CN107473593B - Method for preparing microporous high silica glass powder from waste CRT screen glass - Google Patents
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
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Abstract
The invention relates to a method for preparing micropore high silica glass powder from waste CRT screen glass, which comprises the steps of firstly, crushing the waste CRT screen glass to a certain fineness, and adding 20-50% of B into the screen glass powder2O3、H3BO3、P2O5The potassium carbonate powder mixture (the mass ratio of the four ingredients is 60-80:10-20:5-10:1-10) and fully and uniformly mixed; smelting the mixed powder at 1000-1500 ℃ for 0-4 h; then carrying out phase-splitting heat treatment on the smelted product at 500-650 ℃ for 0-24 h; then the blocky product is crushed and then is treated by acid leaching. The removal rate of barium and strontium is between 98.00 and 99.60 percent, and the obtained high silica glass powder SiO2The content is 88.85 percent to 97.20 percent, and the pore size range of the microporous high silica glass powder is 5 nm to 300 nm. The process established by the invention is simple to operate, has high barium and strontium removal rate, and can prepare high silica glass powder with higher economic value, so the invention has wide industrial application prospect.
Description
Technical Field
The invention relates to a new technology for recycling electronic garbage, belongs to a new technology for recycling hazardous solid wastes in the fields of environmental protection and comprehensive utilization of resources, and is particularly suitable for pollution control and resource utilization of waste barium strontium-containing CRT screen glass.
Background
The waste Cathode ray tube (cathodal ray tube) screen glass contains a large amount of heavy metal oxides BaO and SrO (both in the range of 9-13 wt%). CRT displays are currently being eliminated by a large number of advanced display technologies, and a huge amount of waste CRT screen glass will be generated every year worldwide. If the CRT screen glass is not effectively treated and recycled, the waste heavy metal barium strontium-containing glass accumulated in the open air can occupy a large amount of valuable land resources, and the free landfill can cause the heavy metal pollution of the surrounding soil and water, thereby bringing serious harm to the ecological environment and the human health. However, barium and strontium are also valuable chemical raw materials and have high recycling economic value, so that the recycling of heavy metals barium and strontium in the screen glass has important significance for environmental protection and barium and strontium resource recycling in China.
The waste CRT screen glass can be used for preparing building materials, radiation-proof materials, novel glass-based materials and the like. However, the new products still contain a large amount of heavy metals of barium and strontium, and the potential threat of the heavy metals to the environment cannot be eliminated. Therefore, the technology for separating and recovering barium and strontium in CRT screen glass is very important. Common heavy metal removal methods mainly include pyrometallurgy and wet acid leaching. The traditional pyrometallurgical process utilizes a carbothermic reduction process, so that heavy metal oxides in the glass can be reduced to be in an elemental state and further removed from the glass. However, BaO and SrO in the screen glass cannot be reduced by carbothermal, so that barium and strontium in the screen glass cannot be removed by traditional pyrometallurgy. In addition, BaO and SrO in the cone glass are made of SiO4The tetrahedron is tightly wrapped to form a continuous three-dimensional network structure, so that the barium and the strontium in the screen glass are difficult to remove by common wet acid leaching. Although alkali fusion can be used to form SiO in the glass2Dissolved away so that barium and strontium are recovered as bottom dross. However, the alkali fusion method has high alkali consumption, causes high treatment cost, and is not suitable for industrial treatment. Therefore, the invention aims at the problems to develop a method for preparing microporous high-silica glass powder from waste CRT screen glass, and the method can not remove barium and strontium in the screen glass rapidly and efficiently, and can convert the screen glass into the microporous high-silica glass powder with higher economic value.
