CN107141240B - Preparation method of feed-grade zinc hydroxy methionine chelate - Google Patents
Preparation method of feed-grade zinc hydroxy methionine chelate Download PDFInfo
- Publication number
- CN107141240B CN107141240B CN201710465113.2A CN201710465113A CN107141240B CN 107141240 B CN107141240 B CN 107141240B CN 201710465113 A CN201710465113 A CN 201710465113A CN 107141240 B CN107141240 B CN 107141240B
- Authority
- CN
- China
- Prior art keywords
- zinc
- hydroxymethionine
- chelate
- reaction
- washing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 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 title claims abstract description 33
- 239000013522 chelant Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 239000011701 zinc Substances 0.000 claims abstract description 31
- 238000005406 washing Methods 0.000 claims abstract description 28
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 28
- KFSJYZYQSZKRRQ-BYPYZUCNSA-N (2s)-2-(hydroxyamino)-4-methylsulfanylbutanoic acid Chemical compound CSCC[C@H](NO)C(O)=O KFSJYZYQSZKRRQ-BYPYZUCNSA-N 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 21
- 239000007790 solid phase Substances 0.000 claims abstract description 12
- 230000009920 chelation Effects 0.000 claims abstract description 11
- 239000002893 slag Substances 0.000 claims abstract description 9
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 20
- 238000003825 pressing Methods 0.000 claims description 12
- 235000005074 zinc chloride Nutrition 0.000 claims description 10
- 239000011592 zinc chloride Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 7
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 7
- 229960001763 zinc sulfate Drugs 0.000 claims description 7
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000012043 crude product Substances 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 abstract description 18
- GCOGXXHDWQSECB-FHNDMYTFSA-M N[C@@H](CCSC)C(=O)O.O[Zn] Chemical compound N[C@@H](CCSC)C(=O)O.O[Zn] GCOGXXHDWQSECB-FHNDMYTFSA-M 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 11
- 239000002002 slurry Substances 0.000 abstract description 9
- 239000003674 animal food additive Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 5
- 239000007795 chemical reaction product Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 11
- 230000006872 improvement Effects 0.000 description 5
- 241001465754 Metazoa Species 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002474 experimental method Methods 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
- 239000000203 mixture Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 210000004767 rumen Anatomy 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 241000283690 Bos taurus Species 0.000 description 1
- 241000238557 Decapoda Species 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
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 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
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 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
- 230000015556 catabolic process Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 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
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000008076 immune mechanism Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229940125396 insulin Drugs 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000016709 nutrition Nutrition 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
- 238000012545 processing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 230000036299 sexual function Effects 0.000 description 1
- 230000036559 skin health Effects 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
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000029663 wound healing Effects 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Images
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 invention relates to a production method of a feed additive, and particularly discloses a preparation method of a feed-grade zinc hydroxy methionine chelate, which comprises the following steps: A. adding a sodium hydroxide reagent into an inorganic salt water solution of zinc to obtain a solid phase substance; B. washing the solid phase with water to remove soluble components; C. adding water into the washing slag for homogenate; D. adding hydroxymethionine according to the proportion that the molar ratio of the zinc content in the slurry to the hydroxymethionine is less than or equal to 0.5 to carry out chelation reaction; E. and carrying out post-treatment on the reaction product to obtain the product. The invention has the advantages that: 1) the hydroxyl zinc methionine product with higher purity can be prepared and is more suitable to be used as a feed additive; 2) the hydroxyl zinc methionine chelate can be prepared by the method; 3) the chelating reaction rate is high, the energy consumption is low, and the industrial popularization is facilitated.
Description
Technical Field
The invention relates to the field of animal breeding, in particular to a preparation method of a feed additive.
Background
Since the first confirmation of the animal nutrition of zinc by rat experiments in 1934 by Todd et al, zinc is a component of more than 200 kinds of metalloenzymes, hormones and insulin in animal organisms, and has great nutritional value in the aspects of promoting the growth and development of the organisms, maintaining the normal metabolism of the organisms, promoting appetite, maintaining the normality of sexual organs and sexual functions, accelerating wound healing, protecting skin health, enhancing immune mechanism, improving resistance and the like.
