CN102492663B - Pure draft beer film cleaning and regenerating enzyme preparation and cleaning method using same - Google Patents

Pure draft beer film cleaning and regenerating enzyme preparation and cleaning method using same Download PDF

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CN102492663B
CN102492663B CN201110393743.6A CN201110393743A CN102492663B CN 102492663 B CN102492663 B CN 102492663B CN 201110393743 A CN201110393743 A CN 201110393743A CN 102492663 B CN102492663 B CN 102492663B
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cleaning
enzyme
membrane filtration
filtration system
regeneration
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CN102492663A (en
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蒙健宗
郑翔鹏
李晓明
梁树华
马少敏
张云光
韦函忠
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BANGERKE BIOLOGICAL TECHNOLOGY Co Ltd NANNING
Guangxi University
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BANGERKE BIOLOGICAL TECHNOLOGY Co Ltd NANNING
Guangxi University
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Abstract

The invention discloses a pure draft beer film cleaning and regenerating enzyme preparation and a cleaning method using the same. The film cleaning and regenerating enzyme preparation designed according to the pure draft beer film plug substance composition comprises the following components: cleaning and regenerating enzyme I: 40-80% of pentosan enzyme (10000U/g), 10-50% of beta-glucanase (20000U/g) and 2-20% of mannase (10000U/g); and cleaning and regenerating enzyme II: 40-80% of proline endoproteinase (5U/g) and 20-60% of neutral proteinase (100000U/g). The optimized pure draft beer film cleaning and regenerating method comprises the following steps: conventional water washing and alkaline-process cleaning; cyclic cleaning by an enzyme process while keeping the temperature; impregnated cleaning by an enzyme process; water washing; alkaline-process cleaning; and integrity testing. The film cleaning and regenerating enzyme disclosed by the invention effectively solves the problem of film flux depression caused by the pure draft beer film plug substance, and enhances the film regeneration power and pure draft beer filtration capacity by more than 35%.

Description

A kind of draft beer film cleaning and regeneration zymin and purging method
Technical field
The invention belongs to field of fermentation engineering, relate to beer fermentation production industry, specifically a kind of draft beer film cleaning and regeneration zymin and purging method.
Background technology
In the production of draft beer, adopt low temp. micro-porous membrane filtration degerming technique to replace traditional Chitral fever sterilization process, make the taste of beer fresher, pure, being rich in nutrition, be deeply subject to human consumer's favor.The key of draft beer production technology is non-contaminant brew, sterile filtration and sterile filling, and filtering with microporous membrane technology is the core that draft beer is produced.The membrane filtration system of draft beer, the general employing of brew-house both at home and abroad is at present thick, two cover filtering systems are filtered pure mellow wine eventually, utilize its meticulous physical filtering characteristic (coarse filtration 0.65 μ m, filter eventually 0.45 μ m), cereuisiae fermentum in wine liquid, harmful microorganism and a part of albumen polyphenol etc. are intercepted and filtered, guarantee biology and the non-biostability of draft beer, thereby guarantee nutrition, quality and the flavor stability of beer.Owing to existing some films to block up material in beer fermentation liquid, stop up the film forming after fenestra and pollute filtyration velocity and the wine liquid filtrable volume that can greatly reduce film.In order to reduce film blockage problem, draft beer fermentation generally takes to select expensive Australia wheat, add the high-quality Fructus Hordei Germinatus such as wheat brewages, and for the feature of draft beer raw material, Mashing process is controlled, the content of minimizing hemicellulose etc. is to lower the impact that film is stopped up; When pure mellow wine filters, also by assist the filtration of filter membrane with diatomite, silica gel and PVPP, after membrane filtration is produced, also must there is cleaning and regeneration technique, clean and remove the tamper in fenestra, membrane flux regeneration is recovered.Film cleaning and regeneration technique mainly contains 1. Physical and cleans: as hot-water process, sponge ball ablution, backpressure flushing and circulation cleaning etc.; 2. chemical method: acid/alkali cleans; 3. mechanical curettage method etc.At present in the production of draft beer, cleaning and regeneration technique after membrane filtration finishes is mainly used chemical method, first use water rinse, remove the impurity such as the protein that is attached on film, hop resin, then with warm water, thermokalite, hot water, cold water, clean and regenerate in order.But its membrane flux just declines rapidly after a certain amount of wine liquid of filtering with microporous membrane, and regeneration efficiency is very poor to adopt above chemical method cleaning and regeneration technique, need to change film to reach filtration requirement.The membrane filtration system that each brew-house is equipped with is at present more with the product of import Sartorius, Pall and Seitz company, and the more about 20-40 of the new filtering membrane of transducer set is ten thousand yuan, causes the running cost of draft beer higher.
