CN106167356B - A kind of preparation method and products obtained therefrom of foam pyroceram - Google Patents
A kind of preparation method and products obtained therefrom of foam pyroceram Download PDFInfo
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- CN106167356B CN106167356B CN201610520606.7A CN201610520606A CN106167356B CN 106167356 B CN106167356 B CN 106167356B CN 201610520606 A CN201610520606 A CN 201610520606A CN 106167356 B CN106167356 B CN 106167356B
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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
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- 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)
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Abstract
The present invention relates to a kind of preparation method of foam pyroceram and products obtained therefrom, step is：Using gangue, dolomite, talcum, silica sand are burnt as raw material, and the dosage of each raw material is calculated by glass composition；Each raw material is weighed according to the ratio, and each raw material is crushed, is uniformly mixed, heating melting is formed, annealed at uniform glass metal, glass metal, and bulk glass is obtained；Bulk glass is risen to 900-1200 DEG C by room temperature, 0-2h is kept the temperature, then cools down, obtain foam pyroceram.The present invention provides new idea and method using Coal Refuse as primary raw material, for the utilization of gangue, turns waste into wealth, has achieved the purpose that curb environmental pollution while economizing on resources.Raw material is made bulk glass and then directly heats foaming by the present invention, is not necessarily to glass breaking, without addition various additives, simplify the preparation process of foam pyroceram, production cost is reduced simultaneously, products obtained therefrom good quality can be in building field wide popularization and application.
Description
Technical field
The present invention relates to a kind of preparation method of foam pyroceram and resulting foam pyrocerams, and in particular to a kind of
Using solid waste as primary raw material, in the case where foaming agent is not added voluntarily foaming prepare foam pyroceram method and
Product made from this method belongs to glass and solid waste and utilizes technical field.
Background technique
The recycling of solid waste both economized on resources, and reduces entreprise cost, and protect environment, meets Resources for construction saving
The requirement of type society and sustainable development.Construction material is produced using solid waste（Such as foam glass）It 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
Occupy significant proportion in amount.Gangue, which is stacked, occupies a large amount of soils, and causes environmental pollution.Gangue can be used for generating electricity, make
Sintered hollow block produces the chemical products such as cement and production crystal aluminum chloride instead of clay, also has and is prepared using gangue
The report of glass material, such as：It is micro- that University of Science & Technology, Beijing king long queue et al. using gangue and iron tailings is prepared for calcium and magnesium aluminium silicon systems
Crystal glass；Song Jianjun et al. is prepared for β-wollastonite phase devitrified glass using gangue as primary raw material, using sintering process；Li Yuhua
Et al. using cullet and gangue as primary raw material, Novel microcrystalline foam glass is prepared for using sintering process.These researchs are coal
The utilization of spoil provides a new direction, not only has an economic benefit, and there are also certain environmental benefits.
Foam pyroceram is that have the function of heat-insulated, sound absorption, fire prevention etc., is a kind of novel light construction material and decoration material
Material.The production master of usual foam devitrified glass to be used is sintering process, and the main process of sintering process is：By quantitative broken glass
Glass, foaming agent, modified additive and promotor etc. form batch by finely divided be uniformly mixed, batch are put into spy
In fixed mold, glass is prepared using techniques such as preheating, sintering, foaming, annealing, since glass powder sintering process would generally be sent out
Raw crystallization, therefore resulting glass is often foam pyroceram.The production technology has the following disadvantages：Process is complicated, work
It measures very big；Need the mold of special high temperature resistant and anti-chilling；Annealing time is long；It needs to reprocess after product firing.
Summary of the invention
For deficiency existing for existing foam pyroceram preparation process, the present invention provides a kind of foam pyrocerams
Preparation method and resulting foam pyroceram, this method realize the recycling benefit of waste using solid waste as primary raw material
With in addition, it is not necessary that by glass breaking, raw material type is few, and preparation process is simple, at low cost in preparation process.
The present invention adds the raw material of the composition glass such as dolomite, burning talcum, silica sand using gangue as primary raw material,
By the collocation of each raw material, each raw material is directly prepared into bulk glass when preparation, bulk glass directly carries out hot place without crushing
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 specific technical solution is as follows：
A kind of preparation method of foam pyroceram, this approach includes the following steps：
（1）Using gangue, dolomite, talcum, silica sand are burnt as raw material, and the dosage of each raw material is calculated by following glass composition：
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）Each raw material is weighed according to the ratio, and each raw material is crushed, is uniformly mixed, heating melting is at uniform glass metal, glass
Liquid is formed, is annealed, and bulk glass is obtained；
（3）Bulk glass is risen to 900-1200 DEG C by room temperature, 0-2h is kept the temperature, then cools down, obtain foam pyroceram.
In above-mentioned preparation method, it is with gangue to improve waste utilization amount according to each raw material of composition selection of glass
Primary raw material, i.e. glass ingredient are first provided by gangue as far as possible, if gangue is unable to satisfy glass ingredient content requirement, then
Required content is supplemented to dolomite, burning talcum, silica sand.Al when selecting raw material dosage, in glass2O3Mainly by gangue
It provides, the SiO in glass2By gangue, talcum and silica sand offer are burnt, the MgO in glass is mainly mentioned by burning talcum, dolomite
For the CaO in glass is mainly provided by dolomite, the Fe in glass2O3And other ingredients are 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
Content of the stone in total raw material is greater than 45wt%.
Above-mentioned steps（2）In, each raw material can be crushed by ball mill, be mixed.After each raw material crushes, 120 meshes are crossed, it will
The big raw material of particle screens out.
Above-mentioned steps（2）In, each raw material is heated to 1450 DEG C of heat preservation 2h, is melt into uniform glass metal.Gained glass
Liquid forms according to common process, anneals, and obtains bulk glass, i.e. both bulk glasses.
Above-mentioned steps（3）In, bulk glass is directly heat-treated, heat treatment step is:By bulk glass by room temperature
It is warming up to 900-1200 DEG C, and keeps the temperature 0-2h at this temperature, when keeping the temperature 0h, indicates bulk glass rising to 900- by room temperature
1200 DEG C, not warm direct cooling.The present invention is not necessarily to glass crushing, tabletting, sintering simplifying process flow.Preferably,
Bulk glass is warming up to 1100 DEG C.
Above-mentioned steps（3）In, it is warming up to 900-1200 DEG C of heat preservation 0-2h, preferably 2h.
Above-mentioned steps（3）In, 900-1200 DEG C is risen to the heating rate less than or equal to 5 DEG C/min.
Resulting glass is foam pyroceram according to the method described above, which has a large amount of bubbles, and has crystallite to deposit
Stablize in, property, has a good application prospect.Foam pyroceram obtained also protects model in the present invention according to the method described above
Within enclosing.
The present invention has the following advantages that：
1, the present invention provides new thinking and side using Coal Refuse as primary raw material for the utilization of gangue
Method, the content of gangue advantageously reduces the stockpiling of gangue 45% or more in raw material, realizes waste utilization, change give up into
Treasured has achieved the purpose that curb environmental pollution while economizing on resources, and added value of product is high；
2, raw material is made bulk glass and then directly heats foaming by the present invention, is not necessarily to by glass breaking, without addition
Various additives, simplify the preparation process of foam pyroceram, while reducing production cost.
3, present invention gained foam pyroceram is black to canescence, and inside has a large amount of bubbles, and product quality is excellent,
The crystallite foam glass can be used as heat-insulated, sound absorption, moisture-proof, fire proofing material, be a kind of light high-strength building material of superior performance
And ornament materials, it can be in building field wide popularization and application.
Detailed description of the invention
The sectional view of 1 gained glass sample of Fig. 1 embodiment.
The XRD diagram of 1 gained glass sample of Fig. 2 embodiment.
Specific embodiment
In the following, the present invention is further explained and is illustrated by specific embodiment, it should be appreciated that, under state
It is bright to be intended merely to explain the present invention, its content is not defined.
Each raw material of the present invention can be bought in the market, in following embodiments, the main chemical compositions of each raw material used
It as shown in table 1 below, is to burn to lose and/or decompose the gaseous product generated less than 100% part.
