CN104372436B - A kind of quarternary copolymerized ester fiber and preparation method thereof - Google Patents
A kind of quarternary copolymerized ester fiber and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to polyester fiber technical field, for solving current polyester fiber hydrophily and chromatic problem, the present invention proposes a kind of quarternary copolymerized ester fiber and preparation method thereof, a kind of quarternary copolymerized ester fiber is made up of p-phthalic acid (PTA), ethylene glycol, sorbierite, pentaerythrite, auxiliary agent, wherein the mol ratio of ethylene glycol, sorbierite and pentaerythrite is 1: 0.0001～0.005: 0.0001～0.005, the mol ratio of alkyd is 1.1～1.5: 1, and the mass content of auxiliary agent in quarternary copolymerized ester is 0.01～1%. The present invention, on the basis of not radical change polyester characteristic, carries out performance optimization to polyester fiber, and spinnability, hygroscopicity, the dyeability of polyester fiber are significantly improved.
Description
Technical field
The present invention relates to polyester fiber technical field, be specifically related to the quarternary copolymerized ester fiber of a kind of indium addition andPreparation method.
Background technology
Polyester fiber has that intensity is high, wearability good, smooth surface, can thermal finalization, physical and chemical performance is stable etc. excellentPoint, is widely used in dress ornament field. Although polyester fiber production efficiency is higher, and there is more excellenceWearability, but the pursuit of the comfortableness of the cost of the mankind to product and wear is endless. Therefore, enterOne step is improved machinability in polyester fiber spinning process and hygroscopicity, the dyeability of finished fiber ground alwaysThe target that the person of studying carefully lays siege to. But in the hydrophily and dyeability process of modified poly ester, usually to add largeThe modified monomer of amount causes polyester molecule structural deterioration very serious. So in fiber process process, easily go outExisting lousiness, broken end, spinning speed is low, inefficiency, and the physical property of fiber is also poor, common intensityBelow 3.0cN/dtex, can not meet the requirement of large-scale production.
Application number is 201210323342.8 Chinese patent, discloses a kind of melt direct spinning superfine denier porous poorDo not change manufacture method of polyester fiber and products thereof, this Speciality Pet Fiber with terephthalic acid (TPA) (PTA) andEthylene glycol (EG) is raw material, and adds the additives such as pentaerythrite, in order to improve melt rheological characteristic and canThe property spun, obtains melt through polymerisation, is delivered in filament spinning component, finally by spinneret orifice by pipe-line systemEjection, oil and coiling and molding through quench device quenching curing molding, boundling, makes function admirableSuper fine denier porous polyester fiber. But, because the unpromising polyester fiber molecule of pentaerythrite provides unnecessary hydroxylBase, therefore, so fiber hygroscopicity, colouring property raising not obvious after poly-penta tetrol of interpolation still needs introducingA little hydrophilic radicals carry out modification.
Summary of the invention
For solving current polyester fiber hydrophily and chromatic problem, the present invention proposes a kind of quarternary copolymerized esterFiber and preparation method thereof, on the basis of not radical change polyester characteristic, carries out performance optimization to polyester fiber,Spinnability, hygroscopicity, the dyeability of polyester fiber are significantly improved.
The present invention is achieved by the following technical solutions: a kind of quarternary copolymerized ester fiber is by p-phthalic acid(PTA), ethylene glycol, sorbierite, pentaerythrite, auxiliary agent composition, wherein ethylene glycol, sorbierite and season pentaThe mol ratio of tetrol is 1: 0.0001～0.005: 0.0001～0.005, and the mol ratio of alkyd is 1.1～1.5: 1,The mass content of auxiliary agent in quarternary copolymerized ester is 0.01～1%. Wherein, alcohol is by ethylene glycol, sorbierite, season pentaTetrol composition, acid is p-phthalic acid (PTA).
As preferably, the mol ratio of ethylene glycol, sorbierite and pentaerythrite is 1: 0.0001～0.002:0.002～0.004, the mol ratio of alkyd is 1.18～1.23: 1.
