A quartz tube connection reusing method
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-30
- Publication Date
- 2026-08-11
AI Technical Summary
此外,在镜头材料冷加工及模压加工过程中也会产生一定比例的加工边角料及不良品,此类边角料若无法合理再利用则会导致资源的浪费及生产成本的增加
[0027]本发明提供了一种石英管接驳再利用方法,包括以下步骤:a)将首次蒸馏完成的H形石英管进行焊封,分别得到盛装提纯玻璃液的冷凝管和待清洗蒸馏管;其中,所述待清洗蒸馏管经石英滤芯和管帽的切除后,依次进行清洗和干燥,得到第一次回收的蒸馏管;b)将步骤a)得到的第一次回收的蒸馏管与带有石英滤芯的冷凝管焊接后,进行第二次蒸馏;然后将第二次蒸馏完成的H形石英管进行焊封,得到的蒸馏管部分经石英滤芯和管底的切除后,依次进行清洗和干燥,得到第二次回收的蒸馏管;c)将步骤b)得到的第二次回收的蒸馏管与带有石英滤芯的冷凝管焊接后,进行第三次蒸馏,实现石英管接驳再利用。与现有技术相比,本发明提供的石英管接驳再利用方法,采用特定工艺步骤,实现整体较好相互作用,能够实现硫系玻璃蒸馏提纯用石英管的重复利用,从而节约了石英资源,节省了生产成本;并且再利用H形石英管A管始终作为蒸馏盛料管使用,不经历长时间高温熔炼及淬冷剧烈热冲击等过程,保证其在多次使用过程中不会发生析晶产生热裂纹等不良情况,从而确保其使用过程的安全性。
Smart Images

Figure BDA0004867592300000081 
Figure BDA0004867592300000091 
Figure BDA0004867592300000092
Abstract
Description
Technical Field
[0001] This invention relates to the field of recycling technology, and more specifically, to a method for reusing quartz tube connections. Background Technology
[0002] Chalcogenide glass is a high-performance mid-to-long-wave infrared optical material widely used in infrared lenses, thermal imaging lenses, and other applications. However, impurities such as H₂O, hydroxyl groups, and others in chalcogenide glass can severely affect its infrared transmittance. Therefore, for lens materials with strict requirements on transmittance and transmission wavelength, the raw materials with lower purity usually need to undergo purification pretreatment during the manufacturing process to meet the requirements of end-use. Since most chalcogenide compounds have high saturated vapor pressure and are easily sublimated, the significant difference in saturated vapor pressure between chalcogenide compounds and impurities and oxides can be used to purify chalcogenide glass. Furthermore, a certain proportion of processing scraps and defective products are generated during the cold working and molding processes of lens materials. If these scraps cannot be properly reused, it will lead to resource waste and increased production costs. Direct remelting of these scraps makes it difficult to avoid impurity contamination. Distillation purification can effectively separate impurities, thereby achieving efficient reuse of the scraps, saving resources, and reducing production costs.
[0003] Current technology typically uses H-shaped quartz ampoules to distill and purify chalcogenide glass raw materials and scraps. The raw material is loaded onto one side of the H-shaped quartz tube, and distillation and purification are achieved by controlling the temperature difference between the two tubes. Because chalcogen elements have high vapor pressures at relatively low temperatures, the high-temperature process experienced by the quartz ampoule during distillation is relatively "mild." Therefore, after distillation and purification, the original H-shaped quartz tube containing the raw material still possesses excellent thermal and mechanical properties. If the quartz tube on the containing side can be reused, the use of quartz tubes in the chalcogenide glass manufacturing process can be reduced, thereby further saving quartz resources and significantly reducing the cost of chalcogenide glass purification and scrap recycling. Summary of the Invention
[0004] In view of this, the purpose of this invention is to provide a method for reusing quartz tubes, which enables the reuse of quartz tubes used for distillation and purification of chalcogenide glass, thereby saving quartz resources and reducing production costs. Furthermore, the reused H-shaped quartz tube A is always used as the distillation container, without undergoing prolonged high-temperature melting and severe thermal shock processes such as quenching, ensuring that it will not experience adverse conditions such as crystallization and thermal cracking during multiple uses, thus ensuring its safety during use.
