CN108147379A - A kind of flyash acid dissolution slag prepares the method for matching grand powder - Google Patents
A kind of flyash acid dissolution slag prepares the method for matching grand powder Download PDFInfo
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0602—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with two or more other elements chosen from metals, silicon or boron
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Abstract
The method for matching grand powder is prepared the present invention provides a kind of flyash acid dissolution slag, residue, carbon dust and brown iron oxide after raw material selection fluidization bed fly ash acid is molten regulate and control C/Si molar ratios and Fe2O3Content, and pass through mechanical lapping and be uniformly mixed, 3~6h is kept the temperature in 1300~1500 DEG C under high temperature and flowing nitrogen atmosphere, room temperature is cooled to the furnace later, obtains matching grand powder.In the present invention, utilize the original composition of residue and high activity and the autocatalysis of iron after the molten extraction aluminium oxide of fluidization bed fly ash acid, Sialon powders are made at a lower temperature, it is effectively utilized wherein silicon, aluminium and carbonaceous components, the dosage of external carbon is significantly reduced, improves preparation efficiency, is this siliceous residue of high-carbon for being difficult to directly utilize in building materials of flyash acid dissolution slag, it is able to expand in terms of high value added product using new way, realizes flyash acid dissolution slag recycling.
Description
Technical field
The present invention be directed to after aluminous fly-ash acidity extraction aluminium oxide high silicon aluminum carbon waste residue carry out deep processing and utilization,
The technology belongs to solid waste resource recovery field using the flyash acid dissolution slag high activity of itself and silicon aluminum carbon component.
Background technology
From the perspective of from conventional angle, flyash is the solid waste generated after coal combustion, and wide with flyash in recent years
General development and application have become a kind of new resource.Flyash is SiO due to its key component2、Al2O3Deng being applied first
In the traditional construction materials industry such as cement, brick and tile product and concrete, such product inclusiveness is strong, dosage is big, added value is low, is always
Consume the Main way of flyash.In the coal-fired flyash formed in the coalfields such as the Ordos Basin the northern fringe of China, Al2O3
Content can be up to 40-50wt%[1], utilized as new bauxite resource, become the exploitation hot spot of nearly more than ten years, and obtained
Obtain remarkable effect[2-4].At present, the method for aluminous fly-ash extraction aluminium oxide is mainly limestone sintering process, soda lime burning
Connection, acid extracting etc.[5,6], the level of residue wherein generated after acidity extraction aluminium oxide is minimum, but extracts one ton of aluminium oxide, can still produce
Raw about 1.5 tons of residues.Since acid technological process industrialization is few, the research on utilization about this kind of residue is actually rare.
Fluidization bed fly ash is coal-fired combustion product at a lower temperature, and the master of aluminous fly-ash is produced in Inner Mongol Erdos
Want object mutually for metakaolinite, thus can molten realization alumina extraction sour at a lower temperature, remaining residue is mainly amorphous
State SiO2、Al2O3, a small amount of Fe2O3And unburned carbon, and high carbon content also makes it be difficult to apply in building material industry in such slag.It should
Residue is that flyash experienced remaining solid phase components after the metal oxides such as aluminium largely dissolve out, and acid dissolution leads to silicate bone
Frame caves in, the increase of short texture, specific surface area, has higher chemical reactivity and rebuilds the item of new resistate phase
Part, thus, a kind of siliceous carbonaceous active raw material of new high activity can be become.
