CN109893540A - A kind of preparation method and products thereof of the iron sucrose complex solution of low-heavy metal content - Google Patents
A kind of preparation method and products thereof of the iron sucrose complex solution of low-heavy metal content Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods and products thereof of the iron sucrose complex solution of low-heavy metal content.The iron sucrose complex preparation process prepares and purifies technique by unique iron hydroxide intermediate, and technology controlling and process, and the heavy metal for comprehensively considering complex reaction container introduces, heavy metal removing rate can be significantly improved, it is high to solve heavy metal element impurity risk in existing iron sucrose bulk drug technology, the especially high problem of manganese, nickel, cobalt heavy metal element impurity content, effectively reduce the heavy metal toxicity of iron sucrose Intravenous Iron in Maintenance in human body, improve drug safety, and have technological operation simple, it is easy to accomplish industrialized feature.
Description
Technical field
The invention belongs to field of medicaments, and in particular to a kind of preparation side of the iron sucrose complex solution of low-heavy metal content
Method and products thereof.
Background technique
Hypoferric anemia is one kind relatively conventional in anemia in the world, is referred to one caused by internal iron promoter amount is insufficient
The low pigment anemia of kind cell.Iron intake deficiency, excessive, the iron malabsorption of iron loss etc. will lead to the hair of hypoferric anemia
Raw, most efficient method is supplement chalybeate.
Iron sucrose is common Intravenous Supplement chalybeate, have efficiently quickly, accurate positioning, parenteral administration toxicity it is low etc. excellent
Point.On the other hand, iron sucrose is larger as intravenous formulations first use amount, and is to be directly entered blood circulation system, because
This safety is one of significant challenge of this product.The control of content of beary metal is iron sucrose injection safety control
One importance.
Although manganese is a kind of rare element needed by human, but requirement is less, and 10-20mg is only about contained in human body.
And human body when excess intake manganese, will result in following adverse effect: (1) leading to nerve due to diet or in the work environment
The damage of system extrapyramidal tract and corresponding paralysis agitans syndrome.(2) cause manganese poisoning, mental disease can occur in severe
Symptom.It can causing death when human body soakage is 5-10g.
Nickel is the most common sensitization metal, and clinical manifestation is dermatitis and eczema, and nickel allergic dermatitis clinical manifestation is
Itch, papular or papulovesicular dermatitis, with mossization.In addition, the excessive performance of nickel: (1) daily intaking solubility
Nickel 250mg can cause to be poisoned, some people are more sensitive, intake 600 μ g can cause to be poisoned, can lead to cardiac muscle, brain, lung, liver and
Kidney retrogression.(2) drinking nickeliferous high water daily will increase cancer morbidity, and especially own cancer stricken should must during chemicotherapy
It must prevent to contact with nickel product.
Cobalt is a kind of microelement needed by human, is VB12Composition, maintain the normal physiological function of body in
It plays an important role.But human or animal has taken in excessive cobalt, even and it can produce a series of poisoning symptoms death.It is larger
The cobalt of dosage can cause erythremia, the parenchymatous organs such as Thyroid Gland Swell, liver, kidney, pancreas retrogression and interstitial lung fiber
Change, still influence certain parenchymatous organs and there is centainly carcinogenic, teratogenesis and mutagenesis.
ICH Q3D elementary metal impurities guide provides one using risk management principle described in ICH Q9 to assess and control
The method of element impurity in pharmacy product.This method provides one to limit gold in drug based on the platform of risk control strategy
Belong to element impurity.The metallic element assessed in guide is by the way that scientific impurity, Government R & D are reported and studied, international regulations
In standard (being suitable for drug) and guide and the research of regulation authorities and assessment report, the data that the public can obtain are examined
What core obtained.In guideline, manganese, nickel, cobalt heavy metal are respectively 4 classes, 3 classes and 2A dvielement impurity, in injecting drug use
Object is respectively 250 μ g/day, 20 μ g/day and 5 μ g/day with the PDE value (allowing day exposure value) in bulk pharmaceutical chemicals.
Therefore, a kind of iron sucrose complex of low-heavy metal content is developed, it is ensured that this product drug safety avoids a huge sum of money
It is not only particularly significant but also very necessary to belong to accumulation.
