CN107098366B - The method for handling magnesium-containing waste solution - Google Patents
The method for handling magnesium-containing waste solution Download PDFInfo
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- CN107098366B CN107098366B CN201710278476.5A CN201710278476A CN107098366B CN 107098366 B CN107098366 B CN 107098366B CN 201710278476 A CN201710278476 A CN 201710278476A CN 107098366 B CN107098366 B CN 107098366B
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- magnesium
- calcium
- bicarbonate
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- sulfate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/24—Magnesium carbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of methods for handling magnesium-containing waste solution, comprising: (1) mixes the magnesium-containing waste solution with milk of lime, to obtain the slurry containing magnesium hydroxide and calcium sulfate；(2) it is filtered after the slurry and carbon dioxide exposure by described containing magnesium hydroxide and calcium sulfate, so as to liquid after obtaining calcium sulfate and reaction containing magnesium bicarbonate and calcium bicarbonate；(3) it is filtered after contacting liquid after the reaction containing magnesium bicarbonate and calcium bicarbonate with calcium remover, to obtain calcic slag and deliming containing magnesium bicarbonate is containing liquid after magnesium；(4) deliming containing magnesium bicarbonate is pyrolyzed containing liquid after magnesium, to obtain carbonic acid magnesium products.This method can efficiently remove calcium constituent in carbonic acid magnesium products, and guarantee that the calcium content in carbonic acid magnesium products is up to state standards.
Description
Technical field
The invention belongs to chemical fields, specifically, the present invention relates to the methods of processing magnesium-containing waste solution.
Background technique
Currently, often generating a large amount of containing magnesium waste liquids in many industrial circles.For example, in hydrometallurgy process
Solution largely containing magnesium sulfate can be generated by carrying out Ore Leaching to magnesium-containing ore.It is energy since magnesium sulfate is also referred to as " misery "
Enough cause the noxious material of people's diarrhea, therefore country forbids the direct discharging of waste water containing magnesium sulfate.
The calcium content for the carbonic acid magnesium products that the technique of existing processing magnesium-containing waste solution obtains is exceeded, therefore existing processing is useless containing magnesium
The technology of liquid is further improved.
Summary of the invention
The present invention is directed to solve at least some of the technical problems in related technologies.For this purpose, of the invention
One purpose is to propose a kind of method for handling magnesium-containing waste solution.This method can efficiently remove calcium constituent in carbonic acid magnesium products,
And guarantee that the calcium content in carbonic acid magnesium products is up to state standards.
In one aspect of the invention, the invention proposes a kind of methods for handling magnesium-containing waste solution, in the magnesium-containing waste solution
Containing magnesium sulfate, according to an embodiment of the invention, this method comprises:
(1) magnesium-containing waste solution is mixed with milk of lime, to obtain the slurry containing magnesium hydroxide and calcium sulfate；
(2) it is filtered after the slurry and carbon dioxide exposure by described containing magnesium hydroxide and calcium sulfate, to obtain sulfuric acid
Liquid after calcium and reaction containing magnesium bicarbonate and calcium bicarbonate；
(3) it is filtered after contacting liquid after the reaction containing magnesium bicarbonate and calcium bicarbonate with calcium remover, to obtain
Calcic slag and deliming containing magnesium bicarbonate are containing liquid after magnesium；
(4) deliming containing magnesium bicarbonate is pyrolyzed containing liquid after magnesium, to obtain carbonic acid magnesium products.
The method of processing magnesium-containing waste solution according to an embodiment of the present invention into the magnesium-containing waste solution containing magnesium sulfate by being added
Milk of lime and and carbon dioxide exposure, the calcium ion in solution is precipitated in the form of calcium sulfate precipitation, while being obtained containing carbonic acid
Then liquid after the reaction of hydrogen magnesium and calcium bicarbonate contacts liquid after the reaction containing magnesium bicarbonate and calcium bicarbonate with calcium remover,
Calcium bicarbonate therein is precipitated in the form of calcium carbonate calcic slag under the action of calcium remover, obtains the deliming containing magnesium bicarbonate
It containing liquid after magnesium, then is pyrolyzed, the carbonic acid magnesium products that calcium content is up to state standards can be obtained, and this method can be efficient
Ground removes calcium constituent in carbonic acid magnesium products, and guarantees that the calcium content in carbonic acid magnesium products is up to state standards.
