CN102550824A - Method for producing small peptide amino acid microelement chelate by way of acid hydrolysis of protein - Google Patents
Method for producing small peptide amino acid microelement chelate by way of acid hydrolysis of protein Download PDFInfo
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Abstract
The invention relates to a method for producing small peptide amino acid microelement chelate by way of the acid hydrolysis of protein. Animal protein or vegetable protein is adopted as raw material, and is hydrolyzed by hydrochloric acid. Hydrolysate is subjected to rough filtration and microfiltration, filtrate is deacidified by a nanofiltration membrane separation system, and the deacidified liquor is purified by way of ultrafiltration separation. Obtained small peptide and amino acid, the molecular weight of which is less than 1000 Dalton, are chelated with microelements, so that the small peptide amino acid microelement chelate is produced. The method is suitable for industrial production, the production cycle is short, the product yield is high, the three wastes cannot be produced in the process of production, and the product has good chemical stability, is rich in nutrition, can be easily digested and absorbed, can resist interference, is nonirritant, has the effect of improving the immunity of body, and is an ideal food nutrition enhancer and feed additive. The invention has a positive and profound significance on promoting the development of feed industry and breeding industry, enhancing the safety of poultry, livestock and aquatic products and protecting the health of human being.
Description
Technical field
The invention belongs to the process technology of protein, relate to the membrane separation technique field simultaneously.
Background technology
Protein hydrolysate is peptone, peptide etc., and end product is an amino acid.Peptide is amino acid whose linear polymer.Usually call oligopeptide to the linear peptides that forms by 2～12 amino acid residues, be also referred to as little peptide, small peptide, little peptide, surpass 12 and the title oligopeptides of no more than 20 amino acid residues, contain the polypeptide that is called of 20 above amino acid residues.Modern scientific research finds, the digestion end-product of protein in alimentary canal often major part is little peptide but not free amino acid.Little Toplink intactly gets into the body circulation through intestinal mucosa cells, participates in the synthetic of tissue protein directly.Some has the active little peptide of special physiological can participate in the movable and metabolism adjusting of organism physiology, improves the immunocompetence of animal body.Because the quilt of little peptide structure is illustrated, biotechnology, chemical synthesis and engineered development, the production of little peptide and technology have had many improvement and innovation.The method of at present, producing little peptide both at home and abroad mainly contains protein degradation method, chemical synthesis and thorugh biologic engineering method.Thorugh biologic engineering method is to adopt the DNA recombinant technique, isolates the dna fragmentation that has genes of interest in driven, the Plant Genome, is cloned into appropriate carriers, with ad hoc approach it is imported recipient cell, obtains needed peptide through cellular expression.Or foreign gene is inserted among the phagosome gene order, make peptide with fusion protein form expression on the phagosome surface, obtain product through the processing purifying, only be confined to the production of polypeptide at present.Chemical synthesis has liquid phase method and solid phase method.Liquid phase method is not suitable for the lower situation of reaction intermediate solubility.Solid phase method be the peptide that will synthesize wherein amino acid carboxyl, amino or the side chain radical of an end progressively increase the method for peptide chain then from aminoterminal or c-terminus attached on the solid carrier.Advantage is that product is easy to purifying, and can realize automation.Shortcoming is in the peptide bond forming process, to produce racemization, and productive rate is low, and cost is high.The protein degradation method is the main method of producing peptide at present, wherein is divided into enzymatic isolation method, microbe fermentation method, alkaline hydrolysis method and acid hydrolyzation again.Enzymatic isolation method is to be substrate with the high-quality protein, and shear action is produced peptide, mature production technology in the enzymolysis of utilization protease.Shortcoming is that the production cycle is long, and the three wastes are many, and the repeatability of degree of hydrolysis and enzymolysis process is difficult to control, and particularly any enzyme preparation and enzymatic hydrolysis condition all unavoidably make product have serious bitter taste, influence animal feed intake.Microbe fermentation method is to combine the fermenting and producing of protease and enzymolysis production to produce the method for peptide.Advantage is to have reduced production cost, and product has fermenting aroma.Shortcoming is that product belongs to the polypeptide category, and the screening of bacterial classification, preservation, cultivation, activation, go down to posterity etc. operated loaded down with trivial details, and bacterial classification kind, total amount, ratio, concentration of substrate and the fermentation condition of inoculation is difficult to control.Alkali hydrolysis method generally is not used owing to cause amino acid whose destruction and produce racemization.Acid hydrolysis removes and destroys tryptophan, outside the sulfur-containing amino acid part is oxidized, can not cause the Racemization of Amino Acids effect, and PD is that the speed of peptide is fast, reacts completely.But the key technology of depickling is difficult to break through, the employing neutralisation disacidify that has, and electrodialysis desalination then, not only power consumption is many, and desalination is not thorough, has a strong impact on product quality.
