CN104071983A - Sintering technique for producing microcrystalline glass plate from fluorite tailings - Google Patents
Sintering technique for producing microcrystalline glass plate from fluorite tailings Download PDFInfo
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- CN104071983A CN104071983A CN201410325810.4A CN201410325810A CN104071983A CN 104071983 A CN104071983 A CN 104071983A CN 201410325810 A CN201410325810 A CN 201410325810A CN 104071983 A CN104071983 A CN 104071983A
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Abstract
The invention belongs to the field of inorganic non-metal materials, and particularly relates to a sintering technique for producing a microcrystalline glass plate from fluorite tailings. In order to overcome the defects of recovering the fluorite tailings in the prior art, the technique provides a sintering technique for producing a microcrystalline glass plate from fluorite tailings. The method comprises the following steps: (1) proportioning: preparing fluorite tailings and a modifier used as raw materials, wherein the content of the fluorite tailings is 60-80 wt%; (2) melting: uniformly mixing the fluorite tailings and modifier, melting by heating, sufficiently stirring, and keeping the melting temperature at 1450-1600 DEG C to obtain a glass melt; (3) water quenching; (4) grinding and screening; (5) die-filling; and (6) heat treatment. The method provided by the invention solves the pollution of fluorite tailings, improves the mine environment, and can produce the microcrystalline glass product with excellent properties and high added value.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, relate in particular to a kind of sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate.
Background technology
Present material of construction has higher requirement for wear resisting property, antiacid caustic corrosion, impact resistance, therefore, the material of construction generally using is now cast stone, grouan, marble etc., although cast stone is a kind of silicate material processing from strand, but need to utilize basalt or diabase to melt casting forms, therefore must exploit basalt ore deposit or diabase ore deposit, this is the same with quarry marble and grouan, all can destroy surrounding environment.Devitrified glass is called again microcrystalline jade, is a kind of New Building Materials of abroad just having developed, and formal name used at school is again glass quartz.Its glass common with us is not too identical.Devitrified glass has the dual nature of pottery and glass, and common glass is a kind of sosoloid between solid and liquid, and atomic arrangement is confusing, easily broken.And the internal structure of devitrified glass is the same with pottery, by crystal composition, the atomic arrangement that is to say it is well-regulated, therefore, also be called glass-ceramic, this characteristic has than the higher intensity of pottery and brightness it, and has higher toughness compared with glass.The properties such as the wear resisting property of devitrified glass, antiacid caustic corrosion and shock-resistance are all higher than lithotome, and there is no radiation, can not pollute, and therefore replace gradually lithotome to become a kind of middle and high end material of construction.
In fluorite ore ore dressing, in the byproduct of sorting ore operation, the part that Calcium Fluoride Content is minimum, is called fluorite mine tailing.Due to economic cause, fluorite mine tailing should not further carry out sorting, and therefore, bargh, after ore dressing completes, processes fluorite mine tailing as waste residue, slag, mainly with mud form, arrange outward, accumulates over a long period and has just formed fluorite Tailings Dam.Tailings Dam floor space is very big, and has very large potential safety hazard, and landslide very easily occurs, if meet rainy weather, rubble flow also easily occurs.In addition, the beneficiation reagent being rich in Tailings Dam can be penetrated into underground, to environment, underground water, can cause great pollution, therefore, to the processing of mine tailing, is the significant problem that China producer faces.In fluorite mine tailing, major part is silicate composition, with the needed constituent class of devitrified glass seemingly, thereby likely adopt fluorite mine tailing as raw material, by addition portion, divide industrial chemicals to produce and there is high-wearing feature, high corrosion resistance and high-intensity microcrystal glass material.
As Chinese patent application 201210352021.0 (open day is: on January 2nd, 2013) disclose a kind of method of utilizing fluorite mine tailing to produce autoclaved brick, described method is: isolate the fluorite mine tailing particle that is greater than 0.1mm and carry out after desliming, reagent removal, mix according to the mass ratio of 88:12 with lime, adding water digests again, postdigestive material is through stirring, compression moulding, send into again autoclave and carry out steam pressure, make described autoclaved brick.