[0005] This invention provides a method for reusing quartz tubes, comprising the following steps:
[0006] a) The H-shaped quartz tube after the first distillation is welded and sealed to obtain a condenser tube for holding the purified glass liquid and a distillation tube to be cleaned; wherein, the distillation tube to be cleaned is cleaned and dried in sequence after the quartz filter element and tube cap are removed to obtain the first recovered distillation tube.
[0007] b) Weld the first recovered distillation tube obtained in step a) to the condenser tube with a quartz filter element, and then perform a second distillation; then weld the H-shaped quartz tube after the second distillation is completed, and after the quartz filter element and the bottom of the tube are removed, the distillation tube is cleaned and dried in sequence to obtain the second recovered distillation tube.
[0008] c) After welding the second recycled distillation tube obtained in step b) to the condenser tube with a quartz filter element, a third distillation is performed to achieve the reconnection and reuse of the quartz tube.
[0009] Preferably, the distillation process described in step a) specifically includes:
[0010] A quartz filter element is placed in the vapor transfer tube of the H-shaped quartz tube. Then, the raw material to be distilled is loaded into the distillation tube of the H-shaped quartz tube. After placing a tube cap at the opening of the distillation tube, a vacuum is drawn. Once the required vacuum level is reached, the distillation tube is sealed with an oxyhydrogen flame. Subsequently, the H-shaped quartz tube containing the raw material to be distilled is transferred to a distillation furnace for distillation and purification.
[0011] Preferably, one side of the H-shaped quartz tube is a distillation tube and the other side is a condenser tube, and the distillation tube and the condenser tube are connected and communicate with each other through a vapor transmission tube; the length of the distillation tube is greater than the length of the condenser tube.
[0012] Preferably, the quartz filter element is placed in the vapor transmission pipe at one end near the condenser.
[0013] Preferably, the vacuum level requirement is 10. -3 Pa or above.
[0014] Preferably, the welding method in step a) is oxyhydrogen flame; the welding position is at the end of the steam transmission pipe near the condenser pipe.
[0015] Preferably, the cleaning process in step a) involves first repeatedly washing with water, then washing with sodium hydroxide solution, and finally rinsing with water.
[0016] The drying temperature is 100℃~150℃, and the time is 1h~5h.
[0017] Preferably, the second distillation process in step b) specifically comprises:
[0018] The raw material to be distilled is loaded into the H-shaped quartz tube obtained by welding. After placing a tube cap at the tube opening, a vacuum is drawn. Once the required vacuum level is reached, the distillation tube is sealed with an oxyhydrogen flame. Subsequently, the H-shaped quartz tube containing the raw material to be distilled is transferred to a distillation furnace for distillation and purification, thus realizing the second use of the distillation tube.
[0019] Preferably, before welding the second-recovered distillation tube to the condenser tube with the quartz filter element in step c), the process further includes:
[0020] The second batch of recovered distillation tubes were subjected to annealing, washing, and drying in sequence.
[0021] Preferably, the annealing process specifically includes:
[0022] The first stage involves heating from room temperature to 1100℃ over 350-370 minutes.
[0023] The second stage involves holding the temperature at 1100℃ for 290-310 minutes.
[0024] The third stage involves cooling from 1100℃ to 700℃ over 590 to 610 minutes.
[0025] The fourth stage involves cooling from 700℃ to 400℃ over 290 to 310 minutes.
[0026] The fifth stage involves cooling from 400℃ to room temperature along with the furnace.
[0027] This invention provides a method for reusing quartz tubes, comprising the following steps: a) Welding an H-shaped quartz tube after the first distillation to obtain a condenser tube for holding purified glass melt and a distillation tube to be cleaned; wherein, the distillation tube to be cleaned is cleaned and dried sequentially after the quartz filter element and tube cap are removed, to obtain a first-recovered distillation tube; b) Welding the first-recovered distillation tube obtained in step a) to a condenser tube with a quartz filter element, and then performing a second distillation; then welding the H-shaped quartz tube after the second distillation, and after the quartz filter element and tube bottom are removed, the resulting distillation tube is cleaned and dried sequentially, to obtain a second-recovered distillation tube; c) Welding the second-recovered distillation tube obtained in step b) to a condenser tube with a quartz filter element, and then performing a third distillation, thereby realizing the reusing of quartz tubes. Compared with existing technologies, the quartz tube connection and reuse method provided by this invention adopts specific process steps to achieve better overall interaction, enabling the reuse of quartz tubes used for distillation and purification of chalcogenide glass, thereby saving quartz resources and reducing production costs. Furthermore, the reused H-shaped quartz tube A is always used as the distillation container tube, without undergoing prolonged high-temperature melting and severe thermal shock processes such as quenching, ensuring that it will not experience adverse conditions such as crystallization and thermal cracking during multiple uses, thus ensuring its safety during use. Attached Figure Description
[0028] Figure 1 This is a schematic diagram of the structure of the H-shaped quartz tube used in the embodiments of the present invention;
[0029] Figure 2 This is a schematic diagram of the pre-distillation loading and sealing process;
[0030] Figure 3 This is a schematic diagram showing the completion of distillation;
[0031] Figure 4 This is a schematic diagram of the welding and sealing of tube B after distillation.