Little peptide and amino acid can significantly improve feed conversion rate as feed addictive, improve breeding performonce fo animals, reduce aquaculture cost.But the trace element that growth of animal is essential all is independent interpolation.As the inorganic salts of the first generation, progressively to be eliminated by market, second generation organic acid salt biological value is low, and chemical stability is bad.Third generation single amino acid chelating salt chemical stability is good, and biological value improves.But owing to antagonism takes place in the common absorption point position of vying each other with seed amino acid, infiltration rate is slow, and carrier is prone to saturated, thereby does not reach optimal effect.In order to promote the sound development of feed industry and aquaculture; Satisfy the demand growing, press for a kind of trophism of research and development, functionally have both, chemical stability is good, biological value is high, be prone to digest and assimilate, the new and effective green feed additive of anti-interference, non-stimulated, nonhazardous effect new feed additive.
Summary of the invention
The objective of the invention is to overcome the drawback of prior art, a kind of new feed additive be provided---the production method of little peptide ammino acid microelement chelate.The technical scheme that the present invention adopts is, the method for little peptide ammino acid microelement chelate is produced in the protein acid hydrolysis, is raw material with animal protein or vegetable protein, and said animal protein is as with degreasing blood meal or silkworm chrysalis etc., said vegetable protein such as bean powder, dregs of beans etc.Adopt hydrochloric acid hydrolysis.Hydrolyzate elder generation coarse filtration, micro-filtration is filtrated and after preliminary treatment, is separated depickling with NF membrane again; Hydrolyzate after the depickling separates with milipore filter purifies, and molecular cut off obtains little peptide and the amino acid whose mixture of molecular weight less than 1000Dalton greater than polypeptide and the partially hydrolysed protein of 1000Dalton; Adopt chelating technology again, make growth of animal trace elements necessary metal ion and little peptide and several amino acids generation complexation reaction, generate little peptide ammino acid microelement chelate, as feed addictive with circulus.
As of the present invention a kind of preferred, the method that little peptide ammino acid microelement chelate is produced in said protein acid hydrolysis may further comprise the steps:
One, hydrochloric acid hydrolysis: be the hydrochloric acid of food-grade is diluted to percentage by weight 4～20% concentration with deionized water hydrochloric acid solution at least with purity; The weight ratio of protein raw material and said hydrochloric acid solution is 1: 4～5; 100～120 ℃ of hydrolysis temperatures; Stir, hydrolysis time 24～48h measures degree of hydrolysis with the TCA method;
Two, filter: the feed liquid that obtains after hydrochloric acid hydrolysis finishes is filtered while hot, and earlier with acidproof plate and frame filter press coarse filtration, filter membrane is to strengthen fixing thickening filter paper by two-layer nylon cloth, carries out micro-filtration again, and the pore size filter of micro-filtration is not more than 0.5 μ m;
Three, preliminary treatment: feed liquid after filtration input pretreatment system, hold back because pipeline cleans thoroughly or maloperation gets into the foreign matter of circulation barrel, with the diaphragm element;
Four, nanofiltration depickling: get into the one-level EGR through pretreated feed liquid; Sending into one-level NF membrane piece-rate system separates; NF membrane is separated the aperture and is passed through for the material that allows molecular weight 30～70Dalton, and the hydrochloric acid that separates the aperture less than film and water penetrate the one-level dislysate that the film surface forms under pressure and gets into the collection of concentrated hydrochloric acid retracting device; Little peptide, polypeptide and partially hydrolysed protein tunicle are held back, and can't penetrate the film surface, thereby form trapped fluid; Turn back to and continue the circulation separation in the one-level EGR; When treating that material liquid PH value in the one-level EGR is 1-2, feed liquid is sent into the secondary EGR, add the deionized water dilution after; Be sent to the separation that circulates once more of secondary NF membrane piece-rate system; Till material liquid PH value reached more than 6.5 near 7, the feed liquid after the depickling was sent in 25 ± 5 ℃ of insulation EGRs, and the secondary dislysate gets into the watery hydrochloric acid retracting device and collects;
