CN101161807B - Method for extraction separating hop extract and hop essential oils from hops - Google Patents
Method for extraction separating hop extract and hop essential oils from hops Download PDFInfo
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- CN101161807B CN101161807B CN2006101047462A CN200610104746A CN101161807B CN 101161807 B CN101161807 B CN 101161807B CN 2006101047462 A CN2006101047462 A CN 2006101047462A CN 200610104746 A CN200610104746 A CN 200610104746A CN 101161807 B CN101161807 B CN 101161807B
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Abstract
The invention relates to extraction solvent for extracting effective components from hop raw material and extraction and separation method thereof, wherein, the method for extraction and separation of hop extract and hop essential oil includes following steps as follows: (1) hop is filled in an extraction kettle and when the volume of raw material reaches 30 to 80 percent of that of the extraction kettle, feeding is stopped and a feeding-discharging control valve is closed; (2) a vacuum pump reduces the vacuum degree inside the extraction kettle below 1x10<4>pa to discharge the fixed gas from the kettle; (3) the liquid extract inside a solvent storage tank is fed into the extraction kettle till the hop raw material is completely immersed in the extract; (4) the extraction kettle is heated to maintain the temperature of the kettle between 10 DEG C and 50 DEG C, the extraction pressure between 0.4MPa to 2.0MPa and the extraction time between 40min to 60min and one-off immersion extraction is completed after filtration and separation of solid-liquid phase; (5) mixed liquid is fed into a temporary storage kettle through combined extraction and then is injected into an analytic kettle from the temporary storage kettle through a transfer pump; (6) mixed solution after primary analytic separation is injected into a secondary analytic kettle through the transfer pump to be heated through ajacket type heat exchanger and then is pumped continuously by a vacuum pump set; in addition, in the vacuum state of 1*10<4>pa-5*10<-2>pa, analytic evaporation of entrainer is completed and the entrainer is recycled after condensation by a recovery tank; meanwhile, the mixture of hop extract and hop essential oil is obtained inside the secondary analytic kettle.
Description
Technical field:
The present invention relates to the extraction solvent of extracting effective components from hop raw material and extraction thereof, separation method.
Background technology:
Hops is the basic raw material of beer production, and its known chemical composition has kind more than 200, and special chemical component comprises bitter substance alpha-acid, β-acid and hops essential oil and polyphenol.Wherein, alpha-acid (first kind resin or Humulone) is soluble in alcohol, ether, sherwood oil, and is water insoluble, and the content in fresh flower is 5-11%, in dry state content greater than 6.5%; β-acid (claiming second kind resin or lupulone again) dissolves in ether, the sherwood oil, and is water insoluble, and extremely strong hops fragrance is arranged, and bitter taste is equivalent to 1/9 of alpha-acid, and antiseptic power is equivalent to 1/3 of alpha-acid, in dry state content greater than 2.0%; The hops essential oil is present in the hops body of gland particle, is the yellow-green colour oily liquids, is the important fragrance source of beer, and content is 0.4-2.0%; Polyphenol is the general name of multiple compound, accounts for the 4-8% of hops total amount.
Domestic hops kind mainly is bitter type flowers such as Qingdao Da Hua, Qingdao Xiao Hua, No. 3, Yimianpu, white No. 1 of length, and its processing mode and goods are divided into three kinds:
1, pressure rolling hops: will contain the fresh beer flower of moisture 75-80%, in drying oven with hot air dries to containing moisture 6-8%, to containing about moisture 10-12%, the whole hops of pressure rolling is made in repressed again, packing through artificial moisture regain.
2, hop pellet: under 55 ℃ of hot air actings, hops is dried to contains moisture 5-6%, pulverize and granulation, be processed into hop pellet, be packaged in the airtight container, fill N
2Or CO
2Gas is protected.
3, Hops Extract: utilize CO
2The extracting power that fluid has is strong, the extraction yield height, and selectivity is strong, and advantages such as superior product quality adopt supercritical CO
2Fluid extraction processing Hops Extract.