And for example Chinese patent application 200710178955.6 (open day is: on May 28th, 2008) disclose a kind of method of utilizing fluorite-containing tailings to prepare Portland clinker, related to the preparation of Portland clinker.It is characterized in that, containing CaF
2the mine tailing of weight percent 4-35% is through fragmentation and CaCO
3and Al
2o
3according to the weight percent of 32-34%, 65-67%, 0.2-1%, mix, temperature-gradient method, to 1200-1300 ℃ of calcining, is crossed 0.074mm standard sieve after mechanical mill, obtain cement clinker.
Although above-mentioned existing method can effectively be processed fluorite mine tailing, treatment process is complicated, and products obtained therefrom is low value-added cement, autoclaved brick, cannot improve the economic benefit in fluorite mine tailing recycling process.
Summary of the invention
In order to make up prior art in the deficiency reclaiming on fluorite mine tailing, the invention provides a kind of sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate, solving fluorite tailings pollution, when improving mine environment, produce excellent performance, there is the devitrified glass product of high added value.
In order to achieve the above object, the present invention adopts following technical scheme:
The invention provides a kind of sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate, it is characterized in that, described method comprises the steps:
(1) batching: the raw material of described method utilization comprises fluorite mine tailing, modification agent; The content of described fluorite mine tailing is 60-80%, and described content is quality percentage composition;
(2) melt: fluorite mine tailing is mixed with modification agent, and heat fused also fully stirs, and maintenance temperature of fusion is 1450-1600 ℃, obtains glass melt;
(3) shrend: glass melt first enters in intermediate buffering bag (also referred to as cinder ladle) from molten bath, then flow into water quenching pool by the mouth of a river under buffers packet, carry out Water Quenching, form glass particle;
(4) grind screening: glass particle is ground to screening and process, choosing granularity is 4-100 object glass particle, carries out drying and processing;
(5) dress mould: glass particle spreads to refractory slab after drying, and enters sintering zone;
(6) thermal treatment: comprise that coring, crystallization, insulation, annealing are cooling.
Further, in above-mentioned melt process, soaking time is 2 hours.
Further, in aforesaid method, the addition of described modification agent is 20-40%.
Further, the raw material of aforesaid method utilization also comprises finings, and the addition of finings accounts for the 0-5% of fluorite mine tailing and modification agent total amount.
Further, the raw material of aforesaid method utilization also comprises tinting material, and the addition of tinting material accounts for the 0-5% of fluorite mine tailing and modification agent total amount.
Further, described utilization in the sintering process method that fluorite mine tailing produces microcrystal glass plate, described method also comprises the steps:
(7) grinding, polishing, cutting.
Further, described utilization in the sintering process method that fluorite mine tailing produces microcrystal glass plate, described method comprises the steps:
(1) raw material using in described method comprises fluorite mine tailing, modification agent, finings, tinting material; Fluorite mine tailing is mixed with modification agent, finings, tinting material, and heat fused also fully stirs, and keeps temperature of fusion at 1450-1600 ℃, obtains glass melt;
(2) glass melt first enters in intermediate buffering bag from molten bath, then flows into water quenching pool by the mouth of a river under buffers packet, carries out Water Quenching, forms glass particle;
(3) glass particle is carried out to fine grinding screening and process, choosing granularity is 4-100 object glass particle, carries out drying and processing;
(4) glass particle spreads to refractory slab after drying, and enters sintering zone;
(5) coring: in sintering zone, be warming up to 800-950 ℃ of interval with the rate of heating of 8-15 ℃/min, and be incubated 1-3h;
(6) crystallization: enter crystallization region, be warming up to 1100-1200 ℃ of insulation with the rate of heating of 5-8 ℃/min, and be incubated 1-3h;
(7) be incubated, anneal and be cooling: enter cooling area, with the speed of 5-10 ℃/min, be down to 520-680 ℃, insulation 0.1-2h; Then with the speed of 15-20 ℃/min, be down to 100 ℃ and come out of the stove below, will obtain product.
