CN101215007A - Method for separating sulfur in manganese oxides preparation process - Google Patents
Method for separating sulfur in manganese oxides preparation process Download PDFInfo
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- CN101215007A CN101215007A CNA2008100557448A CN200810055744A CN101215007A CN 101215007 A CN101215007 A CN 101215007A CN A2008100557448 A CNA2008100557448 A CN A2008100557448A CN 200810055744 A CN200810055744 A CN 200810055744A CN 101215007 A CN101215007 A CN 101215007A
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Abstract
The invention provides a process to separate sulfur in a process for preparing manganese oxide. The sulfur of the manganese oxide mainly exists in the form of basic manganese sulfate and soluble sulfate which is partially packed, wherein the manganese oxide is produced by oxidizing manganese sulfate solution which employs air or oxygen at a certain temperature and a certain pH value. The invention utilizes the peculiarity of the basic manganese sulfate which is easy to be dissolved in acid medium, treats by controlling the temperature of the manganese oxide slurry and pH value of the solution, guarantees that the manganese oxide is dissolved as little as possible, simultaneously enables the basis manganese sulfate to be dissolved as much as possible, and enables that the packed soluble sulfate is relieved as much as possible to achieve the purpose of separating the sulfur. Manganomanganic oxide which yields low sulfur or dimanganese trioxide is obtained by the filtering, washing, drying and heat-treating of the slurry which is separated with sulfur. The invention has the advantages that reaction conditions are easy to be controlled, the effect of removing sulfur is fine and the cost is low.
Description
Technical field
The invention belongs to domain of inorganic chemistry, particularly the method for separate sulfur in a kind of oxides preparation process of manganese.
Background technology
Prepare that the oxide compound of manganese is simple because of technology, material cost is low etc. with air or oxygen direct oxidation manganous sulfate and have good development prospect, but the oxide impurity sulphur content height of the manganese that this method prepares, and be difficult to separate and remove.Discover that through me it is the soluble sulphate etc. of alkali formula manganous sulfate and a small amount of parcel that this method causes the high root of sulphur in the oxide products of manganese.Alkali formula manganous sulfate is the product of the mn ion partial hydrolysis in the manganese sulfate solution, and its generation is relevant with factors such as manganese ion concentration, sulfate ion concentration, pH value of solution value, temperature, is difficult to avoid its generation.Research finds that also it is the oxide compound of manganese that alkali formula manganous sulfate is difficult to exhaustive oxidation in addition, so the existence of alkali formula manganous sulfate is the basic reason that causes sulphur content in the oxide compound of manganese.The present invention is that the characteristic of utilizing the oxide compound of alkali formula manganous sulfate and manganese more more to be soluble in the acidic medium is removed the dissolving of the sulphur in the oxide compound of manganese.In the oxide compound of the manganese after the separate sulfur sulphur content less than 0.01% (with SO
3Meter).
Summary of the invention
The object of the present invention is to provide the method for separate sulfur in the oxides preparation process of manganese, utilize the oxide compound of alkali formula manganous sulfate and manganese more more be soluble in the acidic medium characteristic with the sulphur in the oxide compound of manganese all dissolving remove.
The method of separate sulfur in a kind of oxides preparation process of manganese, the oxide compound of the manganese that sulfur-bearing is high and water are by liquid-solid ratio (1~70): 1 mixes, and stirs, adds acid treatment, and the processing condition of separate sulfur are that temperature is room temperature~120 ℃, in 0.1~30 hour treatment time, reaction pH is 0~7.
The used acid of oxide compound of handling the high manganese of sulfur-bearing is sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid, formic acid, and the oxide compound of manganese is manganic oxide and trimanganese tetroxide.
The invention has the advantages that: easy control of reaction conditions, sulfur limitation effect is good, and cost is low.
Embodiment
Example 1: the oxide compound that takes by weighing the higher manganese of certain sulfur-bearing is put into reactor, adds entry at 4: 1 by liquid-solid ratio, stirs, and is heated to 50 ℃, adds sulfuric acid, and control reaction pH is about 2, and reaction 4h filters, washing, oven dry, thermal treatment, sulphur content less than 0.01% (with SO
3The oxide product of manganese meter).
