CN108585826A - The method for preparing magnesium aluminate spinel using Quadratic aluminum dust - Google Patents
The method for preparing magnesium aluminate spinel using Quadratic aluminum dust Download PDFInfo
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- CN108585826A CN108585826A CN201810472454.7A CN201810472454A CN108585826A CN 108585826 A CN108585826 A CN 108585826A CN 201810472454 A CN201810472454 A CN 201810472454A CN 108585826 A CN108585826 A CN 108585826A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
- C04B35/443—Magnesium aluminate spinel
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- Ceramic Engineering (AREA)
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- Inorganic Chemistry (AREA)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract
A method of magnesium aluminate spinel being prepared using Quadratic aluminum dust, is carried out according to the following steps:(1) prepare Quadratic aluminum dust as raw material;(2) 1~3h is calcined at 900~1200 DEG C, Quadratic aluminum dust fine powder material is made in ball milling after cooling;(3) Quadratic aluminum dust fine powder material is added to the water, at 50~98 DEG C of temperature and stirring condition, applies ultrasonic wave and carry out water logging;The ammonia that water logging generates is passed through reactive tank and generates ammonium chloride with hydrochloric acid;(4) leached mud is filtered to isolate, is mixed and finely ground with material containing magnesia after washing and drying;(5) it is pressed into pelletizing;(6) magnesium aluminate spinel is made using high temperature sintering or arc melting in pelletizing.The method reaction speed of the present invention is fast, so that nitrogen is converted into ammonia discharge and recycles, soluble impurity enters liquid phase, realizes further removal of impurities;Magnesium aluminate spinel purity height, the impurity content of preparation are few.
Description
Technical field
The invention belongs to material and environmental technology fields, more particularly to a kind of to prepare magnesium aluminate spinel using Quadratic aluminum dust
Method.
Background technology
Aluminium ash is the system of the slag that the generates product of gained after cooling in electrolytic aluminium, casting aluminium and secondary aluminium production process
Claim, main source is:(1) Molten Anodic is replaced, goes out the processes such as aluminium, electrolytic cell overhaul, generally produces 1 ton of electricity
It solves aluminium and generates 30~50kg aluminium ashes;(2) processes such as ingot casting, remelting, forging, machining during aluminum casting, average every 1 ton of aluminium
30~40kg aluminium ashes are generated from being worked into application process;(3) aluminium scrap regeneration and fabricated product again in secondary aluminium production process
The rate of recovery be about 75~85%, i.e. 1 ton of aluminium scrap generates about 150~250kg aluminium ashes.
Aluminium simple substance, the oxide of aluminium, the nitride of aluminium, fluoride salt, chlorate, other metals are generally mainly contained in aluminium ash
Oxide etc., according to its different respective content difference of source;In addition, as potroom aluminium ash may entrainment portions electrolyte
Ingredient, founding or refining process use aluminium ash to contain a certain amount of chloride and fluoride due to refining agent;There is part aluminium grey
Contain a certain amount of heavy metal;It therefore, can contaminated soil and underground water money if aluminium ash is directly accumulated without recovery processing
Source, aluminium ash is reacted with water to be generated the pollution such as ammonia, hydrogen and methane air, causes fire, and the impurity such as arsenic and aluminium arsenide are sent out with water
The arsine gas generated after raw reaction, not only pollutes air after being enriched in Workplace, can also cause Close contacts
Acute hydrogen arsenide poisoning;In June, 2016 Chinese Ministry of Environmental Protection, National Development and Reform Commission and the Ministry of Public Security joint publication new edition《National Hazard
Waste register》The middle aluminium ash that non-ferrous metal aluminum smelting technology is discharged is classified as toxicity risk waste and flammability hazard waste;Therefore, aluminium
Ash arrived non-process can not stage, urgency is extremely urgent.
