CN106810439A - A kind of three oxalate closes the synthetic method of potassium ferrite - Google Patents
A kind of three oxalate closes the synthetic method of potassium ferrite Download PDFInfo
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- CN106810439A CN106810439A CN201611086121.8A CN201611086121A CN106810439A CN 106810439 A CN106810439 A CN 106810439A CN 201611086121 A CN201611086121 A CN 201611086121A CN 106810439 A CN106810439 A CN 106810439A
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- oxalate
- synthetic method
- closes
- oxalic acid
- potassium ferrite
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/418—Preparation of metal complexes containing carboxylic acid moieties
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compounds Of Iron (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of three oxalate and closes the synthetic method of potassium ferrite, including iron ammonium sulfate solid is dissolved, plus sulfuric acid and oxalic acid, centrifugation, washing of precipitate adds Potassium Oxalate Solution, heating water bath, hydrogen peroxide is added, is heated up and is added oxalic acid, stirring and dissolving, add ethanol, stand still for crystals, washing precipitation, depressurize suction filtration.This method is simple and practical, and the product purity for obtaining is high.
Description
Technical field：
The invention belongs to chemical field, more particularly to a kind of three oxalate closes the synthetic method of potassium ferrite.
Background technology：
The synthetic method usually potassium permanganate for preparing three oxalates conjunction potassium ferrite is aoxidized, and is concentrated with the aqueous solution and separated out, but
It is that the general impurity of such technique is more, conversion ratio is not high.
The content of the invention：
In order to overcome above-mentioned preparation process produced problem, the present invention provides the synthetic method that a kind of three oxalate closes potassium ferrite,
Including iron ammonium sulfate solid is dissolved, plus sulfuric acid and oxalic acid, centrifugation, washing of precipitate adds Potassium Oxalate Solution,
Heating water bath, adds hydrogen peroxide, heats up and adds oxalic acid, and stirring and dissolving adds ethanol, stands still for crystals, and washing precipitation, decompression is taken out
Filter.
Preferably, during three oxalate closes the synthetic method of potassium ferrite, iron ammonium sulfate solid is dissolved in water, and uses
3.0mol/L sulfuric acid regulation solutions PH be 3.0 ~ 4.5, add 1.0mol/L oxalic acid, be constantly stirred and rub chamber wall until
Light yellow ferrous oxalate is no longer produced to precipitate.
Preferably, during three oxalate closes the synthetic method of potassium ferrite, solution is centrifuged using centrifuge
Afterwards, carefully supernatant is sucked with pipette, and with distilled water by washing of precipitate, discards cleaning solution, retain precipitation.
Preferably, during three oxalate closes the synthetic method of potassium ferrite, add saturated oxalic acid molten toward ferrous oxalate precipitation
After liquid, container is put into 40 degrees Celsius of water-bath and is heated, and stir the amount that side is added dropwise the material of 0.5 gallic acid acid ferrous ammonium
3% hydrogenperoxide steam generator.
Preferably, described three oxalates are closed in the synthetic method of potassium ferrite, are dripped water-bath after hydrogenperoxide steam generator
To 90 degrees Celsius, slow oxalic acid to precipitation just dissolves, and obtains green solution for temperature lifting.
Further, three described oxalates are closed in the synthetic method of potassium ferrite, and peer is added toward the green solution
Water-bath is removed immediately after 95% long-pending ethanol, and crystallisation by cooling is stood in shady place.
Preferably, three described oxalates are closed in the synthetic method of potassium ferrite, and the oxalate of three water of green crystal three closes ferrous acid
After potassium crystal is separated out, supernatant is sucked with pipette, with 1:After 1 ethanol washing precipitation decompression suction filtration is carried out with Buchner funnel.
