CN102408555B - Preparation method of anti-ultraviolet antistatic anti-pilling polyester chip - Google Patents
Preparation method of anti-ultraviolet antistatic anti-pilling polyester chip Download PDFInfo
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Abstract
The invention relates to a preparation method of an anti-ultraviolet, antistatic, and anti-pilling polyester chip, which comprises an esterification reaction procedure and a polymerization reaction procedure; the esterification reaction procedure comprises a primary esterification reaction phase and a secondary esterification reaction phase, and flexible polyethylene glycol is introduced into the secondary esterification reaction phase as a third monomer; after the esterification is completed, a hindered amine light stabilizer and a hindered phenol antioxidant, which are respectively blended with solvents of acetic acid and glycol, as well as hydroxyl silicone oil are added; after the prepolymerization of the polymerization reaction procedure is finished and before the final polymerization, an ultraviolet absorbent and an antistatic agent are added. Polyester fibers spun by the polyester chip obtained by the method of the invention have excellent anti-ultraviolet, antistatic, and anti-pilling effect; when the polyester fibers are woven into knitted fabrics and woven fabrics, related technical indexes obtained by testing are that: the ultraviolet transmittance is not more than 5.0%; the anti-pilling performance is not less than grade 4; and the fiber volume specific resistance is not more than 10*1010 omega.cm.
Description
Technical field
The present invention relates to the preparation method of a kind of uvioresistant, the section of antistatic, anti-pilling polyester.
Background technology
Since the autopolyester fiber comes out, rely on its good intensity, good wrinkle resistance, draping property and wash and wear performance and be widely used in apparel textile, through the tremendous development of nearly decades, the PET trevira has become at present the synthesizing polyester kind that output is maximum in the world, range of application is the widest.But it is compared and also exist many deficiencies with various natural fibers: feel is hardened, water absorbability is poor, anti-ultraviolet property is poor, easily produce static, easily balling-up, be difficult to dyeing etc.Although natural fiber has ventilation property as cotton, real silk, hair, fiber crops etc. have good dyeing behavior, fabric, the absorbing sweat performance of keeping humidity is good, without static, characteristics that comfortableness is good, exist and easily wrinkle, lead the deficiencies such as wet and rapid-drying properties is poor.
Along with the progressively expansion of trevira range of application, from the seventies in last century, developed country is for the above-mentioned deficiency of trevira, the plurality of advantages of natural fiber of take is target, aspect the wearing comfort of fiber, from three aspects, improve the wear behavior of trevira.On the one hand: by the innovation of spinning technique technology, produce various differential fibre, progressively develop thin dawn, superfine Denier fibre spining technology, produce a series of differential spinning kinds such as sea-island fibre, tangerine lobe fiber, bicomponent composite fibre, modified cross-section fibre by composite spinning technology, make polyester fabric obtain rapid progress in function aspects such as flexibility, elasticity, Silks; On the other hand: by the co-blended spinning of different components, in the physical blending mode, produce the various fiber species with specific function, by the rear arrangement of fabric, also can give the function that fabric is brand-new; The third aspect: by copolyreaction, improve this body structure of polyester macromolecule chain, by introducing the copolymerization component group can improve the trevira fabric performance, permanently give fiber various properties.At present, comprise a series of functional polyalkylene ester fibers such as fire-retardant, cation-dyeable, high contraction, disperse dyeable, antistatic, uvioresistant, far infrared thermal insulation, trevira and fabric are segmented market and produced material impact.
The rapid progress of the chemical fibre market of China through reforming and opening up to the outside world in decades, in 68% level that has reached Gross World Product aspect the normal polyester fiber production, but the development and application field at the functional polyalkylene ester fiber, China is at present also in the starting stage, be limited at present the exploitation of single functional polyester and fiber more, as anti-ultraviolet polyester fiber, anti-static polyester fiber etc.And, for the exploitation with complex function, high added value functional fiber, also need the scientific research personnel badly and make a breakthrough in the multifunctional composite fiber field.
The Chinese invention patent that notification number is CN1204196C discloses a kind of uvioresistant zinc oxide complex polyester and preparation method thereof, at first the method prepares the suspension of anti ultraviolet agent intermediate zinc subcarbonate ethylene glycol, then after at the PET polyester, synthetic esterification stage finishes, before the rough vacuum polymerization, the suspension of anti ultraviolet agent intermediate zinc subcarbonate ethylene glycol is added, when polyreaction generates polyester, zinc subcarbonate decomposes generation zinc oxide, obtain uvioresistant zinc oxide complex polyester, wherein zinc oxide content is 0.1%～5% of polyester slice weight.In the method gained polyester, zinc oxide can keep less granularity, thereby absorb ultraviolet performance, strengthens.Yet, the method is in order to decompose zinc carbonate, must make to be aggregated in more than 285 ℃ and carry out, and zinc subcarbonate will resolve into carbonic acid gas, water and zinc oxide, and in whole collecting process, carbonic acid gas can affect vacuum tightness and cause section to contain a large amount of bubbles on the one hand, polycondensation final stage on the other hand, produces large quantity of moisture can produce DeR, have a strong impact on quality product, simultaneously, the zinc subcarbonate do not decomposed fully will continue to decompose in spinning process, the fiber spinnability variation, and breaking tenacity reduces.
