CN104557094A - Method for preparing mullite aggregate for high-alumina refractory bricks by taking high-aluminum pulverized fuel ash as single aluminum source - Google Patents

Method for preparing mullite aggregate for high-alumina refractory bricks by taking high-aluminum pulverized fuel ash as single aluminum source Download PDF

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Publication number
CN104557094A
CN104557094A CN201510035904.2A CN201510035904A CN104557094A CN 104557094 A CN104557094 A CN 104557094A CN 201510035904 A CN201510035904 A CN 201510035904A CN 104557094 A CN104557094 A CN 104557094A
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mullite
alumina refractory
mullite aggregate
raw
refractory brick
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李会泉
林滨
李少鹏
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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Abstract

The invention relates to a method for sintering and synthesizing mullite aggregate for high-alumina refractory bricks by taking high-aluminum pulverized fuel ash as a single aluminum source, belonging to the technical field of sintered mullite and high-alumina refractory bricks. The method comprises the following steps: by taking Jungar high-aluminum pulverized fuel ash as a unique raw material, performing pretreatment, ball-milling, molding and sintering, thereby obtaining the high-alumina M60 and M70 series mullite aggregate for refractory bricks. According to the method disclosed by the invention, the solid waste high-aluminum pulverized fuel ash serves as the raw material, an extra aluminum source does not need to be added, the method has the advantages of wide raw material source, low production cost and obvious environmental benefits, and the sintered mullite aggregate accords with the national standard of the raw materials of the high-alumina refractory bricks. Therefore, the mullite aggregate has a certain market advantages.