The high silica glass has many excellent performances similar to quartz glass, such as thermal expansion coefficient slightly larger than that of quartz glass, thermal shock resistance up to 800 ℃, chemical corrosion resistance and mechanical strength similar to those of quartz glass. Thus, high silica glass is often used as the quartz glass substituteThe product is used for manufacturing special purpose glass such as heat-resisting vessels, instruments with complex shapes, vessels for smelting uranium, high-pressure mercury lamp tubes, tungsten bromide lamp tubes and the like. Phase separation is the first technique developed by corning, usa and used to make high silica glass. Na was first studied in 1938 by Hood and Norber2O-B2O3-SiO2Phase separation phenomenon in glass, and SiO produced by using the phenomenon2High silica glass (Vycor) with a content of more than 96%, microporous high silica glass being an intermediate product for the manufacture of Vycor glass. The microporous high silica glass has the advantages of uniform micropore distribution, large specific surface area, good adsorption performance and high radiation and chemical stability. In addition, the microporous high silica glass can be processed at high temperature to prepare high silica glass, high silica glass fiber and other products. The high silica products have the characteristics of high temperature resistance, difficult breakage, no bubbles, strong light transmittance and the like, and are widely applied to the high-tech fields of aviation, aerospace, chemical engineering, electronics, lamps and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention develops the microporous high silica glass powder which has simple process operation, low cost, high removal rate of heavy metal barium and strontium, high economic value and 5-300nm of micropore size and can be prepared while realizing the harmlessness of screen glass, and has wide industrialization prospect.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing microporous high silica glass powder from waste CRT screen glass is characterized by comprising the following steps:
step one, a pretreatment process: removing the fluorescent coating on the surface of the waste CRT screen glass after cone screen separation, crushing the CRT screen glass into particles with the diameter of 1-5 mm by using a combined crusher, and grinding the CRT screen glass particles into CRT screen glass powder with the diameter of 20-200 meshes by using a ball mill;
step two, a material preparation process: mixing CRT screen glass powder with B2O3、H3BO3、P2O5Mixing with potassium carbonate at a certain proportion, and continuously using ball millCrushing to 100-200 mesh (wherein B2O3、H3BO3、P2O560-80 mass ratio of potassium carbonate to 10-20 mass ratio of 5-10 mass ratio of 1-10 mass ratio of B)2O3、H3BO3、P2O5And potassium carbonate accounts for 20-50% of the total mass of the mixture;
step three, a high-temperature smelting process: putting the mixed CRT screen glass powder into a muffle furnace and carrying out smelting treatment at 1000-1500 ℃, wherein the heat preservation time is 0-4 h;
step four, a phase separation treatment process: and (3) carrying out phase separation treatment on the CRT screen glass subjected to high-temperature smelting treatment in the third step at 500-650 ℃, wherein the heat preservation time is 0.5-24 h.
Step five, a crushing procedure: crushing the blocky product treated by the phase splitting procedure in the fourth step to 100-200 meshes;
step six, acid leaching process: performing acid leaching treatment on the product treated in the crushing step in sequence by using nitric acid and sulfuric acid to obtain an acid leaching mixture, wherein the concentration of the used nitric acid is 0.5-10 mol/L, and the concentration of the sulfuric acid is 0.5-10 mol/L; wherein the volume ratio of the product treated in the crushing procedure to the nitric acid and the sulfuric acid is 1: 5-100;
step seven, a liquid-solid separation process: carrying out liquid-solid separation on the acid leaching mixture in the step six by a centrifugal or filtering method to respectively obtain acid leaching liquid and solid residues, and washing and drying the obtained solid residues to obtain microporous high silica glass powder without heavy metals of barium and strontium;
step eight, the pickle liquor recovery process: and D, recycling heavy metals barium and strontium in the acid leaching solution obtained in the step seven by a method of adding sulfuric acid for precipitation to obtain barium sulfate and strontium sulfate, recycling boric acid in the acid leaching solution by a freezing crystallization technology, and finally recycling nitric acid and sulfuric acid leaching solution.
In the second step B2O3、H3BO3、P2O5And potassium carbonate accounts for 20-40% of the total mass of the mixture, and the fineness of the CRT screen glass powder is 100-150 meshes by utilizing a ball mill.
And the high-temperature smelting in the third step is carried out under the condition of air or oxidizing atmosphere, the smelting temperature is 1100-1400 ℃, and the heat preservation time is 0.5-3 h.
The phase separation treatment temperature in the fourth step is 550-650 ℃, and the heat preservation time is 1-20 h.
The concentration of the nitric acid used in the sixth step is 1-8 mol/L, the concentration of the sulfuric acid is 1-7 mol/L, and the acid leaching condition is to soak for 30-240 min at the temperature of 90 ℃; the volume ratio of the product treated in the crushing procedure to the nitric acid and the sulfuric acid is 1: 5-50.
The invention has the beneficial effects that:
1. the method can efficiently and quickly remove heavy metals of barium and strontium in the screen glass, and the existing screen glass utilization technology is mostly focused on directly preparing building materials or other glass products, so that the aim of harmless treatment of the screen glass cannot be fulfilled.
2. The microporous high silica glass powder with higher economic added value is prepared from the waste CRT screen glass, the purity of silicon dioxide in the microporous high silica glass powder exceeds 96 percent, the size range of micropores is 5-300nm, and the microporous high silica glass powder can be used as an adsorbent or a catalyst carrier and the like. In the prior art, high-silica glass is prepared by using high-purity silicon oxide, sodium carbonate and boron oxide as raw materials, so that the raw material cost is high, and the obtained product is the high-silica glass in a non-powder form, so that the application of high-silica glass products in many fields is limited. The method not only enables the waste CRT screen glass to be efficiently utilized, reduces the cost of raw materials, but also realizes the resource utilization of dangerous wastes, and is beneficial to environmental protection.
