CN102605456B - Method for preparing polyester filament yarns by using waste polyester raw materials - Google Patents

Method for preparing polyester filament yarns by using waste polyester raw materials Download PDF

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CN102605456B
CN102605456B CN201210006794.3A CN201210006794A CN102605456B CN 102605456 B CN102605456 B CN 102605456B CN 201210006794 A CN201210006794 A CN 201210006794A CN 102605456 B CN102605456 B CN 102605456B
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polyester
waste
old
bottle
raw material
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CN102605456A (en
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朱海霖
张华鹏
陈建勇
唐红艳
郭玉海
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Cai Linmiao
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Zhejiang Sci Tech University ZSTU
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Abstract

The invention discloses a method for preparing polyester filament yarns by using waste polyester raw materials. The method comprises the following steps of: sorting, washing, crushing and drying waste polyester bottle flakes; conveying the dried waste polyester bottle flakes into a reaction type exhaust screw extruder; adding phenyl dioxazoline and N, N'-carbonyl biscaprolactam) polyester chain extender which is 0.5-3% of the mass of the polyester bottle flakes; conveying the polyester bottle flakes and the polyester chain extender into the reaction type exhaust screw extruder; fusing and mixing, and metering a smelted body and conveying the smelted body to a yarn spinning unit to prepare the polyester filament yarns. According to the method disclosed by the invention, the degradation of waste polyester in a machining and using process can be improved, the molecular weight of the waste polyester is improved, and the machining efficiency and the filament yarn quality of the polyester filament yarns are improved. The polyester filament yarns prepared by the invention can be used for the FDY (Fully Drawn Yarn) filament yarns of clothes, household textiles and some high-quality industry textiles.

