CN106397234A - Preparation method of interfering ion-free ferrous glycinate - Google Patents
Preparation method of interfering ion-free ferrous glycinate Download PDFInfo
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- CN106397234A CN106397234A CN201610802004.0A CN201610802004A CN106397234A CN 106397234 A CN106397234 A CN 106397234A CN 201610802004 A CN201610802004 A CN 201610802004A CN 106397234 A CN106397234 A CN 106397234A
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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
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
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- C07C227/40—Separation; Purification
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Abstract
The invention discloses a preparation method of interfering ion-free ferrous glycinate. The preparation method comprises (1) activated ferrous oxide preparation: heating ferrous oxalate to obtain activated ferrous oxide under the condition of air isolation, (2) synthesizing reaction: under the condition of isolation of air, putting glycine, the activated ferrous oxide, water and an antioxidant in a certain proportion into a reactor for a reaction, and carrying out stirring and heating for some time to obtain a reaction solution, (3) separation and purification: filtering the reaction solution to obtain filter residues and a filtrate, returning the filter residues back to the reactor, carrying out a synthesis reaction process, carrying out alcohol precipitation treatment on the filtrate, carrying out standing and centrifugal treatment to obtain a mixed solution and precipitates, and drying the precipitates to obtain ferrous glycinate products, and (4) post-treatment: carrying out distillation treatment on the mixed liquid, and returning the alcohol and the residue solution obtained through distillation to the reactor for reuse. The invention provides the preparation method of interfering ion-free ferrous glycinate and the preparation method is feasible in economy and technology.
Description
Technical field
The present invention relates to the preparation method of the preparing technical field of ferrous amino acid chelate, especially ferrous bisglycinate chelate.
Background technology
Iron is that growth in humans develops one of necessary trace element, is the important set of ferroheme, myogen and cytochromes
Become part and the agent alive of redox reaction enzyme, be distributed very wide in human body, nearly all tissue has iron, is human development
" construction material ".When human body continuation iron deficiency three to five months, iron can not be supplied normocytic growth needs and will lead to
Iron-deficient is lean, not only have impact on the eubolism of human erythrocyte, also reduces the immunologic function of human body, causes body work energy
Power and the decline of endurance.Status of iron deficiency in pregnant women can to fetus reach maturity and childbirth adversely affects, teenager
Virgin asiderosis will damage its cognitive ability, affect its normal growth and develop, and subsequently mend iron and be difficult to recover.
Hypoferric anemia is the deficiency disease of particularly developing country's generally existing in world wide.Iron in food
When element is through digesting and assimilating, easily forms infusible precipitate with some oxalates, phytate etc., reduce the absorptivity of iron.Ammonia
Base acid iron is third generation source of iron additive, has biological value height, absorptivity height, steady chemical structure, strengthen immunity, profit
The features such as environmental protection, it is the focus currently developed both at home and abroad with development and application.Medical research shows, amino acid chelated iron is in animal
There is very high biology utilization rate in vivo, be equivalent to the 125-185% of same level ferrous sulfate.Amino acid and ferrous ion chela
The dipeptides complex compound of synthesis enters mucomembranous cell from enteron aisle in the way of active transport, can be directly absorbed by the body by small intestine,
It is the very promising ferrous supplement method of one kind.Glycine is the minimum amino acid of molecular weight, should be easier in vivo to be absorbed profit
With being preferable iron supplementary of new generation at present.
At present, domestic amino acid ferrous chelate compound is mainly as the use of feed addictive.This is because current production
Mainly amino acid ferrous chelate compound is prepared for source of iron with ferrous sulfate, frerrous chloride in technique, be difficult to after reaction by product with
Sulfate radical, chlorion separate.With going deep into of research, people start to carry out glycine with reduced iron powder, ferrous carbonate for raw material
Ferrous synthesis, the ferrous content of product is up to more than 20%, but reaction time long, product yield is undesirable.This
Bright ferrous more sub- with glycine chelate generation glycine through isolation air heating preparation active oxidation for source of iron with ferrous oxalate
Iron, the reaction time is short, product yield is high and does not contain interfering ion.
