CN1063853A - A kind of tungsten slag sitall and preparation method thereof - Google Patents

A kind of tungsten slag sitall and preparation method thereof Download PDF

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Publication number
CN1063853A
CN1063853A CN 91100652 CN91100652A CN1063853A CN 1063853 A CN1063853 A CN 1063853A CN 91100652 CN91100652 CN 91100652 CN 91100652 A CN91100652 A CN 91100652A CN 1063853 A CN1063853 A CN 1063853A
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tungsten
slag
fluorite
glass
sitall
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CN1024652C (en
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王承遇
陶瑛
郝彦武
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DALIAN COLLEGE OF LIGHT INDUSTRY
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/16—Halogen containing crystalline phase

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

A kind of tungsten slag sitall and preparation method thereof, it is that tailings with 50～60% exploitation tungsten ore ore dressings are main raw material, add 35～45% Wingdale, 2～10% feldspar, 3～5% soda ash, 1～2% saltcake, the fluorite that also has above-mentioned prescription total amount 6～9%, or 4～6% fluorite and 10～14% Rock Phosphate (72Min BPL), after fusing, moulding, thermal treatment and a kind of type material that has glass and ceramic characteristics concurrently that makes.The present invention becomes refuse and is material of construction, has not only utilized secondary resource but also solved problem of environmental pollution, and the devitrified glass outward appearance that makes is similar to marble, and with low cost.