The hydroxyl zinc methionine has the characteristics of low toxicity, low rumen degradation rate, promotion of rumen microorganism synthesis, protein saving in daily ration, improvement of production performance of dairy cows, improvement of animal production performance and immunity, reduction of nitrogen emission, less environmental pollution, simple production process, lower price and the like, and is the most economical and effective amino acid source and zinc source for animals. Therefore, zinc hydroxy methionine is gradually replacing some amino acids with higher price in the market.
The preparation method of the hydroxyl zinc methionine is generally as follows: mixing hydroxy methionine and inorganic salt water solution of zinc, and maintaining certain reaction temperature in the presence of alkaline solution.
For example, patent document CN1287795A discloses a method for preparing zinc hydroxymethionine feed additive, which comprises reacting liquid hydroxymethionine and zinc inorganic salt aqueous solution at a molar ratio of 1: 1-2 at 50-100 ℃ and in the presence of sodium hydroxide at a pH of 6-8 under normal pressure for 0.8-1.2 hours, washing and drying the reaction product to obtain the final product.
And for example, patent document No. CN102617426A discloses a method for preparing zinc hydroxymethionine for prawns, which comprises the steps of using zinc chloride and hydroxymethionine, oscillating the zinc chloride and hydroxymethionine with an ultrasonic cell disruptor for 5min, mixing the zinc chloride and hydroxymethionine uniformly according to the mass ratio of 1:2, adjusting the pH to 6.8-7.2 with 0.2mol/L NaOH, and finally adsorbing, drying and crushing the zinc hydroxymethionine with zeolite powder to obtain the zinc hydroxymethionine product.
Zinc hydroxy methionine is classified into complexes and chelates:
the hydroxyl methionine zinc complex is generated by complexing one mole of zinc and one mole of hydroxyl methionine through a coordination bond to form a complex cation, and the complex is positively charged. Hydroxymethionine complex formula: ZnC5H8O3S。
The zinc hydroxymethionine chelate is formed by chelating one mole of zinc and two moles of hydroxymethionine through coordination bonds and covalent bonds to form an inner complex salt, and the chelate is electrically neutral. The molecular formula of the hydroxyl zinc methionine chelate is as follows: zn (C)5H10O3S)2。
However, the methods of the two patent documents only can produce hydroxyl zinc methionine complex through complexation reaction, and cannot obtain hydroxyl zinc methionine chelate.
Disclosure of Invention
In order to obtain a feed-grade zinc hydroxymethionine chelate product with less impurity content and higher purity and optimize the production rate, the invention provides a preparation method of the feed-grade zinc hydroxymethionine chelate.
The technical scheme adopted by the invention is as follows: the preparation method of the feed-grade zinc hydroxy methionine chelate comprises the following steps:
A. adding a metered sodium hydroxide reagent into an inorganic salt water solution of zinc, and carrying out solid-liquid separation after full reaction to obtain a solid-phase substance;
B. washing the solid phase substance with water to remove soluble components therein to obtain washing slag;
C. adding water into the washing slag for homogenate to obtain slurry;
D. adding hydroxymethionine according to the proportion that the molar ratio of the zinc content in the slurry to the hydroxymethionine is less than or equal to 0.5 to carry out chelation reaction, and obtaining a reaction product after the reaction is finished;
E. and carrying out solid-liquid separation, washing and drying on the reaction product to obtain a feed-grade zinc hydroxy methionine chelate product.
In the invention, the inventor prepares the intermediate slurry first and then carries out chelation reaction on the intermediate slurry and the hydroxymethionine to prepare the zinc hydroxymethionine chelate. The method can effectively avoid mixing anions and impurity cations in the zinc inorganic salt aqueous solution and non-target product impurities such as cations or anions in the alkaline solution into the product, thereby being capable of preparing the hydroxyl zinc methionine product with higher purity and being more suitable for being used as a feed additive.
