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
- Authority
- CN
- China
- Prior art keywords
- zinc
- hydroxy methionine
- reaction
- chelates
- preparation
- 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.)
- Granted
Links
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.
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 true CN107141240A (en) | 2017-09-08 |
| CN107141240B 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) |
Cited By (3)
| 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 |
Citations (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 Digitizer |
-
2017
- 2017-06-19 CN CN201710465113.2A patent/CN107141240B/en active Active
Patent Citations (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 Digitizer |
Non-Patent Citations (2)
| Title |
|---|
| 《无机化学》编写组: "《无机化学》", 31 July 1979, 江苏科学技术出版社 * |
| 刘正超: "《染化药剂》", 30 June 1980, 纺织工业出版社 * |
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107141240B (en) | 2020-02-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107141240A (en) | The preparation method of feed grade hydroxy methionine chelates of zinc | |
| CN102784622A (en) | Lignin-based dithiocarbamate heavy metal ion capture agent and preparation method | |
| CN102754739A (en) | Preparation method of composite peptide-copper chelate by utilizing meat processing byproduct | |
| CN1308897A (en) | Micronutrient additive | |
| CN101768226B (en) | High-bulk density low-heavy metal content chitosan and preparation method thereof | |
| CN103053812A (en) | Feed additive basic zinc chloride and method for preparing feed additive basic zinc chloride by using zinc suboxide | |
| CN1136029A (en) | Treatment of waste liquid of monosodium glutamate | |
| CN105995947B (en) | A method for producing starch-zinc complex nutritional enhancer by using pulsed electric field | |
| CN107337622A (en) | The preparation method of feed grade hydroxy methionine copper chelate | |
| CN114747668B (en) | Organic composite trace element and preparation method thereof | |
| CN107337625A (en) | The preparation method of feed grade hydroxy methionine manganic chelates | |
| CN115989849B (en) | Semi-wet preparation process of amino acid polysaccharide complex (chelate) | |
| JP3790492B2 (en) | Production of metal complexes of amino acids obtained by hydrolysis of soy protein | |
| CN107382801A (en) | The preparation method of feed grade Hydroxymethionine salt as trace element chelate | |
| CN106745196A (en) | A kind of production method of zinc sulfate | |
| CN108887490A (en) | It is a kind of can microelement-supplementing ox feed and preparation method thereof | |
| CN104291308B (en) | A kind of production method preparing tricalcium phosphate by-product rye (Secale cereale L.) special fertilizer | |
| CN102696886A (en) | Feed additive and preparation method thereof | |
| JP6956250B2 (en) | Methionine-metal chelate and its manufacturing method | |
| CN111094301B (en) | Methionine-metal chelate and preparation method thereof | |
| CN105309776B (en) | A kind of method that discarded shrimp head water phase adds hydrogen to prepare ferrous amino acid chelate | |
| CN110897039B (en) | Preparation method and application of manganese valine | |
| CN114317656B (en) | Bioactive hairtail peptide microelement chelate and preparation method thereof | |
| CN1418885A (en) | Process for preparing ferriporphyrin sodium salt | |
| CN109721517A (en) | A kind of preparation method of feed methionine chelate ferrous iron |
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 | ||
| 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 |
|
| PE01 | Entry into force 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 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
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 | ||
| 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 Granted publication date: 20200221 Pledgee: Deyang Rural Commercial Bank Co.,Ltd. Guanghan Branch Pledgor: Sichuan jilongda Biotechnology Group Co.,Ltd. Registration number: Y2024990000191 |