CN1294183A - Process for extracting hop extract from hop particles by back extraction with supercritical CO2 - Google Patents

Process for extracting hop extract from hop particles by back extraction with supercritical CO2 Download PDF

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CN1294183A
CN1294183A CN 00133516 CN00133516A CN1294183A CN 1294183 A CN1294183 A CN 1294183A CN 00133516 CN00133516 CN 00133516 CN 00133516 A CN00133516 A CN 00133516A CN 1294183 A CN1294183 A CN 1294183A
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hop
extraction
supercritical
extract
hop extract
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CN1100865C (en
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孙传经
孙云鹏
陈斌
孙明华
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孙传经
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Abstract

A process for extracting hop extract from hot partides by supercritical back extraction with CO2 features that the broken hop particles are loaded in multi-layer raw materials container and then put in extracting reactor for back extraction with supercritical CO2 at 58 deg.C and 22 MPa for 2-3 hrs, and separation step is them performed at 20 deg.C and 5 MPa. Its advantages include high output rate (13.6%), high alpha-acid content (41.0%), high extraction rate (92.8%), short period and low consumption of CO2.

Description

Supercritical CO 2The back extraction method is extracted the technology of hop extract from pellet hop
The present invention relates to a kind of supercritical CO 2Extract the technology of hop extract, particularly a kind of supercritical CO 2The back extraction method is extracted the technology of hop extract (Hop Extracts) from pellet hop.
Hops (Hop) is the main raw material of brewing industry, for solving problems such as the transportation and the storage of guaranteeing the quality, product innovation forms such as hops particle, hop extract, different hop extract appear in succession, wherein, hop extract is the main product innovation that replaces hops always, is subjected to the favor in market.At present, the method of extracting hop extract mainly contains three kinds: the one, with organic solvent extraction hop extracts such as hexane, ethanol, methylene dichloride, because organic solvent poor selectivity, in extraction process, useless hardened resin, wax are extracted, and the fragrance of a flower essential oil of also filling a wine cup for when organic solvent is removed in distillation is removed the local flavor that has destroyed beer, simultaneously, remaining organic solvent works the mischief to human body.The 2nd, liquid CO 2Extract the method for hop extract,, cause energy consumption big, the cost height because of the big separation efficiency of solute resistance to mass transfer in liquid is low.The 3rd, supercritical CO 2Extract the hop extract method, this medicinal extract is possessed the effective constituent of hops, does not contain hardened resin and wax, does not contain nitrite, and no solvent residue is free from environmental pollution.But traditional forward extraction method is still continued to use in its extraction, and promptly hops are contained in the extraction kettle of individual layer charging basket, CO 2Flow from bottom to top, hops are at the still inner suspension, and air-teturning mixed phenomenon is serious, has reduced extraction efficiency, has prolonged the extraction time, has increased energy consumption, and cost is increased, and quality product is very not satisfactory.
The purpose of this invention is to provide a kind of supercritical CO 2The back extraction method, the technology of extraction hop extract from pellet hop.The characteristics of this technology are in the multilayer barrel of the pellet hop patent No. ZL99201463.8 that is contained in the inventor, carry out supercritical CO 2Oppositely (in the extraction kettle from top to bottom) flows, and promptly adopts the technical process of the inventor's number of patent application CN-00121565.5, extracts hop extract under the temperature of setting, pressure.The advantage of this technology is: 1, the multilayer barrel makes material bed pressure distribution even, and pressure reduction is little, no air-teturning mixed phenomenon, and mass transfer is fast, the efficient height.2, CO 2Back extraction, the time is short, and energy efficiency is remarkable, is fit to suitability for industrialized production.
Embodiment of the present invention are as follows:
Shown in the processing unit schema that Fig. 1 extracts hop extract: will be crushed to 1-1.2mm, remove the pellet hop of dust, install to the multilayer barrel, put into extraction kettle (E1, E2, E3), open the reverse flow valves V10 of control E1, E2, V13, V14, V17 and corresponding V4, V7, V23 and V25 carry out E1, the extraction of E2 differential concatenation.The processing condition of extraction are: starting heater H 1, a few C02 pump of H2 P1, to make extraction kettle pressure be 22 ± 2MPa, 58 ± 2 ℃ of temperature, and separating still A1 pressure is 5 ± 1MPa, temperature 20-25 ℃, CO 2Flow velocity 3-5Kg/Kg.Hr extracted after 2-4 hour, and separating still A1 emits hop extract, sampling analysis.Then, stream switches to E2, the extraction of E3 differential concatenation: close V4, V7, V23, E1 unloads charging; Open V18, V21 and V5, V8, V24.And the like, carry out two still differential concatenation continuous extractions.
Advantage of the present invention: 1, equipment flowsheet is simple, only increases valve, pipeline and just can carry out reverse continuous extraction, and percentage extraction obviously improves.2, the multilayer barrel makes material bed pressure distribution even, and pressure reduction is little, no air-teturning mixed phenomenon, and mass transfer is fast, the efficient height.3, good product quality keeps the whole effective constituents of hops, and is free from environmental pollution, significantly energy-saving and cost-reducing.
Following preferred embodiment describes supercritical CO in detail in conjunction with Fig. 1 2Oppositely extract the technology of hop extract, but do not mean that and limit the scope of the invention.
Embodiment 1, the supercritical CO of hop extract 2Oppositely extract.The 100Kg pellet hop that is crushed to 1-1.2mm, removes dust is installed to the multilayer barrel, put into extraction kettle (E1, E2, E3), start heater H 1, H2, refrigerator H3, H4 are to design temperature, open control E1, E2 differential concatenation flow valves V10, V13, V14, V17 and corresponding V4, V7, V23 and V25 carry out E1, the extraction of E2 differential concatenation.The processing condition of extraction are: start heater H 1, several CO of H2 2It is 22MPa that pump P1 makes extraction kettle pressure, 58 ℃ of temperature, and separating still A1 pressure is 5MPa, 20 ℃ of temperature, CO 2Flow velocity 4Kg/Kg.Hr extracted after 2.5 hours, and separating still A1 emits 13.6Kg hop extract, sampling analysis.Then, stream switches to E2, the extraction of E3 differential concatenation: promptly close V4, V7, V23, E1 unloads charging; Open V18, V21 and V5, V8, V24; Carry out two still differential concatenation continuous extractions.And the like carry out oppositely two stills series connection continuous extractions.The analysis of product is undertaken by GB GB-10347.1-10347.2-89 method.Measured the content of alpha-acid, β-acid in pellet hop, the hop extract, hop extract yield 13.6%, other data are as follows:
Title Alpha-acid % β-sour %
Pellet hop is formed ????7.06 ????3.74
Hop extract is formed ????41.0 ????32.0
The hop extract yield ????92.8 ????95.1
Fig. 1 is a processing unit schema of the present invention.
Among the figure, A1, A2, B1, B2 separating still, the C condenser, E1, E2, E3 extraction kettle, H1, H2 well heater, H3, H4 refrigerator, K diaphragm type compressor, M properties-correcting agent groove, P1, P2 high-pressure pump, P3 properties-correcting agent pump, T carbon dioxide storage tank, V4~V6 high pressure stream valve, V7~V9 series-parallel connection valve, V10~V13, V14~V17, three groups of flow valves of V18~V21, V22~V24 extractor valve, V25 adjustable needle valve, V26~V28 CO 2Reclaim ball valve, V29~V31 blow-off valve, V32~V34 discharging slag valve.

