CN106167356A - The preparation method of a kind of foam pyroceram and products obtained therefrom - Google Patents
The preparation method of a kind of foam pyroceram and products obtained therefrom Download PDFInfo
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- CN106167356A CN106167356A CN201610520606.7A CN201610520606A CN106167356A CN 106167356 A CN106167356 A CN 106167356A CN 201610520606 A CN201610520606 A CN 201610520606A CN 106167356 A CN106167356 A CN 106167356A
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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
- C03C10/0063—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 waste materials, e.g. slags
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
-
- 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
-
- 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
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
- C03C11/007—Foam glass, e.g. obtained by incorporating a blowing agent and heating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Ceramic Engineering (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Glass Compositions (AREA)
Abstract
The present invention relates to preparation method and the products obtained therefrom of a kind of foam pyroceram, step is: with gangue, dolomite, burning Talcum, silica sand as raw material, calculates the consumption of each raw material by glass composition；Weighing each raw material by proportioning, by each raw material pulverizing, mix homogeneously, heating is melt into uniform vitreous humour, and vitreous humour, through molding, annealing, obtains bulk glass；Bulk glass is risen to 900 1200 DEG C by room temperature, is incubated 0 2h, then cools down, obtain foam pyroceram.The present invention is with Coal Refuse as primary raw material, and the utilization for gangue provides new thinking and method, turns waste into wealth, and has reached the purpose curbed environmental pollution while economizing on resources.Raw material is made bulk glass and is then directly heated foaming by the present invention, it is not necessary to by glass breaking, without adding various additives, simplify the preparation process of foam pyroceram, reduce production cost simultaneously, products obtained therefrom good quality, can be in building field wide popularization and application.
Description
Technical field
The present invention relates to the preparation method of a kind of foam pyroceram and the foam pyroceram of gained, be specifically related to one
With solid waste as primary raw material, in the case of being not added with foaming agent voluntarily foaming prepare foam pyroceram method and
The product that the method prepares, belongs to glass and solid waste utilizes technical field.
Background technology
The recycling of solid waste both economized on resources, and reduces entreprise cost, protects again environment, meet Resources for construction saving
Type society and the requirement of sustainable development.Utilizing solid waste to produce construction material (such as foam glass) is the weight that solid waste utilizes
Want one of approach.Gangue is the solid waste of discharge during coal mining process and coal washing, total in industrial solid wastes discharge
Amount is occupied significant proportion.Gangue is stacked and is taken a large amount of soil, and causes environmental pollution.Gangue can be used for generating electricity, making
Sintered hollow block, replacement clay produce cement and produce the chemical products such as crystal aluminum chloride, also utilize gangue to prepare
The report of glass material, such as: it is micro-that University of Science & Technology, Beijing king long queue et al. utilizes gangue and iron tailings to be prepared for calcium and magnesium aluminum silicon system
Crystal glass；Song Jianjun et al., with gangue as primary raw material, uses sintering process to be prepared for β-wollastonite phase devitrified glass；Li Yuhua
Et al. with cullet and gangue as primary raw material, use sintering process to be prepared for Novel microcrystalline foam glass.These researchs are coal
The utilization of spoil provides a new direction, not only has an economic benefit, the most certain environmental benefit.
Foam pyroceram be have heat insulation, absorb sound, the function such as fire prevention, be a kind of novel light construction material and decoration material
Material.Usual foam devitrified glass produce main use for sintering process, mainly comprising the processes of by quantitative broken glass of sintering process
Glass, foaming agent, property-modifying additive and accelerator etc., form batch through finely divided mix homogeneously, batch put into spy
In fixed mould, then through preheating, sinter, foam, the technique such as annealing prepares glass, owing to glass dust sintering process would generally be sent out
Raw crystallization, therefore the glass of gained is often foam pyroceram.This production technology has the disadvantage in that process is complicated, work
Measure the biggest；Need the mould of special high temperature resistant and anti-chilling；Annealing time is long；Goods need reprocessing after burning till.
