CN101182120B - Method for manufacturing glass-ceramics - Google Patents
Method for manufacturing glass-ceramics Download PDFInfo
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- CN101182120B CN101182120B CN2007101955734A CN200710195573A CN101182120B CN 101182120 B CN101182120 B CN 101182120B CN 2007101955734 A CN2007101955734 A CN 2007101955734A CN 200710195573 A CN200710195573 A CN 200710195573A CN 101182120 B CN101182120 B CN 101182120B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to a microcrystalline glass preparation method, which belongs to the comprehensive utilization of industrial wastes. The invention is characterized in that rare earth tailing powder, feldspar and coal gangue are respectively filled in a ball mill tank in weight proportion of 100 to 8.5-25 to 9.5-17 to 8-22. Through the screening, the proportioning, the material mixing, the granulation, the molding, the drying, the sintering and the micro-crystallization, a main demanded crystal phase is fully precipitated from the sintered material. The powder obtained from the granulation is ball shaped. The molding pressure is 30-100MPa. When the micro-crystallization thermal treatment is finished, the sintered green body lowers to be at the room temperature with the furnace. The invention changes wastes into valuables, solves the secondary pollutions, improves the utilization ratio of industrial wastes, shortens the processing time, improves the working efficiency and reduces the energy consumption. The technology is simple, and the production cost is low. The nucleation activation energy is lowered, the nucleation and the crystallization of glass are promoted, and the micro-glass is finer. Therefore, the mechanical performance of the microcrystalline glass is improved and the cost for producing the tailings microcrystalline glass is greatly lowered.
Description
One, technical field:
The present invention relates to a kind of manufacture method of devitrified glass, specifically, it is to utilize rare method of selecting mine tailing, coal gangue, feldspar and Wingdale pure natural raw material to make devitrified glass, belongs to the comprehensive utilization of trade waste.
Two, background technology:
Along with expanding economy, increasing to the demand of coal, rare earth, its output increases day by day, and the consequent is that rare trade wastes such as mine tailing, coal gangue that select constantly increase.These wastes not only take a large amount of soils, and the water resources and the soil of periphery is caused severe contamination.In recent years, the someone utilizes the coal-fired Water Quenching Slag of flyash etc., can produce high value added product----architectural decoration crystallizing glass sheet material.Doping quantity of fly ash reaches more than 60%.Utilize flyash to produce devitrified glass and can reduce raw materials cost and glass melting temperature, reduce product cost more than 20%.Adopt cullet and devitrified glass scrap stock to replace big portion industrial chemicals or mineral starting material, can melt at a lower temperature and after heat treatment fire the low black glass ceramic of cost.
Utilize the crystallizing glass sheet material of abandoned mine slag as raw material production, the pure texture of color and luster becomes the preferred material of building decoration like mellow and full.
Utilize the iron and steel slag to prepare the devitrified glass technology, the devitrified glass wear resistance of being produced, hardness, erosion resistance, physical strength are all very high, can extensively be used in fields such as building materials, electronics, chemical industry, machinery.
But above all multi-methods need to add industrial chemicals such as additive, nucleating agent in manufacturing processed, have problems such as secondary pollution, production cost height.Simultaneously, generally all adopt melt casting method and molten sintering method to prepare the building microcrystalline glass goods on preparation technology, these two kinds of technologies all need to consume a large amount of energy through two pyroprocesses (glass smelting, micritization are handled).And adopt single-sinter process to prepare devitrified glass, and only need be heated to the semi-melting state to reduce to the crystallization temperature district again and be incubated processing, make full use of sintering state and finished crystallization, technology is simpler, quick than traditional method. and be one of developing direction of saving energy and reduce the cost.
Three, summary of the invention:
The object of the present invention is to provide a kind of secondary pollution that solves effectively, energy-saving and environmental protection have improved the comprehensive utilization ratio of trade waste, and technology is simple, production efficiency height, the manufacture method of the low a kind of devitrified glass of production cost.
