CN109111043A - A kind of processing method of high-COD waste water with high salt - Google Patents
A kind of processing method of high-COD waste water with high salt Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/30—Extraction; Separation; Purification by precipitation
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- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/34—Extraction; Separation; Purification by filtration, ultrafiltration or reverse osmosis
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/24—Treatment of water, waste water, or sewage by flotation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/32—Nature of the water, waste water, sewage or sludge to be treated from the food or foodstuff industry, e.g. brewery waste waters
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
- C02F3/342—Biological treatment of water, waste water, or sewage characterised by the microorganisms used characterised by the enzymes used
Abstract
The present invention relates to a kind of processing method of high-COD waste water with high salt, it is specifically related to the high-COD waste water with high salt containing ingredients such as salt, albumen, fat generated in meat curing food service industry, belongs to water-treatment technology field.The present invention in the prior art cannot by meat pickling waste water resource reutilization, be not suitable for handle meat pickling waste water aiming at the problem that, meat pickling waste water can be effectively treated and can convert micromolecule polypeptide for protein therein by proposing one kind, the method as animal feed.
Description
Technical field
The present invention relates to a kind of processing methods of high-COD waste water with high salt, are specifically related in meat curing food service industry
The high-COD waste water with high salt containing ingredients such as salt, albumen, fat generated, belongs to water-treatment technology field.
Background technique
It is the mistake that addition nitrate, sugar and spice etc. are processed with salt or based on salt that meat is marinated
Journey.Marinated since ancient times is exactly a kind of antiseptic preservation means of meat products, and meat is marinated so far still generally uses.
Method for salting can be divided into dry salting, wet cure and salt water injection method.1) it does marinated method: being to mix salt and nitrate
It closes, rubs on meat surface, be then deposited in container, form saline solution by extravasation juice and carry out marinated method.This is one
The slow method for salting of kind, but pickled product has unique flavor and quality.China's famous product ham, bacon etc. are marinated using this method.
Since salting period is long, it is easy to cause the inside of meat rotten.Furthermore it pickles unevenly, dehydration is serious.2) wet cure: being to match
Salt water is made, meat is immersed in salt water and is pickled.Salt is dense when wet salting, is not less than 25%, nitre is not less than 1%.For
The loss of nutriment is reduced, old halogen pickled system is generally used, but it is rotten to must be prevented from brine.The color and flavor of wet salting product
Too late dry pickled product, and aqueous more unsuitable preservations.3) salt water injection method: being that salt water is injected into meat with syringe.This method
Marinated uniform, the time is short.But for its final product quality not as good as dry pickled product, flavor is slightly poor, and the degree of contraction of muscle also compares when cooking
Greatly.
For wet cure and salt water injection method, can generate largely containing animal protein, sodium chloride, fat it is useless
Water, being mainly characterized by for this kind of waste water be with high salt, high COD.In the prior art, the side of some above-mentioned waste water of processing has been disclosed
Method, such as patent CN103570177A disclose a kind of purification process technique of food service industry saliferous pickling waste water, including following
Step: (1) the bulky grain solid impurity in filtering removal saliferous pickling waste water；(2) heating promotes the protein in waste water to occur
Denaturation flocculation；(3) centrifuge separation removal flocculate；(4) small molecular weight impurity is removed with food processing aid Activated Carbon Adsorption Separation；
(5) filtering removal active carbon；This treatment process can effectively remove protein in saliferous pickling waste water, blood, hair, broken
The impurity such as meat, broken bone and fat.But above-mentioned technology is removed impurity therein simply by physicochemical method,
Still a large amount of industrial residue can be generated, can not by the animal protein effective component reuse again in pickling waste water, and this
Kind method uses chemical floc, and resulting in flocculant is contaminated salt water also, and salt can not reuse again.Patent
CN104150721A discloses a kind of recycling processing method of foodstuff pickling waste water, is obtained using pre-treatment separation waste water with high salt
Produce water and high-enriched organics concentrated water, production water with high salt passes through that reverse osmosis deaslination handles to obtain pure water and high concentration saliferous is dense first
Water；Organic matter concentrated water is diluted by the reverse osmosis obtained pure water, then through biochemical treatment and catalytic ozonation with
After removing organic matter, enter the reverse osmosis treatment after security personnel's filtering；But (implemented according to the record of the patent specification
Example 1-4) it is all to have handled preserved szechuan pickle waste water, for resistance to preserved szechuan pickle waste water compared with meat pickling process, water quality is entirely different, wherein hardly
It is largely salt containing protein and fat, if the high-COD waste water with high salt for meat curing process uses above-mentioned work
Reverse osmosis membrane, reverse osmosis membrane are fallen in skill processing, protein and the fat directly pollution that directly will lead in meat curing process waste water
It not can be carried out work completely, without industrial applicibility.