Description

A kind of is the method that high-alumina refractory brick mullite aggregate is prepared in single aluminium source with aluminous fly-ash
Technical field
The present invention relates to fused mullite and high-alumina refractory brick technical field.
Background technology
China is consumption of coal first big country, the flyash of coal-burning power plant's discharge is the second largest solid waste of China, its discharge causes serious environment and ecological pollution with accumulation, how to utilize fast and efficiently or to dispose flyash, particularly high value added utilization flyash is the very urgent and difficult task of in face of us one of pendulum.
Mullite (3Al 2o 32SiO 2) be a kind of mineral, gain the name because originating in the ground such as Scottish More island, melt temperature about 1910 DEG C.It has features such as expanding evenly, thermal shock resistance is fabulous, load softening point is high, high temperature creep value is little, hardness is large, resistance to chemical corrosion is good, be manufacture high-quality refractory material, ceramic, be used as the raw mineral materials of reinforcement etc. of ceramic matrix composite, metal composite.
Aluminous fly-ash is a kind of flyash type of uniqueness, main containing amorphous glass phase and a large amount of mullite phases in it.Al in aluminous fly-ash 2o 3content can reach about 50%, and foreign matter content is low relative to ordinary fly ash, is the desirable feedstock of producing mullite.
Due to mullite be high temperature, the product that formed under low pressure special conditions, extremely rare at occurring in nature.Industrial mullite is mainly synthetic and obtains.In prior art, the method for mullite synthesizing mainly contains electric smelting method and sintering process.Electric smelting method is formed the melting in electric arc of mixed raw material, and shortcoming is that current consumption is large, synthesis condition is harsh.Sintering process can be divided into silica-alumina gel method and mineral facies political reform according to raw materials used different in kind.Wherein silica-alumina gel method adopts inorganic and organic raw material to make sial colloid according to certain chemical constitution respectively, and then at high temperature roasting forms, and shortcoming is that energy consumption is higher, and organic raw material is expensive.Mineral facies political reform forms with natural mineral high-temperature calcinations in kiln such as alumine, kaolin, agalmatolite, flint claies, there is material choice wide ranges, the feature that production cost is low, the shortcoming of the method is except energy consumption height, also due to its mineral composition and mullite form between there is larger difference, cause mullite transformation efficiency not high, waste resource.At present, natural matter sintering mullite synthesizing, accounts for the overwhelming majority of mullite suitability for industrialized production.
Few with the document of flyash sintering mullite synthesizing both at home and abroad, major part adopts flyash to mix a certain amount of bauxitic clay or commercial alumina obtains mullite through high-temperature calcination, this kind of technology effectively can utilize this solid waste of flyash, reduce production cost, but the commercial alumina price of mixing in raw material is higher.And used in flyash mullite synthesizing technology in the past, do not process flyash, or process is relatively simple, iron-holder is higher, alumina silica ratio is also lower simultaneously, therefore synthesizes the mullite of different alumina content often through aluminium sources such as the commercial alumina added or bauxitic clays.
Summary of the invention
For the deficiency of the above mullite synthesizing.It is single aluminium source (alumina content nearly 50%) with aluminous fly-ash that the present invention proposes a kind of, does not add any natural mineral or commercial alumina, the method for direct sintering synthesis high-alumina refractory brick mullite aggregate.
The present invention propose with aluminous fly-ash, through a series of process, final fused mullite, is reached by following steps:
(1) with accurate Ge Er aluminous fly-ash for raw material, obtain pretreated flyash through links such as magnetic separation, desiliconization, Diluted Acid Washing, washing, dryings.
(2) flyash that obtains of pre-treatment, levigate through ball mill.Adopt wet method or dry ball milling.Wet ball grinding, the mass ratio of abrading-ball, raw material, water is 5 ~ 10:1:1, and milling time is 4 ~ 6h, and rotating speed is 400 ~ 800r/min.After wet-milling sample carry out filtering, dry.Dry ball milling, the mass ratio of abrading-ball and raw material is 5 ~ 10:1, and milling time is 4 ~ 6h, and rotating speed is 400 ~ 800r/min.
(3) after ball milling drying, flyash carries out semidrying compression moulding.It is 5 ~ 10% that the water yield is added in semidrying compression moulding, and forming pressure is 100 ~ 250MPa.For convenience of sample formation, also a small amount of binding agent can be added.Binding agent can be the sodium carboxymethyl-cellulose of 1wt%, 1wt% methylcellulose gum, 1wt% ethyl cellulose or 2wt% flour.
(4) shaping rear sample is put into retort furnace and is sintered.Sintering temperature is 1550 ~ 1650 DEG C, and constant temperature time is 2 ~ 4h.When controlling 50 ~ 1200 DEG C, temperature rise rate is 10 DEG C/min, and when 1200 ~ 1600 DEG C, temperature rise rate is 5 DEG C/min.
The pretreated flyash that above step (1) obtains, its Al 2o 3content can to 60 ~ 70%, Fe 2o 3content is less than 1%.
Flyash particle diameter after the grinding that above step (2) obtains is 10 ~ 40 μm (size distribution in less than 90%).
Feature of the present invention is as described below:
The present invention effectively make use of the solid waste aluminous fly-ash of coal-burning power plant's discharge, and raw material sources are extensive, and do not need to add any aluminium source, ecnomics and enviroment remarkable benefit.