Technical solution: the present invention is made up of the weight ratio of following raw materials according, rare-earth tailing powder: feldspar: coal gangue: 100: 8.5～25: 9.5～17: 8～22;
Processing step is as follows:
1) raw material: take by weighing above-mentioned rare-earth tailing, coal gangue, feldspar respectively, be respectively charged in the ball grinder, weight ratio, material: ball=1: 2, the charging cumulative volume is less than 2/3 of ball grinder volume, ball milling 24h;
2) screening: the rare-earth tailing powder behind the ball milling, coal gangue, feldspar powder raw material are crossed 325 purpose sieves respectively, the powder that makes, it is standby to put into the powder bag;
3) batching: the rare-earth tailing powder after will sieve: feldspar: coal gangue is 100: 8.5～25: 9.5～17: 8～22 to take by weighing respectively by weight proportion, and the ball mill of packing into mixes, and weight ratio is expected: ball=1: 2, mixing time: 40～100 minutes;
4) granulation: with sponging granulator compound is carried out mist projection granulating, the powder of gained is shaped as spherical or subsphaeroidal;
5) moulding: take by weighing the powder after the granulation, pour mould into, compression moulding, forming pressure: 30～100MPa;
6) drying: behind the green compact seasoning 48h of forming, put into electric drying oven with forced convection at 105～110 ℃ of forced air drying 24h;
7) sintering and micritization: dried green compact are placed in the high temperature box type resistance furnace, in the room temperature～400 ℃ temperature rise period, control heat-up rate: 3～4 ℃/min; In 400～600 ℃ of heat-processedes, intensification control speed: 1～2 ℃/min; At 600 ℃～nucleation temperature: 750～850 ℃, temperature rise period, heat-up rate: 15～20 ℃/min; Nucleation temperature-the highest sintering temperature: 1010～1050 ℃, temperature rise period, heat-up rate: 0.5～1 ℃/min, reach the highest sintering temperature after, the insulation 0.5～1.5h, thereafter, fast cooling is to crystallization temperature: 850～950 ℃, and be incubated 1～2h, make agglomerated material fully separate out required principal crystalline phase, after micritization thermal treatment finished, sintered body cooled to room temperature with the furnace.
Above-mentioned raw materials is rare mine tailing that selects: feldspar: coal gangue: Wingdale is respectively 100: 8.5～25: 9.5～17: 8～22: 5～25 by weight proportion.
Beneficial effect of the present invention:
1, turns waste into wealth, eliminated the pollution of industrial residue environment.
2, substitute lithotome and clay Mineral resources, avoided the environmental disruption that mining caused.
3, utilize industrial residue to substitute industrial raw material, and handle nearby and can also save a large amount of trucking costs, utilize industrial residue to belong to environmental protection project, can also enjoy the treatment of reduction or remission of taxes, reduce the production cost of devitrified glass.
4, shorten process period, can enhance productivity, reduce energy consumption.
5, because the rare mine tailing that selects of Baogang not only contains the required main chemical compositions of preparation devitrified glass, and the rare earth that is rich in, niobium, fluorite can be used as compound nucleus agent, by " two alkali effect ", nucleation activation energy is reduced, promote the coring and the crystallization of glass, make crystallite more tiny, thereby improve the mechanical property of devitrified glass, the cost of producing this tailing microcrystal glass is significantly reduced.
Four, description of drawings
Fig. 1 is a process flow sheet of the present invention.
Five, embodiment:
Embodiment 1:
Fig. 1 is seen in its technical process,
1, powder preparing
Used rare-earth tailing is taken from rare earth factory of Baogang, and the rare-earth tailing chemical ingredients sees Table 1; The coal gangue chemical ingredients sees Table 2; The feldspar chemical ingredients sees Table 3.In raw material: ball is that 1: 2 ratio takes by weighing rare-earth tailing, coal gangue, feldspar respectively, is respectively charged in the ball grinder (charging cumulative volume be less than ball grinder volume 2/3), ball milling 24h.
2, screening
Rare-earth tailing powder behind the ball milling and coal gangue, feldspar powder raw material are crossed 325 purpose sieves respectively, the powder that makes, it is standby to put into the powder bag.
