TWI250178B - Process for recycling of PET-materials - Google Patents

Abstract

A process for recycling of PET-materials and/or articles of PET provides that the PET-material to be processed is heated in the course of a pre-processing and is dried and simultaneously crystallized at an elevated temperature. This pre-processing is followed by a main processing that is performed under vacuum conditions. Within this main-processing, the PET-material is again dried and crystallized at a temperature that is higher than the temperature at which the pre-processing is performed. Preferably also within the main-processing step, plasticizing of the material is avoided, and plasticizing and melting is made only after the main-processing step.

Description

1250178 _ Case number V. Invention description (1) [Invention background] 89119294

SUMMARY OF THE INVENTION The present invention is directed to a method and apparatus for recovering PET materials and/or articles made from pET materials, as set forth in the requirements of items 1 and 32 of the patent application, respectively. When recovering polyethylene terephtalate or polyethylene terephthalate materials, in order to avoid hydrolysis caused by hydrogen during plasticization or drying ( Hydr〇lytic) to reduce the molecular chain, it is important that the recovered PET material is as dry as possible. However, an effective drying effect is only when the temperature-increasing and non-crystalline PET particles or PET portions adhere to each other. For this reason, a knot-crystal of a pET material is obtained before the drying process. By uniformly moving (1111丨{0]:11117111(:^11§) or mechanically processing the particles at a temperature that is cooler than the drying temperature, in any case, a temperature lower than the plasticizing temperature can be obtained. The crystallization. However, because the recycled PET material or the material composed of ρΕΊΓ material, especially the PET bottle, is mostly contaminated and cleaned, it may be pre-cut, and the same stained, mostly cut or Milling, washing and drying. Such pre-drying treatment will at least not exceed the treated moisture content of the moisture content (%) of less than 6.5 percent by weight (%). According to the rules, pre-cutting and pre-cleaning treatment are required.

Page 6 1250178 - Case No. 8Q11Q刈4_羊月日攸,不_五,发明说明(2) ' " ' The purpose of the present invention is to provide an efficient and as fast as possible recycling of PET material as described above. A method in which the PET-granulate obtained from the melt or the PET particles has a higher viscosity value than the recycled viscosity value (viscosi ty - values). The melt obtained from the 'further' or the PET pellets obtained from the melt should conform to the rules for the treatment of food residue technology, that is, the most appropriate method in the PET material. Hazardous substances or 9 dosing & substance removal. The method for achieving the foregoing process of the present invention is set forth in the special part of the first item of the patent application. Accordingly, the PET material provided herein is subjected to a two-stage process in the present invention wherein no plasticization (1) 1 & 31 is made for the material in the pre-treatment apparatus. 1^^^〇11) However, in the case of drying, the crystallization and some degree of pre-denication occurred. This pre-concentration is obtained by an appropriate temperature which is produced by mechanical action of the ρΕτ material or by the introduced power. In particular, the temperature is raised or controlled by means of the mechanical means of the material or by at least a mixing and/or cutting element by means of friction: the production of jin = can be converted into kinetic energy. ... In the main processing process in the main processing equipment, the PET material is further dried and crystallized at a higher temperature, and has a period of staying in a high vacuum state, again using mechanical treatment and materials. The coagulation introduces power, and the corresponding thermal energy is introduced into the PET material by the rotation of at least one of the agitation and/or comminuting elements to heat it again.

Page 7 1250178 -MM 89119294__年月日日_Amendment_ V. INSTRUCTIONS (3) The main treatment is affected by the vacuum state, reducing the moisture to a predetermined average value, and the volatile harmful substances will also be from the PET. Material separation. The temperature of the primary treatment is maintained below the melting temperature of the PET material, particularly below the melting temperature, which is between about 4 and 6 degrees Celsius. However, it is best to keep the temperature as high as possible at this temperature. After the primary treatment, the PET material is simultaneously plasticized from an extruder output, preferably attached directly to the primary processing device. Due to the direct vaccum-tight connection, the vacuum in the primary processing unit can be applied to the iiUet section of the extruder. The extruder includes a plasticizing zone after a pressure zone and a compression and damming zone. The screen P early zone 又5 stands again after the volatile matter can be melted by a vacuum (especially a high vacuum) to extract a venting zone or a evacuation zone from the material. Within this range, it is possible to provide exhaust in a single stage or in multiple stages, or to create a plurality of pressure zones and decompression zones with different degrees of vacuum before and after, so that substances that continue to be dirty or difficult to evaporate can also evaporate. The viscosity of the melt obtained from the extruder and the PET pellets can be adjusted by selecting an appropriate temperature and residence time in the main treatment and pretreatment, by vacuum Appropriate long residence time and appropriate temperature conditions can achieve positive impact on viscosity and reach - in order for your reviewers to understand the purpose, features and efficacy of the present invention, by the following specific examples, and The present invention will be described in detail with reference to the accompanying drawings, which are set forth below. x

