CN107141240A - The preparation method of feed grade hydroxy methionine chelates of zinc - Google Patents
The preparation method of feed grade hydroxy methionine chelates of zinc Download PDFInfo
- Publication number
- CN107141240A CN107141240A CN201710465113.2A CN201710465113A CN107141240A CN 107141240 A CN107141240 A CN 107141240A CN 201710465113 A CN201710465113 A CN 201710465113A CN 107141240 A CN107141240 A CN 107141240A
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- China
- Prior art keywords
- zinc
- hydroxy methionine
- reaction
- chelates
- preparation
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- Granted
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000011701 zinc Substances 0.000 title claims abstract description 59
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 47
- KFSJYZYQSZKRRQ-BYPYZUCNSA-N (2s)-2-(hydroxyamino)-4-methylsulfanylbutanoic acid Chemical compound CSCC[C@H](NO)C(O)=O KFSJYZYQSZKRRQ-BYPYZUCNSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 239000000047 product Substances 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 15
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 10
- 239000002893 slag Substances 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 9
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 4
- 229960001763 zinc sulfate Drugs 0.000 claims description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- LKEZBLSQCJEERD-WCCKRBBISA-N (2S)-2-(hydroxyamino)-4-methylsulfanylbutanoic acid zinc Chemical compound [Zn].ON[C@@H](CCSC)C(=O)O LKEZBLSQCJEERD-WCCKRBBISA-N 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract description 2
- 238000012805 post-processing Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 6
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 description 5
- 241001465754 Metazoa Species 0.000 description 5
- YVZATJAPAZIWIL-UHFFFAOYSA-M [Zn]O Chemical compound [Zn]O YVZATJAPAZIWIL-UHFFFAOYSA-M 0.000 description 5
- 229930182817 methionine Natural products 0.000 description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 239000013522 chelant Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000011573 trace mineral Substances 0.000 description 3
- 235000013619 trace mineral Nutrition 0.000 description 3
- 235000005074 zinc chloride Nutrition 0.000 description 3
- 239000011592 zinc chloride Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- NOESYZHRGYRDHS-UHFFFAOYSA-N insulin Chemical compound N1C(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(NC(=O)CN)C(C)CC)CSSCC(C(NC(CO)C(=O)NC(CC(C)C)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CCC(N)=O)C(=O)NC(CC(C)C)C(=O)NC(CCC(O)=O)C(=O)NC(CC(N)=O)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CSSCC(NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2C=CC(O)=CC=2)NC(=O)C(CC(C)C)NC(=O)C(C)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2NC=NC=2)NC(=O)C(CO)NC(=O)CNC2=O)C(=O)NCC(=O)NC(CCC(O)=O)C(=O)NC(CCCNC(N)=N)C(=O)NCC(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC(O)=CC=3)C(=O)NC(C(C)O)C(=O)N3C(CCC3)C(=O)NC(CCCCN)C(=O)NC(C)C(O)=O)C(=O)NC(CC(N)=O)C(O)=O)=O)NC(=O)C(C(C)CC)NC(=O)C(CO)NC(=O)C(C(C)O)NC(=O)C1CSSCC2NC(=O)C(CC(C)C)NC(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CC(N)=O)NC(=O)C(NC(=O)C(N)CC=1C=CC=CC=1)C(C)C)CC1=CN=CN1 NOESYZHRGYRDHS-UHFFFAOYSA-N 0.000 description 2
- 210000004767 rumen Anatomy 0.000 description 2
- DWNBOPVKNPVNQG-LURJTMIESA-N (2s)-4-hydroxy-2-(propylamino)butanoic acid Chemical compound CCCN[C@H](C(O)=O)CCO DWNBOPVKNPVNQG-LURJTMIESA-N 0.000 description 1
- 241000040710 Chela Species 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 1
- 102000004877 Insulin Human genes 0.000 description 1
- 108090001061 Insulin Proteins 0.000 description 1
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000003975 animal breeding Methods 0.000 description 1
- 235000019728 animal nutrition Nutrition 0.000 description 1
- 235000019789 appetite Nutrition 0.000 description 1
- 230000036528 appetite Effects 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 235000019621 digestibility Nutrition 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229940088598 enzyme Drugs 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000007233 immunological mechanism Effects 0.000 description 1
- 229940125396 insulin Drugs 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
- 229940068041 phytic acid Drugs 0.000 description 1
- 239000000467 phytic acid Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 230000035936 sexual power Effects 0.000 description 1
- 230000036559 skin health Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- WQSRXNAKUYIVET-UHFFFAOYSA-N sulfuric acid;zinc Chemical compound [Zn].OS(O)(=O)=O WQSRXNAKUYIVET-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229940110280 zinc methionine Drugs 0.000 description 1
- CNMFGFBWPBBGKX-SCGRZTRASA-L zinc;(2s)-2-amino-4-methylsulfanylbutanoate Chemical compound [Zn+2].CSCC[C@H](N)C([O-])=O.CSCC[C@H](N)C([O-])=O CNMFGFBWPBBGKX-SCGRZTRASA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/14—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides
- C07C319/20—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides by reactions not involving the formation of sulfide groups
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/142—Amino acids; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/30—Oligoelements
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Animal Husbandry (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of production method of feed addictive, a kind of preparation method of feed grade hydroxy methionine chelates of zinc is specifically disclosed, is comprised the following steps：A, the addition metering sodium hydroxide reagent into the inorganic salt solution of zinc, obtain solid formation；B, washing solid formation are to remove wherein soluble component；C, add water homogenate into washing slag；D, the ratio addition hydroxy methionine progress chelatropic reaction according to Zn content in slurry and molar ratio≤0.5 of hydroxy methionine；E, reaction product obtain product by post processing.It is an advantage of the invention that：1) the higher hydroxy methionine zinc product of purity can be prepared, it is preferably to be used as feed addictive；2) hydroxy methionine chelates of zinc can be prepared by the method for the present invention；3) chelatropic reaction speed is fast, and energy consumption is low, beneficial to industrially promoting.