Further, in described heat treatment process:
Glass particle spreads to refractory slab after drying, and enters sintering zone, in sintering zone, is warming up to 800-900 ℃, and is incubated 2-2.5h with the rate of heating of 8-12 ℃/min;
Enter crystallization region, with the rate of heating of 5-8 ℃/min, be warming up to 1100-1180 ℃ of insulation, and be incubated 2-2.5h;
Enter cooling area, with the speed of 5-10 ℃/min, be down to 550-600 ℃, insulation 1h; Then with the speed of 15-20 ℃/min, being down to 100 ℃ comes out of the stove below.
Further, product surface is carried out to polishing grinding, obtain finished product devitrified glass.
Further, in above-mentioned grinding screening process, do not meet granularity requirements glass particle will reenter the modified agitated pool of composition, again melt to process.
The present invention be take fluorite mine tailing as main material production microcrystal glass plate, one of its gordian technique is to control the proportioning of each raw material in formula, obtain being applicable to the formula of production high-performance devitrified glass, two of its gordian technique be controlled at found, the temperature curve in sintering process.
Further, described utilization in the sintering process method that fluorite mine tailing produces microcrystal glass plate, in the raw material using, fluorite mine tailing accounts for the 60-80% of total raw material, modification agent accounts for the 20-40% of total raw material, the addition of tinting material accounts for the 0-5% of fluorite mine tailing and modification agent total amount, and the addition of finings accounts for the 0-5% of fluorite mine tailing and modification agent total amount.Above-mentioned total raw material does not comprise tinting material and finings.
Further, in the raw material that described method is used, fluorite mine tailing accounts for 60% of total raw material, and modification agent accounts for 40% of total raw material, and the addition of finings accounts for the 2-3% of fluorite mine tailing and modification agent total amount.
Further, described utilization in the sintering process method that fluorite mine tailing produces microcrystal glass plate, the composition of described fluorite mine tailing and the quality percentage composition of each composition are as follows: SiO
2content be 70-85%, the content of CaO is 1-8%, the content of MgO is 1-7%, Al
2o
3content be 3-20%, the content of FeO is 1-5%, Calcium Fluoride (Fluorspan) 0-10%, the content of other composition is 0-1%.
Further, the composition of described fluorite mine tailing and the quality percentage composition of each composition are as follows: SiO
2content be 79-84%, the content of CaO is 4-6%, the content of MgO is 2-3%, Al
2o
3content be 3-6%, the content of FeO is 1-4%, Calcium Fluoride (Fluorspan) 2-4%, the content of other composition is 1%.
Further, the composition of described fluorite mine tailing and the quality percentage composition of each composition are as follows: SiO
2content be 79-83%, the content of CaO is 4-6%, the content of MgO is 2-3%, Al
2o
3content be 3-6%, the content of FeO is 2-4%, Calcium Fluoride (Fluorspan) 2-3%, the content of other composition is 1%.
Further, described utilization in the sintering process method that fluorite mine tailing produces microcrystal glass plate, described modification agent (also referred to as composition modification agent) is selected from blast furnace slag, potassium felspar sand, albite, calcite, clay, SODIUMNITRATE, diatomite, kaolin, barium carbonate, potter's clay, triphane, metal tailings, Power Plant Ash, borax, flyash, domestic sludge, one or more in blast furnace titaniferous slag.
The addition of modification agent requires, the price of modification agent and source approach are determined according to the composition of production product.
Further, in the raw material that described method is used, fluorite mine tailing accounts for 60% of total raw material, described modification agent comprises calcite, potassium felspar sand, barium carbonate, the addition of described calcite is 10-15%, and the addition of described potassium felspar sand is 10-15%, and the addition of described barium carbonate is 5-10%.
Further, described utilization in the sintering process method that fluorite mine tailing produces microcrystal glass plate, described tinting material is selected from Cr
2o
3, Cu
2o, CoO, NiO, Fe
2o
3and one or more in rare earth oxide.
The selection of tinting material and addition require to add according to product colour.
Further, described utilization in the sintering process method that fluorite mine tailing produces microcrystal glass plate, described finings is selected from one or more in white arsenic, weisspiessglanz, SODIUMNITRATE, ammonium nitrate, cerium dioxide.
The addition of finings is determined according to the clarification degree of glass melt.
Further, described utilization in the sintering process method that fluorite mine tailing produces microcrystal glass plate, described type of heating comprises the flammable coal dust of winding-up, dedusting ash, inflammable gas; The cooling method adopting comprises and passes into recirculated cooling water or cooling gas carries out cooling.
