CN105967212A - Method for preparing potassium sulphate by using potassium salt in sintering machine head electric dust removal ash - Google Patents
Method for preparing potassium sulphate by using potassium salt in sintering machine head electric dust removal ash Download PDFInfo
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- CN105967212A CN105967212A CN201610314890.2A CN201610314890A CN105967212A CN 105967212 A CN105967212 A CN 105967212A CN 201610314890 A CN201610314890 A CN 201610314890A CN 105967212 A CN105967212 A CN 105967212A
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- potassium
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- potassium salt
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/06—Preparation of sulfates by double decomposition
Abstract
The invention discloses a method for preparing potassium sulphate by using potassium salt in sintering machine head electric dust removal ash, and belongs to the technical field of harmless resource utilization of waste steel and iron slag. The method comprises the following steps: collecting sintering machine head electric dust removal ash which is rich in the potassium salt, washing the sintering machine head electric dust removal ash which is rich in the potassium salt by using a weakly acidic aqueous solution, fully stirring until the solution is homogenized, standing, and performing solid-liquid separation to obtain an eluant I and a precipitate I; adding K2CO3 into the eluant I to remove impurities, fully stirring after the K2CO3 is dissolved, and performing the solid-liquid separation to obtain a filtrate II and a precipitate II; adjusting the pH value of the filtrate II, adding 3K2SO4.Na2SO4 to perform a metathesis reaction, and separating potassium and sodium by adopting the processes of evaporation concentration and crystallization to obtain a potassium sulphate product, wherein the purity of the potassium sulphate product can meet GB20406-2006 powder crystal first-grade product index requirements. The overall process is simple and feasible; the production cost is low; effective recovery of iron, vanadium and titanium and effective utilization of the potassium salt in electric field dust removal ash can be realized.
Description
Technical field
The invention belongs to the application technology as the second resource field of waste steel slag, be specifically related to one sintering machine head end electro-precipitating dust
The method of middle potassium salt preparing potassium sulfate.
Background technology
During sintering machine head end electro-precipitating dust (being called for short sintering ash) is iron ore sintering, the flue gas collected by electric cleaner
With dust, its generation amount accounts for the 1%-2% of Sintering Yield, one of primary pollution source of sintering Hui Shi iron and steel enterprise.Burn at present
The comprehensive Utilization Ways of knot ash, mainly uses directly with addition of to sinter mixture reuse, and sinters adding of ash and make sintering
Compound, rich in the harmful element such as zinc and alkali metal, has a strong impact on blast fumance.Therefore, a lot of iron and steel enterprises are by electric precipitation dust heap
Amass, both wasted soil, financial resources, manpower, also buried the hidden danger of secondary environmental pollution.Exploitation is efficiently, economical and environmentally friendly
Sintering ash in alkali-metal removal and recycling new technique, it has also become the important class that domestic big-and-middle-sized iron and steel enterprise produces
Topic.
After within 2015, new environmental law is implemented, sintering ash is taken out and be there is the problems such as environmental protection joint liability risk, therefore, and sintering ash
Innoxious, application technology as the second resource highlights necessity.And innoxious, the recycling of sintering ash meets what National Development and Reform Committee issued
" industry restructuring guidance list ", belongs to country and encourages class development projects, enjoy preferential tax policy.This technology belongs to simultaneously
" the preferential catalogue of comprehensive utilization of resources enterprise income tax ", the environmental protection technology catalogue of development " country encourage " and " country is first
Enter pollutant abatement technology and promote demonstrative project register " Listed Items, national policy bonus pool can be declared and implementation tax revenue subtracts
Exempt from.
Additionally, China is the country that a potassium resource is the deficientest, 84% soil potassium deficiency, limit the exploitation of potash fertilizer
And development, make crops Main Nutrients nitrogen phosphoris and potassium fertilizer ratio numerous imbalances.The principal item of potash fertilizer has potassium chloride, potassium sulfate, nitric acid
Potassium, owing to fear-chlorion crop can not use potassium chloride, potassium nitrate is expensive, and is explosive, uses and is restricted.Potassium sulfate can be same
Time provide crops need potassium and sulfur, low price, be preferably used for fear-chlorion crop, so potassium sulphate fertilizer is higher than potassium chloride fertilizer has
Use value.Utilize sintering ash in potassium salt produce potassium sulfate, and reclaim the elements such as ferrum, vanadium, titanium return sintering recycling, can realize
Innoxious, the minimizing of sintering ash, recycling, have a extensive future.