Iron sucrose is a kind of water-soluble iron hydroxide sucrose complex, be by ferric hydroxide colloid and sucrose complexing and
At.The study found that molysite-ferric trichloride as iron sucrose key starting material, often gives up since it prepares starting material
Old steel, iron filings, iron ore etc., sources of initial raw materials are complicated, and some heavy metals, such as cobalt, manganese, nickel are usually and ferro element
Association, therefore, the heavy metal element of ferric trichloride, as manganese, nickel, cobalt equal size are often higher.Ferric trichloride content of beary metal is not
It is easy to control, product quality is difficult to stablize, and is the most important source of heavy metal in iron sucrose complex.And presently disclosed sucrose
Iron preparation process is very low to the technique removal rate of heavy metal, this just gives the iron sucrose complex of low-heavy metal content to develop and steady
Fixed production brings huge difficulty.
Iron sucrose preparation process described in technical solution of the present invention is prepared and purified by unique iron hydroxide intermediate
Technique and technology controlling and process, and the heavy metal for comprehensively considering complex reaction container introduces, and can significantly improve heavy metals removal
Rate, it is ensured that sucrose iron product content of beary metal.Iron sucrose of the present invention prepare manganese, nickel, cobalt average removal rate respectively reach
88%, 80%, 71%, it is high to solve in existing iron sucrose bulk drug technology heavy metal element impurity risk, especially manganese,
The high problem of nickel, cobalt heavy metal element impurity content, effectively reduces the heavy metal toxicity of iron sucrose Intravenous Iron in Maintenance in human body,
Drug safety is improved, and has technological operation simple, it is easy to accomplish industrialized feature.
Iron sucrose complex prepared by the present invention has content of beary metal low, and heavy metal free accumulative risk is highly-safe
Advantage.
Summary of the invention
It is compound the purpose of the present invention is in view of the deficiencies of the prior art, providing a kind of iron sucrose of low-heavy metal content
Object solution.
It is a further object of the present invention to provide preparation methods.
The present invention has surprisingly found that iron sucrose preparation process prepares and purifies work by unique iron hydroxide intermediate
Skill and technology controlling and process, and the heavy metal for comprehensively considering complex reaction container introduces, and can significantly improve heavy metals removal
Rate, it is ensured that sucrose iron product content of beary metal.Research is found: iron sucrose prepare manganese, nickel, cobalt average removal rate respectively reach
88%, 80%, 71%, it is high to solve in existing iron sucrose bulk drug technology heavy metal element impurity risk, especially manganese,
The high problem of nickel, cobalt heavy metal element impurity content.
The purpose of the present invention can be achieved through the following technical solutions:
The present invention provides a kind of method of iron sucrose complex solution for being used to prepare low-heavy metal content, including it is following
Step: 1) ferric chloride (FeCl36H2O) and sodium carbonate reaction prepare ferric hydroxide colloid；2) purify water washing purification step 1) in hydrogen
Colloid of iron oxide；3) the ferric hydroxide colloid mixing in sodium hydroxide, sucrose and step 2), it is compound that complex reaction obtains iron sucrose
Object.
Wherein step 1) the following steps are included:
A, sodium carbonate is dissolved in the water, after being heated to 50-80 DEG C, ferric trichloride is added, is stirred to react to solution darkly
After color, filtering removal precipitating, filtrate is cooled to 0-5 DEG C；Wherein, the dosage of the sodium carbonate is theoretically absolutely to react
Natrium carbonicum calcinatum quality 70-75%；Theoretically absolutely the natrium carbonicum calcinatum mass M 2 of reaction is calculated as follows formula:
Wherein, M1 is represented as the quality of ferric chloride (FeCl36H2O)；
B, sodium carbonate liquor is added dropwise in reaction mixture, reaction mixture is risen into pH2-3 in 3-5h, keeps temperature 0-5
DEG C, stir 4-8h；
C, continue that sodium carbonate liquor is added dropwise, until reaction mixture pH7-9, obtains ferric hydroxide colloid.
