CN101760637B - Leaching technology of magnesium-containing ore - Google Patents

Leaching technology of magnesium-containing ore Download PDF

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CN101760637B
CN101760637B CN200810240914XA CN200810240914A CN101760637B CN 101760637 B CN101760637 B CN 101760637B CN 200810240914X A CN200810240914X A CN 200810240914XA CN 200810240914 A CN200810240914 A CN 200810240914A CN 101760637 B CN101760637 B CN 101760637B
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magnesium
ore
hydrate precipitate
sulfate
calcium
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CN101760637A (en
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刘金山
孙宁磊
王魁珽
陆业大
张文
高保军
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China ENFI Engineering Corp
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China ENFI Engineering Corp
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Abstract

The invention discloses a leaching technology of magnesium-containing ore, comprising the following steps: mixing the magnesium-containing ore with sulfuric acid solution and performing the acid leaching to obtain leaching solution containing magnesium sulfate; purifying the leaching solution to obtain magnesium sulfate solution; mixing the magnesium sulfate solution with ammonia water to obtain magnesium hydroxide precipitation; filtering to obtain the magnesium hydroxide precipitation and filter liquor; causticizing the filter liquor by using calcium hydroxide and/or calcium oxide to obtain serous fluid which contains the magnesium hydroxide precipitation and calcium sulfate and produce ammonia; adding carbon dioxide into the serous fluid which contains the magnesium hydroxide precipitation and calcium sulfate so as to carbonizing the magnesium hydroxide to produce magnesium bicarbonate; and heating the serous fluid which contains the magnesium bicarbonate and calcium sulfate so as to disintegrate the magnesium bicarbonate to produce basic magnesium carbonate precipitation and filter liquor. By utilizing the leaching technology of the magnesium-containing ore of the invention, the metallic elements in the magnesium-containing ore can be recovered.

