CN101880772A - Method for recycling magnesium from magnesium-containing waste solution - Google Patents
Method for recycling magnesium from magnesium-containing waste solution Download PDFInfo
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- CN101880772A CN101880772A CN2010101993649A CN201010199364A CN101880772A CN 101880772 A CN101880772 A CN 101880772A CN 2010101993649 A CN2010101993649 A CN 2010101993649A CN 201010199364 A CN201010199364 A CN 201010199364A CN 101880772 A CN101880772 A CN 101880772A
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Abstract
The invention discloses a method for recycling magnesium from magnesium-containing waste solution, which comprises: A) mixing magnesium-containing waste solution and calcium chloride solution for magnesium conversion, and filtering the mixed solution after magnesium conversion, thereby obtaining gypsum and magnesium chloride solution; B) settling magnesium in the magnesium chloride solution with lime milk, and filtering the mixed solution with magnesium settled after reaction, thereby obtaining magnesium hydroxide precipitate and calcium chloride solution; and C) washing and drying the magnesium hydroxide precipitate, thereby obtaining magnesium hydroxide. The method can realize the recovery of magnesium from the magnesium-containing waste solution with low-price raw materials, and can not further cause the environmental pollution.
Description
Technical field
The present invention reclaims the method for magnesium from magnesium-containing waste solution, more specifically, relate to the method that reclaims magnesium in a kind of leach liquor from hydrometallurgy.
Background technology
In field of metallurgy, acid leaching process is a kind of method of refinement valuable metal commonly used.When producing cobalt nickel or other valuable metals, adopt acid leaching process that the valuable metals such as cobalt nickel in the ore are leached usually, meanwhile also leached with impurity such as the magnesium of cobalt nickel association, manganese thereupon.Leach liquor contains a large amount of magnesium in the liquid through purifying and the removal of impurities postprecipitation goes out cobalt nickel behind the heavy cobalt nickel that obtains so subsequently, and a spot of impurity manganese etc. for example, is commonly referred to magnesium-containing waste solution.In addition, owing in acid leaching process, need to use excessive acid, so a large amount of unreacted acid that can contain in the leach liquor.In actual production, need further handle leach liquor, reclaiming the more valuable metal magnesium of content, and excessive acid is utilized again.
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, heat condensing crystal under the mechanical stirring condition, crystallization after drying, calcining obtain primary oxidation magnesium, and the flue gas of generation reclaims as system sulfuric acid and uses; The primary oxidation magnesium that obtains is added water digestion, filtering and impurity removing acquisition magnesium hydroxide emulsion, move into emulsion in the reactor and control pressure, under agitation condition, feed carbonic acid gas and carry out carbonization, obtain magnesium bicarbonate solution after filtration, under heating and agitation condition, carry out the magnesium bicarbonate solution pyrolysis and just obtain the basic carbonate magnesium precipitate; The basic carbonate magnesium precipitate that obtains is obtained activated magnesia through filtering, wash, dry and calcining.
During the magnesium of this technology in reclaiming magnesium-containing waste solution, obtain primary oxidation magnesium by the heating condensing crystal, its energy consumption is big, and the purity of resulting primary oxidation magnesium is low.And, need on the basis of preparation primary oxidation magnesium, add water digestion in order to obtain the intermediate product magnesium hydroxide, thus its technical process complexity, and consumed a large amount of energy, environment has been caused polluted once more, the production cost height.
Summary of the invention
The present invention is intended to one of address the above problem at least, particularly solves production cost height, environmental pollution problems, and a kind of method that can reclaim magnesium with extremely cheap raw material from magnesium-containing waste solution is provided, and can not cause once more environment and pollute.
For achieving the above object, one aspect of the present invention proposes a kind of method that reclaims magnesium from magnesium-containing waste solution, may further comprise the steps: A) magnesium-containing waste solution is mixed transforming reactive magnesium with calcium chloride solution, reaction is filtered after finishing, and obtains plaster stone and magnesium chloride solution; B) with milk of lime described magnesium chloride solution is sunk reactive magnesium, question response filters after finishing, and obtains magnesium hydrate precipitate and rare calcium chloride solution; And C) to described magnesium hydrate precipitate wash, drying, obtain magnesium hydroxide.
