CN108341656A - A kind of innoxious method for preparing ceramics of cathode-ray tube glass - Google Patents
A kind of innoxious method for preparing ceramics of cathode-ray tube glass Download PDFInfo
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- CN108341656A CN108341656A CN201710058226.0A CN201710058226A CN108341656A CN 108341656 A CN108341656 A CN 108341656A CN 201710058226 A CN201710058226 A CN 201710058226A CN 108341656 A CN108341656 A CN 108341656A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1321—Waste slurries, e.g. harbour sludge, industrial muds
- C04B33/1322—Red mud
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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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/102—Glass compositions containing silica with 40% to 90% silica, by weight containing lead
- C03C3/105—Glass compositions containing silica with 40% to 90% silica, by weight containing lead containing aluminium
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Dispersion Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Processing Of Solid Wastes (AREA)
- Glass Compositions (AREA)
Abstract
The invention belongs to dangerous waste disposal and recycling fields, disclose a kind of innoxious method for preparing ceramics of cathode-ray tube glass.This approach includes the following steps：Cathode tube is subjected to screen cone separation, and the cone glass of gained after crushing further clay into power by ball, and the cone glass powder of gained is put into according to different proportion in ball mill with red mud then and is mixed, mixed material is obtained；Mixed material is dried, and is pressed into molding, is subsequently placed in Muffle furnace and be heat-treated up to innoxious ceramics.This method mixes CRT cone glass powder with red mud, and high-temperature heat treatment is carried out after tabletting, and the lead in CRT is cured to stable crystalline phase PbFe12O9In, discard CRT glass harmless treatments to realize.The final Pb leaching concentrations of its ceramic product be less than 0.1mg/L, can security landfill, can also be used as architectural pottery, industrial ceramics and glaze etc..
Description
Technical field
The invention belongs to dangerous waste disposal and recycling field, more particularly to a kind of cathode-ray tube glass is harmless
Change the method for preparing ceramics.
Background technology
Cathode-ray tube (Cathode Ray Tube, CRT) is to realize earliest, most widely used display technology equipment,
Have many advantages, such as that technology maturation, reliability are high, at low cost, was once widely used in the aobvious of television set, computer, industry monitoring device etc.
Show in equipment.As display technology is constantly reformed, a large amount of new displays such as liquid crystal display, flat-panel monitor etc. start to take
For Traditional CRT Display, causes a large amount of CRT to enter and scrap processing stage.China initially entered the CRT dates of retirement from 2003,
2008-2015 peaks the phase, and television set is scrapped especially prominent.According to statistics, 2011, China's household appliances passed through " with old
Renewing " form recycles waste and old television set about 5149.7 ten thousand, wherein 82% is CRT monitor television set.
The UV or X-ray generated in order to avoid electron gun leaks, and CRT glass is added to a large amount of oxidation in preparation process
Lead, content are about 20-23wt.%.CRT flint glass belongs to hazardous waste, it has also become the emphasis of electronic waste processing concern.According to
Statistics, nearly 500,000 tons of the discarded CRT flint glass that in the past few years China recycles every year.Early in 2000, Stephen etc. used TCLP
Toxicity leaching experiment carries out toxicity leaching experiment to CRT flint glass, the results show that its lead leaching concentration is up to 75.3mg/L.
Therefore, the superseded Traditional CRT Display Waste Household Electric Appliances of China's high-volume are faced, discarded CRT glass how is handled and has become
The important topic of field of environment protection.
The secondary use research of discarded CRT flint glass resources at present is concentrated mainly on recycling lead, solidification landfill, prepares glass
Glass product and construction material etc..Since the recycling value of lead is little, the rate of recovery is low, will produce in removal process a large amount of
New lead containing sludge, economic feasibility are poor；And be exclusively used in CRT glass lead smelting method for vacuum smelting, mechanical activation method although
It is higher to the rate of recovery of lead, but at present still in the laboratory research stage, therefore the mode for recycling lead is not used mostly.Solidification landfill
Although a kind of innoxious process for treating, in order to avoid lead contamination does not recommend generally.Preparing novel glass and being one has
The approach of effect, but have the shortcomings that treatment temperature is high, the reaction time is long, energy consumption is big, industrial applications are restricted.Cause
This, the CRT flint glass that application is strong, innoxious handles Land use systems, is increasingly paid attention to by people.Utilize CRT flint glass
It is the effective way for realizing harmless treatment and secondary use to prepare ceramics.
The pollution waste residue that red mud is discharged when being aluminum smelting industry extraction aluminium oxide, average often produces 1 ton of aluminium oxide, attached
Band generates 1.0~2.0 tons of red muds.China is used as the fourth-largest alumina producing state of the world, the red mud discharged every year up to tens million of
Ton.A large amount of red mud cannot be utilized substantially effectively, and the stockyard of large area can only be relied on to stack, occupy a large amount of soils, right
Environment has prodigious potential danger.Increasingly increase constantly the carrying to environmental protection consciousness with people with red mud quantum of output
Height multi-channelly handles and utilizes red mud, extremely urgent.
