CN105837461A - Production technology of high purity iron supplement agent sodium feredetate - Google Patents
Production technology of high purity iron supplement agent sodium feredetate Download PDFInfo
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- CN105837461A CN105837461A CN201510022601.7A CN201510022601A CN105837461A CN 105837461 A CN105837461 A CN 105837461A CN 201510022601 A CN201510022601 A CN 201510022601A CN 105837461 A CN105837461 A CN 105837461A
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Abstract
The invention relates to a production technology of a high purity iron supplement agent sodium feredetate. The technology includes: taking ferric chloride and disodium edentate as the raw materials, adopting water as the solvent, under certain molar equivalent ratio and certain reaction temperature conditions, carrying out reaction to obtain a sodium feredetate solution; adjusting the pH value of the reaction solution with sodium bicarbonate, then adding a certain amount of ethanol into the sodium feredetate solution, then carrying out cooling, standing and crystallization; then performing ethanol washing and crystallization, and conducting filtering and drying so as to obtain a sodium feredetate finished product. The technology provided by the invention has the characteristics of simple operation, short production cycle, complete reaction, and no environmental pollution; under appropriate reaction conditions, the yield of sodium feredetate reaches 88.1%, the purity reaches 99.9%, also the particle size is fine and uniform, the heavy metal residue is low, and impurities are few. Therefore, the obtained sodium feredetate can be used as the raw material of iron supplementation drugs and food.
Description
Technical field
The invention belongs to biomedicine field, be specifically related to the production technology of a kind of iron supplementary editic acid ferrum sodium.
Background technology
Editic acid ferrum sodium (Sodium feredetate) has another name called sodium iron ethylenediaminetetraacetate, hereinafter referred to as FeNaEDTA, and molecular formula is C10H12N2O8FeNa·H2O, molecular weight is 385.1, for yellow or khaki granule or powder, free from extraneous odour, micro-have efflorescence properties, soluble in water, insoluble in ethanol, be heated to 120 DEG C and lose water of crystallization.Editic acid ferrum sodium has the characteristic that dissolubility is high, dissolution velocity is fast, bioavailability is high, toxicity is low, in good taste.
FeNaEDTA can be used as the hardening agent of food additive, child nutrition food, is medically used for supplementing irony, is widely used in the fields such as milk product, beverage, health care of food product, medicine, is mainly used in prevention and the generation for the treatment of iron deficiency anemia.Anemia is a kind of commonly encountered diseases, frequently-occurring disease, and most of anemias are iron deficiency anemia (Iron-deficiency anemia, IDA), is to lack irony due to internal and affect the common anemia of one caused by hemoglobin synthesis.
Since Bland in 1831 is first with Ferrous Sulphate for Treatment " chlorosis ", ferrous sulfate is recorded by pharmacopeia and the food additive code of many countries always.But ferrous sulfate chemical property is very active, easily combines with sulfide polyphenol etc. and cause food discoloration, go bad, and there is the shortcomings such as serious the intestines and stomach stimulation.
Also have ferrous carbonate, ferrous chloride, iron phosphate to receive as the inorganic salt of ferrous-fortifier, ferric phrophosphate, ferrous pyrophosphate, Ferric sodium pyrophosphate, phosphoramidic acid ferrum etc., but the dissolubility that these ferrous-fortifiers are in gastric acid is non-constant, along with the difference often absorption variations of processing mode is the biggest.In order to improve the absorption rate of ferrum, it is developed second filial generation solubility chalybeate small molecular organic acid iron salt complex, such as ferrous lactate, Ferrous gluconate, ferrous succinate, ferrous fumarate, ferrous citrate, ferrous malate etc..It is generally acknowledged that ferrous salt character is unstable, produce and store the most highly difficult, easily cause food discoloration and produce iron taste.
FeNaEDTA stable in properties, can be high temperature resistant, is difficult to oxidized, reserves are constant, fishy smell without metallic iron, in good taste, soluble in water, the sensory properties caused is applied to change less in food, its stable chelate structure is allowed to, without the intestines and stomach stimulation, be tightly combined under one's belt, after entering duodenum, ferrum is just released and absorbs, and in absorption process, FeNaEDTA also can be combined excretion rapidly and play the effect of antidote with harmful element.FeNaEDTA not only promotes the effect that in meals, other sources of iron or endogenous source of iron absorb, and may additionally facilitate the absorption of zinc, does not affect the absorption of calcium.Multiple studies have shown that, the iron absorptivity of FeNaEDTA condensed food is higher 2 ~ 3 times than ferrous sulfate, and also to have dissolubility good for FeNaEDTA simultaneously, the advantage such as change of the less organoleptic quality causing food carrier.