Page 8 1250178 Emperor 89119294 V. INSTRUCTIONS (4) EXAMPLES Description The PET to be recycled, especially a pet material and/or pet, can be ground into a powder in the cutting device 1 and then passed through the washing unit... Washing unit) (2) Transport to pre-drying unit (14) for pre-drying. If desired, the PET bottle can be pre-ground in a suitable powder state to an average size of about 15 to 25 mm. Washed and dried pET material Since the process technology should be as small as possible, the residual moisture after grinding into powder should be up to about 1.25 percent by weight. The PET material that needs to be pre-treated is sent to the pre-process device (3) to be pre-dried, and if necessary, can be further cut, and the pre-process device (3) is heated in addition to the drying process. And crystallization treatment. Rotary agitation = / or cutting element (5) is provided in the front process device (3) to rotate at a peripheral speed of 9 to 15 meters / sec. This ensures that the power of the mechanical motor is converted to thermal energy by the friction between the stirring tool and the ρΕτ debris or PET material. The average dwell-time or the throughput of the PET material is controlled at about 35 to 65*(min), and the optimum time is between 40 and 60 minutes. Within this, the temperature of the PET material is adjusted from about 14 摄 to 190 ° C, but the optimum temperature is between 15 〇 and 16 摄 Celsius. At this temperature, the surface water evaporates immediately, and due to the long residence time, there is also a substantial area containing moisture or other containment emigrates. The processing of the material of the pre-process device (3) can be handled under vacuum, and the bran and the first place are not absolutely absolute, but it is better if possible. The residence time of the PET material in the pre-process device (" should be reduced, and the volume of the device is also 1250178. The case number 891 is defeated by Q4. 5. The invention description (5) 曰 corrected the relative reduction. For the material used in the process, or in the pre-process unit (pre_nrnr^. TT+) to prevent deuteration as 6 prc)c^ssing uni t:)C;3:) θ I ♦ +71 cutting, the process will be more appropriate. ... and cut the PET material into the pre-process unit (7) (four) 35 by # (SUPPlying unit) (18), the supply unit (18) has, for example, a belt, the PE = material by the - transport unit (7) via a special image Yes - wheel = rod outputs the pre-process device (3), the material can be supplied via an intermediate st〇rage means (6), the mother is supplied by a unit, such as a conveyor screw (convey〇r screw) (17f to the transfer process unit (4). ^ ii The transfer unit (7) is to be placed in the front process unit (3) and maintained at a temperature between 140 and 170 degrees, especially between 15 and 16 degrees Celsius. Between the parts - in the main process unit (4), some of the particles of the PET material adhere to each other or are sintered together. These pE T materials are mainly composed of a rotating stirring and/or cutting element (5). Cutting into pieces, and the temperature of the synthetic plastic material is increased to 170 to 180 degrees Celsius, especially at 18 degrees Celsius. The peripheral speed of the stirring and/or cutting element (5,) is substantially matched to the front process device ( 3) The peripheral speed of the stirring and / or cutting element (5): about 9 to 15 meters / sec. The volume of the receptacle of the main process unit (4) can be selected to obtain an average residence time of PET material for about 40 to 90 minutes, especially the average residence time of 50 to 90 minutes. The pressure in the device (4) is adjusted to a value less than 20 mbar, which is best if it can be adjusted to a value smaller than ^ mbar. In the main process unit (4) Screwed (with) or water

