CN109336379B - Method for recycling chalcogenide glass waste residue and obtained glass - Google Patents
Method for recycling chalcogenide glass waste residue and obtained glass Download PDFInfo
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- CN109336379B CN109336379B CN201811458551.7A CN201811458551A CN109336379B CN 109336379 B CN109336379 B CN 109336379B CN 201811458551 A CN201811458551 A CN 201811458551A CN 109336379 B CN109336379 B CN 109336379B
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/024—Chemical treatment of cullet or glass fibres
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Abstract
本发明名称为一种硫系玻璃废渣再利用方法及所得玻璃，属于硫系玻璃制备技术领域。其特征在于包括以下步骤：1）用砂纸打磨玻璃废渣的表面，用水冲洗；2）将冲洗后的玻璃废渣放入亲油性和亲水性溶剂中浸泡，过滤备用；3）将过滤后的玻璃废渣放入清洗设备中清洗一段时间；4）将清洗后的玻璃废渣从清洗设备中取出，再依次用水和酒精冲洗；5）将冲洗后的玻璃废渣放入烘干设备中烘干；6）将烘干后的玻璃废渣敲碎后在密闭的手套箱中装入安瓿瓶内密封；7）将步骤安瓿瓶放入摇摆炉中高温熔炼成玻璃。该方法能有效去除玻璃渣表面和微裂纹固体杂质或油性异物，避免空气中氧、水分对玻璃透过性能的影响，适用于各种硫系玻璃玻璃渣的二次制备。
The name of the invention is a method for reusing chalcogenide glass waste residue and the obtained glass, and belongs to the technical field of chalcogenide glass preparation. It is characterized in that it comprises the following steps: 1) polishing the surface of the glass waste residue with sandpaper, and rinsing with water; 2) soaking the rinsed glass waste residue in lipophilic and hydrophilic solvents, and filtering for later use; 3) filtering the filtered glass waste Put the waste residue into the cleaning equipment for a period of time; 4) Take out the cleaned glass waste from the cleaning equipment, and then rinse it with water and alcohol in turn; 5) Put the rinsed glass waste into the drying equipment for drying; 6) After crushing the dried glass waste residue, put it into an ampoule bottle in a closed glove box and seal it; 7) Put the step ampoule bottle into a swing furnace to smelt into glass at high temperature. The method can effectively remove the surface of the glass slag and the micro-crack solid impurities or oily foreign matter, avoid the influence of oxygen and moisture in the air on the permeability of the glass, and is suitable for the secondary preparation of various chalcogenide glass slag.
Description
Technical Field
The invention relates to the technical field of chalcogenide glass preparation, in particular to a method for recycling chalcogenide glass waste residues and prepared glass.
Background
Chalcogenide glass is a novel infrared material, has excellent infrared transmittance at wave bands of 3-5 microns and 8-14 microns, can be formed into a complex infrared optical element by a precision die pressing technology at one step, has the advantages of simplified process, low cost, high efficiency and the like compared with the traditional processing method, and is widely applied to the military field and the civil field so far.
Hitherto, chalcogenide glass is produced by melting through a melting quenching method, which mainly comprises the steps of filling raw materials into an ampoule bottle for vacuum sealing, and then putting the ampoule bottle into a rocking furnace for melting. The chalcogenide glass has high requirements on production environment, and the problems of more impurities, poor stripes and crystallization of the glass often occur due to the problems of some links in the melting process, so that glass blanks are scrapped, and the blanks are also cracked, crystallized and the like after being processed and pressed later, so that more glass slag is generated, and the problem that the chalcogenide glass is difficult to solve by a chalcogenide glass manufacturing factory due to the fact that the glass scrapped is caused by the fact that the chalcogenide glass is produced by more raw materials with the purity of more than 5N is considered.
Patent 201210372442.X discloses a method for recycling waste glass slag and the obtained glass. The glass is borosilicate glass slag, and is mainly prepared by crushing the glass slag, washing, sieving, drying and firing. The method has a simple treatment process, and the glass is crushed before cleaning, so that impurities are easy to introduce for the second time, and the method is only suitable for treating oxide glass slag and is not suitable for treating chalcogenide glass slag.