Description

The extract technology of magnesium-containing ore
Technical field
The present invention relates to wet method smelting process, especially relate to the extract technology of magnesium-containing ore.
Background technology
Ore smelting traditionally carries out through pyrometallurgical smelting process.Developed wet process smelting technique in recent years.Because hydrometallurgy can reduce the pollution to environment effectively, and can be suitable for multiple different ore deposit, therefore replace pyrometallurgical smelting just gradually.
Present wet method smelting process adopts the sulfuric acid extract technology more, the multiple metallic element that can leach in the ore to be contained.If can not reclaim, will be great waste, and some composition in the leach liquor also possibly damage to human body to these metallic elements.When for example magnesium-containing ore being leached, can produce the solution that contains sal epsom in a large number, because sal epsom is known as " misery " again, be the toxic substance that can cause that the people suffers from diarrhoea, and therefore country forbids containing the direct discharging of waste water of sal epsom.Traditional treatment process is that the solution that contains sal epsom is carried out heating evaporation, obtains magnesium sulfate crystals.But it is high that the shortcoming of this treatment process is a cost, and efficient is low, need to consume a large amount of energy, and the purity of resulting magnesium sulfate crystals is low.
For example, Chinese patent CN101104521 discloses a kind of treatment process of sal epsom waste liquid, and it comprises: measure a certain amount of sal epsom waste liquid; Under the mechanical stirring condition, heat condensing crystal, crystallization after drying, calcining; The primary oxidation magnesium that obtains, the flue gas of generation reclaims, and uses as system sulfuric acid; Add water digestion to the primary oxidation magnesium that obtains, filtering and impurity removing obtains Marinco H emulsion; Move into emulsion in the reaction kettle and control pressure, logical carbonic acid gas carbonization under agitation condition is through filtering; Obtain magnesium bicarbonate solution; Under heating and agitation condition, carry out the magnesium bicarbonate solution pyrolysis and just obtain the basic carbonate magnesium precipitate, filter at last, wash, dry and calcine, obtain activated magnesia.
Because this technology adopts evaporation-incinerating operational path, therefore, mass consumption the energy, environment caused once more polluted, and because technologies such as this process using calcining are therefore high to the requirement of equipment, and then the production cost height.
Summary of the invention
The object of the invention is intended to one of solve the aforementioned problems in the prior at least.
One object of the present invention is to propose a kind of leaching magnesium-containing ore that can high efficiente callback magnesium.Extract technology according to the magnesium-containing ore of the embodiment of the invention may further comprise the steps:
A) magnesium-containing ore is mixed with sulphuric acid soln carry out acidleach to obtain leaching solution containing magnesium sulfate;
B) said leach liquor is purified obtain Adlerika;
C) Adlerika is mixed with ammoniacal liquor, to obtain containing the slurries of magnesium hydrate precipitate and residual magnesium sulfate;
D) filter the slurries that contain magnesium hydrate precipitate and residual magnesium sulfate, obtain magnesium hydrate precipitate and filtrating respectively;
E) with calcium hydroxide and/or quicklime said filtrating is carried out causticization, obtain containing the slurries of magnesium hydrate precipitate and calcium sulfate, and generate ammonia;
F) in the said slurries that contain magnesium hydrate precipitate and calcium sulfate, feed carbonic acid gas, generate Magnesium hydrogen carbonate, separating calcium sulphate Marinco H is carried out carbonization; And
G) magnesium bicarbonate solution that will isolate behind the calcium sulfate heats, and makes Magnesium hydrogen carbonate decompose, and generates basic carbonate magnesium precipitate and carbonic acid gas.
Leaching magnesium-containing ore according to an embodiment of the invention; Can the metallic element in the magnesium-containing ore be reclaimed; Marinco H can be used for the good fire retardant and the weighting agent of macromolecular materials such as plastics, rubber; Aspect environmental protection,, can replace caustic soda and lime neutralizing agent as acid-bearing wastewater as the FGD agent; As oil dope, play anticorrosion and desulfidation; Be used for the refining of electron trade, medicine, granulated sugar; Be used for lagging material and make other magnesium salts product.Magnesium basic carbonate is a kind of important chemical product, and it can be used for the rubber item weighting agent, makes other magnesium salts, as the stopping composition of multiple light industrial goods, also be used to make high-efficiency insulated, refractory materials.By the Natural manganese dioxide of magnesium basic carbonate through the calcining output, can also conduct suppressor factor, the catalyzer in the chemical industry and pottery, enamel pharmaceutically except that possessing such use, the raw material of glass, in hydrometallurgy, can be used as the neutralization precipitation agent.Therefore, utilize the technology that from Adlerika, reclaims magnesium of this embodiment, can reduce the processing cost of wastewater treatment, and bring certain economic benefits, with developing a circular economy a kind of new technology is provided for the protection environment simultaneously.
According to embodiments of the invention, the extract technology of the magnesium-containing ore of the embodiment of the invention also has following additional technical feature:
