CN102408555A - 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 Ginkgo Biloba Leaf Extract, 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 with various natural fibers and also exists many deficiencies: feel is hardened, water absorbability is poor, anti-ultraviolet property is poor, be prone to produce static, be prone to balling-up, be difficult to dyeing etc.Though natural fiber has good dyeing behavior, lining like cotton, real silk, hair, fiber crops etc. and has ventilation property, the absorbing sweat performance of keeping humidity is good, no static, the characteristics that comfortableness is good exist to be prone to wrinkle, to lead deficiencies such as wet and rapid-drying properties difference.
Along with the progressively expansion of trevira range of application, from the seventies in last century, developed country is to the above-mentioned deficiency of trevira; Plurality of advantages with natural fiber is a target; Aspect the wearing comfort of fiber, start with from three aspects, improve the wear behavior of trevira.On the one hand: through 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 through composite spinning technology, make polyester fabric obtain rapid progress in function aspects such as flexibility, elasticity, emulation silks; On the other hand: through the co-blended spinning of different components, produce various fiber species, also can give lining brand-new function through the back arrangement of lining with specific function with the physical blending mode; The third aspect: through copolyreaction, improve this body structure of polyester macromolecule chain, through introducing the copolymerization component group to improve trevira lining performance, permanently give fiber various properties.At present, comprise fire-retardant, cation-dyeable, highly shrink, a series of functional polyalkylene ester fibers such as dispersed dye are prone to dye, antistatic, Ginkgo Biloba Leaf Extract, far infrared thermal insulation that trevira and lining 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 fiber production; But in the development and application field of functional polyalkylene ester fiber, China also is in the starting stage at present, is limited to the exploitation of single functional polyester and fiber at present more; Like 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; This method at first prepares the suspension-s of anti ultraviolet agent midbody zinc subcarbonate terepthaloyl moietie; Then before the PET polyester synthetic esterification stage finishes back, rough vacuum polymerization; The suspension-s of anti ultraviolet agent midbody zinc subcarbonate terepthaloyl moietie is added, and when polyreaction generated polyester, zinc subcarbonate decomposed generation zinc oxide; Obtain Ginkgo Biloba Leaf Extract zinc oxide complex polyester, wherein zinc oxide content is 0.1%～5% of a PET Resin/Poyester Chips Bottle Grade weight.In this method gained polyester, zinc oxide can keep less granularity, strengthens thereby absorb ultraviolet performance.Yet this method is decomposed in order to make 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 influence vacuum tightness and cause section to contain great 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 that does not decompose fully will continue to decompose in spinning process; The fiber spinnability variation, breaking tenacity 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 made up of agent of inorganic anti ultraviolet shielding and organic uv absorbers; The composition of inorganic anti ultraviolet shielding 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 agent of inorganic anti ultraviolet shielding and organic uv absorbers is 1: 1, takes by weighing this compound anti ultraviolet agent and terepthaloyl moietie and is made into slurries, places ball mill to disperse then 0.5-1 hour; (2), the esterification operation: fused terephthalic acid and terepthaloyl moietie, continuously or the intermittent entry esterifying kettle,, carry out esterification under the pressure 0.3Mpa 160～220 ℃ of temperature, water byproduct to be steamed reaches 90% o'clock of theoretical amount, 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 terephthalic acid 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 earlier 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 polymerization degree, the terepthaloyl moietie of generation reclaims behind condensing surface; (4) after condensation reaction finished, material made the uvioresistant polyester section through Cast Strip, cooling, pelletizing, drying.The deficiency of this method is: benzotriazole is an organic phenolic compound, exists as the protonic 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-polymerization process.In addition, because inorganic nanometer powder in polymerization process, continues 4～6 hours time under hot conditions; Nanoparticle generation agglomeration is obvious, and under low temperature ultra-dispersed condition, the inorganic nano ion is to make light when passing lining, produce strong diffuse scattering effect with huge specific surface 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; Diffuse scattering effect to light significantly reduces, and in addition, this 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 through master batch method spinning uvioresistant fiber.Notification number is that the Chinese invention patent of CN1300246C discloses the method that a kind of original position generation nano titanium oxide prepares uvioresistant polyester, though terepthaloyl moietie salt of its preparation titanium carries out surface treatment through organic agent or silane coupling agent, titanium ethylene glycolate is as polymerizing catalyst; The PET polyreaction had strong katalysis and side reaction Degradation; Be prone to cause PET section hue difference, MWD wide, in addition, in-situ hydrolysis generates Nano titanium dioxide in the polymerization process; The water molecules of the decomposition in polymerization later stage generation has a strong impact on polyreaction on the one hand; On the other hand, the Nano titanium dioxide that this method is processed is good organic matter of sewage decompose material, and section is after long-time solar radiation; Viscosity degradation produces and decomposes.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 Ginkgo Biloba Leaf Extract 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 Ginkgo Biloba Leaf Extract matrix material and preparation method thereof, use be to be ultraviolet scattering material with the inorganic nano ultraviolet ray-resistant material, produce certain Ginkgo Biloba Leaf Extract effect.
To sum up; Prior art mainly all is that the huge specific surface area that relies on inorganic nanometer powder to have produces diffuse scattering generation Ginkgo Biloba Leaf Extract effect for basic to ultraviolet ray; The stability of its uvioresistant effect and efficient remain to be improved; This just need start with from Ginkgo Biloba Leaf Extract mechanism, the polyester that preparation has more excellent uvioresistant effect and has good spinnability.In addition, also need exploitation badly when having anti-ultraviolet function, also have other function for example resistance to deterioration, absorbing fast-drying property concurrently, static resistance, the complex function polyester of anti-pilling.
