CN108341656B - Method for preparing ceramic from cathode ray tube glass in harmless manner - Google Patents
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- CN108341656B CN108341656B CN201710058226.0A CN201710058226A CN108341656B CN 108341656 B CN108341656 B CN 108341656B CN 201710058226 A CN201710058226 A CN 201710058226A CN 108341656 B CN108341656 B CN 108341656B
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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
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- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
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Abstract
The invention belongs to the field of hazardous waste disposal and resource utilization, and discloses a method for preparing ceramics by cathode ray tube glass in a harmless manner. The method comprises the following steps: carrying out screen cone separation on a cathode tube, further ball-milling the obtained cone glass into powder after crushing, and then putting the obtained cone glass powder and red mud into a ball mill according to different proportions to be mixed to obtain a mixed material; and drying the mixed material, pressing and molding, and then placing the mixture in a muffle furnace for heat treatment to obtain the harmless ceramic. Mixing CRT cone glass powder with red mud, tabletting, high-temperature heat treatment, and solidifying lead in CRT to stable crystal phase PbFe12O9Thereby realizing the harmless treatment of the waste CRT glass. The final Pb leaching concentration of the ceramic product is lower than 0.1mg/L, and the ceramic product can be safely buried and also can be used as building ceramic, industrial ceramic, glaze and the like.
Description
Technical Field
The invention belongs to the field of hazardous waste disposal and resource utilization, and particularly relates to a method for preparing ceramics by cathode ray tube glass in a harmless manner.
Background
A Cathode Ray Tube (CRT) is the earliest and most widely used display technology device, has the advantages of mature technology, high reliability, low cost, and the like, and has been widely used in display devices such as televisions, computers, industrial monitors, and the like. As display technologies continue to evolve, a large number of new displays, such as liquid crystal displays, flat panel displays, etc., begin to replace conventional CRT displays, resulting in a large number of CRTs entering a waste stage. China starts to enter a CRT (cathode ray tube) rejection period from 2003, and 2008-2015 reaches a peak period, so that the television rejection is particularly prominent. According to statistics, in 2011, about 5149.7 ten thousands of waste televisions are recycled by domestic appliances in a form of 'replacing old appliances with new appliances', wherein 82% of the waste televisions are CRT display televisions.
In order to prevent UV or X-ray leakage from the electron gun, the CRT glass is prepared by adding a large amount of lead oxide in an amount of about 20 to 23 wt.%. CRT lead-containing glass belongs to dangerous waste and has become the focus of electronic waste disposal attention. According to statistics, the amount of waste CRT lead-containing glass recycled in China every year is nearly 50 ten thousand tons in recent years. As early as 2000, Stephen et al performed toxic leaching experiments on CRT lead-containing glass using TCLP toxic leaching experiments, and the results showed that the lead leaching concentration was as high as 75.3 mg/L. Therefore, in order to solve the problem of the traditional CRT display waste household electrical appliances eliminated in large quantities in China, how to treat the waste CRT glass becomes an important topic in the field of environmental protection.
At present, the research on the secondary utilization of the waste CRT lead-containing glass resources mainly focuses on the aspects of lead recovery, solidification and landfill, preparation of glass products and building materials and the like. Because the recycling value of the lead is not high, the recovery rate is low, a large amount of new lead-containing waste residues can be generated in the recovery process, and the economic feasibility is poor; and the vacuum smelting method and the mechanical activation method which are specially used for smelting the lead of the CRT glass have higher lead recovery rate, but are still in the laboratory research stage at present, so the lead recovery mode is mostly not adopted. Solidification landfill is a harmless treatment technique, but is generally not recommended to avoid lead contamination. The preparation of the novel glass is an effective way, but has the defects of high treatment temperature, long reaction time and high energy consumption, and the industrial application of the novel glass is limited. Therefore, the harmless lead-containing glass for CRT has been increasingly used for the treatment. The preparation of ceramics by using CRT lead-containing glass is an effective way for realizing harmless treatment and secondary utilization.