Description

A kind of method of utilizing waste and old polyester raw material to prepare polyester filament
Technical field
The present invention relates to a kind of method of preparing polyester filament, especially relate to a kind of method of utilizing waste and old polyester raw material to prepare polyester filament.
Background technology
Thermoplastic polyester comprises the principal items such as fibre-grade, bottle level and film level polyester by purposes.China in 2010 the only demand of bottle level polyester has just exceeded 3,600,000 tons, and in particular for polyester such as wrapping bottle level such as food, beverage packaging and medicine, daily use chemicals etc., annual growth has exceeded 15%.In the time of PET industry fast development, also to the whole world, brought the problem that cannot avoid: raw material sources and waste disposal.
From the eighties, countries in the world are to problem pay attention to day by days such as the energy, resource and environmental protection, and the recycling of waste and old polyester causes people's great attention, and play just to begin one's study how to recycle waste and old polyester the external sixties.Due to chemical recovery utilization (depolymerization of polyester) complex process (as described in application number China's patent that is 200810123544.1), mainly with the physics of melting reprocessing, be recycled as master at present, the existing multiple applications of China and granted patent relate to the recycling of waste and old polyester.Polyester bottles in thermoplastic polyester is under suitable recovery and utilization technology and technique, all can adopt physical method again to recycle, if application number is in China's patent of 201110176957.8,200610152509.3,201010300670.7 and 200910020159.9, to utilizing waste and old polyester bottle and Polyester Textiles to carry out spinning again, set forth.
Polyester, in processing, use and removal process, under the effect of heat and moisture, inevitably causes the degraded in various degree of polyester, thereby causes the reduction of molecular weight of polyesters.How, for different waste and old polyester raw materials, rationally effectively controlling the molecular weight of polyester, improve working (machining) efficiency and the quality of regenerated fiber, is one of key problem in technology of waste and old, recovery at present and recycled polyester processing polyster fibre (long filament and short fiber).For avoiding the reduction of molecular weight in polyester processing and use procedure, mostly adopt solid phase polycondensation or the reclaimed materials mode mixed with virgin material, in the processing time that the former need to be longer, working (machining) efficiency is lower, and the latter needs higher virgin material ratio, and reclaimed materials utilization rate is not high.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing waste and old polyester raw material to prepare polyester filament, is to utilize waste and old polyester bottle to prepare polyester filament.Prepared polyester filament can be for clothes, household textiles and some high-grade technical textile FDY long filament.
The step of the technical solution used in the present invention is as follows:
(1) raw material preparation: described waste and old polyester raw material is sorted, cleans, pulverized and is dried, obtain moisture content lower than 0.1%, after pulverizing, girth is less than 20mm, and maximal side is less than the returnable bottle sheet of 8mm;
(2) melt preparation and spinning: returnable bottle sheet prepared by step (1) is delivered in drying device dry 10-30min at 120-140 ℃, dry 3-6h at 140-170 ℃, after dry, moisture content is lower than 50ppm, then by the 0.5-3% of polyester bottle slice quality, add polyester chain extender, polyester bottle slice is delivered to together with polyester chain extender to response type exhaust screw extruder, melting, melt-stoichiometry is delivered to spinning unit after mixing, prepare polyester filament, whole melt residence time is 3~10min.
Polyester chain extender described in step (2) is the Ben Ji bisoxazoline of terminal carboxyl group generation addition reaction in energy and polyester bottle slice, and the N of terminal hydroxyl generation addition reaction in energy and polyester bottle slice, N' ?the two caprolactams of carbonyl, the molar ratio of the two is 0~1:1~0.
Described waste and old polyester raw material is waste and old polyester bottle.
The beneficial effect that the present invention has is:
(1) by the adding of polyester chain extender, effectively improve the molecular weight of waste and old polyester, improved the working (machining) efficiency of waste and old polyester spinning and the quality of regenerated polyester fiber;
(2) can there is not being cross-linked between polyester molecule in the polyester chain extender adopting, avoided spinning melt generation gelatin phenomenon, guaranteed the necessary strand linearity of spinning melt;
(3) the method not only can be applied to the preparation of regenerated polyester fiber, can also be applied to other waste and old polyesters and recycle in technologies, as by the processing regenerated polyester plastics goods of the modes such as injection moulding or section bar extrusion.
The prepared polyester filament of the present invention can be for clothes, household textiles and some high-grade technical textile FDY long filament.
The specific embodiment
Below in conjunction with embodiment, illustrate how the present invention specifically implements.
Embodiment 1:
Waste and old polyester raw material used is waste and old polyester Coke bottle (inherent viscosity 0.58g/dl).Adopt following process conditions to carry out the preparation of regenerated terylene long filament:
(1) raw material preparation: waste and old polyester bottle is tentatively sorted by color, then clean to remove spot, cleaning condition is: synthetic detergent 3g/l, sodium phosphate trimer 4g/l, sheet alkali 0.8g/l, 90 ℃ of temperature, remove the non-polyester compositions such as polyester bottles label, bottle cap.Then adopt disintegrating machine that the polyester bottles after cleaning is pulverized as girth is less than 20mm, maximum limit is less than the returnable bottle sheet of 8mm, finally the waste and old polyester bottle sheet after pulverizing is dried to 5h in airflow dryer, makes moisture content be down to 0.1%.