The traditional technology method is processed whole hops of resulting pressure rolling and hop pellet, technological temperature all need surpass more than 50 ℃, easily cause " thermo-sensitivity " effective constituent alpha-acid, β-acid decomposition or sex change in various degree, make product that time biochemistry take place, simultaneously, the hops essential oil also very easily loses because of volatilization.
Supercritical CO
2The fluid extraction Hops Extract is an ideal technology method comparatively at present, and it is strong that this method has extracting power, the extraction yield height, and selectivity is strong, advantages such as superior product quality.But, CO
2Must under the ultra-high voltage state more than the 20MPa, can extract the processing Hops Extract; the product price of being produced is relatively more expensive; and on a set of equipment, can't extract and separate Hops Extract and hops essential oil simultaneously, so be subjected to restriction to a certain degree in the mass-producing application of this method in hops produces.
Summary of the invention:
The objective of the invention is to avoid the deficiencies in the prior art part and provide a kind of from hops the method for extracting and separating Hops Extract and hops essential oil.Hydrofluorocarbons that present method utilization is in a liquid state or C
3-C
4The mixed solvent of saturated alkane to the dissolution characteristics of hops effective constituent uniqueness, the extraction of carrying out target component in the hop raw material selectively with separate, with further raising product extraction rate and raw-material utilization ratio.
Purpose of the present invention is by realizing by the following technical solutions: a kind of from hops the method for extracting and separating Hops Extract and hops essential oil, its principal feature is to include following steps:
(1) with hop raw material oven dry, pulverizing,, when the raw material volume reaches extraction kettle volume 30%-80%, stops material loading, close the input and output material control valve by the extraction kettle of packing into after the granulation of Φ 3mm-Φ 6mm diameter;
(2) vacuum pump reduces to 1 * 10 with vacuum tightness in the extraction kettle
4Below the pa, get rid of noncondensable gas in the still;
(3) liquid extraction liquid in the solvent tank is injected extraction kettle until complete submergence hop raw material:
(4) the heating extraction kettle makes its temperature remain on 10 ℃-50 ℃ scope, and extracting pressure is 0.4MPa-2.0MPa, and the extraction time is 40min-60min, filters, separates the solid-liquid phase, finishes once to soak and extracts; Re-extract 2-4 time is finished an extraction cycle process; Particularly preferred method is to utilize the concentration difference of effective constituent in the solvent to carry out " gradient " extraction, be about to the 3rd, 4 extractions of extraction kettle gained lower concentration mixed solution, directly inject another extraction kettle and carry out its immersion of the 1st, 2 time extraction, so that dissolved effective constituent amount in the raising solvent, reduce the solvent evaporation treatment capacity of extraction-container, reduce energy consumption;
(5) merge the extraction mixed solution to temporary storage kettle, transferpump injects extraction-container with the mixing solutions in the temporary storage kettle; Transferpump carries mixing solutions repeatedly by heat exchanger and jacketed heat exchanger heating, 5 * 10
5Pa-1 * 10
4The pressure range of pa is kept resolution temperature all the time and is higher than solvent boiling point, sprays diffusion through injector at extraction-container, and make liquid extraction solvent in extraction-container, resolve evaporation and be gaseous state, thus separating of oil with Hops Extract and hop extract; Solvent vapo(u)r enters and returns solvent tank after the heat exchange condensation is converted into saturated liquid after the extracting of vacuum pump group, compressor unit compression;
(6) resolve isolating medicinal extract fluid through one-level and inject the secondary extraction-container by transferpump, by the jacketed heat exchanger heating, the vacuum pump group continues extracting, 1 * 10
4Pa-5 * 10
-2Under the vacuum state of pa, ethanol in the still in the medicinal extract fluid or acetone entrainment agent are resolved evaporation, finish recovery after the withdrawing can condensation, obtain the mixture of Hops Extract and hops essential oil simultaneously at the secondary extraction-container.
The method of described extraction from hop raw material, separation Hops Extract and hops essential oil also includes following steps:
(7) jacketed heat exchanger continues the heating extraction kettle, and the hops material slag in the continuous stirred tank is 1 * 10
4Pa-5 * 10
-2Under the vacuum tightness of Pa, material in the slag liquid extraction liquid and the mixed solvent of entrainment agent resolve evaporation, finish separating fully of solvent and raw material; Condensation, recovery, the liquid extraction liquid of separation and entrainment agent are in order to recycling.
