CN106565096B - A method of devitrified glass is prepared using carbide slag - Google Patents
A method of devitrified glass is prepared using carbide slag Download PDFInfo
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- CN106565096B CN106565096B CN201610926640.4A CN201610926640A CN106565096B CN 106565096 B CN106565096 B CN 106565096B CN 201610926640 A CN201610926640 A CN 201610926640A CN 106565096 B CN106565096 B CN 106565096B
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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
- C03C10/0063—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 containing waste materials, e.g. slags
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
Abstract
The invention discloses a kind of methods for preparing devitrified glass using carbide slag, belong to carbide slag resource utilization field, carbide slag is pre-processed at high temperature, it is mixed again with auxiliary material, it melts it at high operating temperatures, the devitrified glass of high added value is prepared by processes such as parent glass annealing, controlled micro crystallization processing.The devitrified glass that the present invention prepares has the characteristics that utility value height, simple process, and raw material is the solid waste generated in industrial processes, and the devitrified glass produced can be widely applied to the industries such as building materials, realizes the innoxious and resource utilization of carbide slag.
Description
Technical field
The present invention relates to a kind of methods for preparing devitrified glass using carbide slag, belong to industrial solid wastes disposal technology neck
Domain, i.e. waste residue resource field.
Background technique
Carbide slag is the hydrolysising by-product of generation during calcium carbide hydrolysis production acetylene, and key reaction formula sees below formula；
CaC2+2H2O→C2H2+Ca(OH)2
Main component is calcium hydroxide and calcium carbonate, and the generation of component calcium carbonate is since calcium hydroxide absorbs in air
Caused by carbon dioxide.In addition to this there are also a small amount of SiO2、Al2O3、Fe2O3Etc. components, belong to high calcium alkaline residue.Currently, domestic
Mainly there are two kinds of stockpiling and comprehensive utilization to the processing disposal options of carbide slag outside, the stockpiling of a large amount of carbide slags does not only take up largely
Land resource, increase entreprise cost, equally cause the pollution of soil, water body, air, become limitation industry development and destruction
An important factor for ecological environment；Comprehensive utilization, which is largely focused on instead of calcareous material, produces cement, building brick, thermal insulating material
Material etc..The features such as these disposal options are big with the quantity of slag is eaten, environmentally friendly, but the product produced by means of which has
The disadvantages such as added value is low.Devitrified glass is a kind of a kind of top-grade building decoration prepared by control composition and heat treating regime
Material can be widely used for the industries such as building materials.The devitrified glass of homologous ray does not have biggish limitation, such as CaO-Al to its component2O3-
SiO2System glass ceramics have the compositional range of calcium containing compound, aluminum contained compound and silicon-containing compound in system higher
It is required that.Calcium hydroxide and calcium carbonate in carbide slag can be changed to the calcium oxide of high-content after pretreatment, be to prepare CaO-Al2O3-
SiO2The main composition of system glass ceramics.
It is to make full use of high Ca resource in solid waste carbide slag that the present invention, which prepares devitrified glass using carbide slag, and to electricity
A small amount of SiO in rock ballast2、Al2O3、Fe2O3Etc. components carry out abundant resource utilization.CaO-Al is prepared using carbide slag2O3-
SiO2System glass ceramics not only can substantially slow down the influence that carbide slag stockpiling occupies a large amount of soils, and the crystallite produced
Glass has high economic benefit.