[0032] Figure 5 This is a schematic diagram showing the cutting of tube A after distillation;
[0033] Figure 6 This is a schematic diagram showing the completed cutting of pipe A.
[0034] Figure 7 This is a schematic diagram of the connection between pipes A and B for the second use;
[0035] Figure 8 This is a schematic diagram of the second-use loading and sealing process;
[0036] Figure 9 This is a diagram showing the cutting of pipe A after its second use.
[0037] Figure 10 This is a schematic diagram showing the completed cutting of pipe A.
[0038] Figure 11 This is a schematic diagram of the connection between pipes A and B for the third time.
[0039] Figure 12 This is a schematic diagram of the third-use loading and sealing process;
[0040] Figure 13 The image shows the morphology of internal impurities in the scrap material before distillation and purification after the first connection and use of tube A in Example 1.
[0041] Figure 14 The results of microscopic observation of the inside of the glass after the first connection of tube A in Example 1 using distillation purification.
[0042] Figure 15 The infrared transmittance spectrum of the glass after distillation and purification is shown for tube A in Example 1 during its first connection.
[0043] Figure 16 The image shows the morphology of internal impurities in the scrap material before distillation and purification after the second connection of tube A in Example 2.
[0044] Figure 17 The results of microscopic observation of the inside of the glass after the first connection of tube A in Example 2 using distillation purification.
[0045] Figure 18 The image shows the infrared transmittance spectrum of the glass after distillation and purification when tube A was first connected in Example 2. Detailed Implementation
[0046] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0047] This invention provides a method for reusing quartz tubes, comprising the following steps:
[0048] a) The H-shaped quartz tube after the first distillation is welded and sealed to obtain a condenser tube for holding the purified glass liquid and a distillation tube to be cleaned; wherein, the distillation tube to be cleaned is cleaned and dried in sequence after the quartz filter element and tube cap are removed to obtain the first recovered distillation tube.
[0049] b) Weld the first recovered distillation tube obtained in step a) to the condenser tube with a quartz filter element, and then perform a second distillation; then weld the H-shaped quartz tube after the second distillation is completed, and after the quartz filter element and the bottom of the tube are removed, the distillation tube is cleaned and dried in sequence to obtain the second recovered distillation tube.
[0050] c) After welding the second recycled distillation tube obtained in step b) to the condenser tube with a quartz filter element, a third distillation is performed to achieve the reconnection and reuse of the quartz tube.
[0051] The present invention first welds and seals the H-shaped quartz tube after the first distillation to obtain a condenser tube for holding the purified glass liquid and a distillation tube to be cleaned; wherein, the distillation tube to be cleaned is cleaned and dried in sequence after the quartz filter element and tube cap are removed to obtain the first recovered distillation tube.
[0052] In this invention, the distillation process is preferably specifically as follows:
[0053] A quartz filter element is placed in the vapor transfer tube of an H-shaped quartz tube. Then, the raw material to be distilled is loaded into the distillation tube of the H-shaped quartz tube. A cap is placed at the opening of the distillation tube, and a vacuum is drawn. Once the required vacuum level is achieved, the distillation tube is sealed using an oxyhydrogen flame (see [link to product description]). Figure 2 (as shown); then the H-shaped quartz tube containing the raw material to be distilled is transferred to a distillation furnace for distillation and purification (see...). Figure 3 (As shown).
[0054] In this invention, one side of the H-shaped quartz tube is a distillation tube (raw material filling tube, which can be referred to as tube A), and the other side is a condenser tube (purified product collection tube, which can be referred to as tube B). The distillation tube and the condenser tube are connected and communicate with each other through a vapor transfer tube; the length of the distillation tube is preferably greater than the length of the condenser tube (see...). Figure 1 (As shown).