Further, described utilization in the sintering process method that fluorite mine tailing produces microcrystal glass plate, in described heat treatment process:
Glass particle spreads to refractory slab after drying, and enters sintering zone, in sintering zone, is warming up to 800-900 ℃, and is incubated 2-2.5h with the rate of heating of 8-12 ℃/min;
Enter crystallization region, with the rate of heating of 5-8 ℃/min, be warming up to 1100-1180 ℃ of insulation, and be incubated 2-2.5h;
Enter cooling area, with the speed of 5-10 ℃/min, be down to 550-600 ℃, insulation 1h; Then with the speed of 15-20 ℃/min, being down to 100 ℃ comes out of the stove below;
In the raw material that described method is used, fluorite mine tailing accounts for 60% of total raw material, and modification agent accounts for 40% of total raw material, and the addition of finings accounts for the 2-3% of fluorite mine tailing and modification agent total amount; Described modification agent comprises calcite, potassium felspar sand, and barium carbonate, the addition of described calcite is 10-15%, and the addition of described potassium felspar sand is 10-15%, and the addition of described barium carbonate is 5-10%; The composition of described fluorite mine tailing and the quality percentage composition of each composition are as follows: SiO
2content be 79-83%, the content of CaO is 4-6%, the content of MgO is 2-3%, Al
2o
3content be 3-6%, the content of FeO is 2-4%, Calcium Fluoride (Fluorspan) 2-3%, the content of other composition is 1%.
With respect to prior art, tool of the present invention has the following advantages:
1, the present invention utilizes microcrystal glass plate that fluorite mine tailing is produced to have to be better than the performances such as the intensity, wear resistance of lithotome, acidproof, alkaline-resisting, resistance to chemical attack, and there is no radioactivity, harmless, it is lower that Billy produces microcrystal glass plate cost with industrial chemicals.
2, the invention solves fluorite tailings pollution environment, take a large amount of soils and there is the problems such as potential safety hazard, utilize it to produce microcrystal glass plate, promoted the utility value of fluorite mine tailing, produce huge economic benefit.
Accompanying drawing explanation
Fig. 1 is the sintering process schema that utilizes fluorite mine tailing to produce microcrystal glass plate provided by the invention.
Embodiment
Below in conjunction with embodiment and accompanying drawing, technical scheme of the present invention is elaborated.
As shown in Figure 1, the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate provided by the invention, comprises the steps:
(1) batching: the raw material of described method utilization comprises fluorite mine tailing, modification agent; The content of described fluorite mine tailing is 60-80%, and described content is quality percentage composition;
(2) melt: fluorite mine tailing is mixed with modification agent, and heat fused also fully stirs, and maintenance temperature of fusion is 1450-1600 ℃, obtains glass melt;
(3) shrend: glass melt first enters in intermediate buffering bag from molten bath, then flow into water quenching pool by the mouth of a river under buffers packet, carry out Water Quenching, form glass particle;
(4) grind screening: glass particle is ground to screening and process, choosing granularity is 4-100 object glass particle, carries out drying and processing;
(5) dress mould: glass particle spreads to refractory slab after drying, and enters sintering zone;
(6) thermal treatment: comprise that coring, crystallization, insulation, annealing are cooling.
(7) grinding, polishing, cutting.
According to method provided by the invention, prepare microcrystal glass plate.
Below table 1 be the fluorite mine tailing that uses in embodiment one-tenth is grouped into.
Below material composition and composition in the method that provides for embodiment of table 2.
Below the microcrystal glass plate salient features detected result that provides for the embodiment of the present invention and comparative example of table 3.
