TW514962B - Method and apparatus for reclaiming used solvent - Google Patents

Abstract

The present invention relates to a method of reclaiming a used solvent that has been used for dissolving a resist resin component or a used solvent containing a resin component that has been spent in a process of separating a resist resin on a substrate when manufacturing semiconductors or liquid crystal substrates. The method comprises the steps of removing a resin component, removing a volatile impurity, such as water, and refining the solvent. First, the resin component removing step is performed. After the refined solvent has been vaporized finally, the reclaimed solvent is recovered as a condensed solvent. An apparatus for performing this method is also described.

Description

514962 V. Description of the invention (1) '~-BACKGROUND OF THE INVENTION Field of the Invention The present invention relates to a method and a device for regenerating used solvents. In particular, the present invention relates to a method and apparatus for regenerating used solvents (e.g., separation liquids or scavengers that have been used to separate substrate barrier layers). The invention also relates to a method and a device for regenerating a diluent, which is a resin used for dissolving a semi-isolated or liquid crystal display or other similar manufacturing technology. Description of Related Art In the known technology, when manufacturing a semiconductor or a liquid crystal display, a heated solvent (scavenger) is a resistance layer for separating a substrate. The scavenger is usually composed of a mixture of monoethanolamine (hereinafter referred to as "MEA") and difluorenylsulfonate (hereinafter referred to as "DMSCT"). The scavenger mixture may also contain a small amount of water. In addition, the diluent may be propylene glycol monoethyl A mixture of ether acetate (hereinafter referred to as "PGMEA") and propylene glycol monoethyl ether (hereinafter referred to as "pGME,"). The diluent mixture is water-soluble and contains a small amount of water. Recently 'semiconductor and liquid crystal displays The size of the substrate has gradually increased. Therefore, more and more scavengers and thinners are used in the manufacture of semiconductors and liquid crystal displays. After using the scavengers and thinners, the service of waste disposal is usually collected Waste (used) liquids are disposed of. However, such collection is costly and the disposal of waste liquids can adversely affect the environment of the planet. Therefore, for used solvents (for example, used scavengers or Diluent) regeneration, there is an increasing demand to replace the treatment with used solvents.

2042-3900-PF.ptd Page 6 514962 V. Description of the invention (2) A known used solvent, in this method, it is difficult to operate in the same way as the original solvent for long-term stable regeneration. of. Therefore, regeneration methods and apparatuses for semi-used solvents are in this field. In addition, there is a need for the ease of maintaining the regenerated solvent even if the solvent is placed on the operation performance. The new solvent of the scavenger made by the regeneration side must also maintain the liquid crystal device. Since the device has been installed, for the quality and smaller methods, it is necessary to add or dilute it. And it has a large demand for distillation. It has been used to provide concrete products. However, in addition to the preparation, the quality is not yet established. Regeneration methods have not been established. The focus is on generating fruit and raw devices. Summary of the Invention Therefore, a form energy method and device of the present invention One or more kinds of solvent regeneration methods: when manufacturing semiconductor or liquid crystal substrates, have used two :: in the state, r is used in further manufacturing operations, and = two of the two: agent Ben Maoming's Another form is to provide a solvent regeneration device, which can be used for manufacturing, living body, or liquid crystal substrates, which can regenerate used solvents (for example, :: remover and thinner). It is also preferable that such a solvent has the stability of Qing and relatively small size. Straight / 、 Long-term 2042-3900-PF.ptd V. Description of the invention (3) Re-impurities in the solvent of this invention; In addition, the present invention is used as a condensing device. Used during the operation of the solvent removal device to remove the volatile solvent, preferably the tree-refined solvent. The dissolved resin removed according to this ingredient has long-term stability and purity. The detailed description of the present invention makes it easier to understand the teaching method, the refined solvent, and the refined solvent. It also provides a solvent-containing solution that can be decomposed in a solvent to remove hairy impurities. The lipid component has been refined after the invention of the downstream invention. The regenerative operation of the shadow of the component is dissolved and the above mentioned forms are involved. step. The solvent is completely resin-containing. Solvent resin composition; and a removal device is a post-evaporation method, because it ’s fine. Therefore agent. In addition to the state shown in the attached diagram for other purposes, the resin component is used to remove the resin component; the volatility is preferably removed, and the first is to remove the resin to evaporate, and then reuse the recycled solvent The regenerating component of the used solvent may include a resin component in the regeneration device for separating the impedance resin, a volatile component removing device, and a refining device for refining the solvent. Provided in an upstream position. In addition, in the method of recovering the regenerated solvent as the solvent component to be regenerated coldly, the resin is not subjected to suspension or the high refining efficiency can be obtained and the device according to the present invention reduces the refining efficiency. , Characteristics and advantages, after reading and Shen Qing patent scope, it will become a simple illustration. Figure 1 is a flow chart showing the steps of the method