Sialon is the compound word of tetra- kinds of elements of Si, Al, O, N, can also regard Si as3N4Middle Si, N atom is former by Al and O
Son replaces the general name of formed a major class solid solution.Sialon ceramics excellent in mechanical performance and easily by chemical composition change into
Row control, is all widely used in fields such as oil, chemical industry, metallurgy, automobile, aerospace.Originally, Sialon ceramics prepares raw material
Si for high-purity3N4, SiO2, Al2O3, AlN etc., but unquestionably so lead to the cost of Sialon ceramics product very
It is high, it is difficult to be generalized to daily necessities field, significantly limit the application development of Sialon ceramics.In recent years, research
Persons have inquired into more natural minerals (such as kaolinite[7,8], illite, montmorillonite[9], pyrophyllite, rice husk[10], coal, river
Sand[11], gangue[12]Deng) and industrial solid castoff (such as waste resistant material and clinker[13], aluminium ash[14,15]And flyash[15])
Substitution pure chemistry reagent is attempted to prepare sialon material, moreover, because uncertain impurity composition is deposited in natural mineral raw
Substantially reduce synthesis temperature.For example, Yoshiyuki Sugahara etc. are using montmorillonite polyacrylonitrile intercalated compound
Raw material carbon thermal reduction prepares β-sialon, it is said that having β-sialon mutually to occur at 1200 DEG C[9]。
For matching grand powder, raw material phosphorus content can cause highly significant for the object phase composition of product and chemical composition
Influence.J.E.Gilbert directly carries out experimental study using the flyash of high carbon content, and carbon silicon mol ratio is 3.54 or so,
β-sialon phases are successfully synthesized[16].The selection carbon silicon mol ratio such as A.A.Kudyba-Jansen is 2.29 using flyash as original
Material prepares β-sialon phases[17].The equal research of yellow army, in theory carbon silicon mol ratio 2:On the basis of 1, carbon it is excessive 10% when,
The amount of α-Sialon and β-Sialon all significantly reduce, while another object phase AlN occur, carbon it is excessive 50% and 100% when, do not have
Sialon occurs, and generates AlN and SiC[18].It can be seen that because of the difference of raw material and preparation temperature, the conclusion obtained may be
Totally different.Iron oxide is in Sialon powder preparation process, since fusing point is relatively low, the change valence effect of ferro element, to reaction
System can generate catalytic effect.
The achievement in research of forefathers confirms, can be prepared using solid waste such as silicoide, industrial silica fume, flyash
Go out Sialon, silicon carbide and beta-silicon nitride powder, siliceous, the aluminum component in all kinds of raw materials participate in reaction by activating, and C/Si
The regulation and control of ratio can take the mode of additional carbon dust to realize.Aluminous fly-ash acid dissolution slag is due to its own siliceous all amorphous of component
State silica, granularity is fine, and almost all is less than 10 μm, has higher reactivity, meanwhile, contain not in flyash
Combustion carbon is significantly enriched with after acid is dissolved except most of metal cation, and acid processing also has an impact the surface of carbon so that should
Raw material is after a small amount of carbon is added, it will be able to which satisfaction forms Sialon powder needs.It is in addition, remaining few in flyash acid dissolution slag
Iron oxide component is measured also in amorphous state, and main occupy-place is inside particle or loose lattice framework deep, this partial oxidation iron exist
Can be that reaction system generates autocatalytic effect under high temperature, therefore, method proposed by the present invention can efficiently utilize flyash acid
Prepared by molten slag matches grand powder new material.
Bibliography
[1] spy of aluminium in Yang Dianfan, Wei Cundi, Jiang Yinshan, Zhang Peiping Ordos Basin the northern fringe coal solid waste
Levy [J] Jilin University's journals (geoscience version), 2012,42 (3):827-831.
[2]A.Seidel,A.Sluszny,G.Shelef,Y.Zimmels.Self inhibition of aluminum
leaching from coal fly ash by sulfuric acid[J].Chemical Engineering Journal,
1999,72:195-207.
[3]Niva Nayak,Chitta R.Panda.Aluminium extraction and leaching
characteristics of Talcher Thermal Power Station fly ash with sulphuric acid
[J].Fuel,2010,89:53-58.
[4]WU Cheng-you,YU Hong-fa,ZHANG Hui-fang.Extraction of aluminum by
pressure ac-id-leaching method from coal fly ash[J].Transactions Nonferrous
Metals Society of Chi-na,2012,22:2282-2288.
[5] the few quasi- Ge Er Gangue Power Plants CFB ash features of south of Xu and comprehensive utilization [D] Changchun:Jilin University, 2009.