Summary of the invention
The present invention for CN103570177A in the prior art cannot by meat pickling waste water resource reutilization,
CN104150721A is not suitable for the problem of handling meat pickling waste water, and meat pickling waste water can be effectively treated by proposing one kind
And micromolecule polypeptide can be converted by protein therein, the method as animal feed.
A kind of processing method of high-COD waste water with high salt, the high-COD waste water with high salt is meat pickling waste water, described
Method includes the following steps:
S1: air-flotation process: air bearing is carried out to meat pickling waste water and removes impurity；
S2: coarse filtration: waste water obtained in S1 is filtered using coarse filter；
S3: extraction: filtrate obtained in S2 is extracted using petroleum ether, removal fat；
S4: it digests for the first time: the first protein enzyme enzymolysis processing being used to raffinate obtained in S3, obtains the first enzymolysis liquid；
S5: hyperfiltration treatment: hyperfiltration treatment is carried out to the first enzymolysis liquid obtained in S4, makes small molecular protein and polypeptide through ultrafiltration
Film；
S6: nanofiltration processing: divalent salts are added in the ultrafiltrated permeation liquid obtained in S5, then carry out nanofiltration processing, make small molecule egg
White and polypeptide and divalent salts are concentrated, and sodium chloride penetrates nanofiltration membrane；
S7: second digests: carrying out enzymolysis processing using the second protease to the nanofiltration concentrate that S6 is obtained, obtains the second enzymatic hydrolysis
Liquid；
S8: precipitating removes divalent salts: the second enzymolysis liquid obtained in step S7 removes divalent salts using adsorbent；
S9: dry: enzymolysis liquid obtained in S8 being concentrated, is dried, Gly-His-Lys are obtained.
Further, in the S1 step, the occurrence quantity of bubble per minute and the volume ratio of waste water can be 1:5~
10。
Further, in the S2 step, coarse filter be can be using quartz filter, manganese sand filter etc..
Further, in the S3 step, the volume ratio of extract liquor and waste water can be 1:10~15, and extraction time can
To be 30~60min.
Further, in the S4 step, the first protein enzyme can be alkali protease, trypsase, Papain
Enzyme etc., in enzymolysis process, temperature is 40~60 DEG C, and enzymolysis time can be 50~100min.
Further, in the S5 step, for ultrafiltration retaining molecular weight in 30~500,000 Da, the pressure of ultra-filtration process can
To be 0.05~0.5Mpa.
Further, in the S6 step, divalent salts refer to Mg2+、Ca2+Or Zn2+Chloride salt, divalent salts
Additional amount is 0.1~0.5mol/L, and nanofiltration membrane is 600~800Da of molecular cut off, nanofiltration process pressure can be 1.0~
3.0Mpa。
Further, in the S7 step, the second protease is bromelain, in enzymolysis process, temperature is 40~
60 DEG C, enzymolysis time can be 50~100min.
Further, in the S8 step, adsorbent is alginic acid fibre.
Further, in the S9 step, concentration can be concentrated with conventional vacuum, and drying can be using spray drying.
A kind of processing unit of high-COD waste water with high salt, comprising:
Air flotation slot, for carrying out air bearing removal of impurities processing to meat pickling waste water；
Aeration tube is set in air flotation slot, for blasting air in air flotation slot；
Coarse filter is connected to air flotation slot, for carrying out coarse filtration to the waste water after air-flotation process；
Extraction tower is connected to coarse filter, carries out petroleum ether extraction except fat for the filtrate to coarse filter；
Tank is added in extractant, extraction tower is connected to, for petroleum ether to be added into extraction tower；
First enzymatic vessel, is connected to extraction tower, and the water phase for obtaining to extraction tower carries out enzymolysis processing；
Ultrafiltration membrane is connected to the first enzymatic vessel, carries out hyperfiltration treatment for the enzymolysis liquid in the first enzymatic vessel, makes small molecular protein
Ultrafiltration membrane is penetrated with polypeptide；
Nanofiltration membrane is connected to ultrafiltration membrane, carries out nanofiltration concentration for the filtrate to ultrafiltration membrane, and polysaccharide and salt is made to penetrate nanofiltration membrane,
Retain small molecular protein and polypeptide by nanofiltration membrane；
Tank is added in divalent salts, the feed inlet of nanofiltration membrane is connected to, for divalent salts to be added in the water inlet of nanofiltration membrane；
Second enzymatic vessel is connected to the retention side of nanofiltration membrane, carries out enzymolysis processing for the concentrate to nanofiltration membrane；
Adsorption column is connected to the second enzymatic vessel, and the enzymolysis liquid for obtaining to the second enzymatic vessel carries out adsorption treatment, removes divalent
Salt；
Enrichment facility is connected to adsorption column, carries out concentration for the enzymolysis liquid after adsorption treatment；
Spray-drying installation is connected to enrichment facility, for being spray-dried to the enzymolysis liquid after concentration.
