CS265342B1 - A way of evaluating the aging of polyesters, especially overweight - Google Patents

A way of evaluating the aging of polyesters, especially overweight Download PDF

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CS265342B1
CS265342B1 CS88397A CS39788A CS265342B1 CS 265342 B1 CS265342 B1 CS 265342B1 CS 88397 A CS88397 A CS 88397A CS 39788 A CS39788 A CS 39788A CS 265342 B1 CS265342 B1 CS 265342B1
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spherulites
aging
chloroform
size
polyesters
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CS88397A
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Czech (cs)
Slovak (sk)
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CS39788A1 (en
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Magda Ing Mitterpachova
Ivan Ing Drsc Diacik
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Magda Ing Mitterpachova
Ivan Ing Drsc Diacik
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Priority to CS88397A priority Critical patent/CS265342B1/en
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Publication of CS265342B1 publication Critical patent/CS265342B1/en

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Abstract

Riešenie sa týká spósobu hodnotenia starnutia polyesterov, hlavně nedlžených polyesterových vláken a fólií, ktorých dlžitelnosí pri dalšom spracovaní závisí od stupňa zostarnutia polymeru. Riešenie spočívá vo vyvolaní sférolitov v polymére pósobením chloroformu na polymer a v meraní velkosti takto vyvolaných sférolitov pomocou elektronomikroskopických obrázkov. Čím je zotrvanie nedlžených polyesterových vláken medzi zvlákňovaním a dlžením vačšie, tým sú vačšie vyvolané sférolity a tak je zhoršená dlžitelnosí.The solution concerns a method for assessing the aging of polyesters, mainly undrawn polyester fibers and films, the elongation of which during further processing depends on the degree of aging of the polymer. The solution consists in inducing spherulites in the polymer by treating the polymer with chloroform and in measuring the size of the thus induced spherulites using electron microscopic images. The longer the residence time of undrawn polyester fibers between spinning and drawing, the larger the induced spherulites are and thus the elongation is impaired.

Description

Vynález sa týká spósobu hodnotenia starnutia polyesterov, najmS nedlžných polyesterových vláken a fólií.The invention relates to a method for assessing the aging of polyesters, in particular non-elongated polyester fibers and films.

V procese přípravy polyesterových technických vláken klasickým - diskontinuálnym postupom medzi vzlákňovaním a dlžením zotrvávajú vlákna v nedlženom stave určitý čas daný technologickým postupom, čo móže vplývať na změny neiktorých štruktúrnych parametrov, a tým ovplyvniť proces díženia.In the process of preparing polyester technical fibers by the classical - discontinuous process between spinning and drawing, the fibers remain in the undrawn state for some time due to the technological process, which may affect changes in some structural parameters and thus affect the process of yielding.

Hodnotenie vplyvu doby zotrvania medzi zvlákňovaním a dlžením týchto vláken na změny štruktúrnych parametrov sa robí využitím fyzikálnych metod.The assessment of the impact of residence time between spinning and drawing of these fibers on changes in structural parameters is made using physical methods.

V literatúre nie sú vóbec známe práce so zameraním na hodnotenie starnutia polyesterov, najma však polyesterových vláken metodou indukovanej kryštalizácie chloroformom.There is no known work in the literature to assess the aging of polyesters, but especially polyester fibers by induced chloroform crystallization.

Podstata hodnotenia starnutia polyesterov najmS polyesterových vláken a fólií podlá tohoto vynálezu spočívá vo vyvolaní sférolitov v polymére pósobením chloformu na polymér po dobu minimálně 5 minút a v meraní velkosti takto vyvolaných sférolitov pomocou elektronomikroskopických obrázkov.The principle of evaluating the aging of the polyesters, in particular the polyester fibers and films of the present invention, consists in inducing spherulites in the polymer by treating the polymer with chloroform for at least 5 minutes and measuring the size of the spherulites thus induced by electronomicroscopic images.

Výsledky fyzikálnych metod hodnotenia vplyvu doby zotrvania nedlžených vláken medzi zvlákňovaním a dlžením vykazujú malé změny hodnót štruktúrnych parametrov (stupeň kryštalinity, orientácie, štruktúrna modifikácia a pod.). Výhoda navrhovaného spósobu hodnotenia starnutia nedlžených vláken spočívá v zaznamenaní podstatnej změny velkosti morfologických útvarov - sférolitov, a vysvětlení příčin zhoršenej dlžitelnosti vláken vplyvom starnutia.The results of physical methods of assessing the influence of the residence time of undrawn fibers between spinning and drawing show small changes in the values of structural parameters (degree of crystallinity, orientation, structural modification, etc.). The advantage of the proposed method of assessing the aging of undrawn fibers lies in recording a significant change in the size of the morphological formations - spherulites, and in explaining the causes of the deteriorated fiber elongation due to aging.

Příklad 1Example 1

Nedlžené polyetyléntereftalátové vlákna, zvláknené pri teplote 295 °C a navíjané rýchlosťou 500 m/min. s logaritmickým viskozitným číslom polyméru 95 ml/g, boli uložené v klimatizovaných podmienkach pri teplote 22 °C a relatívnej vlhkosti 65 % po dobu 30 dní.Unstretched polyethylene terephthalate fibers, spun at 295 ° C and wound at a speed of 500 m / min. with a logarithmic viscosity of the polymer of 95 ml / g, were stored in air-conditioned conditions at 22 ° C and 65% relative humidity for 30 days.