(8) the secondary extraction-container is separated the medicinal extract mixture that obtains, in " decompression diffusion degreasing " device, with pure N
2Be diffusant, medicinal extract is mixed mutually with diffusant, under the pressure of 0.4-0.5MPa, N
2Spray into separating still at a high speed with medicinal extract, volatility hops essential oil is discharged separating still with diffusant, is recovered systematic collection, N after condensation
2By being disposed to atmosphere behind the vacuum unit.Repeat to mix and---spray diffusion---separation---condensation process, reach the mutual isolating purpose of Hops Extract and hop extract oil phase.
Described from hops the method for extracting and separating Hops Extract and hops essential oil, also include in the step (3) entrainment agent in the entrainment agent jar is injected extraction kettle to change the polarity of mixed solvent, the volume ratio of controlling liquid extraction liquid and entrainment agent is 4: 1 to 5: 1, stirs raw material, solvent, entrainment agent and it is mixed fully.
Described from hops the method for extracting and separating Hops Extract and hops essential oil, its extraction solvent is the azeotropic compound 406A that is in a liquid state.
Described from hops the method for extracting and separating Hops Extract and hops essential oil, its extraction liquid is for containing more than one C
1-C
4The liquid carbon hydrofluorocompounds, perhaps C
3-C
4The saturated alkane mixing solutions.
Described from hop raw material the method for extracting and separating Hops Extract and hops essential oil, its liquid C
3-C
4The saturated alkane mixed solution be the propane of 5%-20% and the butane mixture of 80%-95%.
Described from hop raw material the method for extracting and separating Hops Extract and hops essential oil, its extraction liquid is the liquid azeotropic compound 406A of 70%-100%, the ethanol of 1%-30% or acetone entrainment agent.
Described from hop raw material the method for extracting and separating Hops Extract and hops essential oil, its extraction liquid is 70%-100% liquid propane gas, butane mixed solution, the ethanol of 1%-30% or acetone entrainment agent.
The invention has the beneficial effects as follows:
1. utilize hydrofluorocarbons or C
3-C
4The mixed solvent of saturated alkane to the dissolution characteristics of hops effective constituent uniqueness, the extraction of carrying out target component in the hop raw material selectively with separate, further improve product extraction rate and raw-material utilization ratio.
2. utilize hydrofluorocarbons or saturated alkane and mixed solvent dissolving power thereof strong, low-boiling physical property can reduce the energy, the solvent-oil ratio of system, reduces production costs, and improves the market competitiveness of Hops Extract and hops essential oil.
3. bring into play hydrofluorocarbons or saturated alkane and the lower characteristic of mixed solvent boiling point thereof, by improving the vacuum tightness of technological process, make extraction solvent 10 ℃ to 50 ℃ temperature range rapid evaporation, effectively avoid the loss and the destruction of " thermo-sensitivity " composition, preserve the activity of product effective constituent as far as possible, improve product quality.
The course of processing of present method all be in comparison safety in, finish under the low-pressure state, the useful volume of equipment is subjected to the restriction of complete processing little, the safe performance indexes of system improves relatively, simultaneously, has reduced the technology difficulty and the construction costs of device fabrication significantly.
5. system is carried in special design secretly in this extracting process, utilize before extraction or in the middle of the extraction process ethanol, acetone as cosolvent to change polarity of solvent, make solvent and cosolvent performance synergy, the raising extraction efficiency.
6. the extraction of effective constituent and sepn process operation break-down on same set of equipment is finished, and has shortened operational path, has improved production efficiency.
Description of drawings:
Fig. 1: the method synoptic diagram of solvent extraction and separation Hops Extract and hops essential oil;
Fig. 2: the process principle figure of solvent extraction and separation Hops Extract and hops essential oil.
Embodiment:
Below in conjunction with accompanying drawing most preferred embodiment is described in further detail:
Fig. 1 is the method synoptic diagram of solvent extraction and separation Hops Extract and hops essential oil.