Five, ultra-filtration and separation: the feed liquid in the insulation EGR is sent into the ultra-filtration and separation system and is separated purification; The milipore filter molecular weight cut off is 1000Dalton; The little peptide of molecular weight≤1000Dalton and amino acid form ultrafiltrate through the post jamb aperture under pressure; Molecular weight returns in the insulation EGR with the concentrate form greater than polypeptide and the partially hydrolysed protein of 1000Dalton, and through cycle, the feed liquid in the insulation EGR is divided into ultrafiltrate and concentrate;
Six, the chelating of little peptide and amino acid and trace element: ultrafiltrate gets into the chelatropic reaction still; Add the trace element that purity is at least feed grade respectively by proportioning, stir 80～90 ℃ of temperature controls; Chelating time 4～5h; Use the gel filtration chromatography chelation percent, chelating finishes, can warehouse-in after check, sterilization, preservative treatment.0.5～1 ‰ sodium Diacetate is preferably adopted in said preservative treatment.
The technological process explanation:
1 ingredient requirement: protein raw material must be fresh, dry, do not have go mouldy, free from admixture, blood meal, silkworm chrysalis, bean powder etc. carry out ungrease treatment in advance.Hydrochloric acid purity is at least food-grade, the most handy chemical pure and analysis pure hydrochloric acid, and content 36～38%, water are deionized water.
2 hydrochloric acid hydrolysis: hydrochloric acid is diluted to 4～20% weight percent concentration with deionized water.The weight ratio of protein raw material and hydrochloric acid solution is 1: 4～5,100～130 ℃ of hydrolysis temperatures, hydrolysis time 24～48h.Measure degree of hydrolysis with the TCA method.Preferably in the electrical heating enamel reaction still, carry out, agitated reactor is equipped with cycloid speed reducer, frame (anchor) formula glassed agitator, and speed of agitator 85min also has thermocouple temperature regulating device and hydrochloric acid, water vapour condensation reflux unit.
3 filter: open baiting valve when hydrolysis finishes, emit feed liquid, filter while hot.Elder generation's coarse filtration, coarse filtration adopts acidproof plate and frame filter press, and filter membrane is to strengthen fixing thickening filter paper, the larger particles in the filtering hydrolyzate by two-layer nylon cloth.Before using plate and frame filter press, be pressed into clear water with deionized water from the filtered fluid intake channel earlier, guaranteeing does not have water to spill from its elsewhere except that cleaner liquid, with the proof plate and frame filter press in order.Feed liquid is carried out micro-filtration again after coarse filtration, it is 0.5 μ m filter core that the micro-filtration compressor adopts pore size filter, preferred quartz or ceramic element, and the particulate of filtering >=0.5 μ m is with the diaphragm element.Before using the micro-filtration compressor, earlier quartz or ceramic element are put into the 5%NaoH weak solution and clean, wash down with deionized water then, to guarantee best filter effect.Filter residue behind coarse filtration and the micro-filtration with in the KOH solution with after make fertilizer.
4 preliminary treatment: the feed liquid behind the micro-filtration is with in the dehvery pump input feed liquid bucket, and feed liquid bucket bottom is in the isoplanar with the NF membrane piece-rate system.Feed liquid is drawn into feed liquid in the pretreatment system by dehvery pump after getting into the feed liquid bucket then, holds back because pipeline cleans thoroughly or maloperation gets into the foreign matter of circulation bucket, to protect membrane components such as NF membrane or milipore filter.When the pH value of feed liquid surpasses the acidproof limit of membrane component, need to add deionized water and stirring to regulate pH value.