Step 1) preferably includes following steps:
Sodium carbonate is dissolved in the water by a, and after being heated to 50-60 DEG C, ferric trichloride is added, and is stirred to react to solution in black
Afterwards, filtering removal precipitating, filtrate are cooled to 0-5 DEG C；
Sodium carbonate liquor is added dropwise in b reaction mixture, reaction mixture is risen into pH2.5-2.8 at 4.5-5 hours, keeps
0-5 DEG C of temperature, stir 7-8h；
C continues that sodium carbonate liquor is added dropwise, until reaction mixture pH7.5-9, obtains ferric hydroxide colloid.
Step 1) further preferably the following steps are included:
Sodium carbonate is dissolved in the water by a, and after being heated to 50-60 DEG C, ferric trichloride is added, and is stirred to react to solution in black
Afterwards, filtering removal precipitating, filtrate are cooled to 0-2 DEG C；
Sodium carbonate liquor is added dropwise in b reaction mixture, reaction mixture is risen into pH2.5-2.8 in 4.5-5h, keeps temperature
0-2 DEG C of degree stirs 7-8h；
C continues that sodium carbonate liquor is added dropwise, until reaction mixture pH8-9, obtains ferric hydroxide colloid.
Step 1) still more preferably the following steps are included:
Sodium carbonate is dissolved in the water in a, after being heated to 50-60 DEG C, ferric trichloride is added, is stirred to react to solution darkly
After color, filtering removal precipitating, filtrate is cooled to 0-2 DEG C；
Sodium carbonate liquor is added dropwise in b reaction mixture, reaction mixture is risen into pH2.5-2.8 in 4.5-5h, keeps temperature
0-2 DEG C of degree stirs 7-8h；
C continues that sodium carbonate liquor is added dropwise, and to reaction mixture pH8-9 in 1-2 hours, obtains ferric hydroxide colloid.
The terminal that step 2) is preferably washed, which should control, is washing out purifying water conductivity no more than 3000 μ s/cm；
The preferred glassed steel reaction vessels of reaction vessel in step 3), or its material main component of part contacted with feed liquid is not
It is manganese, cobalt and nickel.
Further preferably, the terminal of step 2) washing, which should control, is washing out purifying water conductivity no more than 1500 μ s/cm；
And the reaction vessel of step 3) is glassed steel reaction vessels, or with feed liquid contact its material main component of part be not manganese,
Cobalt and nickel.
The iron sucrose complex solution of the low-heavy metal content prepared according to the method described above, iron content in complex solution
For 3.5-4.0% (g/g), the content of manganese is not more than 1.5 μ g/mgFe, and the content of nickel is not more than 0.125 μ g/mgFe, and cobalt
Content is not more than 0.035 μ g/mgFe.
Further, iron content is 3.5-4.0% (g/g) in complex solution, and the content of manganese is not more than 1.0 μ g/mgFe,
The content of nickel is not more than 0.0875 μ g/mgFe, and the content of cobalt is not more than 0.025 μ g/mgFe.
Further, iron content is 3.5-4.0% (g/g) in complex solution, and the content of manganese is not more than 0.5 μ g/
MgFe, the content of nickel is not more than 0.0375 μ g/mgFe, and the content of cobalt is not more than 0.01 μ g/mgFe.
Wherein, above-mentioned content of beary metal unit μ g/mgFe is indicated in terms of Fe, often containing 1mg's in iron sucrose complex solution
Element of Fe is the heavy metal containing 1 μ g.
The utility model has the advantages that
Iron sucrose preparation process described in technical solution of the present invention is unique, and heavy metal technique removal rate is high, sucrose iron product
Content of beary metal is low, and it is high to solve in existing iron sucrose bulk drug technology heavy metal element impurity risk, especially manganese, nickel,
The high problem of cobalt heavy metal element impurity content.Iron sucrose complex prepared by the present invention has content of beary metal low, a no huge sum of money
Belong to accumulative risk, highly-safe advantage, and technological operation is simple, it is easy to accomplish industrialized feature.
