CN109609757A - A method of standby manganese carbonate is soaked by additive ammonia of ethylenediamine tetra-acetic acid - Google Patents

A method of standby manganese carbonate is soaked by additive ammonia of ethylenediamine tetra-acetic acid Download PDF

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Publication number
CN109609757A
CN109609757A CN201910017143.6A CN201910017143A CN109609757A CN 109609757 A CN109609757 A CN 109609757A CN 201910017143 A CN201910017143 A CN 201910017143A CN 109609757 A CN109609757 A CN 109609757A
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China
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manganese
ammonia
acetic acid
additive
ethylenediamine tetra
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CN201910017143.6A
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梁小平
伍成波
涂忠兵
崔腾飞
王雨
梁爽
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Chongqing University
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Chongqing University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
    • C22B3/14—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions containing ammonia or ammonium salts
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B47/00—Obtaining manganese
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The present invention relates to a kind of methods for being soaked standby manganese carbonate as additive ammonia using ethylenediamine tetra-acetic acid, belong to manganese ore field of hydrometallurgy.1) method is the following steps are included: obtain manganese ore calcining using calcination process to manganese ore；2) the manganese ore calcining for obtaining step 1) carries out ammonia leaching by additive of ethylenediamine tetra-acetic acid.(3) filtrate for obtaining step (2) carries out ammonia still process, obtains manganese carbonate product.Solves the problems, such as manganese leaching rate existing for existing manganese ore ammonia leaching technology, it is an advantage of the invention that the extraction rate of manganese is significantly improved during soaking to manganese ore ammonia and easy to operate, leaching mild condition, gained manganese carbonate product are with high purity.