3, batching
With the rare-earth tailing powder: feldspar: coal gangue is respectively to take by weighing at 100: 48: 12 by weight proportion, and (material: ball=1: 2) mix, mixing time is 50 minutes with ball mill.
4, granulation
With sponging granulator compound is carried out mist projection granulating, the powder of gained is shaped as spherical or subsphaeroidal, has higher loose density and good flowability.
5, moulding
Take by weighing the powder after the granulation, pour mould into, compression moulding notes keeping the mould cleaning, and every pressure first product clean one time mould, and the quality of assurance green compact prevents surface crack and slabbing phenomenon.Forming pressure 50MPa.
6, drying
Behind the green compact seasoning 48h of forming, put into electric drying oven with forced convection at 110 ℃ of forced air drying 24h.
7, sintering and micritization
Dried green compact are placed in the high temperature box type resistance furnace, in the room temperature～400 ℃ temperature rise period, 4 ℃/min of control heat-up rate; In 400～600 ℃ of heat-processedes, heat-up rate is controlled at 2 ℃/min; 600～850 ℃ of temperature rise periods, 18 ℃/min of heat-up rate; 850～1030 ℃ of temperature rise periods, 0.8 ℃/min of heat-up rate is incubated 1h after reaching 1030 ℃, thereafter, fast cooling to 950 ℃, and insulation 1.5h, make agglomerated material fully separate out required principal crystalline phase, after micritization thermal treatment finished, sintered body cooled to room temperature with the furnace.
Rare tailing microcrystal glass performance index of selecting of above-mentioned prepared are: density 2.39g.cm
-3, water-intake rate 0.9%, hardness HV560, folding strength 50Mpa, ultimate compression strength 450Mpa, acid resistance 0.08%, alkali resistance 0.02%.
Embodiment 2:
Fig. 1 is seen in its technical process,
1, powder preparing
Used rare-earth tailing is taken from rare earth factory of Baogang, and the rare-earth tailing chemical ingredients sees Table 1; The coal gangue chemical ingredients sees Table 2; The feldspar chemical ingredients sees Table 3.In raw material: ball is that 1: 2 ratio takes by weighing rare-earth tailing, coal gangue, feldspar respectively, is respectively charged in the ball grinder (charging cumulative volume be less than ball grinder volume 2/3), ball milling 24h.
2, screening
Rare-earth tailing powder behind the ball milling and coal gangue, feldspar powder raw material are crossed 325 purpose sieves respectively, the powder that makes, it is standby to put into the powder bag.
3, batching
With the rare-earth tailing powder: feldspar: coal gangue is respectively to take by weighing at 100: 26: 17 by weight proportion, and (material: ball=1: 2) mix, mixing time is 60 minutes with ball mill.
4, granulation
With sponging granulator compound is carried out mist projection granulating, the powder of gained is shaped as spherical or subsphaeroidal, has higher loose density and good flowability.
5, moulding
Take by weighing the powder after the granulation, pour mould into, compression moulding notes keeping the mould cleaning, and every pressure first product clean one time mould, and the quality of assurance green compact prevents surface crack and slabbing phenomenon.Forming pressure 70MPa.
6, drying
Behind the green compact seasoning 48h of forming, put into electric drying oven with forced convection at 105 ℃ of forced air drying 24h.
7, sintering and micritization
Dried green compact are placed in the high temperature box type resistance furnace, in the room temperature～400 ℃ temperature rise period, 4 ℃/min of control heat-up rate; In 400～600 ℃ of heat-processedes, heat-up rate is controlled at 1 ℃/min; 600～800 ℃ of temperature rise periods, 15 ℃/min of heat-up rate; 800～950 ℃ of temperature rise periods, 1 ℃/min of heat-up rate is incubated 1h after reaching 950 ℃, and thereafter, fast cooling to 900 ℃, and insulation 1.5h make agglomerated material fully separate out required principal crystalline phase, and after micritization thermal treatment finished, sintered body cooled to room temperature with the furnace.