The Chinese invention patent application that publication number is CN101864067A discloses a kind of preparation method with polyester of anti-ultraviolet function, and it comprises the manufacture of (1) compound anti ultraviolet agent: compound anti ultraviolet agent is comprised of inorganic uvioresistant screening agent and organic uv absorbers; The composition of inorganic uvioresistant screening agent is nano level TiO
2and Al
2o
3or SiO
2inorganic oxide; Organic uv absorbers is the benzotriazole category organic substance; The weight ratio of inorganic uvioresistant screening agent and organic uv absorbers is 1: 1, takes this compound anti ultraviolet agent and ethylene glycol and is made into slurries, then is placed in ball mill and disperses 0.5-1 hour; (2), the esterification operation: the terephthalic acid of melting and ethylene glycol, continuously or the intermittent entry esterifying kettle, 160～220 ℃ of temperature, carry out esterification under pressure 0.3Mpa, wait the water byproduct steamed reach theoretical amount 90% the time, esterification stops; (3) polyreaction operation: obtain terephthalic acid dihydroxyl ethyl ester monomer after the esterification operation, add compound anti ultraviolet agent, add catalyst acetic acid antimony simultaneously, send into polymerization process, in the terephthalic acid % by weight, the catalyzer add-on is 0.03-0.04%, and the add-on of compound anti ultraviolet agent is at 1.5-2.0%; Monomer first carries out prepolymerization in polymeric kettle under 215～225 ℃ of normal pressures, then in absolute pressure, is less than 150pa, at 285 ± 2 ℃ of temperature, carries out polymerization, impels reaction to reach certain polymerization degree, and the ethylene glycol of generation reclaims after condenser; (4), after condensation reaction finishes, material makes the uvioresistant polyester section through Cast Strip, cooling, pelletizing, drying.The deficiency of the method is: benzotriazole is organic phenolic compound, under hot conditions, as the protonic acid form, exists, and can destroy inorganic nanometer powder TiO
2and Al
2o
3or SiO
2surperficial organic agent, cause the reunion of inorganic nanometer powder in pre-collecting process.In addition, due to inorganic nanometer powder in polymerization process, continue the time of 4～6 hours under hot conditions, nanoparticle generation agglomeration is obvious, under the loose condition of low temperature oversubscription, the inorganic nano ion is to make light produce strong diffuse scattering effect through fabric the time with huge specific surface area, reach anti-ultraviolet purpose, but after long pyroreaction, inorganic nanometer powder is originally reunited in a large number and has been formed micro-size particles, diffuse scattering effect to light significantly reduces, in addition, the method adds the benzotriazole type organic before prepolymerization reaction, in the prepolymerization reaction process, can be drawn out of system because of a large amount of EG evaporations.
The Chinese invention patent that notification number is CN100503910C discloses a kind of Nano titanium nitride anti-ultraviolet polyester fiber, and it is by master batch method spinning uvioresistant fiber.The Chinese invention patent that notification number is CN1300246C discloses a kind of method of preparing uvioresistant polyester by nanometer titania generated in situ, though its ethylene glycol salt for preparing titanium carries out surface treatment through organic agent or silane coupling agent, but titanium ethylene glycolate is as polymerizing catalyst, the PET polyreaction is had to strong katalysis and side reaction Degradation, easily cause the PET hue of chip poor, molecular weight distribution is wide, in addition, the hydrolysis of polymerization process situ generates Nano titanium dioxide, the water molecules that the decomposition in polymerization later stage produces on the one hand has a strong impact on polyreaction, on the other hand, the Nano titanium dioxide that the method is made is good organic matter of sewage decomposing material, section is after long-time solar radiation, viscosity degradation, produce and decompose.The application for a patent for invention that publication number is CN101864067A, disclose anti-ultraviolet superfine terylene and preparation method thereof, is a kind of uvioresistant additive co-blended spinning technology of crossing through coupling agent treatment.The patent of invention that notification number is CN101735578B discloses a kind of fire-retardant uvioresistant matrix material and preparation method thereof, use be to take the inorganic nano ultraviolet ray-resistant material as ultraviolet scattering material, produce certain uvioresistant effect.
To sum up, prior art is all mainly that the huge specific surface area that relies on inorganic nanometer powder to have produces diffuse scattering generation uvioresistant effect for basic to ultraviolet ray, stability and the efficiency of its UVResistant effect are to be improved, this just need to start with from uvioresistant mechanism, the polyester that preparation has more excellent UVResistant effect and has good spinnability.In addition, also need exploitation badly when thering is anti-ultraviolet function, also have other function for example resistance to deterioration, absorbing fast-drying concurrently, static resistance, the complex function polyester of anti-pilling.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of a kind of uvioresistant, the section of antistatic, anti-pilling polyester.
For solving above technical problem, the present invention takes following technical scheme:
A kind of uvioresistant, the preparation method that antistatic, anti-pilling polyester is cut into slices, comprise esterification operation and the polyreaction operation of carrying out successively, wherein:
Described esterification operation comprises esterification reaction section and secondary esterification reaction section, wherein: a described esterification reaction section is implemented as follows: terephthalic acid, ethylene glycol 1: 1.2 in molar ratio～1.3 is joined in reaction kettle of the esterification, carry out one time esterification under 250 ℃～265 ℃, described secondary esterification reaction section is implemented as follows: after one time esterification reaction section completes, add ethylene glycol, make system be cooled to 230 ℃～235 ℃, under protection of inert gas, add polyoxyethylene glycol that number-average molecular weight is 600～6000 as the 3rd monomer, the add-on of the 3rd monomer is 1.0%～6.5% of polyester slice weight, then add the mixed liquid of the hindered amine light stabilizer that mass concentration is 2%～5% and the mixed liquid of the Hinered phenols antioxidant that mass concentration is 2%～5%, take polyester slice weight as benchmark, the add-on of described hindered amine light stabilizer and Hinered phenols antioxidant is respectively 10～300ppm, the mixed liquid of described hindered amine light stabilizer be hindered amine light stabilizer be dispersed in solvent ethylene glycol and add acetic acid after the gained pH value solution that is 4～5, the mixed liquid of described Hinered phenols antioxidant be Hinered phenols antioxidant be dispersed in solvent ethylene glycol and add acetic acid after the gained pH value solution that is 4～5, after adding, stir, reactor starts to heat up, slowly add the hydroxy silicon oil that hydroxyl value is 0.5%～8.0%, carry out the secondary esterification, finish to the esterification water outlet, temperature of reaction kettle reaches 260 ℃, the add-on of wherein said hydroxy silicon oil is 0.1%～1.2% of polyester slice weight,
Described polyreaction operation is implemented as follows: in the system after the secondary esterification, add polymerizing catalyst, after stirring, deliver in prepolymerization kettle, carry out prepolymerization reaction, the prepolymerization reaction temperature is controlled at 260～275 ℃, and pressure is 0.6～2.0kpa; After prepolymerization reaction finishes, close vacuum system, under nitrogen protection and negative pressure, the UV light absorber of liquid state or melting is injected, stir, then the static inhibitor that melting is good is injected, stir, deliver to terminal polymerization kettle after being filtered, wherein, the add-on of described UV light absorber is 0.1%～2.0% of polyester slice weight, and the add-on of described static inhibitor is 0.5%～4.5% of polyester slice weight; Finally, in terminal polymerization kettle, under 270 ℃～285 ℃ of temperature, pressure 40～100Pa, carry out the final polymerization reaction, after final polymerization has reacted, the discharging pelletizing, obtain uvioresistant, antistatic, anti-pilling polyester section.