Embodiment 1:406A fluid extraction separates Hops Extract and hops essential oil, includes following steps:
(1) with hop raw material oven dry, pulverizing,, when the raw material volume reaches extraction kettle volume 1/2, stops material loading, close input and output material control butterfly valve by the extraction kettle of packing into after the granulation of Φ 3mm-Φ 6mm diameter.
(2) vacuum pump reduces to 1 * 10 with extraction kettle vacuum tightness
4Below the pa, get rid of noncondensable gas in the still.
(3) liquid 406A in the solvent tank is injected extraction kettle until complete submergence hop raw material, the heating extraction kettle makes it be warming up to 40 ℃-45 ℃, and extracting pressure rises to 0.8MPa-1.3MPa, mixes raw material and solvent, soak and extracted filtering separation solid-liquid phase 50 minutes; Re-extract three to four times, and with the 3rd, 4 extraction gained lower concentration mixed solution, inject another extraction kettle and carry out its immersion of the 1st, 2 time extraction, so that improve dissolved effective constituent amount in the solvent.
(4) merge the extraction mixed solution to temporary storage kettle, transferpump injects extraction-container with the mixing solutions in the temporary storage kettle; Transferpump carries mixing solutions repeatedly by heat exchanger and jacketed heat exchanger heating, to keep resolution temperature greater than 10 ℃; 5 * 10
5Pa-1 * 10
4The pressure range of pa, the 406A fluid in the mixing solutions is resolved evaporation in extraction-container; 406A steam is gone into main condenser and is carried out heat exchange through the compression of the extracting of vacuum pump group, compressor unit is laggard, and vapor condensation returns solvent tank after being converted into saturated liquid, obtains the mixture of Hops Extract and hops essential oil simultaneously at the one-level extraction-container.
(5) jacketed heat exchanger continues the heating extraction kettle, and the hops material slag in the continuous stirred tank is 5 * 10
-2Under the Pa high vacuum state, the 406A solvent of material in the slag resolved evaporation, finishes separating fully of raw material and solvent; Condensation, recovery 406A solvent are in order to recycling.
(6) with the mixture that obtains in the extraction-container, in " decompression diffusion degreasing " device, with pure N
2Be diffusant, utilize " Wen Qiuli " absorption principle that medicinal extract is mixed mutually with diffusant, under the pressure of 0.5MPa, N
2Spray into separating still at a high speed with medicinal extract, make the volatility hop essential oil discharge separating still, after condensation, be recovered systematic collection, N with diffusant
2By being disposed to atmosphere behind the vacuum unit.---spray diffusion---separation---condensation process, Hops Extract separates mutually with the hop extract oil phase, obtains containing the Hops Extract and the hop extract oil production of alpha-acid, β-acid respectively to repeat mixing.
Embodiment 2: hydrofluorocarbons 134A fluid extraction separates Hops Extract and hops essential oil
The included step of present embodiment is all identical with embodiment 1.
Embodiment 3:406A fluid and alcohol mixed solution extracting and separating Hops Extract thereof and hops essential oil
The step of present embodiment (1), (2) are identical with embodiment 1.
(3) the liquid 406A in the solvent tank is injected extraction kettle until complete submergence hop raw material, then 95% ethanolic soln in the entrainment agent jar is injected extraction kettle to change the polarity of mixed solvent, control 406A and alcoholic acid volume ratio are about 4: 1, and stirring raw material, solvent, entrainment agent mix fully it.
The step of present embodiment (4), (5) and embodiment 1 step (3), (4) are identical.
(6) resolve isolating mixing solutions through one-level and inject the secondary extraction-container by transferpump, by the jacketed heat exchanger heating, the vacuum pump group continues extracting, 5 * 10
-2Under the vacuum state of pa, entrainment agent ethanol is resolved evaporation, finishes alcohol solvent through the withdrawing can condensation and reclaims, and obtains the mixture of Hops Extract and hops essential oil simultaneously at the secondary extraction-container.