Description

A kind of tungsten slag sitall and preparation method thereof
The present invention relates to a kind of devitrified glass ceramics.
At present cinder microcrystalline glass is to be main raw material with metallurgical slag, solid fuel, lime-ash etc., add other an amount of frit and necessary nucleator, through fusing, moulding, thermal treatment after and a kind of type material that has glass and ceramic characteristics concurrently of formation.Having introduced a kind of in English Patent (BP986289) is the devitrified glass of raw material with the metallurgical slag, and its composition range is SiO 245～65%, CaO 15～45%, Al 2O 35～30%, MgO 5%, and the nucleus agent comprises transition element oxide compound, fluorochemical, phosphoric acid salt or its mixture, compound, open hearth slag, bone ash or fuel ash.It is the devitrified glass of raw material that Japanese Patent (39-1024) has been introduced with the blast furnace slag, and its composition range is SiO 240～70%, Al 2O 35～15%, CaO 13～35%, MgO 2～12%, Na 2O 2～12%, nucleus agent fluorite, potassium bichromate, phosphoric acid.The existing tungsten ore tailings of China is about more than 1,000 ten thousand tons, and annual also with 400,000 tons speed increase, and these slags also do not obtain utilizing at present, be not only the huge waste on the resource, and environment is also done great damage.
The objective of the invention is to utilize the tailings of exploitation tungsten ore ore dressing discharging as the main material production tungsten slag sitall.
Purpose of the present invention can realize by following measure, and a kind of tungsten slag sitall and preparation method thereof is characterized in that the chemical ingredients of this tungsten slag sitall is: SiO 246.7 Al～56.2%, 2O 38.3～11%, CaO 20～25.2%, MgO 0.7～2.5%, Na 2O 3.2～4.2%, K 2O 2～2.6%, Fe 2O 30.8 CaF～1.1%, 20.5 P～3.5%, 2O 50.8～4.3%.It is by raw material and fusing assistant and nucleus agent uniform mixing such as slag, feldspar, Wingdales, after fusing, moulding and coring, crystallization and thermal treatment, make, it is characterized in that: slag is the tailings of exploitation tungsten ore ore dressing, its consumption is 50～60%, and 35～45% Wingdale, 2～10% feldspar, 3～5% soda ash, 1～2% saltcake, also have the fluorite of above-mentioned prescription total amount 6～9% or the Rock Phosphate (72Min BPL) of 4～6% fluorites and 10～14%.Preferably the parent glass batching is tungsten slag 55%, feldspar 5%, Wingdale 40%, soda ash 4%, saltcake 1.5%.Consumption was 6～7% of a parent glass batching sum when nucleus agent fluorite was used separately, and the fluorite consumption was 5～6% when fluorite and Rock Phosphate (72Min BPL) share, the Rock Phosphate (72Min BPL) consumption is 11～12%.
Tungsten slag sitall is that the tailings that produces when utilizing the ore dressing of exploitation tungsten ore is made main raw material, and be aided with other raw materials such as feldspar, Wingdale with fusing assistant, nucleus agent melt, moulding, after coring and crystallization are handled, make again.Its outward appearance of the used tungsten slag of the present invention raw material is particulate state, diameter Distribution: be 2 millimeters to the maximum, content is less than 10%; Minimum is 0.07 millimeter, and content is less than 10%; 0.5～0.6 millimeter of average out to, content are 80%.The scoriaceous essential mineral of tungsten is α-SiO mutually 2, albite (Na[AlSi 3O 8]) or (Na, and Ca) (Si, Al) 4O 8, also have a spot of wolframite [(Mn, Fe) (WO 4)] and sheelite [Ca(WO 4)].This scoriaceous chemical ingredients scope is:
SiO 276.2～86.3% Al 2O 37.4～8.4%
CaO 0.2～1.3% MgO 0.02～0.8%
K 2O 2.0～2.8% Na 2O 1.04～2.02%
Fe 2O 30.9～1.6% MnO 0.007～0.09%
CaF 20.4～0.53% P 2O 50.05～0.73%
WO 30.01～0.062%
Its consumption is 50～60%, if then can not form devitrified glass outside this scope.Preferably the consumption of tungsten tailings makes the glass that makes have flowability 55%, and viscosity is little, the optimum regime that bubble and scum silica frost are all few.
Another kind of raw material of the present invention is a feldspar, and its chemical ingredients is: SiO 266%, Al 2O 317%, Fe 2O 30.5%, Na 2O 14%, and consumption is generally 5～10%.When consumption surpasses 10%, the fusing difficulty.When consumption is lower than 5%, more serious to the refractory corrosion in the High Temperature Furnaces Heating Apparatus, and the glass metal devitrification.Best felspathic consumption is 5%.
It is Wingdale that the present invention also has a kind of raw material, and its chemical ingredients scope is CaO 〉=49%, MgO 〉=3%, Fe 2O 3≤ 0.25%, consumption generally is 35～45%.When its consumption was low, glass did not produce crystallization.The violent devitrification of glass when its consumption is higher, preferably the consumption of Wingdale is 40%.
