CN101723431A - Method for recovering magnesium from magnesium sulfate solution - Google Patents
Method for recovering magnesium from magnesium sulfate solution Download PDFInfo
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- CN101723431A CN101723431A CN200810223691A CN200810223691A CN101723431A CN 101723431 A CN101723431 A CN 101723431A CN 200810223691 A CN200810223691 A CN 200810223691A CN 200810223691 A CN200810223691 A CN 200810223691A CN 101723431 A CN101723431 A CN 101723431A
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- magnesium
- calcium
- adlerika
- hydroxide
- calcium sulfate
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Abstract
The invention provides a method for recovering magnesium from a magnesium sulfate solution, which comprises the following steps of: (A) mixing calcium oxide and/or calcium hydroxide with calcium sulphate which is used as seed crystal; (B) mixing the magnesium sulfate solution with the mixture of the calcium oxide and/or the calcium hydroxide and the calcium sulphate to generate calcium sulphate precipitation and magnesium hydroxide precipitation; and (C) separating the calcium sulphate and the magnesium hydroxide. By recovering the magnesium hydroxide from the magnesium sulfate solution, the invention can recover the magnesium from the magnesium sulfate solution in a low-cost and low-pollution mode so as to achieve resource recycle.
Description
Technical field
The present invention relates to reclaim the method for magnesium, concrete, relate to the method that from Adlerika, reclaims magnesium.
Background technology
At present, in many industrial circles, often produce the waste liquid that contains magnesium in a large number.For example, in hydrometallurgy process ore being carried out acidleach goes out to produce the solution that contains sal epsom in a large number.Because sal epsom is known as " misery " again, is the toxic substance that can cause that the people suffers from diarrhoea, therefore country forbids containing the direct discharging of waste water of sal epsom.
Traditional treatment process is that the solution that will contain sal epsom carries out heating evaporation, obtains magnesium sulfate crystals.But the shortcoming of this treatment process is the cost height, 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; The primary oxidation magnesium that obtains is added water digestion, filtering and impurity removing, obtain magnesium hydroxide emulsion, move into emulsion in the minute-pressure reactor and control pressure, logical carbonic acid gas carbonization under agitation condition, after filtration, 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 methods such as this process using calcinings, therefore to the requirement height of equipment, and then the production cost height, be unsuitable for large-scale industrial application.
Summary of the invention
Purpose of the present invention is intended to one of solve the aforementioned problems in the prior at least.
For this reason, one object of the present invention is to propose a kind of method that reclaims magnesium from Adlerika that can improve organic efficiency.
The method that reclaims magnesium from Adlerika according to the embodiment of the invention may further comprise the steps:
A) calcium oxide and/or calcium hydroxide are mixed with calcium sulfate as crystal seed,
B) mixture of Adlerika with calcium oxide and/or calcium hydroxide and calcium sulfate mixed, to generate calcium sulfate precipitation and magnesium hydrate precipitate; And
C) separating calcium sulphate and magnesium hydroxide.
The method that from Adlerika, reclaims magnesium according to the embodiment of the invention, owing in the reaction system of sal epsom and calcium oxide and/or calcium hydroxide, there is calcium sulfate as crystal seed, the granularity of the calcium sulfate that generates in can the augmenting response process, thereby can utilize the granularity of calcium sulfate precipitation and the difference of magnesium hydroxide granularity, follow-up separating calcium sulphate at an easy rate and magnesium hydrate precipitate, and can improve the rate of recovery and the purity of magnesium hydrate precipitate.Therefore, the present invention can reclaim magnesium with low-cost, oligosaprobic mode from Adlerika, reach the recycling of resource.
In one embodiment of the invention, Adlerika is mixed with the mixture of calcium oxide and/or calcium hydroxide and calcium sulfate comprise Adlerika is added in take part in Taoism calcium oxide and/or calcium hydroxide and the mixture as the calcium sulfate of crystal seed.The present inventor finds, by Adlerika being joined in calcium oxide and/or calcium hydroxide and the mixture as the calcium sulfate of crystal seed, for example splash into wherein, can further improve the granularity of the calcium sulfate precipitation of reaction efficiency and generation, thus more separate easily calcium sulfate and magnesium hydroxide.