According to the present invention, described UV light absorber can be one or more the combination in the UV light absorber of following kind: Benzotriazole Ultraviolet Stabilizer:
326,
234,
350,
320,
328; The low volatility Benzotriazole Ultraviolet Stabilizer
360; The red shift Benzotriazole Ultraviolet Stabilizer
327; And
uV-P, the special UV light absorber CYASORB of cyanogen UV-3638F, triazine series UV light absorber UV-1577, the preferred add-on of UV light absorber is 0.15%～1.10% of polyester slice weight.Preferably, select one or more compound uses of following UV light absorber: benzotriazole category series UV light absorber:
234,
320,
328; The low volatility Benzotriazole Ultraviolet Stabilizer
360; The red shift Benzotriazole Ultraviolet Stabilizer
327; And
uV-P, the special UV light absorber CYASORB of cyanogen UV-3638F, triazine series UV light absorber UV-1577 etc.Particularly preferred, select one or more compound uses of the UV light absorber of following kind: benzotriazole category series UV light absorber:
234,
320,
328; And
uV-P, the special UV light absorber CYASORB of cyanogen UV-3638F.Add UV light absorber churning time afterwards to be preferably 2～8 minutes.
According to the present invention, above-mentioned static inhibitor can be one or more the combination in static inhibitor 102, static inhibitor 103, static inhibitor 105 and static inhibitor 308, and its add-on is preferably 0.65%～2.5% of polyester slice weight.
According to the present invention, described hindered amine light stabilizer can be for being selected from non-polymeric type high molecular weight hindered amine light stabilizer
119FL, 770 pairs (2 of polymerized hindered amine photostabilizer Chimassorb944, Tinuvin 788 and photostabilizers, 2,6,6-tetramethyl-4-piperidyl) one or more in sebate, be preferably the composite light stabilizer that more than two kinds, photostabilizer mixes, be for example Tinuvin 788 with
119FL is the mixture of 1: 1 by weight.The add-on of described hindered amine light stabilizer is preferably 15～90ppm (take the polyester gross weight as benchmark).Described Hinered phenols antioxidant can be Irganox 1076, one or more in Irganox 1010 and Irgafos168, be preferably the composite antioxidant that the oxidation inhibitor more than two kinds mixes, for example Irganox 1076 and the mixture of Irganox 1010 by weight 1: 3.The add-on of Hinered phenols antioxidant is 30～250ppm (take the polyester gross weight as benchmark).Preferably, the add-on of hindered amine light stabilizer is 35～60ppm, and the add-on of Hinered phenols antioxidant is 75～180ppm.A certain amount of hindered amine light stabilizer and Hinered phenols antioxidant can produce synergistic effect with UV light absorber as auxiliary component, have guaranteed that polyester has good photostabilization and antioxidant property.
According to the present invention, polymerizing catalyst can be known various polyester polymerizing catalysts.Particularly in the present invention, polymerizing catalyst is used antimony glycol, its add-on to be generally the 450～550ppm weight of polyester slice (take be benchmark).
According to the present invention, the number-average molecular weight of the described polyoxyethylene glycol as the 3rd monomer is preferably 1500～4000, and add-on is preferably 1.5%～4.0% of polyester slice weight.
When the fiber of preparation is staple fibre, the add-on of hydroxy silicon oil is preferably 0.6%～1.2% of polyester slice weight.When the trevira of preparation is long filament, the add-on of hydroxy silicon oil is preferably 0.1%～0.8% of polyester slice weight.The effect of hydroxy silicon oil is hydroxyl in its two ends on the one hand, participate in polyreaction as comonomer, because the hydroxy silicon oil reaction activity is low, polyreaction is rapid, be conducive to accelerate polymerization rate, and, because the bonding after itself and carboxylic acid reaction belongs to weak bond, easy fracture is heated in spinning process, can make polyester fondant produce evenly and larger viscosity drop, by controlling add-on and the spinning condition of hydroxy silicon oil, can prepare respectively the polyester slice of applicable staple fibre or long filament production characteristics and staple fibre and the long filament that different breaking tenacity requires, the final polyester viscosity controller of its middle short fiber is in 0.58 ± 0.012 left and right, the final viscosity of long filament is controlled at 0.63 ± 0.012 left and right, effectively reduce fibre strength, thereby make fiber there is good anti-pilling property.
In particular, short silk level uvioresistant, antistatic, anti-pilling polyester section, in polymerization process, the usage quantity of hydroxy silicon oil is wanted the high comfortable polyester slice of a little higher than long filament level, mainly will pass through steam-heated stretching process and heat-setting process in the short fiber spinning process, certain thermal destruction of fiber under the condition of high temperature in winding process, in stretching and heat setting type process, the contact high-temperature steam, in macromolecular chain, the estersil bonding further ruptures, and produces the secondary viscosity drop.Its fiber final response viscosity is: 0.58 ± 0.012, and the fibre breakage intensity control exists: 3.2 ± 0.2, meeting processing and taking intensity simultaneously, give the anti-pilling property that fiber is good.
Long filament level uvioresistant, antistatic, anti-pilling polyester section, in polymerization process, the usage quantity of hydroxy silicon oil is slightly lower than the high comfortable copolyester section of staple fibre level, but add relatively the 3rd monomer polyoxyethylene glycol of a large amount, so that in the situation that low-fiber breaking tenacity effectively falls in viscosity drop for once in spinning process.Its fiber final response viscosity is: 0.63 ± 0.012, and the fibre breakage intensity control exists: 2.6 ± 0.2, meeting processing and taking intensity simultaneously, give the anti-pilling property that fiber is good.
Due to the utilization of technique scheme, the present invention compared with prior art has following advantage:
1, the present invention be take UV light absorber as main, the light that is converted into other wavelength by absorbing ultraviolet ray reduces the injury of UV-light to human body skin, simultaneously, by being used in conjunction with hindered amine light stabilizer and Hinered phenols antioxidant, with UV light absorber collaborative, further improved the fabric lining anti-ultraviolet property under the direct sunlight condition out of doors.
2, from after esterification, added anti ultraviolet agent different in the past, the present invention is after prepolymerization reaction completes, poly-reaction adds the UV light absorber of liquid or melting before carrying out eventually, so, effectively reduce the residence time of UV light absorber, significantly reduce the volatilization of UV light absorber or cause side reaction, because melt kinematic viscosity after prepolymerization reaction completes is less, also guaranteed UV light absorber good dispersion effect in melt simultaneously, the add-on of UV light absorber is less, and cost is lower.