2042-3900-PF.ptd Page 8 514962 V. Description of the invention (4) Figure, Figure 2 is a flowchart showing the preliminary method steps of a specific embodiment; Figure 3 is a flowchart showing the method steps of a specific embodiment Figure 4 is a flowchart showing method steps of a specific embodiment; Figure 5 is a flowchart showing method steps modified according to the present invention; Figure 6 is a flowchart showing method steps modified according to the present invention, FIG. 7 is a schematic diagram showing a solvent regeneration device according to a specific embodiment; FIG. 8 is a partial split structure diagram showing a resin component removing device; FIG. 9 is a schematic diagram of a volatile component tank and related device parts; FIG. 11 is a schematic diagram of two processed solvent tanks and related device parts, FIG. 11 is a schematic diagram of a condensation device and related device parts, and FIG. 12 is a schematic diagram of a solvent regeneration device according to another embodiment of the present invention. Explanation of reference numerals I: regeneration device; 2: solvent recovery tank; 3, 43: pump; 4, 8, 1 3, 25, 28, 32, 41, 47, 5 0 ,: pipeline; 5: resin component transfer 6 a: inlet port; 6b: outlet port; 7, 23, 39: tank; 9: distillation column; 10: filler; II: recirculation port; 12: steam discharge port; 1 4, 3 3: condenser; 1, 3, 4: discharge condenser;

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V. Description of the invention (5)%: recirculation tank; 37: recirculation path; return pipeline; volatile component discharge path; volatile component tank; transfer pump; tray; 16, 18, 20 21 22 26 29 31 : Steam discharge port; 42: heat exchanger; 4 5, 4 6: process solvent tank; 49: filter; Μ: spectroscope analyzer; 5 4: low-pressure duct; Ϊ 56, 66: heating device 5 8: rotation Body; 60, 62, 63 · Nitrogen conduit; 17, 36, • Recirculation pump 19 • _ —_ directional valve; 24, 40:: Heating reboiler 27 distillation tube branch; 30 distillation port > 38 Drain passage; 44 passage, 48 concentration control tank; 51 chemical supply tank; 53 pressure reducing device; 55 cylinder 57 evaporation surface; 59 brush, 61, 64, 65: open / close valve; 6 7: thermal insulation material; 6 8, 6 9: Unit. DETAILED DESCRIPTION OF THE INVENTION During the use of a crystalline substrate used in the present invention, the solvent used has been used to dissolve or, in general, a substantially small amount of water has been used. Solvents are waste liquids used in the manufacture of semiconductors or liquid separation resistance resins. 1 Including the main solvent components, resistance resin and

As shown in Fig. 1, the m method of the ancient anti-resin of the present invention includes removing the resin component (resistance, finally, after the solvent evaporates, dissolving the solvent :: damage (for example, 'water :: agent is recovered as a condensing solvent. This 'recyclable resin component can be removed first, for this reason; because of the influence of non-volatile or dissolved resin components,'; :::: will not be affected by suspension operation. This regeneration device can be stably operated In the method of regenerating the solvent, the condensation is removed. The solvent should be used as a part of this resin in Shen Ruqiang. For example, the resin component can be corresponding to 0.0. = Component, and finally the solvent is refined by evaporation and separation. This method of 4 2 can simplify the flow of the solvent (this: item 1 of the Qing patent scope). / Γ As shown in Figure 2, the exhaust gas system will The gas is discharged to the solvent containing the solvent which is evaporated in the method of processing the solvent. Such a milky condensing step is condensed, and the exhaust gas condensation step can be preceded by the step. The condensed liquid can be used as the used solvent ^ corresponding to Shen The scope of the patent is item 2). This can be used as a regenerating solvent. 〇Outside 'According to another method shown in Figure 3, the solvent used in the separation resistance method has been used, for example, by one or more main solvents. The scavenger composed of 'ΜΕΑ and DMSO as main components) is to be regenerated by removing resistance resin, water and other impurities (this method, item 3 of the scope of patent application). In addition, as in section 4 As shown in the figure, another method can be used to separate a variety of main components (for example, PGMEA and PGME as main components) ^

514962 V. Description of the invention (7) The diluent formed by # 7, used dilute: used for separation or other methods. Special and regenerative (this ::: wrong is made by removing resistance resin, water and other impurities resin to item 4 of the patent application scope). (In the falUng flI t component removal step, the use of the falling film should be applied to the patent application scope No. 5). And remove it with high density (this method will help you to allow the solvent of (carbonate); Γ absorbs this: gas / (called) and produces salt in the step, from the salt and Isolate ^ body 疋 in step 6 of volatile component removal step). The & solid method corresponds to the scope of patent application ..., the parent replacement is provided in each transfer, so that it has been fed to the next or previous step upstream or at the temperature of each step; :: Lotion can be used in lower devices: longevity (this method corresponds to the application "Fan Keyan extension") as described above, the solvent composition can be borrowed around item 7). Class. In addition or alternatively, gas such as The conversion of the lice body into salt shows that the gas that has been absorbed will be used in two, in the agent. The steps are removed as shown in Figure 5, and the dissolved gas will be further processed in a similar way to the gas mixture. Separation. As a result, the ultrasonic imprinting method or other beneficial effects can be reduced / reduced, and the regeneration solvent can be increased. The various non-patented scopes of the subsequent steps (item 8). Purity (this method corresponds to the first As shown in Figure 6 *, the quality has been refined, and the quality of the recycled solvent is continuously monitored and optimized to control the stability of the post-regeneration solvent.