Patent 201611228015.9 discloses a method for recycling waste glass slag and the resulting glass. The glass is used for packaging containers such as beer bottles and soda water bottles, only hydrochloric acid and ethanol are used for cleaning, ultrasonic waves are not used for cleaning in the process, residual impurities in cracks cannot be better removed, deionized water is not used for washing reagents on the surface of glass slag, and the residual reagents can possibly influence the infrared transmission performance of chalcogenide glass, so that the method cannot be used for optical glass required by imaging.
Disclosure of Invention
The invention aims to provide a recycling method of chalcogenide glass waste residues, which is used for solving the problem of secondary utilization of chalcogenide glass waste residues, has simple and convenient process and easy control, ensures that the quality and the performance of the molten chalcogenide glass are equivalent to those of the chalcogenide glass which is once smelted, can effectively reduce material waste, saves cost, and is suitable for secondary preparation of various chalcogenide glass waste residues.
The basic idea of the invention is as follows: analysis shows that most of the chalcogenide glass waste residues are blank material residues and type part material residues, the blank material residues are waste residues generated by the explosion cracking or edge breakage of a directly melted glass blank, the surface is generally smooth, and impurities mainly comprise refractory materials, dust, a little of oily stains and the like; the material slag of the formed piece is the material slag generated after the glass blank is subjected to secondary compression forming, most of the material slag is cutting stub bars, explosive formed pieces and the like, and the surface foreign matters are more, mainly including demoulding agents, hard oxidation layers and other impurities which are difficult to remove; secondly, most of the two kinds of material slag have cracks, impurities often remain in the cracks and are difficult to remove, so that the method provided by the invention can be used for determining a corresponding treatment process according to an analysis result by analyzing the impurity condition, so as to ensure that no foreign matters remain in the glass slag, and finally, a traditional melting process is adopted for secondary preparation.
The technical key point of the invention is that the surface foreign matter of the chalcogenide glass slag is polished by sand paper, the glass slag is soaked by acetone, after a period of time, the glass slag is put into an ultrasonic cleaning machine for cleaning, the hydrophilic and lipophilic foreign matter existing on the surface of the glass slag and in cracks is further removed, then the glass slag is washed by alcohol and deionized water, the glass slag is put into a vacuum oven, dried at a certain temperature, taken out and broken, the glass slag is put into an ampoule bottle in a sealed glove box, sealed and melted at high temperature to be made into glass. The technology for treating the chalcogenide glass slag solves the problems of high waste of chalcogenide glass materials, high cost and the like, and is simple and convenient to operate and thorough in treatment of glass slag foreign matters.
The concrete technical solution of the invention is as follows.
A recycling method of chalcogenide glass waste residue is characterized by comprising the following steps:
1) polishing the surface of the glass waste residue by using abrasive paper, and washing by using water;
2) soaking the glass waste residue washed in the step 1) in a lipophilic and hydrophilic solvent, and filtering for later use;
3) putting the glass waste residue filtered in the step 2) into cleaning equipment for cleaning for a period of time;
4) taking the glass waste residue cleaned in the step 3) out of the cleaning equipment, and then sequentially washing with water and alcohol;
5) putting the glass waste residue washed in the step 4) into drying equipment for drying;
6) breaking the dried glass waste residue obtained in the step 5), and then filling the broken glass waste residue into an ampoule bottle in a closed glove box for sealing;
7) and (3) putting the ampoule bottle in the step 6) into a rocking furnace to be smelted into glass at high temperature.
In the scheme, the mesh number of the sand paper in the step 1) is 180-280 meshes.
In the above scheme, the lipophilic and hydrophilic solvent in step 2) is acetone.
In the scheme, the cleaning equipment in the step 3) is an ultrasonic cleaning machine, the frequency of the cleaning equipment is 20-40 KHz, and the cleaning time is 5-10 min.
In the above scheme, the water in step 1) or step 4) is deionized water.
In the scheme, the drying temperature of the drying in the step 5) is 100-150 ℃, and the drying time is 3-5 h.
In the scheme, the high-temperature smelting in the step 5) is carried out for 15 hours at the temperature of 900 ℃, and then the temperature is reduced to 700 ℃ for quenching.
In the scheme, the high-temperature smelting in the step 5) is to smelt at 1000 ℃ for 20 hours and then quench.
In the scheme, the glass obtained by the method for recycling the chalcogenide glass waste residue has glass impurities of grade 1, bubbles of grade 0 and specific gravity of 4.63g/cm3The infrared transmittance of a 2mm thick glass sample in the 14.5 μm wavelength band is 57% or more.