Summary of the invention
Technical problem to be solved by this invention provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, the section of antistatic, anti-pilling polyester.
For solving above technical problem, the present invention takes following technical scheme:
The preparation method of a kind of Ginkgo Biloba Leaf Extract, the section of antistatic, anti-pilling polyester comprises the esterification operation and the polyreaction operation of carrying out successively, wherein:
Said esterification operation comprises esterification reaction section and secondary esterification reaction section; Wherein: a said esterification reaction section is implemented as follows: terephthalic acid, terepthaloyl moietie 1: 1.2 in molar ratio～1.3 is joined in the reaction kettle of the esterification, under 250 ℃～265 ℃, carry out one time esterification; Said secondary esterification reaction section is implemented as follows: after one time esterification reaction section is accomplished; Add terepthaloyl moietie, make system be cooled to 230 ℃～235 ℃, under protection of inert gas; Add number-average molecular weight and be 600～6000 polyoxyethylene glycol as the 3rd monomer; The 3rd monomeric add-on is 1.0%～6.5% of a PET Resin/Poyester Chips Bottle Grade weight, and mixed liquid and the mass concentration that adds mass concentration then and be 2%～5% hindered amine light stabilizer is the mixed liquid of 2%～5% Hinered phenols antioxidant, is benchmark with PET Resin/Poyester Chips Bottle Grade weight; The add-on of said 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 the solvent ethylene glycol and add acetic acid after gained pH value be 4～5 solution, the mixed 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 finishing; Reaction kettle begins to heat up; Slowly add hydroxyl value and be 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 add-on of wherein said hydroxy silicon oil is 0.1%～1.2% of a PET Resin/Poyester Chips Bottle Grade weight;
Said polyreaction operation is implemented as follows: in the system after the secondary esterification, add polymerizing 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; Prepolymerization reaction is closed vacuum system, under nitrogen protection and negative pressure after finishing; Liquid state or fused UV light absorber are injected, stirred, then the static inhibitor that fusion is good is injected; Stir, after strainer filters, deliver to terminal polymerization kettle, wherein; The add-on of said UV light absorber is 0.1%～2.0% of a PET Resin/Poyester Chips Bottle Grade weight, and the add-on of said static inhibitor is 0.5%～4.5% of a PET Resin/Poyester Chips Bottle Grade 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 accomplished, the discharging pelletizing got Ginkgo Biloba Leaf Extract, 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 category UV light absorber:
326,
234,
350,
320,
328; Low volatility benzotriazole category UV light absorber
360; Red shift benzotriazole category UV light absorber
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 a PET Resin/Poyester Chips Bottle Grade weight.Preferably, select one or more compound uses of following UV light absorber: benzotriazole category series UV light absorber:
234,
320,
328; Low volatility benzotriazole category UV light absorber
360; Red shift benzotriazole category UV light absorber
327; And
UV-P; The special UV light absorber CYASORB of cyanogen UV-3638F, triazine series UV light absorber UV-1577 etc.Preferred especially, 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 and 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 the static inhibitor 308, and its add-on is preferably 0.65%～2.5% of PET Resin/Poyester Chips Bottle Grade weight.
According to the present invention; Described hindered amine light stabilizer can be for being selected from non-aggretion 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 the sebate; Being preferably the composite light stabilizer that photostabilizer mixes more than two kinds, for example is Tinuvin 788 and the mixture of
119FL by weight 1: 1.The add-on of described hindered amine light stabilizer is preferably 15～90ppm (is benchmark with the polyester gross weight).Described Hinered phenols antioxidant can be Irganox 1076; Among Irganox 1010 and the Irgafos168 one or more; 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 (is benchmark with the polyester gross weight).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 that known various polyester is used polymerizing catalyst.Particularly in the present invention, polymerizing catalyst uses antimony glycol, and its add-on is generally 450～550ppm (weight with PET Resin/Poyester Chips Bottle Grade is benchmark).
According to the present invention, described number-average molecular weight as the 3rd monomeric polyoxyethylene glycol is preferably 1500～4000, and add-on is preferably 1.5%～4.0% of PET Resin/Poyester Chips Bottle Grade weight.
When the fiber of preparation was staple fibre, the add-on of hydroxy silicon oil was preferably 0.6%～1.2% of PET Resin/Poyester Chips Bottle Grade weight.When the trevira of preparation was long filament, the add-on of hydroxy silicon oil was preferably 0.1%～0.8% of PET Resin/Poyester Chips Bottle Grade weight.The effect of hydroxy silicon oil is hydroxyl in its two ends on the one hand, participates in polyreaction as comonomer, because the hydroxy silicon oil reaction activity is low; Polyreaction is rapid, helps quickening polymerization rate, and; Since its with carboxylic acid reaction after bonding belong to weak bond, the easy fracture that in spinning process, is heated can make the even and bigger viscosity drop of polyester fondant generation; Add-on and spinning condition through the control hydroxy silicon oil; Can prepare the PET Resin/Poyester Chips Bottle Grade of suitable staple fibre or long filament production characteristics and staple fibre and the long filament that different breaking tenacity requires respectively, the final polyester viscosity controller of its middle short fiber is about 0.58 ± 0.012, and the final viscosity of long filament is controlled at about 0.63 ± 0.012; Effectively reduce fibre strength, thereby make fiber have good anti-pilling property.