In one embodiment of the invention, also comprise the magnesium hydrate precipitate magnesium precipitate that is obtained calcined and obtain Natural manganese dioxide.Can obtain the Natural manganese dioxide end product like this.In the further embodiment of the present invention, said calcining is carried out under 600 ℃-800 ℃.The applicant finds can reach calcining effectively 600 ℃ of-800 ℃ of following calcinings, and magnesium hydrate precipitate fully is converted into Natural manganese dioxide, improves productive rate.In further another embodiment of the present invention, before magnesium hydrate precipitate is calcined, it is washed, and washings is mixed with said filtrating.Like this, can improve magnesium hydrate precipitate is calcined the magnesian purity of acquisition, can improve the recovery of magnesium with reclaiming simultaneously attached to the sal epsom on the magnesium hydrate precipitate.
In one embodiment of the invention, comprise that also the ammonia that is generated is used for preparation mixes employed ammoniacal liquor with Adlerika.Can the ammonia that causticization generated be reclaimed and recycling like this, reduce cost, alleviate the pressure of ammonia environment.
In one embodiment of the invention, in the reaction system of sal epsom and ammoniacal liquor reaction generation Marinco H, add the Marinco H crystal seed, can change the size of crystallization crystal grain like this, to satisfy the requirement of different size magnesium products.
In one embodiment of the invention, comprise that also the said slurries that contain Marinco H and calcium sulfate are carried out pickling obtains calcium sulfate precipitation and Adlerika; The separating calcium sulphate deposition; And the Adlerika crystallization that will isolate calcium sulfate precipitation prepares the MAGNESIUM SULPHATE HEPTAHYDRATE 99.5 crystal.Can further improve organic efficiency like this, and obtain the MAGNESIUM SULPHATE HEPTAHYDRATE 99.5 crystal magnesium in the Adlerika.In the further embodiment of the present invention, said pickling is carried out for using dilute sulphuric acid, can magnesium hydrate precipitate fully and effectively be converted into sal epsom like this.
In one embodiment of the invention, said magniferous ore is magniferous nickel sulfide ore or nickel-containing eluvial ore (for example high magnesium nickel ore concentrate), and said purification comprises at least a in iron, aluminium, cobalt, nickel and the manganese of removing in the leach liquor.Thus, not only can reclaim valuable metal compositions such as iron, aluminium, cobalt, nickel and manganese, and reclaim the magnesium in the ore, both reduce pollution, again recycle resource.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize through practice of the present invention.
Description of drawings
Fig. 1 is the schema of extract technology of the magnesium-containing ore of first embodiment of the invention;
Fig. 2 is the schema of extract technology of the magnesium-containing ore of second embodiment of the invention;
Fig. 3 is the schema of extract technology of the magnesium-containing ore of third embodiment of the invention.
Embodiment
Describe embodiments of the invention below in detail, the example of said embodiment is shown in the drawings, is exemplary through the embodiment that is described with reference to the drawings below, only is used to explain the present invention, and can not be interpreted as limitation of the present invention.
Need to prove that the term that is adopted in the present invention " calcium hydroxide and/or quicklime " is meant and can uses quicklime (unslaked lime is called slaked lime and uses after the digestion), also can use calcium hydroxide (white lime), also can use the mixture of the two.In actually operating, can water assimilation of quicklime using (CaO), thus obtaining milk of lime utilization, principal reaction is CaO+H 2O=Ca (OH) 2
Fig. 1 shows the schema of the extract technology of magnesium-containing ore according to an embodiment of the invention.It is as shown in Figure 1,
At first magnesium-containing ore is mixed with sulphuric acid soln and carry out acidleach to obtain leaching solution containing magnesium sulfate, the reaction of generation is following:
MgO+H 2SO 4=MgSO 4+H 2O;
Then, said leach liquor is purified obtain Adlerika.
The sulfuric acid extract technology that is adopted among the present invention does not receive any restriction.For example, leaching can be leached or the leaching of oxygen enrichment high pressure for the oxygen enrichment normal pressure.Leaching process comprises magniferous nickel sulfide ore of fine grinding or nickel-containing eluvial ore, for example high magnesium nickel ore concentrate; Carry out pulp with the high magnesium nickel ore concentrate of sulphuric acid soln after to fine grinding; Concentrate after the pulp joined leach in the container, wherein leaching temperature in the container, to be controlled to be 90 ℃-100 ℃, pressure be normal pressure, and aerating oxygen leaches so that carry out the oxygen enrichment normal pressure in leaching container simultaneously.Before the leach liquor that contains sal epsom is reclaimed magnesium, leach liquor is purified.
Employed in the present invention term " purification " can be at least a in iron, aluminium, cobalt, nickel and the manganese of removing in (or reclaim) sulphuric leachate, but the present invention is not limited to remove mentioned component.
For example, in one embodiment of the invention, the leach liquor that the oxygen enrichment normal pressure is directly leached generation is discharged in leaching container the heavy iron container; With the temperature regulation to 75 of leach liquor ℃~80 ℃; For example 78 ℃, and the pH value of leach liquor is adjusted to 3~4, thus deposition is tapped a blast furnace.Because the purification in the sulfuric acid extract technology is that those of ordinary skills are known, gives unnecessary details no longer in detail here.
Then, Adlerika is mixed reaction below taking place with ammoniacal liquor:
MgSO 4+2NH 4OH=Mg(OH) 2↓+(NH 4) 2SO 4
Thereby obtain containing the slurries of magnesium hydrate precipitate and residual magnesium sulfate.Generally, ammoniacal liquor does not consume the whole sal epsom in the Adlerika, has therefore obtained to contain the slurries of Marinco H and remaining unreacted sal epsom.