[6] Wu Yan extract research [D] the Shenyang of aluminium oxide and silica from flyash:Northeastern University, 2008.
[7]S.Wild.A Noval Route for The Production ofβ'-Sialon Powders[J]
.Journal of Materials Science[J].1976,11:1972-1974.
It is prepared by [8] β-Sialon powder synthesis and composite material of this of Malaysian based on kaolin/flyash mixed raw material
[D] Guilin:Guilin University of Technology, 2013.
[9]Yoshiyuki Sugahara,Kazuyuki Kuroda,Chuzo Kato.Synthesis ofβ-Sialon
from a Montmoril-lonite-Polyacrylonitrile Intercalation Compound by
Carbothermal Reduction[J].Communications of the American Ceramic Society,
1984,67(11):c247-c248.
[10]Varong Pavarajarn,Ruttairat Precharyutasin,and Piyasan
Praserthdam.Synthesis of Silicon Nitride Fibers by the Carbothermal Reduction
and Nitridation of Rice Husk Ash[J].J.Am.Ce-ram.Soc.,2010,93(4):973–979.
[11] Pan Wei, Huang Yue, Chen Jian prepare method [P] China of Sialon combined silicon carbide ceramic powder using river sand specially
Profit：ZL00105941.6,2003-03-05.
[12] Pan Wei, Cao Zhenzhu, Fang Minghao, Wang Ruigang, yellow bright China prepare beta-sialon silicon carbide complex phase with gangue
Method [P] Chinese patents of powder：ZL02103875.9,2004-06-09.
[13] method that Jin Congjin, Li Zeya prepare α/β-complex phase ' Sailong ' ceramic powder using waste resistant material and clinker
[P] Chinese patents：ZL200510111005.2,2008-12-03.
[14] Lee family's mirror prepares research [D] the Shanghai of Sialon materials using aluminium ash:Shanghai Communications University, 2012.
[15]Juntong Huang,Minghao Fang,Zhaohui Huang,et.al.Preparation,
Microstructure,and Me-chanical Properties of Spinel-Corundum-Sialon Composite
Materials from Waste Fly Ash and Aluminum Dross[J].Advances in Materials
Science and Engineering,2014,2014:10pages.
[16]J.E.Gilbert,A.Mosset.PREPARATION OFβ-SiAlON FROM FLY ASHES[J]
.Materials Research Bulletin,1998,33:117-123.
[17]A.A.Kudyba-Jansen,H.T.Hintzen,R.Metselaar.Ca-α/β-sialon ceramics
synthesised from fly ash-preparation,characterization and properties[J]
.Materials Research Bulle-tin,2001,36:1215–1230.
[18] Huang Juntong, Fang Minghao, Wang Xinying wait grinding for the low Al2O3 alumina carbothermal reduction-nitridation synthesis complex phase Sialon of
Study carefully [J] Rare Metals Materials and engineering, 2007,36 (Suppl.1):373-375.
Invention content
The present invention《A kind of flyash acid dissolution slag prepares the method for matching grand powder》, it is for the molten extraction of fluidization bed fly ash acid
The high activity silicon aluminum carbon slag obtained after aluminium oxide carries out carbon heat-nitridation reaction and prepares Sialon powders and carry out, specific steps
It is as follows：
(1) on the basis of the original silicon-carbon content of flyash acid dissolution slag, dose a small amount of carbon dust regulation and control C/Si molar ratios for 2.1~
3.3, adjust Fe2O3Content about 0.2~2wt%, the mixed powder of acquisition are further uniformly mixed by mechanical lapping, are obtained
Sialon powder materials；
(2) sample is placed in corundum porcelain boat, and moved into high temperature furnace, in flowing nitrogen (1~3L/min of flow velocity) atmosphere
Under in 1300~1500 DEG C keep the temperature 3~6h, cool to room temperature with the furnace later, obtain Sialon powders.