The spinning machinability of polyester is relevant with the degree of crystallinity of polyester fiber. In the time of spinning as-spun fibre, bestState is that the degree of crystallinity of fiber is low as much as possible, but keeps again orientation preferably simultaneously, is conducive to posterior drawing.Accordingly, the higher speed of spinning, can increase the fiber degree of orientation and degree of crystallinity. Therefore when POY spinning speed is superWhile crossing 3500m/min, the rapid variation of the processability of fiber. Therefore, want to improve the spinning speed of POYDegree, reduces production costs, and must limit the crystallisation problems of polyester fiber spinning process. By in polyester mistakeIn journey, add crosslinked class monomer and hydrophilic radical, can destroy polyester molecule chain structure, suppress polyester in spinningCrystallization rate in process, is to reduce its degree of crystallinity, and the one that improves POY and FDY spinning speed has efficacious prescriptionsMethod, simultaneously introduce hydrophilic group as hydroxyl also can fundamentally improve polyester fiber hydrophily and can dyeProperty.
Pentaerythrite is that a kind of space structure is the little molecular polylol class of orthopyramid shape, and structural formula is as (I) instituteShow, four hydroxyls are distributed in respectively four angles of orthopyramid, therefore, usually it are used as to the branching of polyesterAgent, obtains the copolyesters with branched structure.
Sorbierite contains six hydroxyls, and space is class zigzag structure, and structural formula is as shown in (II), in polymerizationIn process, add sorbierite, in six hydroxyls, only have minority to participate in reaction and form straight chain or branched structure, major partHydroxyl is present in copolyesters as hydrophilic radical, has improved the dyeability of polyester fiber.
Auxiliary agent is made up of catalyst and stabilizing agent, and wherein, the mass ratio of catalyst and stabilizing agent is 1～5: 1.As preferably, catalyst is selected from antimony glycol; Stabilizing agent is selected from trimethyl phosphate.
The preparation method of described quarternary copolymerized ester fiber is following steps:
(1) making beating: first ethylene glycol, sorbierite, pentaerythrite are mixed, then by mixture and smart terephthaldehydeAcid mixes, then adds auxiliary agent to stir evenly, and is delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is 230 DEG C～250 DEG C,Between pressure 60～550KPa, esterification yield is transported to polycondensation vessel after reaching and being greater than 93.5%;
(3) polycondensation: when polycondensation, condensation temperature is 270～290. DEG C, being evacuated to 20～100MPa, polycondensation is to specialProperty viscosity is 0.65～0.69, obtains quarternary copolymerized ester,
(4) will after quarternary copolymerized ester melting, be spun into quarternary copolymerized ester fiber, then carry out rear processing.
The quarternary copolymerized ester of melting is sent into filter and filter, after metering, enter spinning pack, then willThat the tow of ejection carries out is cooling, oil, and is wound into preoriented yarn, or after deflector roll after drafting forming, reelsBecome drafting silk.
As preferably, the preparation technology of preoriented yarn is 285～295 DEG C of spinning temperatures, spinning speed2700～3600m/min. Preoriented yarn and can be prepared into elastic filament after false twisting.
As preferably, the preparation technology of drafting silk is 285～295 DEG C of spinning temperatures, spinning degree4000～5700m/min, draw ratio 2.6～3.2,70～90 DEG C of roll temperatures, two 115～135 DEG C of roll temperatures.
Compared with prior art, beneficial effect of the present invention is:
(1) the present invention, by indium addition pentaerythrite and sorbierite in normal polyester polymerization process, had both obtained toolThere is the copolyesters of branched structure, improve the spinnability of polyester fiber, introduced again a small amount of hydrophily hydroxyl, fromAnd hydrophily and the dyeability of raising polyester fiber. Spinnability, hydrophily and chromatic raising are simultaneously realized.