The present invention provides a kind of three oxalate and closes the synthetic method of potassium ferrite, including iron ammonium sulfate solid is carried out molten
Solution, plus sulfuric acid and oxalic acid, centrifugation, washing of precipitate adds Potassium Oxalate Solution, and heating water bath adds hydrogen peroxide, heats up
Oxalic acid is added, stirring and dissolving adds ethanol, stands still for crystals, washing precipitation, and depressurize suction filtration.This method is simple and practical, the product for obtaining
Product purity is high.
Brief description of the drawings：
Accompanying drawing 1 is the synthesis specific steps that a kind of three oxalic acid closes potassium ferrite
Specific embodiment：
With reference to case study on implementation, the present invention is described further.
Case study on implementation 1
Referring to the drawings 1, the synthetic method that three oxalate of the invention closes potassium ferrite is comprised the following steps：
1st, ferrous oxalate precipitation is prepared：
Addition 0.4g iron ammonium sulfates, 0.3mL3.0mol/L sulfuric acid and 1.5mL distilled water in 10mL centrifuge tubes, stirring and dissolving,
2.5mL1.0mol/L oxalic acid is added, stir and rub test tube wall about 15min, precipitate the lurid ferrous oxalate of generation.
Reaction equation is：（NH4）2Fe（SO4）2·6H2O+H2C2O4=FeC2O4+（NH4）2SO4+H2SO4+4H2O
2nd, centrifugal treating：
The mixture of step 1 gained is put into centrifuge and is centrifuged, supernatant is carefully sucked with pipette, use 2mL
Distillation water washing precipitation once, retains precipitation.
3rd, three oxalates are prepared and closes potassium ferrite
1.0mL saturated oxalic acid potassium solutions are added toward step 2 gained precipitation, test tube is put into the water-bath of 40 degrees Celsius of water temperature and is added
Heat, is added dropwise 2.0mL3% hydrogenperoxide steam generators while stirring, and control is added in 5min or so, and at this moment precipitation becomes yellowish-brown, Fe2+
It is changed into Fe3+。
Bath temperature is increased to 90 degrees Celsius, 0.8mL1.0mol/L oxalic acid is added toward centrifuge tube, stirring makes precipitation molten
Solution, then 3.0mL95% ethanol is added toward solution, water-bath is removed immediately, standing crystallisation by cooling is carried out in the dark, treat the oxalic acid of three water three
After root closes the precipitation of potassium ferrite crystal, supernatant is sucked with pipette, with 1:1 ethanol washing precipitation, filtration under diminished pressure obtains finished product.
Reaction equation is：2FeC2O4·2H2O+H2O2+H2C2O4+3K2C2O4=2K3[Fe（C2O4）3]·3H2O
The present invention provides a kind of three oxalate and closes the synthetic method of potassium ferrite, including iron ammonium sulfate solid is dissolved, plus
Sulfuric acid and oxalic acid, centrifugation, washing of precipitate adds Potassium Oxalate Solution, and heating water bath adds hydrogen peroxide, heats up and add grass
Acid, stirring and dissolving adds ethanol, stands still for crystals, washing precipitation, and depressurize suction filtration.This method is simple and practical, low cost, obtains
Product purity 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 (7)
1. a kind of three oxalate closes the synthetic method of potassium ferrite, with ferrous sulfate as raw material, comprises the following steps that：
Iron ammonium sulfate solid is dissolved in water, and is 3.0 ~ 4.5 with sulfuric acid regulation solution PH, adds oxalic acid and stirs to not in generation
Precipitation；
Centrifugation, discards washing lotion after cleaning precipitation with distilled water, retain precipitation；
The Potassium Oxalate Solution and iron ammonium sulfate added by 0.5 times of the amount of iron ammonium sulfate material added by 1.5 times are added toward precipitation
The hydrogen peroxide of the amount of material, heating water bath；
Oxalic acid is added toward gained mixture to be completely dissolved until precipitating, add the ethanol with solution even, cooling and standings, knot
It is brilliant；
After crystallization is separated out, supernatant is sucked, precipitation, filtration under diminished pressure are washed with ethanol.