The cleaning and regeneration of film, except washing away the pollutent that is adsorbed on face and fenestra with chemical reagent such as acid, alkali, tensio-active agents, for macromolecular pollutent, can also be hydrolyzed into small molecules with corresponding enzyme, lower absorption and the ponding of pollutent, and then be easy to clean and remove from face and fenestra.Enzyme process cleans and can make film properties recovery extent high, and can not cause any infringement to film, and this has obtained application in some emerging membrane concentration, membrane sepn industry.As Chinese patent CN 100503818C has invented a kind of ultra-filtration membrane cleaning of enzyme for garden spgarden stuff ultrafiltration concentration process and has improved the production method of ultra-filtration membrane flux, for the principal pollutant composition pectin in garden spgarden stuff membrane filtration, Mierocrystalline cellulose, hemicellulose, protein etc., the components such as polygalacturonase, cellulase, hemicellulase, proteolytic enzyme have been designed, the delay material that decomposes film surface, improve chemical cleaning performance, improve membrane flux, solve juice concentration and produced the upper ultra-filtration membrane obstruction occurring, film pollutes, the problem that film processing power reduces.Chinese patent CN 101457182B has invented a kind of liquid membrane clean-out system that contains proteolytic enzyme, for mainly containing organic pollutants, it is the separated cleaning with ceramic membrane of protein-based macromolecular bio-fermented liquid, not only shorten scavenging period, can also slow down the decline of membrane flux speed, reduced cleaning frequency.Some research reports also show, clean the ceramic membrane being polluted by soy sauce, erythromycin, creatinine fermented liquid with trypsin solution, can shorten scavenging period than acid/alkali washing out method, improve filtrate flux.
Summary of the invention
The object of the invention is, for the stifled material of macromole film main in draft beer membrane filtration, provides the combination of the enzyme component of the stifled material of these films of hydrolyzable, and being effectively hydrolyzed macromole is small segment, is easy to clean and remove from face and fenestra; And a kind of enzyme process and chemical method combination are provided, and make draft beer filter membrane membrane flux after production can there is good regeneration recovery effects, improve the filter wine ability of film.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
1. the zymin for draft beer film cleaning and regeneration is comprised of cleaning and regeneration enzyme I and cleaning and regeneration enzyme II;
1) cleaning and regeneration enzyme I is comprised of pentosanase, beta-glucanase and mannase, its vigor scope is: if the enzyme activity of pentosanase is in 10000U/g, the enzyme activity of beta-glucanase is in 20000U/g, the enzyme activity of mannase is with 10000U/g timing, and the mass percent of pentosanase, beta-glucanase and mannase is as follows:
Pentosanase 40-80%
Beta-glucanase 10-50%
Mannase 2-20%
2) cleaning and regeneration enzyme II is comprised of proline(Pro) endo-protease and neutral protease, its vigor scope is: if the enzyme activity of proline(Pro) endo-protease is in 5U/g, the enzyme activity of neutral protease is with 100000U/g timing, and the mass percent of proline(Pro) endo-protease and neutral protease is as follows:
Proline(Pro) endo-protease 40-80%
Neutral protease 20-60%
Each component of draft beer film cleaning and regeneration enzyme of the present invention, by microorganism fermentation, produce, the hygienic requirements of each component all meets the foodstuffs industry of China < < food safety national standard and uses zymin > > (GB 255942010) or Food and Argriculture OrganizationFAO and the foodstuff additive joint specialist council of the World Health Organization (JECFA), U.S. food chemistry code (FCC) about food-processing, to use the hygienic requirements of zymin.The gene of pentosanase can derive from aspergillus niger, Li Shi wood is mould, viride, the thermophilic hyphomycete of cotton shape, pichia spp, lonely humicola lanuginosa, subtilis, aspergillus oryzae etc., the gene source of beta-glucanase can be Bacillus licheniformis, lonely humicola lanuginosa, breathe out time wood mould, aspergillus niger, subtilis, Li Shi wood is mould, bacillus amyloliquefaciens, viride, Disporotrichum dimorphosporum, Talaromyces emersonii etc., the gene source of mannase can derive from subtilis, aspergillus niger, Li Shi wood is mould, streptomycete etc., the gene source of proline(Pro) endo-protease can derive from aspergillus niger, point-like aerogenesis Zymomonas mobilis, Xanthomonas campestris etc., the gene source of neutral protease can derive from subtilis etc., but be all not limited to above bacterial strain.