2042-3900-PF.ptd 514962 w / combined wounds can be fished from the used solvents at lower temperatures and with greater pressure reduction. ι / -waste is used to prevent the device from being corroded by the Corrosion Training Institute. This structure provides anti-corrosion device, which does not need to use special metal as anti-corrosion material (for example, Η / ,,;-network trade name, can resist acid at high temperature and has high strength; another method corresponds to the scope of patent application. Item 10). f The concentration of m: mixed with volatile components (for example, water) separated by evaporation is adjusted in the volatile component removal step. : In this step, the volatile components can be smoked at a higher temperature than subsequent condensation ^.士士 里 —, person, t ρ / Ne Jia's 々, fruit / dish degree, condensed liquid r ^ Ό, in 竑 y step ’steam is transformed into cold Hi method corresponds to the Chinese version, please specialize the Waichuan item). From the tank :; 2: f of the solvent ’is provided by supplying nitrogen under pressure, and what? Day γ is fed and fed into the tank.妗 (This method corresponds to the quality of the virtual solvent from too much *, mouth, and quasi-recycling solvent to item 12 of the scope of patent application). = The volatile component isolated in the refining step or the hunting body is returned to the pump and the waste liquid is returned to the # η 梦 二 成 伤 removal step. Normally, wave the steps. In the result step: the same patent scope item 13 is performed again). σ 刀. # efficient (this method corresponds to the application as shown in Figure 7, #L ti + ro set; volatile component removal step ', want to include the resin component removal sequence from the upstream end to the bottom, 纟浐 j and refined Pei Zhi, which can be smooth, so: 1 heart =: because the resin component is first removed on the device. This ::: The effect will not occur in subsequent steps at the downstream end In addition, the regeneration The solvent is 514962 by evaporation and condensation. 5. Description of the invention (9) is finally obtained, which can obtain a high-purity, regenerated solvent (this method corresponds to item 14 of the scope of patent application). Resin component removal device Including the falling film as shown in Figure 8 makes the resin components easy to separate (this method applies to item 15 of the gamma range). Τ s ~ By removing the resin components (non-volatile components) first, The disadvantages of the device and solvent quality can be removed first. In addition, in the subsequent steps of the portion removal step, the miscellaneous column is added. Therefore, a packaged steam-saturated column (this ^ corresponds to a patent application) Range item 6 ^ Provide condensing device to condense the volatile components by evaporation. Keep the condensing device warm and maintain the condensing device within the target range of freezing / dish degree. Therefore, it is possible to make “a method corresponding to The scope of the patent application is No. 17). '. The knowledge and content Π' * By using a packed distillation column, the size of the regeneration device is small. Therefore, 'the ease of transportation and construction is considered, = the number of units that can be used by the device And the construction (this is around item 18). The application should go to the patent application. The specific embodiments of the present invention will now be described in detail with reference to the attached drawings. (Hereinafter referred to as "regeneration wear 1", 1 regeneration Xiang 1 can be used to carry out the solvent of the present invention), Fig. 12 shows the structure of regeneration t set to 1. Fig. 7 used to be regenerated Solvent L, which can be used in the manufacture of semiconductors or liquid crystal devices

2042-3900-PF.ptd Page 14 V. Description of the invention (10) Waste liquid collected after disposing. In addition, it is collected from the drainage system; condensed liquid. The used dissolver can also be collected via ΐ =: 帮 = 过: Solvent recovery tank 2 for solvent L, yes). (:: Removal of the solvent from the resin solvent removal device and falling film evaporation device from 2 Ming, H 2 / 46a and the paste are placed on the low surface of resin mating. In addition, the resin component outlet can be adjusted from It is discharged and connected to the resin composition tank 7. The resin composition tree r H, the steam discharge port 8a and the return solvent receiving port 8b are arranged on the upper part of the line 8: / multi-removing device 5. The steam discharge port 8a is via a second pipe Detect to the middle position of the steaming pipe (made to the column of the present invention). The steaming hall pipe 9 is a packaged steaming pipe 11 which is placed on the upper section of the steaming pipe column 9. The recycling port The distillate 10a and the steam discharge port 12 are arranged on the top of the distillation column 9. And the second one: 1 is provided by the first condenser 14 and the first-discharge condenser 15, Both include a cooling water circulation path: and the return pipe is wound? 0 is your eighth ^ recirculation tank 16 has a recirculation path 18, the agent can be discharged from the wide component discharge path 21. The solvent in the recirculation tank 16 Ρ Μ ^ 1 7. Divide more than one, and through the recirculation path 18, through the re-preparation of Yuyi Pump 1 7 to the re 掂 俨 + warehouse], LL ^ ^ Back recycled yield; m β shield another port via a return line 20 Valley agent ηιίί Γ valve 20 is furthermore a return line 'volatile components can be moved from the upper end portion of the groove 16 from the recirculation passage 18, a three-knife