3. The method has the advantages of simple process operation, short treatment time and low energy consumption, avoids the defects of the traditional pyrometallurgical process, alkali fusion process and the like, and is easy for large-scale industrial production.
4. The applicant repeatedly proves through a plurality of tests that when the CRT screen glass is ground to a certain particle size, the CRT screen glass can be mixed with the glass B2O3、H3BO3、P2O5And the high-temperature-resistant silicon dioxide and potassium carbonate additive form a good mixture, and a good separation effect is obtained during high-temperature smelting and phase separation treatment.
5. The crushing procedure is adopted after the phase separation treatment, and the massive phase separation product is crushed to a certain particle size, which is an innovative means obtained by a large number of experiments by the applicant. The traditional phase separation method needs to be soaked in acid liquor for about 10-20 hours, but the method greatly saves the processing time of the subsequent acid leaching process by adding a crushing process, shortens the acid leaching time to 0.5-4 hours, and can obviously improve the heavy metal acid leaching and removing effect, thereby laying a foundation for obtaining high-quality microporous high-silica glass powder and reducing the large-scale industrial production and cost.
6, the CRT screen glass is originally added with B with a certain proportion2O3、H3BO3、P2O5And potassium carbonate is used as an additive, and the four additives are matched with each other, so that two independent boron-rich phases and silicon-rich phases in a communicated structure can be rapidly generated in the phase separation treatment process, and heavy metals Ba and Sr and other alkali metal oxides in the screen glass can be simultaneously and thoroughly removed.
7. In the acid leaching process, nitric acid and sulfuric acid with certain concentration are sequentially adopted for acid leaching, so that the removal rate of heavy metals of barium, strontium and zirconium is ensured.
8. And finally, a recycling procedure of the acid leaching solution is developed, so that barium sulfate, strontium sulfate and boric acid can be recycled, the leaching solution can be recycled, the production cost is reduced, and pollution control and full utilization of resources are facilitated.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a photograph of a microporous high silica glass powder
FIG. 3 is a scanning electron micrograph of a microporous high silica glass powder
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1:
removing the fluorescent coating on the surface of the waste CRT screen glass after cone screen separation, crushing the CRT screen glass into particles with the diameter of 1 mm by using a combined crusher, and grinding the CRT screen glass particles into CRT screen glass powder with the diameter of 50 meshes by using a ball mill;
mixing CRT screen glass powder with B2O3、H3BO3、P2O5Mixing with potassium carbonate at a certain proportion, and continuously crushing to 100 meshes by using a ball mill, wherein B2O3、H3BO3、P2O5The mass ratio of the potassium carbonate to the potassium carbonate is 65:20:10:5, B2O3、H3BO3、P2O5And potassium carbonate accounts for 20% of the total mass of the mixture;
putting the mixed CRT screen glass powder into a muffle furnace and carrying out smelting treatment at 1000 ℃ in an air atmosphere, wherein the heat preservation time is 0 h;
carrying out phase separation treatment on the CRT screen glass subjected to high-temperature smelting treatment at 580 ℃ for 6 h;
crushing the blocky product obtained from the phase separation treatment product to 100 meshes;
adding the split-phase crushed product into 5mol/L nitric acid solution, soaking for 60min at 90 ℃, wherein the volume ratio of the product treated in the crushing procedure to the nitric acid is 1: 10;
performing liquid-solid separation on the acid leaching mixture by a centrifugal or filtering method to respectively obtain acid leaching solution and solid residue,
adding the acid-leached solid residues into 5mol/L sulfuric acid solution again, soaking for 60min at 90 ℃, wherein the volume ratio of the product treated in the crushing procedure to sulfuric acid is 1: 20;
carrying out liquid-solid separation on the acid leaching mixture by a centrifugal or filtering method, washing and drying the obtained solid residue to obtain microporous high silica glass powder without heavy metals of barium, strontium and zirconium;
and (3) recovering heavy metals barium and strontium in the recovered acid leaching solution by a method of adding sulfuric acid for precipitation to obtain barium sulfate and strontium sulfate, recovering boric acid in the acid leaching solution by a freezing crystallization technology, and finally recycling the nitric acid leaching solution.
Analyzed barium in CRT screen glassAnd strontium removal rates of 99.54% and 99.48%, respectively. The main component of the acid leaching residue is SiO2(96.29%), NaO (0.85%) and ZrO2(0.12%) and the micropore size of the micropore high silica glass powder is 5-300 nm.