In particular, short silk level Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section, the usage quantity of hydroxy silicon oil is wanted the high comfortable PET Resin/Poyester Chips Bottle Grade of a little higher than long filament level 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 destruction of fiber under the condition of high temperature in winding process, in stretching and heat setting type process, the contact high-temperature steam; The estersil bonding further ruptures in the macromolecular chain, 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, satisfying processing and taking intensity simultaneously, give fiber good anti-pilling property.
Long filament level Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section; The usage quantity of hydroxy silicon oil is lower than the high comfortable copolyester section of staple fibre level slightly in the polymerization process; But the 3rd monomer polyoxyethylene glycol that adds relative higher amount; So that in spinning process, for once under the situation of viscosity drop, effectively reduce the breaking tenacity of fiber.Its fiber final response viscosity is: 0.63 ± 0.012, and the fibre breakage intensity control exists: 2.6 ± 0.2, satisfying processing and taking intensity simultaneously, give fiber good anti-pilling property.
Because the utilization of technique scheme, the present invention compared with prior art has following advantage:
1, the present invention is main with UV light absorber; Be converted into of the injury of the light minimizing UV-light of other wavelength through absorbing ultraviolet ray to human body skin; Simultaneously; Through being used hindered amine light stabilizer and Hinered phenols antioxidant, with UV light absorber collaborative, further improved the fabric lining anti-ultraviolet property under the sunlight direct projection condition out of doors.
2, with after esterification, promptly to add anti ultraviolet agent different in the past; The present invention is after prepolymerization reaction is accomplished, and gathers eventually to add liquid or fused UV light absorber before reaction is carried out, 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 is accomplished 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, through add static inhibitor mid-term in polymerization; And use polyoxyethylene glycol as the 3rd monomer with good moisture absorption property, can keep obtaining good antistatic property on the fiber fundamental property basis; Especially be fit under spring, the autumn north dry climatic condition needs of clothes eliminostatic.The 3rd monomeric adding also is beneficial to and reduces fibre breakage intensity and the anti-pilling property that improves fiber.
4, can add the consumption and the control spinning condition of hydroxy silicon oil through control; 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 technology on the other hand; Can during spinning winding and drawing and setting, control the polyester viscosity drop, effectively reduce fibre strength, thereby make fiber have good anti-pilling property.
5, hindered amine light stabilizer and Hinered phenols antioxidant are dispersed in adding again in acetic acid and the terepthaloyl moietie earlier; Can (flash distillation can take place rapidly in acetic acid in the prepolymerization reaction process under the product quality premise not influencing; The discharge system); The hydroxy silicon oil that effectively suppresses hindered amine light stabilizer and Hinered phenols antioxidant and follow-up adding at high temperature react (it is the protonic acid with certain intensity that hydroxy silicon oil high temperature descends, and can at high temperature produce reaction with hindered amine light stabilizer and Hinered phenols antioxidant).
6, the fiber that is spun into gained PET Resin/Poyester Chips Bottle Grade of the present invention is the knitting and woven fabric of raw material, is uv transmittance≤5.0% through its correlation technique index of test, anti-pilling property>=4 grade, fiber volume fraction resistance≤10
10Ω .cm, Ginkgo Biloba Leaf Extract, anti, antistatic complex function is excellent.
Embodiment
The present invention relates to the preparation method of Ginkgo Biloba Leaf Extract, 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 adds a certain amount of UV light absorber that can in polyester, have a good dispersion and static inhibitor with acquisition ultraviolet-resistent property and antistatic property.Simultaneously, have good anti-pilling property, improve polymerization rate, before polymerization, add a certain amount of hydroxy silicon oil for guaranteeing fiber; 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 the uvioresistant effect.The PET Resin/Poyester Chips Bottle Grade of preparation is through in advance crystallization, drying, through accurate control spinning condition, and control does not have oil silk viscosity drop, thereby the controlling fiber breaking tenacity produces the anti effect, spins various trevira with complex function.
Below in conjunction with specific embodiment the present invention is done further detailed explanation, but the present invention is not limited to following examples.
In following examples; Adopt all that the pH value is 4～5, (solvent is a terepthaloyl moietie 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 a terepthaloyl moietie, and uses the vinegar acid for adjusting pH value) of the composite antioxidant of mass concentration 2%.Wherein, composite light stabilizer is made up of by weight 1: 1 Tinuvin 788 and
119FL; Composite antioxidant is made up of by weight 1: 3 Irganox 1076 and Irganox 1010.
In addition, for adapting to different spinning process requirements, short fiber grade polyester chip limiting viscosity is controlled to be 0.730 ± 0.012; 243 ± 1 ℃ of fusing points; 69 ± 1 ℃ of second-order transition temperatures; Long fine grade polyester chip limiting viscosity is controlled to be 0.710 ± 0.012; 246 ± 1 ℃ of fusing points; 72 ± 1 ℃ of second-order transition temperatures.
Embodiment 1
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1), esterification reaction section: get 18kg pure terephthalic acid (PTA), 70 liters of polyester experimental installations of 7.5kg terepthaloyl moietie (EG) adding; After stirring, begin to heat up and be forced into 0.3Mpa, carry out esterification; Esterification temperature is controlled at 250～265 ℃; Finish to the esterification water outlet, reply normal pressureization, finish reaction.
(2), secondary esterification reaction section: after an esterification is accomplished; At first add terepthaloyl moietie; Making temperature of reaction kettle reduce to 230～235 ℃, is polyoxyethylene glycol adding reaction kettle under nitrogen protection of 2500 then with the 450g number-average molecular weight that heating and melting is good, stirs.Add the 1.125g composite light stabilizer with above-mentioned mixed liquid form then, add the above-mentioned composite antioxidant of 3.375g with above-mentioned mixed liquid form.After finishing, adding stirs.Reaction kettle 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 accomplished, and esterification column backs down the beginning cooling.
(3), polyreaction operation: in system, add polymerizing catalyst, deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of controlled temperature, the open vacuum pump was slowly reduced to 2Kpa in 40 minutes; The rough vacuum polyreaction finishes, and closes vacuum system, under nitrogen protection and negative pressure condition, incites somebody to action the 226g UV light absorber
234 that fusion is good; By the specific equipment injected system, mix after 3 minutes, melting good 226g static inhibitor 102 injected systems; Continue to mix 2 minutes, the reaction kettle pressurization, the pre-polymerization melt gets into terminal polymerization kettle after the pre-polymerization strainer filters; Open high vacuum, pressure is 40～100pa, under 270 ℃～280 ℃ conditions, carries out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section 22.5kg, its test result is seen table 1.
Embodiment 2
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1), esterification reaction section: get 18kg pure terephthalic acid (PTA), 70 liters of polyester experimental installations of 7.5kg terepthaloyl moietie (EG) adding; After stirring, begin to heat up and be forced into 0.3Mpa, carry out esterification; Esterification temperature is controlled at 250～265 ℃; Finish to the esterification water outlet, reply normal pressureization, finish reaction.
(2), secondary esterification reaction section: after an esterification is accomplished; At first add terepthaloyl moietie; Making temperature of reaction kettle reduce to 230～235 ℃, is polyoxyethylene glycol adding reaction kettle under nitrogen protection of 2500 then with the 450g number-average molecular weight that heating and melting is good, stirs.Add the 1.125g composite light stabilizer with above-mentioned mixed liquid form then, add the above-mentioned composite antioxidant of 3.375g with above-mentioned mixed liquid form.After finishing, adding stirs.Reaction kettle 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 accomplished, and esterification column backs down the beginning cooling.
(3), polyreaction operation: in system, add polymerizing catalyst, deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of controlled temperature, the open vacuum pump was slowly reduced to 2Kpa in 40 minutes; The rough vacuum polyreaction finishes, and closes vacuum system, under nitrogen protection and negative pressure condition, incites somebody to action the 113g UV light absorber
234 that fusion is good; By the specific equipment injected system, mix after 3 minutes, melting good 339g static inhibitor 103 injected systems; Continue to mix 2 minutes, the reaction kettle pressurization, the pre-polymerization melt gets into terminal polymerization kettle after the pre-polymerization strainer filters; Open high vacuum, pressure is 40～100pa, under 270 ℃～280 ℃ conditions, carries out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section 22.5kg, its test result is seen table 1.
Embodiment 3
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1), esterification reaction section: get 18kg pure terephthalic acid (PTA), 70 liters of polyester experimental installations of 7.5kg terepthaloyl moietie (EG) adding; After stirring, begin to heat up and be forced into 0.3Mpa, carry out esterification; Esterification temperature is controlled at 250～265 ℃; Finish to the esterification water outlet, reply normal pressureization, finish reaction.
(2), secondary esterification reaction section: after an esterification is accomplished; At first add terepthaloyl moietie; Making temperature of reaction kettle reduce to 230～235 ℃, is polyoxyethylene glycol adding reaction kettle under nitrogen protection of 3000 then with the 450g number-average molecular weight that heating and melting is good, stirs.Add the 1.125g composite light stabilizer with above-mentioned mixed liquid form then, add the above-mentioned composite antioxidant of 3.375g with above-mentioned mixed liquid form.After finishing, adding stirs.Reaction kettle 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 accomplished, and esterification column backs down the beginning cooling.
(3), polyreaction operation: in system, add polymerizing catalyst, deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of controlled temperature, the open vacuum pump was slowly reduced to 2Kpa in 40 minutes; The rough vacuum polyreaction finishes, and closes vacuum system, under nitrogen protection and negative pressure condition, incites somebody to action the 113g UV light absorber
320 that fusion is good; By the specific equipment injected system, mix after 3 minutes, melting good 226g static inhibitor 102 injected systems; Continue to mix 2 minutes, the reaction kettle pressurization, the pre-polymerization melt gets into terminal polymerization kettle after the pre-polymerization strainer filters; Open high vacuum, pressure is 40～100pa, under 270 ℃～280 ℃ conditions, carries out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section 22.5kg, its test result is seen table 1.
Embodiment 4
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1), esterification reaction section: get 18kg pure terephthalic acid (PTA), 70 liters of polyester experimental installations of 7.5kg terepthaloyl moietie (EG) adding; After stirring; Beginning to heat up and being forced into 0.3Mpa. and carrying out esterification, esterification temperature is controlled at 250～265 ℃, finishes to the esterification water outlet; Reply normal pressureization, finish reaction.
(2), secondary esterification reaction section: after an esterification is accomplished; At first add terepthaloyl moietie; Making temperature of reaction kettle reduce to 230～235 ℃, is polyoxyethylene glycol adding reaction kettle under nitrogen protection of 3000 then with the 450g number-average molecular weight that heating and melting is good, stirs.Add the 1.125g composite light stabilizer with above-mentioned mixed liquid form then, add the above-mentioned composite antioxidant of 3.375g with above-mentioned mixed liquid form.After finishing, adding stirs.Reaction kettle 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 accomplished, and esterification column backs down the beginning cooling.
(3), polyreaction operation: in system, add polymerizing catalyst, deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of controlled temperature, the open vacuum pump was slowly reduced to 2Kpa in 40 minutes; The rough vacuum polyreaction finishes, and closes vacuum system, under nitrogen protection and negative pressure condition, incites somebody to action the 226g UV light absorber
320 that fusion is good; By the specific equipment injected system, mix after 3 minutes, melting good 339g static inhibitor 103 injected systems; Continue to mix 2 minutes, the reaction kettle pressurization, the pre-polymerization melt gets into terminal polymerization kettle after the pre-polymerization strainer filters; Open high vacuum, pressure is 40～100pa, under 270 ℃～280 ℃ conditions, carries out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section 22.5kg, its test result is seen table 1.
Embodiment 5
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1), esterification reaction section: get 18kg pure terephthalic acid (PTA), 70 liters of polyester experimental installations of 7.5kg terepthaloyl moietie (EG) adding; After stirring, begin to heat up and be forced into 0.3Mpa, carry out esterification; Esterification temperature is controlled at 250～265 ℃; Finish to the esterification water outlet, reply normal pressureization, finish reaction.
(2), secondary esterification reaction section: after an esterification is accomplished; At first add terepthaloyl moietie; Making temperature of reaction kettle reduce to 230～235 ℃, is polyoxyethylene glycol adding reaction kettle under nitrogen protection of 4000 then with the 450g number-average molecular weight that heating and melting is good, stirs.Add the 1.125g composite light stabilizer with above-mentioned mixed liquid form then, add the above-mentioned composite antioxidant of 3.375g with above-mentioned mixed liquid form.After finishing, adding stirs.Reaction kettle 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 accomplished, and esterification column backs down the beginning cooling.
(3), polyreaction operation: in system, add polymerizing catalyst, deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of controlled temperature, the open vacuum pump was slowly reduced to 2Kpa in 40 minutes; The rough vacuum polyreaction finishes, and closes vacuum system, under nitrogen protection and negative pressure condition, incites somebody to action the 113g UV light absorber that fusion the is good (mixture of
234 and
320; The ratio of the two weight is 1: 1), by the specific equipment injected system, mix after 3 minutes; With melting good 226g static inhibitor 102 injected systems; Continue to mix 2 minutes, the reaction kettle pressurization, the pre-polymerization melt gets into terminal polymerization kettle after the pre-polymerization strainer filters; Open high vacuum; Pressure is 40～100pa, under 270 ℃～280 ℃ conditions, carries out conventional polymerization, to reaching regulation viscosity; Stop polyreaction; Discharging pelletizing after polyreaction is accomplished obtains Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section 22.5kg, and its test result is seen table 1.
Embodiment 6
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1), esterification reaction section: get 18kg pure terephthalic acid (PTA), 70 liters of polyester experimental installations of 7.5kg terepthaloyl moietie (EG) adding; After stirring, begin to heat up and be forced into 0.3Mpa, carry out esterification; Esterification temperature is controlled at 250～265 ℃; Finish to the esterification water outlet, reply normal pressureization, finish reaction.
(2), secondary esterification reaction section: after an esterification is accomplished; At first add terepthaloyl moietie; Making temperature of reaction kettle reduce to 230～235 ℃, is polyoxyethylene glycol adding reaction kettle under nitrogen protection of 4000 then with the 450g number-average molecular weight that heating and melting is good, stirs.Add the 1.125g composite light stabilizer with above-mentioned mixed liquid form then, add the above-mentioned composite antioxidant of 3.375g with above-mentioned mixed liquid form.After finishing, adding stirs.Reaction kettle 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 accomplished, and esterification column backs down the beginning cooling.
(3), polyreaction operation: in system, add polymerizing catalyst, deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of controlled temperature, the open vacuum pump was slowly reduced to 2Kpa in 40 minutes; The rough vacuum polyreaction finishes, and closes vacuum system, under nitrogen protection and negative pressure condition, incites somebody to action the 226g UV light absorber that fusion the is good (mixture of
234 and
320; The ratio of the two weight is 1: 1), by the specific equipment injected system, mix after 3 minutes; With melting good 339g static inhibitor 103 injected systems; Continue to mix 2 minutes, the reaction kettle pressurization, the pre-polymerization melt gets into terminal polymerization kettle after the pre-polymerization strainer filters; Open high vacuum; Pressure is 40～100pa, under 270 ℃～280 ℃ conditions, carries out conventional polymerization, to reaching regulation viscosity; Stop polyreaction; Discharging pelletizing after polyreaction is accomplished obtains Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section 22.5kg, and its test result is seen table 1.
Embodiment 7
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1), esterification reaction section: get 18kg pure terephthalic acid (PTA), 70 liters of polyester experimental installations of 7.5kg terepthaloyl moietie (EG) adding; After stirring; Beginning to heat up and being forced into 0.3Mpa. and carrying out esterification, esterification temperature is controlled at 250～265 ℃, finishes to the esterification water outlet; Reply normal pressureization, finish reaction.
(2), secondary esterification reaction section: after an esterification is accomplished; At first add terepthaloyl moietie; Making temperature of reaction kettle reduce to 230～235 ℃, is polyoxyethylene glycol adding reaction kettle under nitrogen protection of 2000 then with the 450g number-average molecular weight that heating and melting is good, stirs.Add the 1.125g composite light stabilizer with above-mentioned mixed liquid form then, add the above-mentioned composite antioxidant of 3.375g with above-mentioned mixed liquid form.After finishing, adding stirs.Reaction kettle 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 accomplished, and esterification column backs down the beginning cooling.
(3), polyreaction operation: in system, add polymerizing catalyst, deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of controlled temperature, the open vacuum pump was slowly reduced to 2Kpa in 40 minutes; The rough vacuum polyreaction finishes, and closes vacuum system, under nitrogen protection and negative pressure condition, incites somebody to action the 113g UV light absorber that fusion the is good (mixture of the special UV light absorber CYASORB of UV light absorber
234 and cyanogen UV-3638F; The ratio of the two weight is 2: 1), by the specific equipment injected system, mix after 3 minutes; With melting good 275g static inhibitor (forming by weight 1: 1) injected system by static inhibitor 103 and static inhibitor 102, continue to mix 2 minutes, reaction kettle pressurizes; The pre-polymerization melt gets into terminal polymerization kettle after the pre-polymerization strainer filters, open high vacuum, and pressure is 40～100pa; Under 270 ℃～280 ℃ conditions, carry out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section 22.5kg, its test result is seen table 1.
Embodiment 8
Present embodiment provides the preparation method of a kind of Ginkgo Biloba Leaf Extract, the section of antistatic, anti-pilling polyester, and it comprises the steps:
(1), esterification reaction section: get 18kg pure terephthalic acid (PTA), 70 liters of polyester experimental installations of 7.5kg terepthaloyl moietie (EG) adding; After stirring, begin to heat up and be forced into 0.3Mpa, carry out esterification; Esterification temperature is controlled at 250～265 ℃; Finish to the esterification water outlet, reply normal pressureization, finish reaction.
(2), secondary esterification reaction section: after an esterification is accomplished; At first add terepthaloyl moietie; Making temperature of reaction kettle reduce to 230～235 ℃, is polyoxyethylene glycol adding reaction kettle under nitrogen protection of 2000 then with the 450g number-average molecular weight that heating and melting is good, stirs.Add the 1.125g composite light stabilizer with above-mentioned mixed liquid form then, add the above-mentioned composite antioxidant of 3.375g with above-mentioned mixed liquid form.After finishing, adding stirs.Reaction kettle 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 accomplished, and esterification column backs down the beginning cooling.
(3), polyreaction operation: in system, add polymerizing catalyst, deliver to prepolymerization kettle intensification polymerization after stirring; 260～275 ℃ of controlled temperature, the open vacuum pump was slowly reduced to 2Kpa in 40 minutes; The rough vacuum polyreaction finishes, and closes vacuum system, under nitrogen protection and negative pressure condition, incites somebody to action the 113g UV light absorber that fusion the is good (mixture of the special UV light absorber CYASORB of UV light absorber
234 and cyanogen UV-3638F; The ratio of the two weight is 2: 1), by the specific equipment injected system, mix after 3 minutes; With melting good 275g static inhibitor (forming by weight 1: 1) injected system by static inhibitor 103 and static inhibitor 102, continue to mix 2 minutes, reaction kettle pressurizes; The pre-polymerization melt gets into terminal polymerization kettle after the pre-polymerization strainer filters, open high vacuum, and pressure is 40～100pa; Under 270 ℃～280 ℃ conditions, carry out conventional polymerization; To reaching regulation viscosity, stop polyreaction, discharging pelletizing after polyreaction is accomplished; Obtain Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section 22.5kg, its test result is seen table 1.
Comparative Examples 1
This Comparative Examples provides a kind of preparation method of PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification reaction section: get 18kg pure terephthalic acid (PTA), 70 liters of polyester experimental installations of 7.5kg terepthaloyl moietie (EG) adding; After stirring, begin to heat up and be forced into 0.3Mpa, carry out esterification; Esterification temperature is controlled at 250～265 ℃; Finish to the esterification water outlet, reply normal pressureization, finish reaction.
(2), secondary esterification reaction section: after an esterification is accomplished; At first add terepthaloyl moietie; Making temperature of reaction kettle reduce to 230～235 ℃, is polyoxyethylene glycol adding reaction kettle under nitrogen protection of 2500 then with the 450g number-average molecular weight that heating and melting is good, stirs.Add the 1.125g composite light stabilizer with above-mentioned mixed liquid form then, add the above-mentioned composite antioxidant of 3.375g with above-mentioned mixed liquid form.After finishing, adding stirs.Reaction kettle 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 accomplished, and esterification column backs down the beginning cooling.
(3), polyreaction operation: add polymerizing catalyst, 113g UV light absorber
234 liquid or that fusion is good is added, mix after 3 minutes; With melting good 226g static inhibitor 102 injected systems, continue to mix 2 minutes the reaction kettle pressurization; The pre-polymerization melt gets into terminal polymerization kettle, 260～275 ℃ of controlled temperature, open vacuum pump after the pre-polymerization strainer filters; In 40 minutes, slowly reduce to 2Kpa, the rough vacuum polyreaction finishes, and opens 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 is accomplished obtains PET Resin/Poyester Chips Bottle Grade 22.5kg, and its test result is seen table 1.
Comparative Examples 2
This Comparative Examples provides a kind of preparation method of PET Resin/Poyester Chips Bottle Grade, and it comprises the steps:
(1), esterification reaction section: get 18kg pure terephthalic acid (PTA), 70 liters of polyester experimental installations of 7.5kg terepthaloyl moietie (EG) adding; After stirring, begin to heat up and be forced into 0.3Mpa, carry out esterification; Esterification temperature is controlled at 250～265 ℃; Finish to the esterification water outlet, reply normal pressureization, finish reaction.
(2), secondary esterification reaction section: after an esterification is accomplished; At first add terepthaloyl moietie; Making temperature of reaction kettle reduce to 230～235 ℃, is polyoxyethylene glycol adding reaction kettle under nitrogen protection of 3000 then with the 450g number-average molecular weight that heating and melting is good, stirs.Add the 1.125g composite light stabilizer with above-mentioned mixed liquid form then, add the above-mentioned composite antioxidant of 3.375g with above-mentioned mixed liquid form.After finishing, adding stirs.Reaction kettle 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 accomplished, and esterification column backs down the beginning cooling.
(3), polyreaction operation: add polymerizing catalyst; With the 113g UV light absorber (mixture of the special UV light absorber CYASORBUV-3638F of UV light absorber
234 and cyanogen liquid or that fusion is good; The ratio of the two weight is 2: 1); By the specific equipment injected system; Mix after 3 minutes,, continue to mix 2 minutes melting good 226g static inhibitor 102 injected systems; Reaction kettle pressurization, pre-polymerization melt get into terminal polymerization kettle after the pre-polymerization strainer filters.260～275 ℃ of controlled temperature, the open vacuum pump was slowly reduced to 2Kpa in 40 minutes; The rough vacuum polyreaction finishes, and opens high vacuum, and pressure is 40～100pa; Under 270～280 ℃ of conditions, carry out conventional polymerization,, stop polyreaction to reaching regulation viscosity; Discharging pelletizing after polyreaction is accomplished obtains PET Resin/Poyester Chips Bottle Grade 22.5kg, and its test result is seen table 1.
Table 1 Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section physical and chemical index
The quality index of the PET Resin/Poyester Chips Bottle Grade through the foregoing description and Comparative Examples can be found out; The PET Resin/Poyester Chips Bottle Grade of method preparation of the present invention has kept the quality index of conventional PET PET Resin/Poyester Chips Bottle Grade basically; 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 the Comparative Examples 1,2,, causing cutting into slices on the one hand the obvious flavescence of form and aspect because UV light absorber adds the change of mode, 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 terepthaloyl moietie.
Performance for the short silk level Ginkgo Biloba Leaf Extract of further checking the present invention preparation, antistatic, anti-pilling polyester section; The Ginkgo Biloba Leaf Extract that makes with embodiment 1,3,5,7 and Comparative Examples 1 respectively, the section of antistatic, anti-pilling polyester are raw material; Make through preparatory crystallization, drying, spinning, coiling, drawing and setting successively; Different with common PET polyester staple fiber spinning technique, this section is owing to add UV light absorber, static inhibitor, photostabilizer, oxidation inhibitor, the 3rd monomer, hydroxy silicon oil etc., and its section second-order transition temperature is lower; Therefore must just can implement section drying process through preparatory crystallization.
Above-mentioned preparation method is specific as follows: at first PET Resin/Poyester Chips Bottle Grade is carried out preparatory crystallization, 110 ℃～125 ℃ of Tc controls, time are 3～5 hours in advance.Carry out drying then, 130 ℃～145 ℃ of drying temperatures, the time is 3.5～5.0 hours.Carry out spinning after accomplishing drying.Use special crosssection spinning jets such as three leaves, cross, five leaves.At first on the short fiber spinning production line, produce through coiling, oiling process and process the short fiber tow, spinning speed 850m/min, spinning temperature are controlled at 255 ℃～278 ℃, (because a large amount of modified additives are used in this section; The section fusing point descends, in spinning process, and be according to the fusing point of copolyester section; Spinning and condition are adjusted, and the condition of implementing spinning compares the common PET trevira, and 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 stretch, the steam heat setting process, draft temperature is 142 ℃～150 ℃, 110 ℃～135 ℃ of heat setting temperatures; Behind the carrier bar drying process, cut off then, decide to weigh, pack and process finished fiber.Product specification is 1.56dtex/38mm, and its fiber volume fraction resistance test data are seen table 2.This fiber is made into knitting and woven fabric through spinning, through its correlation technique index of test is: uv transmittance≤5.0%, anti-pilling property>=4 grade have good Ginkgo Biloba Leaf Extract, anti complex function.The lining performance index are seen table 2.
In addition; Performance for the long filament level Ginkgo Biloba Leaf Extract of further checking the present invention preparation, antistatic, anti-pilling polyester section; Respectively with embodiment 2,4,6,8 and Comparative Examples 2 make PET Resin/Poyester Chips Bottle Grade carry out preparatory crystallization, in advance 110 ℃～125 ℃ of Tc controls, time are 3～5 hours.Carry out drying then, 130 ℃～145 ℃ of drying temperatures, the time is 3.5～5.0 hours.Carry out spinning after accomplishing drying.Use special crosssection spinning jets such as three leaves, cross, five leaves.At first will 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 fusing point descends, in spinning process, and 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 screw rod is respectively distinguished 8～15 ℃ of temperature downward modulations), POY fiber sprinning 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/72f has the hydroscopic fast-drying function, and its fiber volume fraction resistance is for seeing table 2.Fiber quality is good, and fiber is through the knitting and woven lining of processing, and through test, the lining performance index are seen table 2.
Table 2 Ginkgo Biloba Leaf Extract, antistatic, the high comfortable trevira lining performance of anti
Above-mentioned lining is mainly spring, summer, fashionable dress design in autumn; Therefore, except that having good Ginkgo Biloba Leaf Extract, antistatic, anti function; The present invention is according to this copolyesters special physicochemical characteristic; Three leaves of spinning or the special crosssection staple fibre and the specification of cross special-shaped 0.8～6.5dtex/2.5～specifications such as 10.6mm are 40～111dtex/24～96f long filament; This fiber has good Ginkgo Biloba Leaf Extract, antistatic, anti, 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, through its correlation technique index of test is: uv transmittance≤5.0%, anti-pilling property>=4 grade have good Ginkgo Biloba Leaf Extract, anti complex function.Measure wicking height >=120mm, vaporator rate >=0.20g/hr.
More than the present invention has been done detailed description, all equivalences of doing according to spirit of the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (10)
1. the preparation method of a Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section comprises the esterification operation and the polyreaction operation of carrying out successively, it is characterized in that:
Said esterification operation comprises esterification reaction section and secondary esterification reaction section; Wherein: a said esterification reaction section is implemented as follows: terephthalic acid, terepthaloyl moietie 1: 1.2 in molar ratio～1.3 is joined in the reaction kettle of the esterification, under 250 ℃～265 ℃, carry out one time esterification; Said secondary esterification reaction section is implemented as follows: after one time esterification reaction section is accomplished; Add terepthaloyl moietie, make system be cooled to 230 ℃～235 ℃, under protection of inert gas; Add number-average molecular weight and be 600～6000 polyoxyethylene glycol as the 3rd monomer; The 3rd monomeric add-on is 1.0%～6.5% of a PET Resin/Poyester Chips Bottle Grade weight, and mixed liquid and the mass concentration that adds mass concentration then and be 2%～5% hindered amine light stabilizer is the mixed liquid of 2%～5% Hinered phenols antioxidant, is benchmark with PET Resin/Poyester Chips Bottle Grade weight; The add-on of said 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 the solvent ethylene glycol and add acetic acid after gained pH value be 4～5 solution, the mixed 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 finishing; Reaction kettle begins to heat up; Slowly add hydroxyl value and be 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 add-on of wherein said hydroxy silicon oil is 0.1%～1.2% of a PET Resin/Poyester Chips Bottle Grade weight;
Said polyreaction operation is implemented as follows: in the system after the secondary esterification, add polymerizing 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; Prepolymerization reaction is closed vacuum system, under nitrogen protection and negative pressure after finishing; Liquid state or fused UV light absorber are injected, stirred, then the static inhibitor that fusion is good is injected; Stir, after strainer filters, deliver to terminal polymerization kettle, wherein; The add-on of said UV light absorber is 0.1%～2.0% of a PET Resin/Poyester Chips Bottle Grade weight, and the add-on of said static inhibitor is 0.5%～4.5% of a PET Resin/Poyester Chips Bottle Grade 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 accomplished, the discharging pelletizing got Ginkgo Biloba Leaf Extract, antistatic, anti-pilling polyester section.
2. the preparation method of Ginkgo Biloba Leaf Extract according to claim 1, the section of antistatic, anti-pilling polyester is characterized in that: described UV light absorber is one or more the combination in the UV light absorber of following kind: benzotriazole category UV light absorber:
326,
234,
350,
320,
328; Low volatility benzotriazole category UV light absorber
360; Red shift benzotriazole category UV light absorber
327; And
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 a PET Resin/Poyester Chips Bottle Grade weight.
3. the preparation method of Ginkgo Biloba Leaf Extract 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 the static inhibitor 308, and its add-on is 0.65%～2.5% of a said PET Resin/Poyester Chips Bottle Grade weight.
4. the preparation method of Ginkgo Biloba Leaf Extract 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-aggretion 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 the sebate are benchmark with PET Resin/Poyester Chips Bottle Grade weight, and the add-on of said hindered amine light stabilizer is 15～90ppm.
5. the preparation method of Ginkgo Biloba Leaf Extract according to claim 1, the section of antistatic, anti-pilling polyester; It is characterized in that: described Hinered phenols antioxidant is Irganox 1076; Among Irganox 1010 and the Irgafos 168 one or more; With PET Resin/Poyester Chips Bottle Grade weight is benchmark, and the add-on of described Hinered phenols antioxidant is 30～250ppm.
6. the preparation method of Ginkgo Biloba Leaf Extract according to claim 1, the section of antistatic, anti-pilling polyester; It is characterized in that: with PET Resin/Poyester Chips Bottle Grade weight is 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.
7. the preparation method of Ginkgo Biloba Leaf Extract 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.
8. the preparation method of Ginkgo Biloba Leaf Extract according to claim 1, the section of antistatic, anti-pilling polyester; It is characterized in that: described number-average molecular weight as the 3rd monomeric polyoxyethylene glycol is 1500～4000, and add-on is 1.5%～4.0% of a PET Resin/Poyester Chips Bottle Grade weight.
9. according to the preparation method of the described Ginkgo Biloba Leaf Extract of each claim in the claim 1 to 8, antistatic, anti-pilling polyester section; It is characterized in that: said fiber is a staple fibre, and the add-on of described hydroxy silicon oil is 0.6%～1.2% of a PET Resin/Poyester Chips Bottle Grade weight.
10. according to the preparation method of the described Ginkgo Biloba Leaf Extract of each claim in the claim 1 to 8, antistatic, anti-pilling polyester section; It is characterized in that: said trevira is a long filament, and the add-on of described hydroxy silicon oil is 0.1%～0.8% of a PET Resin/Poyester Chips Bottle Grade weight.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108624010A (en) * | 2018-06-07 | 2018-10-09 | 广东轻工职业技术学院 | A kind of electrostatically dissipative high grade of transparency polyester and preparation method thereof |
| CN113638110A (en) * | 2021-09-16 | 2021-11-12 | 福州市晟浩纺织科技有限公司 | Manufacturing method of quick-drying polyester fabric |
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| CN113638110A (en) * | 2021-09-16 | 2021-11-12 | 福州市晟浩纺织科技有限公司 | Manufacturing method of quick-drying polyester fabric |
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