Claims (1)

1, a kind of supercritical CO 2The back extraction method is extracted the technology of hop extract from pellet hop, it is characterized in that: shown in the processing unit schema that Fig. 1 extracts hop extract: will be crushed to 1-1.2mm, remove the pellet hop of dust, install to the multilayer barrel, put into extraction kettle (E1, E2, E3), open the reverse flow valves V10 of control E1, E2, V13, V14, V17 and corresponding V4, V7, V23 and V25 carry out E1, the extraction of E2 differential concatenation.The processing condition of extraction are: start heater H 1, several CO of H2 2It is 22 ± 2MPa that pump P1 makes extraction kettle pressure, 58 ± 2 ℃ of temperature, and separating still A1 pressure is 5 ± 1MPa, temperature 20-25 ℃, CO 2Flow velocity 3-5Kg/Kg.Hr extracted after 2-4 hour, and separating still A1 emits hop extract, sampling analysis.Then, stream switches to E2, the extraction of E3 differential concatenation: close V4, V7, V23, E1 unloads charging; Open V18, V21 and V5, V8, V24.And the like, carry out two still differential concatenation continuous extractions.
CN 00133516 2000-11-09 2000-11-09 Process for extracting hop extract from hop particles by back extraction with supercritical CO2 Expired - Fee Related CN1100865C (en)

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CN 00133516 CN1100865C (en) 2000-11-09 2000-11-09 Process for extracting hop extract from hop particles by back extraction with supercritical CO2

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CN 00133516 CN1100865C (en) 2000-11-09 2000-11-09 Process for extracting hop extract from hop particles by back extraction with supercritical CO2

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7144590B2 (en) * 2003-01-09 2006-12-05 Lipoprotein Technologies, Inc. Bioactive compositions derived from humulus lupulus
CN100432201C (en) * 2005-05-11 2008-11-12 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
CN101138418B (en) * 2007-10-16 2010-08-11 浙江大学 Hop supercritical residues comprehensive utilization method
CN109329595A (en) * 2018-10-29 2019-02-15 齐鲁工业大学 A kind of application of hop product substitute antibiotics on feed addictive

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7144590B2 (en) * 2003-01-09 2006-12-05 Lipoprotein Technologies, Inc. Bioactive compositions derived from humulus lupulus
US7279186B2 (en) 2003-01-09 2007-10-09 Lipoprotein Technologies, Inc. Methods of administering anti-inflammatory cyclooxygenase-2 selective inhibitors
CN100432201C (en) * 2005-05-11 2008-11-12 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
CN101138418B (en) * 2007-10-16 2010-08-11 浙江大学 Hop supercritical residues comprehensive utilization method
CN109329595A (en) * 2018-10-29 2019-02-15 齐鲁工业大学 A kind of application of hop product substitute antibiotics on feed addictive

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