Flyash acid dissolution slag of the present invention be residue of the fluidization bed fly ash after hydrochloric acid or sulfuric acid solution, wherein SiO2
Content about 56~72wt%, Al2O3Content about 16~29wt%, Fe2O3Content about 0.15~0.42wt%, C content for 8~
13wt%；Nodeless mesh phase in flyash acid dissolution slag；About 2~8 μm of average grain diameter；Heretofore described additional carbon dust, Ke Yishi
The carbon black of common carbon dust of the purity more than 98wt% or filler rank；C/Si molar ratios are 2.1~3.3 in the present invention；
As Fe in raw material2O3When content is too low, the pure Fe of chemistry can be selected2O3Powder is as supplement；To raw material grinding, effect in the present invention
Fruit is to obtain original silicon aluminum carbon matter component in flyash acid dissolution slag to come into full contact with and evenly mix, mechanical masterpiece with dosing component
With higher surface energy is made it have, be conducive in lower temperature and realized in the short time preparation of Sialon powders.
Advantageous effect
In the present invention, the original composition SiO of residue after the molten extraction aluminium oxide of fluidization bed fly ash acid is utilized2、Al2O3、
Fe2O3With the chemical compositions such as C, and all amorphous high activities of each substance are utilized, Sialon powder is made at a lower temperature
Body is effectively utilized wherein silicon, aluminium and carbonaceous components, significantly reduces the dosage of external carbon, improve preparation efficiency, is fine coal
This high-carbon residue for being difficult to directly utilize in building materials of grey acid dissolution slag is able to the expansion in terms of high value added product and utilizes new way
Diameter.
Description of the drawings
Prepared by Fig. 1 flyash acid dissolution slag matches grand powder specific steps flow chart
The product X RD collection of illustrative plates of Fig. 2 difference C/Si molar ratios
Fig. 3 C/Si molar ratios are 2.89 product SEM photograph
Specific embodiment
Of the invention for ease of understanding, with reference to embodiment, the present invention is described in further detail.Art technology
Understanding is of the invention it will be clearly understood that the embodiment is only to aid in by personnel, is not construed as the concrete restriction to the present invention.Using this
The design of invention simply changes all in the scope of protection of present invention to what the present invention carried out.
The acid dissolution slag that Sialon powders use is prepared, is to originate from the fluid bed aluminous fly-ash of Erdos coal through persalt
Acid is molten to wash obtained residue, pH value 4.5 afterwards.SiO in the slag2Content about 56~72wt%, Al2O3Content about 16~
29wt%, Fe2O3Content about 0.15~0.42wt%, C content are 8~13wt%, and average grain diameter is 4.2 μm, and nodeless mesh object is mutually deposited
.
Embodiment 1：Weigh residue 10.0g after the molten aluminum-extracted pulverized fuel ash of hydrochloric acid acid, SiO in the slag2Content is 58.82wt%,
Al2O3Content is 27.05wt%, Fe2O3Content about 0.21wt%, C content 8.97wt%；Carbon content is weighed as 98.5wt%
Carbon dust 2.54g, and the two is mixed, C/Si molar ratios are 2.89 in mixture at this time.The powder of mixing is placed in ball grinder
The middle water for adding in 2 times of powder quality, weighs medium 100g 5mm and 50g 2mm zirconia grinding medias, continuous ball milling 2h, later
Isolated aqueous solid is taken out after 90 DEG C slowly drying, powdery is further ground into, moves into corundum porcelain boat, by porcelain boat
It is placed in GF17Q type atmosphere batch-type furnaces.Nitrogen first is passed through for 2L/min according to flow velocity, pre-aeration 1h excludes furnace chamber air；Later
250 DEG C are warming up to, then 900 DEG C are warming up to, then heat up with 5 DEG C/min with 10 DEG C/min heating rates with 100 DEG C/h heating rates
Rate is warming up to 1400 DEG C, and adjusting nitrogen flow rate is 2L/min；6h is kept the temperature at 1400 DEG C, cools to room temperature, sample with the furnace later
Remaining carbon dust is removed by 750 DEG C of air calcination 2h, obtains matching grand powder.Obtained product X RD analyses are as shown in Figure 1.It obtains
Product SEM figures it is as shown in Figure 2.