The present invention's aluminous fly-ash used, mullite content own is high, and these mullites form through high temperature sintering in powder coal stove, complete primary mullite, only through secondary mullite, synthesis procedure need be decreased during sintering, obtain that mullite productive rate is high, quality better.
By the present invention, can obtain high-alumina refractory brick mullite aggregate, this aggregate meets People's Republic of China's ferrous metallurgy industry standard (YB/T 5267-2005).By the regulation and control to process parameter, the flyash Al after process 2o 3content to 60 ~ 70%, can obtain the mullite aggregate of M60, M70 series after sintering.
Embodiment
Be single aluminium source to what the present invention relates to aluminous fly-ash below by embodiment, the process of sintering synthesis high-alumina refractory brick mullite aggregate is described, but the present invention be not only confined to these embodiments.
Embodiment 1:
By aluminous fly-ash raw material flyash after magnetic separation, desiliconization, Diluted Acid Washing, washing, drying obtain the process of high aluminium silicon ratio, then put into WL-I atype particle sphere grinding machine carries out wet ball grinding, and wherein the mass ratio of abrading-ball, ash, water is 5:1:1, and Ball-milling Time is 5h, and rotating speed is 600r/min, and after ball milling, material after filtration, then puts into baking oven in 105 DEG C of dry 2h.Dried material adds the 1% sodium carboxymethyl-cellulose binding agent prepared in advance, and use electric tablet machine compression moulding after mixing, forming pressure is 170MPa, and sample shape is 2.83cm 2* the right cylinder of 1.2cm.Then sample is put into retort furnace to sinter, when controlling 50 ~ 1200 DEG C, temperature rise rate is 10 DEG C/min, and when 1200 ~ 1600 DEG C, temperature rise rate is 5 DEG C/min, 1600 DEG C of insulation 4h, then by its naturally cooling, obtain mullite product, this product meets fused mullite national standard.After this sample broke, obtain high-alumina refractory brick mullite aggregate.
Embodiment 2:
By aluminous fly-ash raw material flyash after magnetic separation, desiliconization, Diluted Acid Washing, washing, drying obtain the process of high aluminium silicon ratio, then put into WL-I atype particle sphere grinding machine carries out dry ball milling, and wherein the mass ratio of abrading-ball, ash is 5:1, and Ball-milling Time is 5h, and rotating speed is 600r/min, and after ball milling, material after filtration, then puts into baking oven in 105 DEG C of dry 2h.Dried material adds the 1% sodium carboxymethyl-cellulose binding agent prepared in advance, and use electric tablet machine compression moulding after mixing, forming pressure is 170MPa, and sample shape is 2.83cm 2* the right cylinder of 1.2cm.Then sample is put into retort furnace to sinter, when controlling 50 ~ 1200 DEG C, temperature rise rate is 10 DEG C/min, and when 1200 ~ 1600 DEG C, temperature rise rate is 5 DEG C/min, 1400 DEG C of insulation 4h, then by its naturally cooling, obtain mullite product, this product meets fused mullite national standard.After this sample broke, obtain high-alumina refractory brick mullite aggregate.
Embodiment 3:
By aluminous fly-ash raw material flyash after magnetic separation, desiliconization, Diluted Acid Washing, washing, drying obtain the process of high aluminium silicon ratio, then put into WL-I atype particle sphere grinding machine carries out ball milling, and wherein the mass ratio of abrading-ball, ash, water is 5:1:1, and Ball-milling Time is 5h, and rotating speed is 600r/min, and after ball milling, material after filtration, then puts into baking oven in 105 DEG C of dry 2h.Dried material adds the water of about 10%, and use electric tablet machine compression moulding after mixing, forming pressure is 150MPa, and sample shape is 2.83cm 2* the right cylinder of 1.2cm.Then sample is put into retort furnace to sinter, when controlling 50 ~ 1200 DEG C, temperature rise rate is 10 DEG C/min, and when 1200 ~ 1600 DEG C, temperature rise rate is 5 DEG C/min, 1500 DEG C of insulation 2h, then by its naturally cooling, obtain mullite product, this product meets fused mullite national standard.After this sample broke, obtain high-alumina refractory brick mullite aggregate.
Comparative example 1:
By aluminous fly-ash raw material flyash after magnetic separation, desiliconization, Diluted Acid Washing, washing, drying obtain the process of high aluminium silicon ratio, then material is added the 1% sodium carboxymethyl-cellulose binding agent prepared in advance, electric tablet machine compression moulding is used after mixing, forming pressure is 170MPa, and sample shape is 2.83cm 2* the right cylinder of 1.2cm.Then sample is put into retort furnace to sinter, when controlling 50 ~ 1200 DEG C, temperature rise rate is 10 DEG C/min, and when 1200 ~ 1600 DEG C, temperature rise rate is 5 DEG C/min, 1600 DEG C of insulation 4h, then by its naturally cooling, obtain mullite product, this product does not reach fused mullite national standard.
Comparative example 2:
By aluminous fly-ash raw material flyash after magnetic separation, desiliconization, Diluted Acid Washing, washing, drying obtain the process of high aluminium silicon ratio, then put into WL-I atype particle sphere grinding machine carries out ball milling, and wherein the mass ratio of abrading-ball, ash, water is 5:1:1, and Ball-milling Time is 5h, and rotating speed is 600r/min, and after ball milling, material after filtration, then puts into baking oven in 105 DEG C of dry 2h.Dried material is added the 1% sodium carboxymethyl-cellulose binding agent prepared in advance, use electric tablet machine compression moulding after mixing, forming pressure is 170MPa, and sample shape is 2.83cm 2* the right cylinder of 1.2cm.Then sample is put into retort furnace to sinter, when controlling 50 ~ 1200 DEG C, temperature rise rate is 10 DEG C/min, and when 1200 ~ 1500 DEG C, temperature rise rate is 5 DEG C/min, 1100 DEG C of insulation 4h, then by its naturally cooling, obtain mullite product, this product does not reach fused mullite national standard.
The mullite physical properties of embodiment and comparative example is as shown in table 1 below:
The mullite physical properties of table 1 embodiment and comparative example

