CN1686886A - Cinder microcrystalline glass and preparation method - Google Patents

Cinder microcrystalline glass and preparation method Download PDF

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Publication number
CN1686886A
CN1686886A CN 200510046233 CN200510046233A CN1686886A CN 1686886 A CN1686886 A CN 1686886A CN 200510046233 CN200510046233 CN 200510046233 CN 200510046233 A CN200510046233 A CN 200510046233A CN 1686886 A CN1686886 A CN 1686886A
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China
Prior art keywords
glass
shrend
flyash
sintering
240min
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CN 200510046233
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CN1285528C (en
Inventor
史培阳
姜茂发
刘承军
王德永
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Northeastern University China
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Northeastern University China
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0054—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing PbO, SnO2, B2O3
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
    • C03C10/0045—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The present invention relates to a slag nucleated glass and its preparation method. Its chemical composition includes (by wt%) SiO2 40-70%, Al2O3 6-15%, CaO 5-10%, MgO 4-30%, Fe2O3 9-12%, FeO 9-12%, B2O3 0.1-3% and Na2O 0.3-1%. Its microhardness is 7.5-9, bending strength is 150-177 MPa, apparent volume density is 2.7-2.96g, minus cu.cm, acid resistance is 92-99% and alkali resistance is 90-98%. Its preparation method includes the steps of preparing raw materials, mixing materials, melting, water extracting, forming, sintering and crystallization.