Page 10 V. Description of the invention (6) — Set (1 5 ) fill ' to operate two gas seals or tight or vacuum-tight slide gates ( 15 '), thus guiding a batch Batch of PET material enters. A vacuum pump (16) is placed on the main process... device (4). A sander (8) is coupled to the main process unit (4), and the pET material is output from the main process unit (4) and then processed through the extruder (8). In the extruded state (8), the p e T material is plasticized or melted. The extruder (8) may include at least one degassing zone (9)' a vacuum pump (丨〇) coupled to the exhaust opening ^ of the extruder casing, in order to adjust the pressure to the ratio丨〇 mbar is still a small pressure, especially less than 5 mbar. If at least one venting zone is provided, a vacuum-like scent may be provided if possible, and the moisture and/or other separated products may be affected. _ We can see the above process parameters, the viscosity value of the molten pET material or PET particles can be obtained from the viscosity value of the supplied PET material. The remelted PET material has a viscosity that is about 5% higher than the material at the beginning. In particular, the viscosity can be increased by a two-stage process and by adjusting the temperature of the blending, the vacuum pressure, and the number of vacuum zones or venting zones. In a preferred embodiment of the present invention, the extruder (8) is hermetically coupled to the main process device (4), and the vacuum of the main process device (4) is applied to the extruder Opening. A screening or filtering device (11) is coupled to the extruder (8) and passes through the melt input device (12) therein to produce ρΕτ particles. A device (13) can be placed between the extruder (8) and the filtering device (11) to measure the viscosity of the obtained flammable material. 1250178 Case No. 89119294 曰 Amendment 5, Invention Description (7) In the extruder, we can see that not only the water, but also the appropriate adjustment of temperature, pressure, residence time and shearing action (shearing act ion) ) to separate the separated product. - If the PET material is fed into the main process unit (4) from the front process unit (3) in the case of exhaust air, the pre-dried PET material can be prevented from being wet again. In order to prevent the extruder (8) from exhibiting a vacuum, in particular in the exhaust zone, it is returned to the main process unit (4), compressed in the extruder (8), or transported by the extruder. The material is taut, eliminating the vacuum reaction of any major process unit (4). The same vacuum reaction takes place between the main process unit (4) and the pre-process unit (3). However, in this case a reaction with a suitable leeches side door (15,) can be included. If the front process assembly (^) is directly attached to the main process unit (4), the transport screw must be vaccum-t ight. It would be advantageous if the extruder (8) contained at least one pair of venting zones. § Delivered to the main process unit (4), the pET material in the input sluice is preset to pass a vacuum in the main process unit (4), so there is no substantial pressure reduction in the main process unit (4). This is beneficial because the amount of vacuum directly affects the separation and viscosity of harmful substances. An intermediate storage device (6) is provided. An irregular front process device (3) is tolerable. The process used to recover the crushed material comes from pre-classified and pre-cleaned bottles or containers and is cut to a size of 15 to 25 mm.

Page 12 1250178

Case No. 89119294 V. INSTRUCTIONS (8) The temperature increase of the PET material is preferably heated by means of rotary stirring and/or cutting of the device (4). If the main process unit (4) also provides heated pET material α is very beneficial. π is not also in the pretreatment process, the PET material can also be cut first. The configuration of the mixing and/or cutting elements is also matched to each other. The σ-representation shows an embodiment of the invention in which the PET material white-process device (3) is directly delivered to the main process unit (4). First - county one $

According to another embodiment of the invention, the PET material is delivered to the main process unit (4) from the front process unit (=) the intermediate storage unit (6). The necessary driving means for the agitating and/or cutting element (5, 5,) or the wheel device or the extruder (8) are not indicated by the Μ shown in Fig. 1 7), respectively. " ‘Or

1250178 -j No. 89119294_年月曰 修正 _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ [Description of the number] I cutting device (comminuting apparatus) 2 washing unit (u n i ΐ ) 3 pre-processing device (ρ r e -1 r e a t m e η t a ρ ρ a r a t u s ) 4 main processing apparatus (main processing apparatus)

5 rotating mixing and / or comminuting element 5 ' cutting element 6 intermediate storage means 7 conveyor unit (conveyor unite) 8 extruder (extruder) 9 exhaust area (degassing -zone) II filtration, filtration device 12 device 13 device

1 4 unit (un i t) 15 water E device (sluice device) 15' sluice siding gates 16 vacuum pump (vaccum pump) 7, 17 transport device (conveyor means)

Page 14 1250178 Case No. 89119294_Yearly Month Day_Revision Diagram Simple Description 1 7Transport Screw

Round II Page 15

Claims (1)