The red mud is polluting waste residue discharged when aluminum oxide is extracted in the aluminum production industry, and generally 1.0-2.0 tons of red mud are additionally generated when 1 ton of aluminum oxide is produced on average. China, as the fourth major alumina producing country in the world, discharges up to thousands of tons of red mud every year. A large amount of red mud cannot be fully and effectively utilized, and can only be stacked by a large-area yard, thereby occupying a large amount of land and having great potential danger to the environment. With the increasing output of red mud and the increasing awareness of people on environmental protection, the multi-channel treatment and utilization of red mud are urgent.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the present invention provides a method for preparing a ceramic by using a cathode ray tube glass in a harmless manner. The method mixes crushed CRT cone glass with red mud (red mud), carries out high-temperature heat treatment after tabletting and forming, and solidifies lead in the CRT to a stable crystal phase PbFe12O9And (magnetoplumhite), thereby realizing harmless treatment of the waste CRT glass.
The purpose of the invention is realized by the following scheme:
a method for preparing ceramics by harmlessly preparing cathode ray tube glass mainly comprises the following steps:
carrying out screen cone separation on a cathode tube, further ball-milling the obtained cone glass into powder after crushing, and then putting the obtained cone glass powder and red mud into a ball mill according to different proportions to be mixed to obtain a mixed material; and drying the mixed material, pressing and molding, and then placing the mixture in a muffle furnace for heat treatment to obtain the harmless ceramic.
The glass powder of the cathode ray tube is powder obtained by grinding cone glass into powder with the particle size of 1-3 mm and then grinding the powder into powder with the particle size of 1-5 microns by using a ball mill.
The red mud is pollution waste residue discharged after aluminum oxide is extracted in aluminum production industry, preferably the red mud obtained by a Bayer process aluminum production method, and the main component is Fe2O3、CaO、Al2O3、SiO2In which Fe2O3The content of (B) is 30-60 wt%.
The mass ratio of the cone glass powder to the red mud is 5: 95-30: 70, and preferably 25: 75.
The drying refers to drying at 120 ℃ for 12 h.
The pressing is performed under 200-300 MPa, and preferably 250 MPa.
The press molding means that any block-shaped, preferably cylindrical cake is obtained under the above-mentioned pressure, and when the cake is cylindrical, the diameter is 20mm and the thickness is 3 mm.
The heat treatment is carried out at 800-1200 ℃ for 1-15 hours, preferably at 900 ℃ for 10 hours.
The mechanism of the invention is as follows:
the method mixes CRT cone glass powder with red mud, carries out high-temperature thermal treatment after tabletting, and the main reaction of the thermal treatment is as follows: PbO +6Fe2O3＝PbFe12O19Solidifying lead in CRT to stable crystal phase PbFe12O9And (magnetoplumhite), thereby realizing harmless treatment of the waste CRT glass.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the red mud used in the invention is aluminum industrial waste residue, other materials are not needed to be added, the cost is low, and the harmless treatment of two solid wastes is realized. .
(2) The usage amount of the CRT lead-containing glass in the invention can reach 25 wt.%, and the aim of treating a large amount of waste CRT glass can be realized.
(3) The invention can not generate poisonous and harmful gas in the heat treatment process and can not pollute the atmosphere.
(4) The method is carried out under normal pressure, the required temperature is relatively low (900 ℃), the process is simple, the operation is simple, and the large-scale application is easy to carry out.
(5) According to the invention, lead is fixed in a crystal structure, the final leaching concentration of Pb of a ceramic product is lower than 0.1mg/L, and the lead can be safely buried and can be reused as building ceramic, industrial ceramic, glaze and the like.
Drawings
FIG. 1 is an XRD spectrum of harmless ceramic products prepared from CRT glass and red mud according to different mass ratios at a heat treatment temperature of 1000 ℃ and a heat treatment time of 5 h.
FIG. 2 shows PbFe in harmless ceramic products prepared from CRT glass and red mud at different mass ratios at a heat treatment temperature of 1000 deg.C for 5h12O9Comparing the intensity of XRD characteristic peak.
FIG. 3 is an XRD pattern of harmless ceramic products prepared at different heat treatment temperatures at a CRT glass to red mud mass ratio of 25:75 and a heat treatment time of 5 h.
FIG. 4 shows PbFe in harmless ceramic products prepared at different heat treatment temperatures when the mass ratio of CRT glass to red mud is 25:75 and the heat treatment time is 5 hours12O9Comparing the intensity of XRD characteristic peak.
FIG. 5 is an XRD spectrum of harmless ceramic products prepared by different heat treatment times at a CRT glass to red mud mass ratio of 25:75 and a heat treatment temperature of 900 ℃.