Content of the invention
The technical problem to be solved in the invention is to overcome the impact of interfering ion, provides a kind of technique and viable economically
Preparation without interference anion ferrous bisglycinate chelate method.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of the ferrous bisglycinate chelate without interfering ion, comprises the following steps,
1. the ferrous preparation of active oxidation：Under isolation air conditionses, it is ferrous that heating ferrous oxalate is obtained active oxidation；
2. synthetic reaction：Under isolation air conditionses, glycine, active oxidation ferrous iron, water and antioxidant are pressed certain
Ratio put into reactor reaction, stir and heat a period of time reactant liquor；
3. separating-purifying：Reacting liquid filtering is obtained filtrate and filter residue, filter residue reuse to reactor carries out synthetic reaction, will
Filtrate carries out alcohol analysis process with alcohol analysis liquid, standing, and centrifugal treating obtains mixed liquor and precipitate, precipitate is dried, obtains glycine sub-
Iron product；
4. post-process：Mixed liquor is carried out rectification process, the alcohol obtaining after rectifying and kettle liquid return reactor and carry out reuse.
Further improvement is that of technical solution of the present invention：Step 1. 300～400 DEG C of heating-up temperature, reaction time 15～
60 minutes.
Further improvement is that of technical solution of the present invention：2. middle glycine, active oxidation be ferrous and the reaction of water for step
Molar ratio is 2～3：1：15～30, the addition of antioxidant is the 3%～15% of glycine quality, reaction temperature 50～
80 DEG C, 3～9 hours reaction time.
Further improvement is that of technical solution of the present invention：The condition of step 2. middle isolation air be using atoleine or
Vegetable oil carries out fluid-tight or is filled with nitrogen, argon gas or helium atmosphere.
Further improvement is that of technical solution of the present invention：2. middle antioxidant is vitamin C, citric acid, apple to step
One or more of acid, reduced iron powder, acetic acid.
Further improvement is that of technical solution of the present invention：3. middle alcohol analysis liquid is methyl alcohol or ethanol to step, and alcohol analyses liquid and filter
The volume ratio of liquid is 3～10:1.
Further improvement is that of technical solution of the present invention：3. middle time of repose is 2～4 hours to step, and baking temperature is
50～70 DEG C, drying time is 4～8 hours.
Further improvement is that of technical solution of the present invention：4. the alcohol after middle rectifying replaces alcohol analysis liquid to carry out to step in proportion
Alcohol is analysed, and rectifying kettle liquid replaces the water in synthetic reaction.
Further improvement is that of technical solution of the present invention：The step 4. alcohol after middle rectifying and the volume ratio replacing alcohol to analyse liquid
For 1:1～2:3, rectifying kettle liquid is 1 with the volume ratio replacing water:4～3:5.
Further improvement is that of technical solution of the present invention：4. middle rectification temperature is 60～100 DEG C to step.
Due to employing technique scheme, the technological progress that the present invention obtains is：
This method adopts with ferrous oxalate preparation active oxidation ferrous iron as source of iron, replaces frerrous chloride, ferrous sulfate etc. to contain
There are the source of iron of interference anion and the source of iron that the reactivity such as fe, ferrous carbonate is low, be effectively reduced the reaction time, carry
The amino acid-ferrous preparation method of high yield, products obtained therefrom stability is strong, and, more than 20%, having reached GB will for ferrous content
Ask, amino acid is combined, with ferrous salt, the absorption that can promote molysite, improves biological value.
The present invention is not suitable for installing valve during chelatropic reaction, and the inside and outside differential pressure of sealing is not very big and seals
Requiring higher, thus employing the mode of hydraulic seal, or being added not containing under the mode of inert gas shielding
The antioxidant of interfering ion, prevents activated ferrous ion from being aoxidized and inactivated by the air, easy and simple to handle.