Description

A method of standby manganese carbonate is soaked by additive ammonia of ethylenediamine tetra-acetic acid
Technical field
The present invention relates to the skills that a kind of hydrometallurgical technology of manganese ore more particularly to a kind of ammonia of manganese ore are soaked standby manganese carbonate Art.
Background technique
Manganese and its compound are applied to the every field of national economy, wherein steel and iron industry be with the maximum field of manganese amount, 90%~95% is accounted for manganese amount, mainly as the deoxidier and desulfurizing agent in ironmaking and steelmaking process, and for manufacturing alloy. Remaining manganese is used for other industrial circles, as manufactured various manganese salts, for battery, match, print paint, soapmaking, glass and ceramics Colorant and decolourant etc..In short, manganese has highly important strategic position in national economy.
For the average manganese content of the manganese resource in China probably 20%, it is total that the reserves of rich manganese ore only account for national manganese resource The 6.4% of amount.Moreover, China's manganese ore impurity content is higher, Chemical Leaching method is that one of this kind of poor manganese ore of processing can Row approach.The Chemical Leaching that many scholars in home and abroad are directed to low-grade manganese has made numerous studies.
According to the difference of leaching agent, Chemical Leaching method is broadly divided into the acid-hatching of young eggs and ammonia leaching process.The acid-hatching of young eggs is by acid molten Liquid leaching bivalent manganese prepares manganese product by the method for being electrolysed or precipitating after cleaning.Since low product are presented in China's manganese ore more Feature more than position, impurity, other metal impurities such as calcium, magnesium, iron during the acidleach of manganese in ore can also leach simultaneously, make The impurity content for obtaining immersion liquid is high, influences the purity of its subsequent product and then limits its application category.
Ammonia leaching process is to generate manganese amine complex in ammonia solution using manganese monoxide and the property that dissolves is come leaching of manganese Method.Manganese ore includes manganese spar (MnCO in nature3), pyrolusite (MnO2), hausmannite (Mn3O4) and braunite (Mn7SiO12) Deng, but this kind of manganese ore cannot be directly dissolved in ammonia solution.It needs to handle by preroast by manganese spar before ammonia leaching (MnCO3), pyrolusite (MnO2), hausmannite (Mn3O4) and braunite (Mn7SiO12) etc. be changed into the manganese ore calcining containing MnO, example Such as by roasting the MnCO in manganese spar3Thermal decomposition is MnO, obtains the manganese ore calcining containing MnO, or will be soft by reduction roasting MnO in manganese ore, hausmannite and braunite2、Mn3O4And Mn7SiO12It is reduced to MnO, obtains the manganese ore calcining containing MnO.Then Ammonia solution is added in manganese ore calcining containing MnO to leach, finally manganese is precipitated out and can be prepared using the method for heating ammonia still process Obtain manganese carbonate product.During ammonia leaching, in manganese ore calcining MnO be dissolved in ammonia solution and the impurity such as calcium, magnesium, iron not It is molten, so that efficiently separating for manganese and impurity in manganese ore is realized, and leachate is pure, therefore the good impurity removing effect of ammonia leaching process, to leaching The ammonia that liquid generate when heating ammonia still process processing out is only absorbed by the water to form ammonium hydroxide, and ammonium hydroxide can be used as leaching agent and return to ammonia leaching ring Section recycles, therefore ammonia leaching process also has the characteristics that waste liquid is few, process cleans are environmentally friendly.The poor manganese gravity treatment of [autograph] Separation of Zun Yi Manganese Ore high-speed rail Reduction roasting-ammonia leaching method processing [author] Chen Jibin [periodical name] nation manganese industry [digest] report of tailings stone is reducing agent roasting with coal The poor manganese gravity tailings stone of Separation of Zun Yi Manganese Ore high-speed rail is burnt, then the test result of ammonia leaching process processing, in liquid-solid ratio 5:lmL/g, leaching Between 2h, under conditions of ammonia density 16-17mol/L, gas concentration lwevel 4mol/L, the leaching rate of manganese is 62%, and overall recovery is 57%, it obtains containing MnCO388% product.The test of the loose peach high-phosphorus manganese stone of [autograph] reduction roasting-ammonia leaching method processing [is made Person] Chen Jibin [periodical name] nation manganese industry [digest] in the case where adding a small amount of anchracite duff, by manganese ore 800 DEG C at a temperature of Then miberal powder after roasting is added ammonium hydroxide and sal volatile, leaches 2h at room temperature by roasting, for 1# sample, (manganese grade is 17.81%) manganese leaching rate is that the manganese leaching rate of 73.18%, 2# sample (manganese grade is 25.57%) is 89.61%, manganese carbonate Purity is 83.6%~88.9%.
In conclusion ammonia leaching process has easy to operate, good impurity removing effect, product purity is high, and leaching agent is Ke Xunhuanliyong, clearly The features such as clean pollution-free.But the manganese leaching rate of ammonia leaching process is lower, in particular by low-grade manganese ore be raw material when (manganese product Position is usually no more than 80% lower than 20%) becoming apparent.The low utilization efficiency that can reduce manganese ore of the leaching rate of manganese, causes to provide The waste in source can also improve production cost, be one of the important problem of popularization and application for limiting ammonia leaching process therefore.
Summary of the invention
For the low problem of manganese leaching rate existing for existing ammonia leaching technology, of the invention provide a kind of can effectively improve manganese Method mine ammonia dipped Cheng Meng leaching rate and prepare manganese carbonate, it has operating condition simple, and immersion liquid impurity content is few, cleans nothing Pollution, the high feature of product purity.
The present invention to achieve the above object provided by technical solution are as follows:
A method of standby manganese carbonate is soaked by additive ammonia of ethylenediamine tetra-acetic acid, it is characterised in that including following step It is rapid:
(1) calcination process is used to manganese ore, obtains the manganese ore calcining containing MnO；