5 NF membrane are separated depickling: feed liquid is after preliminary treatment gets into one-level circulation bucket; Be pumped in the one-level film separation system by circulating pump and separate; The hydrochloric acid that separates the aperture less than film and water etc., under pressure, it is surperficial to penetrate film; Separated coming formed dislysate, enters into the concentrated hydrochloric acid recycling bin.And separate the material in aperture in the feed liquid greater than film, and hold back like each seed amino acid, little peptide, polypeptide and partially hydrolysed protein tunicle, can't penetrate the film surface, thereby form trapped fluid.Trapped fluid turns back in the one-level circulation bucket and proceeds circulation.Wait to be separated to a certain degree, the feed liquid in the one-level circulation bucket is pumped in the secondary circulation bucket, after adding deionized water and diluting, pump in the secondary film separation system by circulating pump and to separate again with dehvery pump.Residual hydrochloric acid, water etc. penetrated the film surface under pressure in the feed liquid, and separated coming forms dislysate and enter into the low-concentration hcl recycling bin and collect.And each seed amino acid in the feed liquid, little peptide, polypeptide and partially hydrolysed protein tunicle are held back, and can't penetrate the film surface, thereby form trapped fluid.Trapped fluid turns back in the secondary circulation bucket and continues circulation, and the hydrochloric acid in feed liquid almost completely is recovered (material liquid PH value reaches more than 6.5 near 7).The concentrated hydrochloric acid recycle of reclaiming, using during as protein raw material hydrolysis next time is sour.The batching water of the watery hydrochloric acid that reclaims during as next hydrolysis cleans with sour with film.
6 milipore filters separate purifies: the feed liquid after the depickling is delivered in 25 ± 5 ℃ of insulation circulation buckets by dehvery pump; With circulating pump feed liquid is depressed into the ultra-filtration and separation system and separates purification; The ultra-filtration and separation optimum system choosing adopts the Hollow Fiber Ultrafiltration unit of stainless steel casing; The unit operating pressure is not more than 0.6Mpa, and the inside and outside both sides of hollow fiber ultrafiltration membrane pressure reduction is not more than 0.3Mpa.To improve speed of production.The pore size of hollow fiber ultrafiltration membrane allows little peptide and the amino acid of molecular weight≤1000Dalton to pass through, and under pressure, forms ultrafiltrate through the post jamb aperture and flows out, and gets into stainless steel chelating still.The polypeptide of molecular weight＞1000Dalton and partially hydrolysed protein can not can only flow along the fibre columns heart through fibre columns cinclides footpath, return in the insulation circulation bucket with the concentrate form.Through the continuous transportation of circulating pump, the feed liquid in the insulation circulation bucket makes feed liquid be divided into ultrafiltrate and concentrate at last constantly through the ultrafiltration of hollow fiber column.Concentrate gets into storage vat, as polypeptide protein feed.7 chelatings: little peptide ammino acid mixture all gets in the chelatropic reaction still; The chelatropic reaction still preferably has the stainless steel chelating still of agitating device (speed of agitator 85r/min) and thermocouple temperature regulating device; Add the trace element that purity is at least feed grade by proportioning, be preferably chemical pure or analyze pure, 80～90 ℃ of temperature controls; Chelating time 4～5h is with gel filtration chromatography chelating degree.Said proportioning should be announced the requirement of micro-consumption in No. 1224 " feed addictive safe handling standard " according to the national Ministry of Agriculture on June 18th, 2009.
8 products detect
8.1 the mensuration of free aminoacid content is pressed the regulation of NY1429-2007 appendix A automatic amino acid analyzer method and is carried out.
8.2 the mensuration of little peptide content does not still have national standard and industry standard at present.But can detect as follows: get ultrafiltrate 100mL, survey its proportion after, pour in the liquid holding bottle that dries to constant weight in 105 ℃ of baking ovens of warp of Rotary Evaporators, it is concentrated to reduce pressure then, puts into 105 ℃ of baking ovens at last and dries to constant weight.Can calculate the quality of solvent (water) and the quality of little peptide of dry and ispol.And free aminoacid content has recorded through the automatic amino acid analyzer method, so can draw the quality and weight percentage concentration of the medium and small peptide of dry.