Patent of invention CN102795772A is disclosed a kind of to be prepared using kaolin type gangue or flyash and carbide slag
The method of devitrified glass.The method for preparing devitrified glass is that gangue, flyash and carbide slag are first carried out carbon elimination, iron, stone
The pretreatment of electrode ink clast is 10 ~ 55% according still further to gangue boiler ash sediment or flyash, and carbide slag is 8 ~ 24%, silica
It is 20 ~ 55%, the mass percents such as sodium oxide molybdena 5 ~ 12% carry out ingredient, and the particle that a part is not melted is retained in melting process and is made
For the nucleus of subsequent heat treatment, devitrified glass product is obtained using heat treatment.Application for a patent for invention CN103833276A is disclosed
A kind of environment-friendly light carbide slag aerated bricks and preparation method thereof.Wherein use carbide slag 24 ~ 26%, flyash 9 ~ 11%, glass
Fiber 2 ~ 4% etc., construction refuse regenerated powder (including construction refuse regenerated concrete powder and/or construction refuse regenerated brick powder) 11 ~
14% calcines 3 ~ 4h at 770 ~ 850 DEG C, adds diatomite 15 ~ 19%, cement 4 ~ 7% etc. is blended in 1 ~ 3h of precuring at 35 ~ 44 DEG C
After obtain base of laying bricks, then put it into reaction kettle and conserve 13 ~ 15h to get to lightweight carbide slag aerated bricks.Patent of invention
CN103193390A discloses the preparation method of carbide slag foam glass thermal insulation material.The patent of invention is with 70% ~ 90% glass
Powder, 10% ~ 30% carbide slag be raw material and using sodium carbonate as foaming agent, auxiliary additive appropriate is added with 5 ~ 10 DEG C/min's
Rate is warming up to 600 DEG C and keeps the temperature 30min；800 ~ 950 DEG C are warming up to the rate of 10 ~ 15 DEG C/min and keep the temperature 20 ~ 40min；
550 ~ 650 DEG C are cooled to the rate of temperature fall of 15 ~ 20 DEG C/min；Room temperature is annealed to again with the rate of temperature fall of 1 ~ 2 DEG C/min to obtain
Carbide slag foam glass thermal insulation material.Application for a patent for invention CN103738997A is disclosed using carbide slag as waste nano-sized carbon
The method of sour calcium.Carbide slag is separated by solid-liquid separation first, impurity elimination, the pretreatment such as decoloration, by controlling its pH value 12 or so
It is dissolved in leaching in ammonium chloride solution and obtains calcium chloride solution, then be passed through carbon dioxide gas to leaching in filtered solution
Body carries out carburizing reagent, finally obtains spherical superfine nano calcium carbonate.Due to the alkaline nature of carbide slag, many researchers
Then come treatment of acidic wastewater and sour gas as raw material, as patent of invention CN104192970A discloses a kind of processing acid
Property waste water carbide slag slow-release material and preparation method thereof, it is de- that application for a patent for invention CN104984658A discloses a kind of carbide slag
Sulphur system etc..It is this to use " treatment of wastes with processes of wastes against one another " thinking, pass through the method for the special nature treatment of acidic wastewater or gas of carbide slag
Also it is utilized extensively.
Currently, being able in disclosed carbide slag resource utilization mode, obtained added value of product is lower；And it is special in invention
A kind of method preparing devitrified glass using kaolin type gangue or flyash and carbide slag disclosed in sharp CN102795772A
The utilization rate of middle carbide slag is only 8 ~ 24%, eats that the quantity of slag is smaller not to be fully used；And nano-calcium carbonate is extracted by carbide slag
When the chemicals such as calcium, need to wherein a small amount of SiO2、Al2O3、Fe2O3Etc. components carry out impurity elimination so that the process is more complicated.
The present invention is to carry out pre-treatment, so that the dosage of carbide slag significantly improves, the CaO-Al prepared using to carbide slag2O3-
SiO2The added value of microcrystalline glass in series is higher, better economy.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing devitrified glass using carbide slag, first by carbide slag in height
Temperature is lower to carry out pre-treatment, obtains the higher oxidation calcium product of content, and by with auxiliary material SiO2、Al2O3And Na2CO3It is mixed,
Melting is that liquid obtains parent glass at high temperature, and CaO-Al is prepared using glass-ceramic process2O3-SiO2It is crystallite glass
Glass.Specifically includes the following steps:
(1) by carbide slag in high temperature Muffle furnace, 700 ~ 800 DEG C are raised to the heating rate of 5 ~ 7 DEG C/min, then with 1 ~
The rate of 3 DEG C/min is warming up to 1000 ~ 1100 DEG C and keeps the temperature 90 ~ 150min, then cools to room temperature with the furnace and obtain the original rich in CaO
Expect, wherein CaO content >=80wt%；
(2) raw material rich in CaO that obtains step (1) and rich in SiO2Auxiliary material, be rich in Al2O3Auxiliary material and be rich in
Na2CO3Auxiliary material 90 ~ 120min is mixed in mixing machine, the raw material rich in CaO accounts for 40 ~ 55wt% of raw material total amount, be rich in SiO2
Auxiliary material account for 34 ~ 55wt% of raw material total amount, be rich in Al2O3Auxiliary material account for 2 ~ 5wt% of raw material total amount, be rich in Na2CO3Auxiliary material
3 ~ 7wt% of raw material total amount is accounted for, being subsequently placed in alumina crucible melts it in high temperature Muffle furnace, and at 1350-1450 DEG C
Progress thermal state forming, which is placed at 600-650 DEG C, after lower heat preservation 90-150min makes annealing treatment.It is handled using glass-ceramic process
To devitrified glass.
It is described to be rich in SiO2Auxiliary material be quartz sand etc., wherein SiO2Content is more than or equal to 75wt%.