Embodiment 2：Weigh residue 10.0g after the molten aluminum-extracted pulverized fuel ash of hydrochloric acid acid, SiO in the slag2Content is 56.03wt%,
Al2O3Content is 29.26wt%, Fe2O3Content about 0.26wt%, C content 12.92wt%；It is 99wt%'s to weigh carbon content
N550 carbon black 1.072g, and the two is mixed, C/Si molar ratios are 2.10 in mixture at this time.The powder of mixing is placed in ball milling
The water of 2 times of powder quality is added in tank, weighs medium 100g 5mm and 50g 2mm zirconia grinding medias, continuous ball milling 2h, it
Isolated aqueous solid is taken out afterwards after 90 DEG C slowly drying, is further ground into powdery, is moved into corundum porcelain boat, by porcelain
Boat is placed in GF17Q type atmosphere batch-type furnaces.Nitrogen first is passed through for 2L/min according to flow velocity, pre-aeration 1h excludes furnace chamber air；It
250 DEG C are warming up to, then 900 DEG C are warming up to, then with 5 DEG C/min liters with 10 DEG C/min heating rates afterwards with 100 DEG C/h heating rates
Warm rate is warming up to 1350 DEG C, and adjusting nitrogen flow rate is 2L/min；6h is kept the temperature at 1350 DEG C, cools to room temperature, sample with the furnace later
Product remove remaining carbon dust by 750 DEG C of air calcination 2h, obtain matching grand powder.The XRD analysis of obtained product is as shown in Figure 1.
Embodiment 3：Weigh residue 10.0g after the molten aluminum-extracted pulverized fuel ash of hydrochloric acid acid, SiO in the slag2Content is 72.14wt%,
Al2O3Content is 16.13wt%, Fe2O3Content about 0.15wt%, C content 11.62wt%；Carbon content is weighed as 98.5wt%
Carbon dust 3.24g, Fe2O3Powder 0.250g, and three is mixed, C/Si molar ratios are 3.02, Fe in mixture at this time2O3Content
About 2wt%.The powder of mixing is placed in ball grinder to the water for adding in 2 times of powder quality, weighs medium 100g 5mm and 50g 2mm
Zirconia grinding media, continuous ball milling 2h take out isolated aqueous solid after 90 DEG C slowly drying, further grind later
Powdery is worn into, moves into corundum porcelain boat, porcelain boat is placed in GF17Q type atmosphere batch-type furnaces.First it is passed through according to flow velocity for 2L/min
Nitrogen, pre-aeration 1h exclude furnace chamber air；250 DEG C are warming up to, then heat up with 100 DEG C/h heating rates with 10 DEG C/min later
Rate is warming up to 900 DEG C, then is warming up to 1400 DEG C with 5 DEG C/min heating rates, and adjusting nitrogen flow rate is 2L/min；At 1400 DEG C
3h is kept the temperature, cools to room temperature with the furnace later, sample removes remaining carbon dust by 750 DEG C of air calcination 2h, obtains matching grand powder.
The XRD analysis of the product arrived is as shown in Figure 1.
Embodiment 4：Weigh residue 10.0g after sulfuric acid solution aluminum-extracted pulverized fuel ash, SiO in the slag2Content is 61.63wt%,
Al2O3Content is 25.26wt%, Fe2O3Content about 0.42wt%, C content 8.11wt%；Carbon content is weighed as 98.5wt%
Carbon dust 3.31g, and the two is mixed, C/Si molar ratios are 3.30 in mixture at this time.The powder of mixing is placed in ball grinder
The middle water for adding in 2 times of powder quality, weighs medium 100g 5mm and 50g 2mm zirconia grinding medias, continuous ball milling 2h, later
Isolated aqueous solid is taken out after 90 DEG C slowly drying, powdery is further ground into, moves into corundum porcelain boat, by porcelain boat
It is placed in GF17Q type atmosphere batch-type furnaces.Nitrogen first is passed through for 2L/min according to flow velocity, pre-aeration 1h excludes furnace chamber air；Later
250 DEG C are warming up to, then 900 DEG C are warming up to, then heat up with 5 DEG C/min with 10 DEG C/min heating rates with 100 DEG C/h heating rates
Rate is warming up to 1480 DEG C, and adjusting nitrogen flow rate is 2L/min；3h is kept the temperature at 1480 DEG C, cools to room temperature, sample with the furnace later
Remaining carbon dust is removed by 750 DEG C of air calcination 2h, obtains matching grand powder.The XRD analysis of obtained product is as shown in Figure 1.