Description

A kind of cinder microcrystalline glass and preparation method thereof
Technical field
The present invention relates to the comprehensive utilization of trade waste, being specifically related to iron tailings, boron mud and flyash is cinder microcrystalline glass of feedstock production and preparation method thereof.
Background technology
The slag environmental pollution problem is on the rise along with the increase of quantity discharged, the harm of environment is mainly shown: the destruction of water pollution, the serious salinification of soil and natural ecological environment.Because banking up of all kinds of waste residues, barren rock, mine tailing, it is comparatively serious to occupy and destroy the soil.According to the data report, the growing amount of China's flyash in 2000 reaches 1.6 hundred million tons, and this numerical value increased to some extent in recent years.Yet the utilization of coal ash rate is utilized as the master but less than 50% simply again with extensive style, and utilizes cost higher.
Chinese patent application 03128180.x discloses a kind of cordierite glass-ceramic and manufacture method thereof with fly-ash Preparation, the main raw material of making devitrified glass is a flyash, also must add alumina powder or magnesiumcarbonate or magnesium basic carbonate in addition, perhaps magnesite or brucite or magnesium oxide powder and methyl cellulose binder and water.Chinese patent application 03111105.x discloses a kind of compound fly ash building manufacture method of glass-ceramic, is main raw material with flyash, adds nucleator, toughner, tinted shade powder, mineral dye or light-storing and emitting material in addition and makes devitrified glass.Above technological line can both consume trade waste---flyash, to solving problem of environmental pollution positive effect is arranged, yet because it utilizes in the method and must especially add other industrial raw material, therefore utilizes cost higher relatively.
Summary of the invention
Present situation at solid waste processing and utilizing such as flyash, the invention provides a kind of is the method for feedstock production cinder microcrystalline glass with flyash, iron tailings and boron mud, reach the utilization ratio that improves flyash, iron tailings and boron mud, the purpose of alleviate environmental pollution, making rational use of resources.
Cinder microcrystalline glass of the present invention is to be raw material with flyash, iron tailings and boron mud, does not add any other industrial raw material in addition, is prepared from sintering process.Below be the analytical results that the present invention adopts exhausted raw material chemical constitution:
Title Form (%)
????SiO 2 ????Al 2O 3 ????CaO ????MgO ????T ??B 2O 3 ????R 2O Ash
Iron tailings flyash boron mud ????75.91 ????45.65 ????26.43 ????0.65 ????15.45 ????1.78 ????1.82 ????17.05 ????2.11 ????1.51 ????1.62 ????40.26 ????11.69 ????9.12 ????10.11 ??- ??- ??2.62 ????- ????- ????1.68 ?8.42 ?11.11 ?10.75
Processing step of the present invention comprises:
1, batching.According to the chemical composition analysis of flyash, iron tailings and boron mud and to the requirement of product, by weight batching, flyash: 10%～60%, boron mud: 20%～60%, iron tailings: 10%～60%;
2, batch mixing: adopt ball milling to mix, mixing time is 60～240min;
3, found: carry out in High Temperature Furnaces Heating Apparatus, temperature of fusion is 1300～1600 ℃, and soaking time is 60～240min;
4, shrend: the glass melt shrend is become the glass particle of 0.074～0.3mm, and hot blast drying is stand-by;
5, moulding: the shrend glass particle is put into ball mill, grind to form the glass powder of granularity, and the glass powder after will grinding packs in the mould less than 0.074mm, compression moulding, forming pressure is 1500～2000N;
6, sintering and crystallization: the glass powder of compression moulding is placed in the High Temperature Furnaces Heating Apparatus, temperature rise rate with 5～30 ℃/min is warmed up to 800～1000 ℃, constant temperature sintering 100～240min, temperature rise rate with 5～30 ℃/min is warmed up to 850～1120 ℃ then, constant temperature crystallization 100～240min, last air cooling is made devitrified glass to room temperature through polishing, polishing.
The cinder microcrystalline glass chemical constitution by weight percentage of the present invention's preparation is: SiO 2: 40～70%, Al 2O 3: 6～15%, CaO:5～10%, MgO:4～30%, Fe 2O 3: 9～12%, FeO:9～12%, B 2O 3: 0.1～3%, Na 2O:0.3～1%.The inventive method belongs to the utilization that becomes more meticulous of trade wastes such as flyash, prepared devitrified glass microhardness 7.5～9, and folding strength 150～177MPa, apparent bulk density is 2.7～2.96g.cm -3, acid resistance 92～99%, alkali resistance 90～98%, excellent performance has than high added value.Cinder microcrystalline glass of the present invention can be used as material of construction and is applied to building trade, and it is anticorrosion in chemical industry equipment to can be used as anticorrosion ceramic applications.Of the present invention applying will be beneficial to environment protection and avoid the waste of resource.