Further, the ultrafiltration retaining molecular weight is 30~500,000 Da.
Further, nanofiltration retaining molecular weight is 600~800Da.
Further, that be packed into divalent salts addition tank is Mg2+、Ca2+Or Zn2+Chloride salt.
Further, what is be packed into adsorption column is alginic acid fibre.
Detailed description of the invention
Fig. 1 is the flow chart of processing method of the invention；
Fig. 2 is processing unit figure of the invention；Wherein, 1 is air flotation slot, and 2 be aeration tube, and 3 be coarse filter, and 4 be extraction tower, 5
It is that tank is added in extractant, 6 be the first enzymatic vessel, and 7 be ultrafiltration membrane, and 8 be nanofiltration membrane, and 9 be that tank is added in divalent salts, and 10 be the second enzymatic hydrolysis
Tank, 11 be precipitation reactor, and 12 be solid-liquid separator, and 13 be enrichment facility, and 14 be spray-drying installation, and 15 be that precipitating reagent is added
Tank；
Fig. 3 is that nanofiltration membrane compares the rejection of protein/polypeptide；
Fig. 4 is that nanofiltration membrane compares the rejection of NaCl；
Fig. 5 is hydrolysis rate of protein change curve in first time enzymolysis process；
Fig. 6 is hydrolysis rate of protein change curve in second of enzymolysis process；
Fig. 7 is the SDS-PAGE detection electrophoretogram for the Gly-His-Lys being prepared, and wherein swimming lane M is marker, and 1 is that embodiment 1,2 is
It is comparative example 1,5 is comparative example 2 that embodiment 2,3, which is embodiment 3,4,.
Specific embodiment
The present invention for CN103570177A in the prior art cannot by meat pickling waste water resource reutilization,
CN104150721A is not suitable for the problem of handling meat pickling waste water, and meat pickling waste water can be effectively treated by proposing one kind
And micromolecule polypeptide can be converted by protein therein, the method as animal feed.
Water quality to be processed needed for the present invention is meat pickling waste water, more specifically, refers to wet cure or salt water note
Enter the high-COD waste water with high salt of method meat curing food generation, water quality situation can be containing 10~20wt% of sodium chloride, albumen
1~5wt% of matter, 0.5~3wt% of fat, COD range is 3000~12000mg/L.
In processing step of the invention, the first step is to carry out air-flotation process to waste water first, due to meat pickling waste water meeting
Containing more fat, it is easier to blister under conditions of aeration, it therefore, can be by pneumatically supported method by some of which meat
Fiber, granule foreign, fat of a part of lightweight of matter etc. take the water surface to by way of bubble, can be relatively easily by these
Impurity removal.The occurrence quantity of bubble per minute and the volume ratio of waste water can be 1:5~10.
In processing step of the invention, second step is to be carried out to air bearing removal of impurities treated waste water using coarse filter
Filter, coarse filtration can further remove the purpose of some particulate matters in pickling waste water, subcutaneous tissue, can protect subsequent super
Filter membrane improves the flux of ultrafiltration membrane.Coarse filter can be using quartz filter, manganese sand filter etc..
In processing step of the invention, third step is to need to extract pickling waste water by petroleum ether, the purpose is to
The fat in waste water is got rid of, this step is more crucial, with subsequent first time enzymatic hydrolysis, ultrafiltration, nanofiltration, second of enzymolysis processing
Constitute synergistic effect.The volume ratio of extract liquor and waste water can be 1:10~15, and extraction time can be 30~60min.
In processing step of the invention, the 4th step is to need to carry out first time enzymolysis processing, the purpose of this step to waste water
It is the albumen or polypeptide for making the breaks down proteins relatively small molecular weight in waste water, it, can be with after the molecular weight of protein reduces
Ultrafiltration membrane is successfully penetrated in ultra-filtration process, realizes the separation between the colloid in waste water, big molecular impurity, suspended matter,
If do not reduce molecular weight, these impurity can be retained in the follow-up process.In this step, the protease that can use can be with
It is alkali protease, trypsase, papain, alkali protease etc..In enzymolysis process, temperature is 40~60 DEG C, enzymatic hydrolysis
Time can be 50~100min.