Specific embodiment
Embodiment 1
110g natrium carbonicum calcinatum, 2.3kg purified water are added in 5L glass flask, stir about 30min dissolution is heated to 80
DEG C, 250g ferric chloride (FeCl36H2O) (manganese content 934ppm, nickel content 48.12ppm, cobalt content 9.88ppm) then is added, stirring is anti-
Should about 15min, black is presented in solution, and filtering, filtrate is transferred in 5L glass flask and is cooled to 5 DEG C.With 20% sodium carbonate liquor
Be added dropwise about 5h adjust reaction solution pH to about 2.0,5 DEG C at be stirred to react about 4h, with 20% sodium carbonate liquor adjust reaction solution pH to
About 7.0, it is filtered after stirring 30min, filter cake is washed repeatedly 4 times with about 5kg purified water, and washing out purifying water conductivity is 3342 μ s/
Cm, gained ferric hydroxide colloid are added sodium hydroxide and adjust reaction solution pH to being not less than 10, and sucrose 1.3kg, heating reaction is added
Liquid is to boiling to get iron sucrose solution 1.21kg.(iron content 3.6%, 1.11 μ g/mgFe of manganese content, 0.089 μ g/ of nickel content
MgFe, 0.0269 μ g/mgFe of cobalt content；Wherein manganese removal rate 79%, nickel removal rate 68%, cobalt removal rate 52%)
Embodiment 2
110g natrium carbonicum calcinatum, 2.3kg purified water are added in 5L glass flask, stir about 30min dissolution is heated to 60
DEG C, 250g ferric chloride (FeCl36H2O) (manganese content 934ppm, nickel content 48.12ppm, cobalt content 9.88ppm) then is added, stirring is anti-
Should about 15min, black is presented in solution, and filtering, filtrate is transferred in 5L glass flask and is cooled to 0 DEG C.With 20% sodium carbonate liquor
Be added dropwise about 5h adjust reaction solution pH to about 3.0,5 DEG C at be stirred to react about 8h, with 20% sodium carbonate liquor adjust reaction solution pH to
About 8.5, it is filtered after stirring 30min, filter cake is washed repeatedly 4 times with about 5kg purified water, and washing out purifying water conductivity is 2490 μ s/
Cm, gained ferric hydroxide colloid are added sodium hydroxide and adjust reaction solution pH to being not less than 10, and sucrose 1.0kg, heating reaction is added
Liquid is to boiling to get iron sucrose solution 1.26kg.(iron content 3.5%, 0.78 μ g/mgFe of manganese content, 0.057 μ g/ of nickel content
MgFe, 0.0234 μ g/mgFe of cobalt content；Wherein manganese removal rate 85%, nickel removal rate 79%, cobalt removal rate 58%)
Embodiment 3
105g natrium carbonicum calcinatum, 2.3kg purified water are added in 5L glass flask, stir about 30min dissolution is heated to 50
DEG C, 250g ferric chloride (FeCl36H2O) (manganese content 934ppm, nickel content 48.12ppm, cobalt content 9.88ppm) then is added, stirring is anti-
Should about 15min, black is presented in solution, and filtering, filtrate is transferred in 5L glass flask and is cooled to 5 DEG C.With 20% sodium carbonate liquor
Be added dropwise about 3h adjust reaction solution pH to about 2.3,5 DEG C at be stirred to react about 8h, with 20% sodium carbonate liquor adjust reaction solution pH to
About 8.2, it is filtered after stirring 30min, filter cake is washed repeatedly 5 times with about 5kg purified water, and washing out purifying water conductivity is 1216 μ s/
Cm, gained ferric hydroxide colloid are added sodium hydroxide and adjust reaction solution pH to being not less than 10, and sucrose 0.9kg, heating reaction is added
Liquid is to boiling to get iron sucrose solution 1.24kg.(iron content 3.8%, 0.58 μ g/mgFe of manganese content, 0.052 μ g/ of nickel content
MgFe, 0.0179 μ g/mgFe of cobalt content；Wherein manganese removal rate 88%, nickel removal rate 80%, cobalt removal rate 66%)
Embodiment 4
110g natrium carbonicum calcinatum, 2.3kg purified water are added in 5L glass flask, stir about 30min dissolution is heated to 60