In the scheme, the glass obtained by the method for recycling the chalcogenide glass waste residue has 2-grade glass impurities, 1-grade bubbles and 4.42g/cm specific gravity3。
The following preparation method is adopted for recycling the chalcogenide glass waste residues: and (3) placing the ampoule bottle filled with the glass slag and sealed in vacuum into a rocking furnace for high-temperature smelting at 850-1100 ℃ for 10-20 h, rocking in the whole smelting process to ensure that all raw materials are uniformly mixed, and finally taking out the sealed container for water-cooling solidification to form glass in the sealed ampoule bottle.
The waste glass slag is chalcogenide glass slag, chalcogenide glass is infrared-transmitting glass, and the infrared transmission performance is particularly easily influenced by impurity absorption; and the preparation process is sealed single-pot smelting, and foreign matters in the preparation process cannot be removed. Therefore, the chalcogenide glass slag treatment technology is different from the traditional optical glass slag treatment technology, and is characterized in that the measures of fine grinding, organic solvent soaking, ultrasonic vibration cleaning, deionized water flushing and the like are adopted to remove solid impurities or oily foreign matters on the surface of glass slag and microcracks, so that the influence of oxygen and moisture in the air on the permeability of glass is avoided, the operation is simple and convenient, and the treatment effect is good.
Drawings
FIG. 1 is a transmittance curve of a chalcogenide glass in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples 1 and 2 are typical experiments of the present invention illustrating the technology of treating the chalcogenide glass slag. These examples are merely to demonstrate the feasibility of the technology, and the present invention is not limited to these examples.
The method of the invention comprises the following steps:
1) finishing chalcogenide glass slag to be treated, and polishing away foreign matters (mainly dust, a mold release agent on the surface of a molded piece and the like) on the surface of the glass slag and visible cracks (aiming at preventing foreign matters from being mixed in the cracks) by using 180-280-mesh abrasive paper;
2) washing the polished glass slag with deionized water at least twice, then placing the glass slag into a container filled with acetone, soaking for about 10min, and pouring waste acetone into a recovery container;
3) adding deionized water into the soaked glass slag, putting the glass slag into ultrasonic waves, setting the ultrasonic frequency to be 20-40 KHz, and carrying out ultrasonic cleaning for 5-10 min to mainly remove impurities which are included in microcracks of the glass slag and are difficult to remove;
4) taking the glass slag out of the cleaning machine, washing the glass slag twice by using deionized water, and then washing the glass slag at least twice by using alcohol, wherein the alcohol has good wettability and can better remove the surface moisture of the glass slag;
5) putting the cleaned glass slag into an oven, setting the temperature to be 100-150 ℃, keeping the temperature for 3-5 hours, drying the moisture on the surface, cutting off the power, and rapidly cooling to ensure that large glass slag generates large stress and is naturally cracked or broken;
6) and (3) putting the sealed ampoule bottle into a rocking furnace, melting for 10-20 h at the high temperature of 850-1100 ℃, and finally quenching to obtain the glass.
Example 1: commercial As40Se60The recycling method of the chalcogenide glass waste residue comprises the following steps:
1) as to be treated40Se60The chalcogenide glass slag is sorted and collected, visible foreign matters on the surface of the glass slag, including visible cracks at corners and naked eyes, are ground off by adopting 220-mesh sand paper in flowing tap water, and the glass slag is placed into a prepared container;
2) preparing deionized water in advance, repeatedly washing the polished glass residue twice with deionized water, placing into a container filled with acetone, soaking for 10min, and recovering waste acetone;
3) adding deionized water into the soaked glass slag, putting the glass slag into an ultrasonic cleaning machine, setting ultrasonic frequency to be 25KHz, cleaning for 8min, and taking out the glass slag;
4) continuously washing the glass slag twice by using deionized water, washing off sewage generated after the ultrasonic vibration of the glass slag, and washing the glass slag twice by using alcohol;
5) putting the cleaned glass slag into an oven, drying for 3h at the drying temperature of 150 ℃, and taking out the glass slag after power failure and temperature reduction;
6) putting the glass slag into a closed glove box, smashing a larger piece of glass slag to enable the glass slag to be filled into an ampoule bottle, selecting particle glass slag to be filled into the ampoule bottle, scrapping residual glass powder at the bottom, and finally carrying out vacuum sealing on the filled ampoule bottle for later smelting;
7) putting the sealed ampoule bottle into a rocking furnace, melting for 15h at the high temperature of 900 ℃, finally cooling to 700 ℃, and quenching to prepare glass;
8) the obtained glass has the impurity level of 1, the bubble level of 0 (see the national standard GB/T36265) -2018) and the specific gravity of 4.63g/cm3The sample piece with a thickness of 2mm has an infrared transmittance of about 14.5 μm of 57% or more, and has no absorption of other impurities, and the infrared transmittance curve is shown in FIG. 1.