Rare tailing microcrystal glass performance index of selecting of above-mentioned prepared are: density 2.41g.cm
-3, water-intake rate 0.81%, hardness HV600, folding strength 54Mpa, ultimate compression strength 490Mpa, acid resistance 0.03%, alkali resistance 0.01%.
Embodiment 3:
Fig. 1 is seen in its technical process,
1, powder preparing
Used rare-earth tailing is taken from rare earth factory of Baogang, and the rare-earth tailing chemical ingredients sees Table 1; The coal gangue chemical ingredients sees Table 2; The feldspar chemical ingredients sees Table 3; The Wingdale chemical ingredients sees Table 4.In raw material: ball is that 1: 2 ratio takes by weighing rare-earth tailing, coal gangue, feldspar, Wingdale respectively, is respectively charged in the ball grinder (charging cumulative volume be less than ball grinder volume 2/3), ball milling 24h.
2, screening
Rare-earth tailing powder behind the ball milling and Wingdale, coal gangue, feldspar powder raw material are crossed 325 purpose sieves respectively, the powder that makes, it is standby to put into the powder bag.
3, batching
With the rare-earth tailing powder: feldspar: coal gangue: Wingdale is 100: 20: 10 by weight proportion: 20 take by weighing respectively, and (material: ball=1: 2) mix, mixing time is 100 minutes with ball mill.
4, granulation
With sponging granulator compound is carried out mist projection granulating, the powder of gained is shaped as spherical or subsphaeroidal, has higher loose density and good flowability.
5, moulding
Take by weighing the powder after the granulation, pour mould into, compression moulding notes keeping the mould cleaning, and every pressure first product clean one time mould, and the quality of assurance green compact prevents surface crack and slabbing phenomenon.Forming pressure 50MPa.
6, drying
Behind the green compact seasoning 48h of forming, put into electric drying oven with forced convection at 110 ℃ of forced air drying 24h.
7, sintering and micritization
Dried green compact are placed in the high temperature box type resistance furnace, in the room temperature～400 ℃ temperature rise period, 4 ℃/min of control heat-up rate; In 400～600 ℃ of heat-processedes, heat-up rate is controlled at 2 ℃/min; 600～820 ℃ of temperature rise periods, 20 ℃/min of heat-up rate; 820～1030 ℃ of temperature rise periods, 1 ℃/min of heat-up rate is incubated 1h after reaching 1030 ℃, thereafter, fast cooling to 920 ℃, and insulation 1.5h, make agglomerated material fully separate out required principal crystalline phase, after micritization thermal treatment finished, sintered body cooled to room temperature with the furnace.
Rare tailing microcrystal glass performance index of selecting of above-mentioned prepared are: density 2.42g.cm
-3, water-intake rate 0.76%, hardness HV590, folding strength 48Mpa, ultimate compression strength 470Mpa, acid resistance 0.075%, alkali resistance 0.05%.
Embodiment 4:
Fig. 1 is seen in its technical process,
1, powder preparing
Used rare-earth tailing is taken from rare earth factory of Baogang, and the rare-earth tailing chemical ingredients sees Table 1; The coal gangue chemical ingredients sees Table 2; The feldspar chemical ingredients sees Table 3; The Wingdale chemical ingredients sees Table 4.In raw material: ball is that 1: 2 ratio takes by weighing rare-earth tailing, coal gangue, feldspar, Wingdale respectively, is respectively charged in the ball grinder (charging cumulative volume be less than ball grinder volume 2/3), ball milling 24h.
2, screening
Rare-earth tailing powder behind the ball milling and Wingdale, coal gangue, feldspar powder raw material are crossed 325 purpose sieves respectively, the powder that makes, it is standby to put into the powder bag.
3, batching
With the rare-earth tailing powder: feldspar: coal gangue: Wingdale is 100: 10: 20 by weight proportion: 20 take by weighing respectively, and (material: ball=1: 2) mix, mixing time is 80 minutes with ball mill.
4, granulation
With sponging granulator compound is carried out mist projection granulating, the powder of gained is shaped as spherical or subsphaeroidal, has higher loose density and good flowability.
