CN110042243A - A method of processing head ash - Google Patents
A method of processing head ash Download PDFInfo
- Publication number
- CN110042243A CN110042243A CN201910238226.8A CN201910238226A CN110042243A CN 110042243 A CN110042243 A CN 110042243A CN 201910238226 A CN201910238226 A CN 201910238226A CN 110042243 A CN110042243 A CN 110042243A
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- China
- Prior art keywords
- filtrate
- filter residue
- crystal
- head ash
- sediment
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The present invention relates to chemical fields, and in particular to a method of processing head ash, specific steps include that (1) head ash carries out washing process and filters, and obtain the first filtrate and the first filter residue；(2) it adjusts the first filtrate pH value to neutrality to carry out Crystallization Separation, obtains KCl crystal, NaCl crystal and the second filtrate；(3) the second filtrate is separated using methanol crystallization, KBr crystal is precipitated；(4) are dissolved by the oxide in filter residue and is settled out lead sulfate, obtains lead sulfate precipitation object and third filtrate for the first filter residue pickling processes using sulfuric acid；(5) calcium oxide is added into third filtrate to neutralize sulfuric acid, forms calcium sulfate and other metal precipitates；(6) sediment for obtaining step (6) is dehydrated, and sediment is prepared into the granular soil containing middle and trace element using pelletizer.This method can be recycled the ingredients such as sodium, potassium, bromine, lead in head ash, at the same can by head ash sediment and calcium sulfate be prepared by mixing into the granular soil of middle and trace element.
Description
Technical field
The present invention relates to chemical fields, and in particular to a method of processing head ash.
Background technique
Sintering machine head end ash is one of iron and steel enterprise's primary pollution source head, and sintering machine head end ash bulk deposition not only causes environment dirty
Dye, also seriously affects the normal production of blast furnace, be easy to cause dross in State of Blast Furnace, blast furnace ignition difficulty, blast furnace staying to stop production big
The problems such as repairing with equipment safety hidden danger.
It is usually contained in head ash and accounts for the KCl of its total weight 60-75%, accounts for the NaCl of total weight 5-10% and account for total weight
In addition the KBr of 2-3% also contains Fe, Ca, Cu, Al, Zn, the elements such as Mg, Pb, wherein microelement Mg, Cu, Ca, Fe etc. is to plant
Object essential component is suitable as compound fertilizer's additive.
" by the method for potassium ion idetified separation galvanized iron " proposed in patent CN108251650A is by head ash and chlorination
Potassium and the reaction of sodium chloride mixed liquor, under certain temperature, certain pH value, reaction a period of time be separated by solid-liquid separation to obtain lead and
Iron；" a kind of processing method of sintering machine head end ash " provided in patent CN201611053223.X, is to mix head ash with water
It sizes mixing, using links such as gravity separation, low intensity magnetic separation, closed circuit flotation, obtains iron ore concentrate and non-ferrous metal enriched substance；Patent
A kind of " the utilization method of sintering machine head end ash " provided in CN201410248826.X is that sintering machine head end ash is passed through haul, cloth
Material, water atomization spray, are made mini-pellets for sintering machine head end ash, the raw material as sintering uses；The above research focus primarily upon lead,
The recycling of iron, non-ferrous metal etc., but the resource utilization of the ingredients such as collection multiple element sodium, potassium, bromine, lead and head ash are used as
Granular soil is seldom using the research being integrated.
In view of the national conditions of China's high grade iron ore and potassium resource scarcity, General Office is carried out to sintering machine head end dedusting ash
Reason, realization are turned waste into wealth, and can not only promote the level that recycles of resource, and to the sustainable development for realizing metallurgical industry production
Exhibition strategy has important practical significance and real value.
Summary of the invention
In view of the problems of the existing technology and insufficient, the present invention provides a kind of method for handling head ash, this method letter
It is single, the ingredients such as sodium, potassium, bromine, the lead in head ash can be recycled, while can be by the insoluble precipitating in head ash using high speed granulator
Object and calcium sulfide are prepared by mixing into the granular soil of middle and trace element, save the cost of material of granular soil, and without maintenance.