2. the enzyme process film cleaning and regeneration method of carrying out after draft beer membrane filtration, carry out according to the following steps:
1) conventional washing and alkaline process clean
(1) in alkali liquid tank, prepare 55 ℃ of hot water (approximately 75% liquid level), squeeze into membrane filtration system insulation circulation 30 minutes.
(2) residual water in membrane filtration system and pipeline is emptying, suitably carry out standby pressure and put; Squeeze into again 55 ℃ of hot water, be full of filter, soak approximately 40 hours.
(3) soak solution of membrane filtration system is emptying, at membrane filtration system service platform, set with approximately 2 tons of cold water flush membrane filtration systems.
(4) CIP system is manually controlled and is carried out cold water flush alkali tank 5 minutes, emptying draining.
(5) preparation alkaline cleaner, pH value 10-12, enters membrane filtration system alkali playback processing program.
(6) by system program, carry out integrity test.
2) cleaning and regeneration enzyme I cleans
(1) take film cleaning and regeneration enzyme I 0.5-2.0kg, by the 45 ℃ of abundant stirring and dissolving of warm water in 5L left and right.
(2) get clean gauze and be folded into respectively 4,8,16 layers, above-mentioned film cleaning and regeneration enzyme I solution is filtered to clearly step by step.
(3) step (2) is filtered to clean bucket splendid attire for film cleaning and regeneration enzyme I solution clearly, and is placed in 4 ℃ of following cryopreservation to using, the time is no more than 3 days.
(4) alkaline cleaning fluid in emptying CIP system alkali liquid tank is neutral by cold water flush to pH detection paper.
(5) in alkali liquid tank, prepare 55 ℃ of hot water, the clarification film regeneration enzyme I solution of preservation is added in hot water, hot water amount makes 1000 times of enzyme liquid dilutions, insulation circulation 30 minutes.
(6) residual water in membrane filtration system and pipeline is emptying, the enzyme liquid of step (5) dilution is squeezed in membrane filtration system, suitably carry out standby pressure and put, guarantee to be full of Membrane filtering machine, soak 12-40 hour (without reheating).
3) cleaning and regeneration enzyme II cleans
(1) take film cleaning and regeneration enzyme II 0.5-2.0kg, add 37 ℃ of abundant stirring and dissolving of warm water of 5L.
(2) scavenging solution in emptying CIP system alkali liquid tank is neutral by cold water flush to pH detection paper.
(3) in alkali liquid tank, prepare 37 ℃ of hot water, during the clarification film regeneration enzyme solution of preservation is added, hot water amount makes 2000 times of enzyme liquid dilutions, insulation circulation 30 minutes.
(4) residual water in membrane filtration system and pipeline is emptying, the enzyme liquid of step (3) dilution is squeezed in membrane filtration system, suitably carry out standby pressure and put, guarantee to be full of Membrane filtering machine, soak 12-40 hour (without reheating); After immersion finishes, carry out sterile sampling bacterial detection content.
4) washing
Step 3) soak solution of membrane filtration system is emptying after finishing, at membrane filtration system service platform, set with 2-10 ton cold water flush membrane filtration system.
5) alkaline cleaner circulation:
Preparation alkaline cleaner, pH value 10-12, enters membrane filtration system alkali playback processing program, and hot water and alkali lye are heated to 55-60 ℃, select the line that will regenerate to clean on membrane filtration system operating panel.After having regenerated, membrane filtration system carries out integrity test automatically; By watching integrity test situation on operating panel, Δ P < 70mbar.If Δ P >=70mbar can rinse for several times repeatedly with cold water, until pressure reduction lowers as far as possible.