Example 2:
removing the fluorescent coating on the surface of the waste CRT screen glass after cone screen separation, crushing the CRT screen glass into particles with the diameter of 3 mm by using a combined crusher, and grinding the CRT screen glass particles into CRT screen glass powder of 100 meshes by using a ball mill;
mixing CRT screen glass powder with B2O3、H3BO3、P2O5Mixing with potassium carbonate at a certain proportion, and continuously crushing to 100 meshes by using a ball mill, wherein B2O3、H3BO3、P2O5The mass ratio of the potassium carbonate to the potassium carbonate is 80:10:5:5, B2O3、H3BO3、P2O5And potassium carbonate accounts for 30% of the total mass of the mixture;
putting the mixed CRT screen glass powder into a muffle furnace and carrying out smelting treatment at 1200 ℃ in an air atmosphere, wherein the heat preservation time is 1 h;
carrying out phase splitting treatment on the CRT screen glass subjected to high-temperature smelting treatment at 600 ℃ for 3 h;
crushing the blocky product obtained from the phase separation treatment product to 150 meshes;
adding the split-phase crushed product into 3mol/L nitric acid solution, soaking for 60min at 90 ℃, wherein the volume ratio of the product treated in the crushing procedure to the nitric acid is 1: 30;
performing liquid-solid separation on the acid leaching mixture by a centrifugal or filtering method to respectively obtain acid leaching solution and solid residue,
adding the acid-leached solid residues into 8mol/L sulfuric acid solution again, soaking for 60min at 90 ℃, wherein the volume ratio of the product treated in the crushing procedure to sulfuric acid is 1: 50;
carrying out liquid-solid separation on the acid leaching mixture by a centrifugal or filtering method, washing and drying the obtained solid residue to obtain microporous high silica glass powder without heavy metals of barium, strontium and zirconium;
and (3) recovering heavy metals barium and strontium in the recovered acid leaching solution by a method of adding sulfuric acid for precipitation to obtain barium sulfate and strontium sulfate, recovering boric acid in the acid leaching solution by a freezing crystallization technology, and finally recycling the nitric acid leaching solution.
The analyzed CRT screen glass had 98.84% and 99.38% barium and strontium removal, respectively. The main component of the acid leaching residue is SiO2(93.69%), NaO (4.94%) and ZrO2(0.32%) and the pore size of the microporous high silica glass powder is 10-200 nm.
Example 3:
removing the fluorescent coating on the surface of the waste CRT screen glass after cone screen separation, crushing the CRT screen glass into particles with the diameter of 5 mm by using a combined crusher, and grinding the CRT screen glass particles into 150-mesh CRT screen glass powder by using a ball mill;
mixing CRT screen glass powder with B2O3、H3BO3、P2O5Mixing with potassium carbonate at a certain proportion, and continuously crushing to 100 meshes by using a ball mill, wherein B2O3、H3BO3、P2O5The mass ratio of the potassium carbonate to the potassium carbonate is 70:15:10:5, B2O3、H3BO3、P2O5And potassium carbonate accounts for 50% of the total mass of the mixture;
putting the mixed CRT screen glass powder into a muffle furnace and carrying out smelting treatment at 1400 ℃ in an air atmosphere, wherein the heat preservation time is 0 h;
carrying out phase separation treatment on the CRT screen glass subjected to high-temperature smelting treatment at 580 ℃ for 0.5 h;
crushing the blocky product obtained from the phase separation treatment product to 100 meshes;
adding the split-phase crushed product into 10mol/L nitric acid solution, soaking for 180min at 90 ℃, wherein the volume ratio of the product treated in the crushing procedure to the nitric acid is 1: 40;
performing liquid-solid separation on the acid leaching mixture by a centrifugal or filtering method to respectively obtain acid leaching solution and solid residue,
adding the acid-leached solid residues into 5mol/L sulfuric acid solution again, soaking for 120min at 90 ℃, wherein the volume ratio of the product treated in the crushing procedure to sulfuric acid is 1: 70;
carrying out liquid-solid separation on the acid leaching mixture by a centrifugal or filtering method, washing and drying the obtained solid residue to obtain microporous high silica glass powder without heavy metals of barium, strontium and zirconium;
and (3) recovering heavy metals barium and strontium in the recovered acid leaching solution by a method of adding sulfuric acid for precipitation to obtain barium sulfate and strontium sulfate, recovering boric acid in the acid leaching solution by a freezing crystallization technology, and finally recycling the nitric acid leaching solution.