The method that reclaims magnesium from magnesium-containing waste solution according to the embodiment of the invention can also have following additional technical feature:
From magnesium-containing waste solution, reclaim the method for magnesium according to an embodiment of the invention, in steps A) in calcium chloride solution be saturated solution, the calcium chloride coefficient of discharge is 1.0～1.5, the reaction times is 0.5～2h.
From magnesium-containing waste solution, reclaim the method for magnesium according to an embodiment of the invention, at step B) in calculate milk of lime with CaO concentration be 15wt%～20wt%, the milk of lime coefficient of discharge is 1.0～1.3, the reaction times is 0.5～2h.
From magnesium-containing waste solution, reclaim the method for magnesium according to an embodiment of the invention, at step C) in to described magnesium hydrate precipitate washing 3～5 times, drying obtains magnesium hydroxide afterwards.
From magnesium-containing waste solution, reclaim the method for magnesium according to an embodiment of the invention, further comprise: D) concentrate described rare calcium chloride solution and obtain the calcium chloride concentrated solution, and described calcium chloride concentrated solution returned be used for magnesium-containing waste solution is converted into magnesium chloride solution.
From magnesium-containing waste solution, reclaim the method for magnesium according to an embodiment of the invention, at step D) in obtain the calcium chloride concentrated solution by the described rare calcium chloride solution of heating evaporation.
From magnesium-containing waste solution, reclaim the method for magnesium according to an embodiment of the invention, further comprise: E) described plaster stone is washed the back 120～160 ℃ of calcinings 1～5 hour, obtain the plaster of Paris.
From magnesium-containing waste solution, reclaim the method for magnesium according to an embodiment of the invention, to described magnesium-containing waste solution impurity and purification.
Reclaim the method for magnesium according to an embodiment of the invention from magnesium-containing waste solution, described impurity and purification comprise at least a in iron, aluminium, cobalt, nickel and the manganese of removing in the magnesium-containing waste solution.
Reclaim the method for magnesium according to an embodiment of the invention from magnesium-containing waste solution, described magnesium-containing waste solution is the sulphuric leachate in the hydrometallurgy.
Compared with prior art, the present invention has one of following advantage at least:
According to the method that from magnesium-containing waste solution, reclaims magnesium of the present invention, can from the magnesium-containing waste solution that hydrometallurgy process obtains, reclaim magnesium elements efficiently with the preparation magnesium hydroxide and as plaster stone, the plaster of Paris of auxiliary product, whole reaction system only utilizes extremely cheap calcium chloride and milk of lime as raw material, do not produce any waste water in the process, both solve environmental issue, realized the comprehensive utilization of resource again.The cost of entire method is relatively low and method is simple, has proposed to reclaim from magnesium-containing waste solution with tradition the diverse new method of method of magnesium.
According to the method that from magnesium-containing waste solution, reclaims magnesium of the present invention, adopt the Adlerika of output in the hydrometallurgy process, therefore can handle the waste liquid that hydrometallurgy produces effectively, reclaimed the magnesium in the ore effectively, increased economic benefit, reduced the discharging of pollutent, environmental protection more helps realizing recycling economy.
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
The present invention above-mentioned and/or additional aspect and advantage from obviously and easily understanding becoming the description of embodiment, wherein below in conjunction with accompanying drawing:
Fig. 1 is the method flow diagram that reclaims magnesium from magnesium-containing waste solution of the first embodiment of the present invention.
Fig. 2 is the method flow diagram that reclaims magnesium from magnesium-containing waste solution of the second embodiment of the present invention.
Fig. 3 is the method flow diagram that reclaims magnesium from magnesium-containing waste solution of the third embodiment of the present invention.
Fig. 4 is the method flow diagram that reclaims magnesium from magnesium-containing waste solution of the fourth embodiment of the present invention.
Embodiment
Describing embodiments of the invention in detail below in conjunction with accompanying drawing, is exemplary 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.
