CN101428861B - Process for producing high-purity manganese dioxide - Google Patents
Process for producing high-purity manganese dioxide Download PDFInfo
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- CN101428861B CN101428861B CN2008102396436A CN200810239643A CN101428861B CN 101428861 B CN101428861 B CN 101428861B CN 2008102396436 A CN2008102396436 A CN 2008102396436A CN 200810239643 A CN200810239643 A CN 200810239643A CN 101428861 B CN101428861 B CN 101428861B
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- manganse dioxide
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Abstract
A method for preparing high-purity manganese dioxide is characterized in that the method comprises the following steps: adding a certain proportion of additives to high-purity manganese nitrate solution with the weight concentration being 30% to 70%; and pyrolyzing at the temperature of 150 to 250 DEG C to obtain the high-purity manganese dioxide, wherein, the selected additives include one or more of ammonium carbonate, ammonium hydrogen carbonate, ammonium nitrate, carbamide and urea nitrate; and the proportion of the additives in the manganese nitrate solution is 1% to 15% by the weight of manganese nitrate.
Description
Technical field
The present invention relates to the preparation method of the technical field, particularly a kind of high-purity Manganse Dioxide of inorganic functional material preparation.
Background technology
High-purity Manganse Dioxide relates generally to inorganic novel material Application Areas.It still is one of important source material of chemical power source, and its quality quality plays decisive influence to the performance of battery.Also can be used for the manufacturing of high-grade ceramic, artwork, the oxygenant of medicine, food and catalyzer etc.
The method of existing preparation Manganse Dioxide is difficult for the high-purity Manganse Dioxide of preparation.
Electrolytic process is a kind of conventional production methods for preparing Manganse Dioxide, but this method facility investment is big, and power consumption is many, and the production cycle is long, and its product purity is up to 90～94%, can not produce highly purified Manganse Dioxide.
Patent CN 101186340A has introduced a kind of colloidal sol---the method for preparing gel Manganse Dioxide, carry out low temperature and high temperature acidified processing after citric acid and sour mangaic acid manganese is prepared into xerogel, and finally make manganese dioxide product.It is slow that colloidal sol---gel method prepares in the Manganse Dioxide gelation process of system, and synthesis cycle is long, and easily reunites in the calcination process, wayward quality product.
Patent CN 1377832A has also introduced a kind of technology of Hydrothermal Preparation Manganse Dioxide in addition, it is characterized in that with manganous salt and ammonium persulphate (potassium permanganate, clorox) be raw material, with ammonium sulfate is additive, carries out hydro-thermal reaction under 100～220 ℃ in confined conditions and prepares Manganse Dioxide.Though the good product dispersibility of this method preparation can be controlled the product crystal formation, this method requires comparatively strict to closed unit, require certain hyperbaric environment, and entire synthesis process is difficult to observe and control is adjusted, and is difficult for the high-purity Manganse Dioxide of preparation.
In addition to the above methods, it is also more that pyrolysis method prepares the method introduction of Manganse Dioxide.
It is more wherein to prepare the method for Manganse Dioxide with manganese carbonate pyrolysis, patent CN 1323745A has introduced a kind of method and apparatus that manganese carbonate pyrolysis is become Manganse Dioxide, manganous carbonate is contained under 280～400 ℃ in the warm air of 10～80% (percent by volume) steam and carry out pyrolysis, finally make the Manganse Dioxide of content 80～85%, purity is greater than 91% after making with extra care.The advantage of manganous carbonate decomposition method is that reaction principle is simple, production unit less demanding, and easy handling, instant effect, but the manganese carbonate pyrolysis transformation efficiency is lower, and the total quality of product is not high.Therefore manganese carbonate pyrolysis is not suitable for preparing high-purity Manganse Dioxide.
Introduced the method that chemical manganese bioxide is produced in the manganese sulfate monohydrate pyrolysis among the patent CN 101139111A, it is characterized in that behind the manganese sulfate monohydrate pyrolysis generation trimanganese tetroxide, be converted into manganic oxide again, make chemical manganese bioxide through technologies such as disproportionation, oxidizing reaction, pickling, washing, middle press filtration, oven dry then.The technical process of this method is longer, complicated operation, and final product purity is 95～95.5%, can not reach the requirement of high-purity Manganse Dioxide.