6) integrity test:
10 minutes integrity test time, after filter core is wetting, at 20 ℃ ± 5 ℃, carry out integrity test.With pressurized air or nitrogen, to strainer, apply the positive pressure of 3bar, in this process, by pressure, the water in strainer is discharged from testing valve, open wash water valve by whole residuary water emptyings; Slowly strainer pressure is risen to the test pressure of 1.2bar, then close gas feed valve, wait for and make it reach steady state in 5 minutes.
Advantage of the present invention is: use draft beer film cleaning and regeneration enzyme of the present invention and purging method, can significantly improve the regeneration restorability of film, extend the work-ing life of film, improve the filter capacity for liquor of every cover microfiltration membrane more than 35%, save the use cost of film.
Embodiment
For realizing the present invention, to test in advance, the filter membrane after draft beer membrane filtration is produced is dissected, collection membrane blocks up material, analyze its main component and character thereof, and with the reaction that is hydrolyzed of multiple enzyme, therefrom screen enzyme and the working concentration thereof the stifled material of film to good hydrolytic effect.Experimental study shows, the macromole film stifled material of draft beer membrane filtration in producing, mainly comprises protein and protein-polyphenolic substance, piperylene, beta-glucan etc.
Isolated alcohol soluble substance from the stifled material of draft beer film is mainly protein and protein-polyphenolic substance.These protein are hordeins of proline rich, existence due to five yuan of pyrrole ring structures of proline(Pro), on amino proline nitrogen before protein peptide bond, lack a hydrogen atom, make the ketonic oxygen before ring structure become strong hydrogen atom acceptor, derive from like this polyphenols of Fructus Hordei Germinatus and hops not only by hydrophobic interaction and polymerization of protein, also by the region of hydrogen bond and protein,alcohol-soluble proline rich, further stablize the polymerization between them.These stable polymkeric substance are easily separated out, are deposited in face and fenestra when face forms concentration polarization, have formed the important sources that draft beer film pollutes.Proline(Pro) endo-protease is the carboxy-terminal peptide bond site of proline residue in specificity hydrolyzed peptide, the protein of these proline rich in draft beer filter membrane and protein-polyphenol polymer can be hydrolyzed to small peptide more fully, reduce the polymerization that protein and polyphenol form, thereby be easy to clean and remove from face and fenestra; The neutral protease that restriction enzyme site specificity is lower also can have good effect.And other proteolytic enzyme, if the main site of papain hydrolysis protein is that next amino acid is the position of arginine residues, the site of trypsin hydrolyzing protein is by Methionin, the peptide bond that arginic carboxyl forms, Chymotrypsin is mainly identified the phenylalanine in peptide chain, the die aromatischen Aminosaeuren residues such as tyrosine, the recognition site of elastoser is the α-amino-isovaleric acid in peptide chain, leucine, the aliphatic amino acid residues such as Serine, tyrosine is identified and cut off to stomach en-, the N-terminal peptide bond such as phenylalanine, neither can be hydrolyzed well protein and the protein-polyphenol polymer of proline rich.
Isolated polysaccharose substance from the stifled material of draft beer film, be mainly derive from Fructus Hordei Germinatus but in saccharifying, fail the hemicellulose class of fully degraded as piperylene, beta-glucan etc., and derive from mannosans that the beer fermentation later stage produces during yeast autolysis etc.These saccharan materials are when draft beer membrane filtration, the shearing force that mash motion forms can be expanded saccharan molecule random in mash, No-L aw Order, be bound up, by hydrogen bond, form saccharan colloidalmaterial, in membrane filtration processes by concentration polarization and film pollution deposit in film surface and fenestra.These saccharans can be hydrolyzed into micromolecular sugar by corresponding pentosanase, beta-glucanase, mannase etc., are easy to clean and remove from face and fenestra.
Below in conjunction with embodiment, the present invention will be further described.
The raw materials such as pentosanase of the present invention, beta-glucanase, mannonase proline(Pro) endo-protease, neutral protease all can be bought by commercially available mode.