The present invention provides a kind of method for handling head ash, and specific steps include:
(1) head ash is mixed according to certain solid-to-liquid ratio and is put into mixed dissolution in mixed slurry machine and filters, obtain the
One filtrate and the first filter residue；
(2) pH value for adjusting the first filtrate carries out Crystallization Separation processing to neutrality, respectively obtains KCl crystal, NaCl
Crystal and the second filtrate；
(3) excessive alcohols is added into the second filtrate, Crystallization Separation goes out KBr crystal；
(4) pickling processes are carried out to the first filter residue using excessive sulfuric acid, dissolves metal oxide and precipitating in filter residue
Lead sulfate out, filtration washing obtain lead sulfate precipitation object and third filtrate；
(5) excessive calcium oxide is added into third filtrate to neutralize sulfuric acid, adds calcium oxide until in third filtrate no longer
Until generating precipitating, calcium sulfate and other metal precipitates are eventually formed；
(6) sediment for obtaining step (5) is dehydrated, and sediment is prepared into containing middle and trace element using pelletizer
Granular soil, without maintenance.
Further, washing process condition are as follows: head ash solid-to-liquid ratio is 1g:(30-100) ml, the mixed dissolution time is 5-
16min, mixing speed 300-600r/min.
Further, the first filtrate is neutralized with hydrochloric acid to pH=7 in benefit.
Further, alcohols is methanol or ethyl alcohol.
Further, other metal precipitates include magnesium hydroxide, Kocide SD, iron hydroxide, zinc hydroxide etc..
Further, the revolving speed of pelletizer is 2000-4000r/min, time 5-15min.
Compared with prior art, the invention has the benefit that in the processing method of head ash of the invention, using mixing
Washing obtains the first filtrate and the first filter residue, and the first filtrate isolates the recyclable benefit of KCl crystal, NaCl crystal by crystallization treatment
With the KBr crystal also recoverable for utilizing separating methanol to go out；First filter residue isolates sulfuric acid through the pickling processes of persulfuric acid
Lead, resourcebility utilize；Excessive oxidation calcium is added in third filtrate, generates calcium sulfate and zinc hydroxide, magnesium hydroxide, hydroxide
The sediments such as iron, Kocide SD are prepared into the granular soil containing middle and trace element by granulation, can directly substitute normal soil
For planting, the cost of material of granular soil is saved.
Specific embodiment
Below in conjunction with specific embodiment, clear, complete description is carried out to technical solution of the present invention, it is clear that retouched
The embodiment stated is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, originally
Field those skilled in the art all other embodiment obtained without making creative work belongs to this
The protection scope of invention.
The present invention provides a kind of method for handling head ash, specifically includes the following steps:
(1) head ash is mixed according to certain solid-to-liquid ratio and is put into mixed dissolution in mixed slurry machine and filters, obtain the
One filtrate and the first filter residue.It containing accounting for KCl that its total weight is 60-75%, accounting for total weight is 5-10% in specific head ash
NaCl, account for the KBr that total weight is 2-3%, by the way that head ash washing process and filter, can make potassium therein, sodium,
Bromine is converted into ionic species and enters in the first filtrate, other valuable metals stay in slag phase, first point of realization potassium, sodium, bromo element
From.
(2) it adjusts the first filtrate pH value and carries out Crystallization Separation processing to neutrality, it is brilliant to respectively obtain KCl crystal, NaCl
Body and the second filtrate.According to a particular embodiment of the invention, it can use hydrochloric acid and neutralize the first filtrate to pH=7, and then pass through
First filtrate is subjected to Crystallization Separation processing, respectively obtains KCl crystal, NaCl crystal.
(3) excessive methanol is added into the second filtrate until KBr no longer is precipitated, Crystallization Separation goes out KBr crystal.
KBr does not dissolve in alcohols, and alcohols is the stronger organic solvent of polarity, can be miscible with water in any proportion, and methanol can be from aqueous solution
Middle Crystallization Separation goes out KBr.