[0055] In this invention, the quartz filter element is preferably placed in the vapor transmission pipe near the end of the condenser (i.e., the porous quartz filter element is placed between pipes A and B near the end of pipe B).
[0056] In this invention, the vacuum level requirement is preferably 10. -3 Pa or above.
[0057] After the first distillation is completed, the present invention performs a weld seal on the end of the steam transmission pipe near pipe B (see [link]). Figure 4 The process yields a condenser tube containing purified glass melt and a distillation tube to be cleaned; wherein the B tube containing purified glass melt is transferred to a swing furnace for high-temperature melting.
[0058] In this invention, the welding method is preferably oxyhydrogen flame; the welding position is preferably at the end of the steam transmission pipe near the condenser tube.
[0059] This invention cuts off the steam transfer tube connected to tube A at the quartz filter element, and simultaneously removes the cap of tube A (e.g.) Figure 5(As shown); then wash tube A with water, and finally dry it to obtain the first recovered distillation tube, for later use (as shown). Figure 6 (As shown).
[0060] In this invention, the cleaning process preferably involves first repeatedly washing with water, then washing with sodium hydroxide solution, and finally rinsing with water.
[0061] In this invention, the drying temperature is preferably 100℃~150℃, and the drying time is preferably 1h~5h.
[0062] After obtaining the first recovered distillation tube, the present invention welds the first recovered distillation tube to a condenser tube with a quartz filter element and performs a second distillation; then the H-shaped quartz tube after the second distillation is completed is welded and sealed, and the obtained distillation tube is cleaned and dried after the quartz filter element and the bottom of the tube are removed, to obtain the second recovered distillation tube.
[0063] In this invention, the condenser tube with a quartz filter element is preferably a new B-tube with a certain length of vapor transmission tube, and welding is performed at the vapor transmission tube inlet using an oxyhydrogen flame (e.g., Figure 7 (As shown).
[0064] After welding, the initial loading, vacuuming, welding, and distillation processes (second distillation) of the H-shaped quartz tube can be repeated, enabling the second use of tube A (e.g., ...). Figure 8 (As shown).
[0065] In this invention, the second distillation process is preferably specifically as follows:
[0066] The raw material to be distilled is loaded into the H-shaped quartz tube obtained by welding. After placing a tube cap at the tube opening, a vacuum is drawn. Once the required vacuum level is reached, the distillation tube is sealed with an oxyhydrogen flame. Subsequently, the H-shaped quartz tube containing the raw material to be distilled is transferred to a distillation furnace for distillation and purification, thus realizing the second use of the distillation tube.
[0067] Then, the H-shaped quartz tube after the second distillation is welded and sealed. After the quartz filter element and the bottom of the tube are removed, the resulting distillation tube is cleaned and dried in sequence to obtain the second recovered distillation tube.
[0068] After achieving the second use of the distillation tube, the present invention repeats the cutting process at the vapor transmission tube of tube A, and then cuts off the capless end (bottom) of tube A (e.g. Figure 9 (As shown); then repeat the cleaning and drying steps of tube A before its second use.
[0069] After obtaining the second recycled distillation tube, the present invention welds the second recycled distillation tube to a condenser tube with a quartz filter element and performs a third distillation to achieve the reconnection and reuse of the quartz tube.
[0070] In this invention, before the second-recovery distillation tube is welded to the condenser tube with a quartz filter element, it preferably further includes:
[0071] The second batch of recovered distillation tubes were subjected to annealing, washing, and drying in sequence.
[0072] In this invention, tube A is transferred to an annealing furnace for annealing. After annealing, the quartz tube is ultrasonically cleaned with pure water and then dried (e.g., Figure 10 (As shown).
[0073] In this invention, the annealing process is preferably as follows:
[0074] The first stage involves heating from room temperature to 1100℃ over 350-370 minutes.
[0075] The second stage involves holding the temperature at 1100℃ for 290-310 minutes.
[0076] The third stage involves cooling from 1100℃ to 700℃ over 590 to 610 minutes.
[0077] The fourth stage involves cooling from 700℃ to 400℃ over 290 to 310 minutes.
[0078] The fifth stage involves cooling from 400℃ to room temperature along with the furnace.
