CN106809881A - A kind of preparation method of iron ammonium sulfate - Google Patents
A kind of preparation method of iron ammonium sulfate Download PDFInfo
- Publication number
- CN106809881A CN106809881A CN201611078203.8A CN201611078203A CN106809881A CN 106809881 A CN106809881 A CN 106809881A CN 201611078203 A CN201611078203 A CN 201611078203A CN 106809881 A CN106809881 A CN 106809881A
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- Prior art keywords
- ammonium sulfate
- preparation
- heating
- iron
- iron ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The present invention provides a kind of preparation method of iron ammonium sulfate, including iron filings is purified, pickling dissolving, is filtered while hot, adds saturated ammonium sulfate solution, and stirring, heating concentration, crystallization, washing is drained.The purification is that iron filings are put into container, adds the Na2CO3 solution of 1.0moL/L, heating to use distillation water washing iron filings to neutrality after boiling 5min, then uses absolute ethanol washing.Dry again.The pickling dissolving refers to that the iron filings after treatment are put into container, adds 1moL/LH2SO4,10 ~ 15min of heating water bath to be simultaneously stirred toward container.This method is simple and practical, low cost, and the product purity for obtaining is high.
Description
Technical field
The invention belongs to chemical field, more particularly to a kind of preparation method of iron ammonium sulfate.
Background technology
It is usually to be directly added into ammonium sulfate toward ferrous sulfate to carry out heating concentration to prepare iron ammonium sulfate, but so
The general purity of technique it is low, conversion ratio is not high.
The content of the invention
In order to overcome above-mentioned preparation process produced problem, the present invention provides a kind of preparation method of iron ammonium sulfate, bag
Include iron filings are purified, pickling dissolving, filter while hot, add saturated ammonium sulfate solution, stirring, heating concentration, crystallization, washing
Drain.
Preferably, it is in the preparation method of described iron ammonium sulfate, the Na2CO3 of required iron filings addition 1.0moL/L is molten
Liquid, heating uses distillation water washing iron filings to neutrality after boiling 5min, then with absolute ethanol washing, then dries rear stand-by.
Preferably, in the preparation method of described iron ammonium sulfate, iron filings are put into container, 1moL/ is added toward container
LH2SO45mL, 10 ~ 15min of heating water bath and during being stirred, temperature need to be controlled between 60 ~ 70 degrees Celsius, prevented
Reaction is excessively fierce.
Preferably, in the preparation method of described iron ammonium sulfate, need to be counted with PH constantly measuring molten in pickling course of dissolution
The pH value of liquid, when pH value is measured more than 1.0, adds the pH value of the sulfuric acid regulation solution of 3.0moL/L to be less than 1.
Preferably, in the preparation method of described iron ammonium sulfate, in the pickling dissolving, when there is crystal in heating stirring
Add the distilled water of 1.5 ~ 2mL.
Further, in the preparation method of described iron ammonium sulfate, filtered while hot after pickling dissolving, had during filtering
Crystallization appearance need to be washed with 3.0moL/L sulfuric acid, and cleaning solution is attached in filtrate.
Preferably, in the preparation method of described iron ammonium sulfate, the saturation copperas solution adds equimolar
After amount saturated ammonium sulfate solution is stirred, gained mixed liquor need to heat concentration in steam bath, and heating concentration process can not be stirred
Mix.
Preferably, in the preparation method of described iron ammonium sulfate, l ferrous ammonium sulfate solution heating is concentrated into just to be occurred
Stop heating during a thin layer of crystal, taking down standing from steam bath is cooled to room temperature, carry out filtration under diminished pressure, crystallization.
Preferably, in the preparation method of described iron ammonium sulfate, the crystal for obtaining need to be washed with 1.0mL95% ethanol
Wash, be placed into bottle,suction and drained.