5, moulding
Take by weighing the powder after the granulation, pour mould into, compression moulding notes keeping the mould cleaning, and every pressure first product clean one time mould, and the quality of assurance green compact prevents surface crack and slabbing phenomenon.Forming pressure 80MPa.
6, drying
Behind the blank seasoning 48h of forming, put into electric drying oven with forced convection at 110 ℃ of forced air drying 24h.
7, sintering and micritization
Dried green compact are placed in the high temperature box type resistance furnace, in the room temperature～400 ℃ temperature rise period, 4 ℃/min of control heat-up rate; In 400～600 ℃ of heat-processedes, heat-up rate is controlled at 1 ℃/min; 600～820 ℃ of temperature rise periods, 15 ℃/min of heat-up rate; 820～1200 ℃ of temperature rise periods, 0.5 ℃/min of heat-up rate is incubated 1h after reaching 1200 ℃, thereafter, fast cooling to 920 ℃, and insulation 1h, make agglomerated material fully separate out required principal crystalline phase, after micritization thermal treatment finished, sintered body cooled to room temperature with the furnace.
Rare tailing microcrystal glass performance index of selecting of above-mentioned prepared are: density 2.43g.cm
-3, water-intake rate 0.5%, hardness HV 660, folding strength 58Mpa, ultimate compression strength 540Mpa, acid resistance 0.045%, alkali resistance 0.02%.
Rare mine tailing composition (%) that selects in table 1 Baogang mine
Table 2 coal gangue composition (%)
Table 3 feldspar composition (%)
Table 4 Wingdale composition (%)
Claims (4)
1. the manufacture method of devitrified glass, it is characterized in that: manufacture method is as follows:
1) powder preparing
Used rare-earth tailing is taken from rare earth factory of Baogang, and in raw material: ball is that 1: 2 ratio takes by weighing rare-earth tailing, coal gangue, feldspar respectively, is respectively charged in the ball grinder, and the charging cumulative volume is less than 2/3 of ball grinder volume, ball milling 24h;
Wherein the rare mine tailing composition that selects of Baogang is: SiO
215.67%, Al
2O
31.68%, CaO 25.95%, MgO 1.80%, K
2O0.46%, Na
2O 1.36%, BaO 3.58%, FeO 1.50%, TFe 18.84%, P 1.01%, S 2.46%, F 12.85%, Nb
2O
50.18%, REO 3.80%, MnO 0.78%, burning subtract 3.96%;
The coal gangue composition is: Al
2O
343.00%, SiO
253.69%, Fe
2O
30.36%, TiO
20.59%, K
2O 0.07%, Na
2O 0.02%;
The feldspar composition is: SiO
262.8%, Al
2O
317.8%, K
2O 11.5%, other 7.9%;
2) screening
Rare-earth tailing powder behind the ball milling and coal gangue, feldspar powder raw material are crossed 325 purpose sieves respectively, the powder that makes, it is standby to put into the powder bag;
3) batching
With the rare-earth tailing powder: feldspar: coal gangue is respectively to take by weighing at 100: 48: 12 by weight proportion, mixes with ball mill, and material: ball=1: 2, mixing time are 50 minutes;
4) granulation
With sponging granulator compound is carried out mist projection granulating, the powder of gained is shaped as spherical or subsphaeroidal, has higher loose density and good flowability;
5) moulding
Take by weighing the powder after the granulation, pour mould into, compression moulding notes keeping the mould cleaning, and every pressure first product clean one time mould, and the quality of assurance green compact prevents surface crack and slabbing phenomenon, forming pressure 50MPa;
6) drying
Behind the green compact seasoning 48h of forming, put into electric drying oven with forced convection at 110 ℃ of forced air drying 24h;
7) sintering and micritization
Dried green compact are placed in the high temperature box type resistance furnace, in the room temperature～400 ℃ temperature rise period, 4 ℃/min of control heat-up rate; In 400～600 ℃ of heat-processedes, heat-up rate is controlled at 2 ℃/min; 600～850 ℃ of temperature rise periods, 18 ℃/min of heat-up rate; 850～1030 ℃ of temperature rise periods, 0.8 ℃/min of heat-up rate is incubated 1h after reaching 1030 ℃, thereafter, fast cooling to 950 ℃, and insulation 1.5h, make agglomerated material fully separate out required principal crystalline phase, after micritization thermal treatment finished, sintered body cooled to room temperature with the furnace.