(2) melt preparation and spinning: polyester bottle slice prepared by step (1) is delivered in drying device dry 30min at 120 ℃, then dry 6h at 140 ℃, after dry, moisture content is 25ppm, then by 0.5% of polyester bottle slice quality, adding mol ratio is 1 of 1:1, 4-Ben Ji bisoxazoline (1, 4-PBO) and N, N' ?the two caprolactams of carbonyl, (CBC) polyester chain extender, polyester bottle slice is delivered to together with chain extender to response type exhaust screw extruder, screw diameter D is 65mm, and screw slenderness ratio L/D is 30, screw rod has five functional sections, comprises feeding section, melt zone, vacuum exhaust section (vacuum 0.2-0.3MPa), homogenize section and metering section, each section length is 6D, 9D, 3D, 6D, 6D, temperature is 235 ℃, 260 ℃, 265 ℃, 270 ℃, 270 ℃, melting, after mixing, melt-stoichiometry is delivered to spinning unit, 275 ℃ of conveyance conduit temperature, spinning unit major parameter is: fondant filter filtering accuracy 25 μ m, 275 ℃ of spinning body temperatures, spinnerets hole count 48, spinneret orifice diameter 0.2mm, spinneret orifice draw ratio 1.5,30 ℃ of cooling air temperature, humidity 65%, wind speed 4m/min, spinning speed 2500m/min.Cooled spun filament through oiling, the conventional polyester spinning process such as coiling, drawing-off, prepare the POY long filament of 200D/48F.This POY, through DTY deformation technique, prepares the DTY long filament of 150D/48F.For guaranteeing good chain extension effect, whole melt residence time (melt process screw rod melt zone is to the time of leaving spinneret orifice) is 3min.
Figure GDA0000421038540000031
Embodiment 2:
Waste and old polyester raw material used is waste and old polyester water bottle (inherent viscosity 0.75g/dl).Adopt following process conditions to carry out the preparation of regenerated terylene long filament:
(1) raw material preparation: waste and old polyester bottle is tentatively sorted by color, then clean to remove spot, cleaning condition is: synthetic detergent 3g/l, sodium phosphate trimer 4g/l, sheet alkali 0.8g/l, 90 ℃ of temperature, remove the non-polyester compositions such as polyester bottles label, bottle cap.Then adopt disintegrating machine that the polyester bottles after cleaning is pulverized as girth is less than 20mm, maximum limit is less than the returnable bottle sheet of 8mm, finally the waste and old polyester bottle sheet after pulverizing is dried to 4h in airflow dryer, makes moisture content be down to 0.05%.
(2) melt preparation and spinning: polyester bottle slice prepared by step (1) is delivered in drying device dry 10min at 140 ℃, then dry 3h at 170 ℃, moisture content 40ppm after dry, then by 1.5% of polyester bottle slice quality, adding mol ratio is 1 of 1:1, 4-Ben Ji bisoxazoline (1, 4-PBO) polyester chain extender, polyester bottle slice is delivered to together with chain extender to response type exhaust screw extruder, screw diameter D is 90mm, screw slenderness ratio L/D is 30, screw rod has five functional sections, comprises feeding section, melt zone, vacuum exhaust section (vacuum 0.2-0.3MPa), homogenize section and metering section, each section length is 6D, 9D, 3D, 6D, 6D, temperature is 240 ℃, 265 ℃, 265 ℃, 280 ℃, 280 ℃, melting, after mixing, melt-stoichiometry is delivered to spinning unit, 285 ℃ of conveyance conduit temperature, spinning unit major parameter is: fondant filter filtering accuracy 35 μ m, 285 ℃ of spinning body temperatures, spinnerets hole count 96, spinneret orifice diameter 0.4mm, spinneret orifice draw ratio 2.5,30 ℃ of cooling air temperature, humidity 65%, wind speed 4m/min, spinning speed 3500m/min.Cooled spun filament through oiling, the conventional polyester spinning process such as coiling, drawing-off, prepare the POY long filament of 420D/96F.This POY, through draft process, prepares the FDY long filament of 192D/96F.For guaranteeing good chain extension effect, whole melt residence time (melt process screw rod melt zone is to the time of leaving spinneret orifice) is 10min.
Embodiment 3:
Waste and old polyester raw material used is waste and old polyester water bottle (inherent viscosity 0.68g/dl).Adopt following process conditions to carry out the preparation of regenerated terylene long filament:
(1) raw material preparation: waste and old polyester bottle is tentatively sorted by color, then clean to remove spot, cleaning condition is: synthetic detergent 3g/l, sodium phosphate trimer 4g/l, sheet alkali 0.8g/l, 90 ℃ of temperature, remove the non-polyester compositions such as polyester bottles label, bottle cap.Then adopt disintegrating machine that the polyester bottles after cleaning is pulverized as being less than 20mm, maximum limit is less than the returnable bottle sheet of 8mm, finally the waste and old polyester bottle sheet after pulverizing is dried to 4h in airflow dryer, makes moisture content be down to 0.05%.
(2) melt preparation and spinning: polyester bottle slice prepared by step (1) is delivered in drying device dry 20min at 130 ℃, then dry 5h at 160 ℃, moisture content 45ppm after dry, then by 3% of polyester bottle slice quality, add N, N' ?two caprolactam (CBC) polyester chain extenders of carbonyl, polyester bottle slice is delivered to together with polyester chain extender to response type exhaust screw extruder, screw diameter D is 90mm, screw slenderness ratio L/D is 30, screw rod has five functional sections, comprises feeding section, melt zone, vacuum exhaust section (vacuum 0.2-0.3MPa), homogenize section and metering section, each section length is 6D, 9D, 3D, 6D, 6D, temperature is 240 ℃, 265 ℃, 265 ℃, 280 ℃, 280 ℃, melting, after mixing, melt-stoichiometry is delivered to spinning unit, 285 ℃ of conveyance conduit temperature, spinning unit major parameter is: fondant filter filtering accuracy 30 μ m, 285 ℃ of spinning body temperatures, spinnerets hole count 96, spinneret orifice diameter 0.4mm, spinneret orifice draw ratio 2.5,30 ℃ of cooling air temperature, humidity 65%, wind speed 4m/min, spinning speed 3500m/min.Cooled spun filament through oiling, the conventional polyester spinning process such as coiling, drawing-off, prepare the POY long filament of 420D/96F.This POY, through draft process, prepares the FDY long filament of 192D/96F.For guaranteeing good chain extension effect, whole melt residence time (melt process screw rod melt zone is to the time of leaving spinneret orifice) is 5min.