(7) jacketed heat exchanger continues the heating extraction kettle, and the hops material slag in the continuous stirred tank is 5 * 10
-2Under the Pa high vacuum state, 406A, the alcohol solvent of material in the slag resolved evaporation, finishes separating fully of raw material and solvent; Condensation, recovery, separation 406A and alcohol solvent are in order to recycling.
(8) with the mixture that obtains in the extraction-container, in " decompression diffusion degreasing " device, with pure N
2Be diffusant, utilize " Wen Qiuli " absorption principle that medicinal extract is mixed mutually with diffusant, under the pressure of 0.5MPa, N
2Spray into separating still at a high speed with medicinal extract, make the volatility hop essential oil discharge separating still, after condensation, be recovered systematic collection, N with diffusant
2By being disposed to atmosphere behind the vacuum unit.---spray diffusion---separation---condensation process, Hops Extract separates mutually with the hop extract oil phase, obtains containing the Hops Extract and the hop extract oil production of alpha-acid, β-acid respectively to repeat mixing.
Embodiment 4: the third, butane mixing solutions extracting hop medicinal extract and hops essential oil.
The step of present embodiment (1), (2) are identical with embodiment 1.
(3) 15% propane and 85% butane solution are mixed the back and inject solvent tank.
The subsequent step of present embodiment (4)-(7) are identical with embodiment 1 step (3)-(6).
The mixing solutions extracting and separating Hops Extract of embodiment 5: the third, butane and acetone and hops essential oil.
The step of present embodiment (1), (2) are identical with embodiment 1.
(3) 15% propane and 85% butane solution are mixed the back and inject solvent tank.
(4) liquid state in the solvent tank third, butane mixing solutions are injected extraction kettle until complete submergence hop raw material, then the acetone soln in the entrainment agent jar is injected extraction kettle to change the polarity of mixed solvent, the volume ratio of control third, butane and acetone is about 5: 1, mixes raw material, solvent, entrainment agent;
(5) liquid state third, butane in the solvent tank are injected extraction kettle until complete submergence hop raw material, the heating extraction kettle makes it be warming up to 40 ℃-45 ℃, and extracting pressure rises to 0.8MPa-1.3MPa, mixes raw material and solvent, soak and extracted filtering separation solid-liquid phase 50 minutes; Re-extract three to four times, and with the 3rd, 4 extraction gained lower concentration mixed solution, inject another extraction kettle and carry out its immersion of the 1st, 2 time extraction, so that improve dissolved effective constituent amount in the solvent.
(6) merge the extraction mixed solution to temporary storage kettle, transferpump injects extraction-container with the mixing solutions in the temporary storage kettle; Transferpump carries mixing solutions repeatedly by heat exchanger and jacketed heat exchanger heating, to keep resolution temperature greater than 10 ℃; 5 * 10
5Pa-1 * 10
4The pressure range of pa, third in the mixing solutions, butane fluid liquid are resolved evaporation in extraction-container; The third, butane steam is gone into main condenser and is carried out heat exchange through the compression of the extracting of vacuum pump group, compressor unit is laggard, vapor condensation returns solvent tank after being converted into saturated liquid, obtains simultaneously the mixture of Hops Extract and hops essential oil, acetone at the one-level extraction-container.
(7) resolve isolating mixing solutions through one-level and inject the secondary extraction-container by transferpump, by the jacketed heat exchanger heating, the vacuum pump group continues extracting, 5 * 10
-2Under the pa high vacuum state, entrainment agent acetone is resolved evaporation, finishes acetone solvent through the withdrawing can condensation and reclaims, and obtains the mixture of Hops Extract and hops essential oil simultaneously at the secondary extraction-container.
The step of present embodiment (8), (9) and embodiment 1 step (5), (6) are identical.
Application examples: Fig. 2 is the process principle figure of solvent extraction and separation Hops Extract and hops essential oil.