2. the manufacture method of devitrified glass, it is characterized in that: manufacture method is as follows:
1) powder preparing
Used rare-earth tailing is taken from rare earth factory of Baogang, and in raw material: ball is that 1: 2 ratio takes by weighing rare-earth tailing, coal gangue, feldspar respectively, is respectively charged in the ball grinder, and the charging cumulative volume is less than 2/3 of ball grinder volume, ball milling 24h; Wherein the rare mine tailing composition that selects of Baogang is: SiO
215.67%, Al
2O
31.68%, CaO 25.95%, MgO 1.80%, K
2O 0.46%, Na
2O 1.36%, BaO 3.58%, FeO 1.50%, TFe 18.84%, P 1.01%, S 2.46%, F 12.85%, Nb
2O
50.18%, REO 3.80%, MnO 0.78%, burning subtract 3.96%;
The coal gangue composition is: Al
2O
343.00%, SiO
253.69%, Fe
2O
30.36%, TiO
20.59%, K
2O 0.07%, Na
2O 0.02%;
The feldspar composition is: SiO
262.8%, Al
2O
317.8%, K
2O 11.5%, other 7.9%;
2) screening
Rare-earth tailing powder behind the ball milling and coal gangue, feldspar powder raw material are crossed 325 purpose sieves respectively, the powder that makes, it is standby to put into the powder bag;
3) batching
With the rare-earth tailing powder: feldspar: coal gangue is respectively to take by weighing at 100: 26: 17 by weight proportion, mixes with ball mill, and material: ball=1: 2, mixing time are 60 minutes;
4) granulation
With sponging granulator compound is carried out mist projection granulating, the powder of gained is shaped as spherical or subsphaeroidal, has higher loose density and good flowability:
5) moulding
Take by weighing the powder after the granulation, pour mould into, compression moulding notes keeping the mould cleaning, and every pressure first product clean one time mould, and the quality of assurance green compact prevents surface crack and slabbing phenomenon, forming pressure 70MPa:
6) drying
Behind the green compact seasoning 48h of forming, put into electric drying oven with forced convection at 105 ℃ of forced air drying 24h:
7) sintering and micritization
Dried green compact are placed in the high temperature box type resistance furnace, in the room temperature～400 ℃ temperature rise period, 4 ℃/min of control heat-up rate; In 400～600 ℃ of heat-processedes, heat-up rate is controlled at 1 ℃/min; 600～800 ℃ of temperature rise periods, 15 ℃/min of heat-up rate; 800～950 ℃ of temperature rise periods, 1 ℃/min of heat-up rate is incubated 1h after reaching 950 ℃, and thereafter, fast cooling to 900 ℃, and insulation 1.5h make agglomerated material fully separate out required principal crystalline phase, and after micritization thermal treatment finished, sintered body cooled to room temperature with the furnace.
