CN104003450A - Method for preparing ferrous chloride - Google Patents
Method for preparing ferrous chloride Download PDFInfo
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- CN104003450A CN104003450A CN201410234117.6A CN201410234117A CN104003450A CN 104003450 A CN104003450 A CN 104003450A CN 201410234117 A CN201410234117 A CN 201410234117A CN 104003450 A CN104003450 A CN 104003450A
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Abstract
The invention discloses a method for preparing series ferrous chloride. The method comprises the steps: dissolving iron chippings or iron sheets into a hydrochloric solution, then, carrying out depressurized concentration at the pH value being smaller than 1 and the temperature of 70-110 DEG C until the specific weight is 1.30-1.80g/cm<3> and no Fe<3+> is detected, filtrating, cooling, and stirring, so as to crystallize sand-like ferrous chloride tetrahydrate, drying with a centrifuge, baking in vacuum, and then, cooling, so as to obtain ferrous chloride tetrahydrate; putting ferrous chloride tetrahydrate in a vacuum converter with the temperature of 120-130 DEG C, carrying out heating dehydration, vacuumizing, and finally, carrying out furnace cooling, so as to obtain ferrous chloride dihydrate; putting ferrous chloride dihydrate in a vacuum converter, adding an organic mixed solvent, sealing, vacuumizing, rotating and dissolving; then, heating gradually and vacuumizing until the temperature is 150 DEG C, and carrying out furnace cooling, thereby obtaining anhydrous ferrous chloride.
Description
Technical field
The invention belongs to the preparation method of iron protochloride, particularly the preparation method of four water iron protochlorides, two water iron protochlorides and anhydrous chlorides of rase ferrous iron.
Background technology
Iron protochloride is the more satisfactory medicament of sewage disposal, can be directly used in sewage, wastewater treatment, as reductive agent and mordant, is widely used in the industries such as fabric printing, pigment, manufacture.Iron protochloride has exclusive decoloring ability, is applicable to the sewage disposal of dyestuff intermediate, printing and dyeing, paper industry; Can simplify water technology, shorten the water treatment cycle, reduce cost of water treatment; Plating, leather, paper waste and all kinds of sewage are had to obvious treatment effect, the clearance of all kinds of heavy metal ion in waste water, sewage is approached to 100%.Meanwhile, iron protochloride is also for ultra-high voltage lubricating oil component, also for medicine, metallurgical and photograph.
But the chemical purity of the preparation method's of four traditional water iron protochlorides, two water iron protochlorides and anhydrous chlorides of rase ferrous iron product is not ideal enough, especially the chemical purity of anhydrous chlorides of rase ferrous iron more cannot guarantee.
Summary of the invention
For above-mentioned technological deficiency, the object of the invention is to systematically provide the preparation method of a kind of four water iron protochlorides, two water iron protochlorides and anhydrous chlorides of rase ferrous iron, can improve respectively productive rate and the chemical purity of four water iron protochlorides, two water iron protochlorides and anhydrous chlorides of rase ferrous iron.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
(1) preparation method for four water iron protochlorides, is characterized in that, comprises the following steps: first iron filings or iron sheet are dissolved in hydrochloric acid soln, then pH value be less than 1 time 70-110 ℃ to be evaporated to proportion be 1.30-1.80g/cm
3, check is without Fe
3+during ion, filter, cooling and stirring crystallization goes out sand-like four water iron protochlorides, and whizzer dries, cooling after vacuum drying, obtains.
Preferably, iron filings or iron sheet are soft steel iron filings or iron sheet.
Preferably, the volumetric concentration of described hydrochloric acid soln is 2:1.
Preferably, described filtration is first to adopt the whizzer with canvas filter bag to filter, then adopts 747 polypropylene fibre filter cloth vacuum filtrations.
Preferably, cooling after described oven dry is after the vacuum converter vacuumizing and drying of 50-70 ℃, furnace cooling.
(2) preparation method for two water iron protochlorides, is characterized in that, comprises the following steps: four water iron protochlorides inserted to thermal dehydration in the vacuum converter of 120-130 ℃, vacuumize, last furnace cooling, obtains.