The one-tenth of the fluorite mine tailing using in table 1 embodiment 1-6 is grouped into
Material composition and composition in the method that table 2 embodiment 1-6 provides
Embodiment 1
According to method provided by the invention, prepare microcrystal glass plate, comprise the steps:
(1) fluorite mine tailing is mixed with batching weighing, heat fused also fully stirs, and guarantees that temperature of fusion is at 1500 ℃, and insulation 2h, obtains glass melt;
(2) after cinder ladle buffering, from cinder ladle, the mouth of a river flows into water quenching pool to glass melt (also referred to as the molten slurry of fluorite mine tailing), carry out Water Quenching, prepare glass particle, after glass particle is dried, sieve processing, obtaining grade is 4-100 object glass particle;
(3) by grade, be to spread to refractory slab after 4-100 object glass particle is dried, enter sintering zone, in sintering zone, with the rate of heating of 8 ℃/min, be warming up to 800 ℃, and be incubated 2h;
(4) enter crystallization region, with the rate of heating of 5 ℃/min, be warming up to 1100 ℃ of insulations, and be incubated 2h;
(5) enter cooling area, with the speed of 5 ℃/min, be down to 550 ℃, insulation 1h; Then with the speed of 15 ℃/min, be down to 100 ℃ and come out of the stove below, obtain original microcrystal glass plate;
(6) the original microcrystal glass plate that is cooled to room temperature is cut to sanding and polishing, obtain finished product microcrystal glass plate.
The product principal crystalline phase obtaining in embodiment 1 is wollastonite phase, and the salient features of finished product microcrystal glass plate is in Table 3.
Embodiment 2
According to method provided by the invention, prepare microcrystal glass plate, comprise the steps:
(1) fluorite mine tailing is mixed with batching weighing, heat fused also fully stirs, and guarantees that temperature of fusion is at 1530 ℃, insulation 2h;
(2) the molten slurry of fluorite mine tailing after cinder ladle buffering from cinder ladle the mouth of a river flow into water quenching pool, carry out Water Quenching, form glass particle, after will glass particle drying, sieve processing, obtaining grade is 4-100 object glass particle;
(3) by grade, be to spread to refractory slab after 4-100 object glass particle is dried, enter sintering zone, in sintering zone, with the rate of heating of 10 ℃/min, be warming up to 875 ℃, and be incubated 2.5h;
(4) enter crystallization region, with the rate of heating of 6 ℃/min, be warming up to 1120 ℃ of insulations, and be incubated 2.5h;
(5) enter cooling area, with the speed of 10 ℃/min, be down to 580 ℃, insulation 1h; Then with the speed of 18 ℃/min, being down to 100 ℃ comes out of the stove below;
(6) the original microcrystal glass plate that is cooled to room temperature is cut to sanding and polishing, obtain finished product microcrystal glass plate.
The product principal crystalline phase obtaining in embodiment 2 is wollastonite phase, and the salient features of finished product microcrystal glass plate is in Table 3.
Embodiment 3
According to method provided by the invention, prepare microcrystal glass plate, comprise the steps:
(1) fluorite mine tailing is mixed with batching weighing, heat fused also fully stirs, and guarantees that temperature of fusion is at 1580 ℃, insulation 2h;
(2) the molten slurry of fluorite mine tailing after cinder ladle buffering from cinder ladle the mouth of a river flow into water quenching pool, carry out Water Quenching, prepare glass particle, after will devitrified glass drying, sieve processing, obtaining grade is 4-100 object glass particle;
(3) by grade, be to spread to refractory slab after 4-100 object glass particle is dried, enter sintering zone, in sintering zone, with the rate of heating of 12 ℃/min, be warming up to 900 ℃, and be incubated 2h;
(4) enter crystallization region, with the rate of heating of 8 ℃/min, be warming up to 1180 ℃ of insulations, and be incubated 2h;
(5) enter cooling area, with the speed of 10 ℃/min, be down to 600 ℃, insulation 1h; Then with the speed of 20 ℃/min, being down to 100 ℃ comes out of the stove below;
(6) the original microcrystal glass plate that is cooled to room temperature is cut to sanding and polishing, obtain finished product microcrystal glass plate.
The product principal crystalline phase obtaining in embodiment 3 is wollastonite phase, and the salient features of finished product microcrystal glass plate is in Table 3.