In the present invention because in experiment ferrous salt be easily oxidized to the molysite of trivalent, become di-iron trioxide precipitation, so needing
Antioxidant to be added, to prevent the oxidation of ferrous salt.But, the amino acid-ferrous product major part of commercial type all contains
" interference anion ", for example, preparing in ferrous bisglycinate chelate with ferrous sulfate or frerrous chloride for raw material, metal sulfate or chlorine
Salt dissolving and amino acid are to be difficult to reaction completely, and in reacted product, sulfate ion or chlorion are difficult to separate, this
A little interference anion lead to the ferrous bisglycinate chelate product that can not obtain high Fe content, and the anion pair not being completely segregated
Organism is that have harm it is necessary to spend substantial amounts of one-tenth these difficult detached salt of present treatment.The present invention considers the factor of this respect,
And in view of under the conditions of not affecting the complexing rate of amino acid, employ vitamin C, citric acid, malic acid, reduced iron powder,
The combination of one or more of acetic acid can form chelate with ferrous ion.The present invention adopts above-mentioned reducing agent to make
For antioxidant, ferrous salt is protected.
Different coordination ratio be ligand with the ratio of the molal quantity of metal ion be impact chelatropic reaction key factor it
One.In the present invention, the glycine reaction molar ratio ferrous with active oxidation is 2～3：1, if coordination ratio too little it is impossible to formed
Stable circulus, the stability of chelate is poor；If coordination ratio is too big, it is unworthy from the point of view of economy, cause
Cost waste.Therefore, present invention employs a minimum coordination ratio that can reach chelating degree, both save product cost
, can fully utilize glycine again.
In the present invention, Ferrous glycinate does not form precipitation in organic solvent, but forms crystal and separate out, so,
The time of crystallization has a great impact to the formation of crystal.For the present invention, the time of standing is 2～4 hours so that brilliant
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 rectifying can be steamed out, and can recycle previous step
Alcohol analysis during, save production cost, refining effect is more preferable.In traditional ferrous bisglycinate chelate preparation process, do not relate to
And to the reuse problem to raw material, and in the present invention, by replacing alcohol to analyse liquid the alcohol liquid reclaiming according to certain ratio, return
During analysing to alcohol, and in filter residue after filtration, also contain the antioxidant not participating in reaction and active oxidation be ferrous,
Reaction will be continued in its reuse to reactor, saved reaction cost, meanwhile, the kettle liquid through rectifying is dissolved glycine, makes
When must react initial, the concentration of reactant increases, and the forward direction promoting reaction is carried out.In sum, filtrate, rectifying kettle liquid, rectifying
Cut alcohol reuse operation, saved cost, product average weight yield improve 0.94%.Produce 1000 tons of glycine Asias per year
Iron product, yield often raises 0.1 percentage point, year 200000 yuan of additional income, after this project application, increase by 1,880,000 yuan of benefit/
Year.Meanwhile, the experimental condition of the present invention is gentle, and the solvent in production process is all non-toxic, pollution is little, reduces pollution simultaneously
Discharge, it may have certain social benefit.
Brief description
Fig. 1 is the process chart of the present invention.
Specific embodiment
With reference to embodiment, the present invention is described in further details, specific technical process is as shown in Figure 1.