[0079] Subsequently, the present invention repeats the connection processing method for the secondary use of pipe A (e.g.) Figure 11 (As shown); After the connection is completed, the section with the quartz cap is welded to serve as the bottom of tube A, and the original bottom section is cut off to serve as the feeding port for raw material filling. Then, the vacuum extraction and tube end welding steps are repeated (as shown). Figure 12 As shown), the H-type quartz tube has been used for the third time.
[0080] Based on this, the present invention realizes the use and reuse of quartz tubes for distillation and purification of chalcogenide glass, thereby saving quartz resources and reducing production costs; and the reused H-shaped quartz tube A is always used as the distillation container tube, without undergoing long-term high-temperature melting and severe thermal shock processes such as quenching, ensuring that it will not develop defects such as crystallization and thermal cracking during multiple uses, thereby ensuring its safety during use.
[0081] This invention provides a method for reusing quartz tubes, comprising the following steps: a) Welding an H-shaped quartz tube after the first distillation to obtain a condenser tube for holding purified glass melt and a distillation tube to be cleaned; wherein, the distillation tube to be cleaned is cleaned and dried sequentially after the quartz filter element and tube cap are removed, to obtain a first-recovered distillation tube; b) Welding the first-recovered distillation tube obtained in step a) to a condenser tube with a quartz filter element, and then performing a second distillation; then welding the H-shaped quartz tube after the second distillation, and after the quartz filter element and tube bottom are removed, the resulting distillation tube is cleaned and dried sequentially, to obtain a second-recovered distillation tube; c) Welding the second-recovered distillation tube obtained in step b) to a condenser tube with a quartz filter element, and then performing a third distillation, thereby realizing the reusing of quartz tubes. Compared with existing technologies, the quartz tube connection and reuse method provided by this invention adopts specific process steps to achieve better overall interaction, enabling the reuse of quartz tubes used for distillation and purification of chalcogenide glass, thereby saving quartz resources and reducing production costs. Furthermore, the reused H-shaped quartz tube A is always used as the distillation container tube, without undergoing prolonged high-temperature melting and severe thermal shock processes such as quenching, ensuring that it will not experience adverse conditions such as crystallization and thermal cracking during multiple uses, thus ensuring its safety during use.
[0082] To further illustrate the present invention, the following embodiments are provided for detailed description. A schematic diagram of the H-shaped quartz tube used in the following embodiments of the present invention can be found [link to schematic diagram]. Figure 1 As shown, 1 is the distillation cap, 2 is the distillation tube (tube A), 3 is the quartz filter element, 4 is the condenser tube (tube B), 5 is the vapor transfer tube, and 6 is the distillation raw material (sulfur-based glass scraps or raw materials).
[0083] Example 1
[0084] Cut the H-shaped quartz tube A, which has been distilled, along the branch end and remove the cap at the weld bead. Use a test tube brush to repeatedly clean the reused quartz tube A to remove any impurities or foreign matter remaining after the first distillation. Then, transfer the reused tube A to a 10 mol / L sodium hydroxide solution and sonicate for 2 hours to remove any remaining chalcogenide glass residue. After that, remove the quartz tube and rinse it with tap water to remove any remaining alkali.
[0085] Continue to ultrasonically clean the recycled quartz tube A twice with pure water, each time for 1 hour. After cleaning, transfer the quartz tube to a drying oven and dry at 120°C for 3 hours. Use an oxyhydrogen flame to weld the recycled tube A to the new tube B at the steam transfer pipe port. After the temperature at the weld joint drops to room temperature, proceed with the loading operation.
[0086] As₂Se₃ chalcogenide glass cold-working scraps were purified by distillation. Before distillation, the scraps were heated and ultrasonically cleaned with AR-grade alcohol, acetone, and pure water to remove dust, cutting fluid, and other foreign matter adhering to the surface. The cleaned scraps were then transferred to a vacuum oven for drying. During the drying process, the temperature was maintained at 120°C and the pressure inside the oven was maintained at 130 Pa. After complete drying, the scraps were transferred to a clean workbench for loading.
[0087] Weigh 3 kg of As₂Se₃ chalcogenide glass scrap containing internal impurities. The morphology and distribution of the impurities in the scrap are as follows: Figure 13 As shown.