Embodiment
Embodiment 1
1, batching: raw material is by weight ratio: flyash 30%, iron tailings 60%, boron mud 10%;
2, batch mixing: the raw material that will weigh by weight ratio adopts ball milling to mix mixing time 120min;
3, found: above-mentioned material is placed High Temperature Furnaces Heating Apparatus, and temperature of fusion is 1480 ℃ ± 40 ℃, and soaking time is 2 hours;
4, shrend: the glass melt shrend is become glass particle, stand-by with hot blast drying;
5, moulding: the shrend glass particle is ground to form the glass powder of granularity less than 0.074mm, and the glass powder after will grinding packs in the mould into, compression moulding, forming pressure is 2000N;
6, sintering and crystallization: the glass of compression moulding is placed in the High Temperature Furnaces Heating Apparatus, temperature rise rate with 10 ℃/min is warming up to 960 ℃ ± 30 ℃, and constant temperature sintering, sintering time are 2 hours, temperature rise rate with 10 ℃/min is warming up to 1110 ℃ ± 30 ℃, constant temperature crystallization 3 hours then; Be annealed to 600 ℃ of following naturally cooling with 30 ℃/hour speed, make devitrified glass through polishing, polishing again.
The chemical constitution of the cinder microcrystalline glass that above-mentioned technology is prepared is: SiO 2: 66.3%, Al 2O 3: 10.12%, CaO:7.43%, MgO:4.41%, Fe 2O 3: 6.14%, FeO:3.06%, B 2O 3: 2.03%, Na 2O:0.46%.The performance perameter of this devitrified glass is density 2.82g.cm -3, hardness 7.83, folding strength 182MPa, acid resistance 98.2%, alkali resistance 99.5%.
Embodiment 2
1, batching: raw material is by weight ratio: flyash 30%, iron tailings 40%, boron mud 30%;
2, batch mixing: the raw material that will weigh by weight ratio adopts ball milling to mix mixing time 120min;
3, found: above-mentioned material is placed High Temperature Furnaces Heating Apparatus, and glass melting temperature is 1430 ℃ ± 40 ℃, and soaking time is 1.5 hours,
4, shrend: the glass melt shrend is become glass particle, dry stand-by;
5, moulding: the shrend glass particle is ground to form the glass powder of granularity less than 0.074mm, and the glass powder after will grinding packs in the mould into, compression moulding, forming pressure is 1500N;
6, sintering and crystallization: the glass of compression moulding is placed in the High Temperature Furnaces Heating Apparatus, temperature rise rate with 20 ℃/min is warming up to 900 ℃ ± 30 ℃, the constant temperature sintering, sintering time is 2 hours, temperature rise rate with 20 ℃/min is warming up to 970 ℃ ± 30 ℃ then, constant temperature crystallization 2.5 hours is annealed to 600 ℃ of following naturally cooling with 30 ℃/hour speed, makes devitrified glass through polishing, polishing again.
The chemical constitution of the cinder microcrystalline glass that above-mentioned technology is prepared is: SiO 2: 57.68%, Al 2O 3: 8.74%, CaO:7.08%, MgO:13.44%, Fe 2O 3: 7.09%, FeO:2.53%, B 2O 3: 2.77%, Na 2O:0.59%.The performance perameter of this devitrified glass is density 2.86g.cm -3, hardness 7.92, folding strength 187MPa, acid resistance 99.2%, alkali resistance 99.4%.
Embodiment 3
1, batching: raw material is by weight ratio: flyash 60%, iron tailings 10%, boron mud 30%;
2, batch mixing: the raw material that will weigh by weight ratio adopts ball milling to mix mixing time 120min;
3, found: above-mentioned material is placed High Temperature Furnaces Heating Apparatus, and glass melting temperature is 1400 ℃ ± 40 ℃, and soaking time is 1 hour;
4, shrend: the glass melt shrend is become glass particle, dry stand-by;
5, moulding: the shrend glass particle is ground to form the glass powder of granularity less than 0.074mm, and the glass powder after will grinding packs in the mould into, compression moulding, forming pressure is 1800N;
6, sintering and crystallization: the glass of compression moulding is placed in the High Temperature Furnaces Heating Apparatus, temperature rise rate with 5 ℃/min is warming up to 890 ℃ ± 30 ℃, and constant temperature sintering, sintering time are 2 hours, temperature rise rate with 5 ℃/min is warming up to 930 ℃ ± 30 ℃, constant temperature crystallization 2 hours then; Be annealed to 600 ℃ of following naturally cooling with 20 ℃/hour speed, make devitrified glass through polishing, polishing again.
The chemical constitution of the cinder microcrystalline glass that above-mentioned technology is prepared is: SiO 2: 44.39%, Al 2O 3: 7.89%, CaO:6.59%, MgO:26.66%, Fe 2O 3: 8.77%, FeO:1.74%, B 2O 3: 3.08%, Na 2O:0.84%.The performance perameter of this devitrified glass is density 2.81g.cm -3, hardness 7.8, folding strength 172MPa, acid resistance 97.2%, alkali resistance 98.5%.