In processing step of the invention, the 5th step is to need to carry out hyperfiltration treatment to first time enzymolysis liquid, is made in enzymolysis liquid
Small molecular protein and polypeptide penetrate ultrafiltration membrane, the material of used ultrafiltration membrane can be polymer and is also possible to ceramic material
Matter, molecular cut off can be 0.05~0.5Mpa in 30~500,000 Da, the pressure of ultra-filtration process.
In processing step of the invention, the 6th step is to need that the filtrate of ultrafiltration is concentrated using nanofiltration membrane, and nanofiltration membrane is to cut
Stay molecular weight in the charged membrane (preferably 600~800Da) of 200~1000Da, it, can will wherein when ultrafiltrate is concentrated
High molecular weight protein and polypeptide retention, while by pickling waste water with high salt inorganic salts and polysaccharide penetrate film layer, realize to it
The enrichment of middle activity higher albumen and polypeptide, may be implemented the transmission to impurity therein, obtained nanofiltration concentrate passes through again
When crossing second of enzymatic hydrolysis, the enzymolysis polypeptide of high-quality can be obtained.Used herein of nanofiltration membrane, material be can be selected from polyamides
The pressure of the materials such as amine, polyether sulfone, nanofiltration process can control in 1.0~3.0Mpa.In addition, being to need during nanofiltration
It will be first to divalent salts (such as Mg be added in material liquid2+, Ca2+, Zn2+), so that the concentration of salt is reached 0.1~0.5mol/L, due to
Nanofiltration membrane is charged membrane, for divalent or multivalent ion rejection with higher, therefore, after joined divalent salts, by
The balance that charge is kept during the effect of Donnan balance principle, UF membrane will lead to more monovalent salt (i.e. chlorine
Change sodium) film layer is penetrated, nanofiltration membrane can be made stronger to the repulsion effect of sodium chloride, sodium chloride is further reduced and be concentrated in nanofiltration
Retention in liquid reduces nanofiltration membrane to the rejection of sodium chloride；Simultaneously as inorganic salts can reduce protein in water molten
Xie Xing, then proteins and peptides just cannot easily penetrate nanofiltration membrane after the addition of divalent salts, so that nanofiltration membrane is to protein and more
The rejection of peptide is improved；Simultaneously as being to need to carry out albumen second using bromelain in subsequent step
Enzymolysis processing, and inorganic salts (the especially Zn of divalent2+) have the active and right of bromelain that be significantly improved again
Protease protecting effect, therefore divalent salts can be deposited in such concentrate again just, it can achieve many things at one stroke, effectively
Improve hydrolysis result.
In processing step of the invention, the 7th step is second of enzymatic hydrolysis for needing to carry out to nanofiltration concentrate, due to passing through
Polysaccharide, the salt in pickling waste water have been separated in above-mentioned process, depth growth are carried out by this step, on the one hand, can make
Albumen is further broken into the higher polypeptide of more small-molecular-weight activity, on the other hand, retains without impurity such as consideration polysaccharide, salt
In polypeptide.In this step it is preferable to use protease be bromelain, in enzymolysis process, temperature is 40~60 DEG C, enzymatic hydrolysis
Time can be 50~100min.
In processing step of the invention, the 8th step is that the enzymolysis liquid after digesting to second carries out adsorption treatment, is passed through
Adsorbent removes divalent salts, such as can be got rid of in enzymolysis liquid using alginic acid fibre to the selective absorption of zinc ion
Zn2+, improve the purity of polypeptide.
In processing step of the invention, the 9th step be to the 8th step separate adsorption treatment after polypeptide solution be concentrated,
It is dried, obtains Gly-His-Lys.Here concentration can be concentrated with conventional vacuum, and drying here can be using spray drying.
