CN106478438A - A kind of preparation method of magnesium glycinate chelate - Google Patents
A kind of preparation method of magnesium glycinate chelate Download PDFInfo
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- CN106478438A CN106478438A CN201610848602.1A CN201610848602A CN106478438A CN 106478438 A CN106478438 A CN 106478438A CN 201610848602 A CN201610848602 A CN 201610848602A CN 106478438 A CN106478438 A CN 106478438A
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- magnesium
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- glycinate chelate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation method of magnesium glycinate chelate, comprise the following steps：1. synthetic reaction：Glycine, magnesium compound and water are put in reactor in proportion, stirring mixing, be heated to reaction temperature, reaction a period of time, obtain reactant liquor；2. purification of products：Reactant liquor is filtered at a certain temperature, obtains filtrate and filtering residue, then filtrate is carried out alcohol analysis process, after standing a period of time, centrifugation, obtain alcohol analysis liquid and precipitate, dry precipitate, obtain magnesium glycinate chelate product；3. post processing：Alcohol analysis liquid is carried out rectification, process step is analysed in the alcohol reuse obtaining after rectification to alcohol, the kettle liquid after rectification and filtering residue return reactor and carry out reuse.The present invention provides noiseless ion, avoids a kind of preparation method of magnesium glycinate chelate that " three wastes " produce.
Description
Technical field
The present invention relates to magnesium supplement preparation technique field, specifically a kind of preparation method of magnesium glycinate chelate.
Background technology
Magnesium is one of most cation of content in human body cell, is also to adjust intracellular membranes, sodium potassium ion balance
Important substance；Multiple enzyme reactions in catalyzing activation body, almost take part in the conjunction of all energy metabolisms and DNA, RNA etc. in vivo
Become.Because magnesium ion is relevant with the energy production of cell, therefore can treat human body chronic fatigue syndrome and alzheimer disease,
Regain one's strength rapidly, improve intelligence；When magnesium ion is used with ferrum and calcium plasma simultaneously, can be used for treating anemia, sclerotin
Osteoporosis etc..Meanwhile, also has 0.05% magnesium ion in animal body, it not only maintains the integrity of skeleton and tooth, Er Qie
Play an important role in neuromuscular pulse transmission, the activity of enzyme and energy i (in vivo), albumen and lipid metabolism.In recent years, magnesium
In human body, importance and its clinical practice are increasingly subject to pay attention to, and to make up human body magnesium not in the urgent need to suitable magnesium supplement preparation
Foot.At present, the medicine of the supplementary magnesium that human body uses, how based on inorganic salt, can bring substantial amounts of interference anion in donor（Sulfur
Acid group etc.）, this kind of medicine is not easy to be absorbed by the body, and also can produce untoward reaction.
Content of the invention
The technical problem to be solved in the invention is how to provide noiseless ion, avoid the magnesium glycinate that " three wastes " produce
The preparation method of chelate.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is：
1. synthetic reaction：Glycine, magnesium compound and water are put in reactor in proportion, stirring mixing, be heated to reacting
Temperature, reaction a period of time, obtains reactant liquor；
2. purification of products：Reactant liquor is filtered at a certain temperature, obtains filtrate and filtering residue, then filtrate is carried out alcohol analysis process, quiet
After putting a period of time, centrifugation, obtain alcohol analysis liquid and precipitate, dry precipitate, obtain magnesium glycinate chelate product；
3. post processing：By alcohol analysis liquid carry out rectification, the alcohol reuse obtaining after rectification to alcohol analyse process step, the kettle liquid after rectification with
Filtering residue returns reactor and carries out reuse.
Further improvement is that of technical solution of the present invention：1. middle glycine, magnesium compound, the reaction of water rub described step
Your ratio is 2:1.05:11.1～2:1.8:16.7.
Further improvement is that of technical solution of the present invention：Described step 1. in magnesium compound used be magnesium oxide, hydrogen
One or more of magnesium oxide, magnesium acetate, magnesium carbonate, basic magnesium carbonate, water used is deionized water.
Further improvement is that of technical solution of the present invention：1. middle reaction temperature is 50～90 DEG C, during reaction to described step
Between be 1～6 hour.
Further improvement is that of technical solution of the present invention：Described step 2. middle filter when reactant liquor temperature be 60 °～
70°.
Further improvement is that of technical solution of the present invention：Alcohol during 2. middle alcohol analysis is processed for the described step is methanol, second
Any one of alcohol or propanol, alcohol used and filtrate volume are than for 1:2～1:4.