Claims (5)

1. one kind is single aluminium source with aluminous fly-ash, sintering synthesis high-alumina refractory brick mullite aggregate, it is characterized in that with accurate Ge Er aluminous fly-ash be unique raw material, do not add extra aluminium source, through pre-treatment, ball milling, shaping, sintering obtain high-alumina refractory brick mullite aggregate.
2. high-alumina refractory brick mullite aggregate according to claim 1, is characterized in that pre-treatment step is magnetic separation, desiliconization, Diluted Acid Washing, washing, drying.
3. high-alumina refractory brick mullite aggregate according to claim 1 and 2, is characterized in that: adopt wet method or dry ball milling.Wet ball grinding, the mass ratio of abrading-ball, raw material, water is 5 ~ 10:1:1, dry ball milling, and the mass ratio of abrading-ball and raw material is 5 ~ 10:1, and milling time is 4 ~ 6h, and rotating speed is 400 ~ 800r/min.Flyash particle diameter after grinding is 10 ~ 40 μm (size distribution in less than 90%).
4. high-alumina refractory brick mullite aggregate according to claims 1 to 3, is characterized in that: forming method is semidrying compression moulding.Adding the water yield is 5 ~ 10%, and forming pressure is 100 ~ 250MPa.For convenience of sample formation, also a small amount of binding agent can be added.Binding agent can be the sodium carboxymethyl-cellulose of 1wt%, 1wt% methylcellulose gum, 1wt% ethyl cellulose or 2wt% flour.
5. high-alumina refractory brick mullite aggregate according to claims 1 to 4, is characterized in that: sintering temperature is 1550 ~ 1650 DEG C, and constant temperature time is 2 ~ 4h.
CN201510035904.2A 2015-01-23 2015-01-23 Method for preparing mullite aggregate for high-alumina refractory bricks by taking high-aluminum pulverized fuel ash as single aluminum source Pending CN104557094A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107285739A (en) * 2016-04-05 2017-10-24 神华集团有限责任公司 A kind of the multiple element compound phase material and preparation method thereof
CN107285774A (en) * 2016-04-05 2017-10-24 神华集团有限责任公司 A kind of method of white clay or coal ash for manufacturing mullite and the mullite of preparation

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102583409A (en) * 2012-01-10 2012-07-18 中国科学院过程工程研究所 Method for producing mullite and calcium silicate by using high-alumina fly ash

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102583409A (en) * 2012-01-10 2012-07-18 中国科学院过程工程研究所 Method for producing mullite and calcium silicate by using high-alumina fly ash

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107285739A (en) * 2016-04-05 2017-10-24 神华集团有限责任公司 A kind of the multiple element compound phase material and preparation method thereof
CN107285774A (en) * 2016-04-05 2017-10-24 神华集团有限责任公司 A kind of method of white clay or coal ash for manufacturing mullite and the mullite of preparation

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Application publication date: 20150429