Based on above method, the present invention also provides a kind of processing units of high-COD waste water with high salt, as shown in Fig. 2, packet
It includes:
Air flotation slot 1, for carrying out air bearing removal of impurities processing to meat pickling waste water；
Aeration tube 2 is set in air flotation slot 1, for blasting air in air flotation slot；
Coarse filter 3 is connected to air flotation slot 1, for carrying out coarse filtration to the waste water after air-flotation process；
Extraction tower 4 is connected to coarse filter 3, carries out petroleum ether extraction except fat for the filtrate to coarse filter 3；
Tank 5 is added in extractant, extraction tower 4 is connected to, for petroleum ether to be added into extraction tower 4；
First enzymatic vessel 6, is connected to extraction tower 4, and the water phase for obtaining to extraction tower 4 carries out enzymolysis processing；
Ultrafiltration membrane 7 is connected to the first enzymatic vessel 6, carries out hyperfiltration treatment for the enzymolysis liquid in the first enzymatic vessel 6, makes small molecule
Albumen and polypeptide penetrate ultrafiltration membrane 7；
Nanofiltration membrane 8 is connected to ultrafiltration membrane 7, carries out nanofiltration concentration for the filtrate to ultrafiltration membrane 7, makes polysaccharide and salt through nanofiltration
Film 8 retains small molecular protein and polypeptide by nanofiltration membrane 8；
Tank 9 is added in divalent salts, the feed inlet of nanofiltration membrane 8 is connected to, for divalent salts to be added in the water inlet of nanofiltration membrane 8；
Second enzymatic vessel 10 is connected to the retention side of nanofiltration membrane 8, carries out enzymolysis processing for the concentrate to nanofiltration membrane 8；
Adsorption column 11 is connected to the second enzymatic vessel 10, and the enzymolysis liquid for obtaining to the second enzymatic vessel 10 carries out adsorption treatment, goes
Except divalent salts；
Enrichment facility 12 is connected to adsorption column 11, carries out concentration for the enzymolysis liquid after adsorption treatment；
Spray-drying installation 13 is connected to enrichment facility 11, for being spray-dried to the enzymolysis liquid after concentration.
Further, 7 molecular cut off of ultrafiltration membrane is 30~500,000 Da.
Further, 8 molecular cut off of nanofiltration membrane is 600~800Da.
Further, that be packed into divalent salts addition tank 9 is Mg2+、Ca2+Or Zn2+Chloride salt.
Further, what is be packed into adsorption column 11 is alginic acid fibre.
Height with high salt obtained in curing process in the meat pickling waste water handled in following embodiment from Salted pork
COD waste water, main water quality situation is: containing sodium chloride 17.4wt%, protein 2.3wt%, fat 1.1 wt%, COD are
8710mg/L。
Embodiment 1
Meat pickling waste water is fed in air flotation slot, bubble is blasted, impurity is made to be coated on bubble surface, bottom waste water is discharged,
Carry out coarse filtration with quartz filter, remove granule foreign, by filtrate and petroleum ether according to volume ratio 5:1 mixing 30min after,
Stratification takes bottom aqueous layer, in the alkali protease that 0.02wt% is wherein added, digests 50min at a temperature of 40 DEG C, at 100 DEG C
Enzyme deactivation 10min, then the ultrafiltration membrance filter by enzymolysis liquid using molecular cut off in 300,000 Da is handled, and the pressure of ultra-filtration process can
To be 0.05Mpa, then in the filtrate of ultrafiltration membrane be added 0.1mol/L ZnCl2, it is re-fed into the nanofiltration of molecular cut off 600Da
Film is concentrated, and nanofiltration membrane operating pressure is 1.0Mpa, will in the concentrate of nanofiltration be added 0.02wt% bromelain, 40
50min is digested at a temperature of DEG C, then enzymolysis liquid is flowed through the adsorption bed for being filled with alginic acid fibre by enzyme deactivation 10min at 100 DEG C
To Zn2+It is adsorbed and removed, is spray-dried after filtrate decompression is concentrated, obtains Gly-His-Lys.
Embodiment 2
Meat pickling waste water is fed in air flotation slot, bubble is blasted, impurity is made to be coated on bubble surface, bottom waste water is discharged,
Coarse filtration is carried out with quartz filter, granule foreign is removed, by filtrate with petroleum ether according to volume ratio 10:1 mixing 60min
Afterwards, stratification takes bottom aqueous layer, digests 100min at a temperature of the alkali protease that 0.05wt% is wherein added, 60 DEG C,
Enzyme deactivation 10min at 100 DEG C, then the ultrafiltration membrance filter by enzymolysis liquid using molecular cut off in 500,000 Da is handled, ultra-filtration process
Pressure can be 0.5Mpa, then in the filtrate of ultrafiltration membrane be added 0.5mol/L ZnCl2, it is re-fed into molecular cut off
The nanofiltration membrane of 800Da is concentrated, and nanofiltration membrane operating pressure is 3.0Mpa, and the spinach of 0.05wt% will be added in the concentrate of nanofiltration
Trailing plants protease digests 100min at a temperature of 60 DEG C, and enzyme deactivation 10min, then enzymolysis liquid is flowed through be filled with alginic acid at 100 DEG C
The adsorption bed of fiber is to Zn2+It is adsorbed and removed, is spray-dried after filtrate decompression is concentrated, obtains Gly-His-Lys.