Solvent extraction, the device that separates hops effective constituent describe in detail: at the particular requirement to extraction process of the physics-chem characteristic of hop raw material, adapt to device with multiple solvent extraction and separation Hops Extract and hops essential oil, storage tank 1 is arranged, extractor 4a, 4b, extraction-containers 9 etc., adopt following mode of connection to constitute the extracting and separating system: to comprise between each equipment:
1), 17 outlets of storage tank 1, entrainment agent jar 15, storage tank are connected with transferpump 2a, 2e, 2f inlet respectively, transferpump 2a, 2e, 2f export with preheat exchanger 3a, extractor 4a, 4b between be connected by pipeline, valve, constitute solvent delivery system with this.
2), through the outlet of extractor 4a, 4b, wherein one the tunnel through connecting temporary jar 6 input aperture, upper end behind the transferpump 2b;
Another road connects temporary jar 6 following end interface by connecting the inlet of strainer 7 behind the transferpump 2b behind the process centre exit of filter 7.
3), temporary jar 6 bottom delivery port is connected with extraction-container 9a inlet by pipeline with transferpump 2c, heat exchanger 3b; The lower end outlet of extraction-container 9a is divided into two-way, and the transferpump 2d of leading up to connects the last end entrance of secondary extraction-container 9b; Another road is connected with heat exchanger 3b through the outlet of transferpump 2d, makes heat exchanger 3b, extraction-container 9a constitute the local circulation loop.
4), the centre entrance of strainer 7 is connected with the outlet of transferpump 2b, the top exit end divides two-way to be connected respectively with vacuum pump 12a, 12b inlet;
5), extraction-container 9a, 9b centre exit be communicated with withdrawing can 10 respectively, top exit is communicated with vacuum pump 12a, 12b respectively, withdrawing can 10 top port are communicated with vacuum pump 12b, condenser 11b, 11c respectively;
6), extraction-container 9b outlet at bottom is connected with " Venturi " producer 16 centre entrances, " Venturi " producer 16 exit end are connected with dispersion device 14 inlets; N2 or CO2 gas piping are connected with " Venturi " producer 16 entrance ends, and dispersion device 14 outlet at bottoms are connected with " Venturi " producer 16 centre entrances; The outlet of dispersion device 14 upper ends is connected with collection device 18 inlets, constitutes the system of diffusion, separation, collection Hops Extract and essential oil with this.
7), the last end interface of extractor 4a, 4b is connected with sprayed tank 5, sprayed tank 5 outlets through surge tank 8a after, the one tunnel is communicated with surge tank 8b, compressor 13a, surge tank 8c through condenser 11b after connecting vacuum pump 12a outlet; Directly be communicated with behind the process compressor 13b of another road with surge tank 8c inlet;
8), surge tank 8c outlet links to each other with heat exchanger 3b import, the outlet of preheat exchanger 3b lower end enters the mouth with condenser 11a and is connected;
9), condenser 11a outlet both was communicated with solvent tank 1, also entering the mouth with extractor 4a, 4b respectively is communicated with.
Above-mentioned mode of connection, by the control mode of change extraction solvent and extraction equipment, thus the operating mode of formation extracting and separating Hops Extract and hops essential oil.
