CN104030567A - Si-Al-Ca serial microcrystalline glass prepared from low silicon iron tailings and method - Google Patents
Si-Al-Ca serial microcrystalline glass prepared from low silicon iron tailings and method Download PDFInfo
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Abstract
The invention relates to the field of preparation of microcrystalline glass and particularly relates to Si-Al-Ca serial microcrystalline glass prepared from low silicon iron tailings and a method. The microcrystalline glass is prepared from the following raw materials in percentage by weight: 35-45% of low silicon iron tailings, 25-35% of quartz sands, 12-20% of limestones, 4-6% of sodium carbonate, 3-5% of sodium nitrate, 2-7% of zinc oxide, 2-5% of barium carbonate, 0.5-1% of borax and 0.5-1% of antimony oxide, wherein the low silicon iron tailings comprise the following raw materials in percentage by weight: less than 35% of silicon dioxide, 18-23% of aluminum oxide, 8-12% of iron sesquioxide, 8-10% of calcium oxide, 1-3% of titanium oxide, 1-3% of potassium oxide, 2-3% of sodium oxide and the balance of impurities. The breaking strength of the prepared Si-Al-Ca serial microcrystalline glass exceeds that of common microcrystalline glass and further has good bending strength and compressive strength.
Description
Technical field
The present invention relates to the preparation field of devitrified glass, Si-Al-Ca microcrystalline glass in series and method that particularly prepared by low-silicon iron mine tailing.
Background technology
Devitrified glass (CRYSTOE and NEOPARIES) claim again microcrystalline jade or glass-ceramic.Being comprehensive glass, is a kind of novel material of construction, and its formal name used at school is called glass quartz.Devitrified glass and our common glass seem to differ widely.It has glass and ceramic dual nature, and the atomic arrangement of simple glass inside is not have well-regulatedly, and this is also one of reason of Glass breadks easily.And devitrified glass is as pottery, by crystal composition, that is to say, its atomic arrangement is regular.So devitrified glass is higher than ceramic brightness, stronger than glass toughness.
Devitrified glass has been concentrated triple advantages of glass, pottery and lithotome, be better than lithotome and pottery, can be used for building curtain wall and indoor high-grade decoration, also can do structured material mechanically, insulating material on electronics, electrician, baseboard material, microwave oven flameproof ware, chemical industry and impregnating material and the mine high-abrasive material etc. of large-scale integrated circuit.It is type material 21 century with development prospect.
Prepare at present devitrified glass and mainly utilize pure industrial chemicals or glass cullet preparation, also have the successful example that uses glass-ceramics Fabrication with Iron Tailings, as reference paper 1, be mainly limited to tailings of high silicon iron (SiO
2> 45%), also belong to blank for utilizing low-silicon iron mine tailing to prepare devitrified glass.
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
The Si-Al-Ca microcrystalline glass in series and the method that the object of the present invention is to provide a kind of low-silicon iron mine tailing to prepare, not only improved the utilization ratio of low-silicon iron mine tailing, and the Si-Al-Ca microcrystalline glass in series of simultaneously making has anti-folding and anti-bending strength well.
The object of the present invention is achieved like this, and Si-Al-Ca microcrystalline glass in series prepared by low-silicon iron mine tailing by percentage to the quality, is made up of following raw material:
Low-silicon iron mine tailing 35%-45%, quartz sand 25%-35%, Wingdale 12%-20%, soda ash 4%-6%, SODIUMNITRATE 3%-5%, zinc oxide 2%-7%, barium carbonate 2%-5%, borax 0.5%-1%, weisspiessglanz 0.5%-1%;
Wherein, described low-silicon iron mine tailing comprises following material composition: silicon-dioxide below 35%, aluminum oxide 18%-23%, ferric oxide 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, made by following raw material:
Low-silicon iron mine tailing 37%-43%, quartz sand 28%-33%, Wingdale 14%-18%, soda ash 4.5%-5%, SODIUMNITRATE 3.4%-4.5%, zinc oxide 3%-4%, barium carbonate 3%-4%, borax 0.6%-0.8%, weisspiessglanz 0.6%-0.7%;
Wherein, described low-silicon iron mine tailing comprises following material composition: silicon-dioxide 30%-35%, aluminum oxide 19%-21%, ferric oxide 9%-11%, calcium oxide 8.5%-9.5%, titanium oxide 1.5%-2.5%, magnesium oxide 2%-3%, potassium oxide 1.5%-2.5%, sodium oxide 2.5%-2.7%,, surplus is impurity.