Invention content
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of cathode-ray
The innoxious method for preparing ceramics of pipe glass.This method mixes the CRT cone glass after crushing with red mud (red mud),
High-temperature heat treatment is carried out after compression molding, and the lead in CRT is cured to stable crystalline phase PbFe12O9(magnetoplumbite)
In, discard CRT glass harmless treatments to realize.
The purpose of the present invention is realized by following proposal：
A kind of innoxious method for preparing ceramics of cathode-ray tube glass, mainly includes the following steps that：
Cathode tube is subjected to screen cone separation, the cone glass of gained after crushing further clay into power by ball, then by institute
The cone glass powder obtained is put into according to different proportion in ball mill with red mud to be mixed, and mixed material is obtained；Mixed material is dried,
And it is pressed into molding, it is subsequently placed in Muffle furnace and be heat-treated up to innoxious ceramics.
It is further to use ball milling after grain size is 1~3mm that the cathode-ray tube glass powder, which refers to by cone glass crushing,
Machine wears into 1~5 micron of powder.
The red mud is that aluminum smelting industry extracts the pollution waste residue being discharged after aluminium oxide, and preferably Bayer process aluminium metallurgy method obtains
The red mud arrived, main component Fe2O3、CaO、Al2O3、SiO2, wherein Fe2O3Content be 30~60wt%.
The mass ratio of cone glass powder and red mud used is 5:95~30:70, preferably 25:75.
The drying refers in 120 DEG C of dry 12h.
The compacting refers to being suppressed at 200~300MPa, preferably in 250MPa.
The compression moulding refers to that arbitrary bulk is obtained under above-mentioned pressure, preferably cylindrical cake, when for cylinder
When cake, a diameter of 20mm, thickness 3mm.
The heat treatment refers to being handled at 800~1200 DEG C 1~15 hour, and 10h is preferably handled at 900 DEG C.
The present invention mechanism be：
This method mixes CRT cone glass powder with red mud, and high-temperature heat treatment is carried out after tabletting, and heat treatment is main anti-
It should be：PbO+6Fe2O3=PbFe12O19, the lead in CRT is cured to stable crystalline phase PbFe12O9(magnetoplumbite)
In, discard CRT glass harmless treatments to realize.
The present invention compared with the existing technology, has the following advantages and advantageous effect：
(1) red mud used herein is aluminum i ndustry waste residue, need not add other materials, of low cost, is realized simultaneously
The harmless treatment of two kinds of solid waste..
(2) in the present invention CRT flint glass usage amount up to 25wt.%, it can be achieved that the mesh of CRT glass is discarded in a large amount of processing
Mark.
(3) present invention not will produce toxic and harmful gas during heat treatment, will not be polluted to air.
(4) present invention carries out under normal pressure, and required temperature is relatively low (900 DEG C), simple for process, easy to operate, is easy to
Carry out scale application.
(5) lead is fixed in crystal structure by the present invention, and the final leaching concentrations of ceramic product Pb are less than 0.1mg/L, can
Security landfill can also be used as architectural pottery, industrial ceramics and glaze etc. and utilize again.
Description of the drawings
Fig. 1 is to be 1000 DEG C in heat treatment temperature, and when heat treatment time is 5h, CRT glass presses different quality ratio with red mud
The XRD spectrum of the innoxious ceramic product prepared.
Fig. 2 is to be 1000 DEG C in heat treatment temperature, and when heat treatment time is 5h, CRT glass presses different quality ratio with red mud
PbFe in the innoxious ceramic product prepared12O9XRD characteristic peak intensity contrast figures.
It is 25 that Fig. 3, which is in CRT glass and red mud mass ratio,:75, when heat treatment time is 5h, at a temperature of different heat treatment
The XRD spectrum of the innoxious ceramic product prepared.
It is 25 that Fig. 4, which is in CRT glass and red mud mass ratio,:75, when heat treatment time is 5h, at a temperature of different heat treatment
PbFe in the innoxious ceramic product prepared12O9XRD characteristic peak intensity contrast figures.
It is 25 that Fig. 5, which is in CRT glass and red mud mass ratio,:75, heat treatment temperature is 900 DEG C, through the different heat treatment time
The XRD spectrum of the innoxious ceramic product prepared.
It is 25 that Fig. 6, which is in CRT glass and red mud mass ratio,:75, heat treatment temperature is 900 DEG C, through the different heat treatment time
PbFe in the innoxious ceramic product prepared12O9XRD characteristic peak intensity contrast figures.