The Hops Extract examining report
Hops essential oil examining report
Claims (2)
1. the method for extracting and separating Hops Extract and hops essential oil from a hops is characterized in that including following steps:
(1) with hop raw material oven dry, pulverizing,, when the raw material volume reaches extraction kettle volume 30%-80%, stops material loading, close the input and output material control valve by the extraction kettle of packing into after the granulation of Φ 3mm-Φ 6mm diameter;
(2) vacuum pump reduces to 1 * 10 with extraction kettle vacuum tightness
4Pa-5 * 10
-2Pa gets rid of noncondensable gas in the still;
(3) liquid extraction liquid in the solvent tank is injected extraction kettle until complete submergence hop raw material, entrainment agent in the entrainment agent jar is injected extraction kettle to change the polarity of mixed solvent, the volume ratio of controlling liquid extraction liquid and entrainment agent is 4: 1-5: 1, mix raw material, solvent, entrainment agent; Propane that described liquid extraction liquid is 5%-20% and the butane mixing solutions of 80%-95%;
(4) heating makes the extraction kettle temperature keep 10 ℃-50 ℃, and extracting pressure is 0.4MPa-2.0MPa, and the extraction time is 40min-60min, finishes once to soak and extracts; Re-extract 2-4 time, and with the 2-4 time extraction gained lower concentration mixed solution, inject another extraction kettle and carry out its immersion of the 1st, 2 time extraction, so that improve dissolved effective constituent amount in the solvent;
(5) merge the extraction mixed solution to temporary storage kettle, transferpump injects extraction-container with the mixing solutions in the temporary storage kettle; Transferpump carries mixing solutions repeatedly by heat exchanger and jacketed heat exchanger heating, to keep 10 ℃-50 ℃ of resolution temperatures; 5 * 10
5Pa-1 * 10
4The pressure range of pa, the liquid extraction liquid fluid in the mixing solutions is resolved evaporation in extraction-container, and solvent vapo(u)r is gone into main condenser and is carried out heat exchange through the compression of the extracting of vacuum pump group, compressor unit is laggard, and condensation is returned solvent tank after being converted into saturated liquid;
(6) resolve isolating mixing solutions through one-level and inject the secondary extraction-container by transferpump, by the jacketed heat exchanger heating, the vacuum pump group continues extracting, 1 * 10
4Pa-5 * 10
-2Under the pa vacuum state, entrainment agent is resolved evaporation, finishes entrainment agent through the withdrawing can condensation and reclaims, and obtains the mixture of Hops Extract and hops essential oil simultaneously at the secondary extraction-container.
2. as claimed in claim 1 from hops the method for extracting and separating Hops Extract and hops essential oil, it is characterized in that also including following steps:
(7) jacketed heat exchanger continues the heating extraction kettle, and the hops material slag in the continuous stirred tank is 1 * 10
4Pa-5 * 10
-2The pressure range of Pa, material in the slag liquid extraction liquid and the mixed solvent of entrainment agent resolve evaporation, finish separating fully of raw material and solvent; Condensation, recovery, the liquid extraction liquid of separation and entrainment agent are in order to recycling;
(8) the secondary extraction-container is separated the medicinal extract mixture that obtains, in " decompression diffusion degreasing " device, with pure N
2Be diffusant, medicinal extract is mixed mutually with diffusant, under the pressure of 0.4MPa-0.5MPa, N
2Spray into separating still at a high speed with medicinal extract, repeat mixing-injection diffusion-separation-condensation process, make volatility hops essential oil discharge separating still, after condensation, be recovered systematic collection, N with diffusant
2By being disposed to atmosphere behind the vacuum unit, reach the purpose that hops essential oil and Hops Extract are separated from each other.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101047462A CN101161807B (en) | 2006-10-11 | 2006-10-11 | Method for extraction separating hop extract and hop essential oils from hops |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101047462A CN101161807B (en) | 2006-10-11 | 2006-10-11 | Method for extraction separating hop extract and hop essential oils from hops |
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| CN101161807B true CN101161807B (en) | 2011-09-28 |
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| WO2016080007A1 (en) * | 2014-11-19 | 2016-05-26 | アサヒビール株式会社 | Method for producing beer-tasting beverage, and method for imparting hop aroma to beer-tasting beverage |
| CN106345139A (en) * | 2015-07-14 | 2017-01-25 | 中昊晨光化工研究院有限公司 | Extraction device and method of extracting active ingredient from solid matter |
| CN107019930B (en) * | 2016-01-31 | 2019-02-01 | 侯梦斌 | A kind of weak extract equipment of middle vacuum and technique |
| CN106281720A (en) * | 2016-10-30 | 2017-01-04 | 王庆忠 | CO2supercritical extraction hop quintessence oil |
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| CN1122363A (en) * | 1994-04-28 | 1996-05-15 | 斯太纳酒花有限公司 | Extraction of hops |
| CN1541262A (en) * | 2001-08-10 | 2004-10-27 | ά�����ʩ�߿˲�ʿ���Ϲ�˾ | Hops extracts, method for prodn. and use |
| CN1687339A (en) * | 2005-05-11 | 2005-10-26 | 玉门拓璞科技开发有限责任公司 | Method and equipment for recovering hop oil by extracting hop through carbon dioxide |
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