Example 2: commercial Ge33Se55As12The difference from the example 1 in the method for recycling the waste chalcogenide glass slag includes:
1) ge was treated according to the method of example 133Se55As12The chalcogenide glass waste residues are different in types of the treated glass residues, and are melted at the high temperature of 1000 ℃ for 20 hours and then cooled by water to prepare glass;
2) the obtained glass has the impurity level of 2, the bubble level of 1 (see the national standard GB/T36265) -2018) and the specific gravity of 4.42g/cm3The infrared transmission performance is good.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (9)
1. A recycling method of chalcogenide glass waste residue is characterized by comprising the following steps:
1) polishing the surface of the glass slag by using abrasive paper, and washing by using water;
2) soaking the glass waste residue washed in the step 1) in a lipophilic and hydrophilic solvent, and filtering for later use, wherein the lipophilic and hydrophilic solvent is acetone;
3) putting the glass waste residue filtered in the step 2) into an ultrasonic cleaning machine for cleaning for a period of time;
4) taking the glass waste residue cleaned in the step 3) out of the cleaning equipment, and then sequentially washing with water and alcohol;
5) putting the glass waste residue washed in the step 4) into drying equipment for drying;
6) breaking the dried glass waste residue obtained in the step 5), and then filling the broken glass waste residue into an ampoule bottle in a closed glove box for sealing;
7) and (3) putting the ampoule bottle in the step 6) into a rocking furnace to be smelted into glass at high temperature.
2. The method for recycling chalcogenide glass waste residue according to claim 1, characterized in that: the mesh number of the sand paper in the step 1) is 180-280 meshes.
3. The method for recycling the chalcogenide glass waste residue according to claim 1 or 2, characterized in that: the frequency of the ultrasonic cleaning machine in the step 3) is 20-40 KHz, and the cleaning time is 5-10 min.
4. The method for recycling the chalcogenide glass waste residue according to claim 1 or 2, characterized in that: the water in the step 1) or/and the step 4) is deionized water.
5. The method for recycling chalcogenide glass waste residue according to claim 1, characterized in that: the drying temperature of the drying in the step 5) is 100-150 ℃, and the drying time is 3-5 h.
6. The method for recycling chalcogenide glass waste residue according to claim 1, characterized in that: in the step 7), the high-temperature smelting is carried out for 15 hours at the temperature of 900 ℃, and then the temperature is reduced to 700 ℃ for water quenching.
7. The method for recycling chalcogenide glass waste residue according to claim 1, characterized in that: the high-temperature smelting in the step 7) is to smelt at 1000 ℃ for 20h and then quench.
8. Glass obtained by the method for recycling a chalcogenide glass waste residue according to any one of claims 1 to 7, characterized in thatThe glass impurities are 1 grade, the bubbles are 0 grade, and the specific gravity is 4.63g/cm3The infrared transmittance of a 2mm thick glass sample in the 14.5 μm wavelength band is 57% or more.
9. The glass obtained by the method for recycling a chalcogenide glass waste residue according to any one of claims 1 to 7, wherein the glass has a glass impurity of grade 2, a bubble of grade 1 and a specific gravity of 4.42g/cm3。
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| CN110668674B (en) * | 2019-11-07 | 2022-03-04 | 湖南华兴玻璃有限公司 | Waste bottle remelting and waste cleaning system for glass production line |
| CN113754280B (en) * | 2021-09-29 | 2023-06-23 | 宁波阳光和谱光电科技有限公司 | Method for recycling leftover materials of chalcogenide glass, leftover materials and method for preparing chalcogenide glass |
| CN115555346A (en) * | 2022-10-14 | 2023-01-03 | 安徽光智科技有限公司 | Surface treatment method for chalcogenide ball |
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