Claims (2)

1. utilize waste and old polyester raw material to prepare a method for polyester filament, it is characterized in that the step of the method is as follows:
(1) raw material preparation: described waste and old polyester raw material is sorted, cleans, pulverized and is dried, obtain moisture content lower than 0.1%, after pulverizing, girth is less than 20mm, and maximal side is less than the returnable bottle sheet of 8mm;
(2) melt preparation and spinning: returnable bottle sheet prepared by step (1) is delivered in drying device dry 10-30min at 120-140 ℃, dry 3-6h at 140-170 ℃, after dry, moisture content is lower than 50ppm, then by the 0.5-3% of polyester bottle slice quality, add polyester chain extender, polyester bottle slice is delivered to together with polyester chain extender to response type exhaust screw extruder, melting, melt-stoichiometry is delivered to spinning unit after mixing, prepare polyester filament, whole melt residence time is 3~30min;
Polyester chain extender described in step (2) is the Ben Ji bisoxazoline of terminal carboxyl group generation addition reaction in energy and polyester bottle slice, and the N of terminal hydroxyl generation addition reaction in energy and polyester bottle slice, the two caprolactams of N'-carbonyl, the molar ratio of the two is 0~1:1~0.
2. a kind of method of utilizing waste and old polyester raw material to prepare polyester filament according to claim 1, is characterized in that: described waste and old polyester raw material is waste and old polyester bottle.
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CN103882534A (en) * 2012-12-20 2014-06-25 江苏蓝品纤维科技发展有限公司 Production process for utilizing waste bottle chips to produce high-grade core materials for textile use
DE102013107238A1 (en) * 2013-07-09 2015-01-15 L'Air Liquide, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Process for the recovery of epsilon-caprolactam from extract water
CN110205701A (en) * 2019-05-27 2019-09-06 福建师范大学 A kind of high fire-retardance fiber and preparation method thereof using the preparation of waste and old terylene textile fabric

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CN101434689A (en) * 2007-11-13 2009-05-20 北京化工大学 Method for preparing high molecular weight biodegradable polyester by combined chain extension
CN101550608A (en) * 2009-05-01 2009-10-07 洪桂焕 Process for producing polyester spunbonded pre-oriented yarn from waste polyester bottle chips
CN102268744A (en) * 2011-06-28 2011-12-07 中国人民解放军总后勤部军需装备研究所 Device and method for preparing polyester melt from waste pure polyester textiles

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CN101434689A (en) * 2007-11-13 2009-05-20 北京化工大学 Method for preparing high molecular weight biodegradable polyester by combined chain extension
CN101550608A (en) * 2009-05-01 2009-10-07 洪桂焕 Process for producing polyester spunbonded pre-oriented yarn from waste polyester bottle chips
CN102268744A (en) * 2011-06-28 2011-12-07 中国人民解放军总后勤部军需装备研究所 Device and method for preparing polyester melt from waste pure polyester textiles

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