The present invention provides a kind of preparation method of iron ammonium sulfate, including iron filings are purified, pickling dissolving, while hot mistake
Filter, adds saturated ammonium sulfate solution, and stirring, heating concentration, crystallization, washing is drained, and the iron ammonium sulfate purity of preparation is high, makes
Simplicity, required expense is low.
Specific embodiment
With reference to case study on implementation, the present invention is described further.
Case study on implementation 1
The present invention prepares iron ammonium sulfate and comprises the following steps：
1st, clean iron filings are prepared：
5g iron filings are put into evaporating dish, add the Na2CO3 solution of 1.0moL/L, heating to use distillation water washing after boiling 5min
Iron filings to neutrality removes degreasing, then with absolute ethanol washing, then dries rear stand-by.
2nd, copperas solution is prepared：
During the iron filings of step 1 gained are put into container, the sulfuric acid of 3.0moL/L is added, 10 ~ 15min of heating water bath, reaction is opened
Notice that temperature can not be improved during the beginning, whole course of reaction temperature control prevents reaction excessively fierceness from causing molten at 60 ~ 70 degrees Celsius
Liquid is emerged, and pH value is maintained at less than 1.0, and pH value is adjusted with the sulfuric acid of 3.0moL/L, ferrous sulfate can only exist it is acid compared with
In strong solution.
In heating process, in order to prevent errous sulfate crystal from separating out, the distilled water of 1.5 ~ 2mL is added, when reaction is carried out
After being dissolved substantially to solid, filter while hot and solution is filled into evaporating dish, crystal precipitation is had during filtering, with 3.0moL/L's
Sulfuric acid is washed, and cleaning solution pours into stand-by in filtrate.
Reaction equation is：Fe+H2SO4=FeSO4+H2↑
3rd, iron ammonium sulfate is prepared
The saturated ammonium sulfate solution of equimolar amount is added toward step 2 resulting solution, is 1.5mL in this method, use glass bar
It is stirring evenly and then adding into evaporating dish, is placed into heating concentration in steam bath, heating concentration process can not be stirred, Deng Daorong
When liquid surface separates out a thin layer of crystallization, evaporating dish is removed from steam bath, standing is cooled to room temperature, separates out partial crystals,
Gained solidliquid mixture is put into Buchner funnel, filtration under diminished pressure is carried out with bottle,suction, by the gained crystal second of 1.0mL95%
Alcohol washs crystal, and the crystal after washing is drained in putting into clean bottle,suction, obtains finished product.
Because the solubility of iron ammonium sulfate is far smaller than to constitute his compound, sulfuric acid is prepared using above method
Ferrous ammonium.
Reaction equation is：FeSO4+（NH4）2SO4+6H2O=（NH4）2Fe（SO4）2·6H2O
The present invention provides a kind of preparation method of iron ammonium sulfate, including iron filings is purified, pickling dissolving, is filtered while hot,
Saturated ammonium sulfate solution is added, stirring, heating concentration, crystallization, washing is drained.The purification is that iron filings are put into container, plus
Enter the Na2CO3 solution of 1.0moL/L, heating is used distillation water washing iron filings to neutrality, then washed with absolute ethyl alcohol after boiling 5min
Wash.Dry again.The pickling dissolving refers to that the iron filings after treatment are put into container, and 1moL/LH2SO4 is added toward container, and water-bath adds
10 ~ 15min of heat is simultaneously stirred.This method is simple and practical, low cost, and the product purity for obtaining is high.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in specification and implementation method
Utilization, it can be applied to various suitable the field of the invention completely, for those skilled in the art, can be easy
Realize other modification, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not
It is limited to specific details and shown here as the case study on implementation with description.
Claims (9)
1. a kind of preparation method of iron ammonium sulfate, including iron filings are purified, pickling dissolving, is filtered while hot, add saturation
Ammonium sulfate, stirring, heating concentration, crystallization, washing is drained, it is characterised in that：Iron filings are put into container, added toward container etc.