Embodiment 1
In a certain draft beer production, preparation and the film of cleaning and regeneration enzyme clean
Raw material forms: cleaning and regeneration enzyme I, cleaning and regeneration enzyme II.
Cleaning and regeneration enzyme I:
Pentosanase 375g, beta-glucanase 100g, mannase 25g.
Preparation method: pentosanase, beta-glucanase, mannase are mixed by machinery according to the above ratio under gnotobasis.
Cleaning and regeneration enzyme II:
Proline(Pro) endo-protease 250g, neutral protease 250g.
Preparation method: by proline(Pro) endo-protease, neutral protease under gnotobasis according to the above ratio by being mixed.
Film cleans:
A set of millipore filtration (0.45 μ m, 750mm, 36) is by production requirement filtered pure unpasteurized beer, and then soda acid cleaning way is regenerated routinely: in alkali liquid tank, prepare 55 ℃ of hot water, squeeze into membrane filtration system insulation circulation 30 minutes; Residual water in membrane filtration system and pipeline is emptying, carry out standby pressure and put, then squeeze into 55 ℃ of hot water, guarantee to be full of filter, soak 40 hours; The soak solution of membrane filtration system is emptying, at membrane filtration system service platform, set with 2 tons of cold water flush membrane filtration systems; CIP system is manually controlled and is carried out cold water flush alkali tank 5 minutes, emptying draining; Preparation alkaline cleaner, enters membrane filtration system alkali playback processing program.
Getting film cleaning and regeneration enzyme I 0.5kg, is the abundant stirring and dissolving of warm water of 45 ℃ by 5L temperature, is filtered to limpid; Alkaline cleaning fluid in emptying CIP system alkali liquid tank is 6.8-7.2 by 5-8 ℃ of cold water flush to pH detection paper; Residual water in membrane filtration system and pipeline is emptying, above-mentioned enzyme liquid is squeezed in membrane filtration system, with 0.2kg pressure, carry out standby pressure and put, guarantee to be full of Membrane filtering machine, soak 30 hours;
Get film cleaning and regeneration enzyme II 0.5kg, add 5L temperature and be the abundant stirring and dissolving of warm water of 37 ℃, be filtered to limpid; Scavenging solution in emptying CIP system alkali liquid tank is 6.8-7.2 by 5-8 ℃ of cold water flush to pH detection paper; Residual water in membrane filtration system and pipeline is emptying, above-mentioned enzyme liquid is squeezed in membrane filtration system, with 0.2kg pressure, carry out standby pressure and put, guarantee to be full of Membrane filtering machine, soak 30 hours, after immersion finishes, carry out sterile sampling bacterial detection content.
After sampling, the soak solution of membrane filtration system is emptying, at membrane filtration system service platform, set with 5 tons of cold water flush membrane filtration systems, after alkaline cleaner circulates by integrity test.Result is as shown in table 1.
Table 1 conventional chemical cleaning and regeneration effect
Wash number Unit surface filtration yield (hL/10 inch filter core)
1 412
2 436
3 429
4 456
5 421
6 400
7 403
On average 425
A set of millipore filtration (0.45 μ m, 750mm, 36), by production requirement filtered pure unpasteurized beer, is then regenerated by cleaning and regeneration enzyme purging method of the present invention, and result is as shown in table 2.
Table 2 enzyme process cleaning and regeneration effect
Wash number Unit surface filtration yield (hL/10 inch filter core)
1 612
2 579
3 573
4 616
5 580
6 601
7 590
On average 580
Embodiment 2
In another draft beer production, preparation and the film of cleaning and regeneration enzyme clean
Raw material forms: cleaning and regeneration enzyme I, cleaning and regeneration enzyme II.
Cleaning and regeneration enzyme I:
Pentosanase 375g, beta-glucanase 200g, mannase 25g.
Preparation method: pentosanase, beta-glucanase, mannase are mixed by machinery according to the above ratio under gnotobasis.
Cleaning and regeneration enzyme II:
Proline(Pro) endo-protease 300g, neutral protease 200g.
Preparation method: by proline(Pro) endo-protease, neutral protease under gnotobasis according to the above ratio by being mixed.
