CN106866441A - A kind of preparation method of high-purity grade of Ferric Sodium Edetate - Google Patents
A kind of preparation method of high-purity grade of Ferric Sodium Edetate Download PDFInfo
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- CN106866441A CN106866441A CN201610771339.0A CN201610771339A CN106866441A CN 106866441 A CN106866441 A CN 106866441A CN 201610771339 A CN201610771339 A CN 201610771339A CN 106866441 A CN106866441 A CN 106866441A
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- sodium edetate
- naoh
- acetic acid
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a kind of preparation method of high-purity grade of Ferric Sodium Edetate, specific preparation process is as follows：（1）NaOH, ethylenediamine tetra-acetic acid and di-iron trioxide are sequentially added in the reactor for fill pure water, 80 100 DEG C of temperature of control is fully reacted, wherein, the mass ratio of NaOH, ethylenediamine tetra-acetic acid, di-iron trioxide and pure water is 2：2：1：1, the NaOH, ethylenediamine tetra-acetic acid and di-iron trioxide are the pure standard of analysis；（2）Filtering, is concentrated into appearance crystallization, and crystallization is dried after centrifugal dehydration, obtains final product；The preparation method process is simple, compared with traditional handicraft, eliminates wash-out chlorion and the operation decolourized, and shortens the production cycle；And waste liquid quantum of output reduces more than 50%, mother liquor can also carry out reproduction and use, and obtain Ferric Sodium Edetate content 99.2 99.8%, the need for being adapted to scale industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of chemical reagent, especially a kind of system of high-purity grade of Ferric Sodium Edetate
Preparation Method.
Background technology
Ferric Sodium Edetate (NaFeEDTA sodium), molecular formula:C10H12FeN2NaO8·3H2O, molecular weight：421.09, it is yellow
Color powder, odorless, tasteless can be dissolved in water, be mainly used in food additives, and be widely used in food, health products, dairy products, medicine
Deng being preferable iron supplementary.
At this stage, Ferric Sodium Edetate is carried out by tetrasodium ethylenediamine tetraacetate and ferric trichloride at 80~100 DEG C
Reaction, is then prepared from through drying drying, and product purity is not high.
Therefore, seeking a kind of new technology for preparing high-purity grade of Ferric Sodium Edetate has highly important production practices
Meaning.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of high-purity grade of Ferric Sodium Edetate.
In order to solve the above technical problems, the technical scheme is that：
A kind of preparation method of high-purity grade of Ferric Sodium Edetate, specific preparation process is as follows：
(1) NaOH, ethylenediamine tetra-acetic acid and di-iron trioxide are sequentially added in the reactor for fill pure water, is controlled
80-100 DEG C of temperature is fully reacted, wherein, the mass ratio of NaOH, ethylenediamine tetra-acetic acid, di-iron trioxide and pure water is 2：
2：1：1, the NaOH, ethylenediamine tetra-acetic acid and di-iron trioxide are the pure standard of analysis；
(2) filter, be concentrated into appearance crystallization, crystallization is dried after centrifugal dehydration, obtain final product.
The reaction equation of the preparation method of above-mentioned high-purity grade of Ferric Sodium Edetate is：
2C10H16N2O8+2NaOH+Fe2O3→2C10H12FeN2NaO8·3H2O+2H2O
Preferably, it is dense using concentration kettle in the preparation method of above-mentioned high-purity grade of Ferric Sodium Edetate, the step (2)
Contracting, vacuum concentrated under reduced pressure is 0.06-0.1MPa.
Preferably, the preparation method of above-mentioned high-purity grade of Ferric Sodium Edetate, centrifugal dehydration stirs in the step (2)
Speed is mixed for 80-120r/min, to crystals dried temperature control in 90-130 DEG C, duration 3 hours.
The preparation method of above-mentioned high-purity grade of Ferric Sodium Edetate, the mother liquor in the step (2) after centrifugal dehydration can
Used with reproduction after collection.
