CN1163232A - Process for producing mangano-manganic oxide - Google Patents
Process for producing mangano-manganic oxide Download PDFInfo
- Publication number
- CN1163232A CN1163232A CN 96116905 CN96116905A CN1163232A CN 1163232 A CN1163232 A CN 1163232A CN 96116905 CN96116905 CN 96116905 CN 96116905 A CN96116905 A CN 96116905A CN 1163232 A CN1163232 A CN 1163232A
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- Prior art keywords
- trimanganese tetroxide
- mangano
- manganese
- manganese powder
- manganic oxide
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention belongs to the technological field of manganese compound. It produce metal manganese powder in air-tight crusher under the protection of inert gas. It solves the problem of oxidation, firing and explosion during the process of producing mangano-manganic oxide from magnese powder. At the same time, the selection of proper mangano-manganic oxide drying temp. can reasult in mangano-manganic oxide with high purity and more use. The present invention is also suitable for production ofultra-fine metal manganese powder.
Description
The present invention relates to the compound of manganese--a kind of preparation method of-trimanganese tetroxide.
Known to the applicant, trimanganese tetroxide can obtain by many methods.Conclude and to get up mainly can be divided into two kinds of pyrogenic process and wet methods.Pyrogenic process claims roasting method again, is when roasting is to about 1000 ℃ in air or in the oxygen with the oxide compound of manganese, oxyhydroxide, vitriol, carbonate etc. and obtain.Wet method is to prepare trimanganese tetroxide in solution under certain condition.Also have reduction method and electrolytic process etc. in addition.United States Patent (USP) 4812302 is described to be a kind of wet process for preparing trimanganese tetroxide.It is that water-soluble ammonia salt suspensioning liquid with containing metal manganese particulate is heated at least 30 ℃, oxygenant is imported in this suspension then, keep one section time enough of heating so that the manganese powder particle conversion in the suspension becomes desirable trimanganese tetroxide product, then oxidized suspension is sent to separation; By the residual water soluble salt of ammonia of washing method flush away free, drying obtains trimanganese tetroxide under 100～300 ℃ of temperature then afterwards.The advantage of this method is the reaction times short (1-4 hour), temperature of reaction not high (30-100 ℃), and products obtained therefrom purity is higher.But this method has following two shortcomings: 1. easy oxidation when manganese powder prepares and influence reactive behavior, even produce catch fire, explosion phenomenon.2. product oven dry treatment temp is on the low side, easy residual ammonium ion, acid ion in the product.Poor-performing during as the raw material of soft magnetic ferrite.
The objective of the invention is: on the basis of United States Patent (USP) 4812302, improve.Prepare manganese powder with special warfare, make its increased activity, steady quality, operational safety when generating trimanganese tetroxide.The trimanganese tetroxide that generates utilizes optimum temps to carry out pyrogenic attack, thereby obtains more highly purified trimanganese tetroxide.
The present invention is design like this: 1. the manganese powder that preparation activity is strong; its technology is at first the electrolytic metal Mn sheet to be added a kind of roll-type one ball milling to unite brokenly in the pulverizer; flow with 10L/h feeds rare gas element then; after the electrolytic metal Mn sheet is crushed to 40-300 purpose granularity; pack in the double-layer plastic bag, vacuumize earlier, and then the recoil protection of inert gas; the manganese powder that obtains like this has metalluster, and reactive behavior is good.2. after reacted trimanganese tetroxide filters, washs, dry in 300～700 ℃ temperature again, just can obtain more highly purified trimanganese tetroxide.
Advantage of the present invention is: the preparation of manganese powder has adopted gastight roll-type one ball milling to unite brokenly pulverizer and feed the oxidation that rare gas element can prevent manganese powder, has prevented the Peril Incident of the blast of catching fire.Pack into after the manganese powder fragmentation in the double-layer plastic bag, vacuumize earlier, and then the reactive behavior of recoil protection of inert gas can improve manganese powder and generate trimanganese tetroxide the time.The trimanganese tetroxide crystal grain that obtains is thin and even, the purity height, and purposes is wide.