Production test:
A set of millipore filtration (0.45 μ m, 750mm, 36) is by production requirement filtered pure unpasteurized beer, and then soda acid cleaning way is regenerated routinely: in alkali liquid tank, prepare 55 ℃ of hot water, squeeze into membrane filtration system insulation circulation 30 minutes; Residual water in membrane filtration system and pipeline is emptying, carry out standby pressure and put, then squeeze into 55 ℃ of hot water, guarantee to be full of filter, soak 40 hours; The soak solution of membrane filtration system is emptying, at membrane filtration system service platform, set with 2 tons of cold water flush membrane filtration systems; CIP system is manually controlled and is carried out cold water flush alkali tank 5 minutes, emptying draining; Preparation alkaline cleaner, enters membrane filtration system alkali playback processing program.
Get film cleaning and regeneration enzyme I 0.6kg, with 45 ℃ of abundant stirring and dissolving of warm water of 4.5L, be filtered to limpid; Alkaline cleaning fluid in emptying CIP system alkali liquid tank is 6.8-7.2 by 5-8 ℃ of cold water flush to pH detection paper; Residual water in membrane filtration system and pipeline is emptying, above-mentioned enzyme liquid is squeezed in membrane filtration system, with 0.2kg pressure, carry out standby pressure and put, guarantee to be full of Membrane filtering machine, soak 25 hours;
Get film cleaning and regeneration enzyme II 0.5kg, add the 4.5L37 ℃ of abundant stirring and dissolving of warm water, be filtered to limpid; Scavenging solution in emptying CIP system alkali liquid tank is 6.8-7.2 by 5-8 ℃ of cold water flush to pH detection paper; Residual water in membrane filtration system and pipeline is emptying, above-mentioned enzyme liquid is squeezed in membrane filtration system, with 0.2kg pressure, carry out standby pressure and put, guarantee to be full of Membrane filtering machine, soak 25 hours, after immersion finishes, carry out sterile sampling bacterial detection content.
After sampling, the soak solution of membrane filtration system is emptying, at membrane filtration system service platform, set with 5 tons of cold water flush membrane filtration systems, after alkaline cleaner circulates by integrity test.Result is as shown in table 3.
Table 3 conventional chemical cleaning and regeneration effect
Wash number Unit surface filtration yield (hL/10 inch filter core)
1 400
2 421
3 423
4 400
5 439
6 398
7 411
On average 410
A set of millipore filtration (0.45 μ m, 750mm, 36), by production requirement filtered pure unpasteurized beer, is then regenerated by cleaning and regeneration enzyme purging method of the present invention, and result is as shown in table 4.
Table 4 enzyme process cleaning and regeneration effect
Wash number Unit surface filtration yield (hL/10 inch filter core)
1 654
2 590
3 600
4 590
5 605
6 640
7 578
On average 576
Embodiment 3
In another draft beer production, preparation and the film of cleaning and regeneration enzyme clean
Raw material forms: cleaning and regeneration enzyme I, cleaning and regeneration enzyme II.
Cleaning and regeneration enzyme I:
Pentosanase 315g, beta-glucanase 315g, mannase 70g.
Preparation method: pentosanase, beta-glucanase, mannase are mixed by machinery according to the above ratio under gnotobasis.
Cleaning and regeneration enzyme II:
Proline(Pro) endo-protease 375g, neutral protease 125g.
Preparation method: by proline(Pro) endo-protease, neutral protease under gnotobasis according to the above ratio by being mixed.
Production test:
A set of millipore filtration (0.45 μ m, 750mm, 36) is by production requirement filtered pure unpasteurized beer, and then soda acid cleaning way is regenerated routinely: in alkali liquid tank, prepare 55 ℃ of hot water, squeeze into membrane filtration system insulation circulation 30 minutes; Residual water in membrane filtration system and pipeline is emptying, carry out standby pressure and put, then squeeze into 55 ℃ of hot water, guarantee to be full of filter, soak 40 hours; The soak solution of membrane filtration system is emptying, at membrane filtration system service platform, set with 2 tons of cold water flush membrane filtration systems; CIP system is manually controlled and is carried out cold water flush alkali tank 5 minutes, emptying draining; Preparation alkaline cleaner, enters membrane filtration system alkali playback processing program.