The beneficial effects of the invention are as follows：
The preparation method of above-mentioned high-purity grade of Ferric Sodium Edetate, process is simple compared with traditional handicraft, is eliminated and washed
Dechlorination ion and the operation decolourized, shorten the production cycle；And waste liquid quantum of output reduces more than 50%, mother liquor can also be regenerated
Product is used, and obtains Ferric Sodium Edetate content 99.2-99.8%, the need for being adapted to scale industrial production.
Specific embodiment
Technical scheme of the present invention is further described with reference to specific embodiment.
Embodiment 1
A kind of preparation method of high-purity grade of Ferric Sodium Edetate, specific preparation process is as follows：
(1) NaOH, ethylenediamine tetra-acetic acid and di-iron trioxide are sequentially added in the reactor for fill pure water, is controlled
80-100 DEG C of temperature is fully reacted, wherein, the mass ratio of NaOH, ethylenediamine tetra-acetic acid, di-iron trioxide and pure water is 2：
2：1：1, the NaOH, ethylenediamine tetra-acetic acid and di-iron trioxide are the pure standard of analysis；
(2) filter, filtrate is concentrated using concentration kettle, vacuum concentrated under reduced pressure is about 0.08MPa, be concentrated into appearance crystallization
Centrifugal dehydration afterwards, mixing speed is 100r/min, and gained crystallization is dried 3 hours under the conditions of 110-120 DEG C, is obtained final product.
Products obtained therefrom Ferric Sodium Edetate content 99.8%, discrimination method：According to GB 22557-2008, containing measurement
Determine method：Method according to HG/T2336-1993 determines content.
The above-mentioned detailed description carried out to a kind of preparation method of high-purity grade of Ferric Sodium Edetate with reference to embodiment,
It is illustrative rather than limited, several embodiments can be included according to limited scope, therefore do not departing from this hair
Changing and modifications under bright general plotting, should belong within protection scope of the present invention.
Claims (3)
1. a kind of preparation method of high-purity grade of Ferric Sodium Edetate, it is characterised in that：Specific preparation process is as follows：
(1) NaOH, ethylenediamine tetra-acetic acid and di-iron trioxide are sequentially added in the reactor for fill pure water, temperature is controlled
80-100 DEG C of fully reaction, wherein, the mass ratio of NaOH, ethylenediamine tetra-acetic acid, di-iron trioxide and pure water is 2：2：1：
1, the NaOH, ethylenediamine tetra-acetic acid and di-iron trioxide are the pure standard of analysis；
(2) filter, be concentrated into appearance crystallization, crystallization is dried after centrifugal dehydration, obtain final product.
2. the preparation method of high-purity grade of Ferric Sodium Edetate according to claim 1, it is characterised in that：The step
(2) using concentration kettle concentration in, vacuum concentrated under reduced pressure is 0.06-0.1MPa.
3. the preparation method of high-purity grade of Ferric Sodium Edetate according to claim 1, it is characterised in that：The step
(2) mixing speed of centrifugal dehydration is 80-120r/min in, and to crystals dried temperature control at 90-130 DEG C, duration 3 is small
When.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510922780X | 2015-12-11 | ||
| CN201510922780 | 2015-12-11 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106866441A true CN106866441A (en) | 2017-06-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610771339.0A Pending CN106866441A (en) | 2015-12-11 | 2016-08-30 | A kind of preparation method of high-purity grade of Ferric Sodium Edetate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109651180A (en) * | 2019-01-22 | 2019-04-19 | 北京海德恒生科技发展有限公司 | A kind of production method of sodium iron ethylene diamine tetra acetate |
| CN114671774A (en) * | 2022-04-02 | 2022-06-28 | 黑龙江农业经济职业学院 | Preparation method of sodium ferric ethylenediamine tetraacetate and product |
-
2016
- 2016-08-30 CN CN201610771339.0A patent/CN106866441A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109651180A (en) * | 2019-01-22 | 2019-04-19 | 北京海德恒生科技发展有限公司 | A kind of production method of sodium iron ethylene diamine tetra acetate |
| CN114671774A (en) * | 2022-04-02 | 2022-06-28 | 黑龙江农业经济职业学院 | Preparation method of sodium ferric ethylenediamine tetraacetate and product |
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Application publication date: 20170620 |