514962 V. Description of the invention (11) = fI flows from the volatile component discharge path 21 to the volatile component tank 22. Volatile components may be discharged from the volatile component tank 22. Θ = outside, the filler 10b is arranged in the lower section of the steaming hall column 9. Slot 23 2] will be: 2: the bottom of the charge 10b, at the bottom of the column 9. The circulation line is connected to the heating reboiler 24 via the r-line, and the fourth line 28 and the second line 26 are connected to the 4th line 26, and the tank 23 is connected to the rectification column 27. In its ί: 3 I-pillar 27 is a tray-type tube column, and there are most of the trays arranged in the upper row of the second core j. The precision cylinder is arranged on the tray, and the base steam exhaust port 31 is arranged on the top of the precision hall pipe column 27. The second condenser 33 and the second exhaust condensation are set up. The steam exhaust port 31 is connected to J and then to 35. The two condensers 34 and 35 each include a cooling water circulation passage, and the recirculation tank 35 has a recirculation passage 37 and regeneration; = to the recirculation port 3. This section is removed. #Generating a wound discharge path 38 from the upper end of the slot 35 In addition, the slot 39 is provided below the tray, in part. The circulation line 41 connects the groove 39 in the pipe string: the removal of 227 and the return path 44 via heat exchange ... == Buddha ware 40, province 4 2 "+… aunt set) 42 and return pump 43, and The tank 39 in the official column is connected to the tree and the solvent receiving port 8b. The 77 seconds I indicates that the regenerating component discharge path 38 at 5 is connected to the first and second treatment solvent tank 46. The sixth line 47 is 4: : Qi: trough: 5 and the first knife will be the bottom of the grooves 45 and 46. Page 16 2042-3900-PF.ptd 514962 5. The description of the invention (12) is connected to the concentration control tank 48. In addition, the seventh line 5 〇 The concentration control tank 4 8 is connected to the chemical supply tank 5 through the filter 4 9 ′. The Teflon filter material is arranged in the filter 49. The chemical solvent in the chemical supply tank 51 can be supplied to the semiconductor or liquid crystal The manufacturing officer 50a is branched from the seventh guide member 50 located between the filter 49 and the branch of the chemical supply tank 51. The branch pipe 50a is connected to the spectroscope analyzer 52 and is connected to the seventh conduit 50 again. In addition, the low-pressure ducts 5 4 a and 5 4 b connect the pressure reducing device 5 3 (for example, a vacuum pump) to the first exhaust condensation丨 5, the second discharge condenser 34, the volatile component tank 22, and the processing solvent tank brackets and cents. Therefore, the pressure in the base distillation column 9, the rectification column 27, and the resin component removing device 5 can also be Reduce or lower. As shown in Figure 8 the body 5 5 and the surrounding gas are introduced from the outside 55, and the cylinder 55 body 58 is coaxial and can have a brush 5 9, radial 5 8 with a brush 5 9 In addition, the upper, middle temperature and pressure of the thermometer column 27 are rotated. The resin component removing device 5 includes a heating device 56 surrounding a closed cylindrical column 55. Steam or other to the heating device 56. The heating device 56 heats the cylinder The inner surface includes an evaporation surface 57. The cylinder is rotatably disposed inside the cylinder 55. The rotation body 58 extends to the surrounding surface of the rotation body 58. The rotation body contacts the inner surface of the cylinder 55. ^ 力 口 十The knife is provided in the distillation column 9 and the lower part of the rectification, so that the inside of the pipe string can be measured. In this specific embodiment, the outside of the column 9 and the rectification column 27. The boilers 24 and 40 are respectively provided in the distillation. However, the reboilers 24 and 40 can be