Claims (3)

1, a kind of cinder microcrystalline glass, the preparation raw material that it is characterized in that this devitrified glass is flyash, iron tailings and boron mud, its chemical constitution is by weight percentage: SiO 2: 40～70%, Al 2O 3: 6～15%, CaO:5～10%, MgO:4～30%, Fe 2O 3: 9～12%, FeO:9～12%, B 2O 3: 0.1～3%, Na 2O:0.3～1%.
2, according to the described cinder microcrystalline glass of claim 1, it is characterized in that this cinder microcrystalline glass microhardness is 7.5～9, folding strength is 150～177MPa, apparent bulk density is 2.7～2.96g.cm -3, acid resistance is 92～99%, alkali resistance is 90～98%.
3, the preparation method of the described cinder microcrystalline glass of claim 1 is characterized in that comprising batching, batch mixing, founds, shrend, moulding, sintering and crystallization process step:
1. batching: according to the chemical composition analysis of flyash, iron tailings and boron mud and to the requirement of product, by weight batching, flyash: 10%～60%, boron mud: 20%～60%, iron tailings: 10%～60%;
2. batch mixing: adopt ball milling to mix, mixing time is 60～240min;
3. found: carry out in High Temperature Furnaces Heating Apparatus, temperature of fusion is 1300～1600 ℃, and soaking time is 60～240min;
4. shrend: the glass melt shrend is become the glass particle of 0.074～0.3mm, and hot blast drying is stand-by;
5. moulding: the shrend glass particle is put into ball mill, grind to form the glass powder of granularity, and the glass powder after will grinding packs in the mould less than 0.074mm, compression moulding, forming pressure is 1500～2000N;
6. sintering and crystallization: the glass powder of compression moulding is placed in the High Temperature Furnaces Heating Apparatus, temperature rise rate with 5～30 ℃/min is warmed up to 800～1000 ℃, constant temperature sintering 100～240min, temperature rise rate with 5～30 ℃/min is warmed up to 850～1120 ℃ then, constant temperature crystallization 100～240min, last air cooling is made devitrified glass to room temperature through polishing, polishing.
CN 200510046233 2005-04-12 2005-04-12 Cinder microcrystalline glass and preparation method Expired - Fee Related CN1285528C (en)

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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101058480B (en) * 2007-04-04 2010-04-21 大连理工大学 Method of preparing foam glass based on boric sludge
CN101024554B (en) * 2007-02-12 2010-05-26 内蒙古科技大学 Rear-earth-rich, niobium-rich and cand-rich rear sorted tail-ore microcrystal glass and manufacturing method
CN101891389A (en) * 2010-07-22 2010-11-24 西南科技大学 Chrysotile tailing microcrystal glass and preparation method thereof
CN101328021B (en) * 2008-07-22 2010-12-08 内蒙古科技大学 Porous devitrified glass and manufacturing method thereof
CN102060444A (en) * 2010-11-10 2011-05-18 内蒙古科技大学 Foam glass ceramic and preparation method thereof
CN102092950A (en) * 2010-12-16 2011-06-15 沈阳化工大学 Method for preparing glass ceramic by utilizing talcum and bentonite as raw materials
CN102229468A (en) * 2010-07-09 2011-11-02 鞍钢集团矿业公司 Low-expansion micro-crystal glass manufactured from high-silicon iron tailings and preparation method thereof
CN102627406A (en) * 2012-04-10 2012-08-08 达州市海蓝冶金设备制造有限公司 Method for preparing microcrystalline glass by using high titanium blast furnace slag
CN102795772A (en) * 2012-07-23 2012-11-28 北京大有盛和科技有限公司 Method for preparing microcrystalline glass from kaolin-type coal gangue or fly ash and carbide slag
CN102875025A (en) * 2012-11-07 2013-01-16 会理县紫源矿业有限责任公司 Black glass ceramics and preparation method thereof
CN103708732A (en) * 2013-01-12 2014-04-09 上海大学 Method for preparing microcrystalline glass from steel slag
CN105565671A (en) * 2016-01-22 2016-05-11 邢台市晶玉微晶板材有限公司 Method for preparing microcrystalline glass from iron tailings
CN106396412A (en) * 2016-08-31 2017-02-15 望江宇花玻璃有限公司 Perovskite-based ceramic glass containing modified fly ash and preparation process of perovskite-based ceramic glass
CN108751722A (en) * 2018-08-11 2018-11-06 芜湖市新海域智能科技有限公司 A kind of computer hard disk substrate devitrified glass and preparation method
CN115745380A (en) * 2022-10-31 2023-03-07 苏州大学 Light sintered microcrystal plate and sintering process thereof
US12027306B2 (en) 2021-06-10 2024-07-02 Nichia Corporation Method of producing SmFeN-based rare earth magnet
US12027294B2 (en) 2021-09-27 2024-07-02 Nichia Corporation Method of producing SmFeN-based rare earth magnet