A kind of preparation method of the ferrous bisglycinate chelate without interfering ion, comprises the following steps：
1. the ferrous preparation of active oxidation：Under isolation air conditionses, heating ferrous oxalate is obtained active oxidation ferrous iron, heating
300～400 DEG C of temperature, 15～60 minutes reaction time；
2. synthetic reaction：In a kettle., glycine is dissolved in water and obtains lysate, lysate adds activity
Ferrous oxide, glycine, ferrous and water the reaction molar ratio of active oxidation are 2～3：1：15～30, then, using paraffin or
Vegetable oil fluid-tight or add without the antioxidant vitamin C of interfering ion, lemon under conditions of being filled with nitrogen, argon gas or helium
One or more of lemon acid, malic acid, reduced iron powder, acetic acid, the addition of antioxidant be glycine quality 3%～
15%, then, it is stirred and heated to 50～80 DEG C, reaction obtained reactant liquor after 3～9 hours；
3. separating-purifying：Reacting liquid filtering is obtained filtrate and filter residue, filter residue is returned reactor and is circulated utilization, then
Filtrate is carried out alcohol analysis process with ethanol or methyl alcohol, it is 3～10 that alcohol analyses liquid with the volume ratio of filtrate:1, after standing 2～4 hours,
Mixed liquor is centrifuged, obtains solution and precipitate, precipitate is dried under conditions of temperature is 50～70 DEG C, is dried
Time is 4～8 hours, obtains ferrous bisglycinate chelate product；
4. post-process：Solution after alcohol is analysed carries out rectification process, and rectification temperature is 60～100 DEG C, reclaims rectification process
Rear alcohol cut is simultaneously re-used for alcohol analysis, and rectifying kettle liquid replaces the water in synthetic reaction, and the alcohol after rectifying analyses liquid with replacing alcohol
Volume ratio is 1:1～2:3, rectifying kettle liquid is 1 with the volume ratio of the water replacing in synthetic reaction:4～3:5.
With reference to embodiment, the present invention is described in further details：
Embodiment 1,
Weigh 0.1mol ferrous oxalate and be heated to 300 DEG C in the case of isolation air, keep being reacted, instead for 60 minutes
It is cooled to room temperature after the completion of answering and obtain active oxidation ferrous iron；By active oxidation ferrous iron and the 0.25mol glycine weighing, 0.75g
Citric acid is put in the conical flask of 250ml, then is added thereto to the deionized water of 50ml, and adds a certain amount of liquid in the water surface
Paraffin fluid-tight.To 70 DEG C, constant temperature stirs 6 hours heating water bath.After reaction terminates, with separatory funnel by reactant liquor and atoleine
Separately, reactant liquor is filtered, then added 400ml ethanol in filtrate, standing was obtained precipitate, to precipitate after 4 hours
Dry 8 hours at 50 DEG C, obtain ferrous bisglycinate chelate product 18.2g, yield is 75.9%.Total iron content is 21.0% after testing, sub-
Iron content 20.5%.Alcohol analysis liquid, in 60 DEG C of rectifying 1.5 hours, obtains recovery ethanol, remaining as rectifying kettle liquid, will reclaim ethanol again
For alcohol analysis, rectifying kettle liquid and filter residue carry out reuse.
1g product is taken to be dissolved in 100ml deionized water, system pH is 6.0, transparent no precipitates.
Embodiment 2,
Weigh 1mol ferrous oxalate and be heated to 350 DEG C in the case of isolation air, keep being reacted for 30 minutes, reaction
After the completion of be cooled to room temperature to obtain active oxidation ferrous；Ferrous oxide is put into the three of 1L with the 3mol glycine weighing, 10gVc
In mouthful flask, then it is added thereto to the deionized water of 300mL, and add a certain amount of soybean oil fluid-tight in the water surface.Heating water bath
To 60 DEG C, constant temperature stirs 9 hours.After reaction terminates, with separatory funnel, reactant liquor is separated with soybean oil, reactant liquor was carried out
Filter, then add 1000mL methyl alcohol in filtrate, standing obtained precipitate after 2 hours, precipitate is dried 5 hours at 70 DEG C, obtains
Ferrous bisglycinate chelate product 392g, yield 80.4%.Total iron content is 20.7% after testing, ferrous content 20.4%.Alcohol analysis liquid exists
80 rectifying 1 hour, obtain recovery methyl alcohol, remaining as rectifying kettle liquid, are re-used for alcohol analysis by reclaiming methyl alcohol, rectifying kettle liquid and filter residue enter
Row reuse.
