CN101519226A - Method for preparing high-purity manganese oxide - Google Patents
Method for preparing high-purity manganese oxide Download PDFInfo
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- CN101519226A CN101519226A CN200810100882A CN200810100882A CN101519226A CN 101519226 A CN101519226 A CN 101519226A CN 200810100882 A CN200810100882 A CN 200810100882A CN 200810100882 A CN200810100882 A CN 200810100882A CN 101519226 A CN101519226 A CN 101519226A
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Abstract
The invention discloses a method for preparing high-purity manganese oxide, which belongs to the field of hydrometallurgy. The method uses high-impurity manganous carbonate to prepare high-purity trimanganese tetroxide, and the preparing process includes three steps of: step one: roasting the manganous carbonate at the roasting temperature of 150 DEG C to 1300 DEG C for a half hour to 40 hours to obtain the roasted substance; step two: processing the roasted substance by acid to separate impurities for 0.1 minute to 24 hours at the temperature of room temperature to 110 DEG C with the liquid-solid ratio of 0.5 to 50:1 and the reaction pH value of 0 to 7.5, and obtaining the intermediate product of manganese; and step three: roasting the intermediate product of manganese for 0.1 minute to 10 hours at the roasting temperature of 300 DEG C to 1300 DEG C to obtain the high-purity oxide of manganese. The invention has simple process and low cost and can obtain low-impurity and high-quality products.
Description
Technical field
The invention belongs to the hydrometallurgy field, a kind of method for preparing high-purity manganese oxide is provided especially
Background technology
The concentration of foreign ion is all very high in the sulfuric acid of pyrolusite or rhodochrosite or the leach liquor of sulfurous gas, can only remove a part with method calcium-magnesium removing such as common fluorochemicals and with method removing heavy metals ions such as sulfide.In the higher manganese sulfate solution of foreign matter content, directly add carbonate or supercarbonate precipitation mn ion, then the manganous carbonate purity of Huo Deing is very low, wherein the content of impurity such as calcium, magnesium, sulphur is very high, and the manganous carbonate that this foreign matter content is high is not suitable for preparing the oxide compound of high-purity manganese.When utilizing the manganous carbonate legal system to be equipped with the oxide compound of manganese, generally can only prepare the oxide compound of low-level manganese, without any practical significance.Wherein Zui Da difficult point is the foreign matter content height, and remove very difficult the separation.
Summary of the invention
The objective of the invention is to prepare the oxide compound of high-purity manganese, a kind of method for preparing high-purity manganese oxide is provided with the higher manganous carbonate of foreign matter content.
A kind of method for preparing the oxide compound of high-purity manganese is characterized in that preparation process was divided into for three steps, and the first step gets product of roasting for air or oxygen oxidizing roasting manganous carbonate; Second step was the removal of impurity of acid treatment manganous carbonate product of roasting, got the intermediate product of manganese; The 3rd step was the intermediate product of roasting manganese, got the oxide compound of high-purity manganese; Manganous carbonate oxidizing roasting condition is 150~1300 ℃ of maturing temperatures, and roasting time is 0.5~40 hour.The condition of acid treatment manganous carbonate product of roasting is that temperature is room temperature~110 ℃, liquid-solid ratio (0.5~50): 1, and in 0.1~24 hour treatment time, reaction pH is 0~7.5.The condition of the intermediate product of roasting manganese is 300~1300 ℃ of maturing temperatures, and roasting time is 0.1 minute~10 hours.The oxide compound of high-purity manganese is trimanganese tetroxide and manganic oxide.The used acid of acid treatment manganous carbonate product of roasting is sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid, formic acid.
The present invention is with manganous carbonate oxidizing roasting, low price manganese is converted into as far as possible the high price manganese that is insoluble in acid, use the acid treatment calcining matter then, the characteristic of utilizing impurity in the calcining matter more easily to be dissolved in acid will impurity be wherein separated and is removed, manganese intermediate product after the acid treatment is not the simplification compound, make its oxide compound that changes single manganese into through roasting again, the type of oxide compound is relevant with maturing temperature.
Technology of the present invention is simple, and cost is low, and the product foreign matter content is low and quality is good.
Embodiment
Example 1: get a certain amount of manganous carbonate and put into stoving oven, 300 ℃ of control maturing temperatures, atmospheric oxidation, gets calcining matter at 4 hours oxidizing roasting time.Calcining matter is added entry by liquid-solid ratio 4:1, stir, 70 ℃ of controlled temperature add sulfuric acid, pH value in reaction 3.0, and 3 hours reaction times, filter, wash, dry, get the intermediate product of manganese.The intermediate of manganese is put into stoving oven, 950 ℃ of maturing temperatures of control, roasting time 1 minute, the oxide compound of high-purity manganese.
Example 2: get a certain amount of manganous carbonate and put into stoving oven, 600 ℃ of control maturing temperatures, atmospheric oxidation, gets calcining matter at 3 hours oxidizing roasting time.Calcining matter is added entry by liquid-solid ratio 3:1, stir, 90 ℃ of controlled temperature add sulfuric acid, pH value in reaction 3.0, and 3 hours reaction times, filter, wash, dry, get the intermediate product of manganese.The intermediate of manganese is put into stoving oven, 500 ℃ of maturing temperatures of control, roasting time 3 minutes, the oxide compound of high-purity manganese.
Example 3: get a certain amount of manganous carbonate and put into stoving oven, 900 ℃ of control maturing temperatures, atmospheric oxidation, gets calcining matter at 2 hours oxidizing roasting time.Calcining matter is added entry by liquid-solid ratio 6:1, stir, 40 ℃ of controlled temperature add sulfuric acid, pH value in reaction 2.0, and 6 hours reaction times, filter, wash, dry, get the intermediate product of manganese.The intermediate of manganese is put into stoving oven, 600 ℃ of maturing temperatures of control, roasting time 6 minutes, the oxide compound of high-purity manganese.