More research is carried out to the recycling of aluminium ash both at home and abroad at present, generally carries out metallic aluminium in aluminium ash first
Recycling, the recovery process of metallic aluminium is roughly divided into heat treating process and gravity separation method, the electric separations such as the grey absorption method of stir-fry, rotary kiln facture
The cold-treating process two major classes such as method;Aluminium ash after recycling metallic aluminium is known as Quadratic aluminum dust, can be used for preparing nano aluminium oxide, oil
Black aluminium oxide, aluminium hydroxide, aluminum sulfate, aluminium polychloride, construction material, refractory material, steel-making additive etc..
Magnesium aluminate spinel as kiln brick or is poured due to the properties such as alkali resistance slag ability is strong under good thermal stability, high temperature
Material feeding is widely used in metallurgical industry kiln;Li Xiaona etc. is used to regenerate aluminium ash, alumine, fused magnesite, the iron of aluminium manufacturer
Bits and coke blacking are raw material, and the synthesizing aluminum-enriched magnesium aluminate spinel of high melt method is directly carried out without pretreatment, and (aluminium ash prepares magnesium
Aluminate and its in Al2O3-MgAl2O4Application in refractory material, Shanghai Communications University's Master's thesis, 2008);Zhong Xinyu
It is directly calcined at 1300~1500 DEG C Deng by industrial aluminum ash, then with magnesite land waste wet-milling, then adds polyethylene
Alcohol semi-dry pressing, preparing magnesium aluminate spinel in 1300~1500 DEG C of calcinings, (low-grade magnesite prepares magnalium with industrial aluminum ash
Spinelle, inorganic chemicals industry, 2012,44 (12), 32-35).
" method for preparing Antaciron and magnesium aluminate spinel using aluminium ash and forsterite " (CN 101429581) is by aluminium
Ash, forsterite and iron filings directly mix, using in aluminium ash metallic aluminium, aluminium nitride as reducing agent, high-temperature fusion restores
To Antaciron and magnesium aluminate spinel.
" a kind of fused magnesia-aluminum spinel composite fire-resistant material and its production method " (CN100450972) is by aluminium ash and carbonic acid
One or both of magnesium, magnesia mix, and are pressed into base, then electrically smelting is for magnesium aluminate spinel.
Process above aluminium ash is directly used without pretreatment, since aluminium ash self component is complicated, leads to impurity in product
Content is more, influences the performance and quality of final products.
" method of production electric melting magnesium aluminum spinel " (CN1919739A) utilizes processed aluminium ash and caustic-calcined magnesite electric smelting
Synthetic MgAl spinal, but the pretreatments such as its aluminium ash will be calcined, pickling, complex process, and need it that iron filings, carbon is added
Material is as reducing agent.And since the product of bringing into of impurity needs to carry out crushing-magnetic selection, technological process is long.
Invention content
For it is existing using aluminium ash as raw material prepare in magnesium aluminate spinel technique aluminium ash without pretreatment, need that addition is added
The problems such as agent, product impurity is more, poor performance, the present invention proposes a kind of method preparing magnesium aluminate spinel using Quadratic aluminum dust, with
Quadratic aluminum dust is raw material, and after denitrogenation pre-processes, high-quality magnesium aluminate spinel is prepared with magnesia material, realizes aluminium ash synthesis profit
With while reducing environmental pollution, obtaining that quality is high, magnesium aluminate spinel product of good economy performance.