Embodiment 3
Meat pickling waste water is fed in air flotation slot, bubble is blasted, impurity is made to be coated on bubble surface, bottom waste water is discharged,
Carry out coarse filtration with quartz filter, remove granule foreign, by filtrate and petroleum ether according to volume ratio 8:1 mixing 50min after,
Stratification takes bottom aqueous layer, in the alkali protease that 0.04wt% is wherein added, digests 70min at a temperature of 50 DEG C, at 100 DEG C
Enzyme deactivation 10min, then the ultrafiltration membrance filter by enzymolysis liquid using molecular cut off in 400,000 Da is handled, and the pressure of ultra-filtration process can
To be 0.3Mpa, then in the filtrate of ultrafiltration membrane be added 0.3mol/L ZnCl2, it is re-fed into the nanofiltration of molecular cut off 700Da
Film is concentrated, and nanofiltration membrane operating pressure is 2.0Mpa, will in the concentrate of nanofiltration be added 0.04wt% bromelain, 50
55min is digested at a temperature of DEG C, then enzymolysis liquid is flowed through the adsorption bed for being filled with alginic acid fibre by enzyme deactivation 10min at 100 DEG C
To Zn2+It is adsorbed and removed, is spray-dried after filtrate decompression is concentrated, obtains Gly-His-Lys.
Comparative example 1
Difference with embodiment 3 is: divalent salts are not added in nanofiltration charging.
Meat pickling waste water is fed in air flotation slot, bubble is blasted, impurity is made to be coated on bubble surface, bottom waste water is arranged
Out, coarse filtration is carried out with quartz filter, granule foreign is removed, by filtrate with petroleum ether according to volume ratio 8:1 mixing 50min
Afterwards, stratification takes bottom aqueous layer, in the alkali protease that 0.04wt% is wherein added, digests 70min at a temperature of 50 DEG C, and 100
Enzyme deactivation 10min at DEG C, then the ultrafiltration membrance filter by enzymolysis liquid using molecular cut off in 400,000 Da is handled, the pressure of ultra-filtration process
Power can be 0.3Mpa, then the filtrate of ultrafiltration membrane is sent into the nanofiltration membrane of molecular cut off 700Da and is concentrated, nanofiltration membrane work pressure
Power is 2.0Mpa, and the bromelain of 0.04wt% will be added in the concentrate of nanofiltration, digests 55min at a temperature of 50 DEG C, 100 DEG C
Lower enzyme deactivation 10min, then enzymolysis liquid is spray-dried after being concentrated under reduced pressure, and obtains Gly-His-Lys.
Comparative example 2
Difference with embodiment 3 is: not using hyperfiltration treatment to first time enzymolysis liquid.
Meat pickling waste water is fed in air flotation slot, bubble is blasted, impurity is made to be coated on bubble surface, bottom waste water is arranged
Out, coarse filtration is carried out with quartz filter, granule foreign is removed, by filtrate with petroleum ether according to volume ratio 8:1 mixing 50min
Afterwards, stratification takes bottom aqueous layer, in the alkali protease that 0.04wt% is wherein added, digests 70min at a temperature of 50 DEG C, and 100
Then the ZnCl of 0.3mol/L will be added in enzyme deactivation 10min at DEG C in enzymolysis liquid2, it is re-fed into the nanofiltration membrane of molecular cut off 700Da
Be concentrated, nanofiltration membrane operating pressure is 2.0Mpa, will in the concentrate of nanofiltration be added 0.04wt% bromelain, 50 DEG C
At a temperature of digest 55min, then enzymolysis liquid is flowed through the adsorption bed pair for being filled with alginic acid fibre by enzyme deactivation 10min at 100 DEG C
Zn2+It is adsorbed and removed, is spray-dried after filtrate decompression is concentrated, obtains Gly-His-Lys.
Detection method of the invention:
Fat content detection uses soxhlet extraction；
Protein content detection uses Kjeldahl's method；
Sodium chloride is detected using potentiometric titration；
Proteins and peptides molecular weight is measured using SDS-PAGE method: obtained polypeptide powder is made into 0.01g/L protein solution, it is dense
Contracting gum concentration 3% (pH6.8), resolving gel concentration 8% (pH8.8), voltage 140V, electrophoresis time 3h, after, gel coomassie
Brilliant blue dyes 30min, carries out image analysis with gel Image analysis system after decoloration；
The rejection of nanofiltration membrane is to be calculate by the following formula: R=(1- (C1-C2)/C1) × 100%, wherein C1It is solute in water inlet
Concentration, C2It is concentration of the solute in penetrating fluid；
Protein degree is to measure degree of hydrolysis using using pH-Stat method, and formula is as follows:
DH=(B×Nb)/(α×Mp×Htot) × 100%, wherein Nb is the concentration of standard NaOH；Quota of expenditure when B is titration
The amount of NaOH；1/a is NH2Average dissociation degree, based on 7.0；HtotIt is the peptide bond gram equivalent of protein, its value of animal protein is
8.0；MpIt is protein quality.