In addition, the method for processing magnesium-containing waste solution according to the above embodiment of the present invention can also have following additional technology
Feature:
In some embodiments of the invention, the method for above-mentioned processing magnesium-containing waste solution further comprises: (5) are by step (3)
In the calcic slag mixed with sulfuric acid solution after filter, so as to liquid after obtaining calcium sulfate and deliming containing magnesium sulfate, and will
Liquid return step (1) is mixed with the milk of lime after the deliming containing magnesium sulfate.Thus, it can be achieved that magnesium fills in calcic slag
Divide recycling.
In some embodiments of the invention, in step (3), the calcium remover is selected from ammonium hydroxide, sodium hydroxide, hydrogen-oxygen
Change at least one of potassium and hydrazine hydrate.Be conducive to calcium as a result, to be precipitated sufficiently.
In some embodiments of the invention, in step (3), the concentration of the calcium remover is that 5-30wt% as a result, may be used
Improve the rate that calcium is precipitated.
In some embodiments of the invention, in step (3), after the reaction containing magnesium bicarbonate and calcium bicarbonate
Liquid and the calcium remover Contact Temperature are 20-50 degrees Celsius, time 0.5-2h.It can further improve the precipitation speed of calcium as a result,
Rate.
In some embodiments of the invention, in step (3), the use level coefficient of the calcium remover is 1.0~1.5.By
This, can further be conducive to calcium and be precipitated sufficiently.
In some embodiments of the invention, in step (4), the temperature of the pyrolysis processing is 50-100 degrees Celsius.
Carbonic acid magnesium products, while energy saving can be obtained as a result,.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Above-mentioned and/or additional aspect of the invention and advantage will become from the description of the embodiment in conjunction with the following figures
Obviously and it is readily appreciated that, in which:
Fig. 1 is the method flow schematic diagram of processing magnesium-containing waste solution according to an embodiment of the invention；
Fig. 2 is the method flow schematic diagram of the processing magnesium-containing waste solution of further embodiment according to the present invention.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
In one aspect of the invention, the invention proposes a kind of method for handling magnesium-containing waste solution, realities according to the present invention
Example is applied, with reference to Fig. 1, this method comprises:
S100: magnesium-containing waste solution is mixed with milk of lime
In the step, magnesium-containing waste solution is mixed with milk of lime, to obtain the slurry containing magnesium hydroxide and calcium sulfate
Body.Specifically, the magnesium in magnesium-containing waste solution mainly exists in the form of magnesium sulfate, and after milk of lime is added, magnesium sulfate and hydrogen therein
Calcium oxide reaction, generates calcium sulfate and magnesium hydroxide.Main chemical equation is as follows:
MgSO4+Ca(OH)2=CaSO4+Mg(OH)2 (1)
According to one embodiment of present invention, the use level coefficient of milk of lime is not particularly restricted, those skilled in the art
It can be selected according to actual needs, a specific embodiment according to the present invention, the use level coefficient of milk of lime can be 1-
1.1.It should be noted that the use level coefficient of milk of lime is the mole dosage coefficient of milk of lime herein, such as in above-mentioned use
Milk of lime precipitates the equation of magnesium, and calcium and magnesium molar ratio is 1:1, that is, milk of lime use level coefficient is 1, when for 1.1, milk of lime
Excessive 10%mol.Inventors have found that will cause the increase of slurry alkalinity, if milk of lime additional amount is excessive so as to cause containing for slurry
Calcium amount increases；And if the additional amount of milk of lime is very few, magnesium ion in slurry precipitating not exclusively, and then influences deliming effect.
Therefore, the deliming effect of magnesium-containing waste solution is remarkably improved using milk of lime use level coefficient proposed by the present invention.