2. a kind of three oxalate according to claim 1 closes the synthetic method of potassium ferrite, it is characterised in that：Described in step a
Sulfuric acid concentration is 3.0mol/L, and the concentration of oxalic acid is 1.0mol/L.
3. a kind of three oxalate according to claim 1 and 2 closes the synthetic method of potassium ferrite, it is characterised in that：Step a institutes
State add oxalic acid after solution need to be stirred and rub chamber wall until no longer produce precipitation.
4. a kind of three oxalate according to claim 3 closes the synthetic method of potassium ferrite, it is characterised in that：Step b solution
Carefully suck supernatant with pipette after centrifugation carries out distillation water washing again.
5. a kind of three oxalate according to claim 1 closes the synthetic method of potassium ferrite, it is characterised in that：Step c need to be
Carried out in 40 degrees Celsius of heating water bath, added oxalic acid solution is saturated oxalic acid solution, hydrogen peroxide mass concentration is 3%, on one side
Stirring is while be added dropwise hydrogen peroxide.
6. a kind of three oxalate closes the synthetic method of potassium ferrite according to claim 1 or 5, it is characterised in that：Step d exists
Bath temperature should be increased to 90 degrees Celsius before adding oxalic acid, standing cooling need to be carried out in the dark.
7. a kind of three oxalate according to claim 1 or 2 or 5 closes the synthetic method of potassium ferrite, it is characterised in that：Step
E carefully sucks supernatant and uses 1 after the oxalate of green crystal three conjunction potassium ferrite is no longer separated out with pipette：1 ethanol washing is heavy
You is formed sediment, bottle,suction filtration under diminished pressure is used, crystal is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611086121.8A CN106810439A (en) | 2016-11-30 | 2016-11-30 | A kind of three oxalate closes the synthetic method of potassium ferrite |
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| CN201611086121.8A CN106810439A (en) | 2016-11-30 | 2016-11-30 | A kind of three oxalate closes the synthetic method of potassium ferrite |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358777A (en) * | 2018-04-18 | 2018-08-03 | 武汉科技大学 | A kind of preparation method based on three three potassium ferric oxalates of hydration containing vanadium solution |
-
2016
- 2016-11-30 CN CN201611086121.8A patent/CN106810439A/en not_active Withdrawn
Non-Patent Citations (7)
| Title |
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| 任铁强； 孙悦； 乔庆东；: "合成草酸亚铁实验条件的考察", 《化工科技》 * |
| 刘亚楠； 刘葵； 苏秀荣: "硫酸亚铁铵、三草酸合铁(Ⅲ)酸钾的制备及其测定", 《 中国现代教育装备 》 * |
| 卢季红； 高翔； 胡兴龙； 黄家业； 廖源；: "无机化学实验教学中对三草酸合铁(Ⅲ) 酸钾制备的实验改进", 《 教育文化论坛》 * |
| 孙悦； 乔庆东；: "合成草酸亚铁的反应时间对组成的影响", 《 辽宁石油化工大学学报》 * |
| 李芳； 陈静芬； 李灵丽； 贾文平；: "三草酸合铁(Ⅲ)酸钾制备条件的优化", 《 台州学院学报》 * |
| 肖圣雄； 王晓伦； 柏爱玲； 杨斌姣； 郭贤丽； 张禹； 蒋建宏；: "三草酸合铁(Ⅲ)酸钾合成方法的改进", 《 大学化学》 * |
| 苏碧云； 李晓腾； 王家祥； 王旭东: "三草酸合铁(Ⅲ)酸钾的合成方法研究", 《 化工管理》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358777A (en) * | 2018-04-18 | 2018-08-03 | 武汉科技大学 | A kind of preparation method based on three three potassium ferric oxalates of hydration containing vanadium solution |
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Application publication date: 20170609 |