Summary of the invention
The technical problem to be solved in the present invention is to provide potassium salt preparing potassium sulfate in a kind of sintering machine head end electro-precipitating dust
Method.
For solving above-mentioned technical problem, the present invention adopts the following technical scheme that potassium in one sintering machine head end electro-precipitating dust
The method of salt preparing potassium sulfate, concrete grammar comprises the steps:
(1) collect sintering machine head end electric field dedusting ash, in weakly acidic solution wash, be sufficiently stirred for 40-60 minute to homogenizing, quiet
Putting, solid-liquid separation obtains eluent I and precipitate I;
(2) in eluent I, K is added2CO3Remove impurity, is sufficiently stirred for after dissolving and solid-liquid separation obtains filtrate II and precipitate
Ⅱ;
(3) regulate the pH value of filtrate II, add glaserite and carry out metathesis reaction, use evaporation and concentration, crystallization processes to separate
Potassium, sodium, obtain potassium product.
In sintering machine head end electric field dedusting ash in step of the present invention (1), except rich in ferrum, calcium, magnesium, potassium (5-15%),
Outside the element such as sodium, chlorine, efficient recovery need to be carried out possibly together with scarce resource vanadium, titanium.
Water lotion in step of the present invention (1) is faintly acid, it is therefore an objective to make electro-precipitating dust potassium, sodium when washing separate
More thorough.The temperature of this weak acid water washing liquid is 25-35 DEG C, and pH is 2-6, and regulation pH value acid is sulphuric acid, and principle is increased without molten
Interfering ion in liquid.
Precipitate I in step of the present invention (1) is the tailings after electro-precipitating dust is washed under weakly acidic condition, rich in
Ferrum, vanadium, titanium elements, return for sinter mixture after dehydration.
Remove impurity material in step of the present invention (2) selects K2CO3, purpose does not increase the quantity of effects of ion, and it adds
Enter amount and must ensure the pH=8-13, remove impurity material K of eluent I2CO3Removable calcium, magnesium and other metal ion.
The pH value of the regulation filtrate II in step of the present invention (3) is to neutral, and regulation pH value acid is hydrochloric acid, to keep away
Exempt to increase the interfering ion in solution.
Metathesis reaction conditions in step of the present invention (3) is: adds glaserite and is stirred well to homogenizing, reaction temperature
Degree controls at 25-30 DEG C, and question response, completely to potassium sulfate crystal region, stands, and now solution is K+、Na+//Cl-、SO4 2--- H2O
Quaternary salt-water system.
Evaporation, crystallization condition in step of the present invention (3) be: solution evaporation thickening temperature is 90-100 DEG C, and this is
Saturated solution altogether;Solution is cooled to 25-30 DEG C and completes crystallization process afterwards, and saturation is in metasable state saturation region, big in order to separating out
Granular potassium sulfate crystal, 1-3 hour persistent period.
Mother liquor recycle after crystallization in step of the present invention (3), separation uses, higher to ensure in eluent I
The yield of potassium in potassium content and this method.
In step of the present invention (3), potassium sulfate purity is wanted up to GB20406-2006 powder crystallization shape Grade A index
Ask.
Material used by potassium sulfate making of the present invention is glaserite, and its molecular formula is 3K2SO4·Na2SO4, its metathesis reaction
For: 3K2SO4·Na2SO4+2KCl→3K2SO4+2NaCl
Evaporative crystallization theoretical foundation of the present invention is K+、Na+//Cl-、SO4 2--- H2O quaternary Phase Diagram for Aqueous Salt Solutions, any
At a temperature of, potassium sulfate is the most non-conterminous with the crystal region of sodium chloride, is effectively separated the two accordingly.
Use and have the beneficial effect that the potassium salt purity that the present invention prepares is higher produced by technique scheme, can reach
GB20406-2006 powder crystallization shape Grade A index request;Integrated artistic is simple, and production cost is low;Achieve electric field to remove
The efficient recovery of ferrum, vanadium, titanium in dirt ash, the efficient utilization of potassium salt, is to make that electric field dedusting ash is innoxious, the typical case of resource
One of.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further detailed explanation.