Claims (3)
1. a kind of flyash acid dissolution slag prepares the method for matching grand powder, which is characterized in that extracts oxygen with fluid bed aluminous fly-ash
It is raw material to change the high activity silicon aluminum carbon slag after aluminium, by carbon heat-nitridation reaction and what is carried out, is as follows：
A. on the basis of the original silicon of flyash acid dissolution slag and carbon content, dose a small amount of carbon dust, regulation and control C/Si molar ratios for 2.1~
3.3, Fe2O3 content about 0.2~2wt% are adjusted, the mixed powder of acquisition is further uniformly mixed by mechanical lapping, obtains powder
Body raw material；
B. sample is placed in corundum porcelain boat, and moved into high temperature furnace, under flowing nitrogen (1~3L/min of flow velocity) atmosphere in
1300~1500 DEG C of 3~6h of heat preservation, cool to room temperature with the furnace, obtain matching grand powder later.
2. a kind of flyash acid dissolution slag according to claim 1 prepares the method for matching grand powder, wherein the flyash is sour
Molten slag be residue of the fluidization bed fly ash after hydrochloric acid or sulfuric acid solution, wherein SiO2 contents about 56~72wt%, Al2O3 contents
About 16~29wt%, Fe2O3 content about 0.15~0.42wt%, C content are 8~13wt%；Nodeless mesh in flyash acid dissolution slag
Phase；About 2~8 μm of average grain diameter；Carbon dust described in claim 1 can be the common carbon dust that purity is more than 98wt%, also may be used
To be the carbon black of filler rank；When needing to add Fe2O3, the pure Fe2O3 powder of chemistry is selected.
3. a kind of flyash acid dissolution slag according to claim 1 prepares the method for matching grand powder, wherein the raw material powder
Mill, main purpose, which is that acquisition flyash acid dissolution slag is original, to be come into full contact with the carbon added and uniformly mixes, and grinding time is 1~4
Hour, preferably 2~3 hours；1300~1500 DEG C of reaction temperature, preferably 1350~1480 DEG C；Flowing nitrogen flow velocity 1~
3L/min, preferably 2L/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111842404A (en) * | 2020-06-02 | 2020-10-30 | 广东忠能科技集团有限公司 | Low-nitrogen slag treatment method |
| CN114773068A (en) * | 2022-05-25 | 2022-07-22 | 内蒙古海特华材科技有限公司 | Si preparation method by efficiently utilizing fly ash3N4Method for preparing/SiC/AlN composite ceramic |
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| CN1363535A (en) * | 2001-12-24 | 2002-08-14 | 徐利华 | Process for preparing composition 'Sailong' from industrial waste dregs by in-situ synthesis |
| CN1915908A (en) * | 2006-09-06 | 2007-02-21 | 郑州大学 | Method for preparing beta-sialon porous material |
| CN101353256A (en) * | 2008-09-11 | 2009-01-28 | 上海交通大学 | Method for preparing Sialon ceramic powder from aluminum ash and fly ash |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111842404A (en) * | 2020-06-02 | 2020-10-30 | 广东忠能科技集团有限公司 | Low-nitrogen slag treatment method |
| CN114773068A (en) * | 2022-05-25 | 2022-07-22 | 内蒙古海特华材科技有限公司 | Si preparation method by efficiently utilizing fly ash3N4Method for preparing/SiC/AlN composite ceramic |
| CN114773068B (en) * | 2022-05-25 | 2023-07-04 | 内蒙古海特华材科技有限公司 | Preparation of Si by using fly ash efficiently 3 N 4 Method for preparing SiC/AlN composite ceramic |
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