(2) the manganese ore calcining containing MnO for obtaining step (1) carries out ammonia leaching by additive of ethylenediamine tetra-acetic acid, and solid Liquid separation；
(3) leachate that step (2) obtains is subjected to heating ammonia still process, obtains manganese carbonate product.
This method may also comprise the following steps::
(4) phase analysis that step (2) is isolated is washed, cleaning solution return step (2) recycles.
(5) it absorbs the ammonia that step (3) heating ammonia still process generates to obtain ammonia spirit through water, and return step (2) recycles It utilizes.
Method of the present invention, optimal technical scheme are as follows:
Preferably, manganese ore described in step (1) includes pyrolusite, manganese spar, hausmannite, braunite it is one or two kinds of with On mixed mineral.
Preferably, manganese ore described in step (1) after broken, fine grinding granularity less than 50 mesh.
Preferably, calcination process described in step (1) is by roasting manganese spar (MnCO3), pyrolusite (MnO2), it is black Manganese ore (Mn3O4) and braunite (Mn7SiO12) etc. manganese in manganese ores be changed into the manganese ore calcining containing MnO.Such as by roasting water chestnut manganese MnCO in mine3Thermal decomposition is MnO, obtains the manganese ore calcining containing MnO, or by reduction roasting by pyrolusite, hausmannite and MnO in braunite2、Mn3O4And Mn7SiO12It is reduced to MnO, obtains the manganese ore calcining containing MnO.
Preferably, 400 mesh of granularity~50 mesh of manganese ore calcining described in step (1).
Preferably, additive described in step (2) is ethylenediamine tetra-acetic acid, and additive amount is 0.01~0.1mol/L.
Preferably, the concentration of ammonia is 8~18mol/L in ammonia solution described in step (2), and extraction temperature is 20 DEG C~30 ℃。
Preferably, heating ammonia still process temperature described in step (3) is 40~100 DEG C, 20~80min of time, stirring rate 100r/min~600r/min.
Compared with prior art, the present invention its advantages and advantage are:
1, the leaching rate of manganese is high
It is that ethylenediamine tetra-acetic acid is added as additive progress compared with additive carries out ammonia leaching with ethylenediamine tetra-acetic acid is not added Ammonia leaching, the leaching rate of manganese increase substantially.Particularly, for low-grade manganese raw material (manganese grade is lower than 20%), second two is added Amine tetraacethyl is that additive carries out ammonia leaching, and the leaching rate of manganese can be improved 5% or so.
2, product purity is high
Manganese can be efficiently separated with impurity element, and impurity content is low in leachate, prepare manganese carbonate product purity is high.
3, ammonia recycle utilizes
The ammonia that ammonia still process link generates can return to the dipped journey circulation benefit of calcining ammonia by the ammonium hydroxide that water absorption and regeneration obtains With.
4, simplify the work after manganese leaches
Since leachate impurity is less, purification process can be simplified.Waste water is few, and impurity content is few in mother liquor, simplifies waste water Treatment process.
5, cleanliness without any pollution
Wastewater flow rate is few, and the ammonium hydroxide that ammonia is only absorbed by the water can be used as leaching agent and recycle, and reduces discharging of waste liquid, production Cleanliness without any pollution.
Detailed description of the invention
Fig. 1 is the process flow chart of the invention that standby manganese carbonate is soaked by additive ammonia of ethylenediamine tetra-acetic acid.
Specific embodiment
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, below further specifically to the present invention It is bright.But following embodiments is only simple example of the invention, does not represent or limit the scope of the present invention, this The protection scope of invention is subject to claims.
Embodiment
A method of it being soaked standby manganese carbonate by additive ammonia of ethylenediamine tetra-acetic acid, using manganese spar as raw material, including with Lower step:
1) it weighs 50g manganese spar and is put into two hours of drying in drying box, then in the high temp, vertical tubular type for being passed through nitrogen In furnace in 750 DEG C roasting temperature 1 hour, obtain calcining after nitrogen protection is cooling, 200 purposes of obtained manganese spar calcining Sieve screening；
2) ammonium carbonate of certain mass is added in certain density ammonia spirit, ammonia concn 14mol/L, carbonic acid is made Ammonium concentration is the leaching agent of 2mol/L, and then 10g manganese spar calcining is added in leaching agent, the ethylenediamine of 0.05mol/L is added Tetraacethyl (EDTA), ammonia soak temperature be 30 DEG C, ammonia soak the time be 60min, liquid-solid ratio 6:1, stirring rate 400r/min, to After the completion of stirring, filtering takes filtrate, obtains manganese leachate.
3) manganese leachate is heated to 95 DEG C, is 300r/min in stirring rate, after evaporating 60min, obtain manganese carbonate production Product.
Manganese spar used in step 1) is the low grade rhodochrosite from Sichuan Wanyuan somewhere, ingredient in the present embodiment As shown in table 1, manganese content 17.83% belongs to low grade rhodochrosite.
1 manganese spar essential element content of table
There is the content of the manganese in the manganese leachate of additive ethylenediamine tetra-acetic acid (EDTA) to be detected to step 2) it is found that After additive is added, manganese leaching rate is 90.1%.Under the conditions of identical roasting and ammonia are soaked, ethylenediamine tetra-acetic acid is not added When Mn leaching rate be only 84.6%, illustrate the addition due to additive ethylenediamine tetra-acetic acid, the leaching rate of Mn improves 5.5%.
2 manganese carbonate product quality analysis results of table
As shown in table 2 to the quality analysis results of manganese carbonate product obtained by step 3) ammonia still process, the purity of manganese carbonate product is 90.45%, manganese content 43.26%, impurity content is low.Such as according to the technical indicator (HG/T 4203-2011) of industrial carbonic acid manganese Shown in table 3, manganese carbonate product meets the requirement of industrial carbonic acid manganese Grade A.
The technical indicator and leaching manganese carbonate product quality of 3 industrial carbonic acid manganese of table
Illustrate from above-described embodiment, during the leaching of the ammonia of manganese ore, it is that additive can be significant that ethylenediamine tetra-acetic acid, which is added, The ammonia for improving manganese ore soaks efficiency, and gained manganese carbonate product purity is high, impurity content is few, meets wanting for industrial carbonic acid manganese Grade A It asks.