S200: it will be filtered after slurry and carbon dioxide exposure containing magnesium hydroxide and calcium sulfate
In the step, it will be filtered after slurry and carbon dioxide exposure containing magnesium hydroxide and calcium sulfate, to obtain sulphur
Liquid after sour calcium and reaction containing magnesium bicarbonate and calcium bicarbonate.Specifically, the slurry containing magnesium hydroxide and calcium sulfate exists
After carbon dioxide exposure, magnesium hydroxide and calcium hydroxide in slurry react with carbon dioxide respectively, obtain containing carbon
Liquid after the reaction of sour hydrogen magnesium and calcium bicarbonate.Main chemical equation is as follows:
Mg(OH)2+2CO2=Mg (HCO3)2 (2)
Ca(OH)2+2CO2=Ca (HCO3)2 (3)
S300: it is filtered after liquid after the reaction containing magnesium bicarbonate and calcium bicarbonate is contacted with calcium remover
In the step, filtered after liquid after the reaction containing magnesium bicarbonate and calcium bicarbonate is contacted with calcium remover, so as to
Deliming to calcic slag and containing magnesium bicarbonate contains liquid after magnesium.Specifically, the work of calcium bicarbonate after reaction in liquid in calcium remover
Under, the deliming slag of sulfur acid calcium is generated, thus obtains the deliming containing magnesium bicarbonate containing liquid after magnesium.Inventors have found that the step
By the way that calcium remover is added in rapid, the calcium in liquid after reaction can be converted to precipitating and separated, so that subsequent gained
Calcium content in carbonic acid magnesium products is up to state standards.
According to one embodiment of present invention, the concrete type of calcium remover is not particularly restricted, those skilled in the art
It can be selected according to actual needs, a specific embodiment according to the present invention, calcium remover can be for selected from ammonium hydroxide, hydrogen-oxygen
Change at least one of sodium, potassium hydroxide and hydrazine hydrate, preferably saturation sodium hydroxide.Inventors have found that using such calcium remover
It can be significantly better than after other types raisings are reacted and remove ca efficiency in liquid, so that the calcium in subsequent gained carbonic acid magnesium products contains
Amount is up to state standards.
Specifically, main chemical equation is as follows in the step:
Ca(HCO3)2+2OH-=CaCO3↓+2H2O+CO3 2- (4)
The concentration of still another embodiment in accordance with the present invention, calcium remover is not particularly restricted, and those skilled in the art can
To be selected according to actual needs, a specific embodiment according to the present invention, the concentration of calcium remover can be 5-30wt%.
Inventors have found that if the too low water that will cause addition system of calcium remover concentration increases, and if calcium remover excessive concentration can be made
It is excessively high at local base concentration in solution entire after addition, so that losing excessive magnesium.Deliming proposed by the present invention is used as a result,
Agent concentration is remarkably improved the grade for removing ca efficiency and final gained carbonic acid magnesium products of magnesium-containing waste solution.
According to still another embodiment of the invention, liquid is contacted with calcium remover after the reaction containing magnesium bicarbonate and calcium bicarbonate
Condition be not particularly restricted, those skilled in the art can select according to actual needs, one according to the present invention
Specific embodiment, liquid and calcium remover Contact Temperature can be 20-50 degrees Celsius after the reaction containing magnesium bicarbonate and calcium bicarbonate,
Time can be 0.5-2h.Inventors have found that if contact of the liquid with calcium remover after the reaction containing magnesium bicarbonate and calcium bicarbonate
Temperature is excessively high, then magnesium bicarbonate therein can be pyrolyzed；And if liquid and calcium remover after the reaction containing magnesium bicarbonate and calcium bicarbonate
Contact Temperature it is too low, then reaction effect is poor；If contact of the liquid with calcium remover after the reaction containing magnesium bicarbonate and calcium bicarbonate
Overlong time will reduce the amount that magnesium-containing waste solution is handled in the unit time, and if after the reaction containing magnesium bicarbonate and calcium bicarbonate
The time of contact of liquid and calcium remover is too short, then reaction effect is poor.Contain magnesium bicarbonate and carbonic acid using proposed by the present invention as a result,
The condition that liquid is contacted with calcium remover after the reaction of hydrogen calcium can significantly propose to handle the production efficiency of magnesium-containing waste solution and final gained
The grade of carbonic acid magnesium products.
According to still another embodiment of the invention, the use level coefficient of calcium remover is not particularly restricted, those skilled in the art
Member can be selected according to actual needs, a specific embodiment according to the present invention, and the use level coefficient of calcium remover can be
1.0~1.5.It can further improve the rate of deliming as a result, while saving cost of material.
S400: the deliming containing magnesium bicarbonate is pyrolyzed containing liquid after magnesium
In the step, the deliming containing magnesium bicarbonate is pyrolyzed containing liquid after magnesium, to obtain carbonic acid magnesium products.Mainly
Chemical equation it is as follows:
Mg(HCO3)2=MgCO3+CO2+H2O (5)
According to one embodiment of present invention, the temperature of pyrolysis processing is not particularly restricted, and those skilled in the art can
To be selected according to actual needs, a specific embodiment according to the present invention, the temperature of pyrolysis processing can be 50-100
Degree Celsius.Inventors have found that if the temperature of pyrolysis processing is too low, pyrolytic reaction is incomplete, and if the temperature mistake of pyrolysis processing
Height, then energy consumption increases.The processing effect of magnesium-containing waste solution is remarkably improved using the temperature of pyrolysis processing proposed by the present invention as a result,
Rate, while energy saving.
The method of processing magnesium-containing waste solution according to an embodiment of the present invention into the magnesium-containing waste solution containing magnesium sulfate by being added
Milk of lime and and carbon dioxide exposure, the calcium ion in solution is precipitated in the form of calcium sulfate precipitation, while being obtained containing carbonic acid
Then liquid after the reaction of hydrogen magnesium and calcium bicarbonate contacts liquid after the reaction containing magnesium bicarbonate and calcium bicarbonate with calcium remover,
Calcium bicarbonate therein is precipitated in the form of calcium carbonate calcic slag under the action of calcium remover, obtains the deliming containing magnesium bicarbonate
It containing liquid after magnesium, then is pyrolyzed, the carbonic acid magnesium products that calcium content is up to state standards can be obtained, and this method can be efficient
Ground removes calcium constituent in carbonic acid magnesium products, and guarantees that the calcium content in carbonic acid magnesium products is up to state standards.
According to an embodiment of the invention, the method for above-mentioned processing magnesium-containing waste solution further comprises with reference to Fig. 2:
S500: it is filtered after the calcic slag in S300 is mixed with sulfuric acid solution
It in the step, is filtered after the calcic slag in S300 is mixed with sulfuric acid solution, to obtain calcium sulfate and to contain sulphur
Liquid after the deliming of sour magnesium, and liquid after the deliming containing magnesium sulfate is returned into S100 and is mixed with milk of lime.Wherein, calcium sulfate mainly with
The form of dihydrate gypsum exists.Be conducive to improve the sustainability and economy of entire method as a result,.
Below with reference to specific embodiment, present invention is described, it should be noted that these embodiments are only to describe
Property, without limiting the invention in any way.
Embodiment
100g magnesium-containing waste solution is mixed with 30g milk of lime, obtains the slurry containing magnesium hydroxide and calcium sulfate；Then
By its with filtered after carbon dioxide exposure, obtain liquid after calcium sulfate and reaction containing magnesium bicarbonate and calcium bicarbonate, this is anti-
Should after in liquid the content of magnesium be 10g/L, the content of calcium is 0.5g/L, to the reaction after the hydrogen that 4g concentration is 30wt% is added in liquid
Sodium hydroxide solution allows it to react 2h under conditions of 20 degrees Celsius with liquid after reacting containing magnesium bicarbonate and calcium bicarbonate, this
When, the use level coefficient of sodium hydroxide is 1.5, calcic slag and the deliming containing magnesium bicarbonate are obtained after reaction containing liquid after magnesium, wherein
Calcic slag filters after can mixing with sulfuric acid solution, obtains liquid after dihydrate gypsum and deliming containing magnesium sulfate, this contains magnesium sulfate
Deliming after liquid can be used as magnesium-containing waste solution return mixed with milk of lime；Finally the deliming containing magnesium bicarbonate is carried out containing liquid after magnesium
It is pyrolyzed, calcium content is 15ppm in obtained carbonic acid magnesium products, meets national standard.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (6)
1. a kind of method for handling magnesium-containing waste solution, contains magnesium sulfate in the magnesium-containing waste solution characterized by comprising
(1) magnesium-containing waste solution is mixed with milk of lime, to obtain the slurry containing magnesium hydroxide and calcium sulfate；
(2) filtered after the slurry and carbon dioxide exposure by described containing magnesium hydroxide and calcium sulfate, so as to obtain calcium sulfate with
And liquid after the reaction containing magnesium bicarbonate and calcium bicarbonate；
(3) it is filtered after contacting liquid after the reaction containing magnesium bicarbonate and calcium bicarbonate with calcium remover, to obtain calcic
Slag and deliming containing magnesium bicarbonate are containing liquid after magnesium；
(4) deliming containing magnesium bicarbonate is pyrolyzed containing liquid after magnesium, to obtain carbonic acid magnesium products,
In step (3), the calcium remover is selected from least one of ammonium hydroxide, sodium hydroxide, potassium hydroxide and hydrazine hydrate.