1250178 ^S_89U9294 曰Revised Patent Application No. 5. The processing chemist for recycling PET materials as described in claim 4, characterized in that the pre-process stage is between 1500 and 160 degrees Celsius. The temperature is down, and the duration of the process is 40 to 60 minutes. The method for recycling PET material as described in claim 1 or 2, characterized in that the PET-metal foil and/or PET-fiber and/or thin front The process stage is carried out at a temperature in the range of 170 to 200 degrees Celsius, and is provided by the mechanical treatment or heating of a mixing and/or cutting element, which is based on the average residence time or pre-process stage of the PET material. The duration of the duration is 10 to 30 minutes. 7. The processing chemist for recycling PET material according to claim 6, wherein the pre-process stage is performed at a temperature of 180 to 200 degrees Celsius, and the duration of the process is 1 0 to 1 5 points. 8. The method for recovering PET material as described in claim 1 or 2, wherein the pre-process stage is carried out under vacuum. 9. Process for recycling PET material as described in claim 4, characterized in that the pre-process stage is carried out under ambient pressure. 1 0. The method for recycling PET material as described in claim 1 or 2, characterized in that the contaminated PET material in the pre-process stage Page 17 1250178 Amendment f No. 89119294 ', the scope of the patent application is removed under long residence time 11 · The flow of the method of claim. The material for recycling PET material mentioned in Item 1 or 2 of the patent scope is characterized in that the PET material is in continuous reading under the effect of the pre-process stage. The method for recovering pET material according to item 2 is characterized in that in the prior process, the PET material is subjected to intermediate storage for the intermediate storage between the pre-process stage and the main process stage, the storage The duration of the duration of action is between 8 到 % and 1 2 〇 % of the previous process phase and the temperature of the pre-processed PET material is as stable as possible during intermediate storage and/or during delivery to the process. . - The storage method of the present invention is as follows: The treatment method for recovering PET material as described in claim 12 is characterized in that the temperature is maintained at 130 to 190 degrees Celsius. 14. The treatment method for recovering pET material as described in claim 12 is characterized in that the temperature is maintained at 1,500 to 170 degrees Celsius. 15. The method for recycling PET material as described in claim 1 or 2, characterized in that it is carried out under vacuum in a main process stage, the pre-processed PET chips and/or the mill The broken bottle material is mechanically treated at a temperature between 170 and 210 degrees Celsius, or is heated by at least one agitation and/or cutting element input process*, characterized by an average residence time of the PET material or the primary Page 18 1250178 -_Case No. 89119294 __Yearly Month Day_Amendment VI. Patent Application Scope The duration of the period is 40 to 10 minutes. 16. A method of treating PET materials as recited in claim 15 wherein the primary process stage is at an ambient pressure of less than 2 mils. 17. A method of treating PET materials as recited in claim 15 wherein the primary process stage is at an ambient pressure of less than 10 mbar. The method for treating recycled PET materials as described in claim 15 is characterized in that the PET chips to be treated and/or the crushed bottle materials are under 180 to 200 degrees Mechanical treatment. 19. The method for treating recycled PET material according to claim 15 of the patent application, characterized in that the duration of the main process of the PET material is between j50 and 90 minutes. 20. The method for treating recycled PET material according to claim 15, wherein the main process stage is under an environment having a pressure of less than 20 mbar. 21) A method for treating recycled PET material as described in claim 20, wherein the main process stage is performed in an environment having a pressure of less than 1 Torr. Page 19 1250178 Case No. 8911Q is called 4 曰 ▽, the scope of patent application is used. Amendment 22. The method for treating a ρΕτ material as described in claim 6 wherein the main process stage is in a vacuum state, and the pretreated PET foil and/or ΡΕτ fibers are Between 16 摄 and 21 摄 degrees Celsius, or a mechanical power is introduced, which is added by at least one stirring or cutting element, characterized by the average residence time of the bismuth material or the main process stage The duration of the duration is 5 to 25 minutes. 2 3. The method for treating recycled PET material according to claim 22, wherein the main process stage is maintained at 170 to 205 degrees Celsius. 24 as described in claim 22 The method for treating recycled PET material is characterized in that the duration of the main process of the PET material is from J 〇 to 15 minutes. 25. The method for treating recycled PET material according to claim 22, wherein the vacuum pressure is less than 150, and the vacuum pressure is less than 50. In the scope of patent application, item 1 or 2, J, is a reasonable method for recycling PET materials, characterized in that the heat is reduced or cut by 26. As described in claim 25 of the scope of application. For the treatment of recycled PET materials, 丄4+ 士微A吉步厌:七,丨,在5 〇& Page 20 1250178 _ Case No. 89119294_Hand Month VI. Application for Patent Scope Provided. 28. A method of treating a recycled PET material according to claim 1 or 2, wherein the material is previously cut and/or cleaned and/or pre-dried prior to the pre-process stage. The processing method for recycling PET material according to claim 28, wherein the PET material is cut to a size of 15 to 25 mm before the pretreatment, as in claim 1 or as claimed in claim 1 or The method for recovering pet material according to item 2, characterized in that the PET material is provided by a device, and the main process stage of the device 3 is operated by an extruder under vacuum. The processing method for recovering pet material as described in claim 1 or 2 is characterized in that a read vacuum state exists in the main process unit to act on the inlet region of the extruder. ^ 32 The method for recovering NT material according to item j or item 2 of the patent application scope is characterized in that the plasticized or melted pET-material is granulated before being filtered.