The advantage that the manganous nitrate pyrolysis method is produced Manganse Dioxide is that the quality product of producing is higher, and processing step is simple, can be through pyrolysis direct production Manganse Dioxide.If but the manganous nitrate pyrolytic reaction takes surperficial type of heating to carry out, the Manganse Dioxide that generates forms solid duricrust in surface lap easily, be difficult to peel off, yield is reduced, and easily cause being heated inequality in the pyrolytic process and be difficult for making the uniform product of quality.
Summary of the invention
The objective of the invention is to overcome the shortcoming of traditional manganous nitrate pyrolysis method, in manganese nitrate solution, add additive, solve the problem that scabs in the manganous nitrate pyrolytic process, a kind of method that can prepare high-purity Manganse Dioxide is provided.Pyrolysis product can not adhere to the formation hard formation after using additive on hot face, and products obtained therefrom is loose, is easy to separate from heating surface, thereby has effectively avoided the uneven problem of being heated in the pyrolytic process.In addition, additive selected among the present invention can be decomposed into gaseous volatilizations such as carbonic acid gas, ammonia fully in the manganous nitrate pyrolytic process, can residual impurity, therefore can prepare high-purity Manganse Dioxide.
The present invention is a kind of preparation method of high-purity Manganse Dioxide, it is characterized in that: add the additive of certainty ratio in the high pure nitric acid manganese solution of weight concentration 30～70%, carry out pyrolysis at 150～250 ℃ then, make high-purity Manganse Dioxide;
The additive of selecting for use comprises wherein one or more of volatile salt, bicarbonate of ammonia, ammonium nitrate, urea, urea nitrate; The ratio of additive in manganese nitrate solution is 1～15% with the manganous nitrate weight metering.
The preferred version of described the inventive method is characterized in that: high pure nitric acid manganese solution weight concentration is 40-60%; Additive is volatile salt or urea nitrate, and the ratio of additive in manganese nitrate solution is 2-10% with the manganous nitrate weight metering; The pyrolysis stability is 160-200 ℃.
Embodiment
Below be to adopt the inventive method to prepare the example of high-purity Manganse Dioxide, but be not limited only to this example.
Embodiment one:
Take by weighing the 300g70% manganese nitrate solution and the 6g volatile salt places reactor, stir to be placed in the pyrolysis oven, it is 200 ℃ that pyrolysis temperature is set, and carries out thermolysis and finish until reaction under this temperature.Final Manganse Dioxide 101.1g, the product purity 99.9% of getting.
Embodiment two:
Take by weighing the 400g50% manganese nitrate solution and the 14g urea nitrate places reactor, stir to be placed in the pyrolysis oven, it is 160 ℃ that pyrolysis temperature is set, and carries out thermolysis and finish until reaction under this temperature.Final manganese dioxide product 96.0g, the purity 99.8% of getting.
Claims (2)
1. the preparation method of high-purity Manganse Dioxide is characterized in that: add certain proportion of additive in the high pure nitric acid manganese solution of weight concentration 30～70%, carry out pyrolysis at 150～250 ℃ then, make high-purity Manganse Dioxide;
The additive of selecting for use comprises wherein one or both of urea, urea nitrate; The ratio of additive in manganese nitrate solution is 1～15% with the manganous nitrate weight metering.
2. it is characterized in that in accordance with the method for claim 1: high pure nitric acid manganese solution weight concentration is 40-60%; Additive is a urea nitrate, and the ratio of additive in manganese nitrate solution is 2-10% with the manganous nitrate weight metering; Pyrolysis temperature is 160-200 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102396436A CN101428861B (en) | 2008-12-15 | 2008-12-15 | Process for producing high-purity manganese dioxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008102396436A CN101428861B (en) | 2008-12-15 | 2008-12-15 | Process for producing high-purity manganese dioxide |
Publications (2)
| Publication Number | Publication Date |
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| CN101428861A CN101428861A (en) | 2009-05-13 |
| CN101428861B true CN101428861B (en) | 2011-06-01 |
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| CN2008102396436A Expired - Fee Related CN101428861B (en) | 2008-12-15 | 2008-12-15 | Process for producing high-purity manganese dioxide |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101700912B (en) * | 2009-11-17 | 2011-08-03 | 湘潭大学 | Preparation method of silky nano-MnO2 |
| CN101786666B (en) * | 2010-02-10 | 2012-02-22 | 彭天剑 | lithium manganate anode material and preparation method thereof |
| CN109232869A (en) * | 2018-09-13 | 2019-01-18 | 腾龙特种树脂(厦门)有限公司 | A kind of PETG modified copolyester |
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