Described Adlerika is the leach liquor that contains magnesium and the leaching of metal concentrate sulfuric acid.Owing in containing the leaching of magnesium concentrate sulfuric acid, can produce the solution of a large amount of sulfur acid magnesium, the effect of therefore low-cost recovery magnesium technology in the industrial application that concentrate sulfuric acid leaches is better.In the further embodiment of the present invention, described Adlerika is the solution of leach liquor through obtaining after purifying, and has so not only obtained the metal ingredient in the ore effectively, and can reclaim the magnesium in the waste liquid that leaches as sulfuric acid.Purification comprises at least a metal of removing in the leach liquor, and for example iron, copper, cobalt, nickel, chromium thus, not only can reclaim iron, copper, cobalt, nickel, the medium composition of chromium, and reclaim the magnesium in the ore, have both reduced pollution, again recycle resource.
In one embodiment of the invention, calcium sulfate as crystal seed prepares by alkali-metal vitriol and calcium oxide and/or calcium hydroxide reaction, the resulting like this calcium sulfate as crystal seed can make easier being attached on it of calcium sulfate in the Adlerika, generate the precipitation of larger particle, thereby separate easilier with precipitated magnesium hydroxide.In further embodiment, described alkali-metal vitriol is sodium sulfate, can save cost like this.
In one embodiment of the invention, as the calcium sulfate of crystal seed be by Adlerika and calcium oxide and/or calcium hydroxide reaction obtain calcium sulfate with magnesium hydroxide, separating calcium sulphate and magnesium hydroxide, then the calcium sulfate after separating is washed and drying after obtain, can save alkali-metal vitriol like this, save cost.
In one embodiment of the invention, further comprise isolated magnesium hydroxide is washed and/or drying, can improve the magnesian purity of institute's separation of hydrogen like this, and be convenient to prolonged preservation.
In one embodiment of the invention, further comprise with separating the magnesium hydroxide that obtains and make the magnesium goods, for example can be used to prepare fertilizer, also can be used to make artificial board, can utilize further magnesium hydroxide like this, improve the economic value added that reclaims magnesium hydroxide.
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 by practice of the present invention.
Description of drawings
Fig. 1 is the schema of the method for magnesium that reclaims from Adlerika of first embodiment of the invention;
Fig. 2 is the schema of the method for magnesium that reclaims from Adlerika of second embodiment of the invention;
Fig. 3 is the schema of the method for magnesium that reclaims from Adlerika of third embodiment of the invention;
Fig. 4 is the schema of the method for magnesium that reclaims from Adlerika of fourth embodiment of the invention.
Fig. 5 is the schema of the method for magnesium that reclaims from Adlerika of fifth embodiment of the invention.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, is exemplary below by the embodiment that is described with reference to the drawings, and 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 " calcium oxide and/or calcium hydroxide " is meant and can uses calcium oxide (unslaked lime) also can use calcium hydroxide (white lime) in the present invention, also can add the mixture of the two.In actually operating, can water assimilation of quicklime using (CaO), thus obtaining milk of lime, principal reaction is CaO+H
2O=Ca (OH)
2, the mixture of milk of lime as calcium oxide and calcium hydroxide used.
Fig. 1 shows the schema according to the method for magnesium that reclaims of first embodiment of the invention from Adlerika.According to shown in Figure 1, at first calcium oxide and/or calcium hydroxide are mixed with calcium sulfate as crystal seed.Then add Adlerika in resulting mixture, to generate calcium sulfate precipitation and magnesium hydrate precipitate, its reaction that mainly takes place is:
MgSO
4+Ca(OH)
2＝CaSO
4+Mg(OH)
2，
Last separating calcium sulphate and magnesium hydroxide.
As mentioned above, sal epsom in the Adlerika and calcium hydroxide reaction generate calcium sulfate precipitation and magnesium hydrate precipitate.Yet the particle of calcium sulfate precipitation and magnesium hydrate precipitate is all very little, and the granularity difference is smaller, and more specifically, calcium sulfate precipitation is a crystalline form, and magnesium hydroxide is a gel, and magnesium hydroxide is coated on the calcium sulfate, so the two is difficult to separate.In addition, when sal epsom and calcium hydroxide reacted, the formation of magnesium hydrate precipitate had limited the further increase of calcium sulfate granularity, thereby has further increased separating difficulty.