DEG C, 250g ferric chloride (FeCl36H2O) (manganese content 934ppm, nickel content 48.12ppm, cobalt content 9.88ppm) then is added, stirring is anti-
Should about 15min, black is presented in solution, and filtering, filtrate is transferred in 5L glass flask and is cooled to 0 DEG C.With 20% sodium carbonate liquor
It is added dropwise at reaction solution pH to about 2.8,0 DEG C of about 4.5h adjusting and is stirred to react about 7h, adjust reaction solution pH with 20% sodium carbonate liquor
To about 7.5, filtered after stirring 30min, filter cake is washed repeatedly 5 times with about 5kg purified water, and washing out purifying water conductivity is 1030 μ
S/cm, gained ferric hydroxide colloid are added sodium hydroxide and adjust reaction solution pH to being not less than 10, sucrose 1.0kg are added, heating is anti-
Answer liquid to boiling to get iron sucrose solution 1.21kg.(iron content 4.0%, 0.52 μ g/mgFe of manganese content, 0.042 μ g/ of nickel content
MgFe, 0.0083 μ g/mgFe of cobalt content；Wherein manganese removal rate 89%, nickel removal rate 83%, cobalt removal rate 84%)
Embodiment 5
105g natrium carbonicum calcinatum, 2.3kg purified water are added in 5L glass flask, stir about 30min dissolution is heated to 50
DEG C, 250g ferric chloride (FeCl36H2O) (manganese content 934ppm, nickel content 48.12ppm, cobalt content 9.88ppm) then is added, stirring is anti-
Should about 15min, black is presented in solution, and filtering, filtrate is transferred in 5L glass flask and is cooled to 2 DEG C.With 20% sodium carbonate liquor
It is added dropwise at reaction solution pH to about 2.7,2 DEG C of about 4.5h adjusting and is stirred to react about 7h, about 2h is added dropwise with 20% sodium carbonate liquor and adjusts
Reaction solution pH to about 8.0 is filtered after stirring 30min, and filter cake is washed repeatedly 4 times with about 5kg purified water, washes out purifying water conductivity
For 1350 μ s/cm, gained ferric hydroxide colloid is added sodium hydroxide and adjusts reaction solution pH to being not less than 10, and sucrose is added
0.9kg, heating reaction solution to boiling is to get iron sucrose solution 1.19kg.(iron content 3.6%, 0.24 μ g/mgFe of manganese content, nickel contain
Measure 0.016 μ g/mgFe, 0.0050 μ g/mgFe of cobalt content；Wherein manganese removal rate 96%, nickel removal rate 94%, cobalt removal rate
91%)
6 large scale preparation of embodiment
31kg natrium carbonicum calcinatum, 700kg purified water are added in 1000L glassed steel reaction vessels, stir about 60min dissolution,
60 DEG C are heated to, 75kg ferric chloride (FeCl36H2O) (manganese content 695ppm, nickel content 21.07ppm, cobalt content is then added
8.34ppm), it is stirred to react about 1.5h, black is presented in solution, and filter filters pressing is into 1000L glassed steel reaction vessels and is cooled to 2
℃.It is added dropwise at reaction solution pH to about 2.5,2 DEG C of about 5h adjusting with 20% sodium carbonate liquor and is stirred to react 8h, it is molten with 20% sodium carbonate
Liquid adjusts reaction solution pH to about 9.0, filters pressing after stir about 1.5h, and filter cake is washed repeatedly 4 times with about 900kg purified water, washes out pure
Changing water conductivity is 1435 μ s/cm, and resulting ferric hydroxide colloid is added sodium hydroxide and adjusts reaction solution pH to being not less than 10, adds
Enter sucrose 220kg, heating reaction solution to boiling is to get iron sucrose solution 376kg.(iron content 3.7%, 0.32 μ g/ of manganese content
MgFe, 0.030 μ g/mgFe of nickel content, 0.0111 μ g/mgFe of cobalt content；Wherein manganese removal rate 91%, nickel removal rate 74%, cobalt
Removal rate 75%)
Comparative example 1
125g natrium carbonicum calcinatum, 2.3kg purified water are added in 5L glass flask, stir about 30min dissolution is heated to 40