On the other hand, the intermediate slurry in the invention can generate chelation reaction with the hydroxymethionine, thereby realizing the hydroxymethionine chelate Zn (C)5H10O3S)2And (4) preparing. The zinc hydroxy methionine chelate is a slightly soluble substance, so that the zinc hydroxy methionine chelate cannot absorb moisture and is beneficial to feed processing; in addition, zinc hydroxymethionine is more stable in acid environment, and the absorption rate of zinc in the intestinal tract cannot be reduced due to the combination of substances such as phytic acid and oxalic acid.
In the third aspect, the intermediate slurry is formed, so that the chelating reaction is more favorably carried out, the reaction rate is higher, and the energy is saved.
As a further improvement of the invention, the chelating reaction conditions of the step D are as follows: the reaction temperature is 50-60 ℃, the reaction time is 20-40 minutes, the stirring speed in the reaction process is 40-80 r/min, and the pH value of a reaction system is 6-7. The scheme is a better chelation reaction condition summarized by a large number of experiments, under the reaction condition, the chelation reaction can be carried out at a higher speed, and the energy consumption can be maintained at a lower level, so that the scheme is more favorable for industrial popularization.
It will be understood by those skilled in the art that aqueous solutions of inorganic salts capable of reacting with sodium hydroxide reagents to form hydroxide precipitated zinc are generally useful as starting materials for the present invention, but zinc sulfate solutions and zinc chloride solutions are preferred as the starting materials from the standpoint of cost of the starting materials and safety of production.
As a further improvement of the method, the mass percent concentration of zinc (calculated as Zn) in the slurry in the step C is 22-26%, and the proper slurry concentration can ensure that the chelation reaction is performed at a faster rate.
As a further improvement of the method, after the reaction in the step A is finished, the pH value of the liquid phase is 9-10, and the pH value can be used as a control index of the adding amount of the sodium hydroxide reagent to ensure that zinc in the solution is fully precipitated, and excessive sodium hydroxide reagent is not added, so that the waste of raw materials is reduced, and the load of a subsequent washing process is avoided.
The invention has the beneficial effects that: 1) the hydroxyl zinc methionine product with higher purity can be prepared and is more suitable to be used as a feed additive; 2) the hydroxyl zinc methionine chelate can be prepared by the method; 3) the chelating reaction rate is high, the energy consumption is low, and the industrial popularization is facilitated.
Drawings
FIG. 1 is a process flow diagram of the first embodiment.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
The first embodiment is as follows:
a feed-grade zinc hydroxy methionine chelate product A is prepared according to the following method:
(1) dissolving solid zinc sulfate, and removing insoluble substances in a filter pressing mode to obtain a zinc sulfate solution.
(2) Adding a sodium hydroxide solution into a zinc sulfate solution, fully reacting, collecting a solid-phase substance in a filter pressing mode, washing soluble substances such as sodium sulfate, sodium hydroxide and the like contained in the solid-phase substance in a washing mode, and detecting whether sulfate radicals are washed out or not by utilizing barium chloride to obtain washing residues.
(3) Transferring the water washing slag into a reaction tank, and adding clear water for homogenate. The zinc content of the homogenate was 23.3% (mass percent).
(4) By measuring the content of zinc, a chelation reaction is carried out according to the molar ratio of zinc to hydroxymethionine of 1:2.05, the reaction temperature is 50 ℃, the reaction time is 30 minutes, the stirring speed is 60 revolutions per minute, and the pH value of the reaction system is 6.
(5) And removing excessive hydroxymethionine by filter pressing and washing the precipitate of the zinc hydroxymethionine chelate.
(6) And (3) flash drying the obtained hydroxyl methionine zinc chelate crude product to remove redundant water, and finally obtaining a product A.
The composition of product A was analyzed and the results are shown in Table 1.
Example two:
preparing a feed-grade zinc hydroxy methionine chelate product B according to the following method:
(1) dissolving solid zinc chloride, and removing insoluble substances in a filter pressing mode to obtain a zinc chloride solution.
(2) Adding a sodium hydroxide solution into a zinc chloride solution, fully reacting, collecting a solid-phase substance in a filter pressing mode, and washing soluble substances such as sodium chloride, sodium hydroxide and the like contained in the solid-phase substance in a water washing mode to obtain water washing slag.