8.3 the mensuration of average peptide chain length is measured the average peptide chain length and need be measured a-amino acid (α-NH
2-N) content and total nitrogen (TN) content.Measure α-NH with formol titration
2-N content, total nitrogen is measured with triumphant formula nitriding.Calculate average peptide chain length then, formula is following:
9 packings: the trace element chelated liquid of little peptide ammino acid adds 0.5～1 ‰ sodium Diacetate after high temperature uperization sterilization, put in storage with the can of 25kg vinyon bucket.
The beneficial effect that technical scheme of the present invention is brought:
According to existing bibliographical information, prior art has the production method that turns down the peptide preparation all to belong to enzyme hydrolysis method.But any enzyme preparation and enzymatic hydrolysis condition all make product bring serious bitter taste inevitably, influence animal feed intake, increase the debitterize operation and will improve production cost, and enzymatic isolation method production cycle while is long, and the three wastes are many, and the repeatability of degree of hydrolysis and enzymolysis process is difficult to control.The present invention adopts acid-hydrolysis method, and hydrolysis rate is fast, and is with short production cycle, and hydrolysis time, temperature, proportioning raw materials etc. can both be controlled automatically.The acid hydrolysis process produces maillard reaction, generates giving off a strong fragrance flavor flavor substance, can improve animal feed intake.At present domestic producers adopt the neutralisation disacidify, use the electroosmose process desalination then, and salt rejection rate is up to about 90%, and salt residues is many, has a strong impact on product quality.The power consumption of electrodialysis simultaneously is big.The present invention adopts the depickling of NF membrane isolation technics to make the acid recovery recycle, has stopped environmental pollution, and NF membrane is separated the approximate mechanical grading of depickling know-why simultaneously.Since be low pressure reverse osmosis, little power consumption, and depickling (PH is near 7) completely is the breakthrough of protein acid Hydrolyze method depickling key technology.
A lot of in the market little peptide feeds and feed addictive also do not meet the definition of little peptide, are referred to as little peptide to oligopeptides even the less peptide of molecular weight simply, have ignored the difference of little peptide and oligopeptides, polypeptide, cause market confusion, and little peptide product is very different.The present invention adopts milipore filter separate to purify, and the major parts such as oligopeptides, polypeptide of molecular weight >=1000Dalton is trapped, thereby has improved the little peptide content in the product.
Little peptide ammino acid microelement chelate is a third generation novel micro element feed additive, is the compound with circulus of growth of animal trace elements necessary and little peptide, small peptide, amino acid generation complexation reaction generation:
Ferrous as third generation trace element amino-acid chelating salt such as lysine in the market; Lysine selenium, copper methionine etc. all are single amino-acid chelates; Its chemical stability is better like ferrous fumarate, zinc citrate, copper gluconate etc. than second generation acylate, and biological value is also higher.But owing to the common absorption point position of vying each other with seed amino acid produces antagonism, cause infiltration rate slow, carrier is prone to saturated.In recent years, the Animal nutrition scholar discovers both at home and abroad, and the micro-metal ion major part in the animal body exists with the protein salt form, and little peptide ammino acid microelement chelate approaches the micro-existence form of natural form in the animal body.See that from absorption mechanism little peptide ammino acid microelement chelate shows more superiority than single amino acid chelating salt: one of which, because little peptide is when the amino acid quantity of forming is identical, its isoelectric point (P
IValue) close, this just makes metal ion when small-peptide chelated, and is various informative, and it is more to get into animal body interior " target position ", is difficult for saturated; Its two, the absorption point position is many, no antagonism, infiltration rate is fast; Its three, synthetic protein speed is fast, consumes energy is few; They are four years old; After satisfying organism physiology function needs; Remaining little peptide ammino acid microelement chelate can be by organism metabolism, but can with body fluid in will be combined constitutive protein matter by amino acid or the fragments of peptides that metabolism is fallen; Among poultry, fowl or aquatic livestock musculature deposit or deposit to birds, beasts and eggs, thus the production performance of improving.Therefore, little peptide ammino acid microelement chelate has good chemical stability, and biological value is high; Be prone to digest and assimilate, anti-interference, non-stimulated; The nonhazardous effect; And the little peptide ammino acid microelement chelate of partial function property also has certain sterilization and improves the effect of body's immunity, has important function to improving breeding performonce fo animals and anti-stress ability etc., is a kind of comparatively ideal novel feed addictive of greening efficiently.