For an embodiment: manganese metal is added airtight roll-type one ball milling continuously with the delivery rate of 50kg/h unite brokenly and carry out fragmentation in the disintegrating apparatus.This equipment inner chamber is an air hermetic, and broken material has partly adopted Wimet in the equipment.Flow with 10L/h feeds nitrogen then.Gained 100 order manganese powders are packed in the double-layer plastic bag, vacuumize earlier, and the small amount of nitrogen that recoils then, it is standby to seal the back.In beaker, add 600ml water, add water soluble salt of ammonia 7-30g then, add above-mentioned manganese powder 100g, be heated to 30-90 ℃, press the flow aerating oxygen of 30-300L/h, reaction times 1-4 hour.Last suspension is filtered, and obtains trimanganese tetroxide russet.Above-mentioned trimanganese tetroxide is added in the electrically heated rotary dryer in the continuous charging mode, and temperature is controlled at 300～700 ℃, time 1-8 hour, can obtain high-grade trimanganese tetroxide product.
Claims (3)
- One kind by manganese powder oxidation in water-soluble ammonia salt suspensioning liquid generate trimanganese tetroxide, then filtering separation, wash, be dried to the production method of product, it is characterized in that (1) improve the art breading of reactive behavior earlier with manganese powder, (2) with the trimanganese tetroxide that filters to isolate in suitable temperature, heat, to obtain highly purified trimanganese tetroxide.
- 2. by the described a kind of method for preparing trimanganese tetroxide of claim 1, the treatment process that it is characterized in that improving the manganese metal reactive behavior is the electrolytic metal Mn sheet to be added a kind of roll-type one ball milling formula unite brokenly pulverizer, flow with 10L/h feeds inert gas then, after the electrolytic metal Mn sheet is crushed to 40～300 purpose granularities, in the double-layer plastic bag of packing into; Vacuumize earlier, protection of inert gas then recoils.
- 3. by the described a kind of method for preparing trimanganese tetroxide of claim 1, adopt 300--700 ℃ temperature heating when it is characterized in that with the trimanganese tetroxide heat drying that filters to isolate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96116905 CN1163232A (en) | 1996-04-22 | 1996-04-22 | Process for producing mangano-manganic oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96116905 CN1163232A (en) | 1996-04-22 | 1996-04-22 | Process for producing mangano-manganic oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1163232A true CN1163232A (en) | 1997-10-29 |
Family
ID=5123858
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96116905 Pending CN1163232A (en) | 1996-04-22 | 1996-04-22 | Process for producing mangano-manganic oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1163232A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1083803C (en) * | 1998-04-17 | 2002-05-01 | 段希圣 | Roasting process of preparing very pure mangano-manganic oxide and its use |
| CN1112323C (en) * | 1998-10-26 | 2003-06-25 | 冶金工业部长沙矿冶研究院 | Method for producing high-purity mangano-manganic oxide |
| CN113690011A (en) * | 2021-07-13 | 2021-11-23 | 贵州金瑞新材料有限责任公司 | Demagnetisation process for preparing battery-grade trimanganese tetroxide by manganese sheet method |
-
1996
- 1996-04-22 CN CN 96116905 patent/CN1163232A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1083803C (en) * | 1998-04-17 | 2002-05-01 | 段希圣 | Roasting process of preparing very pure mangano-manganic oxide and its use |
| CN1112323C (en) * | 1998-10-26 | 2003-06-25 | 冶金工业部长沙矿冶研究院 | Method for producing high-purity mangano-manganic oxide |
| CN113690011A (en) * | 2021-07-13 | 2021-11-23 | 贵州金瑞新材料有限责任公司 | Demagnetisation process for preparing battery-grade trimanganese tetroxide by manganese sheet method |
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| SE01 | Entry into force of request for substantive examination | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |