CN104030567B - Si-Al-Ca microcrystalline glass in series prepared by Low-silica iron ore tailings and method - Google Patents
Si-Al-Ca microcrystalline glass in series prepared by Low-silica iron ore tailings and method Download PDFInfo
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Abstract
The present invention relates to the preparation field of devitrified glass, the Si Al Ca microcrystalline glass in series prepared particularly to Low-silica iron ore tailings and method.By percentage to the quality, it is made up of following raw material: Low-silica iron ore tailings 35% 45%, quartz sand 25% 35%, limestone 12% 20%, soda 4% 6%, sodium nitrate 3% 5%, zinc oxide 2% 7%, brium carbonate 2% 5%, Borax 0.5% 1%, stibium oxide 0.5% 1%；Wherein, described Low-silica iron ore tailings includes following material composition: silicon dioxide less than 35%, aluminium oxide 18% 23%, iron sesquioxide 8% 12%, calcium oxide 8% 10%, titanium oxide 1% 3%, potassium oxide 1% 3%, sodium oxide 2% 3%, surplus is impurity.The Si Al Ca microcrystalline glass in series rupture strength made exceedes the rupture strength of common devitrified glass and also has good bending strength and comprcssive strength.
Description
Technical field
The present invention relates to the preparation field of devitrified glass, the Si-Al-Ca system crystallite glass prepared particularly to Low-silica iron ore tailings
Glass and method.
Background technology
Devitrified glass (CRYSTOE and NEOPARIES) is also known as microcrystalline jade or glass-ceramic.It is comprehensive glass, is one
Planting novel construction material, its formal name used at school is called glass quartz.Devitrified glass and our common glass seem to differ widely.
It has glass and the double grading of pottery, and the atomic arrangement within simple glass is not have well-regulated, and this is also Glass breadks easily
One of reason.And devitrified glass is as pottery, it is made up of crystal, say, that its atomic arrangement is regular.Institute
With, devitrified glass is higher than the brightness of pottery, stronger than glass toughness.
Triple advantages of glass, pottery and lithotome concentrated by devitrified glass, are better than lithotome and pottery, can be used for
Building curtain wall and indoor high-grade decoration, also can do structural material mechanically, the insulant on electronics, electrician, collect on a large scale
Become the baseboard material of circuit, microwave oven flameproof ware, chemical industry and anti-corrosion material and mine high-abrasive material etc..It is to have 21 century to send out
The new material of exhibition future.
Preparing devitrified glass at present mainly utilizes pure industrial chemicals or cullet to prepare, and also has utilization iron tailings to prepare micro-
The successful examples of crystal glass, such as reference paper 1, is limited primarily to tailings of high silicon iron (SiO2＞ 45%), for utilizing low-silicon iron tail
Ore deposit is prepared devitrified glass and is still belonged to blank.
Reference paper:
1. [application publication number] CN102992622A, [Shen Qing Publication day] 2013.03.27, [denomination of invention] Ca-Si-Al
Microcrystalline glass in series preparation method.
Summary of the invention
It is an object of the invention to provide Si-Al-Ca microcrystalline glass in series and method prepared by a kind of Low-silica iron ore tailings, not only
Improve the utilization rate of Low-silica iron ore tailings, the Si-Al-Ca microcrystalline glass in series being simultaneously manufactured has the most anti-folding and flexing resistance
Energy.
The object of the present invention is achieved like this, and Si-Al-Ca microcrystalline glass in series prepared by Low-silica iron ore tailings, with quality hundred
Proportion by subtraction meter, is made up of following raw material:
Low-silica iron ore tailings 35%-45%, quartz sand 25%-35%, limestone 12%-20%, soda 4%-6%, nitric acid
Sodium 3%-5%, zinc oxide 2%-7%, brium carbonate 2%-5%, Borax 0.5%-1%, stibium oxide 0.5%-1%；
Wherein, described Low-silica iron ore tailings includes following material composition: silicon dioxide less than 35%, aluminium oxide 18%-
23%, iron sesquioxide 8%-12%, calcium oxide 8%-10%, titanium oxide 1%-3%, potassium oxide 1%-3%, sodium oxide 2%-
3%, surplus is impurity.
Further, by percentage to the quality, it is made up of following raw material:
Low-silica iron ore tailings 37%-43%, quartz sand 28%-33%, limestone 14%-18%, soda 4.5%-5%, nitre
Acid sodium 3.4%-4.5%, zinc oxide 3%-4%, brium carbonate 3%-4%, Borax 0.6%-0.8%, stibium oxide 0.6%-
0.7%；
Wherein, described Low-silica iron ore tailings includes following material composition: silicon dioxide 30%-35%, aluminium oxide 19%-
21%, iron sesquioxide 9%-11%, calcium oxide 8.5%-9.5%, titanium oxide 1.5%-2.5%, magnesium oxide 2%-3%, oxygen
Change potassium 1.5%-2.5%, sodium oxide 2.5%-2.7%, surplus is impurity.
Prepare the method that Low-silica iron ore tailings prepares Si-Al-Ca microcrystalline glass in series, including following preparation process:
(1) by the Low-silica iron ore tailings of preset ratio, quartz sand, limestone, soda, sodium nitrate, zinc oxide, brium carbonate, boron
Sand, stibium oxide mix homogeneously；
(2) the raw material intensification of mix homogeneously is heated to 1400-1500 DEG C, is incubated 1-1.5 hour, prepares vitreous humour；
(3) by after prepared described vitreous humour clarification, homogenizing, shrend is carried out；
(4) frit after shrend is heated in high temperature furnace 1100-1150 DEG C and carries out crystallization, be incubated 30-35 minute；
(5) furnace cooling after, prepares iron tailings devitrified glass.
Further, in step (2), the described temperature heating up heating is 1460 DEG C, and temperature retention time is 1 hour.
Further, in step (4), described heating-up temperature is 1110-1140 DEG C.
Further, in step (2) and (4), the speed of described heating is 10 DEG C/min.
The Si-Al-Ca microcrystalline glass in series prepared of Low-silica iron ore tailings that the present invention provides and method, the Si-Al-Ca system made
Devitrified glass, with Low-silica iron ore tailings as raw material, fills into corresponding material composition wherein, the preparation method provided by the present invention
The Si-Al-Ca microcrystalline glass in series made can overall crystallize, wollastonite is principal crystalline phase, even grain size, and is uniformly distributed in
Glass mutually in, the rupture strength meansigma methods of devitrified glass reaches 510 (kg/cm2) exceed the rupture strength of common devitrified glass
490(kg/cm2).Also having good bending strength and comprcssive strength, its anti-freezing property is better than common devitrified glass simultaneously.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail.
Si-Al-Ca microcrystalline glass in series prepared by Low-silica iron ore tailings, by percentage to the quality, is made up of following raw material:
Low-silica iron ore tailings 35%-45%, quartz sand 25%-35%, limestone 12%-20%, soda 4%-6%, nitric acid
Sodium 3%-5%, zinc oxide 2%-7%, brium carbonate 2%-5%, Borax 0.5%-1%, stibium oxide 0.5%-1%；
Wherein, described Low-silica iron ore tailings includes following material composition: silicon dioxide less than 35%, aluminium oxide 18%-
23%, iron sesquioxide 8%-12%, calcium oxide 8%-10%, titanium oxide 1%-3%, potassium oxide 1%-3%, sodium oxide 2%-
3%, surplus is impurity.
This programme mainly preparation Si-Al-Ca microcrystalline glass in series, mainly as construction material, utilizes wollastonite for oikocryst
Phase, this crystal can meet the devitrified glass all properties requirement as construction material.
Be mainly composed of silicon dioxide, silicon dioxide in devitrified glass primarily as the formation body of glass, content mistake
Time high, melt temperature is high, thereby increases and it is possible to cause crystallize, when content is relatively low, it may appear that glass lacks gloss, even devitrification phenomenon.Because
But the most not enough containing part of silica content in iron tailings, it is therefore desirable to additionally increase quartz sand to make up silicon dioxide
Component content, it is preferable that the usage percentage of quartz sand is 25%-35%, it is preferable that the degree of quartz sand is
28%-33%.
Aluminium oxide is as Network former, and along with the increase of alumina content, recrystallization temperature has the trend of rising, sintering temperature
Degree district broadens, and surface can be made to produce the defects such as hole point, projection, fracture and significantly reduce, be conducive to strengthening the compactness of devitrified glass.
And the component content of the aluminium oxide in the Low-silica iron ore tailings provided in this programme is higher, reach 18-23%, so,
Need not increase aluminium oxide, directly use iron tailings.
Calcium oxide, as network modifying oxide, along with the increase of calcium oxide content, reduces the activation energy of system, makes
Glass is prone to crystallization, promotes the formation of devitrified glass, and recrystallization temperature broadens, beneficially crystallize.Calcium oxide content increases, crystallization
Granule increases, and the crystallize migration to particle and the flowing to glass phase produce inhibition, cause surface to be difficult to shakeout, make table
The defects such as the hole point of face generation, projection, fracture become apparent from.And containing partial oxidation in the Low-silica iron ore tailings provided in this programme
Calcium component but calcium oxide in formula can not be replaced completely, it is therefore desirable to increase calcium oxide content, the content of this calcium oxide is main
Source is limestone, and as required, the consumption using limestone in this programme is 12%-20%, it is preferable that the percentage of limestone
It is 14%-18% than content.
Soda, mainly provides sodium oxide, and sodium oxide acts the effect fluxed in formula, can improve the formability of glass
Can, generally higher than 4%, when being up to 9% such as content, in sample, crystal content significantly reduces so that crystalline phase is engaged journey mutually with glass
Degree reduces, and causes devitrified glass bending strength to reduce.Meanwhile, process costs can also be increased.So, the soda provided in this programme
Content be 4-6%, it is preferable that its content is 4.5%-5%.
Zinc oxide, the effect played in formula is to reduce the point of incipient sintering, initial recrystallization temperature and final shakeouing
Temperature, generally 2%-4%.In the scheme that the present invention provides, the degree of zinc oxide is in the range of 2%-7% is somebody's turn to do
?.Preferably, the content of zinc oxide is 3%-4%.
Borax, not only acts as the effect fluxed in formula, it is possible to reduces the temperature of glass melting, more importantly improves
The glossiness of product.Too much kiln, generally 0.5%-1% should not can be corroded in actual production.This programme uses Borax
Consumption be 0.5%-1%.Preferably, its consumption is 0.6%-0.8%.
Sodium nitrate and stibium oxide, as clarifier, contribute to the clarification of vitreous humour, improve the quality of devitrified glass.
Brium carbonate is essentially the same with the effect of calcium oxide, primarily serves the effect of constituent adjustment in formula, can reduce
The fusing of the viscosity of vitreous humour, beneficially glass, is less than sodium oxide to the adverse effect of glass properties.
In order to improve the quality of the devitrified glass made, it is preferable that by percentage to the quality, it is made up of following raw material:
Low-silica iron ore tailings 37%-43%, quartz sand 28%-33%, limestone 14%-18%, soda 4.5%-5%, nitre
Acid sodium 3.4%-4.5%, zinc oxide 3%-4%, brium carbonate 3%-4%, Borax 0.6%-0.8%, stibium oxide 0.6%-
0.7%；
Wherein, described Low-silica iron ore tailings includes following material composition: silicon dioxide 30%-35%, aluminium oxide 19%-
21%, iron sesquioxide 9%-11%, calcium oxide 8.5%-9.5%, titanium oxide 1.5%-2.5%, magnesium oxide 2%-3%, oxygen
Changing potassium 1.5%-2.5%, sodium oxide 2.5%-2.7%, surplus is impurity.
Prepare the method that Low-silica iron ore tailings prepares Si-Al-Ca microcrystalline glass in series, including following preparation process:
(1) by the Low-silica iron ore tailings of preset ratio, quartz sand, limestone, soda, sodium nitrate, zinc oxide, brium carbonate, boron
Sand, stibium oxide mix homogeneously；
(2) the raw material intensification of mix homogeneously is heated to 1400-1500 DEG C, is incubated 1-1.5 hour, prepares vitreous humour；
Raw material is heated to 1400-1500 DEG C i.e. can be the most melted, if improving temperature again, can increase process costs,
And it is more to consume energy.Homo-effect and the compactness of the vitreous humour made in this temperature range are the highest, and bubble-free.
(3) by after prepared described vitreous humour clarification, homogenizing, shrend is carried out；
(4) frit after shrend is heated in high temperature furnace 1100-1150 DEG C and carries out crystallization, be incubated 30-35 minute；
Crystallization temperature is too high, and process costs is high, and it is more to consume energy.Meanwhile, easily cause coarse grains, reduce product
Quality.Temperature retention time is unsuitable long, 30-35 minute, it is preferable that temperature retention time is 30 minutes.
(5) furnace cooling after, prepares iron tailings devitrified glass.
In order to reduce the impurity content in vitreous humour, it is preferable that in step (2), the described temperature heating up heating is 1460
DEG C, temperature retention time is 1 hour.
In order to improve process efficiency, cost is in controlled range, it is preferable that in step (4), described heating-up temperature is
1110-1140℃。
In order to improve the quality of product, it is preferable that in step (2) and (4), the speed of described heating is 10 DEG C/min.
The Si-Al-Ca microcrystalline glass in series prepared of Low-silica iron ore tailings that the present invention provides and method, the Si-Al-Ca system made
Devitrified glass, with Yuanqu, Shanxi Low-silica iron ore tailings as raw material, is filled into corresponding material composition wherein, is provided by the present invention
The Si-Al-Ca microcrystalline glass in series that preparation method is made can overall crystallize, wollastonite is main metallographic, even grain size, and all
Even be distributed in glass mutually in, the rupture strength meansigma methods of devitrified glass reaches 510 (kg/cm2) exceed common devitrified glass
Rupture strength 490 (kg/cm2).Simultaneously also having good bending strength and comprcssive strength, its anti-freezing property is better than common micro-
Crystal glass.
Below, use embodiment to further describe the present invention, but the present invention is not limited to these embodiments.
Embodiment 1
By Low-silica iron ore tailings 35%, quartz sand 35%, limestone 15%, soda 4%, sodium nitrate 3%, zinc oxide 4%, carbon
Acid barium 2%, Borax 1%, stibium oxide 1% mix homogeneously；Intensification is heated to 1400 DEG C, and heating rate is 10 DEG C/min, and insulation 1 is little
Time, prepare vitreous humour, after clarification, homogenizing, carry out shrend；By the speed with 10 DEG C/min in high temperature furnace of the frit after shrend
It is heated to 1100 DEG C and carries out crystallization, furnace cooling after being incubated 30 minutes, prepare iron tailings devitrified glass.
Embodiment 2
By Low-silica iron ore tailings 38%, quartz sand 30%, limestone 17%, soda 5%, sodium nitrate 4%, zinc oxide 3%, carbon
Acid barium 2%, Borax 0.4%, stibium oxide 0.6% mix homogeneously；Intensification is heated to 1500 DEG C, and heating rate is 10 DEG C/min, protects
Temperature 1.5 hours, prepares vitreous humour, after clarification, homogenizing, carries out shrend；By the frit after shrend in high temperature furnace with 10 DEG C/
The speed of min is heated to 1150 DEG C and carries out crystallization, furnace cooling after being incubated 35 minutes, prepares iron tailings devitrified glass.
Embodiment 3
By Low-silica iron ore tailings 40%, quartz sand 30%, limestone 15%, soda 4.5%, sodium nitrate 3.4%, zinc oxide
3%, brium carbonate 3%, Borax 0.6%, stibium oxide 0.5% mix homogeneously；Intensification is heated to 1460 DEG C, and heating rate is 10 DEG C/
Min, is incubated 1 hour, prepares vitreous humour, after clarification, homogenizing, carries out shrend；By the frit after shrend in high temperature furnace with 10
DEG C/speed of min is heated to 1130 DEG C and carries out crystallization, furnace cooling after being incubated 30 minutes, prepares iron tailings devitrified glass.
Embodiment 4
By Low-silica iron ore tailings 45%, quartz sand 28%, limestone 12%, soda 5%, sodium nitrate 4.5%, zinc oxide 2%,
Brium carbonate 2%, Borax 0.8%, stibium oxide 0.7% mix homogeneously；Intensification is heated to 1460 DEG C, and heating rate is 10 DEG C/min,
It is incubated 1.5 hours, prepares vitreous humour, after clarification, homogenizing, carry out shrend；By the frit after shrend in high temperature furnace with 10 DEG C/
The speed of min is heated to 1130 DEG C and carries out crystallization, furnace cooling after being incubated 35 minutes, prepares iron tailings devitrified glass.
The Si-Al-Ca microcrystalline glass in series that the scheme utilizing embodiment 1-4 to provide is made contrasts with common devitrified glass,
Its performance data is added up such as table 1:
Table 1
| Performance/material (unit) | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Ordinary microcrystalline glass |
| Bending strength (MPa) | 45.4 | 45.1 | 45.3 | 45.2 | 40-50 |
| Comprcssive strength (MPa) | 370 | 365 | 372 | 370 | 341.3 |
| Impact strength (cm) | 33cm (impulsive motion point) | 32 | 30 | 31 | 30 |
| Anti-folding (kg/cm2) | 510 | 508 | 512 | 510 | 490 |
| Freeze proof (%) | 0.028 | 0.026 | 0.025 | 0.027 | 0.03 |
| Morse hardness | 6.5 | 6.3 | 6.4 | 6.6 | 6 |
| Proportion | 2.7 | 2.7 | 2.7 | 2.7 | 2.7 |
| Acid resistance (1%H2SO4) | 0.07 | 0.07 | 0.07 | 0.07 | 0.08 |
| Water absorption rate (%) | 0 | 0 | 0 | 0 | 0 |
| Alkali resistance (1%NaOH) | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 |
Experimental data from table 1 is it can be seen that the Si-Al-Ca system made of four embodiments being provided by the present invention
Devitrified glass, its comprcssive strength and rupture strength be substantially better than Ordinary microcrystalline glass, meanwhile, also have excellent bending strength and
Impact strength.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, that is made any repaiies
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (5)
1. the Si-Al-Ca microcrystalline glass in series that prepared by Low-silica iron ore tailings, it is characterised in that by percentage to the quality, by following raw material
Make:
Low-silica iron ore tailings 35%-45%, quartz sand 25%-35%, limestone 12%-20%, soda 4%-6%, sodium nitrate
3%-5%, zinc oxide 2%-7%, brium carbonate 2%-5%, Borax 0.5%-1%, stibium oxide 0.5%-1%；
Wherein, described Low-silica iron ore tailings includes following material composition: silicon dioxide less than 35%, aluminium oxide 18%-23%, three
Aoxidize two ferrum 8%-12%, calcium oxide 8%-10%, titanium oxide 1%-3%, potassium oxide 1%-3%, sodium oxide 2%-3%, remaining
Amount is impurity.
2. the method that preparation Low-silica iron ore tailings described in claim 1 prepares Si-Al-Ca microcrystalline glass in series, it is characterised in that bag
Include following preparation process:
(1) by the Low-silica iron ore tailings of preset ratio, quartz sand, limestone, soda, sodium nitrate, zinc oxide, brium carbonate, Borax, oxygen
Change antimony mix homogeneously；
(2) the raw material intensification of mix homogeneously is heated to 1400-1500 DEG C, is incubated 1-1.5 hour, prepares vitreous humour；
(3) by after prepared described vitreous humour clarification, homogenizing, shrend is carried out；
(4) frit after shrend is heated in high temperature furnace 1100-1150 DEG C and carries out crystallization, be incubated 30-35 minute；
(5) furnace cooling after, prepares iron tailings devitrified glass.
The most according to claim 2 preparing the method that Low-silica iron ore tailings prepares Si-Al-Ca microcrystalline glass in series, its feature exists
In:
In step (2), the described temperature heating up heating is 1460 DEG C, and temperature retention time is 1 hour.
The most according to claim 2 preparing the method that Low-silica iron ore tailings prepares Si-Al-Ca microcrystalline glass in series, its feature exists
In:
In step (4), described heating-up temperature is 1110-1140 DEG C.
The most according to claim 2 preparing the method that Low-silica iron ore tailings prepares Si-Al-Ca microcrystalline glass in series, its feature exists
In:
In step (2) and (4), the speed of described heating is 10-15 DEG C/min.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072398A (en) * | 1992-09-28 | 1993-05-26 | 唐山市古冶玻璃制品厂 | Nucleated glass granite dalle and production technique |
| CN101817640A (en) * | 2009-01-24 | 2010-09-01 | 北京清迈信息材料有限公司 | Method for manufacturing microlite by using high-silicon iron tailings |
| CN101857367A (en) * | 2010-06-23 | 2010-10-13 | 浮山县晋盛新型建筑材料有限责任公司 | Black glass ceramic and production method thereof |
| CN101967043A (en) * | 2009-07-28 | 2011-02-09 | 鞍钢集团矿业公司 | Glass ceramics made from high silicon iron tailings and manufacturing method thereof |
-
2014
- 2014-06-27 CN CN201410302870.4A patent/CN104030567B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072398A (en) * | 1992-09-28 | 1993-05-26 | 唐山市古冶玻璃制品厂 | Nucleated glass granite dalle and production technique |
| CN101817640A (en) * | 2009-01-24 | 2010-09-01 | 北京清迈信息材料有限公司 | Method for manufacturing microlite by using high-silicon iron tailings |
| CN101967043A (en) * | 2009-07-28 | 2011-02-09 | 鞍钢集团矿业公司 | Glass ceramics made from high silicon iron tailings and manufacturing method thereof |
| CN101857367A (en) * | 2010-06-23 | 2010-10-13 | 浮山县晋盛新型建筑材料有限责任公司 | Black glass ceramic and production method thereof |
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