Then, filter the slurries that contain magnesium hydrate precipitate and residual magnesium sulfate, obtain magnesium hydrate precipitate and filtrating.
Next, said filtrating is carried out causticization, reaction below taking place with calcium hydroxide and/or quicklime:
(NH 4) 2SO 4+MgSO 4+2Ca(OH) 2=2CaSO 4+Mg(OH) 2↓+2NH 3↑+2H 2O
Thereby obtain containing the slurries of magnesium hydrate precipitate and calcium sulfate, and generate ammonia, in one embodiment of the invention, the ammonia (NH that in causticizing reaction, is generated 3) can turn back to Adlerika blended step in, can reclaim ammonia like this, and the ammoniacal liquor of having regenerated, reduced cost, alleviated the pressure of ammonia to environment.
And then, in the said slurries that contain magnesium hydrate precipitate and calcium sulfate, feed carbonic acid gas, generate Magnesium hydrogen carbonate Marinco H is carried out carbonization, separating calcium sulphate, reaction below taking place
Mg(OH) 2+CaSO 4+CO 2=MgHCO 3+CaSO 4↓+H 2O
Further, separating calcium sulphate deposition.
At last, the magnesium bicarbonate solution of isolating calcium sulfate precipitation is heated, makes Magnesium hydrogen carbonate decompose, generate magnesium basic carbonate and carbonic acid gas, react as follows:
5Mg(HCO 3) 2=4MgCO 3·Mg(OH) 2↓+6CO 2↑。
Through above-mentioned technology, can reach magnesium in the Adlerika is effectively reclaimed.
In one embodiment of the invention, in the reaction system of sal epsom and ammoniacal liquor reaction generation Marinco H, add the Marinco H crystal seed, can change the size of crystallization crystal grain like this, to satisfy the requirement of different size magnesium products.The magnesium hydrate precipitate that is obtained can directly be used as commodity selling, obtains bigger economic benefit.In addition, also can carry out deep processing to magnesium hydrate precipitate, according to shown in Figure 2, to separate the magnesium hydrate precipitate that obtains calcine and obtain Natural manganese dioxide.The reaction that is taken place is following:
Mg(OH) 2=MgO+H 2O
In one embodiment of the invention, under 600 ℃-800 ℃, magnesium hydrate precipitate is calcined, the applicant finds can reach calcining effectively 600 ℃ of-800 ℃ of following calcinings, and magnesium hydrate precipitate fully is converted into Natural manganese dioxide, improves productive rate.In the further embodiment of the present invention, before magnesium hydrate precipitate is calcined, it is washed, and washings is mixed with said filtrating.Like this, can improve magnesium hydrate precipitate is calcined the magnesian purity of acquisition, can improve the recovery of magnesium with reclaiming simultaneously attached to the sal epsom on the magnesium hydrate precipitate.
In addition,, in another embodiment of the present invention, can carry out pickling, react as follows the slurries that contain Marinco H and calcium sulfate with reference to figure 3:
CaSO 4+Mg(OH) 2+H 2SO 4=CaSO 4↓+MgSO 4+2H 2O
Can reach separating like this to sal epsom and calcium sulfate; After the separating calcium sulphate deposition; Obtained the higher Adlerika of purity,, for example dissolved condition through reduction vaporization, control acid through Adlerika is carried out crystallization; Crystallisation by cooling technology can obtain the crystal of MAGNESIUM SULPHATE HEPTAHYDRATE 99.5, has further improved the organic efficiency of magnesium.
Concrete example according to the embodiment of the invention is described below.
Example 1.
Table 1 contains the composition of leaching table (g/l) of sal epsom, and wherein Adlerika is that the sulphuric leachate of magnesium-containing ore obtains through after purifying.
Mg SO 4 2- Al Ni Co Mn Fe
26-40 103-160 0.023 0.004 0.0016 0.0024 0.002
Ammoniacal liquor: 10-25% ammoniacal liquor
Get the leach liquor 500ml that contains sal epsom of table 1.
Ammoniacal liquor is theoretical amount
Temperature of reaction: normal temperature~60 ℃
The adding mode: ammoniacal liquor joins in the leach liquor that contains sal epsom
Reaction times: 0.5 hour~2 hours
Filtration time: 1 minute~5 minutes
Marinco H productive rate 35~50%
Marinco H purity >=98%
Example 2:
Get the leach liquor 500ml that contains sal epsom of table 1
Ammoniacal liquor is 1-2 times of theoretical amount
Temperature of reaction: normal temperature~60 ℃
The adding mode: ammoniacal liquor joins in the leach liquor that contains sal epsom
Adding Marinco H crystal seed amount is 0.5~3 times of theoretical amount
Reaction times: 0.5 hour~2 hours
Filtration time: 0.5 minute~5 minutes
Mg (OH) 2Productive rate is: 40~60%
Mg (OH) 2Purity>=99%
Example 3.
Get the filtered liq and the washing lotion~500ml of example 1
Add the gypsum seed of preparation in advance
Working concentration 5 weight %~20 weight % lime milks excessive 1.05.
The causticization time: 1 hour~2 hours
Causticization temperature: 45 ℃~105 ℃
Pickling gypsum and Marinco H,
Output gypsum purity>=95%, Mg≤0.5-1% are filtered in PH2~5.5
75-85 ℃ of output temperature, proportion 1.37-1.38 sal epsom is broad
Example 4
With example 3 temperature 75-85 ℃, the Adlerika of proportion 1.37-1.38 is cooled to 25-35 ℃ of crystallization output MAGNESIUM SULPHATE HEPTAHYDRATE 99.5, and the oven dry back is commercially available MAGNESIUM SULPHATE HEPTAHYDRATE 99.5
Example 5.
The ammonia steam water that contains of example 3 outputs is absorbed the ammoniacal liquor that becomes to contain ammonia 15~20% and is used for precipitated magnesium hydroxide.
Example 6
The Marinco H of example 1 or example 2 80~100 ℃ of dehydrations, is generated anhydrous Marinco H.
Anhydrous Marinco H calcining is MgO.
Calcination time 1 hour~3 hours
600~800 ℃ of calcining temperatures
Output MgO purity >=99%
CaO content≤0.1%
Quality product meets lightweight MgO and active MgO specification of quality.
Although illustrated and described embodiments of the invention; For those of ordinary skill in the art; Be appreciated that under the situation that does not break away from principle of the present invention and spirit and can carry out multiple variation, modification, replacement and modification that scope of the present invention is accompanying claims and be equal to and limit to these embodiment.