Further improvement is that of technical solution of the present invention：2. middle time of repose is 2～6 hours to described step, centrifugation point
From rotating speed be 2000～2500 revs/min.
Further improvement is that of technical solution of the present invention：2. middle drying temperature is 60～105 DEG C, during drying to described step
Between be 2～5 hours.
Further improvement is that of technical solution of the present invention：Described step 3. in rectification temperature be 60～80 DEG C.
Due to employing technique scheme, the technological progress that the present invention obtains is：
This method adopted with magnesium oxide, magnesium hydroxide, magnesium acetate, magnesium carbonate, basic magnesium carbonate preparation magnesium glycinate chelate, generation
Replace sulfate radical etc. to contain the interference of interference anion, the response time can have been efficiently reduced, improve yield, products obtained therefrom stability
By force, content of magnesium has reached 10% about, and aminoacid is combined, with magnesium salt, the absorption that can promote iron salt, improves biological value；With
When, low production cost, and the advantages of three wastes produce, technological process is simpler, equipment energy investment is less, and realizes complete
Circulation, zero-emission, more suitable industrialization.
Magnesium compound raw material used in the present invention is magnesium oxide, magnesium hydroxide, magnesium acetate, magnesium carbonate, basic magnesium carbonate
One or more of, generate water during the course of the reaction or generate gas disengaging system, difficult separation inorganic anion will not be introduced,
Obtain pure magnesium glycinate product.
In the building-up process of magnesium glycinate chelate of the present invention, reaction system be glycine under hypersaturated state with magnesium
Compound reacts.Under equal conditions, because the increase of reaction substrate glycine concentration is so that course of reaction reaction rate improves, instead
The conversion ratio answered improves, and product yield is improved.Patent CN103626669A before comparing, yield improves nearly two hundred
Branch.
The purge process of magnesium glycinate chelate of the present invention does not need to be concentrated again it is possible to be carried out alcohol analysis.Compare
Patent CN103626669A before relatively saves concentrating under reduced pressure workshop section, saves the investment of energy device, and technological process is more
Simply, industrialization is more easy to realize.
In the present invention, magnesium glycinate chelate does not form precipitation in organic solvent, but forms crystal and separate out, so, knot
The brilliant time has a great impact to the formation of crystal.For the present invention, the time of standing is 2～6 hours, can make crystalline substance
Body crystallization is more abundant.
The present invention analyses in liquid so that the material analysed in liquid insoluble in alcohol can be big to being added to alcohol in the filtrate after filtering
Measure, fully separate out, then the solution after analysing through alcohol is carried out rectification process again, on the basis of distillation, increase a backflow
Operation, the alcohol in solution after being analysed alcohol by the temperature controlling rectification can be steamed out, and can recycle previous step
Alcohol analysis during, save production cost, refining effect is good.Traditional magnesium glycinate chelate iron standby during, and
It is not involved with the reuse problem to raw material, and in the present invention, by the alcohol liquid reclaiming being replaced alcohol according to certain ratio
Analysis liquid, during reuse to alcohol analysis, and in filtering residue after filtration, will contain the raw material reuse not participating in reaction to reactor
Middle continuation reaction, has saved reaction cost；Meanwhile, by the kettle liquid dissolving glycine through rectification so that reacting when reaction is initial
The concentration of thing increases, and the forward direction promoting reaction is carried out.In sum, the reuse behaviour of the fraction alcohol of filtrate, rectification kettle liquid, rectification
Make, saved cost, product average weight yield improves 2%.Produce 1000 tons of glycine ferrouss products per year, yield often raises 0.1
Percentage point, year 1500000 yuan of additional income, after this project application, increase benefit 3,000,000 yuan/year.Meanwhile, the test bar of the present invention
Part is gentle, and all avirulence, the pollution of the solvent in production process is little, reduces the discharge of pollution, it may have certain society simultaneously
Benefit.
Brief description
Fig. 1 is the process chart of the present invention.
Specific embodiment
Below the present invention is described in further details, specific technical process is as shown in Figure 1.