Prepare low-silicon iron mine tailing and prepare the method for Si-Al-Ca microcrystalline glass in series, comprise following preparation process:
(1) low-silicon iron mine tailing, quartz sand, Wingdale, soda ash, SODIUMNITRATE, zinc oxide, barium carbonate, borax, the weisspiessglanz of preset ratio are mixed;
(2) raw material mixing is heated up and is heated to 1400-1500 DEG C, insulation 1-1.5 hour, makes glass metal;
(3) by after the described glass metal clarification making, homogenizing, carry out shrend;
(4) frit after shrend is heated to 1100-1150 DEG C in High Temperature Furnaces Heating Apparatus and carries out crystallization, insulation 30-35 minute;
(5) furnace cooling afterwards, makes iron tailings devitrified glass.
Further, in step (2), the temperature of described intensification heating is 1460 DEG C, and soaking time is 1 hour.
Further, in step (4), described Heating temperature is 1110-1140 DEG C.
Further, in step (2) and (4), the speed of described heating is 10 DEG C/min.
Si-Al-Ca microcrystalline glass in series and method prepared by low-silicon iron mine tailing provided by the invention, the Si-Al-Ca microcrystalline glass in series of making is taking low-silicon iron mine tailing as raw material, fill into therein corresponding material composition, the Si-Al-Ca microcrystalline glass in series of making by preparation method provided by the invention can overall crystallization, wollastonite is principal crystalline phase, even grain size, and be uniformly distributed in glassy phase, the folding strength mean value of devitrified glass reaches 510 (kg/cm
2) exceed the folding strength 490 (kg/cm of common devitrified glass
2).Also have good bending strength and ultimate compression strength, its anti-freezing property is better than common devitrified glass simultaneously.
Embodiment
Below by specific embodiment, the present invention is described in further detail.
Si-Al-Ca microcrystalline glass in series prepared by low-silicon iron mine tailing, by percentage to the quality, made by following raw material:
Low-silicon iron mine tailing 35%-45%, quartz sand 25%-35%, Wingdale 12%-20%, soda ash 4%-6%, SODIUMNITRATE 3%-5%, zinc oxide 2%-7%, barium carbonate 2%-5%, borax 0.5%-1%, weisspiessglanz 0.5%-1%;
Wherein, described low-silicon iron mine tailing comprises following material composition: silicon-dioxide below 35%, aluminum oxide 18%-23%, ferric oxide 8%-12%, calcium oxide 8%-10%, titanium oxide 1%-3%, potassium oxide 1%-3%, sodium oxide 2%-3%, surplus is impurity.
This programme is mainly preparation Si-Al-Ca microcrystalline glass in series, mainly as material of construction, utilizes wollastonite for principal crystalline phase, and this crystal can meet all properties requirement of devitrified glass as material of construction.
Main component is silicon-dioxide, and silicon-dioxide is mainly the organizer as glass in devitrified glass, and when too high levels, melt temperature is high, and may cause crystallization, when content is lower, there will be glass to lack gloss, even devitrification phenomenon.Because but it is not enough again to contain part silicon-dioxide content in iron tailings, so, need extra increase quartz sand to make up the component content of silicon-dioxide, preferably, the usage percentage of quartz sand is 25%-35%, and preferably, the degree of quartz sand is 28%-33%.
Aluminum oxide is as Network former, and along with the increase of alumina content, recrystallization temperature has the trend of rising, and sintering temperature district broadens, and can make surface produce the defects such as hole point, projection, fracture and obviously reduce, and is conducive to strengthen the compactness of devitrified glass.
And the component content of aluminum oxide in the low-silicon iron mine tailing providing in this programme is higher, reaches 18-23%, so, do not need to increase aluminum oxide, directly use iron tailings.