According to embodiments of the invention, in the reaction system that sal epsom and calcium hydroxide react, contain calcium sulfate as crystal seed, therefore, when sal epsom and calcium hydroxide react, formed calcium sulfate precipitation can be formed on the crystal seed, thereby the granularity of calcium sulfate precipitation can further increase, and promptly forms the calcium sulfate precipitation of volume particle size, is convenient to separating between follow-up calcium sulfate and the magnesium hydrate precipitate thus.
The source of the employed in the present invention calcium sulfate as crystal seed is not restricted, both can be the ready-made calcium sulfate of buying from the market, also can be the calcium sulfate that obtains by independent chemical reaction, the product calcium sulfate that also can be in this technology to be generated.
In addition, in actually operating, at first Adlerika is added take part in Taoism calcium oxide and/or calcium hydroxide and as the mixing of the calcium sulfate of crystal seed, then Adlerika is added and for example splash in the described mixture, can further improve the granularity of the calcium sulfate precipitation of the efficient of reaction and generation like this.
With reference to figure 2, in one embodiment of the invention, be to use calcium sulfate precipitation that alkali-metal vitriol and calcium oxide and/or calcium hydroxide reaction generated in that to separate the back resulting as the calcium sulfate of crystal seed.The contriver finds that the calcium sulfate that uses this method to obtain can obviously increase the granularity of the calcium sulfate precipitation of generation as crystal seed.In addition, in a further embodiment, employed alkali-metal vitriol is sodium sulfate, because the cost of sodium sulfate is low, and the sodium hydroxide that is generated is solvable and can reuse, and therefore when can being convenient to separation of hydrogen sodium oxide and calcium sulfate, has also reduced cost.
With reference to figure 4, in one embodiment of the invention, as the calcium sulfate of crystal seed is to obtain calcium sulfate with magnesium hydroxide, separating calcium sulphate and magnesium hydroxide, then the calcium sulfate after separating is carried out obtaining after the classification washing by Adlerika and calcium oxide and/or calcium hydroxide reaction, do not need extra independent preparation calcium sulfate crystal seed like this and saved alkali-metal vitriol, therefore further saved to produce and produced this.For example, can in the part of sulfuric acid magnesium solution, add a certain amount of calcium oxide and/or calcium hydroxide earlier, obtain calcium sulfate and magnesium hydrate precipitate, from this reaction system, isolate calcium sulfate and magnesium hydroxide then, and the calcium sulfate precipitation that obtains is washed the calcium sulfate that obtains as crystal seed.
In addition, as mentioned above, at the beginning of technological process, also can be earlier in Adlerika, add the calcium sulfate enough as crystal seed from market, then by reaction, separate the calcium sulfate that obtains and just can be used as after the crystal seed of use.
In an embodiment of the present invention, calcium oxide and/or calcium hydroxide are mixed with calcium sulfate as crystal seed, both can use calcium oxide (unslaked lime), also can use calcium hydroxide (white lime), also can use the mixture of the two.Concrete, can water assimilation of quicklime using (CaO), thus obtaining milk of lime, principal reaction is CaO+H
2O=Ca (OH)
2More specifically, unslaked lime adds less water to be made its heating, aquation, is paste, and after thermopositive reaction finished substantially, thin up was sized mixing, and can prolong digestion time under the situation of time permission.When using commercial lime, except that prolonging digestion time, also need to sieve, to remove unreacted residue.It will be appreciated by those skilled in the art that, calcium oxide and/or calcium hydroxide are mixed with calcium sulfate as crystal seed, both promptly milk of lime can have been joined in the calcium sulfate Adlerika as crystal seed, also the calcium sulfate Adlerika as crystal seed can have been joined in the milk of lime.In one embodiment of the invention, be that milk of lime is joined in the calcium sulfate Adlerika as crystal seed, the contriver finds to adopt this method can improve efficient at follow-up sal epsom and calcium hydroxide reaction, further facilitates later separation magnesium hydroxide and calcium sulfate.
