CN102586933B - Method for preparing polyester staple fibers by using waste polyester raw material - Google Patents
Method for preparing polyester staple fibers by using waste polyester raw material Download PDFInfo
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- CN102586933B CN102586933B CN201210007046.7A CN201210007046A CN102586933B CN 102586933 B CN102586933 B CN 102586933B CN 201210007046 A CN201210007046 A CN 201210007046A CN 102586933 B CN102586933 B CN 102586933B
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- 229920000728 polyester Polymers 0.000 title claims abstract description 109
- 239000002699 waste material Substances 0.000 title claims abstract description 59
- 239000000835 fiber Substances 0.000 title claims abstract description 33
- 239000002994 raw material Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000009987 spinning Methods 0.000 claims abstract description 32
- 239000008188 pellet Substances 0.000 claims abstract description 19
- 239000004970 Chain extender Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 7
- UHQZGWJEFFDHSR-UHFFFAOYSA-N 1-(2-oxoazepane-1-carbonyl)azepan-2-one Chemical compound C1CCCCC(=O)N1C(=O)N1CCCCCC1=O UHQZGWJEFFDHSR-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000000155 melt Substances 0.000 claims abstract 2
- 239000004753 textile Substances 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 5
- 238000007259 addition reaction Methods 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000012545 processing Methods 0.000 abstract description 9
- 239000008187 granular material Substances 0.000 abstract description 8
- 239000004744 fabric Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 239000004746 geotextile Substances 0.000 abstract description 2
- 239000011810 insulating material Substances 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- 239000004745 nonwoven fabric Substances 0.000 abstract 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 14
- 229920004933 Terylene® Polymers 0.000 description 13
- 238000004140 cleaning Methods 0.000 description 6
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 6
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000036760 body temperature Effects 0.000 description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 description 3
- 239000001488 sodium phosphate Substances 0.000 description 3
- 239000000271 synthetic detergent Substances 0.000 description 3
- 239000013638 trimer Substances 0.000 description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- -1 or shoe cover Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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Abstract
本发明公开了一种利用废旧聚酯原料制备涤纶短纤维的方法。将废旧聚酯进行清洗、干燥和压缩团粒造粒后，经过干燥后输送入反应型排气式螺杆挤出机，按粒料质量的0.5-3%加入苯基二噁唑啉和N,N'-羰基双己内酰胺聚酯扩链剂，将聚酯粒料和扩链剂一起输送至反应型排气式螺杆挤出机，熔融、混炼后将熔体计量输送至纺丝单元，制备涤纶短纤维。本发明可以改善废旧聚酯在加工和使用过程中的降解，提高废旧聚酯分子量，改善涤纶纤维的加工效率和纤维质量。本发明制备的涤纶纤维可用于服装或家具织物的充填料以及用作土工布、屋顶毡基布和绝缘材料的非织造布，或鞋套、揩布以及一些用即弃的非织造产品。The invention discloses a method for preparing polyester staple fiber by using waste polyester raw materials. Washing, drying and compressing the waste polyester into granules, then transporting them into the reactive exhaust type screw extruder after drying, adding phenyl bisoxazoline and N,N '-Carbonyl biscaprolactam polyester chain extender, the polyester pellets and the chain extender are conveyed to the reactive vented screw extruder, melted and mixed, and then the melt is metered and conveyed to the spinning unit to prepare polyester short fibre. The invention can improve the degradation of waste polyester during processing and use, increase the molecular weight of waste polyester, and improve the processing efficiency and fiber quality of polyester fiber. The polyester fiber prepared by the present invention can be used as filling materials for clothing or furniture fabrics, as nonwoven fabrics for geotextiles, roof felt base fabrics and insulating materials, or shoe covers, wipers and some disposable nonwoven products.
Description
Technical field
The present invention relates to a kind of method of preparing polyester staple fiber, especially relate to a kind of method of utilizing waste and old polyester raw material to prepare polyester staple fiber.