The method of the present invention carries out according to the following steps:
1, prepare Quadratic aluminum dust as raw material;The Quadratic aluminum dust is the aluminium ash that is generated using fusion-casting process of aluminium ash through carrying
The Quadratic aluminum dust formed after aluminium, main component contain Al 0~10%, Al by mass percentage2O330~60%, AlN 5~
30%, MgO0~20%, remaining is impurity;
2, Quadratic aluminum dust at 900~1200 DEG C is calcined to 1~3h, be milled to grain size≤106 μm after being cooled to room temperature, be made
Quadratic aluminum dust fine powder material;
3, Quadratic aluminum dust fine powder material is added to the water, the solid-to-liquid ratio of Quadratic aluminum dust fine powder material and water is 40~200g/L;So
Afterwards at 50~98 DEG C of temperature and stirring condition, applies ultrasonic wave and carry out water logging, the aluminium nitride in Quadratic aluminum dust fine powder material is made to send out
Raw hydrolysis;The alkaline gas ammonia generated during water logging is discharged, and when alkaline gas no longer generates, water logging terminates to obtain
Obtain water logging material;
4, water logging material is filtered to isolate into leached mud, it is washed after drying remove moisture removal, then with material containing magnesia
It is mixed and finely ground to the mesh of granularity≤150, mixed powder is made;The molar ratio of aluminium oxide and magnesia is 1 in mixed powder:1;
5, mixed material is pressed into pelletizing, pressing pressure is 50~250MPa;
6, magnesium aluminate spinel is made using high temperature sintering or arc melting in pelletizing;The temperature of the high temperature sintering is
1600~1700 DEG C, the time is 2~4 hours;The time of the arc melting is 2~4 hours.
Above-mentioned material containing magnesia be light calcined magnesia, or for magnesium hydroxide calcining made of magnesia, grain size≤
106μm。
In the above method, the mixing speed of step 2 is 500~3000r/min, 20~200kHz of ultrasonic frequency.
Above-mentioned light calcined magnesia is made of calcining magnesite or shepardite, and above-mentioned magnesium hydroxide is to be with bischofite
Raw material is made.
In the above method, be connected to reaction system with reactive tank by pipeline liquid injecting device when water logging, be equipped in reactive tank
Hydrochloric acid;The alkaline gas ammonia that water logging generates is reacted with hydrochloric acid generates ammonium chloride.
Above-mentioned magnesium aluminate spinel contains Al by mass percentage2O370.3~71.5%, MgO 27.1~27.9%, volume
Density is 3.25~3.42g/cm3。
The method of the present invention has following characteristics:
(1) remaining pure aluminum in Quadratic aluminum dust is efficiently converted into aluminium oxide by calcining, passes through heating stirring ultrasound
Water logging can make the progress fast hydrolyzing of the aluminium nitride in aluminium ash be converted into aluminium hydroxide, and reaction speed is fast, while making in aluminium ash
Nitrogen is converted into ammonia discharge and generates ammonium chloride realization recycling with hydrochloric acid, and the soluble impurity in aluminium ash is made to enter liquid phase, real
Further removal of impurities in existing Quadratic aluminum dust;
(2) object phase more stable uniform in the leached mud obtained after being pre-processed by Quadratic aluminum dust, impurity is few, and aluminium oxide contains
Amount is high;The magnesium aluminate spinel purity that is prepared using the leached mud as raw material is high, impurity content is few.
Description of the drawings
Fig. 1 is the method and process flow chart that magnesium aluminate spinel is prepared using Quadratic aluminum dust in the embodiment of the present invention;
Fig. 2 is the XRD diagram of the magnesium aluminate spinel in the embodiment of the present invention 1.
Specific implementation mode
It carries out being connected to reaction system with reactive tank by pipeline liquid injecting device when water logging in the embodiment of the present invention, reactive tank is built-in
There is the hydrochloric acid of mass concentration 10~20%;The alkaline gas ammonia that water logging generates is reacted with hydrochloric acid generates ammonium chloride.
Detect whether that ammonia generation is utilized in wire type ammonia detector and carries out on-line checking in the embodiment of the present invention.
Light calcined magnesia in the embodiment of the present invention is made of calcining magnesite or shepardite, purity >=95%, hydroxide
Magnesium is made of purity >=95% using bischofite as raw material.
Weight percent≤10% of the impurity of Quadratic aluminum dust used in the embodiment of the present invention.
With reference to specific embodiment the present invention is further elaborated explanation, the scope of the present invention is not limited to institute
State content.