Summary of the invention
The deficiency existed for existing foam pyroceram preparation technology, the invention provides a kind of foam pyroceram
Preparation method and the foam pyroceram of gained, the method is with solid waste as primary raw material, it is achieved that the recovery profit of refuse
With, additionally, without by glass breaking in preparation process, raw material type is few, preparation technology is simple, low cost.
The present invention, with gangue as primary raw material, adds dolomite, the raw material of the burning composition glass such as Talcum, silica sand simultaneously,
Through the collocation of each raw material, during preparation, each raw material being directly prepared into bulk glass, bulk glass is directly carried out at heat without pulverizing
Reason can be prepared by foam pyroceram, enormously simplify preparation process.The present invention is utilization and the foam crystallite glass of gangue
The preparation of glass provides new thinking, and concrete technical scheme is as follows:
A kind of preparation method of foam pyroceram, the method comprises the following steps:
(1) with gangue, dolomite, burning Talcum, silica sand as raw material, by the consumption of the following glass composition each raw material of calculating:
SiO240-54wt%、Al2O322.5-24 wt%、MgO13.5-14.3 wt%、CaO7-19.5 wt %、Fe2O31.2-1.3 wt
%、SO31.2-1.3 wt %、TiO20.7-0.8 wt %；
(2) weighing each raw material by proportioning, by each raw material pulverizing, mix homogeneously, heating is melt into uniform vitreous humour, vitreous humour warp
Molding, annealing, obtain bulk glass；
(3) bulk glass is risen to 900-1200 DEG C by room temperature, be incubated 0-2h, then cool down, obtain foam pyroceram.
In above-mentioned preparation method, select each raw material according to the composition of glass, in order to improve twice laid amount, with gangue be
Primary raw material, i.e. glass ingredient are first provided by gangue as far as possible, if gangue cannot meet glass ingredient content requirement, then
It is supplemented to desired content with dolomite, burning Talcum, silica sand.When selecting raw material dosage, the Al in glass2O3Main by gangue
There is provided, the SiO in glass2By gangue, burning Talcum and silica sand offer, the MgO in glass is mainly carried by burning Talcum, dolomite
Confession, the CaO in glass is mainly provided by dolomite, the Fe in glass2O3And other composition is all from gangue.
In above-mentioned preparation method, gangue is primary raw material, after selecting each raw material according to mentioned above principle, is computed, bastard coal
Stone content in total raw material is more than 45wt%.
In above-mentioned steps (2), each raw material can be pulverized by ball mill, mixing.After each raw material pulverizing, cross 120 mesh sieves, will
The raw material that granule is big screens out.
In above-mentioned steps (2), each raw material is heated to 1450 DEG C of insulation 2h, is melt into uniform vitreous humour.Gained glass
Liquid, according to common process molding, annealing, obtains bulk glass, i.e. both bulk glasses.
In above-mentioned steps (3), bulk glass directly carrying out heat treatment, heat treatment step is: by bulk glass by room temperature
It is warming up to 900-1200 DEG C, and is incubated 0-2h at this temperature, when being incubated 0h, represent and bulk glass is risen to 900-by room temperature
1200 DEG C, the most warm direct cooling.The present invention is without by glass pulverizing, tabletting, sintering, simplifying technological process.Preferably,
Bulk glass is warming up to 1100 DEG C.
In above-mentioned steps (3), it is warming up to 900-1200 DEG C of insulation 0-2h, preferably 2h.
In above-mentioned steps (3), rise to 900-1200 DEG C with the programming rate less than or equal to 5 DEG C/min.
The glass of gained is foam pyroceram according to the method described above, and this inside glass has a large amount of bubble, and has crystallite to deposit
, stable in properties, there is good application prospect.The foam pyroceram prepared according to the method described above also protects model in the present invention
Within enclosing.
The invention have the advantages that
1, the present invention is with Coal Refuse as primary raw material, and the utilization for gangue provides new thinking and method,
In raw material, the content of gangue is more than 45%, advantageously reduces storing up of gangue, it is achieved that twice laid, turns waste into wealth,
Having reached the purpose curbed environmental pollution while economizing on resources, added value of product is high；
2, raw material is made bulk glass and is then directly heated foaming by the present invention, it is not necessary to by glass breaking, various without adding
Additive, simplifies the preparation process of foam pyroceram, reduces production cost simultaneously.
3, gained foam pyroceram of the present invention be black to canescence, inside has a large amount of bubble, and product quality is excellent,
This crystallite foam glass can be used as heat insulation, sound absorption, moistureproof, fire proofing material, is the light high-strength building material of a kind of superior performance
And ornament materials, can be in building field wide popularization and application.
Accompanying drawing explanation
The sectional view of Fig. 1 embodiment 1 gained glass sample.
The XRD figure of Fig. 2 embodiment 1 gained glass sample.
Detailed description of the invention
Below, by specific embodiment the present invention it is further explained and illustrates, it should be appreciated that stating under,
Bright being intended merely to explains the present invention, is not defined its content.
The each raw material of the present invention all can have been bought in the market, in following embodiment, and the main chemical compositions of each raw material used
As shown in table 1 below, it is to burn lose and/or decompose the gaseous product produced less than 100% part.
Embodiment 1
The preparation method of foam pyroceram is as follows:
That 1, designs foam pyroceram consists of (wt%): SiO253.27%、Al2O322.93%、MgO13.63 %、CaO7%、
Fe2O31.22 %、SO31.20 %、TiO20.75 %；Form according to this glass, calculate feed coal spoil, dolomite, burning Talcum,
The consumption of silica sand, and weigh each raw material by proportioning；
2, use ball mill that colliery powder was milled to 200 mesh sieves, then gangue is mixed by proportioning with other raw materials, through ball
Grinding machine ball milling, crosses 120 mesh sieves；
3, the compound that ball milling sieves is incubated 2h at 1450 DEG C in crucible, is melt into uniform vitreous humour, and gained vitreous humour is again
Through molding, annealing 1h, furnace cooling, obtain bulk glass；
4, bulk glass is placed in high temperature resistance furnace, from room temperature with the programming rate of 5 DEG C/min be raised to respectively 800 DEG C, 900
DEG C, 1000 DEG C, 1050 DEG C, 1100 DEG C, 1150 DEG C, 1200 DEG C, after rising to each temperature, be incubated 0h, 1h, 2h respectively in this temperature and enter
Row heat treatment, stops heating, is cooled to room temperature and obtains glass product after heat treatment.
It can be seen that the foaming effect of heat treatment 2h gained glass is better than 1h in experimentation, heat treatment 1h gained glass
Foaming effect better than 0h, heat treatment 2h foam more horn of plenty, the therefore preferred 2h of heat treatment time.Heat treatment temperature is 800 DEG C
Time, inside glass is almost without bubble formation, time in the range of 900-1100 DEG C, along with the rising of temperature, the bubble of inside glass
Measure into rising trend.Fig. 1 is at 800 DEG C, 900 DEG C, 1000 DEG C, 1050 DEG C, 1100 DEG C, heat treatment 2h gained glass at 1200 DEG C
Sectional drawing, it can be seen that when temperature is 800 DEG C, the bubble of inside glass almost without；When temperature is raised to 900
DEG C time, there is bubble in inside glass, and internal dimmed；When temperature is raised to 1000 DEG C, glass surface starts to turn white, and internal occur
More bubbles, volume becomes big；When temperature is raised to 1100 DEG C, there are a large amount of bubbles in inside glass, and glass volumetric expansion is maximum, close
Spend and less than water can float up at the water surface；When temperature is raised to 1200 DEG C, glass loses its shape, spreads out into one by a large amount of white
The material of color bubble composition.
Boiling method is used to detect 1000 DEG C, 1100 DEG C, the unit weight of gained glass sample under 1200 DEG C of three heat treatment temperatures,
Method is: by the electronic balance weighing foaming aerial dry weight of devitrified glass, be designated as m1, then after claiming foaming devitrified glass boiling
Buoyant weight in the solution, is designated as m2, aerial weight in wet base after finally claiming foaming devitrified glass to boil, it is designated as m3, it is calculated as follows
Go out the unit weight of devitrified glass that foams.
The unit weight of the glass sample that boiling method records is as shown in table 2 below:
By Fig. 1 and Biao 2 it can be seen that at 1100 DEG C the foam pyroceram unit weight of heat treatment 2h gained minimum, performance is
Good.
Additionally, at the inside glass of gained in 900-1200 DEG C of heat-treatment temperature range in addition to having bubble, also crystallite
Separating out, verify through XRD, sample principal crystalline phase is cordierite (Al4Mg2O18Si5), also segment glass phase, see Fig. 2.
Embodiment 2
The preparation method of foam pyroceram is as follows:
That 1, designs foam pyroceram consists of (wt%): SiO247.74%、Al2O323.76%、MgO14.12 %、
CaO11.09%、Fe2O31.27 %、SO31.24 %、TiO20.78 %；Form according to this glass, calculate feed coal spoil, white clouds
Stone, burning Talcum, the consumption of silica sand, and weigh each raw material by proportioning；
2, use ball mill that colliery powder was milled to 200 mesh sieves, then gangue is mixed by proportioning with other raw materials, through ball
Grinding machine ball milling, crosses 120 mesh sieves；
3, the compound that ball milling sieves is incubated 2h at 1450 DEG C in crucible, is melt into uniform vitreous humour, and gained vitreous humour is again
Through molding, annealing 1h, furnace cooling, obtain bulk glass；
4, bulk glass is placed in high temperature resistance furnace, is raised to 1100 DEG C of insulation 2h from room temperature with the programming rate of 5 DEG C/min, so
Rear stopping is heated, and is cooled to room temperature and obtains product.There is a large amount of bubble to produce inside products obtained therefrom, have crystallite to separate out through XRD checking, main
Crystalline phase is cordierite (Al4Mg2O18Si5), the unit weight using boiling method to record glass is 1.0198 g/cm3。
Embodiment 3
Prepare foam pyroceram according to the method for embodiment 2, except for the difference that: glass consist of (wt%): SiO244.01%、
Al2O323.55%、MgO14.00 %、CaO15.18%、Fe2O31.26 %、SO31.23 %、TiO20.77 %.Inside products obtained therefrom
Having a large amount of bubble to produce, have crystallite to separate out through XRD checking, principal crystalline phase is cordierite (Al4Mg2O18Si5), use boiling method to record
The unit weight of glass is 1.4843 g/cm3。
Embodiment 4
Prepare foam pyroceram according to the method for embodiment 2, except for the difference that: glass consist of (wt%): SiO240.19%、
Al2O323.51%、MgO13.75 %、CaO19.31%、Fe2O31.25 %、SO31.22 %、TiO20.77 %.Inside products obtained therefrom
Having a large amount of bubble to produce, have crystallite to separate out through XRD checking, principal crystalline phase is cordierite (Al4Mg2O18Si5), use boiling method to record
The unit weight of glass is 1.4684g/cm3。
Comparative example 1
Prepare foam pyroceram according to the method for embodiment 2, except for the difference that: glass consist of (wt%): SiO237.82%、
Al2O323.13%、MgO12.94%、CaO23.09%、Fe2O31.16%、SO31.14 %、TiO20.72 %.Products obtained therefrom foaming effect
The poorest, unit weight is big.
