CN104609477A - Preparation method of high-purity ferric chloride anhydrous - Google Patents
Preparation method of high-purity ferric chloride anhydrous Download PDFInfo
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- CN104609477A CN104609477A CN201510052850.0A CN201510052850A CN104609477A CN 104609477 A CN104609477 A CN 104609477A CN 201510052850 A CN201510052850 A CN 201510052850A CN 104609477 A CN104609477 A CN 104609477A
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Abstract
The invention relates to a preparation method of chloride anhydrous, and in particular relates to a preparation method of high-purity ferric chloride anhydrous. The preparation method is used for solving the technical problems that impurities are easily mixed in the product and high-temperature reaction leads to potential risk in the general production process. According to the technical scheme, the preparation method comprises the following steps: putting ferrous chloride anhydrous into a closed vessel; adding a chlorine-containing carbon tetrachloride solution to react; filtering, spin-drying and baking the product to obtain ferric chloride anhydrous. By virtue of the method, high-purity ferric chloride anhydrous can be simply and quickly obtained.
Description
Technical field
The present invention relates to the preparation method of iron trichloride, particularly a kind of preparation method of high-purity anhydrous iron trichloride.
Background technology
In recent years, on market, (especially foreign market) demand to high-purity anhydrous iron trichloride is increasing.Pharmaceutical industry can make the catalyzer of many reactions with it, increasing to the demand of high-purity anhydrous iron trichloride.External price, at least at 12 dollars/kilogram, is equivalent to Renminbi 70000 yuan/ton, and the domestic manufacturers rarely having this series products.
The usual processing route of existing production FERRIC CHLORIDE ANHYDROUS: with waste iron filing and chlorine for raw material, react in a vertical response stove, the iron(ic) chloride steam generated and tail gas are discharged by the top of stove, enter trap and are condensed into solid crystal, obtain FERRIC CHLORIDE ANHYDROUS finished product.Containing a small amount of unreacted free chlorine in tail gas.Absorb chlorine with solution of ferrous chloride, obtain ferric chloride Solution as byproduct.In production operation, iron(ic) chloride steam contacts rear intense heat with moisture in air, and releases hydrogen chloride gas, and therefore pipeline and equipment want good seal.There is following problem in conventional anhydrous chlorides of rase process for making iron: chlorination process production FERRIC CHLORIDE ANHYDROUS in practice, owing to taking waste iron filing as raw materials for production, not only it is mingled with various metals, and dust, foreign material are also more, though there is sublimation separation, but has many metallic impurity and enter crystallisation by cooling room along with high temperature gas flow together with iron trichloride, be mixed in FERRIC CHLORIDE ANHYDROUS, cause water-insoluble in product many especially, the content of iron trichloride is mostly about 96%.Be difficult to the requirement meeting high-quality product.
Chinese patent application 201210204349.8 discloses a kind of preparation method of blocky ferric trichloride, is to obtain iron trichloride by the mode of growing the grain, and process is comparatively complicated, and the reaction times is also long.
Summary of the invention
The object of this invention is to provide a kind of preparation method of high-purity anhydrous iron trichloride, mainly solve in conventional production process and be easily mixed into impurity in product, and the technical problem of potential safety hazard that pyroreaction is brought.
Technical scheme of the present invention is: a kind of preparation method of high-purity anhydrous iron trichloride, comprise the following steps: anhydrous chlorides of rase ferrous iron is placed in encloses container, the carbon tetrachloride solution added containing chlorine reacts, product after filtration, dry and oven dry obtain FERRIC CHLORIDE ANHYDROUS.
The purity of described anhydrous chlorides of rase ferrous iron is 98.5%; Some acrylic spheres (5-20) are added in encloses container; The mol ratio of iron protochloride and tetracol phenixin is: 1:5 ~ 11; The mol ratio of iron protochloride and chlorine is 1:1.5 ~ 2.5; In carbon tetrachloride solution, the concentration of chlorine is: 1.0 ~ 2.5 mol/L; The mass percentage concentration of carbon tetrachloride solution is: 99 ~ 99.5%.
The invention has the beneficial effects as follows: the various metals brought due to iron filings in conventional production technique and foreign material, make to produce the problem that high-purity anhydrous iron trichloride has congenital defect, the present invention selects highly purified anhydrous chlorides of rase ferrous, effectively prevent and produces this front end disadvantage of raw material congenital defect.There is the security hidden trouble that pyroreaction is brought in conventional chlorinating method technique; the present invention adopt chlorine in the solution with iron protochloride direct reaction; avoid corresponding security hidden trouble, no matter from safety in production or from environment protection, all there is unrivaled advantage.With the moistening iron protochloride of tetracol phenixin, make iron protochloride become scattered paste shape, be conducive to chlorine oxidation it, and safety.With polypropylene ball milling cylinder and grind iron protochloride with acrylic sphere, can accelerating oxidation reaction thoroughly complete.