1g product is taken to be dissolved in 100ml deionized water, system pH is 5.8, transparent no precipitates.
Embodiment 3,
Weigh 2mol ferrous oxalate and be heated to 380 DEG C in the case of isolation air, keep being reacted for 20 minutes, reaction
After the completion of be cooled to room temperature to obtain active oxidation ferrous；Ferrous oxide is put into the 3mol glycine weighing, 10g reduced iron powder
In the there-necked flask of 1L, then it is added thereto to the deionized water of 300mL, and add a certain amount of soybean oil fluid-tight in the water surface.Water
Bath is heated to 50 DEG C, and constant temperature stirs 3 hours.After reaction terminates, with separatory funnel, reactant liquor is separated with soybean oil, by reactant liquor
Filtered, then added 1000mL methyl alcohol in filtrate, standing was obtained precipitate after 3 hours, at 60 DEG C, 7 are dried to precipitate little
When, obtain ferrous bisglycinate chelate product 392g, yield 81.2%.Total iron content is 20.3% after testing, ferrous content 20.1%.Alcohol is analysed
Liquid, in 70 DEG C of rectifying 1.5 hours, obtains recovery methyl alcohol, remaining as rectifying kettle liquid, is re-used for alcohol analysis, rectifying kettle liquid by reclaiming methyl alcohol
Carry out reuse with filter residue.
1g product is taken to be dissolved in 100ml deionized water, system pH is 5.9, transparent no precipitates.
Embodiment 4,
Weigh 5mol ferrous oxalate and be heated to 400 DEG C in the case of isolation air, keep being reacted for 15 minutes, reaction
After the completion of be cooled to room temperature to obtain active oxidation ferrous；By ferrous oxide and the 11mol glycine weighing, 25g malic acid, 25g
Iron powder is put in the there-necked flask of 2L capacity, then is added thereto to the deionized water of 1500ml, and is passed through nitrogen in there-necked flask
Gas is to completely cut off air.To 80 DEG C, constant temperature stirs 4 hours heating water bath.After reaction terminates, reactant liquor is filtered, then to filter
5000ml ethanol is added, standing obtained precipitate after 2 hours, precipitate is dried 4 hours at 70 DEG C, obtains ferrous bisglycinate chelate in liquid
Product 980g, yield 82.1%.Total iron content is 20.7% after testing, ferrous content 20.1%.Alcohol analysis liquid is in 100 DEG C of rectifying 4
Hour, obtain recovery ethanol, remaining as rectifying kettle liquid, be re-used for alcohol analysis by reclaiming ethanol, rectifying kettle liquid and filter residue carry out reuse
1g product is taken to be dissolved in 100ml deionized water, system pH is 6.1, transparent no precipitates.
Embodiment 5,
The present embodiment is reference examples, with the ferrous sulfate in background technology as source of iron, prepares amino acid using traditional handicraft
Ferrous chelate compound.
Embodiment 6,
The present embodiment is reference examples, with the ferrous carbonate in background technology as source of iron, prepares amino acid using traditional handicraft
Ferrous chelate compound.
The parameters such as the reaction time in embodiment 1～6, yield, ferrous content, iron content total amount, interfering ion are entered
Row contrast, concrete data is shown in Table 1.
Table 1
As fully visible, with the method for the ferrous bisglycinate chelate of present invention process synthesis for traditional handicraft, during reaction
Between shorten, product yield high and without interfering ion so that products obtained therefrom stability is strong, ferrous content, more than 20%, reaches
Standard, amino acid and the compound absorption that can promote molysite of ferrous salt, improve biological value.