It is described to be rich in Al2O3Auxiliary material be bauxite, wherein Al2O3Content is more than or equal to 80wt%.
It is described to be rich in Na2CO3Auxiliary material be one of soda, crystal soda, soda ash, washing soda, wherein Na2CO3Content is greater than
Equal to 70wt%.
Glass-ceramic process processing method described in step (2) is conventional method, such as can refer to and record in following documents
Method is handled: Liu Hongpan etc., TiO2It is manually brilliant to influence [J] of natural cooling yellow phosphorus furnace slag ceramics behavior
Body journal, 2014,06:1561-1567..
The principle of the present invention: easily it is decomposed into the spy of calcium oxide at high temperature using calcium hydroxide in carbide slag and calcium carbonate
Property, without carrying out dedoping step to it, make full use of the SiO in carbide slag2、Al2O3、Fe2O3Etc. components.SiO2And Al2O3As
CaO-Al2O3-SiO2The constitutive material of microcrystalline glass in series, Fe2O3As CaO-Al2O3-SiO2The Nucleating Agent of microcrystalline glass in series is to promote
Into crystallization.
Beneficial effects of the present invention:
(1) method that carbide slag of the present invention prepares devitrified glass, it is simple for process, after pretreatment, with auxiliary material
The processes such as mixing is melted at high operating temperatures, controlled micro crystallization is handled, annealing prepare the devitrified glass haveing excellent performance；
(2) present invention can prepare the devitrified glass haveing excellent performance, and form the economic chain of carbide slag resource recycling, realize electricity
Rock ballast is innoxious, higher value application；
(3) it is of the present invention prepare devitrified glass during, without carrying out raw material except miscellaneous operation, and make full use of calcium carbide
Impurity composition in slag, improves economic value.
Detailed description of the invention
Fig. 1 is that carbide slag of the present invention prepares devitrified glass process flow chart.
Specific embodiment
Below with reference to embodiment, invention is further described in detail, but the scope of the present invention is not limited in described
Hold.
Embodiment 1
(1) by carbide slag in high temperature Muffle furnace, 800 DEG C are raised to the heating rate of 5 DEG C/min, then with 3 DEG C/min
Rate be warming up to 1000 DEG C and keep the temperature 90min, then cool to room temperature with the furnace and obtain the raw material rich in CaO, wherein CaO content is
90.02wt%；
(2) raw material rich in CaO that obtains step (1) and rich in SiO2Auxiliary material, be rich in Al2O3Auxiliary material and be rich in
Na2CO3Auxiliary material 90min is mixed in mixing machine, the raw material rich in CaO accounts for the 40wt% of raw material total amount, be rich in SiO2Auxiliary material
The 54.22wt%(quartz sand of raw material total amount is accounted for, wherein SiO2Content is 75wt%), it is rich in Al2O3Auxiliary material account for raw material total amount
2.53wt%(bauxite, wherein Al2O3Content is 80wt%), it is rich in Na2CO3Auxiliary material account for the 3.25wt%(soda of raw material total amount,
Wherein Na2CO3Content is 70wt%).Being subsequently placed in alumina crucible melts it in high temperature Muffle furnace, and at 1400 DEG C
Progress thermal state forming, which is placed at 650 DEG C, after heat preservation 120min makes annealing treatment.It handles to obtain using a series of glass-ceramic processes
Devitrified glass.
Controlled micro crystallization treatment process: parent glass is risen into 780 DEG C of heat preservation 2h with the heating rate of 2 ~ 5 DEG C/min, then with 1 ~ 2
DEG C/after the heating rate of min rises to 1080 DEG C of heat preservation 1.5h cooling devitrified glass can be obtained.
Using the bulk density of Archimedes method measurement sample, according to " Expectation of Glass-Ceramics Used as Decorated Materials JC/T872-
2000 ", the water absorption rate of sample is measured.The results show that the bulk density of this devitrified glass is 2.2206 cm3/ g, water absorption rate are
0.023%。
Embodiment 2
(1) by carbide slag in high temperature Muffle furnace, 700 DEG C are raised to the heating rate of 7 DEG C/min, then with 2 DEG C/min
Rate be warming up to 1050 DEG C and keep the temperature 120min, then cool to room temperature with the furnace and obtain the raw material rich in CaO, wherein CaO content
For 88.03wt%；
(2) raw material rich in CaO that obtains step (1) and rich in SiO2Auxiliary material, be rich in Al2O3Auxiliary material and be rich in
Na2CO3Auxiliary material mix 100min in mixing machine after, being placed in alumina crucible melts it in high temperature Muffle furnace.It is rich in
The raw material of CaO accounts for the 48wt% of raw material total amount, is rich in SiO2Auxiliary material account for the 44.07wt%(quartz sand of raw material total amount, wherein SiO2
Content is 80wt%), it is rich in Al2O3Auxiliary material account for the 3.72wt%(bauxite of raw material total amount, wherein Al2O3Content is 85wt%),
Rich in Na2CO3Auxiliary material account for the 4.21wt%(crystal soda of raw material total amount, wherein Na2CO3Content is 72wt%).It is kept the temperature at 1350 DEG C
Progress thermal state forming, which is placed at 640 DEG C, after 150min makes annealing treatment.It handles to obtain crystallite using a series of glass-ceramic processes
Glass.