(3) Transferring the water washing slag into a reaction tank, and adding clear water for homogenate. Extracting homogenate to detect the zinc content of 25.1% (mass percentage)
(4) By measuring the content of zinc, chelation reaction is carried out according to the molar ratio of zinc to hydroxymethionine of 1:2.1, the reaction temperature is 60 ℃, the reaction time is 20 minutes, the stirring speed is 80 r/min, and the pH value of the reaction system is 6.8.
(5) And removing excessive hydroxymethionine by filter pressing and washing the precipitate of the zinc hydroxymethionine chelate.
(6) And (3) carrying out flash evaporation drying on the obtained hydroxyl methionine zinc chelate crude product to remove redundant water, and finally obtaining a product B.
The composition of product B was analyzed and the results are shown in Table 1.
Table 1: feed-grade hydroxyl zinc methionine chelate product ingredient analysis table
| Zn(C5H10O3S)2 | Moisture content | Lead (mg/kg) | Arsenic (mg/kg) | Cadmium (mg/kg) | Yield of | |
| 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 (2)
1. The preparation method of the feed-grade zinc hydroxy methionine chelate comprises the following steps:
A. dissolving solid zinc sulfate, and removing insoluble substances in a filter pressing mode to obtain a zinc sulfate solution;
B. adding a sodium hydroxide solution into a zinc sulfate solution, fully reacting, collecting a solid-phase substance in a filter pressing mode, and washing soluble substances in the solid-phase substance in a water washing mode to obtain washing slag;
C. transferring the water washing slag into a reaction tank, adding clear water for homogenate, and extracting the homogenate to detect that the mass percentage content of zinc is 23.3%;
D. according to the measured zinc content, carrying out chelation reaction according to the molar ratio of zinc to hydroxymethionine of 1:2.05, wherein the reaction temperature is 50 ℃, the reaction time is 30 minutes, the stirring speed is 60 revolutions per minute, and the pH of the reaction system is = 6;
E. removing excessive hydroxymethionine by filter pressing and water washing of the precipitate of the zinc hydroxymethionine chelate;
F. and (3) flash drying the obtained hydroxyl methionine zinc chelate crude product to remove redundant moisture to obtain the hydroxyl methionine zinc chelate.
2. The preparation method of the feed-grade zinc hydroxy methionine chelate comprises the following steps:
A. dissolving solid zinc chloride, and removing insoluble substances in a filter pressing mode to obtain a zinc chloride solution;
B. adding a sodium hydroxide solution into a zinc chloride solution, fully reacting, collecting a solid-phase substance in a filter pressing mode, and washing soluble substances in the solid-phase substance completely in a water washing mode to obtain washing residues;
C. transferring the water washing slag into a reaction tank, adding clear water for homogenate, and extracting the homogenate to detect that the mass percentage content of zinc is 25.1%;
D. according to the measured zinc content, carrying out chelation reaction according to the molar ratio of zinc to hydroxymethionine of 1:2.1, wherein the reaction temperature is 60 ℃, the reaction time is 20 minutes, the stirring speed is 80 r/min, and the pH of the reaction system is = 6.8;
E. removing excessive hydroxymethionine by filter pressing and water washing of the precipitate of the zinc hydroxymethionine chelate;
F. and (3) flash drying the obtained hydroxyl methionine zinc chelate crude product to remove redundant moisture to obtain the hydroxyl methionine zinc chelate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710465113.2A CN107141240B (en) | 2017-06-19 | 2017-06-19 | Preparation method of feed-grade zinc hydroxy methionine chelate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710465113.2A CN107141240B (en) | 2017-06-19 | 2017-06-19 | Preparation method of feed-grade zinc hydroxy methionine chelate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107141240A CN107141240A (en) | 2017-09-08 |
| CN107141240B true CN107141240B (en) | 2020-02-21 |
Family