2042-3900-PF.ptd 514962 V. Description of the invention (13) In the columns 9 and 27, one piece (for example, in the form of a row of tubes) is formed with the grooves 23 and 39, which has substantially the same heating effect and can be Reduce space requirements. As shown in FIGS. 7 and 9, the volatile component tank 22 has a nitrogen pipe 6 0 and an open / close valve 6 1 a to introduce nitrogen into the tank 22. In addition, the parent valve 6 1 b, 6 1 c, 6 1 d, and 6 1 e are respectively provided in a system (ie, an air opening system) that is individually connected to the tank 2 2 and an upstream solvent feeding system (volatile The sexual component discharge path 21), the pressure reduction system, and the discharge system of the tank 22. Similarly, as shown in FIG. 10, the first and second processing solvent tanks 45 and 46 'have nitrogen conduits 62 and 63 and open / close valves 64a and 65a to introduce nitrogen into the tanks 4 5 and 4 6 respectively. in. In addition, the switching valves 6 4 b, 64c, 64d, and 64e and 65b, 65c, 65d, and 65e are provided in systems connected to the slots 4/5 and 46. In particular, valves 64b and 65b are arranged in the air-opening system. Valves 6 4 c and 6 5 c are solvent feeding systems arranged upstream (regeneration component discharge paths 38a and 38b); valves 64d and 65d are arranged in pressure reduction. System; and valves 64e and 65e are discharge systems arranged in tanks 45 and 46. As shown in Fig. 11, the insulation material 6 7 covers the f of the first condenser 1 4 and the surrounding surface, which is connected to the top of the distillation column 9, the first discharge === 1 5 and the freezing duct ( Cooling water). The heating device 66 is a heating device 66, which is wrapped in an insulation tube (Example 67, and covers a pressure reducing duct. Heating steam (1), Luo gas), which supplies heat, can be effectively used as the heating device 66. It will now be explained according to the operating procedure and the used solvent branch flow.

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Page 18 514962 V. Description of the invention (14) The operation of the bioreactor 1 is shown in Fig. 7 'due to the pressure reduction, the conductance reduction device 53 (vacuum pump) \ a and 54b conduct, when 5, retort column 9 And the distillation column 27 is a dimensional: tree knowing component removing device. In addition, the heating device moves the resin component :: vacuum state. The rectification column 27 is heated to a predetermined temperature. , Clothes set 5, beam distillation column 9 and then 'operate pump 3 to send the used material to the resin component removing device 5. For example, when a refrigerant recovery tank 2 enters 々 and υ is used, and it crosses the removal device 5, it is shown in Fig. 8 / The solvent L which has been injected into the resin component contacts the evaporation surface. 57.1% fruit transfer I58: brush 59 will be dispersed and used, and separated into volatile to 成 = 9 volatile components U is from steam steam ^ As a resin component removal device 5, can be used by Yue Benshan The thin film evaporator π manufactured and sold by Se1Zal Kalsha company has the same structure as the resin component removing device 5. /, /, $ The non-volatile component L 2 is along the resin component removing device 5 The inner wall is lowered and collected at the bottom and stored in the resin component tank 7 (see Figures 7 and 8). The volatile component L1 that has been introduced into the distillation column 9 is the rectifying solvent Lr moving downward. 1 and gas-liquid contact between steam moving upward due to heat, and steaming the crane in the fillers 10a and 10b. As a result, the volatile component L3 is evaporated. The evaporated volatile component L3 moves upward, And is discharged from the Thai steam exhaust 璋 1 2. Then, the steam is in the first condenser 1 4 and the first The drain condenser 15 is condensed. The cooling water is circulated around the condensers 14 and 15 of the invention description (15). The condensed solvent (that is, the liquid is in the recirculation tank 16. Then by recycling Pump I :: Time storage scale 'is discharged from the bottom of the tank 16 to the second of the distillation column 9; the port; the distillate 2 condensates the solvent. From the recirculated solvent Lrl and the second: = to the recirculation tank 16. In Renli in the recirculation tank 16; / 1Le back =, all rely on the discharge of volatile components .: Hair ::: tank 22, and stored in the tank 22 for discharge. Jun Mao ^ Chengzhi In order to discharge the

1 Γ, Ι ^ Π (X ^ ^ H) 61c ^ 61d Μ Γ, Λ Λ π II valve "exchange valve) 61b is opened, so that the pressure in the groove 22: 'close ^ door force release valve ⑽ and Open / close the door ... and e open. Then, the nitrogen passes through the open / close valve 6 22 = Volatile ingredient care ^: Close and open the wide door 61b, so that it is placed in the groove 22, so that r pinch Ltf. Then 'will open' close the valve 61. And 61 (1 open so that the volatile component L3 can be stored in the tank 22. As = tube; 9 = two '/ Γ has a considerable loss ^ Older, it? Liquid. Operate the transfer pump 26 to pass the portion L4 through the fourth conduit 28 and supply it to the rectification column. "The higher boiling point component L4 'of the precision column 27 is stored in the core = dagger 9. Some higher The composition of the Buddha's point "is moved upward by the heat moving two i〒. The evaporated component U is by the contact of the gas in the lower body-, the night-body 2 ring W and the vapor moving upward due to the heat 'via the tray 29 while distillation. As a result, the rectification component L5