The fusing assistant that the present invention adopts is soda ash and saltcake, when adding the soda ash amount when very few, the glass melting difficulty, viscosity increases, but when the soda ash amount of adding is higher than 5% the glass metal devitrification, thereby the consumption of soda ash is generally 3～5%, preferably 4%.The add-on of general saltcake is 1～2%, and when the add-on of saltcake was higher than 2%, the flash phenomenon can take place in fusing, but when the saltcake amount adds saltcake very little or not, again can be because of SiO 2Surplus scum silica frost occurs on fusion glass liquid surface, and preferably the add-on of saltcake is 1.5%.
For making product obtain reasonable integrally crystallization, thereby need to add suitable nucleus agent, nucleus agent of the present invention is fluorite and ground phosphate rock.The main component of fluorite is CaF 2, content is about 83.96%.When it used separately, consumption was that the parent glass batching is the raw material and 6～9% of the dosage sum of fluxing.Can not fine nucleation when consumption is low, be unfavorable for that when consumption is higher devitrified glass generates, optimum amount is 6～7%.Crystalline phase by the resulting tungsten ore slag of fluorite nucleus agent crystallite glass is wollastonite (CaSiO 3) and gehlenite [Ca, Al(Al, Si 4O 7)].Can be P also with fluorite and main component 2O 5Content share about 37.46% Rock Phosphate (72Min BPL), and this moment, the fluorite consumption was 4～6% of a parent glass batching, and the Rock Phosphate (72Min BPL) consumption then is 10-14, and its optimum amount is that fluorite is 5～6%, and Rock Phosphate (72Min BPL) is 11～12%.Crystalline phase by these two kinds of resulting tungsten slag sitalls of nucleus agent is wollastonite (CaSiO 3), gehlenite [(Ca, Al(Al, Si 4O 7) and phosphatic rock [Ca 5(PO 4) 3].
Preparation technology's process description of tungsten slag sitall is as follows among the present invention:
1450～1520 ℃ 650～720 ℃ 850～1050 ℃ of raw materials
Fusing assistant ()/() fusing ()/() moulding ()/() coring ()/() crystallization
Nucleus agent 2～6 hours 1～6 hour
At first be that various raw materials, fusing assistant and nucleus agent are weighed by the quantity of prescription regulation, wherein various components all need be passed through 40 mesh sieves, behind uniform mixing, put into High Temperature Furnaces Heating Apparatus, in air, melt, its temperature of fusion generally 1450～1520 ℃ make material all fusing do not have ore particle to exist till.The no bubble that melting process is obtained, the glass metal of no sand grains carry out coring and crystallization and thermal treatment again after moulding.Coring thermal treatment is to handle 2～6 hours down at 650～720 ℃.The fast nucleus quantity of nucleating growth speed is many in this temperature range, and too short as the time, the quantity of nucleus is unfavorable for crystallization less; Otherwise nucleation time is long, and nucleus quantity not only no longer increases, and is transformed into chain but also nucleus can take place, and preferably handles 2～4 hours at 680～700 ℃.Coring is carried out crystallization and thermal treatment after handling again, and it is to handle 1～6 hour at 850～1050 ℃, and percent crystallization in massecuite is very low when crystallization temperature is low, but crystal was thick plate when crystallization temperature was too high, percent crystallization in massecuite changes not remarkable, and microhardness descends, so optimum crystallization temperature is 900～1000 ℃.Crystallization time is too short, and it is meticulous to separate out crystal; Crystallization time is long, and percent crystallization in massecuite changes not remarkable, and crystal grain is excessive, and microhardness has decline slightly, and therefore best crystallization time is 2～4 hours.
The chemical ingredients of the tungsten slag microcrystalline glass that is made by aforesaid method is: SiO 246.7 Al～56.2%, 2O 38.3～11%, CaO 20～25.2%, MgO 0.7～2.5%, Na 2O 3.2～4.2%, K 2O 2～2.6%, Fe 2O 30.8 CaF～1.1%, 20.5 P～3.5%, 2O 50.8～4.3%.
The salient features scope of tungsten slag microcrystalline glass of the present invention is as follows: density 2.6-2.725g/cm 3, microhardness 568～766kg/mm 2, linear expansivity 78.0～80 * 10 -7℃ -1, water tolerance (the 0.01N HCl milliliter number that consumes in titration) 0.15～0.20.
Example 1
Get 47.6 parts of tungsten ore slags, 9.5 parts of feldspars, 38.1 parts of Wingdales, 2.9 parts of soda ash, 1.9 parts of saltcake, other adds the agent of 6 parts of fluorite nucleus, more than after each raw material all crosses 40 mesh sieves, uniform mixing places in the melting furnaces, be fused into the uniform glass of no bubble, no sand grains under 1500 ℃, this moment, the glass analysis of components was as follows:
SiO 254.95% Al 2O 310.58% CaO, 22.66% MgO, 2.76% Na 2O 4.27% K 2O 2.20% Fe 2O 31.01% CaF 21.10% P 2O 50.32% WO 3＜0.01% treat the glass metal moulding after, send into and carry out coring, crystallization and thermal treatment in the heat treatment kiln, coring was handled 2 hours when 680 ℃ of temperature, crystallization was handled 2 hours in the time of 900 ℃ again, obtaining outward appearance is linen devitrified glass, density 2.69g/cm 3, microhardness 710.2kg/mm 2, linear expansivity 80.1 * 10 -7℃ -1
Example 2