FIG. 6 shows PbFe in harmless ceramic products prepared by different heat treatment times at a CRT glass to red mud mass ratio of 25:75 and a heat treatment temperature of 900 deg.C12O9Comparing the intensity of XRD characteristic peak.
FIG. 7 shows the comparative results of TCLP toxicity leaching tests (Pb leaching concentration after 16 days) of the harmless ceramic products prepared when the mass ratio of CRT glass to red mud is 25:75, the heat treatment temperature is 900 ℃ and the heat treatment time is 10 hours, and the untreated CRT cone glass powder.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The reagents used in the examples are commercially available without specific reference.
Example 1: preparing ceramic by performing harmless treatment on cathode ray tube glass:
(1) and (3) carrying out cone screen separation on the old color display screen CRT, and taking lead-containing cone glass at the cone position as a sample. And removing the coating on the surface of the lead-containing cone glass by adopting a wet washing method.
(2) And coarsely crushing the lead-containing cone glass with the surface coating removed into particles with the particle size of 1-3 mm, and further crushing the coarsely crushed glass particles in a planetary ball mill to obtain particles with the particle size of about 1-5 microns.
XRF analysis of the leaded cone glass powder was performed and the chemical composition is shown in Table 1:
TABLE 1 chemical composition of lead-containing cone glass powder
(3) The lead-containing cone glass powder was mixed with red mud (Guangxi Pingguo Al industries Co., Ltd.) (5:95, 10:90, 15:85, 20:80, 25:75, 30:70) in a certain ratio, and the mixture was uniformly mixed in a ball mill.
(4) And (3) drying the mixed material in an oven at 120 ℃ for 12 hours to obtain a dried mixed material.
(5) Pressing the mixed material into a cylindrical cake with the diameter of 20mm and the thickness of about 3mm at room temperature under the pressure of 250MPa so as to ensure that the powder is tightly combined in the heating process and facilitate the heat treatment reaction.
(6) The cylindrical cake was placed in a corundum crucible and placed in a muffle furnace. The muffle furnace is heated to 1000 ℃, and after the temperature is stabilized, the heat treatment time is 5 hours.
(7) After the heat treatment was completed, the muffle furnace temperature was lowered to room temperature at a temperature lowering rate of 10 ℃ per minute.
(8) The cylindrical cake in the crucible was taken out, crushed into powder, and subjected to XRD analysis.
In example 1, XRD patterns of harmless ceramic products prepared from CRT glass and red mud at different mass ratios are shown in figure 1 when the heat treatment temperature is 1000 ℃ and the heat treatment time is 5h, and PbFe in the ceramic products12O9The characteristic peak intensity contrast diagram of XRD is shown in figure 2. As can be seen from fig. 1 and 2, when the proportion of the lead-containing CRT glass powder is 5 wt.%, PbFe is present12O9And (4) generation of phases. And PbFe increases with the proportion of the lead-containing CRT glass powder12O9The signal of the phase gradually increases. At a ratio of 25 wt.%, the highest PbFe is obtained12O9Crystal content. PbFe when the proportion is further increased to 30 wt%12O9The phase signal is then attenuated. Therefore, the optimal mass ratio of the lead-containing CRT glass powder to the red mud is 25: 75.
Example 2: method for preparing ceramic by harmless treatment of cathode ray tube glass
Example 2 differs from example 1 in that:
the mass ratio of the lead-containing cone glass powder to the red mud in the step (3) is 25: 75;
the heat treatment condition in the step (6) is heat treatment for 5 hours at 700-1200 ℃.
The XRD patterns of the harmless ceramic products prepared in the example at different heat treatment temperatures are shown in FIG. 3, and PbFe in the ceramic products12O9The characteristic peak intensity contrast diagram of XRD is shown in figure 4. As can be seen from FIGS. 3 and 4, PbFe was observed at a temperature of 800 deg.C12O9And (4) forming a phase. PbFe when the temperature is increased to 900 deg.C12O9The signal of the phase is significantly enhanced. After that, the temperature is increased continuously, PbFe12O9The phase signal gradually decreases with increasing temperature. Therefore, the heat treatment temperature is optimized to 900 ℃.
Example 3: method for preparing ceramic by harmless treatment of cathode ray tube glass
Example 3 differs from example 2 in that:
the heat treatment condition in the step (6) is heat treatment for 1-10 h at 900 ℃.