(3) preparation method for anhydrous chlorides of rase ferrous iron, is characterized in that, comprises the following steps: first two water iron protochlorides inserted in vacuum converter and added organic mixed solvent, sealing, vacuumize, rotate, dissolve; Then, progressively heat up, vacuumize, until 150 ℃ time, furnace cooling, obtains.
Preferably, described organic mixed solvent is acetone or tetrahydrofuran (THF).
Preferably, described progressively intensification is three heating and heat preservation stages, and its temperature spot is respectively 100 ℃, 120 ℃, 150 ℃.
In the present invention, adopt vacuum converter legal system ferrous for four water iron protochlorides, two water iron protochlorides and anhydrous chlorides of rase, its productive rate and chemical purity are high, and its productive rate and purity all can reach more than 99%.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further details.
Embodiment 1
First the iron sheet of 100 kilograms of soft steel is dissolved in 240 liters of hydrochloric acid solns, the volumetric concentration of hydrochloric acid soln is than for 2:1, then at pH value, being less than 1 time, 70-110 ℃, to be evaporated to proportion be 1.30-1.80g/cm
3, while checking without Fe3+ ion, (with 5% sulphosalicylic acid check, should there is not red-purple); Then, adopt the whizzer with canvas filter bag to filter, then adopt 747 polypropylene fibre filter cloth vacuum filtrations; Cooling and stirring crystallization goes out sand-like four water iron protochlorides, after whizzer dries, and after the vacuum converter vacuumizing and drying of 50-70 ℃, furnace cooling, the four water iron protochlorides that obtain, more than its purity to 99%.Vacuum packaging, inner bag is polyethylene food bag, outer bag is nylon vacuum bag, 0.12 millimeter of thickness.Outermost layer is fiber can.In the present embodiment, the iron sheet of soft steel, also the iron filings of available soft steel replace.
Embodiment 2
To according to 250 kilograms of four water iron protochlorides of embodiment 1 preparation, insert thermal dehydration in the vacuum converter of 500 liters of 120-130 ℃, vacuumize last furnace cooling, the two water iron protochlorides that obtain.
Embodiment 3
By the 100kg FeCl preparing according to embodiment 2
2.2H
2o drops in vacuum converter, adds 300 liters of organic mixed solvent tetrahydrofuran (THF)s; Mouth is obturaged, vacuumized, rotate, allow FeCl
2.2H
2o dissolved after 1 hour, stopped operating, and progressively heated up, and was specially: 1 hour to 100 ℃ and keep 1 hour, then 1 hour to 120 ℃ and keep 1 hour, then 1 hour to 150 ℃ and keep 1 hour; Finally, furnace cooling under vacuum, obtains anhydrous chlorides of rase ferrous iron.
In the present embodiment, organic mixed solvent tetrahydrofuran (THF) also available acetone replaces.
Although above, embodiment of the present invention are described, the present invention is not limited to above-mentioned specific embodiments, and above-mentioned specific embodiments is only schematic, guiding, rather than restrictive.Those of ordinary skill in the art, under the enlightenment of this specification sheets, in the situation that do not depart from the scope that the claims in the present invention are protected, can also make a variety of forms, and these all belong to the row of the present invention's protection.
Claims (9)
1. a preparation method for four water iron protochlorides, is characterized in that, comprises the following steps: first iron filings or iron sheet are dissolved in hydrochloric acid soln, then pH value be less than 1 time 70-110 ℃ to be evaporated to proportion be 1.30-1.80g/cm
3, check is without Fe
3+during ion, filter, cooling and stirring crystallization goes out sand-like four water iron protochlorides, and whizzer dries, cooling after vacuum drying, obtains.
2. the preparation method of four water iron protochlorides according to claim 1, is characterized in that, the iron filings that described iron filings or iron sheet are soft steel or iron sheet.
3. the preparation method of four water iron protochlorides according to claim 1, is characterized in that, the volumetric concentration of described hydrochloric acid soln is 2:1.