DEG C, 250g ferric chloride (FeCl36H2O) (manganese content 934ppm, nickel content 48.12ppm, cobalt content 9.88ppm) then is added, stirring is anti-
Should about 15min, black is presented in solution, and filtering, filtrate is transferred in 5L glass flask and is cooled to 10 DEG C.With 20% sodium carbonate liquor
It is added dropwise at reaction solution pH to about 5.0,10 DEG C of about 6h adjusting and is stirred to react about 3h, about 4h is added dropwise with 20% sodium carbonate liquor and adjusts instead
Liquid pH to about 9.5 is answered, is filtered after stirring 30min, filter cake is washed repeatedly 5 times with about 5kg purified water, is washed out purifying water conductivity and is
2100 μ s/cm, gained ferric hydroxide colloid are added sodium hydroxide and adjust reaction solution pH to being not less than 10, and sucrose 0.9kg is added,
Reaction solution is heated to boiling to get iron sucrose solution 1.20kg.(iron content 3.8%, 2.26 μ g/mgFe of manganese content, nickel content
0.196 μ g/mgFe, 0.0445 μ g/mgFe of cobalt content；Wherein manganese removal rate 56%, nickel removal rate 26%, cobalt removal rate 18%)
Comparative example 2
125g natrium carbonicum calcinatum, 2.3kg purified water are added in 5L glass flask, stir about 30min dissolution is heated to
100 DEG C, 250g ferric chloride (FeCl36H2O) (manganese content 934ppm, nickel content 48.12ppm, cobalt content 9.88ppm) then is added, stirs
Reaction about 15min is mixed, black, filtering is presented in solution, and filtrate is transferred in 5L glass flask and is cooled to 15 DEG C.With 20% sodium carbonate
Solution is added dropwise at reaction solution pH to about 4.0,15 DEG C of about 2h adjusting and is stirred to react about 1h, and about 5h tune is added dropwise with 20% sodium carbonate liquor
Reaction solution pH to about 9.2 is saved, is filtered after stirring 30min, filter cake is washed repeatedly 4 times with about 5kg purified water, washes out purified water conductance
Rate is 1874 μ s/cm, and gained ferric hydroxide colloid is added sodium hydroxide and adjusts reaction solution pH to being not less than 10, and sucrose is added
0.9kg, heating reaction solution to boiling is to get iron sucrose solution 1.25kg.(iron content 3.7%, 1.84 μ g/mgFe of manganese content, nickel contain
Measure 0.241 μ g/mgFe, 0.0378 μ g/mgFe of cobalt content；Wherein manganese removal rate 63%, nickel removal rate 8%, cobalt removal rate 29%)
。
Claims (11)
1. a kind of preparation method of the iron sucrose complex of low-heavy metal content, comprising the following steps: 1) ferric chloride (FeCl36H2O) and
Sodium carbonate reaction, prepares ferric hydroxide colloid；2) purify water washing purification step 1) in ferric hydroxide colloid；3) sodium hydroxide,
Ferric hydroxide colloid mixing in sucrose and step 2), complex reaction obtain iron sucrose complex；It is characterized in that step 1) is wrapped
Include following steps:
A, sodium carbonate is dissolved in the water, after being heated to 50-80 DEG C, ferric trichloride is added, be stirred to react after being in black to solution,
Filtering removal precipitating, filtrate are cooled to 0-5 DEG C；Wherein, the dosage of the sodium carbonate is the nothing theoretically absolutely reacted
The 70-75% of aqueous sodium carbonate quality；Theoretically absolutely the natrium carbonicum calcinatum mass M 2 of reaction is calculated as follows formula:
Wherein, M1 is represented as the quality of ferric chloride (FeCl36H2O)；
B, sodium carbonate liquor is added dropwise in reaction mixture, reaction mixture is risen into pH2-3 in 3-5h, is kept for 0-5 DEG C of temperature, stirred
Mix 4-8h；
C, continue that sodium carbonate liquor is added dropwise, until reaction mixture pH7-9, obtains ferric hydroxide colloid.