3. the manufacture method of devitrified glass, it is characterized in that: manufacture method is as follows:
1) powder preparing
Used rare-earth tailing is taken from rare earth factory of Baogang, and in raw material: ball is that 1: 2 ratio takes by weighing rare-earth tailing, coal gangue, feldspar, Wingdale respectively, is respectively charged in the ball grinder, and the charging cumulative volume is less than 2/3 of ball grinder volume, ball milling 24h; Wherein the rare mine tailing composition that selects of Baogang is: SiO
215.67%, Al
2O
31.68%, CaO 25.95%, MgO 1.80%, K
2O 0.46%, Na
2O 1.36%, BaO 3.58%, FeO 1.50%, TFe 18.84%, P 1.01%, S 2.46%, F 12.85%, Nb
2O
50.18%, REO 3.80%, MnO 0.78%, burning subtract 3.96%;
The coal gangue composition is: Al
2O
343.00%, SiO
253.69%, Fe
2O
30.36%, TiO
20.59%, K
2O 0.07%, Na
2O 0.02%;
The feldspar composition is: SiO
262.8%, Al
2O
317.8%, K
2O 11.5%, other 7.9%;
2) screening
Rare-earth tailing powder behind the ball milling and Wingdale, coal gangue, feldspar powder raw material are crossed 325 purpose sieves respectively, the powder that makes, it is standby to put into the powder bag;
3) batching
With the rare-earth tailing powder: feldspar: coal gangue: Wingdale is 100: 20: 10 by weight proportion: 20 take by weighing respectively, mix with ball mill, and material: ball=1: 2, mixing time are 100 minutes;
4) granulation
With sponging granulator compound is carried out mist projection granulating, the powder of gained is shaped as spherical or subsphaeroidal, has higher loose density and good flowability;
5) moulding
Take by weighing the powder after the granulation, pour mould into, compression moulding notes keeping the mould cleaning, and every pressure first product clean one time mould, and the quality of assurance green compact prevents surface crack and slabbing phenomenon, forming pressure 50MPa;
6) drying
Behind the green compact seasoning 48h of forming, put into electric drying oven with forced convection at 110 ℃ of forced air drying 24h;
7) sintering and micritization
Dried green compact are placed in the high temperature box type resistance furnace, in the room temperature～400 ℃ temperature rise period, 4 ℃/min of control heat-up rate; In 400～600 ℃ of heat-processedes, heat-up rate is controlled at 2 ℃/min; 600～820 ℃ of temperature rise periods, 20 ℃/min of heat-up rate; 820～1030 ℃ of temperature rise periods, 1 ℃/min of heat-up rate is incubated 1h after reaching 1030 ℃, thereafter, fast cooling to 920 ℃, and insulation 1.5h, make agglomerated material fully separate out required principal crystalline phase, after micritization thermal treatment finished, sintered body cooled to room temperature with the furnace.
4. the manufacture method of devitrified glass, it is characterized in that: manufacture method is as follows:
1) powder preparing
Used rare-earth tailing is taken from rare earth factory of Baogang, and in raw material: ball is that 1: 2 ratio takes by weighing rare-earth tailing, coal gangue, feldspar, Wingdale respectively, is respectively charged in the ball grinder, and the charging cumulative volume is less than 2/3 of ball grinder volume, ball milling 24h; Wherein the rare mine tailing composition that selects of Baogang is: SiO
215.67%, Al
2O
31.68%, CaO 25.95%, MgO 1.80%, K
2O 0.46%, Na
2O 1.36%, BaO 3.58%, FeO 1.50%, TFe 18.84%, P 1.01%, S 2.46%, F 12.85%, Nb
2O
50.18%, REO 3.80%, MnO 0.78%, burning subtract 3.96%;
The coal gangue composition is: Al
2O
343.00%, SiO
253.69%, Fe
2O
30.36%, TiO
20.59%, K
2O 0.07%, Na
2O 0.02%;
The feldspar composition is: SiO
262.8%, Al
2O
317.8%, K
2O 11.5%, other 7.9%;
2) screening
Rare-earth tailing powder behind the ball milling and Wingdale, coal gangue, feldspar powder raw material are crossed 325 purpose sieves respectively, the powder that makes, it is standby to put into the powder bag;
3) batching
With the rare-earth tailing powder: feldspar: coal gangue: Wingdale is 100: 10: 20 by weight proportion: 20 take by weighing respectively, mix with ball mill, and material: ball=1: 2, mixing time are 80 minutes;
4) granulation
With sponging granulator compound is carried out mist projection granulating, the powder of gained is shaped as spherical or subsphaeroidal, has higher loose density and good flowability;
5) moulding
Take by weighing the powder after the granulation, pour mould into, compression moulding notes keeping the mould cleaning, and every pressure first product clean one time mould, and the quality of assurance green compact prevents surface crack and slabbing phenomenon, forming pressure 80MPa;
6) drying
Behind the blank seasoning 48h of forming, put into electric drying oven with forced convection at 110 ℃ of forced air drying 24h;
7) sintering and micritization
Dried green compact are placed in the high temperature box type resistance furnace, in the room temperature～400 ℃ temperature rise period, 4 ℃/min of control heat-up rate; In 400～600 ℃ of heat-processedes, heat-up rate is controlled at 1 ℃/min; 600～820 ℃ of temperature rise periods, 15 ℃/min of heat-up rate; 820～1200 ℃ of temperature rise periods, 0.5 ℃/min of heat-up rate is incubated 1h after reaching 1200 ℃, thereafter, fast cooling to 920 ℃, and insulation 1h, make agglomerated material fully separate out required principal crystalline phase, after micritization thermal treatment finished, sintered body cooled to room temperature with the furnace.