Fig. 7 is CRT glass and red mud mass ratio is 25:75, heat treatment temperature is 900 DEG C, when the thermally treated time is 10h
The TCLP toxicity characteristic leaching procedures comparing result (Pb after 16 days of the innoxious ceramic product and the untreated CRT cone glass powder that prepare
Leaching concentration).
Specific implementation mode
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Embodiment 1：Cathode-ray tube glass harmless treatment prepares ceramics:
(1) old colorful display screen CRT is subjected to cone screen separation, takes the leaded cone glass of tapering position as sample.Using wet
Formula washing method removes the coating on leaded cone glass surface.
(2) the leaded cone glass for removing face coat is subjected to coarse crushing at the particle that grain size is 1~3mm, after coarse crushing
Glass particle is put into planetary ball mill and further crushes, about 1~5 micron of grain size.
XRF analysis is carried out to leaded cone glass powder, chemical composition is as shown in table 1：
The chemical composition of 1 leaded cone glass powder of table
(3) by leaded cone glass powder, according to a certain percentage with red mud (Pingguo Aluminium Industry Co., Guangxi) (5:95,10:90,
15:85,20:80,25:75,30:70) it mixes, is uniformly mixed in the ball mill.
(4) said mixture material is placed in drying 12 hours in 120 DEG C of baking ovens, obtains dry mixed material.
(5) at room temperature, under 250MPa pressure, said mixture material is pressed into a diameter of 20mm, thickness is about 3mm's
Cylindrical cake is conducive to heat treatment reaction to ensure to be tightly combined between powder during heating.
(6) above-mentioned cylindrical cake is put into corundum crucible, be placed in Muffle furnace.Muffle furnace is heated to 1000 DEG C, temperature
After stabilization, heat treatment time is 5 hours.
(7) after the completion of being heat-treated, muffle furnace is reduced to by room temperature with 10 DEG C of rate of temperature fall per minute.
(8) cylindrical cake in crucible is taken out, powder is broken into, XRD analysis is carried out to it.
In embodiment 1 when heat treatment temperature is 1000 DEG C, and heat treatment time is 5h, CRT glass is with red mud by not homogeneity
The XRD spectrum of the innoxious ceramic product than preparation is measured as shown in Figure 1, PbFe in ceramic product12O9XRD feature peak intensities pair
It is more as shown in Figure 2 than scheming.As can be seen that when leaded CRT glass powders ratio is 5wt.% from Fig. 1 and Fig. 2, that is, have
PbFe12O9The generation of phase.And with the increase of leaded CRT glass powders ratio, PbFe12O9The signal of phase gradually increases.Than
When example is 25wt.%, highest PbFe is obtained12O9Crystalline content.When ratio continues to be increased to 30wt.%, PbFe12O9The letter of phase
Number then weaken.Therefore, leaded CRT glass powders and red mud optimum quality ratio are 25:75.
Embodiment 2：Cathode-ray tube glass harmless treatment prepares ceramics
Embodiment 2 and embodiment 1 difference lies in：
The mass ratio of leaded cone glass powder and red mud is 25 in step (3):75；
The condition of heat treatment described in step (6) is to be heat-treated 5h in 700~1200 DEG C.
The XRD spectrum for the innoxious ceramic product that the present embodiment is prepared at a temperature of different heat treatment is as shown in figure 3, ceramics
PbFe in product12O9XRD characteristic peak intensity contrast figures it is as shown in Figure 4.From Fig. 3 and Fig. 4 as can be seen that when temperature is 800
DEG C when, PbFe can be observed12O9The formation of phase.When temperature is increased to 900 DEG C, PbFe12O9The signal of phase significantly increases.Hereafter
When temperature continues to increase, PbFe12O9The signal of phase gradually weakens with the raising of temperature.Therefore, optimization heat treatment temperature is
900℃。
Embodiment 3：Cathode-ray tube glass harmless treatment prepares ceramics
Embodiment 3 the difference from example 2 is that：
The condition of heat treatment described in step (6) is that 1~10h is heat-treated in 900 DEG C.
The XRD spectrum for the innoxious ceramic product that the present embodiment is prepared through the different heat treatment time is as shown in figure 5, ceramics production
PbFe in product12O9XRD characteristic peak intensity contrast figures it is as shown in Figure 6.As can be known from Fig. 5 and Fig. 6, with heat treatment time
Increase, PbFe12O9The signal of phase gradually increases.After being heat-treated 10h, PbFe12O9Mutually have reached saturation, it is contemplated that heat treatment institute band
The thermal energy consumption problem come, optimization heat treatment time are 10h.