Description
Technical field
The present invention relates to animal-breeding field, especially a kind of preparation method of feed addictive.
Background technology
Trace element zinc is one of necessary trace element of animal, is likened to " biological element " of animal always, since
Since Todd in 1934 et al. confirms that zinc is one of trace element necessary to Animal nutrition by rat test first, people by
Gradually find, zinc is the part of 200 various metals enzymes, hormone and insulin in animal body, can promote the growth of body
Development and regeneration, maintain the eubolism of body, promote appetite, maintain normal, the acceleration wound of sexual organ and sexual performance
There is great nutritive value in terms of healing, protection skin health, enhancing immunologic mechanism, raising resistance.
Methionine hydroxy zinc has low small toxicity, rumen digestibility, promotion rumen microorganism synthesis, saved in daily ration
Protein, the production performance for improving cow, the production performance and immunocompetence that improve animal, the discharge for reducing nitrogen, pollution environment
The features such as less, simple production process, relatively low price, be a kind of most economical effective amino acid source and the zinc source of animal.Therefore hydroxyl
Base zinc methionine commercially just gradually some more expensive amino acid of fictitious hosts.
The preparation method of methionine hydroxy zinc is typically：After hydroxy methionine is mixed with the inorganic salt solution of zinc,
Certain reaction temperature is maintained in the presence of alkaline solution and is made.
For example, Publication No. CN1287795A patent document discloses a kind of system of fodder additive contg. zinc hydroxy methionine
Preparation Method, it is the inorganic salt solution for using liquid hydroxyl methionine and zinc using mol ratio as 1:1~2, temperature 50~
At 100 DEG C, in the presence of sodium hydroxide, pH=6~8 are reacted 0.8~1.2 hour under condition of normal pressure, and reaction product is again through washing
With drying finished product.
And for example Publication No. CN102617426A patent document discloses a kind of preparation of prawn methionine hydroxy zinc
Method, it uses zinc chloride and hydroxy methionine, is vibrated with ultrasonic cell disruption instrument after 5min, by zinc chloride and hydroxyl egg ammonia
Sour mass ratio 1:2 are well mixed, and then adjust pH=6.8~7.2 with 0.2mol/L NaOH, finally adsorbed, dried with zeolite powder,
Crush, produce hydroxy methionine zinc product.
Methionine hydroxy zinc is divided into complex compound, chelate：
Hydroxy methionine zinc complex is that one mole of zinc and a hydroxy methionine are complexed by coordinate bond and generated, shape
Into complex cation, complex compound positive charged ions.Hydroxy methionine complex molecules formula：ZnC5H8O3S。
Hydroxy methionine chelates of zinc is one mole of zinc and two hydroxy methionine by coordinate bond, covalent bond chelating
Generation, forms inner complex salt, and chelate is into electroneutral.Hydroxy methionine chelates of zinc molecular formula：Zn(C5H10O3S)2。
And the method for above-mentioned two pieces patent document can only occur complex reaction and produce hydroxy methionine zinc complex, and
Hydroxy methionine chelates of zinc can not be obtained.
The content of the invention
In order to obtain product impurity content less, the higher feed grade hydroxy methionine chelates of zinc product of purity, and it is excellent
Change throughput rate, the invention provides a kind of preparation method of feed grade hydroxy methionine chelates of zinc.