Using the bulk density of Archimedes method measurement sample, according to " Expectation of Glass-Ceramics Used as Decorated Materials JC/T872-
2000 ", the water absorption rate of sample is measured.The results show that the bulk density of this devitrified glass is 2.2161 cm3/ g, water absorption rate are
0.012%。
Embodiment 3
(1) by carbide slag in high temperature Muffle furnace, 750 DEG C are raised to the heating rate of 6 DEG C/min, then with 1 DEG C/min
Rate be warming up to 1100 DEG C and keep the temperature 100min, then cool to room temperature with the furnace and obtain the raw material rich in CaO, wherein CaO content
For 88.67wt%；
(2) raw material rich in CaO that obtains step (1) and rich in SiO2Auxiliary material, be rich in Al2O3Auxiliary material and be rich in
Na2CO3Auxiliary material mix 110min in mixing machine after, being placed in alumina crucible melts it in high temperature Muffle furnace.It is rich in
The raw material of CaO accounts for the 53wt% of raw material total amount, is rich in SiO2Auxiliary material account for the 40.21wt%(quartz sand of raw material total amount, wherein SiO2
Content is 95wt%), it is rich in Al2O3Auxiliary material account for the 2.13wt%(bauxite of raw material total amount, wherein Al2O3Content is 90wt%),
Rich in Na2CO3Auxiliary material account for the 5.36wt%(soda ash of raw material total amount, wherein Na2CO3Content is 80wt%).It is kept the temperature at 1450 DEG C
Progress thermal state forming, which is placed at 600 DEG C, after 90min makes annealing treatment.It handles to obtain crystallite glass using a series of glass-ceramic processes
Glass.
Using the bulk density of Archimedes method measurement sample, according to " Expectation of Glass-Ceramics Used as Decorated Materials JC/T872-
2000 ", the water absorption rate of sample is measured.The results show that the bulk density of this devitrified glass is 2.3464 cm3/ g, water absorption rate are
0.042%。
Embodiment 4
(1) by carbide slag in high temperature Muffle furnace, 800 DEG C are raised to the heating rate of 5 DEG C/min, then with 3 DEG C/min
Rate be warming up to 1000 DEG C and keep the temperature 150min, then cool to room temperature with the furnace and obtain the raw material rich in CaO, wherein CaO content
For 89.75wt%；
(2) raw material rich in CaO that obtains step (1) and rich in SiO2Auxiliary material, be rich in Al2O3Auxiliary material and be rich in
Na2CO3Auxiliary material mix 120min in mixing machine after, being placed in alumina crucible melts it in high temperature Muffle furnace.It is rich in
The raw material of CaO accounts for the 54.26wt% of raw material total amount, is rich in SiO2Auxiliary material account for the 34.93wt%(quartz sand of raw material total amount, wherein
SiO2Content is 99wt%), it is rich in Al2O3Auxiliary material account for the 4.52wt%(bauxite of raw material total amount, wherein Al2O3Content is
83wt%), it is rich in Na2CO3Auxiliary material account for the 6.29wt%(washing soda of raw material total amount, wherein Na2CO3Content is 85wt%).In
It is kept the temperature at 1375 DEG C and carries out thermal state forming after 135min and be placed at 630 DEG C and make annealing treatment.Using a series of glass-ceramic processes
Processing obtains devitrified glass.