To combine accompanying drawing and specific embodiment that the present invention is described further below.
Description of drawings
Accompanying drawing is the process flow diagram of the specific embodiment of the invention.
The specific embodiment
Referring to accompanying drawing, reflect a kind of specific embodiment of the present invention, equipment comprises: the electrical heating enamel reaction still that is equipped with thermocouple temperature regulating device, steam condensing reflux device and frame (anchor) formula glassed agitator; Be equipped with the electrical heating stainless steel cauldron of thermocouple temperature regulating device and frame (anchor) formula agitator; Acidproof plate and frame filter press; 0.5 the micro-filtration compressor of μ m aperture pottery or quartzy filter core; The two-stage NF membrane separator that separates the aperture and be molecular weight 30～70Dalton with separate the Hollow Fiber Ultrafiltration unit that the aperture is 1000Dalton; Stainless steel feed liquid bucket, circulation bucket, recycling bin, washing bucket and hygiene-type sterilization storage tank; Stainless steel dehvery pump, circulating pump, backwashing pump and corresponding hygiene-type pipe-line system.Said each stainless steel equipment preferred 304 or the preparation of 316L bar section of stainless steel.
The method that little peptide ammino acid microelement chelate is produced in described protein acid hydrolysis comprises following each step:
(1) hydrolysis: with fresh dried, do not have go mouldy, pure degreasing blood meal 300kg pours in the electrical heating enamel reaction still; Extract mass percent concentration 6% (Baume degrees 3.9) hydrochloric acid solution that has prepared from the bucket of getting the raw materials ready and inject agitated reactor; The while turn on agitator; Rotating speed 85r/min closes defeated sour pump when treating meter readings for 1200L.110 ℃ of thermocouple temperature controls when temperature rises to 100 ℃, are opened the reflux condenser cooling water switch, and after hydrolysis reached 24h, per sampling half an hour was once carried out intermediate detection with the TAC method, and performed record.
(2) filter: the protein acid hydrolysis finishes, and powered-down and cooling water switch are opened discharging valve of reaction kettle, emit feed liquid, filter while hot.Earlier with acidproof plate and frame filter press coarse filtration, filtrating is again through micro-filtration compressor micro-filtration, and the feed liquid behind the micro-filtration is with dehvery pump input feed liquid bucket, filter residue with in the KOH solution and after make fertilizer.Blowing finishes, with the hot water injection agitated reactor of high-pressure spray gun with about 90 ℃.
(3) preliminary treatment: deionized water is injected the feed liquid bucket, behind the stirring and adjusting PH,, get in the one-level circulation bucket after holding back foreign matter by dehvery pump input pretreatment system.
(4) depickling: start circulating pump; Feed liquid in the one-level circulation bucket is pumped into one-level NF membrane piece-rate system (i.e. one-level NF piece-rate system among the figure) carry out depickling; The acid of deviating from (dislysate) gets into the concentrated hydrochloric acid recycling bin and collects recycle, and trapped fluid turns back to one-level circulation bucket and continues the circulation depickling.With digital display PH meter monitoring material liquid PH value, and make record.Treat feed liquid PH=1～2 o'clock, the feed liquid in the one-level circulation bucket pumped into secondary circulation bucket with dehvery pump, add deionized water and stirring dilution feed liquid after, depickling again circulates to pump into secondary NF membrane piece-rate system (i.e. secondary NF piece-rate system among the figure) by circulating pump.The acid of deviating from (dislysate) gets into the watery hydrochloric acid recycling bin and collects, and batching water during as the next batch proteolysis and film clean with acid.When material liquid PH value reaches 6.5 when above, stop depickling, by 25 ± 5 ℃ of insulation circulations of dehvery pump input bucket, simultaneously NF membrane I and II piece-rate system is carried out backwash.