In the following description, magnesium-containing waste solution specifically is meant the sulphuric leachate behind the precipitate cobalt nickel that adopts acid leaching process to refine valuable metal such as cobalt nickel in the cobalt nickel ores and obtain, wherein contain a large amount of unreacted sulfuric acid, and since also more in the ore with the Mg content of cobalt nickel association, more magnesium therefore also contained.In addition, also contain other impurity such as a small amount of manganese in this magnesium-containing waste solution.Yet be suitable for being not limited to sulphuric leachate behind the precipitate cobalt nickel with the magnesium-containing waste solution that method of the present invention is handled.
The present invention mainly is by utilizing relatively low calcium chloride of cost and milk of lime to reclaim magnesium from magnesium-containing waste solution, this method can reclaim magnesium elements efficiently with preparation magnesium hydroxide and plaster stone, plaster of Paris product from the magnesium-containing waste solution that hydrometallurgy process obtains, and the simple cost of method is low.
Obtain primary oxidation magnesium by the heating condensing crystal during magnesium of prior art in reclaiming magnesium-containing waste solution, its energy consumption is big, and the purity of resulting primary oxidation magnesium is low, then must behind preparation primary oxidation magnesium, add water digestion in order to obtain the intermediate product magnesium hydroxide, whole technology and consumed a large amount of energy has caused once more environment and to have polluted.In the embodiments of the invention, magnesium-containing waste solution is mixed with calcium chloride solution, question response finishes the back mixed solution is filtered, and obtains plaster stone and magnesium chloride solution; With milk of lime described magnesium chloride solution is sunk magnesium, question response finish the back to heavy magnesium after mixed solution filters, obtain magnesium hydrate precipitate and rare calcium chloride solution; And then to described magnesium hydrate precipitate wash, drying, obtain magnesium hydroxide.According to embodiments of the invention, can utilize cheap raw material, by simple technology, in the time of preparation magnesium hydroxide and plastering, reduced the discharging of pollutent, more environmental protection.
Method according to the processing magnesium-containing waste solution of the embodiment of the invention is described with reference to the accompanying drawings.
As shown in Figure 1, in the method that from magnesium-containing waste solution, reclaims magnesium according to the first embodiment of the present invention, at first get magnesium-containing waste solution, in magnesium-containing waste solution, add calcium chloride solution and transform reactive magnesium, question response finishes the back mixed solution is filtered, and obtains plaster stone and magnesium chloride solution.Then, described magnesium chloride solution is sunk reactive magnesium with milk of lime, question response finish the back to heavy magnesium after mixed solution filters, obtain magnesium hydrate precipitate and rare calcium chloride solution.At last, to described magnesium hydrate precipitate wash, drying, obtain magnesium hydroxide.
As shown in Figure 2, from magnesium-containing waste solution, reclaiming in the method for magnesium according to a second embodiment of the present invention, after preparing magnesium hydroxide with the method identical with first embodiment, by heating evaporation rare calcium chloride solution is concentrated, obtain the calcium chloride concentrated solution, and it is returned the sal epsom that is used for magnesium-containing waste solution be converted into magnesium chloride.All the other steps are identical with first embodiment, for the purpose of simple, do not set forth at this.
Figure 3 shows that the schema of the third embodiment of the present invention.At first, prepare magnesium hydroxide with the method identical with first embodiment.After this, plaster stone is calcined, obtained plaster of Paris product.
Figure 4 shows that the schema of the fourth embodiment of the present invention.In this embodiment, at first magnesium-containing waste solution is carried out impurity and purification, at least a with in iron, aluminium, cobalt, nickel and the manganese of removing described magnesium-containing waste solution, magnesium-containing waste solution after being purified and slag.After this, prepare magnesium hydroxide with the method identical with embodiment 1.
Below will be described embodiments of the invention by concrete example.
For example, in the example below the present invention, use the magnesium-containing waste solution of composition as shown in table 1 below, for the calcium chloride solution that improves the use of reaction efficiency and speed of reaction is saturated calcium chloride solution.But the present invention is not limited to use saturated calcium chloride solution.