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| CN108947258A (en) * | 2018-09-18 | 2018-12-07 | 西南科技大学 | It is a kind of to mention devitrified glass of the titanium slag as raw material containing chlorine |
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| DE102008002475B4 (en) * | 2008-06-17 | 2012-02-16 | Schott Ag | Process for shaping a green glass body and process for producing a glass ceramic with a structured surface |
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| CN106517775A (en) * | 2016-12-27 | 2017-03-22 | 钦州市中玻玻璃有限责任公司 | Glass ceramics |
| CN109133650B (en) * | 2018-09-18 | 2022-02-11 | 西南科技大学 | Method for preparing microcrystalline glass by using chlorine-containing titanium extraction slag |
| CN109133649B (en) * | 2018-09-18 | 2022-03-01 | 西南科技大学 | System for preparing microcrystalline glass by using chlorine-containing titanium extraction slag |
| CN109320090B (en) * | 2018-11-07 | 2022-02-11 | 西南科技大学 | Method for preparing microcrystalline glass by using chlorine-containing titanium extraction hot slag |
| CN109279782B (en) * | 2018-11-07 | 2022-03-01 | 西南科技大学 | System for preparing microcrystalline glass by using chlorine-containing titanium extraction hot slag |
| CN109354415A (en) * | 2018-12-06 | 2019-02-19 | 南华大学 | A kind of devitrified glass and preparation method thereof |
| CN110963669B (en) * | 2019-12-31 | 2021-05-28 | 中建材蚌埠玻璃工业设计研究院有限公司 | Glass raw material pretreatment granulation process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4028121A (en) * | 1975-07-18 | 1977-06-07 | Corning Glass Works | Lead feldspar glass-ceramic bodies |
| CN1087067A (en) * | 1992-11-18 | 1994-05-25 | 大连理工大学 | Utilize flyash to make building nucleated glass |
| CN1243106A (en) * | 1999-05-21 | 2000-02-02 | 彭波 | Crystallized glass for base plate of recording device, and mfg. method |
| CN1872753A (en) * | 2005-05-31 | 2006-12-06 | 电子科技大学 | Ceramic material of microcrystalline glass, and preparation method |
-
2007
- 2007-12-07 CN CN2007101955734A patent/CN101182120B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4028121A (en) * | 1975-07-18 | 1977-06-07 | Corning Glass Works | Lead feldspar glass-ceramic bodies |
| CN1087067A (en) * | 1992-11-18 | 1994-05-25 | 大连理工大学 | Utilize flyash to make building nucleated glass |
| CN1243106A (en) * | 1999-05-21 | 2000-02-02 | 彭波 | Crystallized glass for base plate of recording device, and mfg. method |
| CN1872753A (en) * | 2005-05-31 | 2006-12-06 | 电子科技大学 | Ceramic material of microcrystalline glass, and preparation method |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2004-107183A 2004.04.08 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108947258A (en) * | 2018-09-18 | 2018-12-07 | 西南科技大学 | It is a kind of to mention devitrified glass of the titanium slag as raw material containing chlorine |
| CN108947258B (en) * | 2018-09-18 | 2021-07-02 | 西南科技大学 | Microcrystalline glass using chlorine-containing titanium extraction slag as raw material |
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