The comparison of nanofiltration membrane operational process rejection
As can be seen from the above table, the nanofiltration membrane that the present invention uses is to the rejection with higher of albumen and polypeptide, from implementation
Example 2 and the comparison of embodiment 3 keep the average molecular weight of polypeptide smaller as can be seen that since Degree of Enzymatic Hydrolysis is higher in embodiment 2, and one
Part of polypeptide can penetrate nanofiltration membrane, result in rejection and declined；From embodiment 3 and comparative example 1 as can be seen that due in reality
It applies in the nanofiltration process in example 3, joined divalent salts in charging, reduce the dissolubility of polypeptide and albumen, so that for egg
White and polypeptide rejection is significantly improved, simultaneously because nanofiltration membrane rejection with higher for divalent salts, therefore, root
According to charge balance action principle, nanofiltration membrane may be implemented, the repulsive force of NaCl is improved, decline the rejection of NaCl.Albumen/
Polypeptide, the comparison of NaCl rejection are as shown in Figure 3 and Figure 4.
The comparison of protein degree
Twice the degree of hydrolysis of enzymolysis process change with time as shown in Figure 5 and Figure 6, it can be seen from the figure that protein water
Xie Du be as the variation of time is constantly promoted, as time went on after, growth trend slows down.After enzymatic hydrolysis, degree of hydrolysis
As shown in the table.
As can be seen from the table, since the enzyme concentration of use is higher in embodiment 2, degree of hydrolysis numerical value is also larger；It is real
Example 3 is applied for comparative example 1, the degree of hydrolysis in first time enzymolysis process is not much different, but in second of enzymolysis process
In due to joined divalent salts in nanofiltration charging, the activity and stability of bromelain are improved, so that in second of enzyme
In solution preocess, degree of hydrolysis is significantly improved.
The detection of obtained Gly-His-Lys
As can be seen from the table, the Gly-His-Lys that the present invention is prepared have preferable purity, content of peptides can achieve 95% with
On, it can be seen that from the comparison of embodiment 3 and comparative example 2 and first time enzymolysis liquid handled using ultrafiltration membrane, Ke Yiyou
Effect ground make wherein small molecular protein penetrate film layer, separate it with other impurity, effectively improve the polypeptide in product
Content simultaneously reduces ash；In addition, the comparison of embodiment 3 and reference examples 1 is it can also be seen that after the addition of divalent salts, Ke Yiyou
Effect ground reduces retention of the NaCl in nanofiltration retentate fluid, the purity of the polypeptide improved.
Obtained Gly-His-Lys carry out the detection of molecular weight, as a result as shown in fig. 7, it can be seen from the figure that in obtained Gly-His-Lys
Small molecular protein and polypeptide molecular weight about in 2000~8000Da or so, embodiment 2 since Degree of Enzymatic Hydrolysis is smaller, relatively
Less than normal in embodiment 1 and its molecular weight of embodiment 3, the Gly-His-Lys molecular weight of embodiment 3 is and right absolutely within the scope of 2000~5000Da
Since divalent salt ion not being added in ratio 1, make the hydrolysis result of bromelain lower than embodiment 3, molecular weight is higher, about
Within the scope of 3000~10000Da.
Claims (9)
1. a kind of processing method of high-COD waste water with high salt, the high-COD waste water with high salt is meat pickling waste water, and feature exists
In the method includes the following steps:
S1: air-flotation process: air bearing is carried out to meat pickling waste water and removes impurity；
S2: coarse filtration: waste water obtained in S1 is filtered using coarse filter；
S3: extraction: filtrate obtained in S2 is extracted using petroleum ether, removal fat；
S4: it digests for the first time: the first protein enzyme enzymolysis processing being used to raffinate obtained in S3, obtains the first enzymolysis liquid；
S5: hyperfiltration treatment: hyperfiltration treatment is carried out to the first enzymolysis liquid obtained in S4, makes small molecular protein and polypeptide through ultrafiltration
Film；
S6: nanofiltration processing: divalent salts are added in the ultrafiltrated permeation liquid obtained in S5, then carry out nanofiltration processing, make small molecule egg
White and polypeptide and divalent salts are concentrated, and sodium chloride penetrates nanofiltration membrane；
S7: second digests: carrying out enzymolysis processing using the second protease to the nanofiltration concentrate that S6 is obtained, obtains the second enzymatic hydrolysis
Liquid；
S8: remove divalent salts: the second enzymolysis liquid obtained in step S7 removes divalent salts using adsorbent；
S9: dry: enzymolysis liquid obtained in S8 being concentrated, is dried, Gly-His-Lys are obtained.