Above-mentioned electric field dedusting ash presented below produces the specific embodiment of potash fertilizer.
Embodiment 1
A kind of method of potassium salt preparing potassium sulfate in sintering machine head end electro-precipitating dust, concrete grammar comprises the steps:
(1) the mass fraction scope of each metallic element in electric field dedusting ash 1(electro-precipitating dust of collecting is shown in Table 1), with the sulfur of pH=2.5
Aqueous acid dissolves, be sufficiently stirred for 40 minutes to homogenizing, stand, solid-liquid separation obtains eluent I and precipitate I;Precipitate I is weak
Tailings after washing under acid environment, rich in ferrum, vanadium, titanium elements, returns for sinter mixture after dehydration.
(2) in eluent I, K is added2CO3Remove impurity, is sufficiently stirred for making the pH=8 of solution, solid-liquid separation obtain filtrate II
And precipitate II;K2CO3Remove the metal ions such as Fe, Ca, Mg, Al, Mn;
(3) it is neutral for regulating filtrate II pH value with hydrochloric acid, adds glaserite and carries out metathesis reaction, uses evaporation and concentration, knot
Brilliant technique separating potassium, sodium, obtain potassium product, crystallize, separate after mother liquor recycle use.
Metathesis reaction conditions is: adding glaserite and be stirred well to homogenizing, reaction temperature 30 DEG C, question response is completely to sulfur
Acid potassium crystal region, stands, and now solution is K+、Na+//Cl-、SO4 2--- H2O quaternary salt-water system.
Evaporate, crystallization condition is: evaporation and concentration temperature is 100 DEG C, and this is saturated solution altogether;Solution is cooled to 30 DEG C afterwards
Completing crystallization process, saturation is in metasable state saturation region, in order to separating out large-particle potassium sulfate crystal, 1 hour persistent period.
Embodiment 2
A kind of method of potassium salt preparing potassium sulfate in sintering machine head end electro-precipitating dust, concrete grammar comprises the steps:
(1) the mass fraction scope of each metallic element in electric field dedusting ash 2(electro-precipitating dust of collecting is shown in Table 1), with the sulfur of pH=3.5
Aqueous acid dissolve, be sufficiently stirred for 50 minutes to homogenizing, solid-liquid separation obtains eluent I and precipitate I;Precipitate I is weak acid ring
Tailings after washing under border, rich in ferrum, vanadium, titanium elements, returns for sinter mixture after dehydration.
(2) in eluent I, K is added2CO3Remove impurity, is sufficiently stirred for making the pH=9.5 of solution, solid-liquid separation obtain filtrate
II and precipitate II;K2CO3The metal ions such as removable Fe, Ca, Mg, Al, Mn;
(3) it is neutral for regulating filtrate II pH value with hydrochloric acid, adds glaserite and carries out metathesis reaction, uses evaporation and concentration, knot
Brilliant technique separating potassium, sodium, obtain potassium product, crystallize, separate after mother liquor recycle use.
Metathesis reaction conditions is: adding glaserite and be stirred well to homogenizing, reaction temperature 25 DEG C, question response is completely to sulfur
Acid potassium crystal region, stands, and now solution is K+、Na+//Cl-、SO4 2--- H2O quaternary salt-water system.
Evaporate, crystallization condition is: evaporation and concentration temperature is 90 DEG C, and this is saturated solution altogether;Solution is cooled to 25 DEG C afterwards
Completing crystallization process, saturation is in metasable state saturation region, in order to separating out large-particle potassium sulfate crystal, 1.5 hours persistent period.
Embodiment 3
A kind of method of potassium salt preparing potassium sulfate in sintering machine head end electro-precipitating dust, concrete grammar comprises the steps:
(1) the mass fraction scope of each metallic element in electric field dedusting ash 3(electro-precipitating dust of collecting is shown in Table 1), with the salt of pH=4.5
Aqueous acid dissolve, be sufficiently stirred for 50 minutes to homogenizing, solid-liquid separation obtains eluent I and precipitate I;Precipitate I is weak acid ring
Tailings after washing under border, rich in ferrum, vanadium, titanium elements, returns for sinter mixture after dehydration.