(5) separate to purify: after the feed liquid in the insulation circulation bucket adds the deionized water and stirring dilution, pump into the ultra-filtration and separation system by circulating pump and circulate to separate and purify.Molecular weight directly forms ultrafiltrate through the hollow fiber column cinclides less than the little peptide ammino acid of 1000Dalton under pressure, get into successively in the anti-chelating still of 304 stainless steels, and concentrate gets into storage vat and collects, as polypeptide protein feed.
(6) chelating: open chelating still power supply, when treating that feed temperature is raised to 80 ℃, feed grade or chemical pure and analytically pure trace element are joined respectively in the chelating still by proportioning; Speed of agitator 85r/min; 80～90 ℃ of temperature controls are kept 4～5h, use the gel filtration chromatography chelation percent.
(7) detect, pack: obtain 450 liters of little peptide ammino acid microelement chelates through above-mentioned operation, after detection, high temperature uperization sterilization, add 0.5～1 ‰ sodium Diacetate, put in storage with the can of 25kg vinyon bucket.
Claims (9)
1. the method for little peptide ammino acid microelement chelate is produced in the protein acid hydrolysis, it is characterized in that, and be raw material with animal protein or vegetable protein, adopt hydrochloric acid hydrolysis; Hydrolyzate elder generation coarse filtration, micro-filtration is filtrated and after preliminary treatment, is separated depickling with NF membrane again; Hydrolyzate after the depickling separates with milipore filter purifies, and molecular cut off obtains little peptide and the amino acid whose mixture of molecular weight less than 1000Dalton greater than polypeptide and the partially hydrolysed protein of 1000Dalton; Adopt chelating technology again, make growth of animal trace elements necessary metal ion and little peptide and several amino acids generation complexation reaction, generate little peptide ammino acid microelement chelate, as feed addictive with circulus.
2. the method for little peptide ammino acid microelement chelate is produced in protein acid hydrolysis as claimed in claim 1, it is characterized in that, comprises following each step:
One, hydrochloric acid hydrolysis: be the hydrochloric acid of food-grade is diluted to percentage by weight 4～20% concentration with deionized water hydrochloric acid solution at least with purity; The weight ratio of protein raw material and said hydrochloric acid solution is 1: 4～5; 100～120 ℃ of hydrolysis temperatures; Stir, hydrolysis time 24～48h measures degree of hydrolysis with the TCA method;
Two, filter: the feed liquid that obtains after hydrochloric acid hydrolysis finishes is filtered while hot, and earlier with acidproof plate and frame filter press coarse filtration, filter membrane is to strengthen fixing thickening filter paper by two-layer nylon cloth, carries out micro-filtration again, and the pore size filter of micro-filtration is not more than 0.5 μ m;
Three, preliminary treatment: feed liquid after filtration input pretreatment system, hold back because pipeline cleans thoroughly or maloperation gets into the foreign matter of circulation barrel, with the diaphragm element;
Four, nanofiltration depickling: get into the one-level EGR through pretreated feed liquid; Sending into one-level NF membrane piece-rate system separates; NF membrane is separated the aperture and is passed through for the material that allows molecular weight 30～70Dalton, and the hydrochloric acid that separates the aperture less than film and water penetrate the one-level dislysate that the film surface forms under pressure and gets into the collection of concentrated hydrochloric acid retracting device; Little peptide, polypeptide and partially hydrolysed protein tunicle are held back, and can't penetrate the film surface, thereby form trapped fluid; Turn back to and continue the circulation separation in the one-level EGR; When treating that material liquid PH value in the one-level EGR is 1-2, feed liquid is sent into the secondary EGR, add the deionized water dilution after; Be sent to the separation that circulates once more of secondary NF membrane piece-rate system; Till material liquid PH value reached more than 6.5 near 7, the feed liquid after the depickling was sent in 25 ± 5 ℃ of insulation EGRs, and the secondary dislysate gets into the watery hydrochloric acid retracting device and collects;
Five, ultra-filtration and separation: the feed liquid in the insulation EGR is sent into the ultra-filtration and separation system and is separated purification; The milipore filter molecular weight cut off is 1000Dalton; The little peptide of molecular weight≤1000Dalton and amino acid form ultrafiltrate through the post jamb aperture under pressure; Molecular weight returns in the insulation EGR with the concentrate form greater than polypeptide and the partially hydrolysed protein of 1000Dalton, and through cycle, the feed liquid in the insulation EGR is divided into ultrafiltrate and concentrate;
Six, the chelating of little peptide and amino acid and trace element: ultrafiltrate gets into the chelatropic reaction still; Add the trace element that purity is at least feed grade respectively by proportioning, stir 80～90 ℃ of temperature controls; Chelating time 4～5h; Use the gel filtration chromatography chelation percent, chelating finishes, can warehouse-in after check, sterilization, preservative treatment.