ID=59781955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710465113.2A Active CN107141240B (en) | 2017-06-19 | 2017-06-19 | Preparation method of feed-grade zinc hydroxy methionine chelate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107141240B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185464B (en) * | 2021-06-18 | 2022-11-25 | 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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1735122A (en) * | 2005-07-19 | 2006-02-15 | 兰州理工大学 | Matrix imaging digital device |
-
2017
- 2017-06-19 CN CN201710465113.2A patent/CN107141240B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107141240A (en) | 2017-09-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107141240B (en) | Preparation method of feed-grade zinc hydroxy methionine chelate | |
| CN111718272B (en) | Preparation method and application of alanine metal chelate | |
| CN103494214B (en) | Casein phosphopeptide and zinc chelate compound | |
| CN1069181C (en) | Micronutrient supplement | |
| CN110128307A (en) | A kind of preparation method of stable amino acid-ferrous complex | |
| CN111635331B (en) | Method for preparing glycine chelate and microelement fertilizer/efficient slow release fertilizer by using glycine mother liquor | |
| CN107337622B (en) | Preparation method of feed-grade copper hydroxymethionine chelate | |
| CN102173602B (en) | Glass fiber subjected to surface treatment, preparation method and application | |
| CN107337625B (en) | Preparation method of feed-grade hydroxyl manganese methionine chelate | |
| CN112707850B (en) | Preparation method of oligomer hydroxy methionine metal chelate | |
| CN103749975B (en) | 2 hydroxybenzoic acid zinc is as the application of feeding high dose zinc oxide substitute | |
| CN103275103A (en) | Method for preparing cefquinome sulfate | |
| CN103044571A (en) | Iron dextran bulk drug and preparation method thereof | |
| CN103342722B (en) | Preparation method of alkaline bismuth gallate | |
| CN107382801A (en) | The preparation method of feed grade Hydroxymethionine salt as trace element chelate | |
| CN103497133B (en) | Method for preparing N-methylol group-D,L-calcium methionine microelement chelates by means of saponification liquid produced through D,L- methionine | |
| JP6227762B2 (en) | Use of ethylenediamine metal complexes to deliver superabsorbent metals for animal nutrition | |
| JP6873310B2 (en) | Methionine-metal chelate and its manufacturing method | |
| CN112493363A (en) | Preparation method of composite amino acid chelate | |
| CN111995535A (en) | Preparation method and application of alanine metal chelate | |
| CN112479866B (en) | Method for co-producing citric acid complex calcium, malic acid complex calcium and fruit acid chelate calcium products | |
| CN103497132B (en) | Utilize D, the saponification liquor that L-Methionine is produced prepares N-methylol-D, the method for L-Methionine calcium | |
| CN109824880B (en) | Beta-polymaleate and preparation method and application thereof | |
| CN103467325A (en) | N,N-dimethylglycine hydrochloride preparation method suitable for industrial production | |
| CN103859162A (en) | Preparation method for high-purity tryptophan microelement chelate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 618300, Deyang City, Sichuan province Guanghan City goldfish town cold water village Patentee after: Sichuan jilongda Biotechnology Group Co.,Ltd. Address before: 618300 Sichuan city of Deyang Province Jin Xing Lu goldfish town of Guanghan City, No. 11 Patentee before: GUANGHAN LONGDA FEED Co.,Ltd. |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of feed grade hydroxymethionine zinc chelate Effective date of registration: 20220629 Granted publication date: 20200221 Pledgee: Guanghan Sichuan rural commercial bank Limited by Share Ltd. Pledgor: Sichuan jilongda Biotechnology Group Co.,Ltd. Registration number: Y2022980009395 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20230609 Granted publication date: 20200221 Pledgee: Guanghan Sichuan rural commercial bank Limited by Share Ltd. Pledgor: Sichuan jilongda Biotechnology Group Co.,Ltd. Registration number: Y2022980009395 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation of feed grade zinc hydroxymethionine Chelation Effective date of registration: 20230612 Granted publication date: 20200221 Pledgee: Guanghan Sichuan rural commercial bank Limited by Share Ltd. Pledgor: Sichuan jilongda Biotechnology Group Co.,Ltd. Registration number: Y2023510000145 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |