CN102409427B - Preparation method for polyester fiber with composite ultraviolet, static electricity and pilling resisting functions - Google Patents
Preparation method for polyester fiber with composite ultraviolet, static electricity and pilling resisting functions Download PDFInfo
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- CN102409427B CN102409427B CN 201110276911 CN201110276911A CN102409427B CN 102409427 B CN102409427 B CN 102409427B CN 201110276911 CN201110276911 CN 201110276911 CN 201110276911 A CN201110276911 A CN 201110276911A CN 102409427 B CN102409427 B CN 102409427B
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Abstract
The invention relates to a preparation method for a polyester fiber with a composite ultraviolet, static electricity and pilling resisting function. The preparation method comprises an esterification reaction procedure, a polymerization reaction procedure and a spinning procedure. The esterification reaction procedure comprises a primary esterification reaction stage and a secondary esterification reaction stage, flexible polyethylene glycol is introduced as a third monomer in the secondary esterification reaction stage, and after esterification is finished, a hindered amine light stabilizer, a hindered phenol anti-oxidant and hydroxyl silicone oil are added, wherein the hindered amine light stabilizer and the hindered phenol anti-oxidant are prepared by taking an acetic acid and ethylene glycol as solvents. In the polymerization reaction procedure, after prepolymerization and before final polymerization, an ultraviolet absorbent and an antistatic agent are added. Before the spinning procedure, polyester is sliced for pre-crystallization and drying. The polyester fiber obtained by the method has the outstanding ultraviolet, static electricity and pilling resisting functions, and after being woven into knitted machine-made fabrics, is tested to have related technical indexes comprising the ultraviolet light transmittance of less than or equal to 5.0%, the pilling resistance of more than or equal to level 4 and the fiber volume specific resistance of less than or equal to 10*10<10> ohm.cm.
Description
Technical field
The present invention relates to a kind of preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function.
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 polyester fiber 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 with various natural fabrics and also exists many deficiencies: feel is hardened, hygroscopicity is poor, anti-ultraviolet property is poor, easily produce static, easily balling-up, be difficult to dyeing etc.Although natural fabric has good dyeability, fabric such as cotton, real silk, hair, fiber crops etc. and has gas permeability, the absorbing sweat performance of keeping humidity is good, without static, characteristics that comfortableness is good, exist and easily wrinkle, lead wet and the deficiency such as rapid-drying properties is poor.
Along with the progressively expansion of polyester fiber range of application, from the seventies in last century, developed country is for the above-mentioned deficiency of polyester fiber, take the plurality of advantages of natural fabric as target, aspect the wearing comfort of fiber, from three aspects, improve the wearability of polyester fiber.On the one hand: by the innovation of spinning technique technology, produce various fibres in differentiation, progressively develop thin dawn, superfine Denier fibre spining technology, produce a series of differential spinning kinds such as islands-in-sea type fibre, tangerine lobe fiber, bicomponent composite fibre, profiled 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 component, produce various fiber species with specific function in the physical blending mode, also can give fabric brand-new function by the rear arrangement of fabric; The third aspect: by copolyreaction, improve this body structure of polyester macromolecule chain, by introducing the copolymerization component group to improve the polyester fiber fabric performance, permanently give fiber various properties.At present, comprise a series of functional polyalkylene ester fibers such as fire-retardant, cationic-dyeable, high contraction, disperse dyeable, antistatic, uvioresistant, far infrared thermal insulation, polyester fiber and fabric are segmented market has produced material impact.
The chemical fibre market of China is through reform and opening-up rapid progress in decades, in 68% level that has reached Gross World Product aspect the normal polyester procedure of fibre production, but the development and application field at the functional polyalkylene ester fiber, China also is in the starting stage at present, be limited at present the exploitation of single functional polyester and fiber more, such as anti-ultraviolet polyester fiber, anti-static polyester fiber etc.And for the exploitation with complex function, high added value functional fiber, then also need the scientific research personnel badly and make a breakthrough in the multifunctional composite fiber field.
Notification number is that the Chinese invention patent of CN1204196C discloses a kind of uvioresistant zinc oxide complex polyester and preparation method thereof, the method at first prepares the suspension of anti ultraviolet agent intermediate basic zinc carbonate ethylene glycol, then after the synthetic esterification stage of PET polyester finishes, before the low vacuum polymerization, the suspension of anti ultraviolet agent intermediate basic zinc carbonate ethylene glycol is added, when polymerisation generates polyester, basic zinc carbonate 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 absorbs ultraviolet property enhancement.Yet, the method is in order to decompose basic zinc carbonate, must make to be aggregated in more than 285 ℃ and carry out, and basic zinc carbonate will resolve into carbon dioxide, water and zinc oxide, and in whole collecting process, carbon dioxide can affect vacuum and cause section to contain a large amount of bubbles on the one hand, on the other hand, polycondensation final stage produces large quantity of moisture can produce degradation reaction, have a strong impact on product quality, simultaneously, the basic zinc carbonate that does not decompose fully will continue to decompose in spinning process, the fiber spinnability variation, and fracture strength reduces.
Publication number is that the Chinese invention patent application of CN101864067A discloses a kind of preparation method with polyester of anti-ultraviolet function, and it comprises the manufacturing of (1) compound anti ultraviolet agent: compound anti ultraviolet agent is comprised of inorganic uvioresistant smoke agent for shielding and organic uv absorbers; The composition of inorganic uvioresistant smoke agent for shielding is nanoscale TiO
2And Al
2O
3Or SiO
2Inorganic oxide; Organic uv absorbers is the benzotriazole organic substance; The weight ratio of inorganic uvioresistant smoke agent for shielding and organic uv absorbers is 1: 1, takes by weighing this compound anti ultraviolet agent and ethylene glycol and is made into slurries, then places ball mill to disperse 0.5-1 hour; (2), the esterification operation: the terephthalic acids of melting and ethylene glycol, continuously or the intermittent entry esterifying kettle, 160～220 ℃ of temperature, carry out esterification under the pressure 0.3Mpa, water byproduct to be steamed reach theoretical amount 90% the time, esterification stops; (3) polymerisation operation: obtain terephthalic acid (TPA) dihydroxy ethyl ester monomer after the esterification operation, add compound anti ultraviolet agent, add simultaneously catalyst acetic acid antimony, send into polymerization process, in the terephthalic acid (TPA) % by weight, the catalyst addition is 0.03-0.04%, and the addition of compound anti ultraviolet agent is at 1.5-2.0%; Monomer first carries out prepolymerization under 215～225 ℃ of normal pressures in polymeric kettle, then in absolute pressure less than 150pa, carry out polymerization under 285 ± 2 ℃ of the temperature, impel reaction to reach certain degree of polymerization, the ethylene glycol of generation reclaims behind condenser; (4) after condensation reaction finished, material made the uvioresistant polyester section through Cast Strip, cooling, pelletizing, drying.The deficiency of the method is: benzotriazole is organic phenolic compound, exists as the Bronsted acid form under the hot conditions, can destroy inorganic nanometer powder TiO
2And Al
2O
3Or SiO
2Surperficial organic agent, cause the reunion of inorganic nanometer powder in the pre-collecting process.In addition, because inorganic nanometer powder is in polymerization process, under hot conditions, continue 4～6 hours time, nano particle 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 when passing fabric with huge specific area, reach anti-ultraviolet purpose, but through after the long pyroreaction, inorganic nanometer powder is originally reunited in a large number and has been formed micro-size particles, and the diffuse scattering effect of light is significantly reduced, 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.
Notification number is that the Chinese invention patent of CN100503910C discloses a kind of Nano titanium nitride anti-ultraviolet polyester fiber, and it is by master batch method spinning uvioresistant fiber.Notification number is the method that the Chinese invention patent of CN1300246C discloses a kind of preparing uvioresistant polyester by nanometer titania generated in situ, though the ethylene glycol salt of its preparation titanium carries out surface treatment through organic agent or silane coupler, but titanium ethylene glycolate is as polymerization catalyst, the PET polymerisation had strong catalytic action 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 hydrone of the decomposition in polymerization later stage generation has a strong impact on polymerisation on the one hand, 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 descends, and produces to decompose.Publication number is the application for a patent for invention of CN101864067A, discloses anti-ultraviolet superfine terylene and preparation method thereof, is a kind of uvioresistant additive co-blended spinning technology of crossing through coupling agent treatment.Notification number is that the patent of invention of CN101735578B discloses a kind of fire-retardant uvioresistant composite and preparation method thereof, use be take the inorganic nano ultraviolet ray-resistant material as ultraviolet scattering material, produce certain uvioresistant effect.
To sum up, prior art mainly all is that the huge specific area that relies on inorganic nanometer powder to have produces diffuse scattering generation uvioresistant effect for basic to ultraviolet ray, stability and the efficient 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 having anti-ultraviolet function, also have other function for example ageing resistance, absorbing fast-drying concurrently, antistatic behaviour, the complex function polyester of anti-pilling.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function.
For solving above technical problem, the present invention takes following technical scheme:
A kind of preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function comprises the esterification operation, polymerisation operation and the spinning process that carry 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 (TPA), ethylene glycol 1: 1.2 in molar ratio～1.3 is joined in the 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 is finished; add ethylene glycol; make system be cooled to 230 ℃～235 ℃; under inert gas shielding; add number-average molecular weight and be 600～6000 polyethylene glycol as the 3rd monomer; the addition of the 3rd monomer is 1.0%～6.5% of polyester slice weight; then add mass concentration and be the seasoning liquid of 2%～5% hindered amine light stabilizer and mass concentration and be the seasoning liquid of 2%～5% Hinered phenols antioxidant; take polyester slice weight as benchmark; the addition of described hindered amine light stabilizer and Hinered phenols antioxidant is respectively 10～300ppm; the seasoning liquid of described hindered amine light stabilizer be hindered amine light stabilizer be dispersed in the solvent ethylene glycol and add acetic acid after gained pH value be 4～5 solution; the seasoning liquid of described Hinered phenols antioxidant be Hinered phenols antioxidant be dispersed in the solvent ethylene glycol and add acetic acid after gained pH value be 4～5 solution; add and stir after complete; reactor begins to heat up; slowly the adding hydroxyl value is 0.5%～8.0% hydroxy silicon oil; carry out the secondary esterification; finish to the esterification water outlet; temperature of reaction kettle reaches 260 ℃, and the addition of wherein said hydroxy silicon oil is 0.1%～1.2% of polyester slice weight.
Described polymerisation operation is implemented as follows: in the system after the secondary esterification, add polymerization catalyst, after stirring, deliver in the 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 ultra-violet absorber injection with liquid state or melting stirs, then the antistatic additive that melting is good is injected, stir, deliver to terminal polymerization kettle after being filtered, wherein, the addition of described ultra-violet absorber is 0.1%～2.0% of polyester slice weight, and the addition of described antistatic additive is 0.5%～4.5% of polyester slice weight; At last, in terminal polymerization kettle, carry out the final polymerization reaction under 270 ℃～285 ℃ of temperature, the pressure 40～100Pa, after the final polymerization reaction was finished, the discharging pelletizing got uvioresistant, antistatic, anti-pilling polyester section;
Described preparation method also is included in before the spinning process, pre-crystallized and dry step is successively carried out in described uvioresistant, the section of antistatic, anti-pilling polyester, described pre-crystallizedly carried out 3～5 hours under 110 ℃～125 ℃ of temperature, described drying was carried out 3.5～5.0 hours under 130 ℃～145 ℃ of temperature.According to the present invention, described ultra-violet absorber can be one or more the combination in the ultra-violet 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 ultra-violet absorber CYASORB of cyanogen UV-3638F, triazine series ultra-violet absorber UV-1577, the preferred addition of ultra-violet absorber is 0.15%～1.10% of polyester slice weight.Preferably, select one or more compound uses of following ultra-violet absorber: benzotriazole series ultra-violet absorber:
234,
320,
328; The low volatility Benzotriazole Ultraviolet Stabilizer
360; The red shift Benzotriazole Ultraviolet Stabilizer
327; And
UV-P, the special ultra-violet absorber CYASORB of cyanogen UV-3638F, triazine series ultra-violet absorber UV-1577 etc.Particularly preferred, select one or more compound uses of the ultra-violet absorber of following kind: benzotriazole series ultra-violet absorber:
234,
320,
328; And
UV-P, the special ultra-violet absorber CYASORB of cyanogen UV-3638F.Add ultra-violet absorber mixing time afterwards and be preferably 2～8 minutes.
According to the present invention, above-mentioned antistatic additive can be one or more the combination in antistatic additive 102, antistatic additive 103, antistatic additive 105 and the antistatic additive 308, and its addition 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, polymerized hindered amine light stabilizer Chimassorb944, Tinuvin 788 and light stabilizer 770, two (2,2,6,6-tetramethyl-4-piperidyl) one or more in the sebacate, be preferably the composite light stabilizer that light stabilizer mixes more than two kinds, for example be Tinuvin 788 with
119FL is 1: 1 mixture by weight.The addition 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, among Irganox 1010 and the Irgafos168 one or more, be preferably the composite antioxidant that the antioxidant more than two kinds mixes, for example Irganox 1076 and the mixture of Irganox 1010 by weight 1: 3.The addition of Hinered phenols antioxidant is 30～250ppm (take the polyester gross weight as benchmark).Preferably, the addition of hindered amine light stabilizer is 35～60ppm, and the addition of Hinered phenols antioxidant is 75～180ppm.A certain amount of hindered amine light stabilizer and Hinered phenols antioxidant can produce cooperative effect with ultra-violet absorber as helper component, have guaranteed that polyester has good light resistance and antioxygenic property.
According to the present invention, polymerization catalyst can be known various polyester polymerization catalysts.Particularly in the present invention, polymerization catalyst uses antimony glycol, its addition to be generally 450～550ppm (take the weight of polyester slice as benchmark).
According to the present invention, the number-average molecular weight of described polyethylene glycol as the 3rd monomer is preferably 1500～4000, and addition is preferably 1.5%～4.0% of polyester slice weight.
According to the present invention, the spinning of polyester staple fiber, the use amount of hydroxy silicon oil is wanted a little higher than long filament grade polyester chip in the polymerization process, mainly be to pass through steam-heated stretching process and heat-setting process in the short fiber spinning process, certain thermal degradation of fiber under the condition of high temperature in winding process, in stretching and HEAT SETTING process, the contact high-temperature steam, the estersil bonding further ruptures in the macromolecular chain, produce secondary viscosity and fall, its fiber final response viscosity is: 0.58 ± 0.012, and the fibrous fracture strength control exists: 3.2 ± 0.2, satisfying processing and taking intensity simultaneously, give fiber good anti-pilling property.The spinning of polyester filament, the use amount of hydroxy silicon oil slightly is lower than the high comfortable copolyester section of staple fibre level in the polymerization process, but add relatively the 3rd monomer polyethylene glycol of a large amount so that in the situation that in the spinning process for once viscosity fall, low-fiber fracture strength is effectively fallen.Its fiber final response viscosity is: 0.63 ± 0.012, and the fibrous fracture strength control exists: 2.6 ± 0.2, satisfying processing and taking intensity simultaneously, give fiber good anti-pilling property.Concrete scheme is: when the fiber of preparation was staple fibre, the addition of hydroxy silicon oil was preferably 0.6%～1.2% of polyester slice weight.When the polyester fiber of preparation was long filament, the addition of hydroxy silicon oil was preferably 0.1%～0.8% of polyester slice weight.
Spinning process according to the present invention is identical with the spinning process of conventional PET polyester, generally comprise spinning, coiling, stretching, fixating shape step, but because comparing with conventional PET polyester to some extent, its fusing point of polyester slice of gained of the present invention descends, therefore in spinning process, need spinning condition is adjusted, implement the more common PTT polyester fiber of condition of spinning, screw rod is respectively distinguished 8～15 ℃ of temperature downward modulations.Corresponding drawing and setting temperature also will be reduced.Those skilled in the art can adjust corresponding spinning condition according to the fusing point of concrete polyester slice.According to a concrete aspect of the present invention, spinning temperature is controlled at 255 ℃～278 ℃, and draft temperature is 142 ℃～150 ℃, and heat setting temperature is 110 ℃～135 ℃.
For expanding the use field of polyester fiber, be applied to outdoor exercises spring and summer and easy suit series, above-mentioned fibre section can be the series of shapes such as round, triangle, cross, three leaves, hollow, further enlarge as the product advantage with uvioresistant, antistatic, anti-pilling composite function fiber, the fibre section also can adopt " W " and hollow compound.Also can possess good hydroscopic fast-drying function.With itself and natural fibre blended, can improve the comfortableness of fabric.
Because the utilization of technique scheme, the present invention compared with prior art has following advantage:
1, the present invention is take ultra-violet absorber as main, the light that is converted into other wavelength by absorbing ultraviolet ray reduces ultraviolet light to the injury of human body skin, simultaneously, by being used in conjunction with hindered amine light stabilizer and Hinered phenols antioxidant, with ultra-violet absorber collaborative, further improved the out of doors anti-ultraviolet property under the direct sunlight condition of fabric lining.
2, from namely to add anti ultraviolet agent after esterification different in the past, the present invention is after prepolymerization reaction is finished, gather eventually the ultra-violet absorber that front adding liquid or melting are carried out in reaction, so, effectively reduce the time of staying of ultra-violet absorber, significantly reduce the volatilization of ultra-violet absorber or cause side reaction, because melt kinematic viscosity after prepolymerization reaction is finished is less, also guaranteed simultaneously ultra-violet absorber good dispersion effect in melt, the addition of ultra-violet absorber is less, and cost is lower.
3, by add antistatic additive mid-term in polymerization, and use and to have good hygroscopic polyethylene glycol as the 3rd monomer, can keep obtaining good antistatic property on the fiber key property basis, especially be fit under spring, the autumn north dry climatic condition needs that clothes static is eliminated.The adding of the 3rd monomer also is beneficial to the anti-pilling property that reduces fibrous fracture intensity and improve fiber.
4, the present invention adds hydroxy silicon oil in the secondary esterification reaction section, and in forming the macromolecular chain process, hydroxy silicon oil participates in polymerisation, and on the one hand, the hydroxy silicon oil reaction activity is low, is conducive to accelerate polymerization rate; On the other hand, bonding behind itself and the carboxylic acid reaction belongs to weak bond, easy fracture is heated in spinning process, polyester fondant is produced evenly and larger viscosity is fallen, so, addition and spinning condition by the control hydroxy silicon oil, can produce on the one hand the section kind that is fit 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 control polyester viscosity during spinning silk winding and drawing and setting falls, effectively reduce fibre strength, thereby make fiber have good anti-pilling property.
5, hindered amine light stabilizer and Hinered phenols antioxidant are dispersed in first again adding in acetic acid and the ethylene glycol, can be (flash distillation can occur rapidly in acetic acid in the prepolymerization reaction process under the prerequisite that does not affect product quality, the discharge system), the hydroxy silicon oil of establishment hindered amine light stabilizer and Hinered phenols antioxidant and follow-up adding at high temperature react (for having the Bronsted acid of some strength, can at high temperature produce reaction with hindered amine light stabilizer and Hinered phenols antioxidant under the hydroxy silicon oil high temperature).
6, according to the present invention, prepared uvioresistant, antistatic, anti-pilling polyester section, owing to having added multiple modified component, the more conventional PET polyester of its section vitrification point has decline in various degree, in the spinning chips dry run, easily cause bonding, before spinning, at first carry out pre-crystallized can effectively avoiding and bond.
7, the knitting and woven fabric take gained polyester fiber of the present invention as raw material, its Specifications is uv transmittance≤5.0% after tested, anti-pilling property 〉=4 grade, fiber volume fraction resistance≤10
10Ω .cm, uvioresistant, ANTIPILLING, antistatic complex function is excellent.
The specific embodiment
The present invention relates to have uvioresistant, the preparation method of antistatic, anti-pilling polyester fiber.At first, in the process of synthetic polyethylene terephthalate, choosing flexible polyethylene glycol is the 3rd monomer, and adds a certain amount of ultra-violet absorber that can have good dispersion in polyester and antistatic additive with acquisition ultraviolet-resistent property and antistatic property.Simultaneously, have good anti-pilling property for guaranteeing fiber, improve polymerization rate, before polymerization, add a certain amount of hydroxy silicon oil; For guaranteeing that polyester has good light resistance and antioxygenic property, add a certain amount of hindered amine light stabilizer and Hinered phenols antioxidant as helper component, produce cooperative effect with ultra-violet absorber, further improve UVResistant effect.The polyester slice of preparation through pre-crystallized, dry, by accurate control spinning condition, control is fallen without silk noil viscosity, thus control fibrous fracture intensity, generation ANTIPILLING effect spins various polyester fibers with complex function.
The present invention will be further described in detail below in conjunction with specific embodiment, but the present invention is not limited to following examples.
In following examples, adopt all that the pH value is 4～5, (solvent is ethylene glycol to the seasoning 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 seasoning 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 is comprised of by weight 1: 3 Irganox 1076 and Irganox 1010.
In addition, for adapting to different spinning process requirements, short fiber grade polyester chip inherent viscosity is controlled to be 0.730 ± 0.012; 243 ± 1 ℃ of fusing points; 69 ± 1 ℃ of vitrification points; Long fine grade polyester chip inherent viscosity is controlled to be 0.710 ± 0.012; 246 ± 1 ℃ of fusing points; 72 ± 1 ℃ of vitrification points.
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), esterification reaction section: get 18kg p-phthalic acid (PTA), 70 liters of polyester experimental provisions of 7.5kg ethylene glycol (EG) adding, after stirring, begin 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 is finished; at first add ethylene glycol; making temperature of reaction kettle be down to 230～235 ℃, then is that 2500 polyethylene glycol adds reactor with the 450g number-average molecular weight that heating and melting is good under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned seasoning liquid form, add the above-mentioned composite antioxidant of 3.375g with above-mentioned seasoning liquid form.Add and stir after complete.Reactor begins to heat up, and slowly to add the 160g hydroxyl value be 5.5% hydroxy silicon oil, carries out the secondary esterification, reaches 260 to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification is finished, and esterification column backs down the cooling of beginning.
(3), polymerisation operation: in system; add polymerization catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of control temperature; open vavuum pump, slowly be down to 2Kpa in 40 minutes, the low vacuum polymerisation finishes; close vacuum system, under nitrogen protection and negative pressure condition, incite somebody to action the 226g ultra-violet absorber that melting is good
234, by the special equipment injected system, mix after 3 minutes, good 226g antistatic additive 102 injected systems will be melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization filter filters, open high vacuum, and pressure is 40～100pa, under 270 ℃～280 ℃ conditions, carry out conventional polymerization, to reaching regulation viscosity, stop polymerisation, discharging pelletizing after polymerisation is finished, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, its test result sees 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), esterification reaction section: get 18kg p-phthalic acid (PTA), 70 liters of polyester experimental provisions of 7.5kg ethylene glycol (EG) adding, after stirring, begin 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 is finished; at first add ethylene glycol; making temperature of reaction kettle be down to 230～235 ℃, then is that 2500 polyethylene glycol adds reactor with the 450g number-average molecular weight that heating and melting is good under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned seasoning liquid form, add the above-mentioned composite antioxidant of 3.375g with above-mentioned seasoning liquid form.Add and stir after complete.Reactor begins to heat up, and slowly to add the 120g hydroxyl value be 5.5% hydroxy silicon oil, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification is finished, and esterification column backs down the cooling of beginning.
(3), polymerisation operation: in system; add polymerization catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of control temperature; open vavuum pump, slowly be down to 2Kpa in 40 minutes, the low vacuum polymerisation finishes; close vacuum system, under nitrogen protection and negative pressure condition, incite somebody to action the 113g ultra-violet absorber that melting is good
234, by the special equipment injected system, mix after 3 minutes, good 339g antistatic additive 103 injected systems will be melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization filter filters, open high vacuum, and pressure is 40～100pa, under 270 ℃～280 ℃ conditions, carry out conventional polymerization, to reaching regulation viscosity, stop polymerisation, discharging pelletizing after polymerisation is finished, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, its test result sees 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), esterification reaction section: get 18kg p-phthalic acid (PTA), 70 liters of polyester experimental provisions of 7.5kg ethylene glycol (EG) adding, after stirring, begin 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 is finished; at first add ethylene glycol; making temperature of reaction kettle be down to 230～235 ℃, then is that 3000 polyethylene glycol adds reactor with the 450g number-average molecular weight that heating and melting is good under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned seasoning liquid form, add the above-mentioned composite antioxidant of 3.375g with above-mentioned seasoning liquid form.Add and stir after complete.Reactor begins to heat up, and slowly to add the 160g hydroxyl value be 5.5% hydroxy silicon oil, carries out the secondary esterification, reaches 260 to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification is finished, and esterification column backs down the cooling of beginning.
(3), polymerisation operation: in system; add polymerization catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of control temperature; open vavuum pump, slowly be down to 2Kpa in 40 minutes, the low vacuum polymerisation finishes; close vacuum system, under nitrogen protection and negative pressure condition, incite somebody to action the 113g ultra-violet absorber that melting is good
320, by the special equipment injected system, mix after 3 minutes, good 226g antistatic additive 102 injected systems will be melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization filter filters, open high vacuum, and pressure is 40～100pa, under 270 ℃～280 ℃ conditions, carry out conventional polymerization, to reaching regulation viscosity, stop polymerisation, discharging pelletizing after polymerisation is finished, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, its test result sees 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), esterification reaction section: get 18kg p-phthalic acid (PTA), 70 liters of polyester experimental provisions of 7.5kg ethylene glycol (EG) adding, after stirring, beginning heats up and be forced into 0.3Mpa. carries 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 is finished; at first add ethylene glycol; making temperature of reaction kettle be down to 230～235 ℃, then is that 3000 polyethylene glycol adds reactor with the 450g number-average molecular weight that heating and melting is good under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned seasoning liquid form, add the above-mentioned composite antioxidant of 3.375g with above-mentioned seasoning liquid form.Add and stir after complete.Reactor begins to heat up, and slowly to add the 120g hydroxyl value be 5.5% hydroxy silicon oil, carries out the secondary esterification, reaches 260 to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification is finished, and esterification column backs down the cooling of beginning.
(3), polymerisation operation: in system; add polymerization catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of control temperature; open vavuum pump, slowly be down to 2Kpa in 40 minutes, the low vacuum polymerisation finishes; close vacuum system, under nitrogen protection and negative pressure condition, incite somebody to action the 226g ultra-violet absorber that melting is good
320, by the special equipment injected system, mix after 3 minutes, good 339g antistatic additive 103 injected systems will be melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization filter filters, open high vacuum, and pressure is 40～100pa, under 270 ℃～280 ℃ conditions, carry out conventional polymerization, to reaching regulation viscosity, stop polymerisation, discharging pelletizing after polymerisation is finished, obtain uvioresistant, antistatic, anti-pilling polyester section 22.5kg, its test result sees 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), esterification reaction section: get 18kg p-phthalic acid (PTA), 70 liters of polyester experimental provisions of 7.5kg ethylene glycol (EG) adding, after stirring, begin 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 is finished; at first add ethylene glycol; making temperature of reaction kettle be down to 230～235 ℃, then is that 4000 polyethylene glycol adds reactor with the 450g number-average molecular weight that heating and melting is good under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned seasoning liquid form, add the above-mentioned composite antioxidant of 3.375g with above-mentioned seasoning liquid form.Add and stir after complete.Reactor begins to heat up, and slowly to add the 160g hydroxyl value be 5.5% hydroxy silicon oil, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification is finished, and esterification column backs down the cooling of beginning.
(3), polymerisation operation: in system; add polymerization catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of control temperature; open vavuum pump, slowly be down to 2Kpa in 40 minutes, the low vacuum polymerisation finishes; close vacuum system, general's 113g ultra-violet absorber that melting is good under nitrogen protection and negative pressure condition (
234 with
320 mixture, the ratio of the two weight is 1: 1), by the special equipment injected system, mix after 3 minutes, good 226g antistatic additive 102 injected systems will be melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization filter filters, open high vacuum, pressure is 40～100pa, carries out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polymerisation, discharging pelletizing after polymerisation is finished obtains uvioresistant, antistatic, anti-pilling polyester section 22.5kg, and its test result sees 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), esterification reaction section: get 18kg p-phthalic acid (PTA), 70 liters of polyester experimental provisions of 7.5kg ethylene glycol (EG) adding, after stirring, begin 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 is finished; at first add ethylene glycol; making temperature of reaction kettle be down to 230～235 ℃, then is that 4000 polyethylene glycol adds reactor with the 450g number-average molecular weight that heating and melting is good under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned seasoning liquid form, add the above-mentioned composite antioxidant of 3.375g with above-mentioned seasoning liquid form.Add and stir after complete.Reactor begins to heat up, and slowly to add the 120g hydroxyl value be 5.5% hydroxy silicon oil, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification is finished, and esterification column backs down the cooling of beginning.
(3), polymerisation operation: in system; add polymerization catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of control temperature; open vavuum pump, slowly be down to 2Kpa in 40 minutes, the low vacuum polymerisation finishes; close vacuum system, general's 226g ultra-violet absorber that melting is good under nitrogen protection and negative pressure condition (
234 with
320 mixture, the ratio of the two weight is 1: 1), by the special equipment injected system, mix after 3 minutes, good 339g antistatic additive 103 injected systems will be melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization filter filters, open high vacuum, pressure is 40～100pa, carries out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polymerisation, discharging pelletizing after polymerisation is finished obtains uvioresistant, antistatic, anti-pilling polyester section 22.5kg, and its test result sees 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), esterification reaction section: get 18kg p-phthalic acid (PTA), 70 liters of polyester experimental provisions of 7.5kg ethylene glycol (EG) adding, after stirring, beginning heats up and be forced into 0.3Mpa. carries 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 is finished; at first add ethylene glycol; making temperature of reaction kettle be down to 230～235 ℃, then is that 2000 polyethylene glycol adds reactor with the 450g number-average molecular weight that heating and melting is good under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned seasoning liquid form, add the above-mentioned composite antioxidant of 3.375g with above-mentioned seasoning liquid form.Add and stir after complete.Reactor begins to heat up, and slowly to add the 180g hydroxyl value be 5.5% hydroxy silicon oil, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification is finished, and esterification column backs down the cooling of beginning.
(3), polymerisation operation: in system; add polymerization catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of control temperature; open vavuum pump, slowly be down to 2Kpa in 40 minutes, the low vacuum polymerisation finishes; close vacuum system, under nitrogen protection and negative pressure condition, incite somebody to action the 113g ultra-violet absorber (ultra-violet absorber that melting is good
234 with the mixture of the special ultra-violet absorber CYASORB of cyanogen UV-3638F, the ratio of the two weight is 2: 1), by the special equipment injected system, mix after 3 minutes, good 275g antistatic additive (being comprised of by weight 1: 1 antistatic additive 103 and antistatic additive 102) injected system will be melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization filter filters, open high vacuum, pressure is 40～100pa, carries out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polymerisation, the discharging pelletizing obtained uvioresistant after polymerisation was finished, antistatic, anti-pilling polyester section 22.5kg, its test result sees 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), esterification reaction section: get 18kg p-phthalic acid (PTA), 70 liters of polyester experimental provisions of 7.5kg ethylene glycol (EG) adding, after stirring, begin 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 is finished; at first add ethylene glycol; making temperature of reaction kettle be down to 230～235 ℃, then is that 2000 polyethylene glycol adds reactor with the 450g number-average molecular weight that heating and melting is good under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned seasoning liquid form, add the above-mentioned composite antioxidant of 3.375g with above-mentioned seasoning liquid form.Add and stir after complete.Reactor begins to heat up, and slowly to add the 140g hydroxyl value be 5.5% hydroxy silicon oil, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification is finished, and esterification column backs down the cooling of beginning.
(3), polymerisation operation: in system; add polymerization catalyst; deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of control temperature; open vavuum pump, slowly be down to 2Kpa in 40 minutes, the low vacuum polymerisation finishes; close vacuum system, under nitrogen protection and negative pressure condition, incite somebody to action the 113g ultra-violet absorber (ultra-violet absorber that melting is good
234 with the mixture of the special ultra-violet absorber CYASORB of cyanogen UV-3638F, the ratio of the two weight is 2: 1), by the special equipment injected system, mix after 3 minutes, good 275g antistatic additive (being comprised of by weight 1: 1 antistatic additive 103 and antistatic additive 102) injected system will be melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization filter filters, open high vacuum, pressure is 40～100pa, carries out conventional polymerization under 270 ℃～280 ℃ conditions, to reaching regulation viscosity, stop polymerisation, the discharging pelletizing obtained uvioresistant after polymerisation was finished, antistatic, anti-pilling polyester section 22.5kg, its test result sees Table 1.
Comparative Examples 1
This Comparative Examples provides a kind of preparation method of polyester slice, and it comprises the steps:
(1), esterification reaction section: get 18kg p-phthalic acid (PTA), 70 liters of polyester experimental provisions of 7.5kg ethylene glycol (EG) adding, after stirring, begin 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 is finished; at first add ethylene glycol; making temperature of reaction kettle be down to 230～235 ℃, then is that 2500 polyethylene glycol adds reactor with the 450g number-average molecular weight that heating and melting is good under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned seasoning liquid form, add the above-mentioned composite antioxidant of 3.375g with above-mentioned seasoning liquid form.Add and stir after complete.Reactor begins to heat up, and slowly to add the 160g hydroxyl value be 5.5% hydroxy silicon oil, carries out the secondary esterification, reaches 260 ℃ to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification is finished, and esterification column backs down the cooling of beginning.
(3), polymerisation operation: add polymerization catalyst, with 113g ultra-violet absorber liquid or that melting is good
234 add, mix after 3 minutes, good 226g antistatic additive 102 injected systems will be melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization filter filters, 260～275 ℃ of control temperature, open vavuum pump, slowly be down to 2Kpa in 40 minutes, the low vacuum polymerisation finishes, open high vacuum, pressure is 40～100pa, carries out conventional polymerization under 270～280 ℃ of conditions, to reaching regulation viscosity, stop polymerisation, discharging pelletizing after polymerisation is finished obtains polyester slice 22.5kg, and its test result sees Table 1.
Comparative Examples 2
This Comparative Examples provides a kind of preparation method of polyester slice, and it comprises the steps:
(1), esterification reaction section: get 18kg p-phthalic acid (PTA), 70 liters of polyester experimental provisions of 7.5kg ethylene glycol (EG) adding, after stirring, begin 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 is finished; at first add ethylene glycol; making temperature of reaction kettle be down to 230～235 ℃, then is that 3000 polyethylene glycol adds reactor with the 450g number-average molecular weight that heating and melting is good under nitrogen protection, stirs.Then add the 1.125g composite light stabilizer with above-mentioned seasoning liquid form, add the above-mentioned composite antioxidant of 3.375g with above-mentioned seasoning liquid form.Add and stir after complete.Reactor begins to heat up, and slowly to add the 120g hydroxyl value be 5.5% hydroxy silicon oil, carries out the secondary esterification, reaches 260 to temperature of reaction kettle.The water outlet of hydroxy silicon oil secondary esterification is finished, and esterification column backs down the cooling of beginning.
(3), polymerisation operation: add polymerization catalyst, with 113g ultra-violet absorber (ultra-violet absorber liquid or that melting is good
234 with the mixture of the special ultra-violet absorber CYASORBUV-3638F of cyanogen, the ratio of the two weight is 2: 1), by the special equipment injected system, mix after 3 minutes, good 226g antistatic additive 102 injected systems will be melted, continue to mix 2 minutes, the reactor pressurization, the pre-polymerization melt enters terminal polymerization kettle after the pre-polymerization filter filters.260～275 ℃ of control temperature, open vavuum pump, slowly be down to 2Kpa in 40 minutes, the low vacuum polymerisation finishes, open high vacuum, pressure is 40～100pa, carries out conventional polymerization under 270～280 ℃ of conditions, to reaching regulation viscosity, stop polymerisation, discharging pelletizing after polymerisation is finished obtains polyester slice 22.5kg, and its test result sees Table 1.
Table 1 uvioresistant, the physical and chemical index that antistatic, anti-pilling polyester is cut into slices
The quality index of the polyester slice by above-described embodiment and Comparative Examples can be found out, the polyester slice of method preparation 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 be short silk grade pet chip, embodiment 2,4,6,8 and Comparative Examples 2 be the long filament grade pet chip.And in the Comparative Examples 1,2, because ultra-violet absorber adds the change of mode, causing the on the one hand obvious flavescence of hue of chip, fusing point and vitrification point rising show that the part ultra-violet absorber takes system in the low vacuum stage out of with a large amount of evaporations of ethylene glycol.
Embodiment 9
The present embodiment relates to a kind of uvioresistant that has, antistatic, the preparation method of the high comfortable polyester fiber of ANTIPILLING, polyester fiber is staple fibre, the uvioresistant that makes with embodiment 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 ultra-violet absorber, antistatic additive, light stabilizer, antioxidant, the 3rd monomer, hydroxy silicon oil etc., its section vitrification point is lower, therefore must 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, 110 ℃～125 ℃ of pre-crystallized temperature controls, time are 3～5 hours.Then carry out drying, 130 ℃～145 ℃ of baking temperatures, the time is 3.5～5.0 hours.Carry out spinning after finishing drying.Use the odd-shaped cross section spinneretss such as three leaves, cross, five leaves.At first produce through reeling at the short fiber spinning production line, 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 polyester fiber, screw rod is respectively distinguished 8～15 ℃ of temperature downward modulations), then, the short fiber tow is through falling barrel balance after 24 hours, then boundling stretches, steam heat setting process, draft temperature are 142 ℃～150 ℃, 110 ℃～135 ℃ of heat setting temperatures, then behind 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 is 0.93 * 10
10Ω .cm.This fiber is made into knitting and woven fabric through spinning, 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 sees Table 2.
Embodiment 10
The present embodiment relates to the preparation method of a kind of uvioresistant, antistatic, the high comfortable polyester fiber of ANTIPILLING, polyester fiber is long filament, its process is: at first embodiment 2 prepared polyester slices are carried out pre-crystallizedly, 110 ℃～125 ℃ of pre-crystallized temperature controls, time are 3～5 hours.Then carry out drying, 130 ℃～145 ℃ of baking temperatures, the time is 3.5～5.0 hours.Carry out spinning after finishing drying.Use the odd-shaped cross section spinneretss 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, according to the fusing point of copolyester section, spinning and condition are adjusted, the condition of implementing spinning compares the common PET polyester fiber, and screw rod is respectively distinguished 8～15 ℃ of temperature downward modulations.), POY fibre spinning speed 2750m/min.The POY fiber of spinning stretches and texturing craft through corresponding through after 24 hours balances again, and draft temperature is 142 ℃～150 ℃, prepares corresponding drawing and setting temperature and also will reduce.The preparation specification is the low stretch network product that 55.5dtex/36f has the hydroscopic fast-drying function, and its fiber volume fraction resistance is 0.98 * 10
10Ω .cm.Fiber quality is good, and fiber is through the knitting and woven fabric of making, and after tested, the fabric performance index sees Table 2.
Embodiment 11
The present embodiment relates to the preparation method of a kind of uvioresistant, antistatic, the high comfortable polyester staple fiber of ANTIPILLING, and substantially with embodiment 9, different is that its polyester slice that adopts embodiment 3 is raw material.
Embodiment 12
The present embodiment relates to the preparation method of a kind of uvioresistant, antistatic, the high comfortable polyester filament of ANTIPILLING, and substantially with embodiment 10, different is that its section of adopting embodiment 4 is raw material.
Embodiment 13
The present embodiment relates to the preparation method of a kind of uvioresistant, antistatic, the high comfortable polyester staple fiber of ANTIPILLING, and substantially with embodiment 9, different is that its polyester slice that adopts embodiment 5 is raw material.
Embodiment 14
The present embodiment relates to the preparation method of a kind of uvioresistant, antistatic, the high comfortable polyester filament of ANTIPILLING, and substantially with embodiment 10, different is that its section of adopting embodiment 6 is raw material.
Embodiment 15
The present embodiment relates to the preparation method of a kind of uvioresistant, antistatic, the high comfortable polyester staple fiber of ANTIPILLING, and substantially with embodiment 9, different is that its polyester slice that adopts embodiment 7 is raw material.
Embodiment 16
The present embodiment relates to the preparation method of a kind of uvioresistant, antistatic, the high comfortable polyester filament of ANTIPILLING, and substantially with embodiment 10, different is that its section of adopting embodiment 8 is raw material.
Comparative Examples 3
This Comparative Examples provides the preparation method of a kind of uvioresistant, antistatic, the high comfortable polyester staple fiber of ANTIPILLING, and substantially with embodiment 9, different is that its section of adopting Comparative Examples 1 is raw material.
Comparative Examples 4
This Comparative Examples provides the preparation method of a kind of uvioresistant, antistatic, the high comfortable polyester filament of ANTIPILLING, basic embodiment 10, and different is that its section of adopting Comparative Examples 2 is raw material.
Table 2 has the polyester fiber fabric performance of uvioresistant, antistatic, anti-pilling composite function
Above-mentioned fabric is mainly spring, summer, autumn Fashion Design, therefore, except having good uvioresistant, antistatic, ANTIPILLING function, the physicochemical characteristics that the present invention is special according to this polyester, three leaves of spinning or odd-shaped cross section 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, ANTIPILLING, 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, measure wicking height 〉=120mm, evaporation rate 〉=0.20g/hr.
Above the present invention has been done detailed description, the equivalence that all Spirit Essences 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 with polyester fiber of uvioresistant, antistatic, anti-pilling composite function comprises the esterification operation, polymerisation operation and the spinning process that carry 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 (TPA), ethylene glycol are joined in the 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 is finished, add ethylene glycol, make system be cooled to 230 ℃～235 ℃, under inert gas shielding, add number-average molecular weight and be 600～6000 polyethylene glycol as the 3rd monomer, the addition of the 3rd monomer is 1.0%～6.5% of polyester slice weight, then add mass concentration and be the seasoning liquid of 2%～5% hindered amine light stabilizer and mass concentration and be the seasoning liquid of 2%～5% Hinered phenols antioxidant, take polyester slice weight as benchmark, the addition of described hindered amine light stabilizer and Hinered phenols antioxidant is respectively 10～300ppm, the seasoning liquid of described hindered amine light stabilizer be hindered amine light stabilizer be dispersed in the solvent ethylene glycol and add acetic acid after gained pH value be 4～5 solution, the seasoning liquid of described Hinered phenols antioxidant be Hinered phenols antioxidant be dispersed in the solvent ethylene glycol and add acetic acid after gained pH value be 4～5 solution, add and stir after complete, reactor begins to heat up, slowly the adding hydroxyl value is 0.5%～8.0% hydroxy silicon oil, carry out the secondary esterification, finish to the esterification water outlet, temperature of reaction kettle reaches 260 ℃, and the addition of wherein said hydroxy silicon oil is 0.1%～1.2% of polyester slice weight;
Described polymerisation operation is implemented as follows: in the system after the secondary esterification, add polymerization catalyst, after stirring, deliver in the 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 ultra-violet absorber of liquid state or melting is injected, stir, then the antistatic additive that melting is good is injected; stir; deliver to terminal polymerization kettle after being filtered, wherein, described ultra-violet absorber is one or more the combination in the ultra-violet 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 ultra-violet absorber CYASORB of cyanogen UV-3638F, triazine series ultra-violet absorber UV-1577, the addition of ultra-violet absorber is 0.15%～1.10% of polyester slice weight, the addition of described antistatic additive is 0.5%～4.5% of polyester slice weight; At last, in terminal polymerization kettle, carry out the final polymerization reaction under 270 ℃～285 ℃ of temperature, the pressure 40～100Pa, after the final polymerization reaction was finished, the discharging pelletizing got uvioresistant, antistatic, anti-pilling polyester section;
Described preparation method also is included in before the spinning process, pre-crystallized and dry step is successively carried out in described uvioresistant, the section of antistatic, anti-pilling polyester, described pre-crystallizedly carried out 3～5 hours under 110 ℃～125 ℃ of temperature, described drying was carried out 3.5～5.0 hours under 130 ℃～145 ℃ of temperature.
2. the preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function according to claim 1, it is characterized in that: described antistatic additive is one or more the combination in antistatic additive 102, antistatic additive 103, antistatic additive 105 and the antistatic additive 308, and its addition is 0.65%～2.5% of described polyester slice weight.
3. the preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function according to claim 1, 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
119FL, 770 pairs (2 of polymerized hindered amine light stabilizer Chimassorb944, Tinuvin788 and light stabilizers, 2,6,6-tetramethyl-4-piperidyl) one or more in the sebacate, take polyester slice weight as benchmark, the addition of described hindered amine light stabilizer is 15～90ppm.
4. the preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function according to claim 1, it is characterized in that: described Hinered phenols antioxidant is Irganox1076, among the Irganox1010 one or more, take polyester slice weight as benchmark, the addition of described Hinered phenols antioxidant is 30～250ppm.
5. the preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function according to claim 1, it is characterized in that: take polyester slice weight as benchmark, the addition of described hindered amine light stabilizer is 35～60ppm, and the addition of described Hinered phenols antioxidant is 75～180ppm.
6. the preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function according to claim 1, it is characterized in that: described hindered amine light stabilizer is the composite light stabilizer that the light stabilizer more than two kinds mixes; Described Hinered phenols antioxidant is the composite antioxidant that the antioxidant more than two kinds mixes.
7. the preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function according to claim 1, it is characterized in that: the number-average molecular weight of described polyethylene glycol as the 3rd monomer is 1500～4000, and addition is 1.5%～4.0% of polyester slice weight.
8. the described preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function of each claim in 7 according to claim 1, it is characterized in that: when described polyester fiber was long filament, the addition of described hydroxy silicon oil was 0.1%～0.8% of polyester slice weight; When described polyester fiber was staple fibre, the addition of described hydroxy silicon oil was 0.6%～1.2% of polyester slice weight.
9. the described preparation method with polyester fiber of uvioresistant, antistatic, anti-pilling composite function of each claim in 7 according to claim 1, it is characterized in that: described spinning process comprises the spinning of carrying out successively, reel, stretch and the HEAT SETTING step, wherein, spinning temperature is 255 ℃～278 ℃, and draft temperature is 142 ℃～150 ℃, and heat setting temperature is 110 ℃～135 ℃.
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| CN102926023B (en) * | 2012-11-16 | 2014-07-23 | 东华大学 | Preparation method of antistatic hydrophilic polyester fiber |
| CN104294395B (en) * | 2013-07-17 | 2016-04-20 | 福建百宏聚纤科技实业有限公司 | The processing method of the ventilative ANTIPILLING hygroscopic fibre of high anti-UV height |
| CN103409834A (en) * | 2013-07-25 | 2013-11-27 | 安徽东锦化纤科技有限公司 | Differentiated polyester fiber preparation method |
| CN103467717B (en) * | 2013-09-27 | 2015-12-02 | 苏州大学 | A kind of copolyesters melt and preparation method thereof |
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