Embodiment 1
Flow is as shown in Figure 1;
Prepare Quadratic aluminum dust as raw material;The Quadratic aluminum dust be aluminium ash carried using fusion-casting process formed after aluminium it is secondary
Aluminium ash, main component contain Al 6%, Al by mass percentage2O359.5%, AlN 26%, MgO 6%, impurity 3.5%;
Quadratic aluminum dust is calcined into 2h at 1000 DEG C, grain size≤106 μm is milled to after being cooled to room temperature, it is thin that Quadratic aluminum dust is made
Powder;
Quadratic aluminum dust fine powder material is added to the water, the solid-to-liquid ratio of Quadratic aluminum dust fine powder material and water is 100g/L;Then in temperature
Under 90 DEG C of degree and stirring condition, apply ultrasonic wave and carry out water logging, makes the aluminium nitride in Quadratic aluminum dust fine powder material that hydrolysis occur;
The alkaline gas ammonia generated during water logging is discharged, and when alkaline gas no longer generates, water logging terminates to obtain water logging material;
Wherein mixing speed is 700r/min, ultrasonic frequency 50kHz;
Water logging material is filtered to isolate into leached mud, is dried after washed and removes moisture removal, it is then light with grain size≤106 μm
Burned magnesium oxide is mixed and finely ground to the mesh of granularity≤150, and mixed powder is made;The molar ratio of aluminium oxide and magnesia in mixed powder
It is 1:1;
Mixed material is pressed into pelletizing, pressing pressure 200MPa;
Magnesium aluminate spinel is made using high temperature sintering in pelletizing;The temperature of high temperature sintering is 1600 DEG C, and the time is 2 hours;
Magnesium aluminate spinel contains Al by mass percentage2O370.5%, MgO 27.6%, bulk density 3.25g/cm3;
XRD testing results are as shown in Figure 2.
Embodiment 2
With embodiment 1, difference is method:
(1) Quadratic aluminum dust, main component contain Al 10%, Al by mass percentage2O360%, AlN 22%, MgO 6%,
Impurity 2%;
(2) mixing speed is 800r/min, ultrasonic frequency 100kHz when water logging;After leached mud washing and drying with hydroxide
Magnesia (grain size≤106 μm) is mixed and finely ground made of magnesium calcining;
(3) temperature of high temperature sintering is 1700 DEG C, and the time is 4 hours;
Magnesium aluminate spinel contains Al by mass percentage2O370.3%, MgO 27.9%, bulk density 3.29g/cm3。
Embodiment 3
With embodiment 1, difference is method:
(1) Quadratic aluminum dust, main component contain Al by mass percentage2O355%, AlN 12%, MgO 20%, impurity
3%;
(2) magnesium aluminate spinel is made using arc melting (temperature is more than 1700 DEG C) in pelletizing;Arc melting when
Between be 2 hours;
Magnesium aluminate spinel contains Al by mass percentage2O371.5%, MgO 27.1%, bulk density 3.42g/cm3。
Embodiment 4
With embodiment 1, difference is method:
(1) Quadratic aluminum dust, main component contain Al 10%, Al by mass percentage2O330%, AlN 30%, MgO
20%, impurity 10%;
(2) 3h is calcined at 900 DEG C;
(3) solid-to-liquid ratio of Quadratic aluminum dust fine powder material and water is 40g/L;Under temperature 50 C and stirring condition, apply ultrasound
Wave carries out water logging, mixing speed 3000r/min, ultrasonic frequency 20kHz;
(4) briquetting pressure is 250MPa;
(5) temperature of high temperature sintering is 1650 DEG C, and the time is 3 hours;
Magnesium aluminate spinel contains Al by mass percentage2O371.2%, MgO 27.5%, bulk density 3.33g/cm3。
Embodiment 5
With embodiment 1, difference is method:
(1) Quadratic aluminum dust, main component contain Al 10%, Al by mass percentage2O345%, AlN 25%, MgO
18%, impurity 2%;
(2) 1h is calcined at 1200 DEG C;
(3) solid-to-liquid ratio of Quadratic aluminum dust fine powder material and water is 200g/L;At 98 DEG C of temperature and stirring condition, apply ultrasound