3, by add static inhibitor mid-term in polymerization, and use and to there is good hygroscopic polyoxyethylene glycol as the 3rd monomer, can keep, on fiber fundamental property basis, obtaining good antistatic property, especially be applicable under spring, the autumn north dry climatic condition needs of clothes eliminostatic.Adding of the 3rd monomer also is beneficial to the anti-pilling property that reduces fibre breakage intensity and improve fiber.
4, can add the consumption of hydroxy silicon oil and control spinning condition by control, can produce on the one hand the section kind that is applicable to staple fibre and the different spinning requirement of long filament, different according to staple fibre and continuous yarn spinning technique on the other hand, can during spinning winding and drawing and setting, control the polyester viscosity drop, effectively reduce fibre strength, thereby make fiber there is good anti-pilling property.
5, hindered amine light stabilizer and Hinered phenols antioxidant first are dispersed in acetic acid and ethylene glycol and add, can under the prerequisite that does not affect quality product, (flash distillation can occur rapidly in acetic acid in the prepolymerization reaction process, the discharge system), effectively suppress hindered amine light stabilizer at high temperature react with Hinered phenols antioxidant and the follow-up hydroxy silicon oil added (be the protonic acid with some strength under hydroxy silicon oil high temperature, can at high temperature produce and react with hindered amine light stabilizer and Hinered phenols antioxidant).
6, take the knitting and woven fabric that fiber that gained polyester slice of the present invention is spun into is raw material, its Specifications is uv transmittance≤5.0% after tested, anti-pilling property>=4 grade, fiber volume fraction resistance≤10
10Ω .cm, uvioresistant, anti pilling, antistatic complex function excellence.
Embodiment
The present invention relates to the preparation method of uvioresistant, the section of antistatic, anti-pilling polyester.At first, in the process of synthetic polyethylene terephthalate, choosing flexible polyoxyethylene glycol is the 3rd monomer, and add a certain amount of UV light absorber that can in polyester, there is good dispersion with static inhibitor with acquisition ultraviolet-resistent property and antistatic property.Simultaneously, for guaranteeing fiber, there is good anti-pilling property, improve polymerization rate, add a certain amount of hydroxy silicon oil before polymerization; For guaranteeing that polyester has good photostabilization and antioxidant property, add a certain amount of hindered amine light stabilizer and Hinered phenols antioxidant as auxiliary component, produce synergistic effect with UV light absorber, further improve UVResistant effect.The polyester slice of preparation through pre-crystallized, dry, by accurately controlling spinning condition, control without the silk noil viscosity drop, thereby control fibre breakage intensity, generation anti pilling effect, spin the various trevira with complex function.
Below in conjunction with specific embodiment, the present invention will be further described in detail, but the present invention is not limited to following examples.
In following examples, all adopt that the pH value is 4～5, (solvent is ethylene glycol to the mixed liquid of the composite light stabilizer of mass concentration 2%, and use the vinegar acid for adjusting pH value), and the pH value is 4～5, the mixed liquid (solvent is ethylene glycol, and uses the vinegar acid for adjusting pH value) of the composite antioxidant of mass concentration 2%.Wherein, composite light stabilizer by Tinuvin 788 with
119FL formed by weight 1: 1; Composite antioxidant consists of by weight Irganox 1076 and Irganox 1010 at 1: 3.
In addition, for adapting to different spinning process requirements, it is 0.730 ± 0.012 that short fiber grade polyester chip limiting viscosity is controlled; 243 ± 1 ℃ of fusing points; 69 ± 1 ℃ of second-order transition temperatures; It is 0.710 ± 0.012 that long fine grade polyester chip limiting viscosity is controlled; 246 ± 1 ℃ of fusing points; 72 ± 1 ℃ of second-order transition temperatures.
Embodiment 1
The present embodiment provides the preparation method of a kind of uvioresistant, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1) a, esterification reaction section: get 18kg pure terephthalic acid (PTA), 7.5kg ethylene glycol (EG) adds 70 liters of polyester experimental installations, after stirring, start to heat up and be forced into 0.3Mpa, carry out esterification, esterification temperature is controlled at 250～265 ℃, complete to the esterification water outlet, reply atmospheric pressure, finish reaction.
(2), secondary esterification reaction section: after an esterification completes; at first add ethylene glycol; make temperature of reaction kettle be down to 230～235 ℃, the polyoxyethylene glycol that is then 2500 by the 450g number-average molecular weight that heating and melting is good adds reactor under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned mixed liquid form, with above-mentioned mixed liquid form, add the above-mentioned composite antioxidant of 3.375g.After adding, stir.Reactor starts to heat up, and slowly adds the hydroxy silicon oil that the 160g hydroxyl value is 5.5%, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification completes, and esterification column backs down the cooling of beginning.
(3), polyreaction operation: in system; add polymerizing catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; control 260～275 ℃ of temperature; open vacuum pump, slowly be down to 2Kpa in 40 minutes, the rough vacuum polyreaction finishes; close vacuum system, under nitrogen protection and negative pressure condition by melting is good 226g UV light absorber
234, by the specific equipment injected system, mix after 3 minutes, by 226g static inhibitor 102 injected systems of having melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization strainer filters, and opens high vacuum, and pressure is 40～100pa, carry out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction completes, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, its test result is in Table 1.
Embodiment 2
The present embodiment provides the preparation method of a kind of uvioresistant, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1) a, esterification reaction section: get 18kg pure terephthalic acid (PTA), 7.5kg ethylene glycol (EG) adds 70 liters of polyester experimental installations, after stirring, start to heat up and be forced into 0.3Mpa, carry out esterification, esterification temperature is controlled at 250～265 ℃, complete to the esterification water outlet, reply atmospheric pressure, finish reaction.
(2), secondary esterification reaction section: after an esterification completes; at first add ethylene glycol; make temperature of reaction kettle be down to 230～235 ℃, the polyoxyethylene glycol that is then 2500 by the 450g number-average molecular weight that heating and melting is good adds reactor under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned mixed liquid form, with above-mentioned mixed liquid form, add the above-mentioned composite antioxidant of 3.375g.After adding, stir.Reactor starts to heat up, and slowly adds the hydroxy silicon oil that the 120g hydroxyl value is 5.5%, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification completes, and esterification column backs down the cooling of beginning.