(2) the quarternary copolymerized ester fiber of indium addition that the present invention obtains, compared with normal polyester fiber, its POY spinsSilk speed has improved 0～400m/min, and FDY spinning speed has improved 0～200m/min.
(3) the quarternary copolymerized ester fiber of indium addition that the present invention obtains, compared with normal polyester fiber, its look that dyesPoor dark 3～4 grades, measure wicking height is high by 0～15.0.
Detailed description of the invention:
Below in conjunction with embodiment, technical scheme of the present invention and effect are further described. Modification in embodimentThe machinability of polyester fiber is by the maximum spinning speed of POY in spinning process and FDY, and evaluation is disconnectedThe frequency that captacula, roll banding occur obtains; Hygroscopicity is by measuring measure wicking height by standard FZ/T01071-2008Determine (the measure wicking height value of normal polyester is 21.0); Dyeability is measured with normal by standard GB/T250-2008The aberration of rule polyester fiber is determined.
Embodiment 1
(1) making beating: get 744.0g (12mol) ethylene glycol and sorbierite 2.9g (0.016mol), pentaerythrite2.9g (about 0.021mol) dissolves mixing, then its mixture mixed with the PTA of 1660g (10mol),Add catalyst glycol antimony 20g, stabilizing agent trimethyl phosphate 4g, and stir evenly, be delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is controlled at 240 DEG C, pressesPower 100KPa, esterification yield reaches more than 93.5%, is transported to polycondensation vessel;
(3) polycondensation: when polycondensation, condensation temperature is controlled at 280 DEG C, is evacuated to 60MPa, polycondensation is sticky to targetDegree (inherent viscosity 0.66);
(4) the quarternary copolymerized ester of melting is sent into filter and filter, obtain quarternary copolymerized ester fiber, through meteringAfter, enter spinning pack, 289 DEG C of assembly temperatures, then by the tow of ejection carry out cooling, oil, through deflector rollAfter be wound into POY, maximum spinning speed 3600m/min;
Spinning process, without broken end, occurs without roll banding phenomenon, and fiber measure wicking height is 28.7, the painted conventional fibre that comparesDeeply, 3 grades of aberration.
Embodiment 2
(1) making beating: get 744.0g (12mol) ethylene glycol and sorbierite 7.8g (0.048mol), pentaerythrite5.8g (about 0.042mol) dissolves mixing, then its mixture mixed with the PTA of 1660g (10mol),Add catalyst glycol antimony 10g, stabilizing agent trimethyl phosphate 4g, and stir evenly, be delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is controlled at 237 DEG C, pressesPower 100KPa, esterification yield reaches more than 93.5%, is transported to polycondensation vessel;
(3) polycondensation: when polycondensation, condensation temperature is controlled at 270 DEG C, is evacuated to 80MPa, polycondensation is sticky to targetDegree (inherent viscosity 0.65);
(4) the quarternary copolymerized ester of melting is sent into filter and filter, obtain quarternary copolymerized ester fiber, through meteringAfter, enter spinning pack, 289 DEG C of assembly temperatures, then by ejection tow through drafting forming, be wound into FDY,Wherein 2.8 times of draw ratios, 70 DEG C of roll temperatures, two 115 DEG C of roll temperatures, maximum spinning speed 5700m/min.
Spinning process breaks end on a small quantity, and a small amount of roll banding phenomenon occurs, and fiber measure wicking height is 31.1, painted than conventionalFiber is dark, 4 grades of aberration.