(2) in eluent I, K is added2CO3Remove impurity, is sufficiently stirred for making the pH=10.5 of solution, solid-liquid separation obtain filtrate
II and precipitate II;K2CO3The metal ions such as removable Fe, Ca, Mg, Al, Mn;
(3) it is neutral for regulating filtrate II pH value with sulphuric acid, adds glaserite and carries out metathesis reaction, uses evaporation and concentration, knot
Brilliant technique separating potassium, sodium, obtain potassium product, crystallize, separate after mother liquor recycle use.
Metathesis reaction conditions is: adding glaserite and be stirred well to homogenizing, reaction temperature 28 DEG C, question response is completely to sulfur
Acid potassium crystal region, stands, and now solution is K+、Na+//Cl-、SO4 2--- H2O quaternary salt-water system.
Evaporate, crystallization condition is: evaporation and concentration temperature is 95 DEG C, and this is saturated solution altogether;Solution is cooled to 29 DEG C afterwards
Completing crystallization process, saturation is in metasable state saturation region, in order to separating out large-particle potassium sulfate crystal, 2.5 hours persistent period.
Embodiment 4
A kind of method of potassium salt preparing potassium sulfate in sintering machine head end electro-precipitating dust, concrete grammar comprises the steps:
(1) the mass fraction scope of each metallic element in electric field dedusting ash 4(electro-precipitating dust of collecting is shown in Table 1), with the sulfur of pH=5.5
Aqueous acid dissolve, be sufficiently stirred for 60 minutes to homogenizing, solid-liquid separation obtains eluent I and precipitate I;Precipitate I is weak acid ring
Tailings after washing under border, rich in ferrum, vanadium, titanium elements, returns for sinter mixture after dehydration.
(2) in eluent I, K is added2CO3Remove impurity, is sufficiently stirred for making the pH=13 of solution, solid-liquid separation obtain filtrate II
And precipitate II;K2CO3The metal ions such as removable Fe, Ca, Mg, Al, Mn;
(3) it is neutral for regulating filtrate II pH value with hydrochloric acid, adds glaserite and carries out metathesis reaction, uses evaporation and concentration, knot
Brilliant technique separating potassium, sodium, obtain potassium product, crystallize, separate after mother liquor recycle use.
Metathesis reaction conditions is: adding glaserite and be stirred well to homogenizing, reaction temperature 26 DEG C, question response is completely to sulfur
Acid potassium crystal region, stands, and now solution is K+、Na+//Cl-、SO4 2--- H2O quaternary aqueous systems.
Evaporate, crystallization condition is: evaporation and concentration temperature is 97 DEG C, and this is saturated solution altogether;Solution is cooled to 27 DEG C afterwards
Completing crystallization process, saturation is in metasable state saturation region, in order to separating out large-particle potassium sulfate crystal, 3 hours persistent period.
The elementary analysis result (%) of table 1 sintering machine head end each electric field dedusting ash
Sequence number | Element | Electro-precipitating dust 1 | Electro-precipitating dust 2 | Electro-precipitating dust 3 | Electro-precipitating dust 4 |
1 | Fe | 35.2 | 32.7 | 38.8 | 41.7 |
2 | Ca | 6.00 | 5.71 | 6.39 | 5.43 |
3 | Mg | 0.87 | 0.73 | 1.22 | 0.92 |
4 | K | 10.60 | 12.5 | 7.45 | 5.76 |
5 | Na | 2.22 | 2.55 | 1.89 | 1.52 |
6 | Ti | 0.59 | 0.49 | 0.83 | 0.72 |
7 | Pb | 0.034 | 0.041 | 0.036 | 0.19 |
8 | Zn | 0.058 | 0.064 | 0.017 | 0.045 |
9 | Al | 0.62 | 0.56 | 0.93 | 0.75 |
10 | Mn | 0.16 | 0.14 | 0.24 | 0.20 |
11 | V | 0.088 | 0.08 | 0.106 | 0.099 |
12 | Cr | 0.065 | 0.062 | 0.091 | 0.076 |
13 | Cu | 0.12 | 0.15 | 0.017 | 0.073 |
14 | P | 0.047 | 0.041 | 0.071 | 0.053 |
15 | S | 1.79 | 2.17 | 0.60 | 0.82 |
Aforementioned four embodiment test data result such as table 2 below
Table 2 embodiment 1-4 test data
Above example is only in order to illustrative not limiting technical scheme, although entering the present invention with reference to above-described embodiment
Go detailed description, it will be understood by those within the art that: still the present invention can be modified or be equal to and replace
Changing, any modification or partial replacement without departing from the spirit and scope of the present invention, its right that all should contain in the present invention is wanted
Ask in the middle of scope.