(3), polyreaction operation: in system; add polymerizing catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; control 260～275 ℃ of temperature; open vacuum pump, slowly be down to 2Kpa in 40 minutes, the rough vacuum polyreaction finishes; close vacuum system, under nitrogen protection and negative pressure condition by melting is good 113g UV light absorber
234, by the specific equipment injected system, mix after 3 minutes, by 339g static inhibitor 103 injected systems of having melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization strainer filters, and opens high vacuum, and pressure is 40～100pa, carry out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction completes, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, its test result is in Table 1.
Embodiment 3
The present embodiment provides the preparation method of a kind of uvioresistant, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1) a, esterification reaction section: get 18kg pure terephthalic acid (PTA), 7.5kg ethylene glycol (EG) adds 70 liters of polyester experimental installations, after stirring, start to heat up and be forced into 0.3Mpa, carry out esterification, esterification temperature is controlled at 250～265 ℃, complete to the esterification water outlet, reply atmospheric pressure, finish reaction.
(2), secondary esterification reaction section: after an esterification completes; at first add ethylene glycol; make temperature of reaction kettle be down to 230～235 ℃, the polyoxyethylene glycol that is then 3000 by the 450g number-average molecular weight that heating and melting is good adds reactor under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned mixed liquid form, with above-mentioned mixed liquid form, add the above-mentioned composite antioxidant of 3.375g.After adding, stir.Reactor starts to heat up, and slowly adds the hydroxy silicon oil that the 160g hydroxyl value is 5.5%, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification completes, and esterification column backs down the cooling of beginning.
(3), polyreaction operation: in system; add polymerizing catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; control 260～275 ℃ of temperature; open vacuum pump, slowly be down to 2Kpa in 40 minutes, the rough vacuum polyreaction finishes; close vacuum system, under nitrogen protection and negative pressure condition by melting is good 113g UV light absorber
320, by the specific equipment injected system, mix after 3 minutes, by 226g static inhibitor 102 injected systems of having melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization strainer filters, and opens high vacuum, and pressure is 40～100pa, carry out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction completes, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, its test result is in Table 1.
Embodiment 4
The present embodiment provides the preparation method of a kind of uvioresistant, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1) a, esterification reaction section: get 18kg pure terephthalic acid (PTA), 7.5kg ethylene glycol (EG) adds 70 liters of polyester experimental installations, after stirring, start to heat up and be forced into 0.3Mpa. and carry out esterification, esterification temperature is controlled at 250～265 ℃, complete to the esterification water outlet, reply atmospheric pressure, finish reaction.
(2), secondary esterification reaction section: after an esterification completes; at first add ethylene glycol; make temperature of reaction kettle be down to 230～235 ℃, the polyoxyethylene glycol that is then 3000 by the 450g number-average molecular weight that heating and melting is good adds reactor under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned mixed liquid form, with above-mentioned mixed liquid form, add the above-mentioned composite antioxidant of 3.375g.After adding, stir.Reactor starts to heat up, and slowly adds the hydroxy silicon oil that the 120g hydroxyl value is 5.5%, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification completes, and esterification column backs down the cooling of beginning.
(3), polyreaction operation: in system; add polymerizing catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; control 260～275 ℃ of temperature; open vacuum pump, slowly be down to 2Kpa in 40 minutes, the rough vacuum polyreaction finishes; close vacuum system, under nitrogen protection and negative pressure condition by melting is good 226g UV light absorber
320, by the specific equipment injected system, mix after 3 minutes, by 339g static inhibitor 103 injected systems of having melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization strainer filters, and opens high vacuum, and pressure is 40～100pa, carry out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction completes, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, its test result is in Table 1.
Embodiment 5
The present embodiment provides the preparation method of a kind of uvioresistant, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1) a, esterification reaction section: get 18kg pure terephthalic acid (PTA), 7.5kg ethylene glycol (EG) adds 70 liters of polyester experimental installations, after stirring, start to heat up and be forced into 0.3Mpa, carry out esterification, esterification temperature is controlled at 250～265 ℃, complete to the esterification water outlet, reply atmospheric pressure, finish reaction.
(2), secondary esterification reaction section: after an esterification completes; at first add ethylene glycol; make temperature of reaction kettle be down to 230～235 ℃, the polyoxyethylene glycol that is then 4000 by the 450g number-average molecular weight that heating and melting is good adds reactor under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned mixed liquid form, with above-mentioned mixed liquid form, add the above-mentioned composite antioxidant of 3.375g.After adding, stir.Reactor starts to heat up, and slowly adds the hydroxy silicon oil that the 160g hydroxyl value is 5.5%, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification completes, and esterification column backs down the cooling of beginning.
(3), polyreaction operation: in system; add polymerizing catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; control 260～275 ℃ of temperature; open vacuum pump, slowly be down to 2Kpa in 40 minutes, the rough vacuum polyreaction finishes; close vacuum system, under nitrogen protection and negative pressure condition by melting is good 113g UV light absorber (
234 with
320 mixture, the ratio of the two weight is 1: 1), by the specific equipment injected system, mix after 3 minutes, by 226g static inhibitor 102 injected systems of having melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization strainer filters, open high vacuum, pressure is 40～100pa, carries out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction completes, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, and its test result is in Table 1.
Embodiment 6
The present embodiment provides the preparation method of a kind of uvioresistant, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1) a, esterification reaction section: get 18kg pure terephthalic acid (PTA), 7.5kg ethylene glycol (EG) adds 70 liters of polyester experimental installations, after stirring, start to heat up and be forced into 0.3Mpa, carry out esterification, esterification temperature is controlled at 250～265 ℃, complete to the esterification water outlet, reply atmospheric pressure, finish reaction.
(2), secondary esterification reaction section: after an esterification completes; at first add ethylene glycol; make temperature of reaction kettle be down to 230～235 ℃, the polyoxyethylene glycol that is then 4000 by the 450g number-average molecular weight that heating and melting is good adds reactor under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned mixed liquid form, with above-mentioned mixed liquid form, add the above-mentioned composite antioxidant of 3.375g.After adding, stir.Reactor starts to heat up, and slowly adds the hydroxy silicon oil that the 120g hydroxyl value is 5.5%, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification completes, and esterification column backs down the cooling of beginning.