Background technology
Thermoplastic polyester comprises the principal items such as fibre-grade, bottle level and film level polyester by purposes.China in a 2010 only demand for fibre-grade and bottle level polyester has just exceeded 2,300 ten thousand tons, and keeps certain growth rate, and in particular for the wrapping bottle of sheet polyester such as packaging for foodstuff and medicine, daily use chemicals, annual growth has exceeded 15%.When PET industry fast development, also bring the problem that cannot avoid to the whole world: raw material sources and waste disposal.In polyester fiber processing, there is approximately 2% waste material, the discarded object after fibre uses, and nonrecoverable food has produced a large amount of waste and old polyester raw materials by packaging polyesters.
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), be recycled as master mainly with the physics of melting reprocessing at present, the existing multiple applications of China and granted patent relate to the recycling of waste and old polyester (polyester bottles and polyester waste silks).Waste and old terylene textiles after waste silk in polyester bottles, terylene spinning in thermoplastic polyester and part are used, 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, set forth utilizing waste and old polyester bottle and Polyester Textiles to carry out spinning again.
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 staple fiber, the waste silk that utilizes waste and old terylene textiles and terylene spinning processing to produce, improve method waste and old and recovery molecular weight of polyesters by liquid phase, utilize the method to prepare Regenerated Polyester Staple Fiber dimension.
The step of the technical solution used in the present invention is as follows:
(1) raw material preparation: waste and old polyester raw material is cleaned to remove spot and finish, by clean after waste and old polyester raw material stoving to moisture content lower than 0.1%, then dried waste and old polyester raw material is prepared to spherical pellet at 235 ℃ of semi-molten state lower compression granules;
(2) melt preparation and spinning: spherical pellet 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 add polyester chain extender by 0.5～3% of pellet mass, polyester granules 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 polyster fibre, 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 granules, and the N of terminal hydroxyl generation addition reaction in energy and polyester granules, 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 silk or the waste pure polyester textiles producing in waste and old terylene textiles, terylene spinning process.
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 mode such as injection moulding or section bar extrusion.
The prepared polyster fibre of the present invention can be for the casting resin of clothes or furniture fabric and as the non-weaving cloth of geotextiles, roof felt and insulating materials, or shoe cover, cloth for wiping or dusting and some are used disposable nonwoven products.
The specific embodiment
Illustrate below in conjunction with embodiment how the present invention specifically implements.
Embodiment 1:
Waste and old polyester raw material used is waste pure polyester textiles (inherent viscosity 0.5g/dl).Adopt following process conditions to carry out the preparation of regenerated polyester fiber:
(1) raw material preparation: waste and old terylene textiles is cleaned to remove spot, and cleaning condition is: synthetic detergent 5g/l, sodium phosphate trimer 5g/l, sheet alkali 0.8g/l, 90 ℃ of temperature.Waste and old terylene textiles after cleaning is dried to 5h in airflow dryer, after moisture content is down to 0.1%, waste and old polyester raw material is prepared to a spherical pellet with a machine compression under 235 ℃ of semi-molten state.
(2) melt preparation and spinning: pellet prepared by step (1) is delivered in drying device dry 30min at 120 ℃, then dry 6h at 140 ℃, after dry, moisture content is 30ppm, then adding mol ratio by 0.5% of pellet mass is 1 of 1:1, 4-Ben Ji bisoxazoline (1, 4-PBO) and N, N' ?two caprolactam (CBC) polyester chain extenders of carbonyl, polyester granules is delivered to together with chain extender to response type exhaust screw extruder, screw diameter D is 65mm, screw slenderness ratio L/D is 30, and 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 245 ℃, 260 ℃, 280 ℃, 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 25 μ m, 285 ℃ of spinning body temperatures, spinnerets hole count 1200, spinneret orifice diameter 0.3mm, spinneret orifice draw ratio 1.0,30 ℃ of cooling air temperature, humidity 65%, wind speed 4m/min, spinning speed 1000m/min.Cooled spun filament through oiling, the conventional polyester spinning process such as coiling, boundling, stretching, curling and cut-out, preparing fiber number is 3D, the cotton type regenerated polyester fiber that length is 38mm.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.