Embodiment 4：TCLP (Toxicity Characteristic Leaching Procedure) toxicity characteristic leaching procedure
The ceramic product that 10h is obtained will be heat-treated in embodiment 3 in 900 DEG C and is improved type TCLP (Toxicity
Characteristic Leaching Procedure) toxicity characteristic leaching procedure, while leaching examination is carried out to CRT cone glass powder
It tests as a contrast.
The acetum of addition 10mL pH=4.88 and 0.5g ceramic powders or CRT cone glass in 15mL centrifuge tubes
Powder rotates 18h~22d respectively, then tests Pb concentration in acetum.
Obtained ceramic powders of 10h and unprocessed are heat-treated in 900 DEG C when TCLP proceeds to 16d, in embodiment 3
The TCLP toxicity characteristic leaching procedures of CRT cone glass powder the results are shown in Figure 7, it can be seen from figure 7 that untreated CRT
The final Pb leaching concentrations of cone glass powder reach 400mg/L or more, and ceramics Pb leaching concentrations are less than 0.1mg/L after hot setting.
Show that CRT cone glass and red mud, Pb is fixed on crystal knot with certain proportion innoxious ceramic preparation process according to the invention
In structure, leaching risk is extremely low in long-range circumstances exposure.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of method that cathode-ray tube glass harmless treatment prepares ceramics, it is characterised in that include the following steps：It will be cloudy
Pole pipe carries out screen cone separation, and the cone glass of gained after crushing further clay into power by ball, then by the cone glass powder of gained
End, which is put into red mud in ball mill, to be mixed, and mixed material is obtained；Mixed material is dried, and is pressed into molding, is subsequently placed in horse
It not carries out being heat-treated up to innoxious ceramics in stove.
2. the method that cathode-ray tube glass harmless treatment according to claim 1 prepares ceramics, it is characterised in that：
The mass ratio of cone glass powder and red mud used is 5:95~30:70.
3. the method that cathode-ray tube glass harmless treatment according to claim 2 prepares ceramics, it is characterised in that：
The mass ratio of cone glass powder and red mud used is 25:75.
4. the method that cathode-ray tube glass harmless treatment according to claim 1 prepares ceramics, it is characterised in that：
The heat treatment refers to 1~15h of processing at 800~1200 DEG C.
5. the method that cathode-ray tube glass harmless treatment according to claim 4 prepares ceramics, it is characterised in that：
The heat treatment refers to processing 10h at 900 DEG C.
6. the method that cathode-ray tube glass harmless treatment according to claim 1 prepares ceramics, it is characterised in that：
It is further to be ground with ball mill after grain size is 1~3mm that the cathode-ray tube glass powder, which refers to by cone glass crushing,
At 1~5 micron of powder.
7. the method that cathode-ray tube glass harmless treatment according to claim 1 prepares ceramics, it is characterised in that：
The red mud is the red mud that Bayer process aluminium metallurgy method obtains, main component Fe2O3、CaO、Al2O3、SiO2, wherein Fe2O3
Content be 30~60wt%.
8. the method that cathode-ray tube glass harmless treatment according to claim 1 prepares ceramics, it is characterised in that：
The drying refers in 120 DEG C of dry 12h；
The compacting refers to being suppressed at 200~300MPa.
9. the method that cathode-ray tube glass harmless treatment according to claim 1 prepares ceramics, it is characterised in that：
The compression moulding refers to being pressed into arbitrary bulk under stress.
10. the method that cathode-ray tube glass harmless treatment according to claim 9 prepares ceramics, it is characterised in that：
The compression moulding refers to being pressed into cylinder cheese under stress, a diameter of 20mm, thickness 3mm.
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| CN201710058226.0A CN108341656B (en) | 2017-01-23 | 2017-01-23 | Method for preparing ceramic from cathode ray tube glass in harmless manner |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408802A (en) * | 2020-11-27 | 2021-02-26 | 昆明理工大学 | Method for preparing microcrystalline glass by using CRT (cathode ray tube) cone glass |
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| CN105541371A (en) * | 2015-12-24 | 2016-05-04 | 湖北工业大学 | Foamed ceramic prepared by virtue of oil well earth and waste glass and method for foamed ceramic |
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| CN102643994A (en) * | 2012-05-07 | 2012-08-22 | 清华大学 | Waste cathode-ray tube cone glass machinery activation wet-process sulphur treatment method |
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| CN112408802A (en) * | 2020-11-27 | 2021-02-26 | 昆明理工大学 | Method for preparing microcrystalline glass by using CRT (cathode ray tube) cone glass |
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Address after: No. 808, Tianyuan Road, Tianhe District, Guangzhou, Guangdong 510316 Applicant after: Institute of ecological environment and soil, Guangdong Academy of Sciences Address before: No. 808, Tianyuan Road, Tianhe District, Guangzhou, Guangdong 510316 Applicant before: GUANGDONG INSTITUTE OF ECO-ENVIRONMENT AND SOIL SCIENCES |
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