(Final regenerative ingredient) Come up. Then, the refined ingredient L5 is condensed in the exhauster 34 discharged from the steam exhaust port 31. The cooling water is the second condenser 33 and the rectified component L5 condensed by the second discharge is temporarily circulated around. The condensate tube is recirculated in the tender hall: any bottom of the predetermined level of the tank 35: ί re: shield, bath Lr2. Exceeded recycling 38 and passed to the processing solvent sample 45: 2: 疋 through the regenerative component discharge path central benefit: "One of them, and stored in tanks 45 and 46: as. When one of the regenerant bath ingredients (Seikan ingredient) L5 is filled, you can choose to use another processing solvent ;;. As shown in Fig. 10, the first processing solvent tank 45 is filled / closed and 64d is closed ', and the second processing solvent is opened 2 The valves 65c and 65d are opened S, so that the recycled solvent composition can be stored in the second processing Solvent tank 4-6. When the first or second processing solvent tank 45 or 46 is filled, nitrogen gas is passed into the tank under pressure. As a result, the solvent component is regenerated. It is from one or the other of the filled tanks “or 46” to alternately enter the concentration control tank 48 via the sixth line 47a or 47b. As shown in FIG. The regenerated solvent component L5 was discharged, and the opening / closing valve 64b was opened so that the pressure in the tank 45 returned to atmospheric pressure. Then, the valve 64b was closed and the opening / closing valves 6 4 a and 6 4 e were opened. Next, nitrogen Feed to tank 45 via opening / closing valve 6 4 a to discharge the regenerated solvent component L5 from tank 45. When the discharge is completed 'close / open valves 6 4 a and 6 4 e and open valve 6 4 b ,

514962 V. Description of the invention (17) The pressure in the groove 45 is returned to atmospheric pressure. Then, the opening / closing valves 6 4 c and 6 4 d are opened, so that the regenerated solvent component L 5 can be stored in the tank 4 5. A similar operation of opening and closing the valve is performed to discharge the regenerated solvent component L 5 from the second processing solvent tank 46. The concentration of the regenerating solvent component L5 in the concentration control tank 48 is controlled within a specific concentration range required. In particular, the spectroscopic analyzer 52 is provided downstream of the concentration control tank 48 and quickly analyzes the > degree of the regenerated solvent component L5. According to the result of the analysis', if the concentration of any component (for example, μ E A and DMSO) does not reach a specific concentration range, an additional amount of component will be supplied. If the concentration of the ingredients is within a specific concentration range, no such adjustment is required (see Figures 6 and 7). The spectroscopic analyzer 52 measures the component concentration of the regenerating solvent component L6 flowing through the branch duct 50a by analyzing the infrared light of the absorption wavelength. If the concentration of the regeneration solvent component L 6 is not within a specific concentration range, the spectroscopic analyzer 52 stops the regeneration device or adjusts the concentration. Various spectroscopes can be used as the spectroscope analyzer. The filter 49 removes the coarse particles in the regenerated solvent component D6 with the adjusted concentration. The filtered solvent L6 is stored in the chemical supply tank 51 to be supplied to the manufacturing steps in the reverse direction. ^ According to this embodiment, the efficiency of regenerating the used solvent can be improved, a regenerating solvent with stable quality can be obtained, the life of the regenerating device can be extended, and the amount of waste solvent can be reduced, and thus the disposal cost of the waste solvent can be reduced. It also reduces the harmful effects of used solvents on the planet's environment. In addition, in the distillation column 9 and the rectification column 27,

514962 V. Description of the invention (18) ---- (evaporation under reduced pressure), and the solvent component is separated from the used solvent containing the mixed component at a lower temperature. Therefore, by separating the solvent at or below a specific temperature, the regeneration device can be operated for a long time 'without using special materials or requiring frequent replacement of parts. For example, as shown in Table i below, regarding the mixture of MEA and DMS0, when the pressure is reduced by 12.7 kPa from the conventional pressure p0, the temperature of SUS304 can be reduced by about 40% from the conventional temperature TO. As a result, the corrosion rate can be greatly reduced. Therefore, the life of the regeneration device can be extended without using special materials. In addition, it can also reduce the manufacturing cost and the transmission time. Table 1: Temperature and corrosion rate pressure (kPa) of the separation solution (70% MEA, 30% DMS〇) in SUS3 04 (P0 P0-6.7 P0-12.7 temperature rc) TO T0-15 T0-40 Corrosion button rate XΙΟ · 5 (ml / year) 20 15 7 ~ 0 Furthermore, according to this embodiment, the used solvent L can be regenerated and recovered. As shown in Table 2 below, up to about 90% of the used solvent L can be regenerated. Therefore, the amount of solvent that must be purchased can significantly reduce the total amount of new solvent to be supplied by less than 10%. On the other hand, if such a regeneration device cannot be used, the conventional method requires the purchase of a solvent of 1000%. Therefore 'can reduce the cost of purchase and the amount of waste solvent, and therefore can also significantly reduce the disposal cost of waste solvent. In addition, the method of discharging condensation