A kind of preparation method of magnesium glycinate chelate, preparation method comprises the following steps：
1. synthetic reaction：It is 2 that glycine, magnesium compound and water are pressed reaction molar ratio:1.05:11.1～2:1.8:16.7 throwings
Enter in reactor, stirring mixing, be heated to 50～90 DEG C, after reacting 1～6 hour, obtain reactant liquor, magnesium compound is oxidation
One or more of magnesium, magnesium hydroxide, magnesium acetate, magnesium carbonate, basic magnesium carbonate, water used is deionized water；
2. purification of products：Reactant liquor is filtered at 60 °～70 °, obtains filtrate and filtering residue, then filtrate is carried out alcohol analysis process, used
Alcohol be methanol, ethanol, second two or propanol any one, alcohol used and filtrate volume ratio is for 1:2～1:4.；Standing 2～6
After hour, centrifugation, the rotating speed of centrifugation is 2000～2500 revs/min, obtains alcohol analysis liquid and precipitate；Dry precipitate,
Setting drying temperature is 60～105 DEG C, and drying time is 2～5 hours, obtains magnesium glycinate chelate product；
3. post processing：Alcohol analysis liquid is carried out rectification, rectification temperature is 60～80 DEG C, and the alcohol reuse obtaining after rectification to alcohol analysis is processed
Step, the kettle liquid after rectification and filtering residue return reactor and carry out reuse.
With reference to embodiment, the present invention is described in further details：
Embodiment 1,
Take raw material glycine 150Kg（About 2 kilomols）, magnesium hydroxide 63.8Kg（About 1.1 kilomols）With deionized water 125Kg,
Raw material is put in reactor, stirring mixing, be heated to 80 DEG C, react 4 hours, obtain reactant liquor；By reacting liquor while hot（Temperature
For 70 DEG C）Filter, obtain filtrate and filtering residue, then add 375 liters of ethanol to carry out alcohol analysis, after standing 4 hours, in centrifuge in filtrate
Rotating speed is centrifuged under the conditions of being 2000 revs/min, obtains alcohol analysis liquid and precipitate, precipitate is dried 2 hours at 105 DEG C,
Obtain magnesium glycinate chelate product 187.2kg, yield is 97.5%, after testing, product content of magnesium is 11.8%.By alcohol analysis liquid 85
DEG C rectification 4 hours, obtains 367 liters of ethanol, remaining as rectification kettle liquid, ethanol is reclaimed and is reused in alcohol analysis and process, rectification kettle liquid
Return reactor with filtering residue and carry out reuse.
Embodiment 2,
Take raw material glycine 75Kg（About 1 kilomol）, magnesium oxide 22.4Kg（About 0.56 kilomol）With deionized water 150Kg, incite somebody to action
Raw material is put in reactor, stirring mixing, is heated to 70 DEG C, reacts 4 hours, obtain reactant liquor；By reacting liquor while hot（Temperature is
60℃）Filter, obtain filtrate and filtering residue, then add 300 liters of propanol to carry out alcohol analysis, after standing 4 hours, in centrifugal basket in filtrate
Speed is centrifuged under the conditions of 2200 revs/min, obtains alcohol analysis liquid and precipitate, precipitate is dried 3 hours at 85 DEG C, obtains sweet
Propylhomoserin magnesium chelate product 164.2kg, yield is 85.1%, and after testing, product content of magnesium is 9.8%.By alcohol analysis liquid in 85 DEG C of essences
Evaporate 3 hours, obtain 292 liters of propanol, remaining as rectification kettle liquid, propanol is reclaimed and is reused in alcohol analysis process, rectification kettle liquid and filter
Slag returns reactor and carries out reuse.
Embodiment 3,
Take raw material glycine 75Kg（About 1 kilomol）, magnesium hydroxide 30.16Kg（About 0.52 kilomol）, magnesium acetate 6.65Kg（About
0.08 kilomol）With deionized water 140Kg, raw material is put in reactor, stirring mixing, be heated to 90 DEG C, reaction 4 is little
When, obtain reactant liquor；By reacting liquor while hot（Temperature is 70 DEG C）Filter, obtain filtrate and filtering residue, then add 405 liters of ethanol in filtrate
Carry out alcohol analysis, after standing 4 hours, centrifugation under the conditions of centrifuge speed is 2400 revs/min, obtain alcohol analysis liquid and precipitate,
Precipitate is dried 2 hours at 105 DEG C, obtains magnesium glycinate chelate product 88.3kg, yield is 91.8%, after testing, product magnesium
Content is 12.5%.By alcohol analysis liquid in 85 DEG C of rectification 4 hours, obtain 389 liters of ethanol, remaining as rectification kettle liquid, by ethanol recovery and again
It is used in alcohol analysis to process, rectification kettle liquid and filtering residue return reactor and carry out reuse.