Embodiment 1
The preparation method of foam pyroceram is as follows：
1, the group for designing foam pyroceram becomes（wt%）： SiO253.27%、Al2O322.93%、MgO13.63 %、
CaO7%、Fe2O31.22 %、SO31.20 %、TiO20.75 %；It is formed according to the glass, calculates raw material gangue, dolomite, burning
The dosage of talcum, silica sand, and each raw material is weighed according to the ratio；
2, coal gangue powder was milled to by 200 meshes using ball mill, then mixed gangue according to the ratio with other raw materials,
Through ball mill ball milling, 120 meshes are crossed；
3, the mixture of ball milling sieving is melt into uniform glass metal, gained glass in 1450 DEG C of heat preservation 2h in crucible
Liquid formed again, the 1h that anneals, furnace cooling, obtains bulk glass；
4, bulk glass is placed in high temperature resistance furnace, from room temperature with the heating 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, this temperature keep the temperature respectively 0h, 1h,
2h is heat-treated, and is stopped heating after heat treatment, is cooled to room temperature to obtain glass product.
As can be seen that the foaming effect of glass obtained by heat treatment 2h is better than 1h in experimentation, glass obtained by heat treatment 1h
Foaming effect it is better than 0h, be heat-treated 2h foam more horn of plenty, therefore the preferred 2h of heat treatment time.Heat treatment temperature is 800 DEG C
When, inside glass is almost without bubble formation, when within the scope of 900-1100 DEG C, as the temperature rises, the bubble of inside glass
Measure into raising trend.Fig. 1 is that glass obtained by 2h is heat-treated at 800 DEG C, 900 DEG C, 1000 DEG C, 1050 DEG C, 1100 DEG C, 1200 DEG C
Cross-section diagram, it can be seen from the figure that when temperature is 800 DEG C, the bubble of inside glass almost without；When temperature is raised to 900
DEG C when, there is bubble in inside glass, and internal dimmed；When temperature is raised to 1000 DEG C, glass surface starts to whiten, and inside occurs
More bubbles, volume become larger；When temperature is raised to 1100 DEG C, there are a large amount of bubbles in inside glass, and glass volume expansion is maximum, close
Degree is smaller than water can be floated up in the water surface；When temperature is raised to 1200 DEG C, glass loses its shape, and booth is at one by a large amount of white
The substance of color bubble composition.
Using boiling method detect 1000 DEG C, 1100 DEG C, under 1200 DEG C of three heat treatment temperatures gained glass sample bulk density,
Method is：With the electronic balance weighing foaming aerial dry weight of devitrified glass, it is denoted as m1, then claim to foam after devitrified glass boils
Buoyant weight in the solution, is denoted as m2, finally claim foaming devitrified glass to boil rear aerial weight in wet base, be denoted as m3, it is calculated as follows
The bulk density of foaming devitrified glass out.
The bulk density for the glass sample that boiling method measures is as shown in table 2 below：
By Fig. 1 and table 2 as can be seen that being heat-treated the resulting foam pyroceram bulk density minimum of 2h, property at 1100 DEG C
It can be best.
In addition, resulting inside glass is other than having bubble in 900-1200 DEG C of heat-treatment temperature range, there are also crystallites
It is precipitated, is verified through XRD, sample principal crystalline phase is cordierite（Al4Mg2O18Si5）, there are also segment glass phases, see Fig. 2.
Embodiment 2
The preparation method of foam pyroceram is as follows：
1, the group for designing foam pyroceram becomes（wt%）： SiO247.74%、Al2O323.76%、MgO14.12 %、
CaO11.09%、Fe2O31.27 %、SO31.24 %、TiO20.78 %；It is formed according to the glass, calculates raw material gangue, white clouds
Stone, the dosage for burning talcum, silica sand, and each raw material is weighed according to the ratio；
2, coal gangue powder was milled to by 200 meshes using ball mill, then mixed gangue according to the ratio with other raw materials,
Through ball mill ball milling, 120 meshes are crossed；
3, the mixture of ball milling sieving is melt into uniform glass metal, gained glass in 1450 DEG C of heat preservation 2h in crucible
Liquid formed again, the 1h that anneals, furnace cooling, obtains bulk glass；
4, bulk glass is placed in high temperature resistance furnace, is raised to 1100 DEG C of heat preservations from room temperature with the heating rate of 5 DEG C/min
Then 2h stops heating, is cooled to room temperature to obtain product.There are a large amount of bubbles to generate inside products obtained therefrom, has crystallite analysis through XRD verifying
Out, principal crystalline phase is cordierite（Al4Mg2O18Si5）, boiling method is used to measure the bulk density of glass as 1.0198 g/cm3。
Embodiment 3
Foam pyroceram is prepared according to the method for embodiment 2, unlike：The group of glass becomes（wt%）：
SiO244.01%、Al2O323.55%、MgO14.00 %、CaO15.18%、Fe2O31.26 %、SO31.23 %、TiO20.77 %.Institute
Obtaining interiors of products has a large amount of bubbles to generate, and has crystallite precipitation through XRD verifying, principal crystalline phase is cordierite（Al4Mg2O18Si5）, use
The bulk density that boiling method measures glass is 1.4843 g/cm3。
Embodiment 4
Foam pyroceram is prepared according to the method for embodiment 2, unlike：The group of glass becomes（wt%）：
SiO240.19%、Al2O323.51%、MgO13.75 %、CaO19.31%、Fe2O31.25 %、SO31.22 %、TiO20.77 %.Institute
Obtaining interiors of products has a large amount of bubbles to generate, and has crystallite precipitation through XRD verifying, principal crystalline phase is cordierite（Al4Mg2O18Si5）, use
The bulk density that boiling method measures glass is 1.4684g/cm3。
Comparative example 1
Foam pyroceram is prepared according to the method for embodiment 2, unlike：The group of glass becomes（wt%）：
SiO237.82%、Al2O323.13%、MgO12.94%、CaO23.09%、Fe2O31.16%、SO31.14 %、TiO20.72 %.Gained
Product foaming effect is poor, and bulk density is big.
Claims (8)
1. a kind of preparation method of foam pyroceram, it is characterized in that including the following steps：
（1）Using gangue, dolomite, talcum, silica sand are burnt as raw material, and the dosage of each raw material is calculated by following glass composition：
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）Each raw material is weighed according to the ratio, each raw material is crushed, is uniformly mixed, and heating melting is at uniform glass metal, glass metal warp
Molding, annealing, obtain bulk glass；
（3）Bulk glass is risen to 900-1200 DEG C by room temperature, 0-2h is kept the temperature, then cools down, obtain foam pyroceram；Gangue
Content in total raw material is greater than 45wt%.
2. preparation method according to claim 1, it is characterized in that：Al2O3Mainly provided by gangue.
3. preparation method according to claim 1, it is characterized in that：Step（2）In, after each raw material crushes, cross 120 meshes.
4. preparation method according to claim 1, it is characterized in that：Step（2）In, each raw material is heated to 1450 DEG C of heat preservations
2h is melt into uniform glass metal.
5. preparation method according to claim 1, it is characterized in that：Step（3）In, bulk glass rises to 1100 by room temperature
℃。
6. preparation method according to claim 1 or 4, it is characterized in that：Step（3）In, keep the temperature 2h.
7. preparation method according to claim 1 or 4, it is characterized in that：Step（3）In, to be less than or equal to the liter of 5 DEG C/min
Warm speed rises to 900-1200 DEG C.
8. foam pyroceram made from the preparation method according to foam pyroceram of any of claims 1-7.
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| 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 |
| CN115108726B (en) * | 2022-08-12 | 2023-05-12 | 西南科技大学 | Porous microcrystalline glass using coal gangue as raw material and preparation method thereof |
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| Title |
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| 微晶泡沫玻璃与固体废弃物的循环利用;张雪峰等;《中国陶瓷》;20120630;第48卷(第6期);第55页右栏第1段~第56页左栏第1段 * |
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