(3), polyreaction operation: in system; add polymerizing catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; control 260～275 ℃ of temperature; open vacuum pump, slowly be down to 2Kpa in 40 minutes, the rough vacuum polyreaction finishes; close vacuum system, under nitrogen protection and negative pressure condition by melting is good 226g UV light absorber (
234 with
320 mixture, the ratio of the two weight is 1: 1), by the specific equipment injected system, mix after 3 minutes, by 339g static inhibitor 103 injected systems of having melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization strainer filters, open high vacuum, pressure is 40～100pa, carries out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction completes, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, and its test result is in Table 1.
Embodiment 7
The present embodiment provides the preparation method of a kind of uvioresistant, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1) a, esterification reaction section: get 18kg pure terephthalic acid (PTA), 7.5kg ethylene glycol (EG) adds 70 liters of polyester experimental installations, after stirring, start to heat up and be forced into 0.3Mpa. and carry out esterification, esterification temperature is controlled at 250～265 ℃, complete to the esterification water outlet, reply atmospheric pressure, finish reaction.
(2), secondary esterification reaction section: after an esterification completes; at first add ethylene glycol; make temperature of reaction kettle be down to 230～235 ℃, the polyoxyethylene glycol that is then 2000 by the 450g number-average molecular weight that heating and melting is good adds reactor under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned mixed liquid form, with above-mentioned mixed liquid form, add the above-mentioned composite antioxidant of 3.375g.After adding, stir.Reactor starts to heat up, and slowly adds the hydroxy silicon oil that the 180g hydroxyl value is 5.5%, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification completes, and esterification column backs down the cooling of beginning.
(3), polyreaction operation: in system, add polymerizing catalyst, deliver to prepolymerization kettle intensification polymerization after stirring, control 260～275 ℃ of temperature, open vacuum pump, slowly be down to 2Kpa in 40 minutes, the rough vacuum polyreaction finishes, close vacuum system, under nitrogen protection and negative pressure condition by melting is good 113g UV light absorber (UV light absorber
234 with the mixture of the special UV light absorber CYASORB of cyanogen UV-3638F, the ratio of the two weight is 2: 1), by the specific equipment injected system, mix after 3 minutes, by 275g static inhibitor (being formed at 1: 1 by weight by static inhibitor 103 and the static inhibitor 102) injected system of having melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization strainer filters, open high vacuum, pressure is 40～100pa, carry out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction completes, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, its test result is in Table 1.
Embodiment 8
The present embodiment provides the preparation method of a kind of uvioresistant, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1) a, esterification reaction section: get 18kg pure terephthalic acid (PTA), 7.5kg ethylene glycol (EG) adds 70 liters of polyester experimental installations, after stirring, start to heat up and be forced into 0.3Mpa, carry out esterification, esterification temperature is controlled at 250～265 ℃, complete to the esterification water outlet, reply atmospheric pressure, finish reaction.
(2), secondary esterification reaction section: after an esterification completes; at first add ethylene glycol; make temperature of reaction kettle be down to 230～235 ℃, the polyoxyethylene glycol that is then 2000 by the 450g number-average molecular weight that heating and melting is good adds reactor under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned mixed liquid form, with above-mentioned mixed liquid form, add the above-mentioned composite antioxidant of 3.375g.After adding, stir.Reactor starts to heat up, and slowly adds the hydroxy silicon oil that the 140g hydroxyl value is 5.5%, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification completes, and esterification column backs down the cooling of beginning.
(3), polyreaction operation: in system, add polymerizing catalyst, deliver to prepolymerization kettle intensification polymerization after stirring, control 260～275 ℃ of temperature, open vacuum pump, slowly be down to 2Kpa in 40 minutes, the rough vacuum polyreaction finishes, close vacuum system, under nitrogen protection and negative pressure condition by melting is good 113g UV light absorber (UV light absorber
234 with the mixture of the special UV light absorber CYASORB of cyanogen UV-3638F, the ratio of the two weight is 2: 1), by the specific equipment injected system, mix after 3 minutes, by 275g static inhibitor (being formed at 1: 1 by weight by static inhibitor 103 and the static inhibitor 102) injected system of having melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization strainer filters, open high vacuum, pressure is 40～100pa, carry out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction completes, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, its test result is in Table 1.
Comparative Examples 1
This Comparative Examples provides a kind of preparation method of polyester slice, and it comprises the steps:
(1) a, esterification reaction section: get 18kg pure terephthalic acid (PTA), 7.5kg ethylene glycol (EG) adds 70 liters of polyester experimental installations, after stirring, start to heat up and be forced into 0.3Mpa, carry out esterification, esterification temperature is controlled at 250～265 ℃, complete to the esterification water outlet, reply atmospheric pressure, finish reaction.
(2), secondary esterification reaction section: after an esterification completes; at first add ethylene glycol; make temperature of reaction kettle be down to 230～235 ℃, the polyoxyethylene glycol that is then 2500 by the 450g number-average molecular weight that heating and melting is good adds reactor under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned mixed liquid form, with above-mentioned mixed liquid form, add the above-mentioned composite antioxidant of 3.375g.After adding, stir.Reactor starts to heat up, and slowly adds the hydroxy silicon oil that the 160g hydroxyl value is 5.5%, carries out the secondary esterification, reaches 260 to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification completes, and esterification column backs down the cooling of beginning.
(3), polyreaction operation: add polymerizing catalyst, by 113g UV light absorber liquid or that melting is good
234 add, mix after 3 minutes, by 226g static inhibitor 102 injected systems of having melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization strainer filters, control 260～275 ℃ of temperature, open vacuum pump, slowly be down to 2Kpa in 40 minutes, the rough vacuum polyreaction finishes, open high vacuum, pressure is 40～100pa, carry out conventional polymerization under 270～280 ℃ of conditions, to reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction completes, obtain polyester slice 22.5kg, its test result is in Table 1.
Comparative Examples 2
This Comparative Examples provides a kind of preparation method of polyester slice, and it comprises the steps:
(1) a, esterification reaction section: get 18kg pure terephthalic acid (PTA), 7.5kg ethylene glycol (EG) adds 70 liters of polyester experimental installations, after stirring, start to heat up and be forced into 0.3Mpa, carry out esterification, esterification temperature is controlled at 250～265 ℃, complete to the esterification water outlet, reply atmospheric pressure, finish reaction.