Get film cleaning and regeneration enzyme I 0.7kg, by 45 ℃ of abundant stirring and dissolving of warm water of 4.5L, be filtered to limpid; Alkaline cleaning fluid in emptying CIP system alkali liquid tank is 6.8-7.2 by 5-8 ℃ of cold water flush to pH detection paper; Residual water in membrane filtration system and pipeline is emptying, above-mentioned enzyme liquid is squeezed in membrane filtration system, with 0.2kg pressure, carry out standby pressure and put, guarantee to be full of Membrane filtering machine, soak 20 hours;
Get film cleaning and regeneration enzyme II 0.5kg, add the 4.5L37 ℃ of abundant stirring and dissolving of warm water, be filtered to limpid; Scavenging solution in emptying CIP system alkali liquid tank is 6.8-7.2 by 5-8 ℃ of cold water flush to pH detection paper; Residual water in membrane filtration system and pipeline is emptying, above-mentioned enzyme liquid is squeezed in membrane filtration system, with 0.2kg pressure, carry out standby pressure and put, guarantee to be full of Membrane filtering machine, soak 20 hours, after immersion finishes, carry out sterile sampling bacterial detection content.
After sampling, the soak solution of membrane filtration system is emptying, at membrane filtration system service platform, set with 5 tons of cold water flush membrane filtration systems, after alkaline cleaner circulates by integrity test.Result is as shown in table 5.
Table 5 conventional chemical cleaning and regeneration effect
Wash number Unit surface filtration yield (hL/10 inch filter core)
1 400
2 413
3 400
4 420
5 400
6 380
7 401
On average 405
A set of millipore filtration (0.45 μ m, 750mm, 36), by production requirement filtered pure unpasteurized beer, is then regenerated by cleaning and regeneration enzyme purging method of the present invention, and result is as shown in table 6.
Table 6 enzyme process cleaning and regeneration effect
Wash number Unit surface filtration yield (hL/10 inch filter core)
1 600
2 570
3 571
4 580
5 560
6 581
7 571
On average 561
Above-described embodiment be the present invention's concrete application preferably in draft beer is produced, but concrete technology contents of the present invention and application is not subject to the limitation of embodiment.

Claims (1)

1. the enzyme process film cleaning and regeneration method of carrying out after draft beer membrane filtration, carry out according to the following steps:
1) conventional washing and alkaline process clean
(1) in alkali liquid tank, prepare 55 ℃ of hot water of 75% liquid level of tank, squeeze into membrane filtration system insulation circulation 30 minutes;
(2) residual water in membrane filtration system and pipeline is emptying, suitably carry out standby pressure and put; Squeeze into again 55 ℃ of hot water and be full of filter, soak 40 hours;
(3) soak solution of membrane filtration system is emptying, at membrane filtration system service platform, set with 2 tons of cold water flush membrane filtration systems;
(4) CIP system is manually controlled and is carried out cold water flush alkali tank 5 minutes, emptying draining;
(5) preparation alkaline cleaner, pH value 10-12, enters membrane filtration system alkali playback processing program;
(6) by system program, carry out integrity test;
2) cleaning and regeneration enzyme I is cleaned
Cleaning and regeneration enzyme I is comprised of pentosanase, beta-glucanase and mannase, its vigor scope is: the enzyme activity of pentosanase is in 10000U/g, the enzyme activity of beta-glucanase is in 20000U/g, the enzyme activity of mannase is in 10000U/g, and the mass percent of pentosanase, beta-glucanase and mannase is as follows:
Pentosanase 40-80%
Beta-glucanase 10-50%
Mannase 2-20%;
(1) take cleaning and regeneration enzyme I 0.5-2.0kg, by the 1L-10L45 ℃ of abundant stirring and dissolving of warm water;
(2) getting clean gauze is filtered to above-mentioned cleaning and regeneration enzyme I solution clearly step by step;
(3) step (2) is filtered to clean bucket splendid attire for cleaning and regeneration enzyme I solution clearly, and is placed in 4 ℃ of following cryopreservation to using, the time is no more than 3 days;
(4) alkaline cleaning fluid in emptying CIP system alkali liquid tank is neutral by cold water flush to pH detection paper;