Embodiment 3
(1) making beating: get 744.0g (12mol) ethylene glycol and sorbierite 5.8g (0.032mol), pentaerythrite 0.29g(0.021mol), dissolve and mix, then its mixture is mixed with the PTA of 1660g (10mol), addCatalyst glycol antimony 2g, stabilizing agent trimethyl phosphate 0.4g, and stir evenly, be delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is controlled at 239 DEG C, pressesPower 100KPa, esterification yield reaches more than 93.5%, is transported to polycondensation vessel;
(3) polycondensation: when polycondensation, condensation temperature is controlled at 290 DEG C, is evacuated to 40MPa, polycondensation is sticky to targetDegree (inherent viscosity 0.67);
(4) the quarternary copolymerized ester of melting is sent into filter and filter, obtain quarternary copolymerized ester fiber, through meteringAfter, enter spinning pack, 289 DEG C of assembly temperatures, then by the tow of ejection carry out cooling, oil, through deflector rollAfter be wound into POY, maximum spinning speed 3600m/min;
Spinning process, without broken end, occurs without roll banding phenomenon, and fiber measure wicking height is 30.1, the painted conventional fibre that comparesDeeply, 3 grades of aberration.
Embodiment 4
(1) making beating: get 744.0g (12mol) ethylene glycol and sorbierite 0.58g (0.032mol), pentaerythrite0.58g (0.042mol), dissolves and mixes, then its mixture mixed with the PTA of 1328g (8mol),Add catalyst glycol antimony 20g, stabilizing agent trimethyl phosphate 4g, and stir evenly, be delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is controlled at 240 DEG C, pressesPower 100KPa, esterification yield reaches more than 93.5%, is transported to polycondensation vessel;
(3) polycondensation: when polycondensation, condensation temperature is controlled at 280 DEG C, is evacuated to 60MPa, polycondensation is sticky to targetDegree (inherent viscosity 0.67);
(4) the quarternary copolymerized ester of melting is sent into filter and filter, obtain quarternary copolymerized ester fiber, through meteringAfter, enter spinning pack, 291 DEG C of assembly temperatures, then by ejection tow through drafting forming, be wound into FDY,Wherein 2.8 times of draw ratios, 70 DEG C of roll temperatures, two 115 DEG C of roll temperatures, maximum spinning speed 5700m/min.
Spinning process, without broken end, occurs without roll banding phenomenon, and fiber measure wicking height is 35.6, the painted conventional fibre that comparesDeeply, 5 grades of aberration.
Embodiment 5
(1) making beating: get 744.0g (12mol) ethylene glycol and sorbierite 0.29g (0.016mol), pentaerythrite1.45g (0.0107mol) dissolves mixing, then its mixture mixed with the PTA of 1328g (8mol),Add catalyst glycol antimony 0.20g, stabilizing agent trimethyl phosphate 0.14g, and stir evenly, be delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is controlled at 230 DEG C, pressesPower 100KPa, esterification yield reaches more than 93.5%, is transported to polycondensation vessel;
(3) polycondensation: when polycondensation, condensation temperature is controlled at 275 DEG C, is evacuated to 100MPa, and polycondensation is to targetViscosity (inherent viscosity 0.68);
(4) the quarternary copolymerized ester of melting is sent into filter and filter, obtain quarternary copolymerized ester fiber, through meteringAfter, enter spinning pack, 285 DEG C of assembly temperatures, then by the tow of ejection carry out cooling, oil, through deflector rollAfter be wound into POY, maximum spinning speed 3400m/min;
Spinning process breaks end on a small quantity, occurs without roll banding phenomenon, and fiber measure wicking height is 29.1.7, painted than conventionalFiber is dark, 3 grades of aberration.
Embodiment 6
(1) making beating: get 744.0g (12mol) ethylene glycol and sorbierite 0.87g (0.048mol), pentaerythrite0.58g (0.042mol) dissolves mixing, then its mixture mixed with the PTA of 1494g (9mol),Add catalyst glycol antimony 10g, stabilizing agent trimethyl phosphate 4g, and stir evenly, be delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is controlled at 240 DEG C, pressesPower 100KPa, esterification yield reaches more than 93.5%, is transported to polycondensation vessel;
(3) polycondensation: when polycondensation, condensation temperature is controlled at 275 DEG C, is evacuated to 80MPa, polycondensation is sticky to targetDegree (inherent viscosity 0.68);
(4) the quarternary copolymerized ester of melting is sent into filter and filter, obtain quarternary copolymerized ester fiber, through meteringAfter, enter spinning pack, 289 DEG C of assembly temperatures, then by ejection tow through drafting forming, be wound into FDY,Wherein 3.2 times of draw ratios, 90 DEG C of roll temperatures, two 135 DEG C of roll temperatures, maximum spinning speed 5700m/min.