(2), secondary esterification reaction section: after an esterification completes; at first add ethylene glycol; make temperature of reaction kettle be down to 230～235 ℃, the polyoxyethylene glycol that is then 3000 by the 450g number-average molecular weight that heating and melting is good adds reactor under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned mixed liquid form, with above-mentioned mixed liquid form, add the above-mentioned composite antioxidant of 3.375g.After adding, stir.Reactor starts to heat up, and slowly adds the hydroxy silicon oil that the 120g hydroxyl value is 5.5%, carries out the secondary esterification, reaches 260 to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification completes, and esterification column backs down the cooling of beginning.
(3), polyreaction operation: add polymerizing catalyst, by 113g UV light absorber (UV light absorber liquid or that melting is good
234 with the mixture of the special UV light absorber CYASORBUV-3638F of cyanogen, the ratio of the two weight is 2: 1), by the specific equipment injected system, mix after 3 minutes, by 226g static inhibitor 102 injected systems of having melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization strainer filters.Control 260～275 ℃ of temperature, open vacuum pump, slowly be down to 2Kpa in 40 minutes, the rough vacuum polyreaction finishes, open high vacuum, pressure is 40～100pa, under 270～280 ℃ of conditions, carries out conventional polymerization, to reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction completes, obtain polyester slice 22.5kg, and its test result is in Table 1.
Table 1 uvioresistant, antistatic, anti-pilling polyester section physical and chemical index
The quality index of the polyester slice by above-described embodiment and Comparative Examples can be found out, polyester slice prepared by method of the present invention has kept the quality index of conventional PET polyester slice substantially, show that the preparation method is reasonable, wherein embodiment 1,3,5,7 and Comparative Examples 1 are short silk grade pet chip, and embodiment 2,4,6,8 and Comparative Examples 2 are the long filament grade pet chip.And, in Comparative Examples 1,2, because UV light absorber adds the change of mode, causing the obvious flavescence of hue of chip on the one hand, fusing point and second-order transition temperature rising, show that the part UV light absorber takes system in the rough vacuum stage out of with a large amount of evaporations of ethylene glycol.
For the short silk level uvioresistant that further prepared by checking the present invention, antistatic, the performance of anti-pilling polyester section, respectively with embodiment 1, 3, 5, 7 and the uvioresistant that makes of Comparative Examples 1, antistatic, the anti-pilling polyester section is raw material, pass through successively pre-crystallized, dry, spinning, reel, drawing and setting makes, different from common PET polyester staple fiber spinning technique, this section is owing to adding UV light absorber, static inhibitor, photostabilizer, oxidation inhibitor, the 3rd monomer, hydroxy silicon oil etc., its section second-order transition temperature is lower, therefore must be through pre-crystallized, just can implement section drying process.
Above-mentioned preparation method is specific as follows: at first polyester slice is carried out pre-crystallizedly, it is 3～5 hours that pre-crystallized temperature is controlled 110 ℃～125 ℃, time.Then carry out drying, 130 ℃～145 ℃ of drying temperatures, the time is 3.5～5.0 hours.Carry out spinning after completing drying.Use the special crosssection spinning jets such as three leaves, cross, five leaves.At first on the short fiber spinning production line, produce through reeling, oiling process is made the short fiber tow, spinning speed 850m/min, spinning temperature is controlled at 255 ℃～278 ℃, (because a large amount of modified additives are used in this section, the section melting point depression, in spinning process, will be according to the fusing point of copolyester section, spinning and condition are adjusted, the condition of implementing spinning compares the common PET trevira, each district's temperature of screw rod is lowered 8～15 ℃), then, the short fiber tow is through falling barrel balance after 24 hours, then boundling is stretched, the steam heat setting process, draft temperature is 142 ℃～150 ℃, 110 ℃～135 ℃ of heat setting temperatures, then after the carrier bar drying process, cut off, fixed heavy, finished fiber is made in packing.Product specification is 1.56dtex/38mm, and its fiber volume fraction resistance test data are in Table 2.This fiber, through spinning, is made into knitting and woven fabric, and its Specifications is after tested: uv transmittance≤5.0%, anti-pilling property >=4 grade, have good uvioresistant, anti-pilling composite function.The fabric performance index is in Table 2.
Separately, for the long filament level uvioresistant that further prepared by checking the present invention, the performance that antistatic, anti-pilling polyester is cut into slices, with embodiment 2,4,6,8 and Comparative Examples 2, make respectively polyester slice carry out pre-crystallizedly, it is 3～5 hours that pre-crystallized temperature is controlled 110 ℃～125 ℃, time.Then carry out drying, 130 ℃～145 ℃ of drying temperatures, the time is 3.5～5.0 hours.Carry out spinning after completing drying.Use the special crosssection spinning jets such as three leaves, cross, five leaves.At first to spin the pre-oriented yarn (POY) of corresponding product, spinning temperature is controlled at 255 ℃～278 ℃, (because a large amount of modified additives are used in this section, the section melting point depression, in spinning process, be according to the fusing point of copolyester section, spinning and condition are adjusted, the condition of implementing spinning compares the common PET trevira, and each district's temperature of screw rod is lowered 8～15 ℃), POY fiber sprinning speed 2750m/min.The POY fiber of spinning is through after 24 hours balances, then stretches and texturing craft through corresponding, and draft temperature is 142 ℃～150 ℃, prepares corresponding drawing and setting temperature and also will lower.The preparation specification is the low stretch network product that 55.5dtex/72f has the hydroscopic fast-drying function, and its fiber volume fraction resistance is in Table 2.Fiber quality is good, and fiber is through the knitting and woven fabric of making, and after tested, the fabric performance index is in Table 2.
Table 2 uvioresistant, antistatic, the high comfortable trevira fabric performance of anti pilling
Above-mentioned fabric is mainly spring, summer, autumn Fashion Design, therefore, except thering is good uvioresistant, antistatic, anti pilling function, the physics-chem characteristic that the present invention is special according to this copolyesters, three leaves of spinning or special crosssection staple fibre and the specification of cross special-shaped 0.8～6.5dtex/2.5～10.6mm equal-specification are 40～111dtex/24～96f long filament, this fiber has good uvioresistant, antistatic, anti pilling, hydroscopic fast-drying complex function, and can purely spin or natural fibre blended with hair, suede etc.This fiber is made into knitting and woven fabric, and its Specifications is after tested: uv transmittance≤5.0%, anti-pilling property >=4 grade, have good uvioresistant, anti-pilling composite function.Measure wicking height >=120mm, vaporator rate >=0.20g/hr.