Wave carries out water logging, mixing speed 500r/min, ultrasonic frequency 200kHz;
(4) briquetting pressure is 50MPa;
(5) magnesium aluminate spinel is made using arc melting in pelletizing, the time is 4 hours;
Magnesium aluminate spinel contains Al by mass percentage2O370.9%, MgO 27.4%, bulk density 3.38g/cm3。
Claims (4)
1. a kind of method preparing magnesium aluminate spinel using Quadratic aluminum dust, it is characterised in that carry out according to the following steps:
(1) prepare Quadratic aluminum dust as raw material;The Quadratic aluminum dust is the aluminium ash that is generated using fusion-casting process of aluminium ash through carrying aluminium
The Quadratic aluminum dust formed afterwards, main component contain Al 0~10%, Al by mass percentage2O330~60%, AlN 5~30%,
MgO0~20%, remaining is impurity;
(2) Quadratic aluminum dust is calcined to 1~3h at 900~1200 DEG C, grain size≤106 μm is milled to after being cooled to room temperature, is made two
Secondary aluminium ash fine powder material;
(3) Quadratic aluminum dust fine powder material is added to the water, the solid-to-liquid ratio of Quadratic aluminum dust fine powder material and water is 40~200g/L;Then exist
At 50~98 DEG C of temperature and stirring condition, apply ultrasonic wave and carry out water logging, makes the aluminium nitride in Quadratic aluminum dust fine powder material that water occur
Solution reaction;The alkaline gas ammonia generated during water logging is discharged, and when alkaline gas no longer generates, water logging terminates to obtain water
Soak material;It wherein carries out being connected to reaction system with reactive tank by pipeline liquid injecting device when water logging, hydrochloric acid is housed in reactive tank;Water logging
The alkaline gas ammonia of generation is reacted with hydrochloric acid generates ammonium chloride;
(4) water logging material is filtered to isolate into leached mud, is dried after washed and remove moisture removal, is then mixed with material containing magnesia
It is levigate to the mesh of granularity≤150, mixed powder is made;The molar ratio of aluminium oxide and magnesia is 1 in mixed powder:1;
(5) mixed material is pressed into pelletizing, pressing pressure is 50~250MPa;
(6) magnesium aluminate spinel is made using high temperature sintering or arc melting in pelletizing;The temperature of the high temperature sintering is
1600~1700 DEG C, the time is 2~4 hours;The time of the arc melting is 2~4 hours.
2. the method according to claim 1 for preparing magnesium aluminate spinel using Quadratic aluminum dust, it is characterised in that described contains
Magnesia material is light calcined magnesia, or is magnesia, grain size≤106 μm made of magnesium hydroxide calcining.
3. the method according to claim 1 for preparing magnesium aluminate spinel using Quadratic aluminum dust, it is characterised in that step (2)
Mixing speed is 500~3000r/min, 20~200kHz of ultrasonic frequency.
4. the method according to claim 1 for preparing magnesium aluminate spinel using Quadratic aluminum dust, it is characterised in that the magnesium
Aluminate contains Al by mass percentage2O370.3~71.5%, MgO 27.1~27.9%, bulk density be 3.25~
3.42g/cm3。
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CN109052445A (en) * | 2018-10-24 | 2018-12-21 | 中南大学 | A kind of method of Quadratic aluminum dust innoxious use |
CN111170750A (en) * | 2020-01-22 | 2020-05-19 | 北京矿冶科技集团有限公司 | Method for producing refractory material by innocent treatment of secondary aluminum ash |
CN111233356A (en) * | 2020-03-10 | 2020-06-05 | 山东大学 | Method and system for preparing sulphoaluminate cement from all solid waste of aluminum ash pretreatment |
CN111807829A (en) * | 2020-07-15 | 2020-10-23 | 沈阳北冶冶金科技有限公司 | Method for preparing magnesia-alumina spinel by using aluminum ash and bischofite |
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