514962 V. Description of the invention (19) It can further increase the amount of renewable used solvents. Therefore, the absolute amount of the regenerating solvent can be increased, the treatment method of the exhaust gas is also mild to the environment, and the purchase amount of the new solvent can be reduced. In addition, "the quality of the regeneration solvent can be stably maintained", and the life of the regeneration device can be extended. Table 2: Comparison of effects between regenerating devices with or without solvent (the amount of new solvent to be supplied is considered as 100) used solvent L regenerated solvent waste solvent other C including release system) newly supplied solvent (Purchasing solvent) Unused regeneration device 102 0 102 7 100 (100) Utilized regeneration slurry 102 92 10 7 100 (8) Drain condensation 107 96 11 2 100 (4) Although the regeneration device 1 described above is in order It is formed by combining the resin component removing device 5, the distillation column 9, the rectification column 27, and other parts, but the regeneration device 1 can also be divided into device parts so as to form a large number of units first. Each unit can be connected together at the installation site to form the regeneration device 1. For example, as shown in FIG. 12, the units 68 and 69 are first constructed separately and connected together at the installation site by bolts or other tethering devices.

The connecting ducts and transmission pipes between 68 and 69 are easy to install by connecting flange structure. J

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Page 24 514962 V. Description of the invention (20) Efficacy of the invention According to the application, the agent can be used. The cold obtained according to the application system is based on the application or multiple main components. According to the application or multiple main components according to the application, the components in the solvent used in the application can be separated according to the application. Regeneration efficiency in solvents. Depending on the composition of the application agent, actions can be taken to correct the solvent. The resin of the patent range composed of the patent range of the liquid patent range can be easily removed. The excess of the patent range of the patent range of the patent range can be easily changed. The first invention defined in the item is recovered and regenerated in a solvent-forming / cereal formulation, thereby obtaining a usable solution. The second invention defined in the second item is recovered and discharged into a solvent component. The third invention defined in item 3 can be recovered and regenerated by a scavenger. The fourth invention defined in item 4 can be recovered and regenerated by a thinner. The fifth invention defined in item 5 can be effectively removed first so that it can be carried out later. The sixth invention as defined in item 6, is separated in the gas removal step. The seventh invention, as defined in item 7, can be extended. The eighth invention, as defined in item 8, can be removed first. The dissolved gas can be removed first to improve the recovery and definition of item 9 The ninth invention, regeneration; continuous analysis during operation of the bioreactor, and can quickly = why not suitable conditions. Because of &, the stable product should go to the chemical supply tank. θ

^ 62

According to the scope of the patent application, the separation temperature can be reduced by the decrease in pressure; Tenth invention ’Solvent is separated at a temperature lower than a certain temperature. It is separated at a specific temperature or special operation. * No special materials are required. Dry cracking can be used for a long time and stable operation. According to the scope of the patent application, u; =! Replace parts. Considering the optimum conditions of cold temperature, l m " month 'is liquefied under consideration. Military injuries can be defined by condensing equipment = as defined in item 12 of the scope of the patent application ^ ^ ,, ^ ^, ~ av A "π W The meaning of the twelfth =: No impurities will be mixed into the solvent. The thirteenth invention, as defined in the thirteenth invention, can be separated and re-extracted to improve the efficiency of regeneration. The dry% μ is based on the fourteenth invention defined in item 14 of the scope of the patent application. The solvent = wound can be recovered and regenerated from the used solvent. The defined fifteenth invention, the resin component contained in the used solvent, can be effectively removed first. ^ According to the sixteenth invention defined in item 16 of the scope of the patent application, the steamed crane official column and the complete device obtained therefrom are already smaller to reduce costs and improve the solution properties of the construction. According to the seventeenth invention defined in item 7 of the scope of the patent application, the production of $ Shen Dianwu can be avoided, which may be caused by the change of the surrounding temperature in a particular season. Especially in winter, super-cooling caused by low ambient temperature conditions can increase the generation of precipitation. However, the present invention can overcome such

2042-3900.pp.ptd

Page 26 514962 V. Description of the invention (22) The problem and a stable quality recycled solvent can be obtained. According to the eighteenth invention defined in item 18 of the scope of patent application, the complete device can be functionally divided into a plurality of units to improve the ease of transportation and construction.

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Claims (1)