2. the processing method of high-COD waste water with high salt according to claim 1, which is characterized in that in the S1 step, often
The occurrence quantity of bubble and the volume ratio of waste water of minute can be 1:5~10.
3. the processing method of high-COD waste water with high salt according to claim 1, which is characterized in that in the S2 step, slightly
Filter can be using quartz filter, manganese sand filter etc..
4. the processing method of high-COD waste water with high salt according to claim 1, which is characterized in that in the S3 step, extraction
The volume ratio of liquid and waste water is taken to can be 1:10~15, extraction time can be 30~60min.
5. the processing method of high-COD waste water with high salt according to claim 1, which is characterized in that in the S4 step, the
One protease can be alkali protease, trypsase, papain etc., and in enzymolysis process, temperature is 40~60 DEG C, enzymatic hydrolysis
Time can be 50~100min.
6. the processing method of high-COD waste water with high salt according to claim 1, which is characterized in that in the S5 step, surpass
Membrane retention molecular weight can be 0.05~0.5Mpa in 30~500,000 Da, the pressure of ultra-filtration process.
7. the processing method of high-COD waste water with high salt according to claim 1, which is characterized in that in the S6 step, two
Valence salt refers to Mg2+、Ca2+Or Zn2+Chloride salt, the additional amount of divalent salts is 0.1~0.5mol/L, and nanofiltration membrane is retention
600~800Da of molecular weight, nanofiltration process pressure can be 1.0~3.0Mpa；In the S7 step, the second protease is spinach
Trailing plants protease, in enzymolysis process, temperature is 40~60 DEG C, and enzymolysis time can be 50~100min；In the S8 step, inhale
Attached dose is alginic acid fibre；In the S9 step, concentration can be concentrated with conventional vacuum, and drying can be using spray drying.
8. a kind of processing unit of high-COD waste water with high salt characterized by comprising
Air flotation slot (1), for carrying out air bearing removal of impurities processing to meat pickling waste water；
Aeration tube (2) is set in air flotation slot (1), for blasting air in air flotation slot；
Coarse filter (3) is connected to air flotation slot (1), for carrying out coarse filtration to the waste water after air-flotation process；
Extraction tower (4) is connected to coarse filter (3), carries out petroleum ether extraction except fat for the filtrate to coarse filter (3)；
Tank (5) are added in extractant, are connected to extraction tower (4), for petroleum ether to be added into extraction tower (4)；
First enzymatic vessel (6) is connected to extraction tower (4), and the water phase for obtaining to extraction tower (4) carries out enzymolysis processing；
Ultrafiltration membrane (7) is connected to the first enzymatic vessel (6), carries out hyperfiltration treatment for the enzymolysis liquid in the first enzymatic vessel (6), makes
Small molecular protein and polypeptide penetrate ultrafiltration membrane (7)；
Nanofiltration membrane (8) is connected to ultrafiltration membrane (7), carries out nanofiltration concentration for the filtrate to ultrafiltration membrane (7), keeps polysaccharide and salt saturating
Nanofiltration membrane (8) are crossed, retain small molecular protein and polypeptide by nanofiltration membrane (8)；
Tank (9) are added in divalent salts, are connected to the feed inlet of nanofiltration membrane (8), for divalent to be added in the water inlet of nanofiltration membrane (8)
Salt；
Second enzymatic vessel (10) is connected to the retention side of nanofiltration membrane (8), for carrying out at enzymatic hydrolysis to the concentrate of nanofiltration membrane (8)
Reason；
Adsorption column (11) is connected to the second enzymatic vessel (10), and the enzymolysis liquid for obtaining to the second enzymatic vessel (10) adsorbs
Processing removes divalent salts；
Enrichment facility (12) is connected to adsorption column (11), carries out concentration for the enzymolysis liquid after adsorption treatment；
Spray-drying installation (13) is connected to enrichment facility (11), for being spray-dried to the enzymolysis liquid after concentration.
9. the processing unit of high-COD waste water with high salt according to claim 8, which is characterized in that the ultrafiltration membrane (7) is cut
Staying molecular weight is 30~500,000 Da；Nanofiltration membrane (8) molecular cut off is 600~800Da；Loading in tank (9) is added in divalent salts
It is Mg2+、Ca2+Or Zn2+Chloride salt；What is be packed into adsorption column (11) is alginic acid fibre.
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| CN111410327A (en) * | 2020-03-29 | 2020-07-14 | 南京霄祥工程技术有限公司 | Restaurant wastewater treatment process and system |
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