Therefore developing the production technology of a kind of FeNaEDTA, the production technology of high-purity FeNaEDTA particularly developing a kind of pharmaceutical grade has the most real meaning.
Summary of the invention
The present invention develops that a kind of easy to operate, technique is simple, high-purity FeNaEDTA of high yield pulp1, the preparation method of the most medicinal FeNaEDTA, the production technology of a kind of high-purity iron supplementary editic acid ferrum sodium.
The present invention is with Calcium Disodium Versenate and iron chloride as raw material, with water as reaction dissolvent, and single step reaction synthesis FeNaEDTA, crystallize FeNaEDTA with ethanol/water, then with the crystallization of washing with alcohol FeNaEDTA, finally crystallize filtration drying, obtain high-purity FeNaEDTA.
Concrete production technology: weigh Calcium Disodium Versenate (EDTA) and the iron chloride of certain mol proportion example, first iron chloride is dissolved in a certain amount of water, under agitation EDTA is slowly added in above-mentioned solution, reactant liquor is slowly raised certain reaction temperature simultaneously, regulation pH value, to 6 ~ 8, continues reaction a period of time；After reaction terminates, certain volume ethanol is added in reactant liquor, be slowly cooled to uniform temperature, stand crystallization a period of time；Centrifuge dripping, filter cake certain volume washing with alcohol, agitation and filtration, obtain FeNaEDTA single-size powder；50oC is dried, and obtains FeNaEDTA fine work.
In above-mentioned production technology, iron chloride molar concentration in water be 0.20 ~ 0.60mol/L, preferably molar concentration be 0.30 ~ 0.50 mol/L, FeNaEDTA purity reaches 99.9%.
In above-mentioned production technology, the mol ratio of iron chloride and EDTA be 1:0.5 ~ 1:1.5, i.e. mass ratio be 45:31 ~ 15:31, preferred molar ratio be 1:0.8 ~ 1:1.2, i.e. mass ratio be 9:10 ~ 9:15.
In above-mentioned production technology, charging sequence is first that iron chloride is soluble in water, then is slowly added into EDTA.
In above-mentioned production technology, iron chloride and EDTA reaction temperature are 80 ~ 100oC, preferable reaction temperature is 85 ~ 95 oC, FeNaEDTA yield reaches 88.1%.
In above-mentioned production technology, iron chloride and EDTA response time are 30 ~ 90 minutes, and the preferably response time is 50 ~ 70 minutes.
In above-mentioned production technology, after iron chloride and EDTA reaction terminate, adding 1/30 ~ 3/10 in reactant liquor, the medicinal alcohol of preferably 1/20 ~ 2/10 times of water consumption stands crystallization.
In above-mentioned production technology, standing crystallization temperature is-5 ~ 15 oC, preferably crystallization temperature are 0-10oC；Standing crystallization time is 5 ~ 15 hours, and preferably crystallization time is 8-12 hour.
In above-mentioned production technology, after crystallization, with 1/3 ~ 1/5 times, the medicinal alcohol washing of preferably 1/4 times of water yield.
In above-mentioned production technology, the FeNaEDTA that final filtration obtains is yellow or the khaki graininess powder of uniform loose, under the conditions of appropriate reaction, FeNaEDTA yield is up to 88.1%, purity is up to 99.9%, and granularity is tiny homogeneous, and impurity is few, heavy-metal residual is extremely low, is suitable on medicine and food application.
Accompanying drawing explanation
Fig. 1 ferric chloride concn and the relation of FeNaEDTA purity.
Fig. 2 reaction temperature and the relation of FeNaEDTA yield.
Detailed description of the invention
With embodiment, the invention will be further described below, but the invention is not limited in these embodiments.
Embodiment 1
90 mL water and 10 g iron chloride are added in 250 mL reaction bulbs, stirring, after ferrum to be chlorinated all dissolves, EDTA is slowly added in above-mentioned solution, temperature is risen to 90oC, is then slowly added into sodium bicarbonate 6.3 g in reactor and makes pH value of solution be adjusted to about 7, and 90oContinue stirring 60 min reaction under C to terminate, reactant liquor is poured in 500 mL beakers, add 9 mL ethanol, stir, stand cooling, after 8 h, crystallization content reaches maximum, filter, rinse filter cake with 23 mL medicinal alcohols, collect filter cake, filter cake is yellow or the khaki graininess powder of uniform loose, 50oC is dried, and obtains FeNaEDTA fine work, and weigh 12.5 g, yield 87.7%, and purity is 99.94%.