The analyzed CRT screen glass has barium and strontium removing rate of 99.64% and 99.58%, respectively. The main component of the acid leaching residue is SiO2(95.29%), NaO (2.85%) and ZrO2(0.31%) and the size of the micropores of the microporous high silica glass powder is 5-280 nm.
Claims (4)
1. A method for preparing microporous high silica glass powder from waste CRT screen glass is characterized by comprising the following steps:
step one, a pretreatment process: removing the fluorescent coating on the surface of the waste CRT screen glass after cone screen separation, crushing the CRT screen glass into particles with the diameter of 1-5 mm by using a combined crusher, and grinding the CRT screen glass particles into CRT screen glass powder with the diameter of 20-200 meshes by using a ball mill;
step two, a material preparation process: mixing CRT screen glass powder with B2O3、H3BO3、P2O5Mixing the mixture and potassium carbonate uniformly according to a certain proportion, and continuously crushing the mixture to 100-200 meshes by using a ball mill, wherein B2O3、H3BO3、P2O5The mass ratio of the potassium carbonate to the potassium carbonate is 60-80:10-20:5-10:1-10, B2O3、H3BO3、P2O5And potassium carbonate accounts for 20-50% of the total mass of the mixture;
step three, a high-temperature smelting process: putting the mixed CRT screen glass powder into a muffle furnace and carrying out smelting treatment at 1000-1500 ℃, wherein the heat preservation time is 0-1 h;
step four, a phase separation treatment process: performing phase splitting treatment on the CRT screen glass treated by the high-temperature smelting procedure in the third step at 500-650 ℃, and keeping the temperature for 0.5-3 h;
step five, a crushing procedure: crushing the blocky product treated by the phase separation treatment procedure in the fourth step to 100-200 meshes;
step six: adding the product treated in the crushing step in the fifth step into 1-8 mol/L nitric acid solution, and soaking for 30-240 min at 90 ℃, wherein the volume ratio of the product treated in the crushing step to the nitric acid is 1: 5-50;
performing liquid-solid separation on the acid leaching mixture by a centrifugal or filtering method to respectively obtain acid leaching solution and solid residue,
adding the acid-leaching solid residue into 1-7 mol/L sulfuric acid solution again, and soaking for 30-240 min at 90 ℃, wherein the volume ratio of the product treated in the crushing procedure to sulfuric acid is 1: 5-50;
carrying out liquid-solid separation on the acid leaching mixture by a centrifugal or filtering method, washing and drying the obtained solid residue to obtain microporous high silica glass powder without heavy metals of barium, strontium and zirconium;
step seven, the pickle liquor recovery process: and D, recycling heavy metals barium and strontium in the acid leaching solution obtained in the step six by a method of adding sulfuric acid for precipitation to obtain barium sulfate and strontium sulfate, recycling boric acid in the acid leaching solution by a freezing crystallization technology, and finally recycling the nitric acid leaching solution.
2. The method of claim 1, wherein in step two, B is a step of preparing a fine pore high silica glass powder from waste CRT screen glass2O3、H3BO3、P2O5And potassium carbonate accounts for 20-40% of the total mass of the mixture, and the fineness of the CRT screen glass powder is 100-150 meshes by utilizing a ball mill.
3. The method for preparing a microporous high silica glass powder from waste CRT screen glass according to claim 1, wherein the high temperature melting in the third step is carried out under the condition of air or oxidizing atmosphere, and the melting temperature is 1100-1400 ℃.
4. The method for preparing a microporous high silica glass powder from waste CRT screen glass according to claim 1, wherein the phase separation treatment temperature in the fourth step is 550 to 650 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102701590A (en) * | 2012-06-29 | 2012-10-03 | 中国科学院上海光学精密机械研究所 | Preparation method of near ultraviolet-excited high silica blue-light-emitting glass |
| CN103864295A (en) * | 2014-03-07 | 2014-06-18 | 陕西科技大学 | Preparation method of high silica glass |
| EP2813297A1 (en) * | 2012-02-06 | 2014-12-17 | Tottori Prefecture | Method for separating heavy metal from glass |
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| EP1440951A4 (en) * | 2001-09-12 | 2009-04-01 | Japan Science & Tech Agency | Method for recycling waste glass and recycled glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2813297A1 (en) * | 2012-02-06 | 2014-12-17 | Tottori Prefecture | Method for separating heavy metal from glass |
| CN102701590A (en) * | 2012-06-29 | 2012-10-03 | 中国科学院上海光学精密机械研究所 | Preparation method of near ultraviolet-excited high silica blue-light-emitting glass |
| CN103864295A (en) * | 2014-03-07 | 2014-06-18 | 陕西科技大学 | Preparation method of high silica glass |
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