The 1moL/LH2SO4 of the amount of material, 10 ~ 15min of heating water bath are simultaneously stirred, and filter on evaporating dish while hot, toward evaporating dish
Upper addition saturated ammonium sulfate solution 1.5mL stirrings, heating evaporation concentration, cooling, filtration under diminished pressure, washing is drained.
2. the preparation method of a kind of iron ammonium sulfate according to claim 1, it is characterised in that：The iron filings need to add
The Na2CO3 solution of 1.0moL/L, heating uses distillation water washing iron filings to neutrality after boiling 5min, then with absolute ethanol washing,
Dry again rear stand-by.
3. the preparation method of a kind of iron ammonium sulfate according to claim 1, it is characterised in that：Course of dissolution is write in the calculation
Middle temperature control is between 60 ~ 70 degrees Celsius.
4. the preparation method of a kind of iron ammonium sulfate according to claim 3, it is characterised in that：In the pickling dissolving,
Heating stirring occurs adding distilled water during crystal.
5. the preparation method of a kind of iron ammonium sulfate according to claim 1, it is characterised in that：The pickling course of dissolution
The middle pH value that constantly measurement solution need to be counted with PH, when pH value is measured more than 1.0, adds the sulfuric acid regulation solution of 3.0moL/L
PH value is less than 1.
6. the preparation method of a kind of iron ammonium sulfate according to claim 1, it is characterised in that：Taken advantage of after pickling dissolving
Heat filtering, has crystallization appearance to be washed with 3.0moL/L sulfuric acid during filtering, cleaning solution is attached in filtrate.
7. the preparation method of a kind of iron ammonium sulfate according to claim 1 or 2 or 3 or 4 or 5 or 6, it is characterised in that：
After the saturation copperas solution adds equimolar amount saturated ammonium sulfate solution to be stirred, gained mixed liquor need to be in steam
Concentration is heated in bath, heating concentration process can not be stirred.
8. the preparation method of a kind of iron ammonium sulfate according to claim 7, it is characterised in that：The iron ammonium sulfate is molten
Liquid heating is concentrated into and stops heating when just there is a thin layer of crystal, and taking down standing from steam bath is cooled to room temperature, enters
Row filtration under diminished pressure, crystallization.
9. the preparation method of a kind of iron ammonium sulfate according to claim 8, it is characterised in that：The crystal need to use 95%
Ethanol is washed, and is drained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611078203.8A CN106809881A (en) | 2016-11-30 | 2016-11-30 | A kind of preparation method of iron ammonium sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611078203.8A CN106809881A (en) | 2016-11-30 | 2016-11-30 | A kind of preparation method of iron ammonium sulfate |
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| Publication Number | Publication Date |
|---|---|
| CN106809881A true CN106809881A (en) | 2017-06-09 |
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ID=59106141
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611078203.8A Pending CN106809881A (en) | 2016-11-30 | 2016-11-30 | A kind of preparation method of iron ammonium sulfate |
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| Country | Link |
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| CN (1) | CN106809881A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111847520A (en) * | 2020-08-07 | 2020-10-30 | 攀枝花学院 | Preparation method of ammonium ferrous sulfate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1138009A (en) * | 1996-03-28 | 1996-12-18 | 西安交通大学 | Method for production of ferrous sulfate and ferrous ammonium sulfate |
-
2016
- 2016-11-30 CN CN201611078203.8A patent/CN106809881A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1138009A (en) * | 1996-03-28 | 1996-12-18 | 西安交通大学 | Method for production of ferrous sulfate and ferrous ammonium sulfate |
Non-Patent Citations (1)
| Title |
|---|
| 黎春秀等: "《普通化学实验》", 30 April 2015, 中国环境出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111847520A (en) * | 2020-08-07 | 2020-10-30 | 攀枝花学院 | Preparation method of ammonium ferrous sulfate |
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Application publication date: 20170609 |