Using the bulk density of Archimedes method measurement sample, according to " Expectation of Glass-Ceramics Used as Decorated Materials JC/T872-
2000 ", the water absorption rate of sample is measured.The results show that the bulk density of this devitrified glass is 2.1365 cm3/ g, water absorption rate are
0.0063%。
Embodiment 5
(1) by carbide slag in high temperature Muffle furnace, 700 DEG C are raised to the heating rate of 7 DEG C/min, then with 2 DEG C/min
Rate be warming up to 1100 DEG C and keep the temperature 130min, then cool to room temperature with the furnace and obtain the raw material rich in CaO, wherein CaO content
For 91.50wt%；
(2) raw material rich in CaO and auxiliary material obtained step (1) is rich in SiO2Auxiliary material, be rich in Al2O3Auxiliary material and
Rich in Na2CO3Auxiliary material mix 100min in mixing machine after, being placed in alumina crucible melts it in high temperature Muffle furnace.
Raw material rich in CaO accounts for the 55wt% of raw material total amount, is rich in SiO2Auxiliary material account for the 34.86wt%(quartz sand of raw material total amount, wherein
SiO2Content is 98wt%), it is rich in Al2O3Auxiliary material account for the 3.29wt%(bauxite of raw material total amount, wherein Al2O3Content is
90wt%), it is rich in Na2CO3Auxiliary material account for the 6.85wt%(soda of raw material total amount, wherein Na2CO390%) content is.At 1425 DEG C
Progress thermal state forming, which is placed at 620 DEG C, after lower heat preservation 105min makes annealing treatment.It is handled using a series of glass-ceramic processes
To devitrified glass.
Using the bulk density of Archimedes method measurement sample, according to " Expectation of Glass-Ceramics Used as Decorated Materials JC/T872-
2000 ", the water absorption rate of sample is measured.The results show that the bulk density of this devitrified glass is 2.1041 cm3/ g, water absorption rate are
0.027%。
Claims (2)
1. a kind of method for preparing devitrified glass using carbide slag carries out as follows:
(1) carbide slag is once warming up to 700 ~ 800 DEG C, secondary temperature elevation is to 1000 ~ 1100 DEG C and keeps the temperature 90 ~ 150min, then cold
But the raw material rich in CaO is obtained to room temperature；
(2) raw material rich in CaO that obtains step (1) and rich in SiO2Auxiliary material, be rich in Al2O3Auxiliary material and be rich in Na2CO3
Auxiliary material be sufficiently mixed after, melting, and at 1350-1450 DEG C keep the temperature 90-150min after carry out thermal state forming, be placed in 600-
It is made annealing treatment at 650 DEG C, obtains devitrified glass using glass-ceramic process；
(1) heating rate of step is 5 ~ 7 DEG C/min；Secondary temperature elevation rate is 1 ~ 3 DEG C/min；
CaO content >=80wt% in step (1) raw material obtained rich in CaO；
Raw material rich in CaO accounts for 40 ~ 55wt% of raw material total amount, is rich in SiO2Auxiliary material account for 34 ~ 55wt% of total amount, be rich in Al2O3
Auxiliary material account for 2 ~ 5wt% of total amount, be rich in Na2CO3Auxiliary material account for 3 ~ 7wt% of total amount.
2. according to the method described in claim 1, it is characterized by: being rich in SiO2Auxiliary material be quartz sand, wherein SiO2Content >=
75wt%；Rich in Al2O3Auxiliary material be bauxite, wherein Al2O3Content >=80wt%；Rich in Na2CO3Auxiliary material is soda, crystal soda, pure
One of alkali, washing soda, wherein Na2CO3Content >=70wt%.
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| CN1958499A (en) * | 2006-09-28 | 2007-05-09 | 贵州省遵义碱厂 | Heat preservation insulator of xonaltite, and preparation method |
| CN101805128A (en) * | 2010-04-20 | 2010-08-18 | 香港福山实业有限公司 | Jade-type glass-ceramic and preparation method thereof |
| CN102206045A (en) * | 2010-03-31 | 2011-10-05 | 徐州康腾微晶玻璃制品科技有限公司 | Black microcrystalline glass and manufacturing method thereof |
| CN105731808A (en) * | 2016-04-20 | 2016-07-06 | 昆明理工大学 | Method for preparing glass ceramics |
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- 2016-10-31 CN CN201610926640.4A patent/CN106565096B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958499A (en) * | 2006-09-28 | 2007-05-09 | 贵州省遵义碱厂 | Heat preservation insulator of xonaltite, and preparation method |
| CN102206045A (en) * | 2010-03-31 | 2011-10-05 | 徐州康腾微晶玻璃制品科技有限公司 | Black microcrystalline glass and manufacturing method thereof |
| CN101805128A (en) * | 2010-04-20 | 2010-08-18 | 香港福山实业有限公司 | Jade-type glass-ceramic and preparation method thereof |
| CN105731808A (en) * | 2016-04-20 | 2016-07-06 | 昆明理工大学 | Method for preparing glass ceramics |
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