Example 4: get a certain amount of manganous carbonate and put into stoving oven, 300 ℃ of control maturing temperatures, atmospheric oxidation, gets calcining matter at 4 hours oxidizing roasting time.Calcining matter is added entry by liquid-solid ratio 4:1, stir, 70 ℃ of controlled temperature add nitric acid, pH value in reaction 2.0, and 6 hours reaction times, filter, wash, dry, get the intermediate product of manganese.The intermediate of manganese is put into stoving oven, 950 ℃ of maturing temperatures of control, roasting time 30 minutes, the oxide compound of high-purity manganese.
Example 5: get a certain amount of manganous carbonate and put into stoving oven, 700 ℃ of control maturing temperatures, atmospheric oxidation, gets calcining matter at 6 hours oxidizing roasting time.Calcining matter is added entry by liquid-solid ratio 2:1, stir, 90 ℃ of controlled temperature add hydrochloric acid, pH value in reaction 2.0, and 6 hours reaction times, filter, wash, dry, get the intermediate product of manganese.The intermediate of manganese is put into stoving oven, 1000 ℃ of maturing temperatures of control, roasting time 0.2 minute, the oxide compound of high-purity manganese.
Example 6: get a certain amount of manganous carbonate and put into stoving oven, 400 ℃ of control maturing temperatures, dioxygen oxidation, gets calcining matter at 3 hours oxidizing roasting time.Calcining matter is added entry by liquid-solid ratio 5:1, stir, 90 ℃ of controlled temperature add acetic acid, pH value in reaction 4.0, and 6 hours reaction times, filter, wash, dry, get the intermediate product of manganese.The intermediate of manganese is put into stoving oven, 950 ℃ of maturing temperatures of control, roasting time 2 minutes, the oxide compound of high-purity manganese.
Example 7: get a certain amount of manganous carbonate and put into stoving oven, 380 ℃ of control maturing temperatures, atmospheric oxidation, gets calcining matter at 4 hours oxidizing roasting time.Calcining matter is added entry by liquid-solid ratio 5:1, stir, 98 ℃ of controlled temperature add sulfuric acid, pH value in reaction 2.0, and 6 hours reaction times, filter, wash, dry, get the intermediate product of manganese.The intermediate of manganese is put into stoving oven, 950 ℃ of maturing temperatures of control, roasting time 0.5 minute, the oxide compound of high-purity manganese.
Claims (6)
1. a method for preparing the oxide compound of high-purity manganese is characterized in that preparation process was divided into for three steps, and the first step gets product of roasting for air or oxygen oxidizing roasting manganous carbonate; Second step was the removal of impurity of acid treatment manganous carbonate product of roasting, got the intermediate product of manganese; The 3rd step was the intermediate product of roasting manganese, got the oxide compound of high-purity manganese.
2. according to the described a kind of method for preparing the oxide compound of high-purity manganese of claim 1, it is characterized in that manganous carbonate oxidizing roasting condition is 150~1300 ℃ of maturing temperatures, roasting time is 0.5~40 hour.
3. according to the described a kind of method for preparing the oxide compound of high-purity manganese of claim 1, the condition that it is characterized in that acid treatment manganous carbonate product of roasting is that temperature is room temperature~110 ℃, liquid-solid ratio (0.5~50): 1, in 0.1~24 hour treatment time, reaction pH is 0~7.5.
4. according to the described a kind of method for preparing the oxide compound of high-purity manganese of claim 1, the condition that it is characterized in that the intermediate product of roasting manganese is 300~1300 ℃ of maturing temperatures, and roasting time is 0.1 minute~10 hours.
5. according to the described a kind of method for preparing the oxide compound of high-purity manganese of claim 1, the oxide compound that it is characterized in that high-purity manganese is trimanganese tetroxide and manganic oxide.
6. according to the described a kind of method for preparing the oxide compound of high-purity manganese of claim 2, it is characterized in that the used acid of acid treatment manganous carbonate product of roasting is sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid, formic acid.
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CN200810100882A CN101519226A (en) | 2008-02-25 | 2008-02-25 | Method for preparing high-purity manganese oxide |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102464355A (en) * | 2010-11-05 | 2012-05-23 | 中国石油化工股份有限公司 | Preparation method of superfine manganese oxide |
CN108557892A (en) * | 2018-06-07 | 2018-09-21 | 江苏大学 | A kind of oxide preparation method and application for the manganese that object is mutually controllable |
CN109336183A (en) * | 2018-10-10 | 2019-02-15 | 北京科技大学 | It is a kind of to be raw material preparation Mn with value Mn and low price manganese compound2O3Method |
-
2008
- 2008-02-25 CN CN200810100882A patent/CN101519226A/en active Pending
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102464355A (en) * | 2010-11-05 | 2012-05-23 | 中国石油化工股份有限公司 | Preparation method of superfine manganese oxide |
CN102464355B (en) * | 2010-11-05 | 2013-11-06 | 中国石油化工股份有限公司 | Preparation method of superfine manganese oxide |
CN108557892A (en) * | 2018-06-07 | 2018-09-21 | 江苏大学 | A kind of oxide preparation method and application for the manganese that object is mutually controllable |
CN109336183A (en) * | 2018-10-10 | 2019-02-15 | 北京科技大学 | It is a kind of to be raw material preparation Mn with value Mn and low price manganese compound2O3Method |
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Open date: 20090902 |