Claims (8)

1. a kind of method for soaking manganese using ethylenediamine tetra-acetic acid as additive ammonia, it is characterised in that the following steps are included:
(1) calcination process is used to manganese ore, obtains the manganese ore calcining containing MnO；
(2) the manganese ore calcining containing MnO for obtaining step (1) carries out ammonia leaching, and solid-liquid point by additive of ethylenediamine tetra-acetic acid From；
(3) leachate that step (2) obtains is subjected to heating ammonia still process, obtains manganese carbonate product.
This method may also comprise the following steps::
(4) the washed obtained cleaning solution return step (2) of the phase analysis of step (2) solid-liquid separation is recycled.
(5) the ammonia spirit return step (2) that the ammonia that step (3) heating ammonia still process generates is absorbed through water is recycled.
2. a kind of method for soaking manganese using ethylenediamine tetra-acetic acid as additive ammonia according to claim 1, which is characterized in that Manganese ore described in step (1) includes pyrolusite, manganese spar, hausmannite, one or more kinds of mixed minerals of braunite.
3. a kind of method for soaking manganese using ethylenediamine tetra-acetic acid as additive ammonia according to claim 1, which is characterized in that Manganese ore described in step (1) after broken, fine grinding granularity less than 50 mesh.
4. a kind of method for soaking manganese using ethylenediamine tetra-acetic acid as additive ammonia according to claim 1, which is characterized in that Calcination process described in step (1) is by roasting manganese spar (MnCO3), pyrolusite (MnO2), hausmannite (Mn3O4) and it is brown Manganese ore (Mn7SiO12) etc. manganese in manganese ores be changed into the manganese ore calcining containing MnO.Such as by roasting the MnCO in manganese spar3Heat It is decomposed into MnO, obtains the manganese ore calcining containing MnO, or by reduction roasting by pyrolusite, in hausmannite and braunite MnO2、Mn3O4And Mn7SiO12It is reduced to MnO, obtains the manganese ore calcining containing MnO.
5. a kind of method for soaking manganese using ethylenediamine tetra-acetic acid as additive ammonia according to claim 1, which is characterized in that 400 mesh of granularity~50 mesh of manganese ore calcining described in step (1).
6. a kind of method for soaking manganese using ethylenediamine tetra-acetic acid as additive ammonia according to claim 1, which is characterized in that Additive described in step (2) is ethylenediamine tetra-acetic acid, and additive amount is 0.01~0.1mol/L.
7. a kind of method for soaking manganese using ethylenediamine tetra-acetic acid as additive ammonia according to claim 1, which is characterized in that The concentration of ammonia is 6~20mol/L in ammonia solution described in step (2), and extraction temperature is 20 DEG C~30 DEG C.
8. a kind of method for soaking manganese using ethylenediamine tetra-acetic acid as additive ammonia according to claim 1, which is characterized in that Heating ammonia still process temperature described in step (3) is 40~100 DEG C, 20~80min of time, stirring rate 100r/min~600r/ min。
CN201910017143.6A 2019-01-08 2019-01-08 A method of standby manganese carbonate is soaked by additive ammonia of ethylenediamine tetra-acetic acid Pending CN109609757A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103014320A (en) * 2012-12-07 2013-04-03 中信大锰矿业有限责任公司 Method for preparing manganese sulfate by using sulfur-containing carbonaceous manganese carbonate ore
CN106399724A (en) * 2016-10-27 2017-02-15 中南大学 Microwave reduction roasting and extracting method for manganese oxide ore
CN107475526A (en) * 2017-08-26 2017-12-15 麻江县金泰工业废渣综合利用回收有限责任公司 A kind of method for preparing zinc metal sheet and ammonium chloride using high chlorine smelting ash

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103014320A (en) * 2012-12-07 2013-04-03 中信大锰矿业有限责任公司 Method for preparing manganese sulfate by using sulfur-containing carbonaceous manganese carbonate ore
CN106399724A (en) * 2016-10-27 2017-02-15 中南大学 Microwave reduction roasting and extracting method for manganese oxide ore
CN107475526A (en) * 2017-08-26 2017-12-15 麻江县金泰工业废渣综合利用回收有限责任公司 A kind of method for preparing zinc metal sheet and ammonium chloride using high chlorine smelting ash

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
崔腾飞: "添加剂对菱锰矿氨浸过程的影响研究", 《中国学位论文全文数据库》 *

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Application publication date: 20190412