Get 52.1 parts of tungsten ore slags, 4.7 parts of feldspars, 37.9 parts of Wingdales, 3.8 parts of soda ash, 1.4 parts of saltcake, other adds the agent of 7 parts of fluorite nucleus.By example 1 operation, 1500 ℃ of fusings down, the analysis of components of gained glass is as follows:
SiO 257.58% Al 2O 38.31% CaO, 22.47% MgO, 2.25% Na 2O 4.16% K 2O 2.40% Fe 2O 31.07% CaF 21.13% P 2O 50.58% WO 3＜0.01% treats after the glass ware forming, sends into and carries out coring, crystallization and thermal treatment in the heat treatment kiln.Coring was handled 2 hours when 685 ℃ of temperature, after coring is handled, handled 2 hours 950 ℃ of crystallization again, obtained the devitrified glass of appearance off-white, density 2.711g/cm 3, microhardness 766.1kg/mm 2, linear expansivity 78.5 * 10 -7℃ -1
Example 3
Get 56.6 parts of tungsten ore slags, 4.7 parts, 33.0 parts Wingdales of feldspar, 4.7 parts of soda ash, 0.94 part of saltcake, other adds the agent of 9 parts of fluorite nucleus, repeats example 1 operation, 1520 ℃ of melting furnace temperatures, and gained glass analysis of components is as follows:
SiO 258.04% Al 2O 38.52% CaO 21.43% MgO 2.07% Na 2O 4.66% K 2O 2.01% Fe 2O 31.05% CaF 21.63% P 2O 50.57% WO 3＜0.01%。Treat to send into behind the glass ware forming and carry out coring in the heat treatment kiln and crystallization is handled, when 685 ℃ of temperature, handled 2 hours, in the time of 950 ℃, handled 2 hours again, obtain the appearance off-white devitrified glass, density 2.723g/cm 3, microhardness 723.3kg/mm 2, linear expansivity is 79.3 * 10 -7℃ -1
Example 4
Get 47.40 parts of tungsten ore slags, 4.7 parts of feldspars, 42.7 parts of Wingdales, 3.8 parts of soda ash, 1.4 parts of saltcake, other adds the agent of 6 parts of fluorite nucleus, repeats example 1 operation, 1500 ℃ of fusings down of melting furnace temperature, and the analysis of components of glass is as follows:
SiO 254.30% Al 2O 38.43% CaO 25.46% MgO 2.86% Na 2O 3.65% K 2O 2.13% Fe 2O 31.00% CaF 21.01% P 2O 50.35% WO 3＜0.01%。After treating the glass metal moulding, send into and carry out coring, crystallization and thermal treatment in the heat treatment kiln.Coring was handled 3 hours when 720 ℃ of temperature, and crystallization 4 hours in the time of 1000 ℃ obtains the appearance off-white devitrified glass, density 2.72g/cm again 3, microhardness 700.2kg/mm 2, linear expansivity is 81.0 * 10 -7℃ -1
Example 5
Get 52.1 parts of tungsten ore slags, 4.7 parts of feldspars, 37.9 parts of Wingdales, 3.8 parts of soda ash, 1.4 parts of saltcake, other adds 4 parts of fluorites and the agent of 14 parts of ground phosphate rock nucleus, by example 1 operation, and 1480 ℃ of temperature of fusion, the analysis of components of gained glass is as follows:
SiO 246.77% Al 2O 312.64% CaO 25.45% MgO 0.72% Na 2O 3.29% K 2O 2.02% Fe 2O 30.84% CaF 23.23% P 2O 54.67% WO 3＜0.01%。Treat to send into behind the glass ware forming and carry out coring, crystallization and thermal treatment in the heat treatment kiln.Handled 2 hours in 685 ℃ of coring of temperature, crystallization 2 hours in the time of 950 ℃ obtains the appearance off-white devitrified glass, density 2.681g/cm again 3, microhardness 700kg/mm 2, linear expansivity 86.6 * 10 -7℃ -1
Example 6
Get 52.1 parts of tungsten ore slags, 4.7 parts of feldspars, 37.9 parts of Wingdales, 3.8 parts of soda ash, 1.4 parts of saltcake, other adds 6 parts of fluorites and the agent of 10 parts of ground phosphate rock nucleus, by example 1 operation, and 1450 ℃ of temperature of fusion, the analysis of components of gained glass is as follows:
SiO 246.87%、Al 2O 312.54%、CaO 25.5%、MgO 0.74%、Na 2O 3.28%、K 2O 2.0%、Fe 2O 30.90%、CaF 23.10%、P 2O 54.55%、WO 3＜0.01%。Treat to send into behind the glass ware forming and carry out coring, crystallization and thermal treatment in the heat treatment kiln.Handled 4 hours in 685 ℃ of coring of temperature, crystallization was handled 4 hours in the time of 950 ℃ again, obtained the appearance off-white devitrified glass, density 2.682g/cm 3, microhardness 700.5kg/mm 2, linear expansivity 86.8 * 10 -7℃ -1
50～60% is the tungsten ore tailings in the raw material of the present invention, the waste residue of discharging when it is the tungsten ore ore dressing, and its secondary resource that rationally is utilized as the tungsten slag utilizes the approach opened up again.Feldspar, Wingdale are the raw materials of factory's fusion cast glass, and price is low, supply is sufficient.Therefore be that the cost of main material production devitrified glass is low with tungsten slag, feldspar, Wingdale.Contain Na in the tungsten slag 2O, K 2The O(summation is 3～4.5%) only need add a spot of fusing assistant soda ash when making molten glass and get final product, save a large amount of soda ash, and the glass metal clarification is good.General high slag microcrystallite glass is a Vandyke brown, needs to add discoloring agent and can produce shallow white micro-crystals glass.And the tungsten slag microcrystalline glass need not to add discoloring agent, can direct production go out the light gray-white devitrified glass, reaches the effect of parian.
(annotate: the per-cent in the present specification all is weight percentage)