Claims (10)
1. a kind of preparation method of the ferrous bisglycinate chelate without interfering ion is it is characterised in that comprise the following steps：
1. the ferrous preparation of active oxidation：Under isolation air conditionses, it is ferrous that heating ferrous oxalate is obtained active oxidation；
2. synthetic reaction：Under isolation air conditionses, by glycine, active oxidation ferrous iron, water and antioxidant by a certain percentage
Put into reactor reaction, stir and heat a period of time reactant liquor；
3. separating-purifying：Reacting liquid filtering is obtained filtrate and filter residue, filter residue reuse to reactor carries out synthetic reaction, by filtrate
Carry out alcohol analysis process with alcohol analysis liquid, standing, centrifugal treating, obtain mixed liquor and precipitate, precipitate is dried, obtain ferrous bisglycinate chelate and produce
Product；
4. post-process：Mixed liquor is carried out rectification process, the alcohol obtaining after rectifying and kettle liquid return reactor and carry out reuse.
2. a kind of ferrous bisglycinate chelate without interfering ion according to claim 1 preparation method it is characterised in that：Step
Rapid 1. 300～400 DEG C of heating-up temperature, 15～60 minutes reaction time.
3. a kind of ferrous bisglycinate chelate without interfering ion according to claim 1 preparation method it is characterised in that：Step
Rapid 2. middle glycine, ferrous and water the reaction molar ratio of active oxidation are 2～3：1：15～30, the addition of antioxidant is
The 3%～15% of glycine quality, 50～80 DEG C of reaction temperature, 3～9 hours reaction time.
4. a kind of ferrous bisglycinate chelate without interfering ion according to claim 1 preparation method it is characterised in that：Step
The condition of rapid 2. middle isolation air is to carry out fluid-tight using atoleine or vegetable oil or be filled with nitrogen, argon gas or helium atmosphere.
5. a kind of ferrous bisglycinate chelate without interfering ion according to claim 1 preparation method it is characterised in that：Step
Rapid 2. middle antioxidant is one or more of vitamin C, citric acid, malic acid, reduced iron powder, acetic acid.
6. a kind of ferrous bisglycinate chelate without interfering ion according to claim 1 preparation method it is characterised in that：Step
Rapid 3. middle alcohol analysis liquid is methyl alcohol or ethanol, and it is 3 ~ 10 that alcohol analyses liquid with the volume ratio of filtrate:1.
7. a kind of ferrous bisglycinate chelate without interfering ion according to claim 1 preparation method it is characterised in that：Step
Rapid 3. middle time of repose is 2～4 hours, and baking temperature is 50～70 DEG C, and drying time is 4～8 hours.
8. a kind of ferrous bisglycinate chelate without interfering ion according to claim 1 preparation method it is characterised in that：Step
Alcohol after rapid 4. middle rectifying replaces alcohol analysis liquid to carry out alcohol analysis in proportion, and rectifying kettle liquid replaces the water in synthetic reaction.
9. a kind of ferrous bisglycinate chelate without interfering ion according to claim 1 preparation method it is characterised in that：Step
Alcohol after rapid 4. middle rectifying and the volume ratio replacing alcohol to analyse liquid are 1:1～2:3, rectifying kettle liquid is 1 with the volume ratio replacing water:4
～3:5.
10. a kind of ferrous bisglycinate chelate without interfering ion according to claim 1 preparation method it is characterised in that：
4. middle rectification temperature is 60～100 DEG C to step.
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Cited By (2)
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| CN111777523A (en) * | 2020-06-08 | 2020-10-16 | 四川爱隆植物营养科技有限公司 | Preparation method of glycine iron chelate |
| CN115504487A (en) * | 2022-10-12 | 2022-12-23 | 雅迪科技集团有限公司 | Preparation method of positive electrode material, positive electrode material and sodium-ion battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111777523A (en) * | 2020-06-08 | 2020-10-16 | 四川爱隆植物营养科技有限公司 | Preparation method of glycine iron chelate |
| CN115504487A (en) * | 2022-10-12 | 2022-12-23 | 雅迪科技集团有限公司 | Preparation method of positive electrode material, positive electrode material and sodium-ion battery |
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| CN106397234B (en) | 2018-08-24 |
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