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101024554B (en) * 2007-02-12 2010-05-26 内蒙古科技大学 Rear-earth-rich, niobium-rich and cand-rich rear sorted tail-ore microcrystal glass and manufacturing method
CN101058480B (en) * 2007-04-04 2010-04-21 大连理工大学 Method of preparing foam glass based on boric sludge
CN101328021B (en) * 2008-07-22 2010-12-08 内蒙古科技大学 Porous devitrified glass and manufacturing method thereof
CN102229468A (en) * 2010-07-09 2011-11-02 鞍钢集团矿业公司 Low-expansion micro-crystal glass manufactured from high-silicon iron tailings and preparation method thereof
CN101891389A (en) * 2010-07-22 2010-11-24 西南科技大学 Chrysotile tailing microcrystal glass and preparation method thereof
CN101891389B (en) * 2010-07-22 2011-11-30 西南科技大学 Chrysotile tailing microcrystal glass and preparation method thereof
CN102060444B (en) * 2010-11-10 2012-09-26 内蒙古科技大学 Foam glass ceramic and preparation method thereof
CN102060444A (en) * 2010-11-10 2011-05-18 内蒙古科技大学 Foam glass ceramic and preparation method thereof
CN102092950B (en) * 2010-12-16 2012-10-17 沈阳化工大学 Method for preparing glass ceramic by utilizing talcum and bentonite as raw materials
CN102092950A (en) * 2010-12-16 2011-06-15 沈阳化工大学 Method for preparing glass ceramic by utilizing talcum and bentonite as raw materials
CN102627406A (en) * 2012-04-10 2012-08-08 达州市海蓝冶金设备制造有限公司 Method for preparing microcrystalline glass by using high titanium blast furnace slag
CN102795772B (en) * 2012-07-23 2014-09-24 北京大有盛和科技有限公司 Method for preparing microcrystalline glass from kaolin-type coal gangue or fly ash and carbide slag
CN102795772A (en) * 2012-07-23 2012-11-28 北京大有盛和科技有限公司 Method for preparing microcrystalline glass from kaolin-type coal gangue or fly ash and carbide slag
CN102875025A (en) * 2012-11-07 2013-01-16 会理县紫源矿业有限责任公司 Black glass ceramics and preparation method thereof
CN103708732B (en) * 2013-01-12 2016-01-20 上海大学 A kind of prepared from steel slag is for the method for devitrified glass
CN103708732A (en) * 2013-01-12 2014-04-09 上海大学 Method for preparing microcrystalline glass from steel slag
CN105565671A (en) * 2016-01-22 2016-05-11 邢台市晶玉微晶板材有限公司 Method for preparing microcrystalline glass from iron tailings
CN106396412A (en) * 2016-08-31 2017-02-15 望江宇花玻璃有限公司 Perovskite-based ceramic glass containing modified fly ash and preparation process of perovskite-based ceramic glass
CN108751722A (en) * 2018-08-11 2018-11-06 芜湖市新海域智能科技有限公司 A kind of computer hard disk substrate devitrified glass and preparation method
US12027306B2 (en) 2021-06-10 2024-07-02 Nichia Corporation Method of producing SmFeN-based rare earth magnet
US12027294B2 (en) 2021-09-27 2024-07-02 Nichia Corporation Method of producing SmFeN-based rare earth magnet
CN115745380A (en) * 2022-10-31 2023-03-07 苏州大学 Light sintered microcrystal plate and sintering process thereof

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