the same as steps 210 to 230 of FIG. 8 to avoid unnecessary duplication. Description is omitted. 11 is a flow chart showing in detail the process of obtaining an oil-soluble extract (second active ingredient) from the solid phase component obtained as a result of step 340.

Referring to FIG. 10, in the freeze-dried raw material obtained as a result of step 330, methanol is mixed with a raw material and stirred, followed by extracting the solid component from which the methanol and the aqueous solution components are removed (340). That is, in step 340, a solid component obtained by removing the aqueous component and the methanol solution is obtained. More specifically, the process of mixing and stirring methanol may be performed by using ultrasonic waves for 30 minutes. The solution can be extracted (filtered) and filtered (9, if necessary, centrifuged) to extract the solid phase and remove the remaining components.

10 and 11, water is mixed with the solid component obtained in step 340, and then useful materials are extracted using an aqueous solution (350). More specifically, 1L of purified water or DI water was added to the solid component obtained in step 340, stirred for 30 minutes using ultrasonic waves, followed by extraction (Fitraction), for example, centrifugation, and the filtrate (aqueous solution). Separate solid phase from solid phase. The separated solid phase is wasted (Waste material). The aqueous solution is lyophilized to extract useful material (second active ingredient, extract material).

The first and second active ingredients obtained through the above processes (steps 210 to 250 and steps 310 to 350) have been experimentally confirmed to have various effective effects including antioxidant and whitening effects.

As an example, an evaluation of the antioxidant effect was performed on the first active ingredient obtained as a result of step 250 and the second active ingredient obtained as a result of step 350. More specifically, the free radical scavenging ability of the DDPH (1,1-diphenyl-2-picrylhydrazyl radical) scavenging ability and the inhibitory effect on Peroxyl acid was confirmed for the first and second active ingredients, and SOD (SuperOxide) was confirmed. The enzyme activity against radical deoxygenase was also measured. As a result of DPPH scavenging activity, it showed 2% higher inhibitory activity in the first active ingredient than in the second active ingredient. It showed high activity inhibitory ability.

As another example, the whitening effect was evaluated for the first active ingredient obtained as a result of step 250 and the second active ingredient obtained as a result of step 350. More specifically, in order to confirm the whitening efficacy of the first and second active ingredients, the inhibitory activity of Tyrosinase enzyme activity and DOPA (dihydroxyphenylalanine) activity related to melanin fish process were measured. As a result of measuring DOPA activity inhibitory activity, the inhibitory activity was 17% higher in the first active ingredient than in the second active ingredient, and the result of measuring the inhibitory activity of Tyrosinase enzyme activity was about 15 in the first effective ingredient compared to the second active ingredient. It showed a high activity inhibitory activity by about%.

The above description is only an embodiment of the present invention, and the technical idea of the present invention should not be construed as being limited by this embodiment. The technical idea of the present invention should be specified only by the invention described in the claims. Therefore, it will be apparent to those skilled in the art that the above-described embodiments may be implemented in various forms without departing from the spirit of the present invention.

1 is a flow chart showing an example of a method for producing an oil-soluble extract using coffee grounds according to an embodiment of the present invention.

2 and 3 are flowcharts illustrating in more detail the steps constituting the flowchart of FIG. 1.

4 is a flow chart showing an example of a process for obtaining biodiesel from the bio-oil extracted in FIG.

5 to 7 are flowcharts showing each step of FIG. 4 in more detail.

8 is a flow chart showing one embodiment of preparing a useful oil extract other than bio oil from coffee grounds.

FIG. 9 is a flowchart illustrating a process of preparing the oil-soluble extract of FIG. 8 from water waste from which methanol is removed in the flowchart of FIG.

FIG. 10 is a flow chart showing another embodiment of preparing a useful oil extract other than bio oil from coffee grounds.

FIG. 11 is a flowchart showing in detail a process of obtaining a useful oil extract from the solid component obtained as a result of step 340 of FIG. 10.

Claims (12)

Mixing coffee grounds with alcohol, stirring and filtering to extract biomass from which alcohol extract is removed; Hexane is mixed with the biomass, stirred, and filtered to remove solid components to extract crude bio-oil; Reacting the crude bio-oil with an acidic solvent to separate the aqueous solution layer and the crude bio-oil layer; And Removing a free fatty acid from the crude bio-oil layer using a basic solvent to extract the bio-oil, the method of producing an oil-soluble extract using coffee grounds. The method of claim 1, Esterifying the biooil with an alcohol under an acid catalyst and then extracting deoxidized bio-oil; Transesterifying the deoxidized biooil with alcohol under a base catalyst and then extracting the crude biodiesel; And Removing impurities from the crude biodiesel and producing a bio-diesel, characterized in that it further comprises the step of synthesizing the biodiesel. The method of claim 2, The acid catalyst is a method of producing an oil-soluble extract using coffee grounds, characterized in that containing sulfuric acid. The method of claim 3, The deoxidation bio-oil extraction step is a method of producing an oil-soluble extract using coffee grounds, comprising the step of separating and removing impurities after the acidity (pH) of the esterified bio-oil is 5.5 to 6.5. The method of claim 2, The base catalyst is a method for producing an oil-soluble extract using coffee grounds, characterized in that containing potassium hydroxide or sodium hydroxide. The method of claim 1, The alcohol is a method of producing an oil-soluble extract using coffee grounds, characterized in that it comprises at least one of methanol, ethanol, and butanol. The method of claim 1, Distilling the alcohol extract to remove the alcohol and then freeze drying; Mixing the freeze-dried raw material with methylene chloride (Methylene Chloride, MC) to remove non-polar substances dissolved in the methylene chloride; Stirring and mixing methanol with a substance not dissolved in the methylene chloride in the freeze-dried raw material and then extracting a liquid component from which the methanol and the solid phase component have been removed; And Distilling the liquid component to extract the useful component, characterized in that it further comprises the step of extracting the useful component. Mixing, stirring and filtering coffee grounds with alcohol to obtain an alcohol extract from which biomass has been removed; Distilling the alcohol extract to remove the alcohol and freeze drying the remaining aqueous extract; Mixing the freeze-dried raw material with methylene chloride (Methylene Chloride, MC) to remove non-polar substances dissolved in the methylene chloride; Stirring and mixing methanol with a substance not dissolved in the methylene chloride in the freeze-dried raw material and then extracting a liquid component from which the methanol and the solid phase component have been removed; And A method of producing an oil-soluble extract using coffee grounds, comprising distilling the liquid component to extract a first useful component. The method of claim 8, In the step of removing the non-polar material, the method for producing an oil-soluble extract using coffee grounds, characterized in that the non-polar material dissolved in the methylene chloride is separated by a centrifugal separator using ultrasonic cleaning. The method of claim 8, The method of producing a useful oil extract using coffee grounds further comprises the step of mixing the solid component removed in the extraction step of the liquid component with water, stirring and extracting the liquid component to freeze-drying to extract the second useful component. Mixing, stirring and filtering coffee grounds with alcohol to obtain an alcohol extract from which biomass has been removed; Distilling the alcohol extract to remove the alcohol and freeze drying the remaining aqueous extract; Mixing the freeze-dried raw material with methylene chloride (Methylene Chloride, MC) to remove non-polar substances dissolved in the methylene chloride; Mixing methanol with a substance which is not soluble in the methylene chloride in the freeze-dried raw material, stirring the mixture, and then extracting the solid phase component from which the methanol and liquid components are removed; And Mixing the solid component with water, stirring and extracting the liquid component to freeze-drying to extract the useful component. Oil-soluble extract prepared according to any one of claims 1 to 11.

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