Claims (7)

1. the extract technology of a magnesium-containing ore may further comprise the steps:
A) magnesium-containing ore is mixed with sulphuric acid soln carry out acidleach to obtain leaching solution containing magnesium sulfate, said magniferous ore is magniferous nickel sulfide ore or nickel-containing eluvial ore;
B) said leach liquor is purified obtain Adlerika, said purification comprises at least a in iron, aluminium, cobalt, nickel and the manganese of removing in the leach liquor;
C) Adlerika is mixed with ammoniacal liquor,, wherein in this step, add the Marinco H crystal seed to obtain containing the slurries of magnesium hydrate precipitate and residual magnesium sulfate;
D) filter the slurries that contain magnesium hydrate precipitate and residual magnesium sulfate, obtain magnesium hydrate precipitate and filtrating respectively;
E) with calcium hydroxide and/or quicklime said filtrating is carried out causticization, obtain containing the slurries of magnesium hydrate precipitate and calcium sulfate, and generate ammonia;
F) in the said slurries that contain magnesium hydrate precipitate and calcium sulfate, feed carbonic acid gas, generate Magnesium hydrogen carbonate, separating calcium sulphate Marinco H is carried out carbonization; And
G) magnesium bicarbonate solution that will isolate calcium sulfate heats, and makes Magnesium hydrogen carbonate decompose, and generates basic carbonate magnesium precipitate and carbonic acid gas.
2. the extract technology of magnesium-containing ore according to claim 1 is characterized in that, further comprises:
With step D) in the magnesium hydrate precipitate that obtained calcine and obtain Natural manganese dioxide.
3. the extract technology of magnesium-containing ore according to claim 2 is characterized in that, said calcining is carried out under 600 ℃-800 ℃.
4. the extract technology of magnesium-containing ore according to claim 2 is characterized in that, before magnesium hydrate precipitate is calcined, it is washed, and washings is mixed with said filtrating.
5. the extract technology of magnesium-containing ore according to claim 1 is characterized in that, with step e) in the ammonia that generated be used for preparation process C) employed ammoniacal liquor.
6. the extract technology of magnesium-containing ore according to claim 1 is characterized in that, further comprises:
The said slurries that contain magnesium hydrate precipitate and calcium sulfate are carried out pickling obtain calcium sulfate precipitation and Adlerika;
The separating calcium sulphate deposition; And
The Adlerika crystallization of isolating behind the calcium sulfate precipitation is prepared the MAGNESIUM SULPHATE HEPTAHYDRATE 99.5 crystal.
7. the extract technology of magnesium-containing ore according to claim 6 is characterized in that, said acid is dilute sulphuric acid.
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EP2609226B1 (en) * 2010-08-27 2018-03-21 Ecoengineers Pty Ltd Process for magnesium production
CN102634680A (en) * 2012-05-03 2012-08-15 长春黄金研究院 Method for comprehensively recovering magnesium during process of extracting gold from magnesium-containing gold ore pile
WO2015154196A1 (en) * 2014-04-10 2015-10-15 Karnalyte Resources Inc. Process for producing high grade hydromagnesite and magnesium oxide
CN106277417A (en) * 2015-05-26 2017-01-04 有研稀土新材料股份有限公司 The method that smelting waste water comprehensive containing magnesium reclaims

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN88102284A (en) * 1988-04-19 1988-12-21 曾宪科 The production method of magnesium salts from dolomite with sulfuric acid wet process

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN88102284A (en) * 1988-04-19 1988-12-21 曾宪科 The production method of magnesium salts from dolomite with sulfuric acid wet process

Non-Patent Citations (1)

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Title
杨重愚.《氧化镁生产及其氯化过程》.《轻金属冶金学》.冶金工业出版社,2004,(第1版),第232页第15-17行,第23-30行. *

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