The XRD patterns of the harmless ceramic products prepared by different heat treatment times in the example are shown in FIG. 5, and PbFe in the ceramic products12O9The characteristic peak intensity contrast of XRD is shown in figure 6. As can be seen from FIGS. 5 and 6, PbFe increases with the heat treatment time12O9The signal of the phase gradually increases. After heat treatment for 10h, PbFe12O9The phases are saturated, and the heat treatment time is optimized to be 10h in consideration of the heat energy consumption problem caused by heat treatment.
Example 4: TCLP (toxicity testing of viral Leaching procedure) toxicity Leaching test
The ceramic product obtained in example 3 after heat treatment at 900 ℃ for 10h was subjected to a modified TCLP (toxicity characterised Leaching procedure) toxicity Leaching test, while the CRT cone glass powder was subjected to a Leaching test as a control.
A 15mL centrifugal tube was charged with 10mL of an acetic acid solution having a pH of 4.88 and 0.5g of a ceramic powder or CRT cone glass powder, rotated for 18 hours to 22 days, respectively, and then the acetic acid solution was tested for Pb concentration.
When TCLP is carried out for 16d, the results of TCLP toxicity leaching tests of the ceramic powder obtained in example 3 after heat treatment for 10h at 900 ℃ and the untreated CRT cone glass powder are shown in FIG. 7, and it can be seen from FIG. 7 that the final Pb leaching concentration of the untreated CRT cone glass powder is more than 400mg/L, and the Pb leaching concentration of the ceramic after high-temperature curing is lower than 0.1 mg/L. The harmless ceramic preparation process of the invention has the advantages that Pb is fixed in a crystal structure, and the leaching risk is extremely low in long-term environmental exposure.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A method for preparing ceramics by harmless treatment of cathode ray tube glass is characterized by comprising the following steps: carrying out screen cone separation on a cathode tube, further ball-milling the obtained cone glass into powder after crushing, and then putting the obtained cone glass powder and red mud into a ball mill for mixing to obtain a mixed material; drying the mixed material, pressing and forming, and then placing the mixture in a muffle furnace for heat treatment to obtain harmless ceramic;
the heat treatment refers to treatment at 900 ℃ for 10 hours;
the mass ratio of the cone glass powder to the red mud is 5: 95-25: 75.
2. The method for producing ceramics by harmless treatment of glass for a cathode ray tube according to claim 1, wherein:
the glass powder of the cathode ray tube is powder obtained by grinding cone glass into powder with the particle size of 1-3 mm and then grinding the powder into powder with the particle size of 1-5 microns by using a ball mill.
3. The method for producing ceramics by harmless treatment of glass for a cathode ray tube according to claim 1, wherein:
the red mud is obtained by a Bayer process aluminum production method, and the main component of the red mud is Fe2O3、CaO、Al2O3、SiO2In which Fe2O3The content of (B) is 30-60 wt%.
4. The method for producing ceramics by harmless treatment of glass for a cathode ray tube according to claim 1, wherein:
the drying refers to drying at 120 ℃ for 12 h;
the pressing is performed under 200-300 MPa.
5. The method for producing ceramics by harmless treatment of glass for a cathode ray tube according to claim 1, wherein:
the pressing forming refers to pressing into any block shape under pressure.
6. The method for producing ceramics by harmless treatment of glass for a cathode ray tube according to claim 5, wherein:
the pressing forming means that the materials are pressed into a cylindrical cake shape under pressure, the diameter of the cylindrical cake shape is 20mm, and the thickness of the cylindrical cake shape is 3 mm.
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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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| WO2009084484A1 (en) * | 2007-12-28 | 2009-07-09 | Nippon Crucible Co., Ltd. | Casting material based on silicon carbide |
| 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 |
| CN102660686A (en) * | 2012-05-07 | 2012-09-12 | 清华大学 | Method for treating waste cathode ray tube (CRT) cone glass by strengthening acid leaching through mechanical activation technology |
| CN102838282A (en) * | 2012-09-28 | 2012-12-26 | 刘立强 | Method for preparing high-strength foam glass by utilizing red mud and waste glass |
| CN103280390A (en) * | 2013-06-09 | 2013-09-04 | 南开大学 | Innocent treatment method for leaded glass of abandoned cathode ray tube |
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