2. the method according to claim 1, wherein further comprising:
(5) it is filtered after mixing the calcic slag in step (3) with sulfuric acid solution, to obtain calcium sulfate and to contain magnesium sulfate
Deliming after liquid, and liquid return step (1) after the deliming containing magnesium sulfate is mixed with the milk of lime.
3. method according to claim 1 or 2, which is characterized in that in step (3), the concentration of the calcium remover is 5-
30wt%.
4. described to contain magnesium bicarbonate and bicarbonate according to the method described in claim 3, it is characterized in that, in step (3)
Liquid and the calcium remover Contact Temperature are 20-50 degrees Celsius after the reaction of calcium, time 0.5-2h.
5. according to the method described in claim 3, it is characterized in that, in step (3), the use level coefficient of the calcium remover is
1.0~1.5.
6. the method according to claim 1, wherein the temperature of the pyrolysis processing is 50- in step (4)
100 degrees Celsius.
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| CN115385366A (en) * | 2022-09-01 | 2022-11-25 | 广东邦普循环科技有限公司 | Treatment method of magnesium-containing waste liquid |
| CN115818679A (en) * | 2022-12-19 | 2023-03-21 | 中国建筑材料科学研究总院有限公司 | Magnesium-containing wastewater direct CO 2 Method for preparing magnesium carbonate by mineralization |
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| CN101016175A (en) * | 2006-02-12 | 2007-08-15 | 山东滨化集团有限责任公司 | Method of eliminating magnesium sulfate from magnesium sulfate containing waste water solution |
| CN101104522A (en) * | 2007-06-05 | 2008-01-16 | 昆明贵金属研究所 | Method for preparing active magnesium chloride by using magnesium sulfate waste liquid |
| CN101880772A (en) * | 2010-06-07 | 2010-11-10 | 中国恩菲工程技术有限公司 | Method for recycling magnesium from magnesium-containing waste solution |
| CN101870461B (en) * | 2010-03-22 | 2012-03-14 | 中国恩菲工程技术有限公司 | Method for treating waste liquid containing magnesium |
| CN103272572A (en) * | 2013-06-27 | 2013-09-04 | 武汉科梦环境工程有限公司 | Preparation method capable of absorbing Ca<2+> material from magnesium sulfate waste water |
| CN105858692A (en) * | 2016-05-13 | 2016-08-17 | 国家海洋局天津海水淡化与综合利用研究所 | Method for treating magnesium sulfate and magnesium sulfite wastewater by virtue of lime method |
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2017
- 2017-04-25 CN CN201710278476.5A patent/CN107098366B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016175A (en) * | 2006-02-12 | 2007-08-15 | 山东滨化集团有限责任公司 | Method of eliminating magnesium sulfate from magnesium sulfate containing waste water solution |
| CN101104522A (en) * | 2007-06-05 | 2008-01-16 | 昆明贵金属研究所 | Method for preparing active magnesium chloride by using magnesium sulfate waste liquid |
| CN101870461B (en) * | 2010-03-22 | 2012-03-14 | 中国恩菲工程技术有限公司 | Method for treating waste liquid containing magnesium |
| CN101880772A (en) * | 2010-06-07 | 2010-11-10 | 中国恩菲工程技术有限公司 | Method for recycling magnesium from magnesium-containing waste solution |
| CN103272572A (en) * | 2013-06-27 | 2013-09-04 | 武汉科梦环境工程有限公司 | Preparation method capable of absorbing Ca<2+> material from magnesium sulfate waste water |
| CN105858692A (en) * | 2016-05-13 | 2016-08-17 | 国家海洋局天津海水淡化与综合利用研究所 | Method for treating magnesium sulfate and magnesium sulfite wastewater by virtue of lime method |
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