Milk of lime is mixed with Adlerika, and stir, thereby sal epsom and milk of lime react, and have generated throw out calcium sulfate and magnesium hydroxide, principal reaction is MgSO
4+ Ca (OH)
2=Mg (OH)
2↓+CaSO
4↓.
Because it is big that the granularity of the size ratio magnesium hydroxide of calcium sulfate is wanted, and owing to added the calcium sulfate crystal seed, compare with not adding crystal seed, the granulometric facies of calcium sulfate can further increase for the granularity of magnesium hydroxide.Therefore can easily calcium sulfate be separated with magnesium hydroxide according to two kinds of sedimentary granular size differences.
In addition, in one embodiment of the invention, in order to obtain the higher magnesium hydroxide of purity, and prolonged preservation, isolated magnesium hydroxide is washed and/or dry.Washings can adopt deionized water, can prevent that like this magnesium hydroxide suspension from flocculating.
With reference to figure 5, in one embodiment of the invention, separate the magnesium hydroxide that obtains and to be used to prepare the magnesium goods.For example, in a specific embodiment of the present invention, separate the magnesium hydroxide that obtains, therefore can be used for fertiliser containing magnesium, also can be used to make artificial board as farm crop because it contains high-load magnesium.
With reference to figure 4, in one embodiment of the invention, as previously mentioned, the calcium sulfate that separation is obtained can be used as crystal seed and turns back in the reaction system after removing the impurity (as magnesium hydroxide) on surface through washing.In addition, resulting calcium sulfate can also be used to prepare sulfuric acid and cement.
The source of Adlerika is not subjected to any restriction in the present invention, as long as contain sal epsom in its solution.With reference to figure 3, in one embodiment of the invention, Adlerika is the leach liquor that contains magnesium and the leaching of metal concentrate sulfuric acid.Using at present sulfuric acid that ore is carried out that acidleach goes out is that development is very fast at present, uses very wide wet process smelting technique, and still the sulfate waste liquid that is produced also becomes the factor that environment is made a very bad impression.Traditionally, the solution that contains sal epsom not only is untreated as waste liquid, and magnesium wherein abandons as waste liquid.Consider that mining industry can produce the waste liquid of several tons even tens of tons every day, therefore use treatment process of the present invention can obtain extraordinary economic benefit, greatly reduce production cost.
In further embodiment of the present invention, employed Adlerika is a sulphuric leachate through the solution that obtains after purifying, and promptly reclaims other compositions in (removals) leach liquor earlier, and then reclaims the interior magnesium that exists with the sal epsom form of waste liquid.For example, " purification " can be at least a metal of removing in the sulphuric leachate, for example iron, copper, cobalt, nickel and chromium, but the present invention is not limited to remove mentioned component.
In one embodiment of the invention, employed sulphuric acid soln be to the sulphuric leachate of high magnesium low-grade nickel minerals (laterite, nickel sulfide concentrate) through deironing, reclaim the solution that obtains after copper, nickel, the cobalt process.Particularly, the method for purification is with milk of lime the pH value of solution to be transferred to 7.5-8 under 60-80 ℃, feeds pressurized air, with the Fe of small amount of residual
2+Oxidation, hydrolytic precipitation.Further adjust pH value to 9.2, under this pH value, heavy metal ion etc. all can be reduced to 10-5mM.Obtain containing the MgSO of small amount of calcium after the filtration
4Solution contains Mg 10-20g/L.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification that scope of the present invention is by claims and be equal to and limit to these embodiment.
Claims (10)
1. method that reclaims magnesium from Adlerika may further comprise the steps:
A) calcium oxide and/or calcium hydroxide are mixed with calcium sulfate as crystal seed,
B) mixture of Adlerika with calcium oxide and/or calcium hydroxide and calcium sulfate mixed, to generate calcium sulfate precipitation and magnesium hydrate precipitate; And
C) separating calcium sulphate and magnesium hydroxide.
2. the method that from Adlerika, reclaims magnesium according to claim 1, it is characterized in that, Adlerika is mixed with the mixture of calcium oxide and/or calcium hydroxide and calcium sulfate comprise Adlerika is added in take part in Taoism calcium oxide and/or calcium hydroxide and the mixture as the calcium sulfate of crystal seed.