[0088] Load the scrap material into pipe A, place a new pipe cap at the pipe opening of pipe A, and then connect the pipe opening of pipe A to a quick vacuum connector to perform vacuum evacuation, achieving a vacuum level of 10. -3 Above Pa, tube A is welded using an oxyhydrogen flame. After welding, the quartz tube is transferred to a distillation furnace for distillation purification. The distillation purification temperatures for tubes A and B are set as shown in Table 1 below.
[0089] Table 1. Distillation temperature settings for As2Se3 glass scraps in Example 1
[0090]
[0091]
[0092] After distillation, the purified glass melt is quenched and shaped in water. Once the glass melt has fully hardened, the quartz tube is transferred to an annealing furnace for rough annealing at 160°C for 1 hour. The furnace is then powered off and allowed to cool. After rough annealing, the vapor transfer tube is sealed with an oxyhydrogen flame near the condenser tube. The original condenser tube is then transferred to a oscillating furnace for vacuum melting and homogenization. The melting temperature is set as follows, and the oscillation angular velocity is 15° / s. After the oscillating melting is completed, once the furnace temperature drops to 400℃, the quartz ampoule (original condenser tube) containing the high-temperature glass melt is removed from the oscillating furnace and smoothly transferred to water for quenching and shaping. After the glass melt has completely dewalled and hardened, the ampoule is transferred to an annealing furnace for fine annealing. The furnace temperature is 180℃, and after holding at that temperature for 3 hours, it is slowly cooled to room temperature at a cooling rate of 2℃ / h. The quartz tube is then removed, broken, and the rod is taken out. The rod is then inspected.
[0093] The test results show that the impurity level of the bar stock is grade 0, and the average transmittance in the 8-12μm band is 64.27%.
[0094] In Example 1, the results of the first connection of tube A using distillation purification and internal microscopic observation of the glass are shown in the attached diagram. Figure 14As shown; the infrared transmittance spectrum of the glass after distillation and purification used in the first connection of tube A in Example 1 is shown in the figure. Figure 15 As shown.
[0095] Example 2
[0096] Cut the H-shaped quartz tube A, which has undergone two distillations, along the end of the steam transfer tube. Cut off the bottom of the quartz tube away from the end of the quartz tube cap. Use a test tube brush to repeatedly clean the reused quartz tube A to remove the impurities and foreign matter remaining after the first distillation. Then, transfer the reused tube A to a 10 mol / L sodium hydroxide solution and sonicate for 2 hours to remove the residual chalcogenide glass residue. After that, take out the quartz tube and rinse off the residual alkali solution with tap water. After the quartz tube is dried, transfer the quartz tube A to an annealing furnace for annealing treatment. The annealing process is shown in Table 2 below.
[0097] Table 2. Annealing process temperature setting table in Example 2
[0098]
[0099] The annealed quartz A tube underwent the same pure water cleaning, connection, loading, and vacuum extraction steps as in Example 1. The cold-worked chalcogenide glass scraps (As2Se3 composition) were purified by distillation. Before distillation, the scraps were heated and ultrasonically cleaned with AR-grade alcohol, acetone, and pure water to remove dust, cutting fluid, and other foreign matter adhering to the surface. The cleaned scraps were then transferred to a vacuum oven for drying. During drying, the temperature was maintained at 120°C, and the pressure inside the oven was maintained at 130 Pa. After complete drying, the scraps were transferred to a clean workbench for loading.
[0100] Weigh 2 kg of As₂Se₃ chalcogenide glass scrap containing internal impurities. The morphology and distribution of the impurities in the scrap are as follows: Figure 16 As shown.
[0101] Load the scrap material into pipe A, place a new pipe cap at the pipe opening of pipe A, and then connect the pipe opening of pipe A to a quick vacuum connector to perform vacuum evacuation, achieving a vacuum level of 10. -3 Above Pa, tube A was welded using an oxyhydrogen flame. After welding, the quartz tube was transferred to a distillation furnace for distillation purification. The distillation purification temperature settings for tubes A and B were exactly the same as in Example 1. The melting and annealing processes after distillation purification were consistent with those in Example 1. After annealing, the bar stock prepared from the purified scrap was tested.
[0102] The test results show that the impurity level of the bar stock is grade 0, and the average transmittance in the 8-12μm band is 64.38%.
[0103] In Example 2, the results of the first connection of tube A using distillation purification and internal microscopic observation of the glass are shown below. Figure 17 As shown; the infrared transmittance spectrum of the glass after distillation and purification used for the first connection of tube A in Example 2 is shown in the figure. Figure 18 As shown.