Embodiment 4
According to the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate provided by the invention, prepare microcrystal glass plate, described method comprises the steps:
(1) raw material using in described method comprises fluorite mine tailing, modification agent; Fluorite mine tailing is mixed with modification agent, and heat fused also fully stirs, and keeps temperature of fusion at 1450-1500 ℃, obtains glass melt; (2) glass melt first enters in intermediate buffering bag from molten bath, then flows into water quenching pool by the mouth of a river under buffers packet, carries out Water Quenching, forms glass particle;
(3) glass particle is carried out to fine grinding screening and process, choosing granularity is 4-100 object glass particle, carries out drying and processing;
(4) glass particle spreads to refractory slab after drying, and enters sintering zone;
(5) coring: in sintering zone, be warming up to 800 ℃ of intervals with the rate of heating of 8 ℃/min, and be incubated 1h;
(6) crystallization: enter crystallization region, be warming up to 1100 ℃ of insulations with the rate of heating of 5 ℃/min, and be incubated 1h;
(7) be incubated, anneal and be cooling: enter cooling area, with the speed of 5 ℃/min, be down to 520 ℃, insulation 0.1h; Then with the speed of 15 ℃/min, be down to 100 ℃ and come out of the stove below, will obtain product.
Embodiment 5
According to the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate provided by the invention, prepare microcrystal glass plate, described method comprises the steps:
(1) raw material using in described method comprises fluorite mine tailing, modification agent, finings, tinting material; Fluorite mine tailing is mixed with modification agent, finings, tinting material, and heat fused also fully stirs, and keeps temperature of fusion at 1550-1600 ℃, obtains glass melt;
(2) glass melt first enters in intermediate buffering bag from molten bath, then flows into water quenching pool by the mouth of a river under buffers packet, carries out Water Quenching, forms glass particle;
(3) glass particle is carried out to fine grinding screening and process, choosing granularity is 4-100 object glass particle, carries out drying and processing;
(4) glass particle spreads to refractory slab after drying, and enters sintering zone;
(5) coring: in sintering zone, be warming up to 950 ℃ of intervals with the rate of heating of 15 ℃/min, and be incubated 3h;
(6) crystallization: enter crystallization region, be warming up to 1200 ℃ of insulations with the rate of heating of 8 ℃/min, and be incubated 3h;
(7) be incubated, anneal and be cooling: enter cooling area, with the speed of 10 ℃/min, be down to 680 ℃, insulation 2h; Then with the speed of 20 ℃/min, be down to 100 ℃ and come out of the stove below, will obtain product.
Embodiment 6
According to the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate provided by the invention, prepare microcrystal glass plate, described method comprises the steps:
(1) raw material using in described method comprises fluorite mine tailing, modification agent, finings, tinting material; Fluorite mine tailing is mixed with modification agent, finings, tinting material, and heat fused also fully stirs, and keeps temperature of fusion at 1450-1600 ℃, obtains glass melt;
(2) glass melt first enters in intermediate buffering bag from molten bath, then flows into water quenching pool by the mouth of a river under buffers packet, carries out Water Quenching, forms glass particle;
(3) glass particle is carried out to fine grinding screening and process, choosing granularity is 4-100 object glass particle, carries out drying and processing;
(4) glass particle spreads to refractory slab after drying, and enters sintering zone;
(5) coring: in sintering zone, be warming up to 900 ℃ of intervals with the rate of heating of 11 ℃/min, and be incubated 2h;
(6) crystallization: enter crystallization region, be warming up to 1150 ℃ of insulations with the rate of heating of 7 ℃/min, and be incubated 2h;
(7) be incubated, anneal and be cooling: enter cooling area, with the speed of 8 ℃/min, be down to 600 ℃, insulation 1h; Then with the speed of 18 ℃/min, be down to 100 ℃ and come out of the stove below, will obtain product.
Comparative example 1
Method as described in Example 2, the consumption of different is fluorite mine tailing is 50%, the consumption of calcite is 50%, does not add other modification agent.In the method that this example provides, the content of fluorite mine tailing used is too low, and the consumption of modification agent calcite is too high, and the over-all properties of products obtained therefrom is poor.
Comparative example 2
Method as described in Example 2, the consumption of different is fluorite mine tailing is 85%, and modification agent is calcite, and the consumption of modification agent is 15%.The too high levels of fluorite mine tailing used in the method that this example provides, the consumption of modification agent is too low, and the over-all properties of products obtained therefrom is also poor.