Above the present invention is described in detail, the equivalence that all spirit according to the present invention are done changes or modifies, and all should be encompassed in protection scope of the present invention.
Claims (9)
1. the preparation method of a uvioresistant, antistatic, anti-pilling polyester section, comprise esterification operation and the polyreaction operation of carrying out successively, it is characterized in that:
Described esterification operation comprises esterification reaction section and secondary esterification reaction section, wherein: a described esterification reaction section is implemented as follows: terephthalic acid, ethylene glycol are joined in reaction kettle of the esterification 1:1.2～1.3 in molar ratio, carry out one time esterification under 250 ℃～265 ℃, described secondary esterification reaction section is implemented as follows: after one time esterification reaction section completes, add ethylene glycol, make system be cooled to 230 ℃～235 ℃, under protection of inert gas, add polyoxyethylene glycol that number-average molecular weight is 600～6000 as the 3rd monomer, the add-on of the 3rd monomer is 1.0%～6.5% of polyester slice weight, then add the mixed liquid of the hindered amine light stabilizer that mass concentration is 2%～5% and the mixed liquid of the Hinered phenols antioxidant that mass concentration is 2%～5%, take polyester slice weight as benchmark, the add-on of described hindered amine light stabilizer and Hinered phenols antioxidant is respectively 10～300ppm, the mixed liquid of described hindered amine light stabilizer be hindered amine light stabilizer be dispersed in solvent ethylene glycol and add acetic acid after the gained pH value solution that is 4～5, the mixed liquid of described Hinered phenols antioxidant be Hinered phenols antioxidant be dispersed in solvent ethylene glycol and add acetic acid after the gained pH value solution that is 4～5, after adding, stir, reactor starts to heat up, slowly add the hydroxy silicon oil that hydroxyl value is 0.5%～8.0%, carry out the secondary esterification, finish to the esterification water outlet, temperature of reaction kettle reaches 260 ℃, the add-on of wherein said hydroxy silicon oil is 0.1%～1.2% of polyester slice weight, described polyreaction operation is implemented as follows: in the system after the secondary esterification, add polymerizing catalyst, after stirring, deliver in prepolymerization kettle, carry out prepolymerization reaction, the prepolymerization reaction temperature is controlled at 260～275 ℃, and pressure is 0.6～2.0KPa, after prepolymerization reaction finishes, close vacuum system, under nitrogen protection and negative pressure, the UV light absorber of liquid state or melting is injected, stirred, then the static inhibitor that melting is good is injected, stir, deliver to terminal polymerization kettle after being filtered, wherein, the combination of one or more in the UV light absorber that described UV light absorber is following kind: Benzotriazole Ultraviolet Stabilizer: Tinuvin
326, Tinuvin
234, Tinuvin
350, Tinuvin
320, Tinuvin
328, low volatility Benzotriazole Ultraviolet Stabilizer Tinuvin
360, red shift Benzotriazole Ultraviolet Stabilizer Tinuvin
327, and Tinuvin
uV-P, the special UV light absorber CYASORB of cyanogen UV-3638F, triazine series UV light absorber UV-1577, the add-on of UV light absorber is 0.15%～1.10% of polyester slice weight, the add-on of described static inhibitor is 0.5%～4.5% of polyester slice weight, finally, in terminal polymerization kettle, under 270 ℃～285 ℃ of temperature, pressure 40～100Pa, carry out the final polymerization reaction, after final polymerization has reacted, the discharging pelletizing, obtain uvioresistant, antistatic, anti-pilling polyester section.
2. the preparation method of uvioresistant according to claim 1, the section of antistatic, anti-pilling polyester, it is characterized in that: described static inhibitor is one or more the combination in static inhibitor 102, static inhibitor 103, static inhibitor 105 and static inhibitor 308, and its add-on is 0.65%～2.5% of described polyester slice weight.
3. the preparation method of uvioresistant according to claim 1, the section of antistatic, anti-pilling polyester, it is characterized in that: described hindered amine light stabilizer is for being selected from non-polymeric type high molecular weight hindered amine light stabilizer CHIMASSORB
119FL, polymerized hindered amine photostabilizer Chimassorb 944, Tinuvin 788 and two (2,2,6,6-tetramethyl--4-piperidyl) one or more in sebate, take polyester slice weight as benchmark, and the add-on of described hindered amine light stabilizer is 15～90ppm.
4. the preparation method of uvioresistant according to claim 1, the section of antistatic, anti-pilling polyester, it is characterized in that: described Hinered phenols antioxidant is Irganox 1076, one or more in Irganox 1010 and Irgafos168, take polyester slice weight as benchmark, and the add-on of described Hinered phenols antioxidant is 30～250ppm.
5. the preparation method of uvioresistant according to claim 1, the section of antistatic, anti-pilling polyester, it is characterized in that: take polyester slice weight as benchmark, the add-on of described hindered amine light stabilizer is 35～60ppm, and the add-on of described Hinered phenols antioxidant is 75～180ppm.
6. the preparation method of uvioresistant according to claim 1, the section of antistatic, anti-pilling polyester, it is characterized in that: described hindered amine light stabilizer is the composite light stabilizer that the photostabilizer more than two kinds mixes; Described Hinered phenols antioxidant is the composite antioxidant that the oxidation inhibitor more than two kinds mixes.
7. the preparation method of uvioresistant according to claim 1, the section of antistatic, anti-pilling polyester, it is characterized in that: the number-average molecular weight of the described polyoxyethylene glycol as the 3rd monomer is 1500～4000, and add-on is 1.5%～4.0% of polyester slice weight.
8. according to the preparation method of the described uvioresistant of any one claim in claim 1 to 7, antistatic, anti-pilling polyester section, it is characterized in that: when described polyester slice, during for the preparation of staple fibre, the add-on of described hydroxy silicon oil is 0.6%～1.2% of polyester slice weight.
9. according to the preparation method of the described uvioresistant of any one claim in claim 1 to 7, antistatic, anti-pilling polyester section, it is characterized in that: when described polyester slice for the preparation of trevira while being long filament, the add-on of described hydroxy silicon oil is 0.1%～0.8% of polyester slice weight.
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