Embodiment 4,
Take raw material glycine 75Kg（About 1 kilomol）, basic magnesium carbonate 140Kg（About 1.15 kilomols）With water 150Kg, by raw material
Put in reactor, stirring mixing, be heated to 90 DEG C, react 4 hours, obtain reactant liquor；By reacting liquor while hot（Temperature is 70
℃）Filter, obtain filtrate and filtering residue, then add 500 liters of methanol to carry out alcohol analysis, after standing 4 hours, in centrifuge speed in filtrate
For centrifugation under the conditions of 2500 revs/min, obtain alcohol analysis liquid and precipitate, precipitate is dried 2 hours at 105 DEG C, obtains glycine
Magnesium chelate product 83kg, yield is 85%, and after testing, product content of magnesium is 10.8%.By alcohol analysis liquid in 85 DEG C of rectification 5 hours,
476 liters of methanol, remaining as rectification kettle liquid, by Methanol Recovery and be reused in alcohol analysis and process, rectification kettle liquid and filtering residue return anti-
Kettle is answered to carry out reuse.
Technical scheme arbitrarily can convert in above-mentioned each numerical value, constitutes different technical schemes, not office
It is limited to above-described embodiment.
Claims (9)
1. a kind of preparation method of magnesium glycinate chelate is it is characterised in that comprise the following steps：
1. synthetic reaction：Glycine, magnesium compound and water are put in reactor in proportion, stirring mixing, be heated to reacting
Temperature, reaction a period of time, obtains reactant liquor；
2. purification of products：Reactant liquor is filtered at a certain temperature, obtains filtrate and filtering residue, then filtrate is carried out alcohol analysis process, quiet
After putting a period of time, centrifugation, obtain alcohol analysis liquid and precipitate, dry precipitate, obtain magnesium glycinate chelate product；
3. post processing：By alcohol analysis liquid carry out rectification, the alcohol reuse obtaining after rectification to alcohol analyse process step, the kettle liquid after rectification with
Filtering residue returns reactor and carries out reuse.
2. a kind of magnesium glycinate chelate according to claim 1 preparation method it is characterised in that：Described step 1. in
Glycine, magnesium compound, the reaction molar ratio of water are 2:1.05:11.1～2:1.8:16.7.
3. a kind of magnesium glycinate chelate according to claim 1 preparation method it is characterised in that：Described step 1. in
Magnesium compound used is one or more of magnesium oxide, magnesium hydroxide, magnesium acetate, magnesium carbonate, basic magnesium carbonate, used
Water is deionized water.
4. a kind of magnesium glycinate chelate according to claim 3 preparation method it is characterised in that：Described step 1. in
Reaction temperature is 50～90 DEG C, and the response time is 1～6 hour.
5. a kind of magnesium glycinate chelate according to claim 4 preparation method it is characterised in that：Described step 2. in
During filtration, the temperature of reactant liquor is 60 °～70 °.
6. a kind of magnesium glycinate chelate according to claim 1 preparation method it is characterised in that：Described step 2. in
Alcohol analysis process in alcohol be methanol, ethanol or propanol any one, alcohol used and filtrate volume ratio is for 1:2～1:4.
7. a kind of magnesium glycinate chelate according to claim 6 preparation method it is characterised in that：Described step 2. in
Time of repose is 2～6 hours, and the rotating speed of centrifugation is 2000～2500 revs/min.
8. a kind of magnesium glycinate chelate according to claim 7 preparation method it is characterised in that：Described step 2. in
Drying temperature is 60～105 DEG C, and drying time is 2～5 hours.
9. the preparation method according to described a kind of magnesium glycinate chelate arbitrary in claim 1～8 it is characterised in that：Institute
State step 3. in rectification temperature be 60～80 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107712910A (en) * | 2017-09-22 | 2018-02-23 | 西安交通大学 | A kind of gelatin small peptide or collagen tripeptide chelating calcium and magnesium and preparation method thereof |
| CN109608349A (en) * | 2018-12-12 | 2019-04-12 | 河北东华冀衡氨基酸科技有限公司 | A kind of environment-friendly preparation method thereof of magnesium glycinate |
| CN111084281A (en) * | 2019-12-24 | 2020-05-01 | 长沙兴嘉生物工程股份有限公司 | Preparation method and application of magnesium threonine |
| CN113321592A (en) * | 2021-06-16 | 2021-08-31 | 安徽安力肽生物科技有限公司 | Preparation method of magnesium glycinate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107712910A (en) * | 2017-09-22 | 2018-02-23 | 西安交通大学 | A kind of gelatin small peptide or collagen tripeptide chelating calcium and magnesium and preparation method thereof |
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| CN111084281A (en) * | 2019-12-24 | 2020-05-01 | 长沙兴嘉生物工程股份有限公司 | Preparation method and application of magnesium threonine |
| CN113321592A (en) * | 2021-06-16 | 2021-08-31 | 安徽安力肽生物科技有限公司 | Preparation method of magnesium glycinate |
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