Embodiment 2:
Waste and old polyester raw material used is the waste silk (inherent viscosity 0.6g/dl) producing in terylene spinning process.Adopt following process conditions to carry out the preparation of regenerated polyester fiber:
(1) raw material preparation: waste and old terylene textiles is cleaned to remove spot, and cleaning condition is: synthetic detergent 5g/l, sodium phosphate trimer 5g/l, sheet alkali 0.8g/l, 90 ℃ of temperature.Waste and old terylene textiles after cleaning is dried to 5h in airflow dryer, after moisture content is down to 0.1%, waste and old polyester raw material is prepared to a spherical pellet with a machine compression under 235 ℃ of semi-molten state.
(2) melt preparation and spinning: pellet prepared by step (1) is delivered in drying device dry 10min at 140 ℃, then dry 3h at 170 ℃, moisture content 40ppm after dry, then adds Isosorbide-5-Nitrae-Ben Ji bisoxazoline (1 by 3% of pellet mass, 4-PBO) polyester chain extender, polyester granules 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 260oC, 275 ℃, 285 ℃, 290 ℃, 290 ℃, melting, after mixing, melt-stoichiometry is delivered to spinning unit, 285 ℃ of conveyance conduit temperature, spinning unit major parameter is: fondant filter filtering accuracy 25 μ m, 290 ℃ of spinning body temperatures, spinnerets hole count 900, spinneret orifice diameter 0.2mm, spinneret orifice draw ratio 1.5,30 ℃ of cooling air temperature, humidity 65%, wind speed 3m/min, spinning speed 900m/min.Cooled spun filament through oiling, the conventional polyester spinning process such as coiling, boundling, stretching, curling and cut-out, preparing fiber number is 1.5D, the cotton type regenerated polyester fiber that length is 40mm.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 pure polyester textiles (inherent viscosity 0.52g/dl).Adopt following process conditions to carry out the preparation of regenerated polyester fiber:
(1) raw material preparation: waste and old terylene textiles is cleaned to remove spot, and cleaning condition is: synthetic detergent 5g/l, sodium phosphate trimer 5g/l, sheet alkali 0.8g/l, 90 ℃ of temperature.Waste and old terylene textiles after cleaning is dried to 5h in airflow dryer, after moisture content is down to 0.1%, waste and old polyester raw material is prepared to a spherical pellet with a machine compression under 235 ℃ of semi-molten state.
(2) melt preparation and spinning: pellet prepared by step (1) is delivered in drying device dry 20min at 130 ℃, then dry 4h at 160 ℃, after dry, moisture content is 45ppm, then add N by 2.5% of pellet mass, N' ?two caprolactam (CBC) polyester chain extenders of carbonyl, polyester granules 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, and 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 245 ℃, 255 ℃, 270 ℃, 275 ℃, 275 ℃, melting, after mixing, melt-stoichiometry is delivered to spinning unit, 280 ℃ of conveyance conduit temperature, spinning unit major parameter is: fondant filter filtering accuracy 25 μ m, 280 ℃ of spinning body temperatures, spinnerets hole count 1200, spinneret orifice diameter 0.45mm, spinneret orifice draw ratio 2.0,40 ℃ of cooling air temperature, humidity 65%, wind speed 4m/min, spinning speed 800m/min.Cooled spun filament through oiling, the conventional polyester spinning process such as coiling, boundling, stretching, curling and cut-out, preparing fiber number is 3D, the cotton type regenerated polyester fiber that length is 45mm.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 6min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210007046.7A CN102586933B (en) | 2012-01-11 | 2012-01-11 | Method for preparing polyester staple fibers by using waste polyester raw material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210007046.7A CN102586933B (en) | 2012-01-11 | 2012-01-11 | Method for preparing polyester staple fibers by using waste polyester raw material |
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| CN102586933A CN102586933A (en) | 2012-07-18 |
| CN102586933B true CN102586933B (en) | 2014-06-18 |
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| JP平4-24215A 1992.01.28 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2728780C2 (en) * | 2015-09-21 | 2020-07-31 | Колорматрикс Холдингс, Инк. | Polymer materials |
| WO2025031553A1 (en) * | 2023-08-09 | 2025-02-13 | Hamza Pakinam Mounir Elsayed Fahmy | Method of recycling polyethylene terephthalate (pet) consumed bottles by extrusion spinning |
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| CN102586933A (en) | 2012-07-18 |
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