Embodiment 2
9 L water and 1 kg iron chloride is added in 50 L reactor, stirring, after ferrum to be chlorinated all dissolves, EDTA is slowly added in above-mentioned solution, temperature is risen to 90oC, is then slowly added into sodium bicarbonate 630 g in reactor and makes pH value of solution be adjusted to about 7, and 90oContinue stirring 60 min reaction under C to terminate, reactant liquor is poured in 50 L container tank, add 900 mL ethanol, stir, stand cooling, after 9 h, crystallization content reaches maximum, filter, rinse filter cake with 2.3 L medicinal alcohols, collect filter cake, filter cake is yellow or the khaki graininess powder of uniform loose, 50oC is dried, and obtains FeNaEDTA fine work, and weigh 1.26 kg, yield 88.1%, and purity is 99.96%.
Claims (10)
1. the production technology of high-purity iron supplementary editic acid ferrum sodium (FeNaEDTA), it is characterised in that include following synthesis step:
Iron chloride and Calcium Disodium Versenate are raw material；
With water as reaction dissolvent；
Single step reaction synthesis FeNaEDTA；
Reacting liquid pH value is regulated with sodium bicarbonate；
FeNaEDTA is crystallized with ethanol/water；
Crystallize by washing with alcohol FeNaEDTA again；
High-purity FeNaEDTA is obtained after crystallizing and drying.
2. the production technology of claim 1, it is characterised in that iron chloride molar concentration in water be 0.20 ~ 0.60 mol/L, preferably molar concentration be 0.30 ~ 0.50 mol/L, FeNaEDTA yield reaches 88.1%.
3. the production technology of claim 1, it is characterised in that the mol ratio of iron chloride and EDTA be 1:0.5 ~ 1:1.5, i.e. mass ratio be 45:31 ~ 15:31, preferred molar ratio be 1:0.8 ~ 1:1.2, i.e. mass ratio be 9:10 ~ 9:15.
4. the production technology of claim 1, it is characterised in that charging sequence is first that iron chloride is soluble in water, then is slowly added into EDTA.
5. the production technology of a high-purity iron supplementary FeNaEDTA, it is characterised in that iron chloride and EDTA reaction temperature are 80 ~ 100oC, preferable reaction temperature is 85 ~ 95 oC, calcium lactate purity reaches 99.9%.
6. the production technology of claim 1, it is characterised in that iron chloride and EDTA response time are 30 ~ 90 minutes, preferably response time are 50 ~ 70 minutes, regulate reacting liquid pH value to 6 ~ 8 with sodium bicarbonate.
7. the production technology of claim 1, it is characterised in that after reaction terminates, adds 1/30 ~ 3/10 in reactant liquor, and the medicinal alcohol of preferably 1/20 ~ 2/10 times of water consumption stands crystallization.
8. the production technology of claim 1, it is characterised in that standing crystallization temperature is-5 ~ 15oC, preferably crystallization temperature are 0-10oC；Standing crystallization time is 5 ~ 15 hours, and preferably crystallization time is 8-12 hour.
9. the production technology of claim 1, it is characterised in that after crystallization, washs with the medicinal alcohol of 1/3 ~ 1/5 times of water yield.
10. the production technology of claim 1, it is characterized in that the FeNaEDTA that final filtration obtains is yellow or the khaki graininess powder of uniform loose, under the conditions of appropriate reaction, FeNaEDTA yield can reach 88.1%, purity can reach 99.9%, is suitable on medicine and food application.
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| CN201510022601.7A CN105837461A (en) | 2015-01-17 | 2015-01-17 | Production technology of high purity iron supplement agent sodium feredetate |
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| CN201510022601.7A CN105837461A (en) | 2015-01-17 | 2015-01-17 | Production technology of high purity iron supplement agent sodium feredetate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1192334A (en) * | 1998-01-23 | 1998-09-09 | 北京维他营养保健品公司 | Method for preparing iron enriched nutrient and products thereof |
| CN1390484A (en) * | 2001-06-07 | 2003-01-15 | 李卫平 | Preparing process and product of EDTA iron chelate as nutritive intensifier of food |
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- 2015-01-17 CN CN201510022601.7A patent/CN105837461A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1192334A (en) * | 1998-01-23 | 1998-09-09 | 北京维他营养保健品公司 | Method for preparing iron enriched nutrient and products thereof |
| CN1390484A (en) * | 2001-06-07 | 2003-01-15 | 李卫平 | Preparing process and product of EDTA iron chelate as nutritive intensifier of food |
Non-Patent Citations (1)
| Title |
|---|
| 窦建芝: "乙二胺四乙酸铁钠的制备", 《辽宁化工》 * |
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Application publication date: 20160810 |