Table 1 (magnesium-containing waste solution component list (g/l))
Example 1
At first get the magnesium-containing waste solution that the 500ml Mg content is 26g/L, it is carried out impurity and purification, the calcium chloride saturated solution is added stirring reaction in the magnesium-containing waste solution, wherein the calcium chloride coefficient of discharge is 1.0, reaction times is 1.5 hours, and the reaction after-filtration obtains plaster stone and magnesium chloride solution.Then, the milk of lime that in order to the CaO calculating concentration is 15wt% sinks magnesium to described magnesium chloride solution, milk of lime be 1.0 with coefficient of discharge, the reaction times is 1 hour, after question response finishes mixed solution behind the heavy magnesium is filtered, obtain magnesium hydrate precipitate and rare calcium chloride solution.At last, described magnesium hydrate precipitate is carried out 3 washings, this after drying obtains magnesium hydroxide.
By analysis, the content of the plaster stone of gained＞95%, the content of magnesium hydroxide＞92%.
Example 2
At first get the magnesium-containing waste solution that the 500ml Mg content is 26g/L, it is carried out impurity and purification, the calcium chloride saturated solution is added stirring reaction in the magnesium-containing waste solution, wherein the calcium chloride coefficient of discharge is 1.3, reaction times is 0.5 hour, and the reaction after-filtration obtains plaster stone and magnesium chloride solution.Then, the milk of lime that in order to the CaO calculating concentration is 20wt% sinks magnesium to described magnesium chloride solution, milk of lime be 1.2 with coefficient of discharge, the reaction times is 0.5 hour, after question response finishes mixed solution behind the heavy magnesium is filtered, obtain magnesium hydrate precipitate and rare calcium chloride solution.At last, described magnesium hydrate precipitate is carried out 3 washings, this after drying obtains magnesium hydroxide.
By analysis, the content of the plaster stone of gained＞95%, the content of magnesium hydroxide＞92%.
Than example 1,, and, accelerated heavy magnesium speed because the concentration of milk of lime increases and consumption increases along with the consumption increase speed of response of calcium chloride is accelerated.
Example 3
Get rare calcium chloride solution 500ml that example 1 obtains, be heated to 85 ℃ and its volatilization is concentrated, after this be cooled to room temperature, obtain saturated calcium chloride solution and crystallization of calcium chloride.
Resulting saturated calcium chloride solution can return and be used for magnesium-containing waste solution is converted into magnesium chloride solution.
Example 4
Get the plaster stone that example 1 obtains, after its washing 3 times,, obtain the plaster of Paris 150 ℃ of calcinings 3 hours.
Gained plaster of Paris content＞94%.
Although illustrated and described embodiments of the invention and concrete example, 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 magnesium-containing waste solution may further comprise the steps:
A) magnesium-containing waste solution is mixed with calcium chloride solution transform reactive magnesium, reaction is filtered after finishing, and obtains plaster stone and magnesium chloride solution;
B) with milk of lime described magnesium chloride solution is sunk reactive magnesium, reaction is filtered after finishing, and obtains magnesium hydrate precipitate and rare calcium chloride solution; With
C) to described magnesium hydrate precipitate wash, drying, obtain magnesium hydroxide.
2. the method that reclaims magnesium from magnesium-containing waste solution according to claim 1 is characterized in that, in steps A) in calcium chloride solution be saturated solution, the calcium chloride coefficient of discharge is 1.0～1.5, the reaction times is 0.5～2h.
3. the method that reclaims magnesium from magnesium-containing waste solution according to claim 1 is characterized in that, at step B) in calculate milk of lime with CaO concentration be 15wt%～20wt%, the milk of lime coefficient of discharge is 1.0～1.3, the reaction times is 0.5～2h.
4. the method that reclaims magnesium from magnesium-containing waste solution according to claim 1 is characterized in that, at step C) in to described magnesium hydrate precipitate washing 3～5 times, drying obtains magnesium hydroxide afterwards.
5. the method that from magnesium-containing waste solution, reclaims magnesium according to claim 1, it is characterized in that, further comprise: D) concentrate described rare calcium chloride solution and obtain the calcium chloride concentrated solution, and described calcium chloride concentrated solution returned be used for magnesium-containing waste solution is converted into magnesium chloride solution.