The technical solution adopted in the present invention is：The preparation method of feed grade hydroxy methionine chelates of zinc, including it is following
Step：
A, the addition metering sodium hydroxide reagent into the inorganic salt solution of zinc, fully separation of solid and liquid obtains solid phase after reaction
Thing；
B, washing solid formation obtain washing slag to remove wherein soluble component；
C, add water homogenate into washing slag, obtains slurry；
D, the ratio addition hydroxy methionine progress according to Zn content in slurry and molar ratio≤0.5 of hydroxy methionine
Chelatropic reaction, reaction obtains reaction product after terminating；
E, reaction product by separation of solid and liquid, wash, be dried to obtain feed grade hydroxy methionine chelates of zinc product.
In the present invention, inventor, which uses, first prepares intermediate slip, then carries out chela with slurry and hydroxy methionine
Close reaction and prepare hydroxy methionine chelates of zinc.This method can be prevented effectively from anion in the inorganic salt solution of zinc and miscellaneous
The non-targeted impurity in products such as cation or anion in matter cation and alkaline solution is mixed into product, so as to prepare
Go out the higher hydroxy methionine zinc product of purity, it is preferably to be used as feed addictive.
On the other hand, with hydroxy methionine chelatropic reaction can occur for the intermediate slip in the present invention, realize hydroxyl egg
Propylhomoserin chelate Zn (C5H10O3S)2Preparation.Because hydroxy methionine chelates of zinc is microsolubility material, thus will not the moisture absorption,
Be conducive to feed manufacturing；In addition, methionine hydroxy zinc is more stable under acid environment, zinc will not be by phytic acid, oxalic acid etc. in enteron aisle
Material, which is combined, causes absorptivity to decline.
The third aspect, by forming intermediate slurry, more conducively chelatropic reaction is carried out so that reaction rate faster, is more saved
Energy.
As a further improvement on the present invention, step D chelatropic reaction condition is：50~60 DEG C of reaction temperature, during reaction
Between 20~40 minutes, 40~80 revs/min of the mixing speed in course of reaction, reaction system pH=6~7.The program is invention
The preferable chelatropic reaction condition that people is summed up by many experiments, under the reaction conditions, both can guarantee that chelatropic reaction with very fast
Speed carry out, also energy consumption can be maintained reduced levels so that this programme is more conducively industrially promoted.
It will be appreciated by those skilled in the art that the nothing of the zinc of generation hydroxide precipitation can be reacted with sodium hydroxide reagent
Machine saline solution generally can serve as the raw material of the present invention, but consider from the cost of raw material and the security standpoint of production, best
Make raw materials for production from solution of zinc sulfate, liquor zinci chloridi.
As a further improvement on the present invention, in step C slurry the mass percent concentration of zinc (being counted using Zn) as 22~
26%, suitable pulp density can ensure that chelatropic reaction is carried out with faster rate.
As a further improvement on the present invention, the reaction in step A terminates rear liquid phase pH=9~10, can be used as with this
The Con trolling index of sodium hydroxide reagent addition, it is ensured that the zinc in solution is fully precipitated, while being added without the hydrogen of undue excess again
Sodium reagent is aoxidized, being also avoided that while reducing wastage of material increases the load of follow-up washing step.
The beneficial effects of the invention are as follows：1) the higher hydroxy methionine zinc product of purity, conduct preferably can be prepared
Feed addictive is used；2) hydroxy methionine chelates of zinc can be prepared by the method for the present invention；3) chelatropic reaction speed is fast,
Energy consumption is low, beneficial to industrially promoting.
Brief description of the drawings
Fig. 1 is the process chart of embodiment one.
Embodiment
The present invention is further described with reference to the accompanying drawings and examples.
Embodiment one：
Feed grade hydroxy methionine chelates of zinc product A is prepared in accordance with the following methods：
(1) solid sulphuric acid zinc is dissolved, insoluble matter is removed by way of press filtration, obtain solution of zinc sulfate.
(2) sodium hydroxide solution is added into solution of zinc sulfate, solid formation is fully collected by way of press filtration after reaction,
Again by way of washing by the sodium sulphate contained in solid formation, the solable matter such as sodium hydroxide is rinsed well, utilizes chlorination
Whether barium detection sulfate radical is rinsed well, obtains washing slag.
(3) washing slag is transferred to retort, adds clear water homogenate.It is 23.3% (quality hundred to extract homogenate detection Zn content
Divide ratio).
(4) it is 1 according to zinc and hydroxy methionine mol ratio by determining Zn content:2.05 carry out chelatropic reaction, reaction temperature
50 DEG C of degree, 30 minutes reaction time, 60 revs/min of mixing speed, the pH=6 of reaction system.
(5) hydroxy methionine chelates of zinc precipitation is by press filtration, and washing removes excessive hydroxy methionine.
(6) hydroxy methionine chelates of zinc crude product is obtained by expansion drying, is removed unnecessary moisture, is finally produced
Product A.