(4) pickling processes are carried out to the first filter residue using excessive sulfuric acid, dissolves metal oxide and precipitating in filter residue
Lead sulfate out, filtration washing obtain lead sulfate precipitation object and third filtrate.Specifically, by the way that the first filter residue is carried out at acidleach
The dissolution of the oxides such as amounts of insoluble iron, zinc, copper, magnesium in the first filter residue can be entered solution by reason, while it is insoluble to be converted into lead
Property lead sulfate precipitation, is obtained by filtration third filtrate, to realize the separation of iron, magnesium, copper etc. with lead；
(5) excessive calcium oxide is added into third filtrate to neutralize sulfuric acid, adds calcium oxide until in third filtrate no longer
Until generating precipitating, calcium sulfate and other metal precipitates are finally formed in third filtrate, specifically, excessive calcium oxide one
On the other hand aspect can make the second filtrate made alkaline with neutralisation of sulphuric acid, hydroxide is generated in conjunction with magnesium, copper, iron plasma
The sediments such as magnesium, Kocide SD, iron hydroxide, zinc hydroxide.
(6) sediment for obtaining step (5) is dehydrated, and sediment is prepared into containing middle and trace element using pelletizer
Granular soil, without maintenance.Specifically, sediment includes calcium sulfate, magnesium hydroxide, Kocide SD, iron hydroxide etc., these are heavy
Starch contains to elements such as magnesium, calcium necessary to plant growth, copper, iron, zinc, prepares granular soil using head ash, saves former
Expect cost.
Further, washing process condition are as follows: head ash solid-to-liquid ratio is 1g:(30-100) ml, the mixed dissolution time is 5-
16min, mixing speed 300-600r/min.
Further, the revolving speed of pelletizer is 2000-4000r/min, time 5-15min.
Specifically, pelletizer is one of granulating disc, sugar coating machine, high speed granulator, preferably high speed granulator.
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 1
Table one is head ash sample composition/wt%
| Ingredient | KCl | NaCl | KBr | CaO | Fe2O3 | MgO | PbO | ZnO | Al2O3 | CuO |
| Content | 60 | 5.5 | 2.3 | 6.72 | 12.9 | 2.57 | 4.23 | 0.71 | 2.75 | 2.32 |
Processing head is grey according to the following steps:
(1) head ash is put into progress mixed dissolution 16min in mixed slurry machine, stirring speed according to solid-to-liquid ratio 1g:30ml
Degree is 300r/min, obtains the first filtrate and the first filter residue；
(2) pH value=7 for adjusting the first filtrate using hydrochloric acid are to carry out Crystallization Separation processing, respectively obtain KCl crystal,
NaCl crystal and the second filtrate；
(3) excessive methanol is added into the second filtrate until KBr no longer is precipitated, Crystallization Separation goes out KBr crystal；
(4) pickling processes are carried out to the first filter residue using excessive dilute sulfuric acid, dissolve the metal oxide in filter residue and sunk
Form sediment lead sulfate out, and filtration washing obtains lead sulfate precipitation object and third filtrate；
(5) excessive calcium oxide is added into third filtrate to neutralize sulfuric acid, until no longer generating precipitating in third filtrate
Until, form calcium sulfate and Kocide SD, iron hydroxide, magnesium hydroxide, zinc hydroxide precipitation object；
(6) sediment for obtaining step (5) is dehydrated, and obtains the mixture of a variety of precipitatings.Using high speed granulator, turning
Speed is 2000r/min, and the time to be prepared into the granular soil containing middle and trace element under conditions of 15min, is not necessarily to maintenance.
The granular soil for taking 400mL embodiment 1 to prepare is layered in 500mL flowerpot, and garlic is inserted in granular soil, is added
150mL water observes and records garlic bolt growing state.