4. the preparation method of four water iron protochlorides according to claim 1, is characterized in that, described filtration is first to adopt the whizzer with canvas filter bag to filter, then adopts 747 polypropylene fibre filter cloth vacuum filtrations.
5. the preparation method of four water iron protochlorides according to claim 1, is characterized in that, cooling after described oven dry is after the vacuum converter vacuumizing and drying of 50-70 ℃, furnace cooling.
6. a preparation method for two water iron protochlorides, is characterized in that, comprises the following steps: four water iron protochlorides inserted to thermal dehydration in the vacuum converter of 120-130 ℃, vacuumize, last furnace cooling, obtains.
7. a preparation method for anhydrous chlorides of rase ferrous iron, is characterized in that, comprises the following steps: first two water iron protochlorides inserted in vacuum converter and added organic mixed solvent, sealing, vacuumize, rotate, dissolve; Then, progressively heat up, vacuumize, until 150 ℃ time, furnace cooling, obtains.
8. the preparation method of anhydrous chlorides of rase ferrous iron according to claim 7, is characterized in that, described organic mixed solvent is acetone or tetrahydrofuran (THF).
9. the preparation method of anhydrous chlorides of rase ferrous iron according to claim 8, is characterized in that, described progressively intensification is three heating and heat preservation stages, and its temperature spot is respectively 100 ℃, 120 ℃, 150 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410234117.6A CN104003450B (en) | 2014-05-29 | 2014-05-29 | Method for preparing ferrous chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410234117.6A CN104003450B (en) | 2014-05-29 | 2014-05-29 | Method for preparing ferrous chloride |
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| CN104003450A true CN104003450A (en) | 2014-08-27 |
| CN104003450B CN104003450B (en) | 2017-01-18 |
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| CN201410234117.6A Expired - Fee Related CN104003450B (en) | 2014-05-29 | 2014-05-29 | Method for preparing ferrous chloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107585792A (en) * | 2017-09-28 | 2018-01-16 | 唐山市斯瑞尔化工有限公司 | The preparation method and Ferrous dichloride dihydrate solid of Ferrous dichloride dihydrate solid |
| CN110980833A (en) * | 2019-12-16 | 2020-04-10 | 斯瑞尔环境科技股份有限公司 | Preparation method of electronic-grade ferrous chloride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1938461A (en) * | 1932-02-11 | 1933-12-05 | Dow Chemical Co | Method for preparing anhydrous iron chlorides |
| JPS5447896A (en) * | 1977-09-22 | 1979-04-14 | Agency Of Ind Science & Technol | Dehydration method for hydrated ferrous chloride |
-
2014
- 2014-05-29 CN CN201410234117.6A patent/CN104003450B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1938461A (en) * | 1932-02-11 | 1933-12-05 | Dow Chemical Co | Method for preparing anhydrous iron chlorides |
| JPS5447896A (en) * | 1977-09-22 | 1979-04-14 | Agency Of Ind Science & Technol | Dehydration method for hydrated ferrous chloride |
Non-Patent Citations (2)
| Title |
|---|
| THERALD MOELLER: "《无机合成 第五卷》", 31 December 1963, article "二水合氯化亚铁", pages: 158 * |
| 周学良主编: "《精细化工产品手册 常用试剂与高纯物》", 31 January 2003, 化学工业出版社 精细化工出版中心 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107585792A (en) * | 2017-09-28 | 2018-01-16 | 唐山市斯瑞尔化工有限公司 | The preparation method and Ferrous dichloride dihydrate solid of Ferrous dichloride dihydrate solid |
| CN107585792B (en) * | 2017-09-28 | 2021-07-27 | 唐山市斯瑞尔化工有限公司 | Preparation method of ferrous chloride dihydrate solid and ferrous chloride dihydrate solid |
| CN110980833A (en) * | 2019-12-16 | 2020-04-10 | 斯瑞尔环境科技股份有限公司 | Preparation method of electronic-grade ferrous chloride |
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| CN104003450B (en) | 2017-01-18 |
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