Calcium oxide, as network modifying oxide, along with the increase of calcium oxide content, has reduced the activation energy of system, makes glass be easy to crystallization, has promoted the formation of devitrified glass, and recrystallization temperature broadens, and is conducive to crystallization.Calcium oxide content increases, and crystalline particle increases, and the migration of crystallization to particle and the mobile generation inhibition to glassy phase, cause surface to be difficult to shakeout, and makes the defects such as the surperficial hole point producing, projection, fracture more obvious.And in the low-silicon iron mine tailing providing in this programme, contain partial oxidation calcium component but can not replace calcium oxide in formula completely, so, need to increase the content of calcium oxide, the content main source of this calcium oxide is Wingdale, as required, the consumption that uses Wingdale in this programme is 12%-20%, and preferably, the degree of Wingdale is 14%-18%.
Soda ash, is mainly to provide sodium oxide, and sodium oxide plays a part to flux in formula, can improve the forming property of glass, generally be greater than 4%, if content is up to 9% time, in sample, crystal content obviously reduces, and crystalline phase and glassy phase degree of engagement are reduced, and causes devitrified glass bending strength to reduce.Meanwhile, also can increase process costs.So the content of the soda ash providing in this programme is 4-6%, preferably, its content is 4.5%-5%.
Zinc oxide, in formula, role is to reduce the point of incipient sintering, initial recrystallization temperature and the final temperature of shakeouing, and is generally 2%-4%.In scheme provided by the invention, the degree of zinc oxide is 2%-7% all can within the scope of this.Preferably, the content of zinc oxide is 3%-4%.
Borax not only plays the effect of fluxing in formula, can reduce the temperature of glass melting, and main is the glossiness that improves product.Too much unsuitable in actual production, can corrode kiln, be generally 0.5%-1%.The consumption that uses borax in this programme is 0.5%-1%.Preferably, its consumption is 0.6%-0.8%.
SODIUMNITRATE and weisspiessglanz, as finings, contribute to the clarification of glass metal, improve the quality of devitrified glass.
Barium carbonate is substantially the same with the effect of calcium oxide, mainly plays the effect of constituent adjustment in formula, can reduce the viscosity of glass metal, is conducive to the fusing of glass, and the disadvantageous effect of glass properties is less than to sodium oxide.
In order to improve the quality of the devitrified glass of making, preferably, by percentage to the quality, made by following raw material:
Low-silicon iron mine tailing 37%-43%, quartz sand 28%-33%, Wingdale 14%-18%, soda ash 4.5%-5%, SODIUMNITRATE 3.4%-4.5%, zinc oxide 3%-4%, barium carbonate 3%-4%, borax 0.6%-0.8%, weisspiessglanz 0.6%-0.7%;
Wherein, described low-silicon iron mine tailing comprises following material composition: silicon-dioxide 30%-35%, aluminum oxide 19%-21%, ferric oxide 9%-11%, calcium oxide 8.5%-9.5%, titanium oxide 1.5%-2.5%, magnesium oxide 2%-3%, potassium oxide 1.5%-2.5%, sodium oxide 2.5%-2.7%, surplus is impurity.
Prepare low-silicon iron mine tailing and prepare the method for Si-Al-Ca microcrystalline glass in series, comprise following preparation process:
(1) low-silicon iron mine tailing, quartz sand, Wingdale, soda ash, SODIUMNITRATE, zinc oxide, barium carbonate, borax, the weisspiessglanz of preset ratio are mixed;
(2) raw material mixing is heated up and is heated to 1400-1500 DEG C, insulation 1-1.5 hour, makes glass metal;
Heating raw materials, to 1400-1500 DEG C of i.e. melting completely, if improve temperature, can increase process costs, and it is more to consume energy again.The homo-effect of the glass metal of making in this temperature range and compactness are all higher, and without bubble.
(3) by after the described glass metal clarification making, homogenizing, carry out shrend;
(4) frit after shrend is heated to 1100-1150 DEG C in High Temperature Furnaces Heating Apparatus and carries out crystallization, insulation 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, reduced the quality of product.Soaking time is unsuitable long, 30-35 minute, and preferably, soaking time is 30 minutes.
(5) furnace cooling afterwards, makes iron tailings devitrified glass.
In order to reduce the foreign matter content in glass metal, preferably, in step (2), the temperature of described intensification heating is 1460 DEG C, and soaking time is 1 hour.