V určitých časových intervaloch, ako je uvedené v tabulke, boli odoberané vzorky vláken a hodnotené změny velkosti sférolitov spósobené stárnutím. Na vyvolanie sekundárnej kryštalizácie boli vzorky nedlžených vláken ponořené do chloroformu po dobu 5 minút. Změny velkosti sférolitov s dobou uloženia nedlžených vláken a vplyv na dlžitelnosť sú uvedené v tabulke:At certain time intervals, as shown in the table, fiber samples were taken and the size changes of the spherulites were evaluated due to aging. To induce secondary crystallization, samples of undrawn fibers were immersed in chloroform for 5 minutes. The changes in the size of the spherulites with the length of storage of the undrawn fibers and the influence on the elongation are given in the table:

Tabulkatable

Vzorka čísloSample number

Doba skladovania (h)Shelf life (h)

Velkosť sférolitov d (^m)Size of spherulites d (^ m)

Prírastok Dlžitelnosť d (%)Increment Diligence d (%)

1 1 1 1 2,6 2.6 - - dobrá good 2 2 96 96 3,7 3.7 42 42 dobrá good 3 3 720 720 5,0 5.0 92 92 zhoršená impaired

Vyhodnotenie: Dlženie polyesterových vláken v priebehu zotrvania po zvlákňovaní do hodin prebiehalo bez ťažkostí. Po uplynutí 30 dní medzi zvlákňovaním a dlžením dochádzalo hlavně na začiatku dlženia k pretrhávaniu kapilár, pričom boli zaznamenané i pretrhy. Tento nedostatok súvisí so zváčšením kryštalických zoskupení v polymérnom systéme medzi zvlákňovaním a dlžením, v čom je aj póvod váčších rozmerov sekundárné vykrystalizovaných sférolitov. Zhodným postupom sa pósobilo na vlákna chloroformom po dobu 15 a 20 minút a získali sa rovnaké hodnoty, čo značí, že doba pósobenia neovplyvňuje velkosť sférolitov. Pri pósobení chloroformu len 3 minuty sférolity neboli dobré vyvinuté.Evaluation: The elongation of the polyester fibers during the retention time after spinning to hours proceeded without difficulty. After 30 days between spinning and owing, capillaries ruptured mainly at the beginning of owing, and breaks were also noted. This drawback is related to an increase in crystalline groupings in the polymer system between spinning and drawing, which also has the origin of larger dimensions of secondary crystallized spherulites. By the same procedure, the fibers were treated with chloroform for 15 and 20 minutes and the same values were obtained, indicating that the duration of exposure did not affect the size of the spherulites. Only 3 minutes of spherulites were not well developed when chloroform was applied.

Příklad 2Example 2

Boli použité komerčně vyrábané polyesterové fólie o hrúbke 30 jim, 60 yrn a 100 yim.Commercially produced polyester films having a thickness of 30 µm, 60 µm and 100 µm were used.

Na vyvolanie sekundárnej kryštalizácie bol použitý postup uvedený v příklade 1 s tým rozdielom, že na fólie sa pósobilo chloroformom 10 minút.The procedure described in Example 1 was used to induce secondary crystallization except that the films were treated with chloroform for 10 minutes.

Změny velkosti sférolitov v závislosti na hrúbke použitých fólií sú uvedené v tabulke:The changes in the size of the spherulites depending on the thickness of the foils used are given in the table:

Tabulkatable

Vzorka číslo sample number Hrúbka fólie (/im) Foil thickness (/ im) Velkost sférolitov d (yim) Size of spherulites d (yim) 1 1 30 30 5,1 5.1 2 2 60 60 4,9 4.9 3 3 100 100 5,2 5.2

Vyhodnotenie: Velkost sférolitov vyvolaných sekundárnou kryštalizáciou chloroformom nie je závislá na hrúbke fólií.Evaluation: The size of the spherulites induced by secondary crystallization with chloroform is not dependent on the film thickness.

Claims (1)

3 265342 Bolí použité komerčně vyrábané polyesterové fólie o hrúbke 30 ρνλ, 60 a 100 yim. Na vyvolanie sekundárnej kryštalizácie bol použitý postup uvedený v příklade 1 s tým roz- dielom, že na fólie sa pósobilo chloroformom 10 minut. Změny velkosti sférolitov v závislosti na hrúbke použitých fólii sú uvedené v tabulke: Tabulka Příklad 2 Vzorka číslo Hrúbka fólie Velkost sférolitovd (yim) 1 30 5,1 2 60 4,9 3 100 5,2 Vyhodnotenie: Velkost sférolitov vyvolaných sekundárnou kryštalizáciou chloroformomnie je závislá na hrúbke fólií. PREDMET VYNÁLEZU Spósob hodnotenia starnutia polyesterov, najma nedlžených polyesterových vláken afólií metodou indukovanej kryštalizácie vyznačujúci sa tým, že sférolity sa v polymerevyvolájú pósobením chloroformu po dobu viac ako 3 minúty, a ich velkost sa stanoví pomocouelektrónovej mikroskopie.Commercially manufactured polyester films having a thickness of 30 µm, 60 and 100 µm were used. To induce secondary crystallization, the procedure described in Example 1 was used, except that the films were treated with chloroform for 10 minutes. Changes in spherulite size depending on the thickness of the film used are given in the table: Table Example 2 Sample number Film thickness Thickness spherulite 1 (yim) 1 30 5.1 2 60 4.9 3 100 5.2 Evaluation: The size of spherulites induced by secondary crystallization of chloroform is dependent on the film thickness. DISCLOSURE OF THE INVENTION A method for assessing the aging of polyesters, in particular non-long-fiber polyester fibers by induced crystallization, characterized in that spherulites are selected in the polymer by the action of chloroform for more than 3 minutes, and their size determined by electron microscopy.
CS88397A 1988-01-21 1988-01-21 A way of evaluating the aging of polyesters, especially overweight CS265342B1 (en)

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