Claims (10)
1. one kind by the method for potassium salt preparing potassium sulfate in sintering machine head end electro-precipitating dust, it is characterised in that concrete grammar include as
Lower step:
(1) collect the sintering machine head end electric field dedusting ash rich in potassium salt, wash in slightly acidic water solution, be sufficiently stirred for 40-60 and divide
Clock, to homogenizing, stands, and solid-liquid separation obtains eluent I and precipitate I;
(2) in described eluent I, K is added2CO3Remove impurity, is sufficiently stirred for after dissolving and solid-liquid separation obtains filtrate II and precipitation
Thing II;
(3) regulate the pH value of filtrate II, add glaserite and carry out metathesis reaction, use evaporation and concentration, crystallization processes to separate
Potassium, sodium, obtain potassium product.
The method of potassium salt preparing potassium sulfate, its feature in a kind of sintering machine head end electro-precipitating dust the most according to claim 1
It is: in the sintering machine head end electric field dedusting ash in described step (1), in addition to rich in elements such as ferrum, calcium, magnesium, potassium, sodium, chlorine, also
Efficient recovery need to be carried out containing scarce resource vanadium, titanium.
The method of potassium salt preparing potassium sulfate, its feature in a kind of sintering machine head end electro-precipitating dust the most according to claim 1
It is: the precipitate I in described step (1) is the tailings after electro-precipitating dust is washed under weakly acidic condition, rich in ferrum, vanadium, titanium unit
Element, returns for sinter mixture after dehydration.
4. according to the side of potassium salt preparing potassium sulfate in a kind of sintering machine head end electro-precipitating dust described in claim 1-3 any one
Method, it is characterised in that: in described step (1), the washing temperature of weakly acidic solution is 25-35 DEG C, and pH is 2-6, regulation pH value acid
For sulphuric acid.
5. according to the side of potassium salt preparing potassium sulfate in a kind of sintering machine head end electro-precipitating dust described in claim 1-3 any one
Method, it is characterised in that: the remove impurity material in described step (2) selects K2CO3, its addition must ensure the pH=8-13 of eluent I,
Remove impurity material K2CO3Removable calcium, magnesium and other metal ion.
6. according to the side of potassium salt preparing potassium sulfate in a kind of sintering machine head end electro-precipitating dust described in claim 1-3 any one
Method, it is characterised in that: the pH value of the regulation filtrate II in described step (3) is to neutral, and regulation pH value acid is hydrochloric acid.
7. according to the side of potassium salt preparing potassium sulfate in a kind of sintering machine head end electro-precipitating dust described in claim 1-3 any one
Method, it is characterised in that: the metathesis reaction conditions in described step (3) is: adds glaserite and is stirred well to homogenizing, reaction temperature
Degree controls at 25-30 DEG C, and question response, completely to potassium sulfate crystal region, stands, and now solution is K+、Na+//Cl-、SO4 2--- H2O
Quaternary salt-water system.
8. according to the side of potassium salt preparing potassium sulfate in a kind of sintering machine head end electro-precipitating dust described in claim 1-3 any one
Method, it is characterised in that: evaporation, crystallization condition in described step (3) be: evaporation and concentration temperature is 95-100 DEG C, and this is for the fullest
And solution;Solution is cooled to 25-30 DEG C and completes crystallization process afterwards, and saturation is in metasable state saturation region, in order to separating out bulky grain
Potassium sulfate crystal, 1-3 hour persistent period.