3. according to claim 1 or claim 2 the protein acid hydrolysis method of producing little peptide ammino acid microelement chelate; It is characterized in that; Said hydrochloric acid hydrolysis carries out in the electrical heating enamel reaction still, and agitated reactor is equipped with thermocouple temperature regulating device, steam condensing reflux device, frame or anchor formula glassed agitator.
4. according to claim 1 or claim 2 the protein acid hydrolysis method of producing little peptide ammino acid microelement chelate is characterized in that said micro-filtration adopts the micro-filtration compressor of 0.5 μ m aperture pottery or quartzy filter core; Filter residue behind coarse filtration and the micro-filtration with in the KOH solution with after make fertilizer.
5. according to claim 1 or claim 2 the protein acid hydrolysis method of producing little peptide ammino acid microelement chelate; It is characterized in that; The recycle and reuse of nanofiltration depickling gained hydrochloric acid, the secondary dislysate that the watery hydrochloric acid retracting device is collected cleans with acid as the batching water and the film of the hydrolysis of next batch protein raw materials; After the one-level dislysate that the concentrated hydrochloric acid recycling bin is collected suitably replenishes concentrated hydrochloric acid, as the acid-hydrolyzed raw material of next batch albumen.
6. according to claim 1 or claim 2 the protein acid hydrolysis method of producing little peptide ammino acid microelement chelate; It is characterized in that; Ultra-filtration and separation adopts the Hollow Fiber Ultrafiltration unit of stainless steel casing; The unit operating pressure is not more than 0.6Mpa, and the inside and outside both sides of hollow fiber ultrafiltration membrane pressure reduction is not more than 0.3Mpa.
7. according to claim 1 or claim 2 the protein acid hydrolysis method of producing little peptide ammino acid microelement chelate; It is characterized in that; The chelatropic reaction of little peptide and amino acid and trace element carries out in the electrical heating stainless steel cauldron, and agitated reactor is equipped with thermocouple temperature regulating device, frame or anchor agitator.
8. the method for little peptide ammino acid microelement chelate is produced in protein acid hydrolysis as claimed in claim 2, it is characterized in that, said concentrate is collected by storage device, as polypeptide protein feed.
9. the method for little peptide ammino acid microelement chelate is produced in protein acid hydrolysis as claimed in claim 2, it is characterized in that, adopts 0.5～1 ‰ sodium Diacetate to carry out preservative treatment.
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Effective date of registration: 20140508 Address after: 410300, Hunan province Changsha Liuyang Jinsha Road three lane ten science and Technology Bureau Dormitory Patentee after: Luo Xianzhang Address before: 410000 Hunan province Changsha Yuhua District of Shaoshan City Road No. 448, section thirty thousand feet apartment No. 3 Building Room 1202 Patentee before: CHANGSHA OUYANGBAO AGRICULTURAL SCIENCE & TECHNOLOGY Co.,Ltd. |
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Address after: 410300, Hunan Province, Changsha Friendship Road West tiger pond No. 9, Hunan Jiayuan B building, room 1806 Patentee after: Luo Xianzhang Address before: 410300, Hunan province Changsha Liuyang Jinsha Road three lane ten science and Technology Bureau Dormitory Patentee before: Luo Xianzhang |
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