In order to improve process efficiency, cost is in controlled range, and preferably, in step (4), described Heating temperature is 1110-1140 DEG C.
In order to improve the quality of product, preferably, in step (2) and (4), the speed of described heating is 10 DEG C/min.
Si-Al-Ca microcrystalline glass in series and method prepared by low-silicon iron mine tailing provided by the invention, the Si-Al-Ca microcrystalline glass in series of making is taking Yuanqu, Shanxi low-silicon iron mine tailing as raw material, fill into therein corresponding material composition, the Si-Al-Ca microcrystalline glass in series of making by preparation method provided by the invention can overall crystallization, wollastonite is main metallographic, even grain size, and be uniformly distributed in glassy phase, the folding strength mean value of devitrified glass reaches 510 (kg/cm
2) exceed the folding strength 490 (kg/cm of common devitrified glass
2).Also have good bending strength and ultimate compression strength, its anti-freezing property is better than common devitrified glass simultaneously.
Use embodiment to further describe the present invention, but the present invention is not limited to these embodiment below.
Embodiment 1
Low-silicon iron mine tailing 35%, quartz sand 35%, Wingdale 15%, soda ash 4%, SODIUMNITRATE 3%, zinc oxide 4%, barium carbonate 2%, borax 1%, weisspiessglanz 1% are mixed; Intensification is heated to 1400 DEG C, and temperature rise rate is 10 DEG C/min, is incubated 1 hour, makes glass metal, after clarification, homogenizing, carries out shrend; Frit after shrend is heated to 1100 DEG C with the speed of 10 DEG C/min in High Temperature Furnaces Heating Apparatus and carries out crystallization, be incubated 30 minutes after furnace cooling, make iron tailings devitrified glass.
Embodiment 2
Low-silicon iron mine tailing 38%, quartz sand 30%, Wingdale 17%, soda ash 5%, SODIUMNITRATE 4%, zinc oxide 3%, barium carbonate 2%, borax 0.4%, weisspiessglanz 0.6% are mixed; Intensification is heated to 1500 DEG C, and temperature rise rate is 10 DEG C/min, is incubated 1.5 hours, makes glass metal, after clarification, homogenizing, carries out shrend; Frit after shrend is heated to 1150 DEG C with the speed of 10 DEG C/min in High Temperature Furnaces Heating Apparatus and carries out crystallization, be incubated 35 minutes after furnace cooling, make iron tailings devitrified glass.
Embodiment 3
Low-silicon iron mine tailing 40%, quartz sand 30%, Wingdale 15%, soda ash 4.5%, SODIUMNITRATE 3.4%, zinc oxide 3%, barium carbonate 3%, borax 0.6%, weisspiessglanz 0.5% are mixed; Intensification is heated to 1460 DEG C, and temperature rise rate is 10 DEG C/min, is incubated 1 hour, makes glass metal, after clarification, homogenizing, carries out shrend; Frit after shrend is heated to 1130 DEG C with the speed of 10 DEG C/min in High Temperature Furnaces Heating Apparatus and carries out crystallization, be incubated 30 minutes after furnace cooling, make iron tailings devitrified glass.
Embodiment 4
Low-silicon iron mine tailing 45%, quartz sand 28%, Wingdale 12%, soda ash 5%, SODIUMNITRATE 4.5%, zinc oxide 2%, barium carbonate 2%, borax 0.8%, weisspiessglanz 0.7% are mixed; Intensification is heated to 1460 DEG C, and temperature rise rate is 10 DEG C/min, is incubated 1.5 hours, makes glass metal, after clarification, homogenizing, carries out shrend; Frit after shrend is heated to 1130 DEG C with the speed of 10 DEG C/min in High Temperature Furnaces Heating Apparatus and carries out crystallization, be incubated 35 minutes after furnace cooling, make iron tailings devitrified glass.