(5) in alkali liquid tank, prepare 55 ℃ of hot water, the cleaning and regeneration enzyme I solution of the clarification of preservation is added in hot water, hot water amount makes 1000 times of enzyme liquid dilutions, insulation circulation 30 minutes;
(6) residual water in membrane filtration system and pipeline is emptying, the enzyme liquid of step (5) dilution is squeezed in membrane filtration system, suitably carry out standby pressure and put, guarantee to be full of Membrane filtering machine, soak 12-40 hour;
3) cleaning and regeneration enzyme II is cleaned
Cleaning and regeneration enzyme II is comprised of proline(Pro) endo-protease and neutral protease, its vigor scope is: the enzyme activity of proline(Pro) endo-protease is in 5U/g, the enzyme activity of neutral protease is in 100000U/g, and the mass percent of proline(Pro) endo-protease and neutral protease is as follows:
Proline(Pro) endo-protease 40-80%
Neutral protease 20-60%;
(1) take cleaning and regeneration enzyme II 0.5-2.0kg, add the 5L37 ℃ of abundant stirring and dissolving of warm water;
(2) scavenging solution in emptying CIP system alkali liquid tank is neutral by cold water flush to pH detection paper;
(3) in alkali liquid tank, prepare 37 ℃ of hot water, the cleaning and regeneration enzyme II solution of the clarification of preservation is added wherein, hot water amount makes 2000 times of enzyme liquid dilutions, insulation circulation 30 minutes;
(4) residual water in membrane filtration system and pipeline is emptying, the enzyme liquid of step (3) dilution is squeezed in membrane filtration system, suitably carry out standby pressure and put, guarantee to be full of Membrane filtering machine, soak 12-40 hour; After immersion finishes, carry out sterile sampling bacterial detection content;
4) washing
Step 3) after finishing, the soak solution of membrane filtration system is emptying, at membrane filtration system service platform, set with 2-10 ton cold water flush membrane filtration system;
5) alkaline cleaner circulation
Preparation alkaline cleaner, pH value 10-12, enters membrane filtration system alkali playback processing program, and hot water and alkali lye are heated to 55-60 ℃, select the line that will regenerate to clean on membrane filtration system operating panel; After having regenerated, membrane filtration system carries out integrity test automatically; By watching integrity test situation on operating panel, should be △ P<70mbar, if △ P >=70mbar can rinse for several times repeatedly with cold water, until pressure reduction lowers;
6) integrity test
10 minutes integrity test time, after filter core is wetting, at 20 ℃ ± 5 ℃, carry out integrity test; With pressurized air or nitrogen, to strainer, apply the positive pressure of 3bar, in this process, by pressure, the water in strainer is discharged from testing valve, open wash water valve by whole residuary water emptyings; Slowly strainer pressure is risen to the test pressure of 1.2bar, then close gas feed valve, wait for and make it reach steady state in 5 minutes.
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CN103463992B (en) * 2013-09-30 2015-07-22 武汉钢铁(集团)公司 Cleaning fluid for water treatment ultrafiltration membranes
CN103816809A (en) * 2014-03-13 2014-05-28 孟州市华兴生物化工有限责任公司 Cleaning method for semipermeable membrane used for extracting amino acid from fermentation liquor
SG11201803587UA (en) 2015-11-20 2018-06-28 Emd Millipore Corp Enhanced stability filter integrity test
CN109603562A (en) * 2018-12-20 2019-04-12 武汉新华扬生物股份有限公司 A kind of enzyme preparation and its application method for beer filtration Membrane cleaning
FR3090423B1 (en) * 2018-12-21 2021-05-21 Ifp Energies Now PROCESS FOR CLEANING A LIGNOCELLULOSIC BIOMASS TREATMENT REACTOR
CN109589796B (en) * 2019-02-13 2020-09-01 中国科学院过程工程研究所 Membrane cleaning method in membrane sugar preparation process
CN113881645A (en) * 2020-07-02 2022-01-04 北京世城双清科技有限公司 Complex enzyme cleaning agent and application thereof

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CN101457182B (en) * 2009-01-08 2011-03-30 立宇化学技术(郑州)有限公司 Liquid enzyme film cleaning agent
CN102078770B (en) * 2010-12-02 2012-06-27 华南农业大学 Solid compound enzyme for cleaning filtering membrane of draught beer
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