Spinning process breaks end on a small quantity, occurs without roll banding phenomenon, and fiber measure wicking height is 35.9, painted more fine than conventionalDimension is dark, 5 grades of aberration.
Embodiment 7
(1) making beating: get 744.0g (12mol) ethylene glycol and sorbierite 0.29g (0.016mol), pentaerythrite5.8g (0.042mol) dissolves mixing, then its mixture is mixed with the PTA of 1494g (9mol), addsEnter catalyst glycol antimony 2g, stabilizing agent trimethyl phosphate 1.8g, and stir evenly, be delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is controlled at 240 DEG C, pressesPower 100KPa, esterification yield reaches more than 93.5%, is transported to polycondensation vessel;
(3) polycondensation: when polycondensation, condensation temperature is controlled at 270 DEG C, is evacuated to 60MPa, polycondensation is sticky to targetDegree (inherent viscosity 0.69);
(4) the quarternary copolymerized ester of melting is sent into filter and filter, obtain quarternary copolymerized ester fiber, through meteringAfter, enter spinning pack, 288 DEG C of assembly temperatures, then by the tow of ejection carry out cooling, oil, through deflector rollAfter be wound into POY, maximum spinning speed 3500m/min;
Spinning process breaks end on a small quantity, occurs without roll banding phenomenon, and fiber measure wicking height is 34.9, painted more fine than conventionalDimension is dark, 4 grades of aberration.
Embodiment 8
(1) making beating: get 744.0g (12mol) ethylene glycol and sorbierite 8.7g (0.032mol), pentaerythrite0.29g (0.021mol) dissolves mixing, then its mixture mixed with the PTA of 1809g (10.9mol),Add catalyst glycol antimony 2g, stabilizing agent trimethyl phosphate 0.4g, and stir evenly, be delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is controlled at 230 DEG C, pressesPower 100KPa, esterification yield reaches more than 93.5%, is transported to polycondensation vessel;
(3) polycondensation: when polycondensation, condensation temperature is controlled at 285 DEG C, is evacuated to 60MPa, polycondensation is sticky to targetDegree (inherent viscosity 0.69);
(4) the quarternary copolymerized ester of melting is sent into filter and filter, obtain quarternary copolymerized ester fiber, through meteringAfter, enter spinning pack, 292 DEG C of assembly temperatures, then by ejection tow after drafting forming, be wound into FDY,3.2 times of draw ratios, 70 DEG C of roll temperatures, two 120 DEG C of roll temperatures, maximum spinning speed 5700m/min.
Spinning process, without broken end, occurs without roll banding phenomenon, and fiber measure wicking height is 33.8, the painted conventional fibre that comparesDeeply, 4 grades of aberration.
Those of ordinary skill in the field are to be understood that: the foregoing is only specific embodiments of the invention and, be not limited to the present invention, within the spirit and principles in the present invention all, any amendment of making, etc.With replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a quarternary copolymerized ester fiber, it is characterized in that, described quarternary copolymerized ester fiber is made up of p-phthalic acid, ethylene glycol, sorbierite, pentaerythrite, auxiliary agent, wherein the mol ratio of ethylene glycol, sorbierite and pentaerythrite is 1:0.0001 ~ 0.005:0.0001 ~ 0.005, the mol ratio of alkyd is 1.1 ~ 1.5:1, and the mass content of auxiliary agent in quarternary copolymerized ester is 0.01 ~ 1%;
Its preparation method is following steps:
(1) making beating: first ethylene glycol, sorbierite, pentaerythrite are mixed, then mixture is mixed with p-phthalic acid, then add auxiliary agent to stir evenly, be delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is 230 DEG C ~ 250 DEG C, and between pressure 60 ~ 550KPa, esterification yield is transported to polycondensation vessel after reaching and being greater than 93.5%;
(3) polycondensation: when polycondensation, condensation temperature is 270 ~ 290 DEG C, is evacuated to 20 ~ 100MPa, polycondensation to inherent viscosity is 0.65 ~ 0.69, obtains quarternary copolymerized ester,
(4) will after quarternary copolymerized ester melting, be spun into quarternary copolymerized ester fiber, then carry out rear processing.