3. the method that reclaims magnesium from Adlerika according to claim 1 is characterized in that, described Adlerika is the leach liquor that contains magnesium and the leaching of metal concentrate sulfuric acid.
4. the method that reclaims magnesium from Adlerika according to claim 3 is characterized in that, described Adlerika is the solution of described leach liquor through obtaining after purifying.
5. the method that reclaims magnesium from Adlerika according to claim 4 is characterized in that described purification comprises at least a metal of removing in the leach liquor.
6. the method that reclaims magnesium from Adlerika according to claim 1 is characterized in that, prepares by alkali-metal vitriol and calcium oxide and/or calcium hydroxide reaction as the calcium sulfate of crystal seed.
7. the method that reclaims magnesium from Adlerika according to claim 6 is characterized in that described alkali-metal vitriol is sodium sulfate.
8. the method that from Adlerika, reclaims magnesium according to claim 1, it is characterized in that, as the calcium sulfate of crystal seed be by Adlerika and calcium oxide and/or calcium hydroxide reaction obtain calcium sulfate with magnesium hydroxide, separating calcium sulphate and magnesium hydroxide, then the calcium sulfate after separating is washed and drying after obtain.
9. the method that reclaims magnesium from Adlerika according to claim 1 is characterized in that, further comprises isolated magnesium hydroxide is washed and drying.
10. the leaching method of magnesium-containing ore according to claim 1 is characterized in that, further comprises with separating the magnesium hydroxide that obtains making the magnesium goods.
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| CN2008102236916A CN101723431B (en) | 2008-10-07 | 2008-10-07 | Method for recovering magnesium from magnesium sulfate solution |
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|---|---|---|---|
| CN2008102236916A CN101723431B (en) | 2008-10-07 | 2008-10-07 | Method for recovering magnesium from magnesium sulfate solution |
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| CN101723431B CN101723431B (en) | 2012-03-14 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275958A (en) * | 2011-07-29 | 2011-12-14 | 武汉工程大学 | Method for preparing magnesium hydroxide utilizing magnesium sulfate as raw material |
| CN102351221A (en) * | 2011-07-29 | 2012-02-15 | 武汉工程大学 | Method for preparing magnesium hydroxide from acid-dissolved magnesium ion-containing raw materials |
| CN103950957A (en) * | 2014-04-22 | 2014-07-30 | 彭振超 | Process method for preparing magnesium hydroxide from magnesium sulfate |
| CN106282553A (en) * | 2015-05-26 | 2017-01-04 | 有研稀土新材料股份有限公司 | The smelting separation method of Rare Earth Mine |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016175B (en) * | 2006-02-12 | 2011-10-05 | 滨化集团股份有限公司 | Method of eliminating magnesium sulfate from magnesium sulfate containing waste water solution |
-
2008
- 2008-10-07 CN CN2008102236916A patent/CN101723431B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275958A (en) * | 2011-07-29 | 2011-12-14 | 武汉工程大学 | Method for preparing magnesium hydroxide utilizing magnesium sulfate as raw material |
| CN102351221A (en) * | 2011-07-29 | 2012-02-15 | 武汉工程大学 | Method for preparing magnesium hydroxide from acid-dissolved magnesium ion-containing raw materials |
| CN102275958B (en) * | 2011-07-29 | 2013-02-06 | 武汉工程大学 | Method for preparing magnesium hydroxide utilizing magnesium sulfate as raw material |
| CN102351221B (en) * | 2011-07-29 | 2013-05-01 | 武汉工程大学 | Method for preparing magnesium hydroxide from acid-dissolved magnesium ion-containing raw materials |
| CN103950957A (en) * | 2014-04-22 | 2014-07-30 | 彭振超 | Process method for preparing magnesium hydroxide from magnesium sulfate |
| CN106282553A (en) * | 2015-05-26 | 2017-01-04 | 有研稀土新材料股份有限公司 | The smelting separation method of Rare Earth Mine |
| CN106282553B (en) * | 2015-05-26 | 2019-05-31 | 有研稀土新材料股份有限公司 | The smelting separation method of Rare Earth Mine |
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| CN101723431B (en) | 2012-03-14 |
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