The examination criteria of the microcrystal glass plate salient features that the embodiment of the present invention and comparative example provide is as follows:
The detection method of glossiness is with reference to GB/T13891-1992;
The detection method of flexural strength is with reference to GB/T9966.2-2001;
The detection method of water-intake rate is with reference to GB/T9966.3-2001;
The detection method of apparent porosity, acid resistance (1.0% sulphuric acid soln soaking at room temperature 650 hours), alkali resistance (1.0% sodium hydroxide solution soaking at room temperature 650 hours), Mohs' hardness, resistance to rapid heat cycle is with reference to JC/T872-2000.
The salient features detected result of the microcrystal glass plate that table 3 embodiment 1-6 and comparative example 1-2 provide
By the experimental result in table 3 above, can be drawn, microcrystal glass plate prepared by the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate that the embodiment of the present invention provides has good over-all properties.Microcrystal glass plate prepared by the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate that especially, embodiment of the present invention 1-3 provides has better over-all properties.
The above, be only preferred embodiment of the present invention, is not intended to limit protection scope of the present invention.Every equalization that content is done according to the present invention changes and modifies, and is all encompassed in the scope of the claims of the present invention.
Claims (10)
1. utilize fluorite mine tailing to produce a sintering process method for microcrystal glass plate, it is characterized in that, described method comprises the steps:
(1) batching: the raw material of described method utilization comprises fluorite mine tailing, modification agent; The content of described fluorite mine tailing is 60-80%, and described content is quality percentage composition;
(2) melt: fluorite mine tailing is mixed with modification agent, and heat fused also fully stirs, and maintenance temperature of fusion is 1450-1600 ℃, obtains glass melt;
(3) shrend: glass melt first enters in intermediate buffering bag from molten bath, then flow into water quenching pool by the mouth of a river under buffers packet, carry out Water Quenching, form glass particle;
(4) grind screening: glass particle is ground to screening and process, choosing granularity is 4-100 object glass particle, carries out drying and processing;
(5) dress mould: glass particle spreads to refractory slab after drying, and enters sintering zone;
(6) thermal treatment: comprise that coring, crystallization, insulation, annealing are cooling.
2. utilize according to claim 1 fluorite mine tailing to produce the sintering process method of microcrystal glass plate, it is characterized in that, described method also comprises the steps:
(7) grinding, polishing, cutting.
3. utilize according to claim 1 fluorite mine tailing to produce the sintering process method of microcrystal glass plate, it is characterized in that, described method comprises the steps:
(1) raw material using in described method comprises fluorite mine tailing, modification agent, finings, tinting material; Fluorite mine tailing is mixed with modification agent, finings, tinting material, and heat fused also fully stirs, and maintenance temperature of fusion is 1450-1600 ℃, obtains glass melt;
(2) glass melt first enters in intermediate buffering bag from molten bath, then flows into water quenching pool by the mouth of a river under buffers packet, carries out Water Quenching, forms glass particle;
(3) glass particle is carried out to fine grinding screening and process, choosing granularity is 4-100 object glass particle, carries out drying and processing;
(4) glass particle spreads to refractory slab after drying, and enters sintering zone;
(5) coring: in sintering zone, be warming up to 800-950 ℃ of interval with the rate of heating of 8-15 ℃/min, and be incubated 1-3h;
(6) crystallization: enter crystallization region, be warming up to 1100-1200 ℃ of insulation with the rate of heating of 5-8 ℃/min, and be incubated 1-3h;
(7) be incubated, anneal and be cooling: enter cooling area, with the speed of 5-10 ℃/min, be down to 520-680 ℃, insulation 0.1-2h; Then with the speed of 15-20 ℃/min, be down to 100 ℃ and come out of the stove below, will obtain product.
4. the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate according to claim 1, it is characterized in that, in the raw material that described method is used, fluorite mine tailing accounts for the 60-80% of total raw material, modification agent accounts for the 20-40% of total raw material, the addition of tinting material accounts for the 0-5% of fluorite mine tailing and modification agent total amount, and the addition of finings accounts for the 0-5% of fluorite mine tailing and modification agent total amount.