Constituent analysis is carried out to product A, 1 is the results are shown in Table.
Embodiment two：
Feed grade hydroxy methionine chelates of zinc product B is prepared in accordance with the following methods：
(1) Zinc chloride solid is dissolved, insoluble matter is removed by way of press filtration, obtain liquor zinci chloridi.
(2) sodium hydroxide solution is added into liquor zinci chloridi, solid formation is fully collected by way of press filtration after reaction,
Again by way of washing by the sodium chloride contained in solid formation, the solable matter such as sodium hydroxide is rinsed well, is washed
Slag.
(3) washing slag is transferred to retort, adds clear water homogenate.It is 25.1% (quality hundred to extract homogenate detection Zn content
Divide ratio)
(4) it is 1 according to zinc and hydroxy methionine mol ratio by determining Zn content:2.1 carry out chelatropic reaction, reaction temperature
60 DEG C of degree, 20 minutes reaction time, 80 revs/min of mixing speed, the pH=6.8 of reaction system.
(5) hydroxy methionine chelates of zinc precipitation is by press filtration, and washing removes excessive hydroxy methionine.
(6) hydroxy methionine chelates of zinc crude product is obtained by expansion drying, is removed unnecessary moisture, is finally produced
Product B.
Constituent analysis is carried out to product B, 1 is the results are shown in Table.
Table 1：Feed grade hydroxy methionine chelates of zinc product composition analytical table
| Zn(C5H10O3S)2 | Moisture | Lead (mg/kg) | Arsenic (mg/kg) | Cadmium (mg/kg) | Yield | |
| Product A | 86.2% | 7.6% | 4.6 | 3.2 | 6.8 | 96.8% |
| Product B | 85.9% | 7.7% | 5.3 | 4.1 | 5.2 | 96.2% |
Claims (5)
1. the preparation method of feed grade hydroxy methionine chelates of zinc, comprises the following steps：
A, the addition metering sodium hydroxide reagent into the inorganic salt solution of zinc, fully separation of solid and liquid obtains solid formation after reaction；
B, washing solid formation obtain washing slag to remove wherein soluble component；
C, add water homogenate into washing slag, obtains slurry；
D, according to Zn content in slurry and molar ratio≤0.5 of hydroxy methionine ratio add hydroxy methionine chelated
Reaction, reaction obtains reaction product after terminating；
E, reaction product by separation of solid and liquid, wash, be dried to obtain feed grade hydroxy methionine chelates of zinc product.
2. the preparation method of feed grade hydroxy methionine chelates of zinc according to claim 1, it is characterised in that：Step D
Chelatropic reaction condition be：50~60 DEG C of reaction temperature, 20~40 minutes reaction time, mixing speed 40 in course of reaction~
80 revs/min, reaction system pH=6~7.
3. the preparation method of feed grade hydroxy methionine chelates of zinc according to claim 1, it is characterised in that：The zinc
Inorganic salt solution be solution of zinc sulfate, liquor zinci chloridi in one kind.
4. the preparation method of the feed grade hydroxy methionine chelates of zinc according to any claim in claims 1 to 3,
It is characterized in that：The mass percent concentration of zinc (being counted using Zn) is 22~26% in step C slurry.
5. the preparation method of the feed grade hydroxy methionine chelates of zinc according to any claim in claims 1 to 3,
It is characterized in that：Reaction in step A terminates rear liquid phase pH=9~10.
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| CN113185464A (en) * | 2021-06-18 | 2021-07-30 | 仲恺农业工程学院 | Preparation method of zinc histidine |
| CN114702418A (en) * | 2022-04-25 | 2022-07-05 | 长沙兴嘉生物工程股份有限公司 | Preparation method of environment-friendly hydroxymethionine metal chelate |
| CN114958951A (en) * | 2022-07-07 | 2022-08-30 | 卫仕宠物营养科学研究院(江苏)有限公司 | Preparation method of casein phosphopeptide for improving digestion function of pet dogs and cats |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185464A (en) * | 2021-06-18 | 2021-07-30 | 仲恺农业工程学院 | Preparation method of zinc histidine |
| CN114702418A (en) * | 2022-04-25 | 2022-07-05 | 长沙兴嘉生物工程股份有限公司 | Preparation method of environment-friendly hydroxymethionine metal chelate |
| CN114958951A (en) * | 2022-07-07 | 2022-08-30 | 卫仕宠物营养科学研究院(江苏)有限公司 | Preparation method of casein phosphopeptide for improving digestion function of pet dogs and cats |
| CN114958951B (en) * | 2022-07-07 | 2024-04-09 | 卫仕宠物营养科学研究院(江苏)有限公司 | Preparation method of casein phosphopeptide for improving digestion function of pet dogs and cats |
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