6. the method that reclaims magnesium from magnesium-containing waste solution according to claim 1 is characterized in that, at step D) in obtain the calcium chloride concentrated solution by the described rare calcium chloride solution of heating evaporation.
7. the method that reclaims magnesium from magnesium-containing waste solution according to claim 1 is characterized in that, further comprises: E) described plaster stone is washed the back 120～160 ℃ of calcinings 1～5 hour, obtain the plaster of Paris.
8. the method that reclaims magnesium from magnesium-containing waste solution according to claim 1 is characterized in that, to described magnesium-containing waste solution impurity and purification.
9. the method that reclaims magnesium from magnesium-containing waste solution according to claim 8 is characterized in that, described impurity and purification comprise at least a in iron, aluminium, cobalt, nickel and the manganese of removing in the magnesium-containing waste solution.
10. according to Claim 8 or the 9 described methods that from magnesium-containing waste solution, reclaim magnesium, it is characterized in that described magnesium-containing waste solution is the sulphuric leachate in the hydrometallurgy.
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| CN2010101993649A CN101880772B (en) | 2010-06-07 | 2010-06-07 | Method for recycling magnesium from magnesium-containing waste solution |
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| CN2010101993649A CN101880772B (en) | 2010-06-07 | 2010-06-07 | Method for recycling magnesium from magnesium-containing waste solution |
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| CN101880772B CN101880772B (en) | 2012-07-04 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098366A (en) * | 2017-04-25 | 2017-08-29 | 中国恩菲工程技术有限公司 | The method for handling magnesium-containing waste solution |
| CN107364879A (en) * | 2017-06-29 | 2017-11-21 | 中国恩菲工程技术有限公司 | The method that magnesium elements and calcium constituent are reclaimed from Adlerika |
| CN107488787A (en) * | 2017-08-10 | 2017-12-19 | 云南龙蕴科技环保股份有限公司 | A kind of method that manganese is reclaimed in sewage containing manganese |
| CN108754138A (en) * | 2018-05-25 | 2018-11-06 | 包头稀土研究院 | Magnesium chloride solution circulating leaching sulfuric acid rare earth roasted ore method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1924046A (en) * | 2006-08-25 | 2007-03-07 | 四川大学 | Method of retrieving magnesium from high magnesium phosphorus ore |
| CN101104521A (en) * | 2007-06-05 | 2008-01-16 | 昆明贵金属研究所 | Method for treating magnesium sulfate waste liquid and coproducing active magnesium chloride |
-
2010
- 2010-06-07 CN CN2010101993649A patent/CN101880772B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1924046A (en) * | 2006-08-25 | 2007-03-07 | 四川大学 | Method of retrieving magnesium from high magnesium phosphorus ore |
| CN101104521A (en) * | 2007-06-05 | 2008-01-16 | 昆明贵金属研究所 | Method for treating magnesium sulfate waste liquid and coproducing active magnesium chloride |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098366A (en) * | 2017-04-25 | 2017-08-29 | 中国恩菲工程技术有限公司 | The method for handling magnesium-containing waste solution |
| CN107098366B (en) * | 2017-04-25 | 2018-12-04 | 中国恩菲工程技术有限公司 | The method for handling magnesium-containing waste solution |
| CN107364879A (en) * | 2017-06-29 | 2017-11-21 | 中国恩菲工程技术有限公司 | The method that magnesium elements and calcium constituent are reclaimed from Adlerika |
| CN107364879B (en) * | 2017-06-29 | 2019-11-15 | 中国恩菲工程技术有限公司 | The method of magnesium elements and calcium constituent is recycled from Adlerika |
| CN107488787A (en) * | 2017-08-10 | 2017-12-19 | 云南龙蕴科技环保股份有限公司 | A kind of method that manganese is reclaimed in sewage containing manganese |
| CN108754138A (en) * | 2018-05-25 | 2018-11-06 | 包头稀土研究院 | Magnesium chloride solution circulating leaching sulfuric acid rare earth roasted ore method |
| CN108754138B (en) * | 2018-05-25 | 2020-06-16 | 包头稀土研究院 | Method for circularly leaching rare earth sulfate roasted ore by magnesium chloride solution |
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| CN101880772B (en) | 2012-07-04 |
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