Embodiment 2
Table two is head ash sample composition/wt%
| Ingredient | KCl | NaCl | KBr | CaO | Fe2O3 | MgO | PbO | ZnO | Al2O3 | CuO |
| Content | 67.2 | 7.34 | 2.21 | 6.31 | 8.9 | 2.32 | 3.11 | 0.38 | 1.28 | 0.95 |
Processing head is grey according to the following steps:
(1) head ash is put into progress mixed dissolution 16min in mixed slurry machine, stirring speed according to solid-to-liquid ratio 1g:50ml
Degree is 400r/min, obtains the first filtrate and the first filter residue；
(2) pH=7 for adjusting the first filtrate using hydrochloric acid is to carry out Crystallization Separation processing, respectively obtain KCl crystal,
NaCl crystal and the second filtrate；
(3) excessive methanol is added into the second filtrate until KBr crystal no longer is precipitated, Crystallization Separation goes out KBr crystalline substance
Body；
(4) pickling processes are carried out to the first filter residue using excessive sulfuric acid, dissolves metal oxide and precipitating in filter residue
Lead sulfate out, filtration washing obtain lead sulfate precipitation object and third filtrate；
(5) excessive calcium oxide is added into third filtrate to neutralize sulfuric acid, adds calcium oxide until in third filtrate no longer
Until generating precipitating, the sediments such as calcium sulfate and Kocide SD, iron hydroxide, magnesium hydroxide, zinc hydroxide are formed；
(6) sediment for obtaining step (5) is dehydrated, and obtains the mixture of a variety of precipitatings.Using high speed granulator, turning
Speed is 2500r/min, and the time to be prepared into the granular soil containing middle and trace element under conditions of 12min, is not necessarily to maintenance.
The granular soil for taking 400mL embodiment 2 to prepare is layered in 500mL flowerpot, and garlic is inserted in granular soil, is added
150mL water observes and records garlic bolt growing state.
Embodiment 3
Table three is head ash sample composition/wt%
| Ingredient | KCl | NaCl | KBr | CaO | Fe2O3 | MgO | PbO | ZnO | Al2O3 | CuO |
| Content | 73.1 | 6.1 | 2.64 | 3.2 | 7.47 | 1.28 | 2.78 | 0.41 | 1.36 | 1.66 |
Processing head is grey according to the following steps:
(1) head ash is put into progress mixed dissolution 8min, mixing speed in mixed slurry machine according to solid-to-liquid ratio 1g:80ml
For 500r/min, the first filtrate and the first filter residue are obtained；
(2) pH=7 for adjusting the first filtrate using hydrochloric acid is to carry out Crystallization Separation processing, respectively obtain KCl crystal,
NaCl crystal and the second filtrate；
(3) excessive methanol is added into the second filtrate until KBr crystal no longer is precipitated, Crystallization Separation goes out KBr crystalline substance
Body；
(4) pickling processes are carried out to the first filter residue using excessive sulfuric acid, dissolves metal oxide and precipitating in filter residue
Lead sulfate out, filtration washing obtain lead sulfate precipitation object and third filtrate；
(5) excessive calcium oxide is added into third filtrate to neutralize sulfuric acid, adds calcium oxide until in third filtrate no longer
Until generating precipitating, the sediments such as calcium sulfate and Kocide SD, iron hydroxide, magnesium hydroxide, zinc hydroxide are formed；
(6) sediment for obtaining step (5) is dehydrated, and obtains the mixture of a variety of precipitatings.Using high speed granulator, turning
Speed is 3500r/min, and the time to be prepared into the granular soil containing middle and trace element under conditions of 7min, is not necessarily to maintenance.
The granular soil for taking 400mL embodiment 3 to prepare is layered in 500mL flowerpot, and garlic is inserted in granular soil, is added
150mL water observes and records garlic bolt growing state.
Embodiment 4
Table four is head ash sample composition/wt%
| Ingredient | KCl | NaCl | KBr | CaO | Fe2O3 | MgO | PbO | ZnO | Al2O3 | CuO |
| Content | 71.1 | 9.45 | 2.72 | 2.22 | 7.21 | 2.03 | 2.69 | 0.83 | 0.25 | 1.5 |
Processing head is grey according to the following steps:
(1) head ash is put into progress mixed dissolution 5min in mixed slurry machine, stirring speed according to solid-to-liquid ratio 1g:100ml
Degree is 600r/min, obtains the first filtrate and the first filter residue；
(2) PH=7 for adjusting the first filtrate using hydrochloric acid is to carry out Crystallization Separation processing, respectively obtain KCl crystal,
NaCl crystal and the second filtrate；
(3) excessive methanol is added into the second filtrate until KBr crystal no longer is precipitated, Crystallization Separation goes out KBr crystalline substance
Body；
(4) pickling processes are carried out to the first filter residue using excessive sulfuric acid, dissolves metal oxide and precipitating in filter residue
Lead sulfate out, filtration washing obtain lead sulfate precipitation object and third filtrate；
(5) excessive calcium oxide is added into third filtrate to neutralize sulfuric acid, adds calcium oxide until in third filtrate no longer
Until generating precipitating, the sediments such as calcium sulfate and Kocide SD, iron hydroxide, magnesium hydroxide, zinc hydroxide are formed；
(6) sediment for obtaining step (5) is dehydrated, and obtains the mixture of a variety of precipitatings.Using high speed granulator, turning
Speed is 4000r/min, and the time to be prepared into the granular soil containing middle and trace element under conditions of 5min, is not necessarily to maintenance.