Claims (4)

1, a kind of tungsten slag sitall and preparation method thereof is characterized in that: the chemical ingredients of this tungsten slag sitall is: SiO 246.7 Al～56.2%, 2O 38.3～11%, CaO 20～25.2%, MgO 0.7～2.5%, Na 2O 3.2～4.2%, K 2O 2～2.6%, Fe 2O 30.8 CaF～1.1%, 20.5 P～3.5%, 2O 50.8～4.3%.
2, a kind of tungsten slag sitall and preparation method thereof, it is by raw material and fusing assistant and nucleus agent uniform mixing such as slag, feldspar, Wingdales, after fusing, moulding and coring, crystallization and thermal treatment, make, it is characterized in that: slag is the tailings of exploitation tungsten ore ore dressing, its consumption is 50～60%, and 35～45% Wingdale, 2～10% feldspar, 3～5% soda ash, 1～2% saltcake, also has the fluorite of above-mentioned prescription total amount 6～9% or the Rock Phosphate (72Min BPL) of 4～6% fluorites and 10～14%.
3, tungsten slag sitall according to claim 2 and preparation method thereof is characterized in that: the parent glass batching is tungsten slag 55%, feldspar 5%, Wingdale 40%, soda ash 4%, saltcake 1.5%.
4, according to claim 2 or 3 described tungsten slag sitalls and preparation method thereof, it is characterized in that: consumption was 6～7% of a parent glass batching sum when nucleus agent fluorite was used separately, when nucleus agent fluorite and Rock Phosphate (72Min BPL) share, the fluorite consumption was 5～6%, the Rock Phosphate (72Min BPL) consumption is 11～12%.
CN 91100652 1991-01-29 1991-01-29 Nucleated glass made from tungsten slag and prep. thereof Expired - Fee Related CN1024652C (en)

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CN 91100652 CN1024652C (en) 1991-01-29 1991-01-29 Nucleated glass made from tungsten slag and prep. thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100383072C (en) * 2004-08-12 2008-04-23 李章大 Microcrystalline glass produced from molybdenum containing gangue and its method
CN103011601A (en) * 2012-12-05 2013-04-03 毛庆云 Microcrystalline glass taking quartz sand as main material and preparation method thereof
CN103232158A (en) * 2013-05-09 2013-08-07 南京师范大学 Composite slag glass flux composition and application for same
CN103951193A (en) * 2014-05-08 2014-07-30 中国科学院过程工程研究所 Glass ceramics prepared from tailings obtained by nickel-molybdenum ore dressing and smelting and preparation method thereof
CN104926134A (en) * 2015-06-01 2015-09-23 安徽省益民工贸集团有限公司 Acid and alkali corrosion-resistant glass ceramic plate and preparation method for same
CN108585509A (en) * 2018-04-27 2018-09-28 南昌大学 A kind of devitrified glass preparation method
CN109865734A (en) * 2019-03-13 2019-06-11 兰州有色冶金设计研究院有限公司 A method of vitreum is produced using chemical industry abraum salt

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100383072C (en) * 2004-08-12 2008-04-23 李章大 Microcrystalline glass produced from molybdenum containing gangue and its method
CN103011601A (en) * 2012-12-05 2013-04-03 毛庆云 Microcrystalline glass taking quartz sand as main material and preparation method thereof
CN103011601B (en) * 2012-12-05 2016-04-27 毛庆云 A kind of take quartz sand as devitrified glass of major ingredient and preparation method thereof
CN103232158A (en) * 2013-05-09 2013-08-07 南京师范大学 Composite slag glass flux composition and application for same
CN103232158B (en) * 2013-05-09 2015-09-30 南京师范大学 A kind of complex ore slag glass flux composition and application thereof
CN103951193A (en) * 2014-05-08 2014-07-30 中国科学院过程工程研究所 Glass ceramics prepared from tailings obtained by nickel-molybdenum ore dressing and smelting and preparation method thereof
CN103951193B (en) * 2014-05-08 2016-02-24 中国科学院过程工程研究所 A kind of nickel-molybdenum ore selects smelting tailing microcrystal glass and preparation method thereof
CN104926134A (en) * 2015-06-01 2015-09-23 安徽省益民工贸集团有限公司 Acid and alkali corrosion-resistant glass ceramic plate and preparation method for same
CN108585509A (en) * 2018-04-27 2018-09-28 南昌大学 A kind of devitrified glass preparation method
CN109865734A (en) * 2019-03-13 2019-06-11 兰州有色冶金设计研究院有限公司 A method of vitreum is produced using chemical industry abraum salt

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