Example 2: the oxide compound that takes by weighing the higher manganese of certain sulfur-bearing is put into reactor, adds entry at 9: 1 by liquid-solid ratio, stirs, and is heated to 90 ℃, adds sulfuric acid, and control reaction pH is about 4, and reaction 3h filters, washing, oven dry, thermal treatment, sulphur content less than 0.01% (with SO
3The oxide product of manganese meter).
Example 3: the oxide compound that takes by weighing the higher manganese of certain sulfur-bearing is put into reactor, adds entry at 3: 1 by liquid-solid ratio, stirs, and is heated to 80 ℃, adds sulfuric acid, and control reaction pH is about 1, and reaction 5h filters, washing, oven dry, thermal treatment, sulphur content less than 0.01% (with SO
3The oxide product of manganese meter).
Example 4: the oxide compound that takes by weighing the higher manganese of certain sulfur-bearing is put into reactor, adds entry at 5: 1 by liquid-solid ratio, stirs, and is heated to 40 ℃, adds hydrochloric acid, and control reaction pH is about 3, and reaction 4h filters, washing, oven dry, thermal treatment, sulphur content less than 0.01% (with SO
3The oxide product of manganese meter).
Example 5: the oxide compound that takes by weighing the higher manganese of certain sulfur-bearing is put into reactor, adds entry at 6: 1 by liquid-solid ratio, stirs, and is heated to 40 ℃, adds nitric acid, and control reaction pH is about 4, and reaction 3h filters, washing, oven dry, thermal treatment, sulphur content less than 0.01% (with SO
3The oxide product of manganese meter).
Example 6: the oxide compound that takes by weighing the higher manganese of certain sulfur-bearing is put into reactor, adds entry at 4: 1 by liquid-solid ratio, stirs, and is heated to 40 ℃, adds acetic acid, and control reaction pH is about 3, and reaction 6h filters, washing, oven dry, thermal treatment, sulphur content less than 0.01% (with SO
3The oxide product of manganese meter).
Claims (2)
1. the method for a separate sulfur from the oxide compound of manganese, the oxide compound that it is characterized in that the manganese that sulfur-bearing is high and water are by liquid-solid ratio (1~70): 1 mixes, stir, add acid treatment, the processing condition of separate sulfur are that temperature is room temperature~120 ℃, in 0.1~30 hour treatment time, reaction pH is 0~7, filters, washes clean, oven dry.
2. according to the method for claim 1 separate sulfur from the oxide compound of manganese, the used acid of oxide compound that it is characterized in that handling the high manganese of sulfur-bearing is sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid, formic acid, and the oxide compound of manganese is manganic oxide and trimanganese tetroxide.
Priority Applications (1)
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CNA2008100557448A CN101215007A (en) | 2008-01-08 | 2008-01-08 | Method for separating sulfur in manganese oxides preparation process |
Applications Claiming Priority (1)
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CNA2008100557448A CN101215007A (en) | 2008-01-08 | 2008-01-08 | Method for separating sulfur in manganese oxides preparation process |
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CN101215007A true CN101215007A (en) | 2008-07-09 |
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CNA2008100557448A Pending CN101215007A (en) | 2008-01-08 | 2008-01-08 | Method for separating sulfur in manganese oxides preparation process |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111807414A (en) * | 2020-06-18 | 2020-10-23 | 贵州金瑞新材料有限责任公司 | Method for producing fluorine-free ultrapure manganese sulfate monohydrate by using basic salt method |
-
2008
- 2008-01-08 CN CNA2008100557448A patent/CN101215007A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111807414A (en) * | 2020-06-18 | 2020-10-23 | 贵州金瑞新材料有限责任公司 | Method for producing fluorine-free ultrapure manganese sulfate monohydrate by using basic salt method |
CN111807414B (en) * | 2020-06-18 | 2022-06-17 | 贵州金瑞新材料有限责任公司 | Method for producing fluorine-free ultrapure manganese sulfate monohydrate by using basic salt method |
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Open date: 20080709 |