The Si-Al-Ca microcrystalline glass in series that the scheme of utilizing embodiment 1-4 to provide is made and the contrast of common devitrified glass, its performance data is added up as table 1:
Table 1
| Performance/material (unit) | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Common devitrified glass |
| Bending strength (MPa) | 45.4 | 45.1 | 45.3 | 45.2 | 40-50 |
| Ultimate compression strength (MPa) | 370 | 365 | 372 | 370 | 341.3 |
| Resistance to impact shock (cm) | 33cm (impulsive motion point) | 32 | 30 | 31 | 30 |
| Anti-folding (kg/cm 2) | 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%H 2SO 4) | 0.07 | 0.07 | 0.07 | 0.07 | 0.08 |
| Water-intake 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 can be found out, the Si-Al-Ca microcrystalline glass in series of making by four embodiment provided by the invention, and its ultimate compression strength and folding strength are obviously better than common devitrified glass, meanwhile, also have good bending strength and resistance to impact shock.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (6)
1. the Si-Al-Ca microcrystalline glass in series that prepared by low-silicon iron mine tailing, is characterized in that, by percentage to the quality, is made up of following raw material:
Low-silicon iron mine tailing 35%-45%, quartz sand 25%-35%, Wingdale 12%-20%, soda ash 4%-6%, SODIUMNITRATE 3%-5%, zinc oxide 2%-7%, barium carbonate 2%-5%, borax 0.5%-1%, weisspiessglanz 0.5%-1%;
Wherein, described low-silicon iron mine tailing comprises following material composition: silicon-dioxide below 35%, aluminum oxide 18%-23%, ferric oxide 8%-12%, calcium oxide 8%-10%, titanium oxide 1%-3%, potassium oxide 1%-3%, sodium oxide 2%-3%, surplus is impurity.
2. the Si-Al-Ca microcrystalline glass in series that prepared by low-silicon iron mine tailing according to claim 1, is characterized in that, by percentage to the quality, is made up of following raw material:
Low-silicon iron mine tailing 37%-43%, quartz sand 28%-33%, Wingdale 14%-18%, soda ash 4.5%-5%, SODIUMNITRATE 3.4%-4.5%, zinc oxide 3%-4%, barium carbonate 3%-4%, borax 0.6%-0.8%, weisspiessglanz 0.6%-0.7%;
Wherein, described low-silicon iron mine tailing comprises following material composition: silicon-dioxide 30%-35%, aluminum oxide 19%-21%, ferric oxide 9%-11%, calcium oxide 8.5%-9.5%, titanium oxide 1.5%-2.5%, magnesium oxide 2%-3%, potassium oxide 1.5%-2.5%, sodium oxide 2.5%-2.7%, surplus is impurity.
3. the low-silicon iron mine tailing described in preparation claim 1 or 2 is prepared the method for Si-Al-Ca microcrystalline glass in series, it is characterized in that, comprises following preparation process:
(1) low-silicon iron mine tailing, quartz sand, Wingdale, soda ash, SODIUMNITRATE, zinc oxide, barium carbonate, borax, the weisspiessglanz of preset ratio are mixed;
(2) raw material mixing is heated up and is heated to 1400-1500 DEG C, insulation 1-1.5 hour, makes glass metal;
(3) by after the described glass metal clarification making, homogenizing, carry out shrend;
(4) frit after shrend is heated to 1100-1150 DEG C in High Temperature Furnaces Heating Apparatus and carries out crystallization, insulation 30-35 minute;
(5) furnace cooling afterwards, makes iron tailings devitrified glass.
4. according to claim 3ly prepare the method that low-silicon iron mine tailing is prepared Si-Al-Ca microcrystalline glass in series, it is characterized in that:
In step (2), the temperature of described intensification heating is 1460 DEG C, and soaking time is 1 hour.
5. according to claim 3ly prepare the method that low-silicon iron mine tailing is prepared Si-Al-Ca microcrystalline glass in series, it is characterized in that:
In step (4), described Heating temperature is 1110-1140 DEG C.
6. according to claim 3ly prepare the method that low-silicon iron mine tailing is prepared Si-Al-Ca microcrystalline glass in series, it is characterized in that:
In step (2) and (4), the speed of described heating is 10-15 DEG C/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112225459A (en) * | 2019-07-15 | 2021-01-15 | 国合通用测试评价认证股份公司 | Black iron tailing microcrystalline glass and preparation method thereof |
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| 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 |
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| CN112225459A (en) * | 2019-07-15 | 2021-01-15 | 国合通用测试评价认证股份公司 | Black iron tailing microcrystalline glass and preparation method thereof |
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