9. according to the side of potassium salt preparing potassium sulfate in a kind of sintering machine head end electro-precipitating dust described in claim 1-3 any one
Method, it is characterised in that: the Recycling Mother Solution after crystallization in described step (3), separation uses, to ensure potassium higher in eluent I
The yield of potassium in content and this method.
10. according to potassium salt preparing potassium sulfate in a kind of sintering machine head end electro-precipitating dust described in claim 1-3 any one
Method, it is characterised in that: in described step (3), potassium sulfate purity is wanted up to GB20406-2006 powder crystallization shape Grade A index
Ask.
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Cited By (9)
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CN107161968A (en) * | 2017-05-31 | 2017-09-15 | 攀枝花火凤凰再生资源回收利用有限责任公司 | The method of comprehensive utilization of potassium in a kind of sintering flue dust |
CN108946767A (en) * | 2018-08-27 | 2018-12-07 | 中国科学院过程工程研究所 | A kind of method of sodium potassium sulphur chlorine quaternary system separation potassium sulfate |
CN111498870A (en) * | 2020-04-23 | 2020-08-07 | 苏州固利环保科技有限公司 | Method for treating sintering machine head ash in steel mill by using chemical production byproduct potassium carbonate |
CN111847484A (en) * | 2020-06-17 | 2020-10-30 | 五矿(湖南)铁合金有限责任公司 | Method and system for preparing agricultural potassium sulfate from manganese-series ferroalloy smelting dedusting ash |
CN113800538A (en) * | 2020-06-17 | 2021-12-17 | 南风化工集团股份有限公司 | Method for extracting potassium sulfate and sodium chloride from sintering ash |
CN114314613A (en) * | 2021-12-24 | 2022-04-12 | 安阳钢铁股份有限公司 | Method for preparing potassium sulfate by sintering desulfurization dust removal ash based on ammonia additive |
CN114702188A (en) * | 2021-09-07 | 2022-07-05 | 中冶长天国际工程有限责任公司 | Method and system for co-processing high-salinity solid waste ash and acid wastewater of iron and steel plant |
CN114956424A (en) * | 2022-05-31 | 2022-08-30 | 中冶赛迪技术研究中心有限公司 | Sintering machine head ash deamination method using desulfurization waste liquid treatment system |
CN115365279A (en) * | 2021-05-21 | 2022-11-22 | 钢铁研究总院 | Method for cooperatively treating machine head fly ash and garbage fly ash by magnesium desulfurization wastewater |
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CN108946767A (en) * | 2018-08-27 | 2018-12-07 | 中国科学院过程工程研究所 | A kind of method of sodium potassium sulphur chlorine quaternary system separation potassium sulfate |
CN108946767B (en) * | 2018-08-27 | 2020-11-20 | 中国科学院过程工程研究所 | Method for separating potassium sulfate by using sodium-potassium-sulfur-chlorine quaternary system |
CN111498870A (en) * | 2020-04-23 | 2020-08-07 | 苏州固利环保科技有限公司 | Method for treating sintering machine head ash in steel mill by using chemical production byproduct potassium carbonate |
CN111847484A (en) * | 2020-06-17 | 2020-10-30 | 五矿(湖南)铁合金有限责任公司 | Method and system for preparing agricultural potassium sulfate from manganese-series ferroalloy smelting dedusting ash |
CN113800538A (en) * | 2020-06-17 | 2021-12-17 | 南风化工集团股份有限公司 | Method for extracting potassium sulfate and sodium chloride from sintering ash |
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CN114702188B (en) * | 2021-09-07 | 2023-10-10 | 中冶长天国际工程有限责任公司 | Method and system for cooperatively treating high-salt solid waste ash and acid wastewater of steel plant |
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CN114314613A (en) * | 2021-12-24 | 2022-04-12 | 安阳钢铁股份有限公司 | Method for preparing potassium sulfate by sintering desulfurization dust removal ash based on ammonia additive |
CN114956424B (en) * | 2022-05-31 | 2023-09-26 | 中冶赛迪技术研究中心有限公司 | Sintering machine head ash deamination method utilizing desulfurization waste liquid disposal system |
CN114956424A (en) * | 2022-05-31 | 2022-08-30 | 中冶赛迪技术研究中心有限公司 | Sintering machine head ash deamination method using desulfurization waste liquid treatment system |
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