Embodiment
Embodiment 1, by 1260 grams of purity be 98.5% anhydrous chlorides of rase ferrous iron to be placed in volume be that the polypropylene seal cylinder of 20 liters (has acrylic sphere 5 in cylinder, each heavy 200 grams), (carbon tetrachloride solution mass percentage concentration is 99% to add 10 liters of carbon tetrachloride solutions containing chlorine, in this carbon tetrachloride solution, the concentration of chlorine is 1.5Mol/L), sealing, rotational response, inspection is arrived without Fe
+ 2time discharging (about 1 hour), filtration under diminished pressure, then centrifuge dripping, be placed in vacuum drying oven, dries under-0.09MPa and 80 DEG C condition, and obtained 1600 grams of FERRIC CHLORIDE ANHYDROUS, purity reaches 98%.
Embodiment 2, by 1260 grams of purity be 98.5% anhydrous chlorides of rase ferrous iron to be placed in volume be that the polypropylene seal cylinder of 20 liters (has acrylic sphere 10 in cylinder, each heavy 200 grams), (carbon tetrachloride solution mass percentage concentration is 99.2% to add 7.5 liters of carbon tetrachloride solutions containing chlorine, in this carbon tetrachloride solution, the concentration of chlorine is 2Mol/L), sealing, rotational response, inspection is arrived without Fe
+ 2time discharging (about 1 hour), filtration under diminished pressure, then centrifuge dripping, be placed in vacuum drying oven, dries under-0.09MPa and 80 DEG C condition, and obtained 1595 grams of FERRIC CHLORIDE ANHYDROUS, purity reaches 98.4%.
Embodiment 3, by 1260 grams of purity be 98.5% anhydrous chlorides of rase ferrous iron to be placed in volume be that the polypropylene seal cylinder of 20 liters (has acrylic sphere 20 in cylinder, each heavy 200 grams), (carbon tetrachloride solution mass percentage concentration is 99.5% to add 6 liters of carbon tetrachloride solutions containing chlorine, in this carbon tetrachloride solution, the concentration of chlorine is 2.5Mol/L), sealing, rotational response, inspection is arrived without Fe
+ 2time discharging (about 1 hour), filtration under diminished pressure, then centrifuge dripping, be placed in vacuum drying oven, dries under-0.09MPa and 80 DEG C condition, and obtained 1597 grams of FERRIC CHLORIDE ANHYDROUS, purity reaches 98.5%.
Claims (4)
1. a preparation method for high-purity anhydrous iron trichloride, is characterized in that comprising the following steps: anhydrous chlorides of rase ferrous iron is placed in encloses container, and the carbon tetrachloride solution added containing chlorine reacts, product after filtration, dry and oven dry obtain FERRIC CHLORIDE ANHYDROUS.
2. the preparation method of a kind of high-purity anhydrous iron trichloride according to claim 1, is characterized in that the purity of described anhydrous chlorides of rase ferrous iron is 98.5%.
3. the preparation method of a kind of high-purity anhydrous iron trichloride according to claim 1, is characterized in that adding some acrylic spheres in encloses container.
4. the preparation method of a kind of high-purity anhydrous iron trichloride according to claim 1, is characterized in that the mol ratio of iron protochloride and tetracol phenixin is: 1:5 ~ 11; The mol ratio of iron protochloride and chlorine is 1:1.5 ~ 2.5; In carbon tetrachloride solution, the concentration of chlorine is: 1.0 ~ 2.5 mol/L; The mass percentage concentration of carbon tetrachloride solution is: 99 ~ 99.5%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510052850.0A CN104609477B (en) | 2015-02-03 | 2015-02-03 | A kind of preparation method of high-purity anhydrous ferric trichloride |
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| CN201510052850.0A CN104609477B (en) | 2015-02-03 | 2015-02-03 | A kind of preparation method of high-purity anhydrous ferric trichloride |
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| CN104609477A true CN104609477A (en) | 2015-05-13 |
| CN104609477B CN104609477B (en) | 2016-05-11 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54150392A (en) * | 1978-05-16 | 1979-11-26 | Mineral Process Licensing Corp | Method of reducing ferric chloride |
| CN1037881A (en) * | 1988-04-29 | 1989-12-13 | 阿托化学公司 | The synthetic method of iron trichloride |
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2015
- 2015-02-03 CN CN201510052850.0A patent/CN104609477B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54150392A (en) * | 1978-05-16 | 1979-11-26 | Mineral Process Licensing Corp | Method of reducing ferric chloride |
| CN1037881A (en) * | 1988-04-29 | 1989-12-13 | 阿托化学公司 | The synthetic method of iron trichloride |
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