514962 ^ July y amended the sixth edition of the scope of the patent application1. A method that completely removes the solvent from the removal of refined solvents2. If the cold solvent gas in the application system is recovered 3 Used solvents. 5 · Rushen Resin composition shift 6 · Rushen Volatile content Gas components can be separated. 7. Rushen will transfer each transfer room. 8. Recycling method of used solvents. Including: Resin components are removed from used solvents. Hairy impurities; and agents; where resin components are first processed. In the removing step, after the solvent, the regenerated solvent is recovered as a condensing solvent. The method mentioned in item 1 of the claim / profit scope further includes a step of condensing and discharging the gas, and the exhaust system discharge includes evaporation, wherein the condensed liquid obtained in the condensation step is a part of the used solvent. Serving. The method described in item 1 or 2 of the patent scope, which includes a scavenger composed of one or more solvents. The method described in item 1 or 2 of the patent scope, wherein the method includes A diluent, which is composed of one or more solvents, and the method described in item 1 or 2 of the patent scope, wherein the removing step includes a falling film evaporation step. μ Please refer to the method described in item 1 or 2 of the patent scope, in which the volatile components and gas components in the step of dividing are divided at a temperature above or above the threshold temperature of the separation " ^ Patent Range No. 1 The method according to item 2 or item 2, wherein a heat exchange device is provided upstream of: the agent is recycled, transferred or returned.隹 ^ 之 or the method described in item 2, wherein in ίΜΟΙΗΛΗ. ') Iwi "••… Cafe " "' ― 丨 丨 丨 ·· --- / 丄 丄 Amendment No. 9mnQ Prior to the patent scope resin component removal step, the & & ^ ^ ^ A Λ, Shi ^ ^ also includes a gas removal step. 9. The method described in item 1 or 2 of the patent application scope, n P Ϊ essence = agent, the main feed J "jin" and return to the main feed conduit, where the analysis device J controls the components of the processing solvent and controls the operation of the device.,-\ 0 · The method as described in item 1 or 2 of the scope of the patent application, which means that the separation of the solvent components in the used solvent by evaporation is separated by a decrease in pressure, and the separation temperature is low: Threshold temperature for anti-corrosion. Inverse material Π • The method described in item 1 or 2 of the scope of patent application, wherein the concentration of the solvent in Ϊ Ϊ Ϊ ΐ is adjusted in the volatile component removal step. The temperature of the outlet during the volatile component removal step is controlled at the condensation temperature. The temperature is within the range of, and is higher than the cold temperature in the condensation step. ^ 12. The method as described in claim 1 or 2, wherein the solvent is supplied by nitrogen under pressure, and Supply from a tank and / or a processing solvent tank to the subsequent steps. 1 3 · The method as described in item 1 or 2 of the patent application scope, wherein the return path is provided in the waste liquid path, wherein, in the refining step The residual liquid in the liquid is discharged as waste liquid, and the return path can be selectively used to return the residue to the resin component removing step. 1 4 · A device for regenerating a used solvent containing a resin component, including · Resin component removing device for removing resin component; Page 514962 Amend ______ a volatile component removing device to remove volatile impurities; and a refining device 'for refining the solvent; wherein the resin component removing device is provided upstream, after the refined solvent has evaporated downstream The recovered solvent is recovered as a condensing solvent. 15. The device according to item 14 of the scope of patent application, wherein the resin component removing device includes a falling film evaporation device. ^ 16. The device according to item 14 or item 15 of the scope of patent application, wherein one or both of the volatile component removing device and the refining device include a packaged steaming tube column. The device according to item 14 or item 15 of the scope of patent application, which includes: providing a condensing device to condense volatile components, removing the volatile surname removing device ', and wherein the condensing device is holding Warm, pre-chilled circulating freezing temperature range. 2. The device described in item 14 or 15 of the scope of patent application, the j solvent regeneration device is mainly composed of a resin component removal device, a volatile removal device and a purification device, and the device is divided in ^ Between the two devices, so as to form the majority of the units, the combination is formed to form the device. 19. The method according to item 3 of the scope of patent application, wherein the volatile components and gas components are separated at a temperature above the threshold temperature or threshold temperature of the gas. Xingjie is the device described in item 14 of the scope of patent application, in which the volatile distillation tube ^: ^ 2-one or two of the refining device, including-packaging X's Jiang w > and & a condensing device for Volatile components are condensed, basin p — ----- injury removal device, and the condensing device is kept warm "Duo Zheng Shan-^^ J〇109865 6. The scope of the patent application is warm, so as to maintain a ^ 21 \ The temperature range of the circulating freezing temperature in which the resin is included. The volatilization includes a package of taxi. The removal of the ingredients as described in item 20 of the patent application scope. 4k only. A falling film evaporation device. Μ #: As described in item 14 of the scope of the patent application, one or both of the removal device and the refining device are placed i divided = a condensation device to remove the volatile components: solidified removal device, volatile The component removing device and the refining device are divided into at least two devices, and then the number of units is formed first, and the units can be combined to form the device. 23. The device according to item 22 of the scope of patent application, wherein the resin component removing device comprises a falling film evaporation device. 24. The device according to item 16 of the scope of patent application, wherein the solvent regeneration device is mainly composed of a resin component removing device, a volatile component removing device, and a refining device, and wherein the device is divided into at least two Between the two devices so as to form a plurality of units first, the units can be combined together to form the device. '° 25. The method as described in item 4 of the scope of the patent application, wherein the volatile component and the gas component in the volatile component removal step are at a threshold temperature at which the gas component can be separated or a temperature above the threshold temperature. Separation. Page 31