[0104] In summary, the quartz tube connection and reuse method provided by this invention enables the reuse of quartz tubes used for distillation and purification of chalcogenide glass, thereby saving quartz resources and reducing production costs. Furthermore, the reused H-shaped quartz tube A is always used as the distillation container tube, without undergoing prolonged high-temperature melting and severe thermal shock processes such as quenching, ensuring that it will not experience adverse conditions such as crystallization and thermal cracking during multiple uses, thus ensuring its safety during use.
[0105] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A method for reusing quartz tube connections, comprising the following steps: a) The H-shaped quartz tube after the first distillation is welded and sealed to obtain a condenser tube for holding the purified glass liquid and a distillation tube to be cleaned; wherein, the distillation tube to be cleaned is cleaned and dried in sequence after the quartz filter element and tube cap are removed to obtain the first recovered distillation tube. b) After welding the first-recovery distillation tube obtained in step a) to the condenser tube with the quartz filter element, a second distillation is performed; then the H-shaped quartz tube after the second distillation is completed is welded and sealed. After the quartz filter element and the bottom of the tube are removed, the resulting distillation tube is cleaned and dried in sequence to obtain the second-recovery distillation tube. c) The second recycled distillation tube obtained in step b) is annealed, washed and dried in sequence, then welded to a condenser tube with a quartz filter element, and then distilled for the third time to realize the reuse of the quartz tube. The annealing process is specifically as follows: The first stage involves heating from room temperature to 1100℃ over 350-370 minutes. The second stage involves holding the temperature at 1100℃ for 290-310 minutes. The third stage involves cooling from 1100℃ to 700℃ over 590-610 minutes. The fourth stage involves cooling from 700℃ to 400℃ over 290-310 minutes. The fifth stage involves cooling from 400℃ to room temperature along with the furnace.
2. The quartz tube splicing and reuse method according to claim 1, characterized in that, The distillation process described in step a) is specifically as follows: A quartz filter element is placed in the vapor transfer tube of the H-shaped quartz tube. Then, the raw material to be distilled is loaded into the distillation tube of the H-shaped quartz tube. After placing a tube cap at the opening of the distillation tube, a vacuum is drawn. Once the required vacuum level is reached, the distillation tube is sealed with an oxyhydrogen flame. Subsequently, the H-shaped quartz tube containing the raw material to be distilled is transferred to a distillation furnace for distillation and purification.
3. The quartz tube splicing and reuse method according to claim 2, characterized in that, One side of the H-shaped quartz tube is a distillation tube, and the other side is a condenser tube. The distillation tube and the condenser tube are connected and communicate with each other through a vapor transmission tube; the length of the distillation tube is greater than the length of the condenser tube.
4. The method for reusing quartz tubes according to claim 2, characterized in that, The quartz filter element is placed in the vapor transmission pipe near the end of the condenser tube.
5. The method for reusing quartz tubes according to claim 2, characterized in that, The required vacuum level is 10. -3 Pa or above.
6. The method for reusing quartz tubes according to claim 1, characterized in that, The welding method described in step a) is oxyhydrogen flame; the welding position is at the end of the steam transmission pipe near the condenser.
7. The method for reusing quartz tubes according to claim 1, characterized in that, The cleaning process described in step a) involves first repeatedly rinsing with water, then rinsing with sodium hydroxide solution, and finally rinsing with water. The drying temperature is 100℃~150℃, and the time is 1h~5h.
8. The method for reusing quartz tubes according to claim 1, characterized in that, The second distillation process described in step b) is specifically as follows: The raw material to be distilled is loaded into the H-shaped quartz tube obtained by welding. After placing a tube cap at the tube opening, a vacuum is drawn. Once the required vacuum level is reached, the distillation tube is sealed with an oxyhydrogen flame. Subsequently, the H-shaped quartz tube containing the raw material to be distilled is transferred to a distillation furnace for distillation and purification, thus realizing the second use of the distillation tube.
Citation Information
Patent Citations
Regenerated process method for welding glass tube neck of vertical color kinescope
CN101350280A
Preparation device of gallium-containing chalcogenide glass having high melting point and high boiling point, and preparation method thereof
CN102786222A
Glass chip tube seal-cutting method
CN1816891A