Claims (9)
1. a preparation method for foam pyroceram, is characterized in that comprising the following steps:
(1) with gangue, dolomite, burning Talcum, silica sand as raw material, by the consumption of the following glass composition each raw material of calculating:
SiO240-54wt%、Al2O322.5-24 wt%、MgO13.5-14.3 wt%、CaO7-19.5 wt %、Fe2O31.2-1.3 wt
%、SO31.2-1.3 wt %、TiO20.7-0.8 wt %；
(2) weighing each raw material by proportioning, by each raw material pulverizing, mix homogeneously, heating is melt into uniform vitreous humour, vitreous humour warp
Molding, annealing, obtain bulk glass；
(3) bulk glass is risen to 900-1200 DEG C by room temperature, be incubated 0-2h, then cool down, obtain foam pyroceram.
Preparation method the most according to claim 1, is characterized in that: Al2O3Mainly provided by gangue.
Preparation method the most according to claim 1, is characterized in that: gangue content in total raw material is more than 45wt%.
Preparation method the most according to claim 1, is characterized in that: in step (2), after each raw material pulverizing, crosses 120 mesh sieves.
Preparation method the most according to claim 1, is characterized in that: in step (2), and each raw material is heated to 1450 DEG C of insulations
2h, is melt into uniform vitreous humour.
Preparation method the most according to claim 1, is characterized in that: in step (3), bulk glass is risen to 1100 by room temperature
℃。
The most according to claim 1 or 5, preparation method, is characterized in that: in step (3), is incubated 2h.
The most according to claim 1 or 5, preparation method, is characterized in that: in step (3), with the liter less than or equal to 5 DEG C/min
Temperature speed rises to 900-1200 DEG C.
9. the foam pyroceram prepared according to the preparation method of the foam pyroceram according to any one of claim 1-7.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098592A (en) * | 2017-04-07 | 2017-08-29 | 东莞市银通玻璃有限公司 | A kind of method for producing foam pyroceram using high silicon vanadium mine tailing and High-Mg phosphate tailings |
| CN109020243A (en) * | 2018-10-18 | 2018-12-18 | 陕西理工大学 | The method that v-ti magnetite tailing prepares crystallite foam glass |
| CN115108726A (en) * | 2022-08-12 | 2022-09-27 | 西南科技大学 | Porous glass ceramics taking coal gangue as raw material and preparation method thereof |
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| JPS5992944A (en) * | 1982-11-15 | 1984-05-29 | Ihara Chikuro Kogyo Kk | Foam glass |
| CN102815869A (en) * | 2012-09-05 | 2012-12-12 | 北京盛康宁科技开发有限公司 | Foam microcrystalline glass and preparation method thereof |
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2016
- 2016-07-05 CN CN201610520606.7A patent/CN106167356B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5992944A (en) * | 1982-11-15 | 1984-05-29 | Ihara Chikuro Kogyo Kk | Foam glass |
| CN102815869A (en) * | 2012-09-05 | 2012-12-12 | 北京盛康宁科技开发有限公司 | Foam microcrystalline glass and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098592A (en) * | 2017-04-07 | 2017-08-29 | 东莞市银通玻璃有限公司 | A kind of method for producing foam pyroceram using high silicon vanadium mine tailing and High-Mg phosphate tailings |
| CN107098592B (en) * | 2017-04-07 | 2020-06-16 | 东莞市银泰玻璃有限公司 | Method for producing foam glass ceramics by using high-silicon vanadium tailings and high-magnesium phosphorus tailings |
| CN109020243A (en) * | 2018-10-18 | 2018-12-18 | 陕西理工大学 | The method that v-ti magnetite tailing prepares crystallite foam glass |
| CN109020243B (en) * | 2018-10-18 | 2021-08-31 | 陕西理工大学 | Method for preparing microcrystalline foam glass from vanadium-titanium magnet tailings |
| CN115108726A (en) * | 2022-08-12 | 2022-09-27 | 西南科技大学 | Porous glass ceramics taking coal gangue as raw material and preparation method thereof |
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