2. the preparation method of the iron sucrose complex of low-heavy metal content as claimed in claim 1, it is characterised in that step 2) washing
Terminal should control and washing out purifying water conductivity no more than 3000 μ s/cm.
3. the iron sucrose complex preparation method of low-heavy metal content as claimed in claim 1, it is characterised in that the reaction of step 3)
Container is glassed steel reaction vessels, or its material main component of part contacted with feed liquid is not the reaction vessel of manganese, cobalt and nickel.
4. the preparation method of the iron sucrose complex of low-heavy metal content as claimed in claim 1, it is characterised in that step 2) washing
Terminal should control and washing out purifying water conductivity no more than 1500 μ s/cm；And the reaction vessel of step 3) is that enamel is anti-
Kettle is answered, or its material main component of part contacted with feed liquid is not the reaction vessel of manganese, cobalt and nickel.
5. the iron sucrose complex preparation method of low-heavy metal content as claimed in claim 4, it is characterised in that step 1) packet
Include following steps:
Sodium carbonate is dissolved in the water by a, and after being heated to 50-60 DEG C, ferric trichloride is added, and is stirred to react after being in black to solution,
Filtering removal precipitating, filtrate are cooled to 0-5 DEG C；
Sodium carbonate liquor is added dropwise in b reaction mixture, reaction mixture is risen into pH2.5-2.8 at 4.5-5 hours, keeps temperature
0-5 DEG C, stir 7-8h；
C continues that sodium carbonate liquor is added dropwise, until reaction mixture pH7.5-9, obtains ferric hydroxide colloid.
6. the iron sucrose complex preparation method of low-heavy metal content as claimed in claim 5, it is characterised in that step 1) packet
Include following steps:
Sodium carbonate is dissolved in the water by a, and after being heated to 50-60 DEG C, ferric trichloride is added, and is stirred to react after being in black to solution,
Filtering removal precipitating, filtrate are cooled to 0-2 DEG C；
Sodium carbonate liquor is added dropwise in b reaction mixture, reaction mixture is risen into pH2.5-2.8 in 4.5-5h, keeps temperature 0-2
DEG C, stir 7-8h；
C continues that sodium carbonate liquor is added dropwise, until reaction mixture pH8-9, obtains ferric hydroxide colloid.
7. the iron sucrose complex preparation method of low-heavy metal content as claimed in claim 6, it is characterised in that step 1) packet
Include following steps:
Sodium carbonate is dissolved in the water by a, and after being heated to 50-60 DEG C, ferric trichloride is added, and is stirred to react after being in black to solution,
Filtering removal precipitating, filtrate are cooled to 0-2 DEG C；
Sodium carbonate liquor is added dropwise in b reaction mixture, reaction mixture is risen into pH2.5-2.8 in 4.5-5h, keeps temperature 0-2
DEG C, stir 7-8h；
C continues that sodium carbonate liquor is added dropwise, and to reaction mixture pH8-9 in 1-2 hours, obtains ferric hydroxide colloid.
8. the iron sucrose complex solution of the low-heavy metal content of preparation method preparation according to claim 1, feature
It is in complex solution that iron content is 3.5-4.0wt%.
9. the iron sucrose complex solution of low-heavy metal content as claimed in claim 7 or 8, it is characterised in that the content of manganese is not
Greater than 1.5 μ g/mgFe, the content of nickel is not more than 0.125 μ g/mgFe, and the content of cobalt is not more than 0.035 μ g/mgFe.
10. the iron sucrose complex solution of low-heavy metal content as claimed in claim 9, it is characterised in that the content of manganese is little
In 1.0 μ g/mgFe, the content of nickel is not more than 0.0875 μ g/mgFe, and the content of cobalt is not more than 0.025 μ g/mgFe.
11. the iron sucrose complex solution of low-heavy metal content as claimed in claim 9, it is characterised in that the content of manganese is little
In 0.5 μ g/mgFe, the content of nickel is not more than 0.0375 μ g/mgFe, and the content of cobalt is not more than 0.01 μ g/mgFe.
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| WO2022072439A1 (en) * | 2020-09-29 | 2022-04-07 | Lg Bionano Co. Ltd | Methods of preparing iron complexes |
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