CN109095484A - A method of utilizing desulfurization wastewater preparing magnesium hydroxide - Google Patents
A method of utilizing desulfurization wastewater preparing magnesium hydroxide Download PDFInfo
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- CN109095484A CN109095484A CN201811274295.6A CN201811274295A CN109095484A CN 109095484 A CN109095484 A CN 109095484A CN 201811274295 A CN201811274295 A CN 201811274295A CN 109095484 A CN109095484 A CN 109095484A
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- desulfurization wastewater
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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
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The present invention provides a kind of methods using desulfurization wastewater preparing magnesium hydroxide, the calcium ions and magnesium ions in desulfurization wastewater are separated by homogeneous, separation calcium ion, separation magnesium ion three phases, during softening desulfurization wastewater, improve byproduct, the especially purity of magnesia, to reach the standard that can be applied or sell, to generate economic benefit, realizing while handling waste water turns waste into wealth, and meets the theory of energy-saving and emission-reduction.
Description
Technical field
The present invention relates to technical field of waste water processing, and in particular to a kind of side using desulfurization wastewater preparing magnesium hydroxide
Method.
Background technique
China is a coal big country, statistics display, the SO in the whole nation 90%2Discharge amount is from fire coal, coal-fired SO2Control
System more seems extremely urgent.Currently, reducing SO2The approach of pollution has desulfurization before burning, desulfurization three after desulfurization and burning in burning
Class.FGD technology belongs to desulfurization technology after burning.By desulfurizing agent property, FGD technology can be divided into calcium method, magnesium processes, sodium method, ammonia process, have
Five kinds of methods of machine alkaline process.Wherein the main component of calcium method desulfurization is CaCO3(lime stone), since lime stone is cheap, obtains
What 90% or more commercial technologies used simply, therefore in the world is all calcium method.The U.S., Japan and Germany are all to burn at present
Afterwards based on desulphurization system.According to the existence form of desulfurizing agent, wet process, half-dried and three kinds of methods of dry desulfurization can be divided into.Wet process cigarette
Desulfurization technology with its device simple, desulfuration efficiency is high, at low cost the advantages that, account in flue gas desulfurization technique in the world leading
Status.Wherein most widely used Treatment process is calcium base wet-process flue gas desulfurization technology.But in removing SO2While, also produce
A large amount of desulfurization wastewater is given birth to.Since China is mainly based on calcium base wet-process flue gas desulfurization technology, so desulfurization wastewater is main
Ingredient includes Na+、Ca2+、Mg2+、Cl-、SO4 2-, COD, heavy metal ion, suspended matter.Currently, common desulfurization wastewater handles hand
Section has following several:
Chemical precipitation method relies primarily on and adds a large amount of soda ash and caustic soda to realize.The method is easy to operate, can remove big
Part COD, heavy metal ion, suspended matter and bivalent cation.But Cl-And SO4 2-Concentration does not reduce, and generates a large amount of
Muddy water mixed waste does not recycle valuable magnesium ion；And dosage is big, economic cost is high.
Evaporation (flue evaporation), is evaporated waste water using thermal energy.It is very simple with the method processing desulfurization wastewater.But
It is that cost is very high, and treating capacity is small.There is no substantive processing pollutants for the method, only by pollutant from liquid phase,
It is transferred in gas phase, this will result in the pollution of ambient enviroment salt, increases heavy metal in flue gas amount.In addition, in evaporating concentration process
Before, it needs to carry out softening pretreatment, this process needs to consume a large amount of medicaments, and cost price is high.It is highly concentrated in evaporating concentration process
The Cl of degree-The corrosion of serious unrepairable can be caused to evaporation equipment, flue, therefore it is corrosion-resistant to need to put into substantial contribution construction
Evaporation equipment flue.
There is scholar to be improved on the basis of chemical precipitation method principle in recent years, proposes new processing desulfurization wastewater
Method, major technique are as follows: the flue gas of power plant emission is passed through desulfurization wastewater, while Ca (OH) is added2, calcium ion is a large amount of
Precipitating；Then, NaOH is added into liquid phase to produce Mg (OH)2.But the method also has serious defect.First, flue gas
In not only contain CO2, there are also some other ingredients, and flue gas, which is passed through reaction tank, can hinder to react.Second, the method need by
Separating calcium and magnesium finally produces Mg (OH)2, but a large amount of Ca (OH) is but added during the reaction2, Ca is introduced again2+This
Sample is unfavorable for separating calcium and magnesium.Third, since separating calcium and magnesium is not thorough, so pressing this process route, finally obtained Mg (OH)2In
Necessarily contain Ca (OH)2, purity is low therefore economic benefit is low.4th, the method does not refer to Cl-、SO4 2-Whereabouts and processing disposition.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of method using desulfurization wastewater preparing magnesium hydroxide,
During softening waste water, by calcium ions and magnesium ions step-by-step processing, preparing magnesium hydroxide can be significantly reduced costs.
In order to achieve the above objectives, used technical solution is as follows by the present invention:
The present invention includes the following steps:
(1) homogeneous: by the abundant homogeneous of desulfurization wastewater, precipitate indissoluble object；Isolate supernatant；It can be in homogenizing process
So that various uniform ions dispersion in waste water, since desulfurization waste water quality water is there are certain fluctuation, abundant homogeneous can be with
So that the indissoluble object in desulfurization wastewater is obtained preliminary sedimentation, following chemical reaction occur in the process:
Ca2++SO4 2-=CaSO4↓
(2) it separates calcium ion: adding excessive readily soluble acid carbonate into supernatant, while adding and recapturing agent；It is to be precipitated
The precipitating and supernatant separation that will be generated after reaction when reaching maximum value；Will precipitating through filtering, obtain after drying and dehydrating mainly at
It is divided into calcium carbonate solid product；Need during this calcium ion concentration in first sample detection supernatant and heavy metal ion dense
Degree, is then calculated the amount of calcium ion and heavy metal ion according to supernatant total amount, so that it is determined that the carbonate that adds and again
Catch the amount of agent；The reaction occurred in the process is as follows:
Ca2++CO3 2-=CaCO3↓
Mg2++CO3 2-=MgCO3↓
M2++S2-=MS ↓
(3) it separates magnesium ion: slowly adding sodium hydroxide or potassium hydroxide solution in the supernatant in step (2), sink
When shallow lake reaches maximum value, it is aged；Precipitation and separation and supernatant；Precipitating is obtained into magnesium hydroxide after filtering, drying and dehydrating
Solid product；Need to control pH in the process in 10.0-11.5, the chemical reaction occurred in the process is as follows:
Mg2++2OH-=Mg (OH)2↓
(4) by supernatant reuse after film concentration in step (3).
As a further improvement of the present invention, readily soluble acid carbonate described in step (2) is sodium carbonate or potassium carbonate.
As a further improvement of the present invention, to guarantee that calcium ion precipitates completely, sodium carbonate or potassium carbonate should be excessive, add
Amount is 1.1-1.3 according to: the molar ratio of carbanion and calcium ion.
As a further improvement of the present invention, step (1) reaction time is 20~50min, pH control 7.0~
8.5,30~40 DEG C of reaction temperature.
As a further improvement of the present invention, due to Mg (OH)2Ksp be 5.61 × 10-12, therefore in the step (4)
PH control is 60-80 DEG C in 10-11.5, reaction time 20-50min, reaction temperature, this condition can guarantee magnesium hydroxide
Rate of deposition reach peak.
As a further improvement of the present invention, precipitation and separation and supernatant are divided using tubular membrane in the step (2)
From.
As a further improvement of the present invention, precipitation and separation and supernatant are divided using tubular membrane in the step (3)
From.
As a further improvement of the present invention, the digestion time be 60~90min, 60~80 DEG C of Aging Temperature, at this
Under the conditions of one, it is ensured that sedimentation is complete.
As a further improvement of the present invention, the magnesium hydroxide solid product is ground by grinder, obtains nanometer
The magnesium hydroxide products of grade.
Compared with prior art, the present invention has the following technical effect that
Traditional mode, which prepares magnesium hydroxide, to be prepared by raw material of magnesite, and the present invention is original with desulfurization wastewater
The magnesium hydroxide of material preparation high-purity, not only magnesium hydroxide purity obtained fully meets requirement, also reduces production cost, subtracts
Few waste discharge, brings huge economic benefit.
The present invention recycles calcium ions and magnesium ions step-by-step processing during softening desulfurization wastewater, the hydrogen-oxygen of high-purity
Change magnesium, can significantly reduce costs.And all production water are back to front end and continue in the process, end produces water reuse, realizes
Wastewater zero discharge, saves water resource, and economy is high.
The present invention utilizes tubular membrane precipitation and separation and supernatant, and the advantages of tubular membrane is, mandatory filtering, filter efficiency
It is high；Radius 20nm is retained, retention magnesium hydrate precipitate is facilitated；It can obviously solve the problems, such as the wall built-up in traditional intermediate processing；Automatically
Change degree is high, and occupied area is small.
Detailed description of the invention
Attached drawing 1 is process flow chart of the invention.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
As shown in Figure 1, the present invention includes the following steps:
(1) homogeneous: by the abundant homogeneous of desulfurization wastewater, precipitate indissoluble object；Isolate supernatant；It can be in homogenizing process
So that various uniform ion dispersions, indissoluble object precipitate under the effect of gravity in waste water, certain anion are also had in dispersion process
It is combined with cation and generates indissoluble object, following chemical reaction occurs in the process:
Ca2++SO4 2-=CaSO4↓
(2) separate calcium ion: adding excessive sodium carbonate liquor into supernatant, dosage according to: carbanion with
The molar ratio of calcium ion is 1.1-1.3, while adding and recapturing agent；Reaction time is 20~50min, pH control 7.0~8.5,
30~40 DEG C of reaction temperature；The precipitating generated after reaction is separated with supernatant using tubular type film device；Precipitating is filtered, is done
It is calcium carbonate solid product that main component is obtained after dry dehydration；Need the calcium ion in first sample detection supernatant dense during this
Degree and concentration of heavy metal ion, are then calculated the amount of calcium ion and heavy metal ion according to supernatant total amount, so that it is determined that
The carbonate added and the amount for recapturing agent；
The reaction occurred in the process is as follows:
Ca2++CO3 2-=CaCO3↓
Mg2++CO3 2-=MgCO3↓
M2++S2-=MS ↓
(3) it separates magnesium ion: slowly adding sodium hydroxide or potassium hydroxide solution, Mg in the supernatant in step (2)
(OH)2Ksp be 5.61 × 10-12, therefore pH control is in 10.0-11.5, reaction time 20-50min, reaction temperature 60-
80 DEG C, be aged, digestion time be 60~90min, 60~80 DEG C of Aging Temperature, under this condition, it is ensured that sedimentation
Completely；With tubular type film device precipitation and separation and supernatant；Precipitating is obtained to magnesium hydroxide solid to produce after filtering, drying and dehydrating
Product；The chemical reaction occurred in the process is as follows:
Mg2++2OH-=Mg (OH)2↓
Magnesium hydroxide solid product is ground by grinder, obtains nanoscale magnesium hydroxide products.
(4) by supernatant reuse after film concentration in step (3).
Embodiment 1:
Take certain factory desulfurization wastewater 100L, after chemical examination, calcium ion concentration 5763mg/L, magnesium ion concentration 2978mg/L.
Desulfurization wastewater is imported and flows into reaction tank 1 behind homogeneous pond, homogeneous 3h, 1600g Na is added in reaction tank 12CO3, during which add
Enter NaOH control pH in 7.0~8.5, reaction time 30min, 35 DEG C of reaction temperature；The water removed in plate and frame filter press imports equal
Matter pond；The solids of generation carries out disposition of solid waste.15% NaOH solution is slowly added in reaction tank 2, this process
PH is controlled in 10.0~11.5, reaction time 30min, 70 DEG C of reaction temperature, is aged 90min, 70 DEG C of Aging Temperature.Plate compression
The water removed in machine imports homogeneous pond；The mud cake of plate and frame filter press discharge, the product after nano-level grinder is ground is hydrogen
Magnesia；In this example, the rate of recovery of magnesium ion is 95.55%, and the purity of nanometric magnesium hydroxide obtained is 97.37%,
Flowing into calcium ion concentration in the water of film condensing device is 2mg/L, magnesium ion concentration 13mg/L.
Embodiment 2:
Take certain factory desulfurization wastewater 100L, after chemical examination, calcium ion concentration 3457mg/L, magnesium ion concentration 6784mg/L.
Desulfurization wastewater is imported and flows into reaction tank 1 behind homogeneous pond, homogeneous 3h, 980g Na is added in reaction tank 12CO3, during which it is added
NaOH controls pH in 7.0~8.5, reaction time 40min, and 33 DEG C of reaction temperature；The water removed in plate and frame filter press imports homogeneous
Pond；The solids of generation carries out disposition of solid waste.15% NaOH solution is slowly added in reaction tank 2, this is excessively program-controlled
PH processed is in 10.0~11.5, reaction time 40min, 60 DEG C of reaction temperature, is aged 60min, and 60 DEG C of Aging Temperature.Plate and frame filter press
The water of middle removing imports homogeneous pond；The mud cake of plate and frame filter press discharge, the product after nano-level grinder is ground is hydrogen-oxygen
Change magnesium；In this example, the rate of recovery of magnesium ion is 94.37%, and the purity of nanometric magnesium hydroxide obtained is 97.23%, stream
Entering calcium ion concentration in the water of film condensing device is 3mg/L, magnesium ion concentration 16mg/L.
Embodiment described above is only that preferred embodiment of the invention is described, and is not carried out to the scope of the present invention
It limits, without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention
Various changes and improvements, should all fall into claims of the present invention determine protection scope in.
Claims (9)
1. a kind of method using desulfurization wastewater preparing magnesium hydroxide, which comprises the steps of:
(1) homogeneous: by the abundant homogeneous of desulfurization wastewater, precipitate indissoluble object；Isolate supernatant；
(2) it separates calcium ion: adding excessive readily soluble acid carbonate into supernatant, while adding and recapturing agent；It is to be precipitated to reach
The precipitating and supernatant separation that will be generated after reaction when maximum value；It is carbon that precipitating obtains main component after filtering, drying and dehydrating
Sour calcium solid product；
(3) it separates magnesium ion: slowly adding sodium hydroxide or potassium hydroxide solution in the supernatant in step (2), precipitating reaches
When to maximum value, it is aged；Wait settle completely, precipitation and separation and supernatant；Precipitating is obtained into hydrogen after filtering, drying and dehydrating
Magnesia solid product；
(4) by supernatant reuse after film concentration in step (3).
2. a kind of method using desulfurization wastewater preparing magnesium hydroxide according to claim 1, which is characterized in that step
(2) the readily soluble acid carbonate described in is sodium carbonate or potassium carbonate.
3. a kind of method using desulfurization wastewater preparing magnesium hydroxide according to claim 2, which is characterized in that sodium carbonate
Or potassium carbonate dosage is 1.1-1.3 according to: the molar ratio of carbanion and calcium ion.
4. a kind of method using desulfurization wastewater preparing magnesium hydroxide according to claim 1, which is characterized in that the step
Suddenly (1) reaction time is 20~50min, and pH is controlled 7.0~8.5,30~40 DEG C of reaction temperature.
5. a kind of method using desulfurization wastewater preparing magnesium hydroxide according to claim 1, which is characterized in that the step
Suddenly pH control is in 10.0-11.5 in (4), and reaction time 20-50min, reaction temperature is 60-80 DEG C.
6. a kind of method using desulfurization wastewater preparing magnesium hydroxide according to claim 1, which is characterized in that the step
Suddenly precipitation and separation is separated with supernatant using tubular membrane in (2).
7. a kind of method using desulfurization wastewater preparing magnesium hydroxide according to claim 1, which is characterized in that the step
Suddenly precipitation and separation is separated with supernatant using tubular membrane in (3).
8. a kind of method using desulfurization wastewater preparing magnesium hydroxide according to claim 7, which is characterized in that described old
The change time be 60~90min, 60~80 DEG C of Aging Temperature.
9. a kind of method using desulfurization wastewater preparing magnesium hydroxide according to claim 1, which is characterized in that will be described
Magnesium hydroxide solid product is ground by grinder, obtains nanoscale magnesium hydroxide products.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111675229A (en) * | 2020-04-27 | 2020-09-18 | 广东粤电靖海发电有限公司 | Process for purifying magnesium hydroxide from desulfurization wastewater of coal-fired power plant |
| CN114853212A (en) * | 2022-05-09 | 2022-08-05 | 纪宏轩 | Zero-emission recycling treatment method for magnesium sulfate wastewater |
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| CN114853212A (en) * | 2022-05-09 | 2022-08-05 | 纪宏轩 | Zero-emission recycling treatment method for magnesium sulfate wastewater |
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