2. according to the quarternary copolymerized ester fiber of the said one of claim 1, it is characterized in that, alcohol is made up of ethylene glycol, sorbierite, pentaerythrite, and acid is p-phthalic acid.
3. according to the quarternary copolymerized ester fiber of the said one of claim 1, it is characterized in that, auxiliary agent is made up of catalyst and stabilizing agent, and wherein, the mass ratio of catalyst and stabilizing agent is 1 ~ 5:1.
4. according to the quarternary copolymerized ester fiber of the said one of claim 3, it is characterized in that, catalyst is selected from antimony glycol; Stabilizing agent is selected from trimethyl phosphate.
5. a preparation method for the quarternary copolymerized ester fiber as described in any one in claim 1 to 4, is characterized in that, said preparation method is following steps:
(1) making beating: first ethylene glycol, sorbierite, pentaerythrite are mixed, then mixture is mixed with p-phthalic acid, then add auxiliary agent to stir evenly, be delivered to esterifying kettle;
(2) esterification: carry out continuous esterification in esterification (I), (II) still, esterification temperature is 230 DEG C ~ 250 DEG C, and between pressure 60 ~ 550KPa, esterification yield is transported to polycondensation vessel after reaching and being greater than 93.5%;
(3) polycondensation: when polycondensation, condensation temperature is 270 ~ 290 DEG C, is evacuated to 20 ~ 100MPa, polycondensation to inherent viscosity is 0.65 ~ 0.69, obtains quarternary copolymerized ester,
(4) will after quarternary copolymerized ester melting, be spun into quarternary copolymerized ester fiber, then carry out rear processing.
6. the preparation method of quarternary copolymerized ester fiber according to claim 5, it is characterized in that, in step (4), the quarternary copolymerized ester of melting being sent into filter filters, after metering, enter spinning pack, then by the tow of ejection carry out cooling, oil, after deflector roll, be wound into preoriented yarn, or after drafting forming, be wound into drafting silk.
7. the preparation method of quarternary copolymerized ester fiber according to claim 6, is characterized in that, the preparation technology of preoriented yarn is 285 ~ 295 DEG C of spinning temperatures, spinning speed 2700 ~ 3600m/min.
8. the preparation method of quarternary copolymerized ester fiber according to claim 6, is characterized in that, the preparation technology of drafting silk is 285 ~ 295 DEG C of spinning temperatures, spinning speed 4000 ~ 5700m/min, draw ratio 2.6 ~ 3.2,70 ~ 90 DEG C of roll temperatures, two 115 ~ 135 DEG C of roll temperatures.
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| CN103774267A (en) * | 2014-01-26 | 2014-05-07 | 东华大学 | Preparation method of flexible polyhydroxyl polyester fibers |
| CN103789866A (en) * | 2014-01-26 | 2014-05-14 | 东华大学 | Preparation method of polyhydric polyester fiber |
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| CN103774267A (en) * | 2014-01-26 | 2014-05-07 | 东华大学 | Preparation method of flexible polyhydroxyl polyester fibers |
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Effective date of registration: 20200410 Address after: 314000 no.1288, Hongye Road, Xiuzhou District, Jiaxing City, Zhejiang Province Patentee after: Jiaxing Yipeng Chemical Fiber Co., Ltd Address before: 311228 Linjiang hi tech Industrial Park, Hangzhou, Zhejiang, Xiaoshan Patentee before: ZHEJIANG HENGYI HI-TECH MATERIALS Co.,Ltd. |