The granular soil for taking 400mL embodiment 4 to prepare is layered in 500mL flowerpot, and garlic is inserted in granular soil, is added
150mL water observes and records garlic bolt growing state.
Comparative example 1
It takes 400mL soil to be layered in 500mL flowerpot, garlic is inserted in the soil, 150mL water is added, in identical environment
Under observe and record garlic bolt growing state.
The plant height situation after the garlic bolt in embodiment 1-4 and comparative example 1 is cultivated 15 days is observed, as a result as shown in Table 5.
Five plant height test result of table
| Group | Plant plant height/cm |
| Embodiment 1 | 21.2 |
| Embodiment 2 | 20.7 |
| Embodiment 3 | 19.6 |
| Embodiment 4 | 23.1 |
| Comparative example 1 | 17.3 |
As shown in Table 5, garlic bolt is planted using granular soil obtained in each embodiment, compared with soil plantation, due to
Containing ferro element, magnesium elements, copper, calcium constituent necessary to plant growth etc. in granular soil, vegetation growth state is preferable,
Further illustrate that granular soil produced by the present invention can be used as cultivation matrix substitution soil plantation crops.
The present invention is further described by specific embodiment above, it should be understood that, here specifically
Description, should not be construed as the restriction for the essence of the present invention with range, and one of ordinary skilled in the art is reading this explanation
The various modifications made after book to above-described embodiment belong to the range that the present invention is protected.
Claims (6)
1. a kind of method for handling head ash, which is characterized in that specific method includes the following steps:
(1) head ash is mixed according to certain solid-to-liquid ratio and is put into mixed dissolution in mixed slurry machine and filters, obtain the first filter
Liquid and the first filter residue；
(2) pH value for adjusting the first filtrate carries out Crystallization Separation processing to neutrality, respectively obtains KCl crystal, NaCl crystal
With the second filtrate；
(3) excessive alcohols is added into the second filtrate until KBr crystal no longer is precipitated, Crystallization Separation goes out KBr crystal；
(4) pickling processes are carried out to the first filter residue using excessive sulfuric acid, dissolve the metal oxide in filter residue and is settled out sulphur
Lead plumbate, filtration washing obtain lead sulfate precipitation object and third filtrate；
(5) be added into third filtrate excessive calcium oxide until no longer generate precipitating until, eventually form calcium sulfate and other
Metal precipitates；
(6) sediment for obtaining step (5) is dehydrated, and sediment is prepared into the particle containing middle and trace element using pelletizer
Soil, without maintenance.
2. the method according to claim 1, wherein in step (1), washing process condition are as follows: the head ash
Solid-to-liquid ratio is 1g:(30-100) ml, the mixed dissolution time is 5-16min, mixing speed 300-600r/min.
3. the method according to claim 1, wherein first filtrate is neutralized with hydrochloric acid extremely in benefit in step (2)
PH=7.
4. the method according to claim 1, wherein the alcohols is methanol or ethyl alcohol in step (3).
5. the method according to claim 1, wherein other described metal precipitates include hydrogen in step (5)
Magnesia, Kocide SD, iron hydroxide, zinc hydroxide.
6. the method according to claim 1, wherein the revolving speed of the pelletizer is 2000- in step (6)
4000r/min, time 5-15min.
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| CN201910238226.8A CN110042243A (en) | 2019-03-27 | 2019-03-27 | A method of processing head ash |
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| CN201910238226.8A CN110042243A (en) | 2019-03-27 | 2019-03-27 | A method of processing head ash |
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| CN110042243A true CN110042243A (en) | 2019-07-23 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113247959A (en) * | 2021-06-09 | 2021-08-13 | 东北大学 | Method for preparing functional iron oxide nanoparticles by using machine head ash as raw material |
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Application publication date: 20190723 |