5. the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate according to claim 1, is characterized in that: the composition of described fluorite mine tailing and the quality percentage composition of each composition are as follows: SiO
2content be 70-85%, the content of CaO is 1-8%, the content of MgO is 1-7%, Al
2o
3content be 3-20%, the content of FeO is 1-5%, Calcium Fluoride (Fluorspan) 0-10%, the content of other composition is 0-1%.
6. the sintering process method of utilizing fluorite mine tailing to produce devitrified glass according to claim 1, is characterized in that, described modification agent (also referred to as composition modification agent) is selected from blast furnace slag, potassium felspar sand, albite, calcite, clay, SODIUMNITRATE, diatomite, kaolin, barium carbonate, potter's clay, triphane, metal tailings, Power Plant Ash, borax, flyash, domestic sludge, one or more in blast furnace titaniferous slag.
7. the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate according to claim 1, is characterized in that, described tinting material is selected from Cr
2o
3, Cu
2o, CoO, NiO, Fe
2o
3and one or more in rare earth oxide.
8. the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate according to claim 1, is characterized in that, described finings is selected from one or more in white arsenic, weisspiessglanz, SODIUMNITRATE, ammonium nitrate, cerium dioxide.
9. the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate according to claim 1, is characterized in that, the type of heating adopting in described method comprises the flammable coal dust of winding-up, dedusting ash, inflammable gas; The cooling method adopting comprises and passes into recirculated cooling water or cooling gas carries out cooling.
10. the sintering process method of utilizing fluorite mine tailing to produce microcrystal glass plate according to claim 1, is characterized in that, in described heat treatment process:
Glass particle spreads to refractory slab after drying, and enters sintering zone, in sintering zone, is warming up to 800-900 ℃, and is incubated 2-2.5h with the rate of heating of 8-12 ℃/min;
Enter crystallization region, with the rate of heating of 5-8 ℃/min, be warming up to 1100-1180 ℃ of insulation, and be incubated 2-2.5h;
Enter cooling area, with the speed of 5-10 ℃/min, be down to 550-600 ℃, insulation 1h; Then with the speed of 15-20 ℃/min, being down to 100 ℃ comes out of the stove below;
In the raw material that described method is used, fluorite mine tailing accounts for 60% of total raw material, and modification agent accounts for 40% of total raw material, and the addition of finings accounts for the 2-3% of fluorite mine tailing and modification agent total amount;
Described modification agent comprises calcite, potassium felspar sand, and barium carbonate, the addition of described calcite is 10-15%, and the addition of described potassium felspar sand is 10-15%, and the addition of described barium carbonate is 5-10%;
The composition of described fluorite mine tailing and the quality percentage composition of each composition are as follows: SiO
2content be 79-83%, the content of CaO is 4-6%, the content of MgO is 2-3%, Al
2o
3content be 3-6%, the content of FeO is 2-4%, Calcium Fluoride (Fluorspan) 2-3%, the content of other composition is 1%.
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| CN104370524A (en) * | 2014-10-27 | 2015-02-25 | 福州大学 | Environment-friendly rare-earth sintered brick prepared from micro/nano CeO2 and ZrO2 powder by doping lead zinc tailings |
| CN107032620A (en) * | 2017-06-09 | 2017-08-11 | 江苏耀兴安全玻璃有限公司 | A kind of method that utilization mine tailing prepares devitrified glass |
| CN107043217A (en) * | 2017-04-07 | 2017-08-15 | 东莞市银通玻璃有限公司 | A kind of production method of low-porosity micro-crystal glass |
| CN108358456A (en) * | 2018-05-24 | 2018-08-03 | 苏州大学 | A method of preparing devitrified glass using golden tailing and fluorite tailing |
| CN113526870A (en) * | 2021-07-14 | 2021-10-22 | 四川领先微晶玻璃有限公司 | Microcrystalline glass production process and production equipment thereof |
| CN115677226A (en) * | 2022-10-24 | 2023-02-03 | 苏州大学 | Method for preparing microcrystalline glass by sintering process |
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| CN115677226A (en) * | 2022-10-24 | 2023-02-03 | 苏州大学 | Method for preparing microcrystalline glass by sintering process |
| CN115677226B (en) * | 2022-10-24 | 2024-05-17 | 苏州大学 | Method for preparing microcrystalline glass by sintering method |
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